svc summer 2004 nb

Summer 2004www.svc.org

NewsNews

A P u b l i c a t i o n f o r t h e V a c u u m C o a t i n g I n d u s t r yA P u b l i c a t i o n f o r t h e V a c u u m C o a t i n g I n d u s t r y

What’s Inside:TechCon Perspectives from

the Program Chairs 4

Vacuum Coating—AnEnabling Technology 21

Advances in Multi-ComponentSputter Deposition 25

What’s Inside:TechCon Perspectives from

the Program Chairs 4

Vacuum Coating—AnEnabling Technology 21

Advances in Multi-ComponentSputter Deposition 25

2004 Summer News Bulletin 3

First, a big thank you to the membership for attending the 47th Annual Society of Vacuum Coaters(SVC) Technical Conference (TechCon) held at the Adam’s Mark Hotel in Dallas, TX. You made it

a huge success!Next, I want to thank the people who worked so hard to put on the TechCon: our management

organization (MPI) led by Vivienne and Don Mattox, the Technical Program Committee chaired byRic Shimshock and Ludvik Martinu, and all the members of the Technical Advisory Committees(TACs). This year for the first time our conference ran for four days due to the addition of the SmartMaterials Symposium, jointly sponsored by SVC and Elsevier Publications. This Symposium was verywell attended, and we plan to continue the four-day format at the 2005 TechCon in Denver.

The TechCon opened with the Keynote Lecture by Dr. Chikara Hayashi of ULVAC speaking onUHV processing and applications. Outstanding technical sessions followed and are discussed later inthis issue by the TAC Chairs. Other TechCon program highlights included the Technology ForumBreakfasts, the Heuréka! Sessions for post-deadline developments, and The Donald M. MattoxTutorial Program. As always, we offered a wide variety of excellent short courses, providing trainingat all knowledge levels and taught by industry and academic experts in the various fields. TheTechCon also featured, I believe, the best array of exhibitors in our industry.

Sunday evening, Nobel Prize winner, Dr. John B. Fenn, gave the Plenary talk, which was simplydelightful. Professor Fenn told the entertaining human side of the struggles in the developments ofelectrospray, the vacuum techniques used to ionize large organic molecules.

Preceding the Plenary talk, election results were announced at our annual business meeting.We welcomed two new SVC Board of Directors members: Doug Smith and Michael Andreasen. Onbehalf of the Society, I want to thank outgoing Board members, Angus Macleod, Don McClure, andTony Broomfield for their many years of valuable service. Don McClure left the Board after servingadmirably as Secretary of the Society (and Director) for several years. Your new SVC Officers includeDave Glocker, Secretary; Peter Martin, Vice President; and Clark Bright, President. John Feltsbecame immediate Past President succeeding Tony Broomfield.

At the Awards Ceremony, we honored our 2004 SVC Mentors (Russ Hill, Harold Gadon, andRichard Swisher) for their major contributions to the vacuum coating industry. Please join with mein congratulating them for their outstanding careers and thanking them for their willingness to sharetheir knowledge with others. The 2004 SVC Sugerman Award recipient is Don McClure. Don hascontributed greatly to our industry, especially in web coating technology, and to the SVC in amultitude of areas. A special award was also presented to our SVC Technical Director, Don Mattox.In recognition of his major technical contributions and SVC service, we have officially named thetutorials at the TechCon, the Donald M. Mattox Tutorials.

The above is just a sampling of the activities at the 2004 TechCon. I hope you didn’t miss it!Mark your calendar now for next year; the TechCon is April 23–28, 2005, in Denver, Colorado!

Looking forward, your new Board and Officers will attend the SVC summer Board meeting inmid June at the site of the TechCon in 2005. In addition to our regular business meeting, we also willhave a training session the prior evening to orient and focus the new Board and Officers on strategicSVC topics. We are challenged with many strategic issues, including growing the Society whileensuring that we retain the friendly spirit and industry focus that has made us successful. Pleasehelp us to be successful in these tasks by providing your opinions and feedback. You may contact me([email protected]), Vivienne Mattox ([email protected]), or any member of the Board.And, if you really are interested in further influencing the course of SVC, join a TAC, run for theBoard, and become an Officer. We need your ideas, your help, and your support. Remember, this isYOUR Society.

Clark Bright, 3M Company ([email protected]), is the SVC President.

Letter from the President Board of Directors

PresidentClark Bright3M [email protected]

Vice PresidentPeter MartinBattelle Pacific Northwest [email protected]

Immediate Past PresidentJohn T. FeltsNano Scale Surface Systems, [email protected]

SecretaryDavid A. GlockerIsoflux [email protected]

TreasurerEdward WegenerAFG Industries, [email protected]

DirectorsMichael AndreasenVON ARDENNE Coating [email protected]

Hana BaránkováUppsala [email protected]

Pamela DiesingSAGE industrial sales, [email protected]

Elizabeth JosephsonApplied Films [email protected]

Traci LangevinSoleras [email protected]

Ludvik MartinuÉcole [email protected]

Paolo RaugeiGalileo Vacuum Systems, [email protected]

Ric ShimshockMLD Technologies [email protected]

Douglas SmithVacuum Process Technology, [email protected]

Frank ZimoneDenton Vacuum, [email protected]

SVC Administrative Offices71 Pinon Hill Place NEAlbuquerque, NM 87122-1914

Telephone 505/856-7188 Fax 505/856-6716E-mail [email protected] Site www.svc.org

Executive DirectorVivienne Harwood Mattox

Technical DirectorDonald M. Mattox

Inside This Issue

Cover Photo: Triode Sputtering System, R.D. Mathis Company, 1967.

TechCon Perspectives from theProgram Chairs . . . . . . . . . . . . . . . . . . . . . 4

Sample Education Guide . . . . . . . . . . . . . 18by Donald M. Mattox

SVC TechCon Exhibit is Well Received. . . 20

Vacuum Coating—An EnablingTechnology . . . . . . . . . . . . . . . . . . . . . . . . 21Tutorial by Donald M. Mattox

Effective Closed-Loop Control forReactive Sputtering Using TwoReactive Gases . . . . . . . . . . . . . . . . . . . . . 25by D.C. Carter, W.D. Sproul, and D.J. Christie,Advanced Energy Industries, Inc.

Corporate Sponsor Profile . . . . . . . . . . . . 28

Corporate Sponsor News . . . . . . . . . . . . 29

Society and Industry News . . . . . . . . . . . 30

TechCon Perspectives from theProgram Chairs

The Dallas TechCon was a success! Feedback from the many attendees wasoverwhelmingly positive, and the internal metrics we keep on the TechCon

are also good. We certainly hope you were able to make it to the 47th Society ofVacuum Coaters (SVC) TechCon held April 24–29th at the Dallas Adam’s MarkHotel and participate in some of the many networking opportunities, partake insome of the educational offerings, spend some time in the exhibit hall withsome of the many vendors who make the TechCon their conference of choice,listen and dialogue with the many interesting TechCon lectures and presenta-tions, and catch up with old friends. For those who did participate, weappreciate your investment in time and talents in keeping the SVC TechConstrong and vital. We also appreciate that many of you did take advantage of thegood lodging rates at the Adam’s Mark Hotel. By electing to stay at the confer-ence hotel, our attendees help keep the cost of TechCon reasonable.

The time invested by the Program and TAC Committees and the MPI teampaid off handsomely for the attendees during the four full days of this well-runevent. Even with the addition of an extra day, the days were still full! One ofour goals was to increase the time for networking, and secondly, to create moretime in the program that would allow a trip to the exhibits that did not competewith the many interesting oral presentations at the TechCon. Convening theSVC/Elsevier Smart Materials Symposium at our TechCon allowed us to adjustthe TechCon sessions over four days. While we intend to tweak this formatslightly for the upcoming TechCon in Denver, judging by the number of sidemeetings that took place in Dallas and the traffic in the exhibit hall, we thinkwe made good progress on achieving both goals.

The TechCon ran smoothly over the course of the four days. The days werefilled with interesting events running from breakfast to late in the evening. TheProgram Committee and the TACs assembled a strong program. The sessionswere full and the addition of the Smart Materials Symposium brought some newfaces to the TechCon. Based on the success in Dallas we have decided tocontinue a similar forum and format next year. The Program Committee isalready at work lining up interesting speakers for next year. We will also run theDenver TechCon over fours days as we did in Dallas.

The venue at the Adam’s Mark Hotel worked extremely well. It providedample space for a sit-down meeting with friends and colleagues and for makingnew acquaintances. We will maintain our approach of co-locating the hotel andmeeting rooms for the Denver TechCon. If you have opinions on this—positiveor negative—please share these with our SVC Future Sites Committee ChairPamela Diesing ([email protected]) and Vivienne Mattox, our ExecutiveDirector and Meeting Planner ([email protected]).

The Plenary talk on Sunday evening by the Nobel Prize winner, Dr. John B.Fenn (father of our own Nat Sugerman Award winner and Past President Dr.John B. Fenn, Jr.), was well attended and was very enlightening andentertaining. The topic of “Electrospray Wings for Molecular Elephants” toldthe story of the many struggles and developments needed to establish thevacuum techniques necessary to ionize large organic molecules. This techniqueis used widely now, and will have many future impacts on the characterization ofbiological molecules. Professor Fenn gave us a very human view of the develop-ments in this exciting field.

The Plenary talk was preceded by the Awards Ceremony, which highlightedthe contributions made by our 2004 SVC Mentors, Russ Hill, Harold Gadon, andRichard Swisher, and the 2004 Sugerman Award Winner, Don McClure. A specialaward was made to our SVC Technical Director, Don Mattox by henceforthrenaming the Lunchtime Tutorials as The Donald M. Mattox Tutorial Program.

We were honored this year to have Dr. Chikara Hayashi of ULVAC presentthe Keynote TechCon Lecture on the many applications of UHV Processing. Dr.Hayashi provided us with an overview of the many implementations that thispowerful technology has played in enabling many materials processing applica-tions such as the preparation of specific nanoparticles. He also reviewed someof the many innovations that the researchers at ULVAC developed over thedecades and showed some very interesting results from their collaborations withresearchers.

4 2004 Summer News Bulletin

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The tutorials by Charlie Bishop, Don Mattox, and Don McClure continuedto be a great success. Traditionally, these tutorials are well attended and verystimulating. Once again the turnout was high, and the discussions carried onpast the allotted time and continued over the course of the TechCon. We lookforward to further stimulating tutorials in Denver.

Because we had more room in the TechCon program for extendedTechnology Forum Breakfasts, we increased both the number of topics andconvened them on Tuesday and Wednesday. They were well attended; in fact,they were so well attended that we will need to refine the format so that ageneral discussion could be held with so many participants. The “Meet theExperts” sessions went well and were extended to a three-day offering.

The success of the Heuréka! session continued, and the format was extendedthis year to include two full sessions. The attendance was high, and the contribu-tions were interesting. We look forward to the continued success of this forum.The Joint Sessions also worked out well in Dallas, and we look to more use of theJoint Sessions in our future TechCons. We also had a good collection of postersthis year and excellent student participation at the TechCon.

Look to the summaries by the TAC chairs of the highlights of their sessionslater in this bulletin. I will mention one item here that is of considerableinterest and that is that we intend to hold a special session on high-powerimpulse magnetron sputtering (HIPIMS) as a highlighted topic in a PlasmaProcessing Session in Denver. Save your presentations and be sure to mark yourcalendar.

In summary, it was a very successful TechCon. Many people worked veryhard to pull off this event, and it paid off. We made some changes, and theyseemed to get a positive response. However, we are always looking for your inputon the program. Finally, think about joining a TAC, and more importantly, thinkabout making a presentation. We look forward to reviewing your abstracts forDenver this coming October.

Ric Shimshock, MLD Technologies LLC ([email protected]), and LudvikMartinu, École Polytechnique, Montreal, Canada ([email protected]), are the2004 and 2005 SVC Program Chairs.

Emerging Technologies

The Monday afternoon Emerging Technologies session of SVC’s TechCon 2004opened with an invited presentation by Gerhard Pfaff from Merck KGaA on

special-effect pigments. Most of these optical and functional coatings consist ofnanostructured metal oxides on thin mica platelets or on silica, alumina and metalflakes, or are based on liquid crystal polymers (LCP). Aims of new developmentsare new effects and colors, increased stability, improved dispersibility, andfunctional properties. Uwe Beck of BAM Berlin introduced a versatile clustersystem consisting of three clusters: PECVD cluster, ion-assisted electron beamevaporation, and sputter clusters. The effect of process parameters on layerquality was shown for optical multilayers. Lad Bárdos of Uppsala Universityfollowed with a presentation on hot hollow cathode arc deposition of highlyoriented Cr and CrN. Reactive PVD rates for highly oriented, dense CrN on steeland silicon reach values as high as 4.5 µm/min. Bill Sproul from Advanced EnergyIndustries, Inc., reported on the reactive sputter deposition of dielectric Al2O3coatings using high-power pulsed magnetron sputtering (HPPMS) with oxygenpartial pressure control and arc handling capabilities in the power supply.Comparison with pulsed DC power sputter deposition was given.

Peter Siemroth of Arc Precision GmbH kicked off the EmergingTechnologies session on Tuesday afternoon with the invited presentation onindustrial precision deposition by filtered high curent pulsed arc. Ultrathincoatings deposited by filtered high current pulsed arc exhibit enhancedhardness, mass density, and scratch resistance compared to PECVD ormagnetron sputtering. Hynek Biederman from Charles University, Prague,reported on RF magnetron sputtering from polymeric targets. Emission of ionsfrom the discharge and ion flux effect on the deposition process were investi-gated. David Christie from Advanced Energy Industries, Inc., presented a designof a new pulsed-power supply for HPPMS. The power supply has pulse leading-edge control and arc suppression capability, enabling deposition from materialsas carbon and aluminum. Wilfred Kittler of Gnomic Enterprises devoted hispresentation to a novel method for the continuous production of unsupported

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nanoparticles and nanosheets. Substrateless deposition methods simplify theproduction process of “thin film particles”. The final presentation by Tal Davidfrom Tel Aviv University featured p-type Sb-doped ZnO growth by filteredvacuum arc deposition.

Hana Baránková, Uppsala University ([email protected]), and LadBárdos, Uppsala University ([email protected]), are the EmergingTechnologies TAC Co-Chairs.

Heuréka! Post-Deadline RecentDevelopments

The “Heuréka!” session is a very important and prestigious forum forimportant late-breaking results at the SVC TechCon. After its premiere in

2003, the program at the 2004 TechCon in Dallas expanded considerably intotwo very interesting evening sessions.

The Monday evening session began with the presentation by Jay Lewisfrom MCNC R&D Institute on electromechanics of highly flexible transparentconductors for display applications. Thin film stacks of ITO/Ag/ITO weredescribed to have favorable properties over single ITO films. Klaus Nauenburgfrom Leybold Optics GmbH discussed the quality of plasma-polymerizedcorrosion-resistant layers of new materials in large-scale coating machines forproduction of car reflectors. He introduced new siloxanes and their mixtureswith gases for higher PECVD rates and better corrosion resistance of polymer-based films. Tansel Karabacak from Polytechnic Institute introduced a newstrategy in stress reduction in sputter-deposited thin films that use physicallyself-assembled nanostructures as compliant layers. Decrease of stress (e.g., insputtered W films) allows much better adhesion and a higher limiting filmthickness. David Glocker from Isoflux Incorporated presented results of jointwork with Advanced Energy Industries, Inc., on high-power pulsed reactivesputtering of zirconium oxide and tantalum oxide. This novel approach offersvery encouraging improvements to the reactive sputtering process. CorinneNouvellon from Materia Nova described a novel hybrid plasma system based oninternal inductively coupled plasma combined with magnetron sputtering forfast deposition of Ti and TiO2 films at low pressure (10-4 mbar range) in a semi-industrial coating chamber (0.5 m3). The last presentation on Monday eveningwas given by Nicola Magriotis from the Arcotronics Nissei Group with co-authorsfrom the University of Udine about the vacuum deposition of thick multi-layerson thin flexible polymer substrates. Solving thermal load problems in the fastcoating of Cu and Al thick layers on thin web was discussed.

The Tuesday evening session began with the presentation of Bernd Szyszkafrom Fraunhofer Institute for Surface Engineering and Thin Films (IST) onmodeling the reactive sputter process in in-line coaters for architectural glassand its experimental verification. A sophisticated computer simulation modelcan generate detailed data on the overall process and could allow completecomputer control of the real production systems. Hallgeir Klette from SintefMaterials Technology described sputtering of very thin Pd-alloy hydrogenseparation membranes. The free-standing Pd foils have diverse applications inhydrogen-related processes. Holger Nörenberg from Technolox Ltd. presentedresults of work with the University of Oxford on recent developments inmeasuring permeation through barrier films and an understanding ofpermeation processes. The work is of interest for testing barrier films (e.g., inthe food industry). Gail Ludtka from Oak Ridge National Laboratory presentedjointly with individuals from the HY-Tech Research Corporation on aluminumsoldering performance testing of H13 steel coated with boron by the cathodicarc technique. Boron has unique properties due to its highly attractive interac-tion for steel and a repulsive chemical interaction for aluminum. Reiner Kuklafrom Applied Films GmbH & Co. KG described a new modular roll-to-roll PVDweb coater for cleanroom production. Construction details of this novel systemwere discussed with the audience.

The session was closed by the presentation of W. Klug from Leybold OpticsGmbH about the innovative production of high-quality optical coatings forapplications in optics and optoelectronics. A sophisticated system with optical

TechCon Perspectivescontinued from page 5


monitoring and inductively coupled plasma combined with dual magnetronsputtering in a device with load lock and cassette substrate handling wasproved to produce optical multilayer coatings with outstanding properties.

The “Heuréka!” sessions in Dallas were a big success, reflected by arecord interest of conference participants and stimulating questions anddiscussions from the audience. The sessions were a great forum for exciting“hot-off-the-press” developments at the TechCon.

Lad Bárdos, Uppsala University ([email protected]), and HanaBaránková, Uppsala University ([email protected]), are theHeuréka! Session Chairs.

Innovators Showcase

The 2004 Innovators Showcase once again raised the bar in terms of qualityand relevance of the subject matter. Special thanks go out to all the

participants who took the time and energy to craft a fascinating roster ofpresentations. The Adam’s Mark hotel afforded us ample room and, onceagain, the SVC staff did a fabulous job ensuring that everything ran smoothly.

Extending the conference for a day and reducing the number ofparallel conference sessions from four to three had a dramatic impact onattendance at the Innovators Showcase. This is quite a change from thedays (which were not all that long ago) where the majority of the attendeeswere “booth mates” and competitors! We’re on a roll. Let’s continue oursuccess in Denver next year!

Frank Zimone, Denton Vacuum LLC, ([email protected]) is the SVCInnovators Showcase organizer.

Joint Session

This was the third consecutive year of the Special Joint Session focusingon Display Technologies. This continues to be the hot topic within the

SVC community. Again, this session was organized by the Chairs of the

Optical Coating, Web Coating, and Large Area Coating TACs. The Tuesdaymorning session was moderated by Ludvik Martinu of École Polytechniqueand Peter Moulds of Ursa International. The session was kicked off whenMartinu introduced the invited presentation, Mechanisms of VaporPermeation through Multilayer Barrier Films, by Gordon Graff of PacificNorthwest Laboratory. This presentation discussed a thin film oforganic/inorganic composite layers on PET that can achieve excellent watervapor permeation rates; further improvements of flexible thin film vaporbarriers were discussed. Influence of DC and MF-Sputter Technology on theQualities of ITO Layers on PET Film and Glass was the second presentationof the Joint Session and was made by Hans-Georg Lotz of Applied FilmsGmbH. This presentation described the work, tests, and results ofcomparing conventional DC and MF sputtering of ITO layers. The pros andcons of both methods were discussed. The third presentation of the sessionwas Control of Transparent Conductive and Antireflection CoatingsDeposition Process by Viktor Kozlov of Sidrabe, Inc. The presentation dealtwith criteria for estimation of the overall performance of magnetronsputtering systems for the deposition of oxide coatings in the reactiveprocess. Osamu Sakakura of Dia Nippon Printing Company gave the nextpresentation entitled, Anti-Reflection Coating by PECVD on FlexibleSubstrate. This presentation discussed the increasing need for antireflec-tive films brought about by the display market and the use of PECVD as atemperature and cost advantage for deposition. Paul Hambourger ofCleveland Sate University presented a very interesting discussion, SlightlyConductive Transparent Films for Space Applications: Manufacturing andDurability. Solar panels and other spacecraft surfaces need protection dueto charging by particles emitted from the Sun. Vacuum coating of highlytransparent, slightly conductive films may be the solution.

The final activity for the Joint Session was the Workshop on VacuumCoated Flexible Webs for Use in Displays. Again, a special thank you toJohn B. Fenn, Jr., for coordinating this panel discussion and to those whoparticipated in this well-attended event. The panel members were:

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Johannes Strümpfel of VON ARDENNEANLAGENTECHNIK GmbH; Hans-Georg Lotz ofApplied Films GmbH; Mohtashim Saif ofCPFilms, Inc.; Steve Sargeant of Toray PlasticsAmerica; Robert Rustin of DuPont Teijin;Charles A. Bishop of C.A. Bishop Consulting Ltd.;and Don McClure of the 3M Corporate ResearchMaterials Laboratory. After an overview by JohnB. Fenn, Jr., each panel member presented abrief summary of their company’s developments,concerns, plans, and progress toward a trulyfunctional flexible display. A brief audiencediscussion followed.

The panel members represented manyaspects of the market for the use of vacuumcoated flexible webs in the display industry, bothpresent and future. Even though they camefrom diverse backgrounds such as the vacuumequipment manufacturers, the substrateproducers, the vacuum converts, and end users,there was a definite consensus reached onseveral important points during the discussion.The following is a summary of the critical pointsthat were raised.

• The substrate itself was identified as oneof the keys to a successful entry into the displaymarket. It was obvious that “standard” polymerfilms off the shelf do not have the properties ofsurface smoothness, low debris contamination,and process temperature compatibles thatcurrent designs of flexible displays require.However, the issue of the cost of engineering andmaking acceptable flexible substrates keptcoming up. The general feeling was that unlessthere was a “killer application” that could onlyuse plastic materials, glass substrates wouldremain competitive.

• It was pointed out several times that thesheet resistivity of the transparent conductivecoatings was currently not low enough forOLEDs and other applications. Also, the risingcost of indium is causing concerns in this marketthat is now based on using indium tin oxide asthe TCO of choice.

• Substrate handling and processing these

materials in a suitable cleanroom environment,estimated to be at least class 100, were alsomentioned by many of the panel members. Also,the yield factors involved with every processingstep were stressed as well.

• The ever-present issue of suitable vaporbarrier layers was raised continuously. It is stillnot clear that a cost-effective and robust barriermaterial exists for use with plastic-based OLEDs.However, there were many other flexible displaydesigns, such as e-paper and lids that do nothave as stringent requirements as the OLEDmaterials do.

• The last issue consistently mentioned wasthe question, “Is there enough marketinginformation available now that could help guidepotential manufacturers in decisions of where toinvest the capital and development effort?”Right now there are many opportunities, but willall of them succeed?

In spite of the concerns enumerated, theoverall feeling presented by the panel was one ofoptimism. Almost everyone on the panel feltthat there were good opportunities valuable tomembers of the flexible vacuum coatingcommunity to participate in this opportunity,even if it is not clear yet where the best bet lies.

Peter J. Moulds, Ursa International Corporation([email protected]), Ludvik Martinu, ÉcolePolytechnique ([email protected]), andMichael Andreasen, VON ARDENNE CoatingTechnology ([email protected]), workedjointly to develop this session.

Large Area Coating

Thanks to all of the presenters who, duringthe two Large Area Coating Sessions of the

2004 SVC TechCon, covered a broad range ofapplications, processes, equipment, and basicimprovements in technology of interest to theLarge Area Coatings community.

Highlights of the first session included thefollowing. Steve Selkowitz, Lawrence BerkeleyNational Laboratories, led off the session onTuesday morning, presenting an invited talktitled, Saving $40B per year: Performance Needsfor Energy-Efficient Coated Glazings inBuildings. Selkowitz showed that buildingsaccount for one-third of all energy use in the

United States and showed ways that coatings canhelp meet the U.S. Department of Energy goal of“Zero Energy Buildings” by 2025. Data werepresented on the costs and impacts that solarcontrol, low emissivity, and active coatings havehad and can have on HVAC load in buildings indifferent climate areas—enough to meet theDOE goal if combined with innovative fenestra-tion technologies to reach U values under 0.15.In fact, one low-E coater capable of producing200 million square feet per year of low-emissivitycoatings can save the equivalent of 36 milliongallons of oil—and that equals the production ofone off-shore oil platform. This presentation wasfollowed by three discussions in the area ofreactive sputtering of SiO2 and TiO2, two of themost important materials for large area coatings.

Roman Nyderle of Fraunhofer presentedReactive Pulsed-Magnetron Sputtering of SiO2:Influence of Process Parameters on LayerProperties. This presentation explained usingpulse-packet mode deposition as a means toadjust layer properties in SiO2 and other reactedmaterials. Deposition rate, residual stress, andsurface roughness were shown to be conjointlyinfluenced by changing the pulse parameterswhile holding other deposition conditionsconstant.

John Davis of Applied Films presentedHigh-Power Pulse Reactive Sputtering of TiO2 inwhich he showed that the deposition rate usingHPPMS with a rotary magnetron is less forcomparable power than DC sputtering; but,there is an increase in the index of refraction,possibly due to increased density of thedeposited films. Phil Greene of VON ARDENNEpresented Plasma Emission Monitoring of Low-Rate Materials on Rotating CylindricalMagnetrons. Greene showed new data on thePEM closed-loop control system operating highon the transition curve with SiO2 and TiO2. ForTiO2, stable deposition rates of up to six timesthe 100% O2 rate with +/- 2% cross-coaterthickness uniformity with on-average operatorintervention only every four hours were attained.For SiO2, deposition rates of five times the 100%O2 rate with +/- 2% uniformity were achieved.

Dermot Monaghan of Gencoa thenpresented Principles and Techniques for



Thickness Uniformity Control in Planar Magnetron Sputtering. Monaghanshowed how to use variables of target size, target-to-substrate separation,substrate motion, magnetic field design, materials, and gas pressure to simulatethe coating distribution. We then had three presentations discussing improve-ments to sputtering equipment.

Jim Rietzel of VON ARDENNE led off with Enhancements to RotatingCylindrical Magnetrons in which he discussed recent improvements to rotatingcylindrical magnetrons for higher quality and lower cost. Rietzel showed theoperating principles of a new AC (or DC) end block designed to run at up to 400amps and an improved magnet bar incorporating a center support for improvedcross-coater uniformity. Data were shown from full-width industrial coaterssupporting +/-2% thickness uniformity or better at high rates for all of thenormally used reacted materials. Rietzel also showed the results of experimentswith slow-sputtering metal rings at the ends of the targets that allow targetutilization into the 90+ % range.

Michael Geisler of Applied Films presented Latest Developments andApplications of Large Area Coaters. Geisler showed recent progress on anarchitectural glass horizontal coater design with respect to chamber configura-tion, process tooling, and process control technology. Geisler discussed flexiblebays (pump/cathode), tooling for uniformity, closed-loop process control, andtheir impact on improving cross-coater and lead-to-trail thickness uniformity.Examples of use for heat-treatable coatings were provided.

Thomas Rettich of Huettinger presented Arc Management in DC and MFGenerators for Large Area Coating Systems, a favorite topic for large areacoaters. Rettich showed how Huettinger’s digital signal processor (DSP) basedarc suppression system with adaptable (user-configurable) parameters can beconfigured to stabilize deposition at optimum deposition rate, film quality,homogeneity, and optical properties. Examples from production coating systemswere provided.

The final presentation of the first session was made by Johan Zijp, TNOTPD, on the topic High Rate Evaporation of Alloys, which explained the use ofchoked orifices in the vapor streams that, when properly disposed, can independ-ently control the vapor flow for mixing and compositional control on thesubstrate. Zijp showed results from the deposition of Zn-Mg on a coiled metalstrip where the deposition rate could be predicted from the temperature of thevapor generator.

Highlights of the second session on Large Area Coating included thefollowing. The first four papers constituted a mini-conference on targets andtarget technology. James Finley of PPG led off with an invited presentation,Effects of Methods of Manufacturing Sputtering Targets on Characteristics ofCoatings. Finley discovered that starting with the same composition of pre-alloyed TiAl powders, hot isostatic pressed targets showed a very fine grainmicrostructure with no porosity versus cast targets, which showed shrinkageporosity and a variation in grain size ranging from fine near the edges to verycourse in the center. Even so, there was essentially no difference in DCsputtered film properties, deposition rates, or arcing rates.

Frank Jürgens of Fremat followed with Rotatable ZnO Targets: a NewGeneration of Ceramic Targets. Jürgens showed a capability to manufacturehomogeneous ZnO targets with 95% theoretical density. These are made bymixing the materials at high energy, pressing and sintering up to 25 mm thicktube segments, then joining the tube segments onto a steel cylindrical backingtube. Such targets have been successfully tested in a large area coater for aboutsix months.

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The next presentation was by Falk Milde ofVON ARDENNE on Sputtering of Conductive ZAOFilms from Metallic and Ceramic Targets UsingPlanar and Cylindrical Magnetrons. Thereactive cylindrical magnetron ZAO depositionprocess was investigated and compared toplanar reactive and ceramic target depositionprocesses. Good layer properties were obtainedwith both planar cathodes and cylindricalmagnetrons, using DC, pulsed-DC, and AC powerin the transition mode. With thick layers, layerproperties close to the theoretical limit wereobtained as shown by SEM micrographs, XRDdata, and optical modeling. The AC cylindricalmagnetron reactive ZAO deposition seems to bevery promising, especially with regard to lack ofnodule growth, which can limit production whenusing planar cathode processes.

The last presentation in the target mini-conference was presented by Jocelyne McGeeverof Technology Assessment International on thetopic New Sputtering Targets: to Test or Not toTest? Using the example of silicon aluminumtargets, McGeever showed how a sensitivityanalysis of the cost versus potential benefit priorto committing to testing can help make thedecision about whether or not to spendresources on testing.

The next presentation, by Guy Buyle ofGhent University, discussed Characterization ofthe Electron Movement in Varying MagneticFields and the Resulting Anomalous Erosion.Anyone interested in improving magnetronperformance will be interested in reviewing thispresentation that shows, for example, that theheight of ionization above a target surface candecrease when the electrons go from a strong toa relatively weak magnetic field.

Russ Pylkki of Aspen Research then gave arare glimpse into the requirements of end usersin his presentation, Glass Coating: What WindowManufacturers Want. Pylkki provided numerousdata on the residential window market,discussing how it has grown and the conditionsfor further growth of coatings. For example,Pylkki showed that of the 100 million residencesin the United States, approximately 10% havelow emissivity coatings, due to the preponder-ance of older homes. This means there is still agreat opportunity for low emissivity coatings inthe United States. Windows are being replacedat about 2 to 3% per year now and 50% or betterof these have low emissivity coatings. Accordingto Pylkki, going forward, window manufacturerswant temperable, low-emissivity coatings withhigh selectivity, antireflective, and self-cleaningproperties, as well as dynamic coatings forshading and privacy. Pylkki states thatconsumers would be willing to pay $5,000 to save$1,000 per year in energy costs.

Soren Berg of Upsalla University followedwith a presentation on The Influence of Rotating

Magnets on Hysteresis in Reactive Sputtering.In this presentation, Berg discussed the case ofthe rotating cylindrical magnetron where thetarget is rotating through a fixed magnetic fieldand when not in the field itself is subject toovercoating and chemical reaction with reactivegases to produce slow sputtering compounds. Amathematical model of the dynamic system waspresented and validated with experimentalobservations, one of which is that the speed oftarget rotation influences the reactive sputteringprocess so that the hysteresis region is shifted.

Anja Blondeel of Bekaert followed withOptimizing AC Switching Parameters forRotating Cylindrical Magnetron Sputtering inwhich some surprising results were presented.Blondeel showed that there is a loss of powerwith increasing power supply frequency, which ispartially dependent on the sputter gas (oxygen,-12%) having twice the loss of argon or nitrogen.The experimental setup used a commerciallyavailable variable frequency-switching unit incombination with a DC power supply.

Also shown was that process parameterssuch as plasma restoration time, anode voltage,arc rates, cross-coater uniformity, and depositionrate are also frequency- and sputter-gasdependent, with arc rate decreasing at higherfrequencies, and uniformity and deposition rateincreasing at lower frequencies.

The final presentation of the session wasCylindrical Magnetron Sputter Deposition ofChromium Coatings for Erosion- and Wear-Resistant Application made by KrystynaTruszkowska of Benet Laboratories. Thisinteresting presentation discussed sputtercoating as an environmentally friendly way tocoat a chromium hardcoat on the bore (inner)surface of long gun tubes. Data on the resultantcoating hardness, adhesion, fracture, etc. werepresented and thoughts on how to improvehardness were proposed.

All in all the Large Area sessions provideda wide assortment of technology updates tochallenge our thinking processes and stimulatefurther advances in the field.

Michael Andreasen, VON ARDENNE CoatingTechnology ([email protected]), is theLarge Area Coating TAC Chair, and JohannesStrümpfel, VON ARDENNE ANLAGENTECHNIKGMBH ([email protected]), is theAssistant TAC Chair.

Optical Coating

From the point of view of those interested inOptical Coatings, the 2004 Technical

Conference of the SVC was again very successful.The three half-day sessions attracted threeinvited speakers, two student presentations, 14contributed talks, and four poster presentations.This does not include the optical coating presen-tations that were made during the Special Joint

Session on Display Technologies and Control ofEnergy. This number of presentations issomewhat smaller than at last year’s TechnicalConference, but it is still very impressive consid-ering the unusually large number of competingthin film conferences that will be held this year.As in previous years, the sessions provided a goodoverview of current developments in our field.

The first Optical Coating session onMonday morning was devoted to the topic ofProcesses for Advanced Optical Coatings. It wasopened by an invited presentation on theInterface Engineering and Growth Control forHigh Reflectance Soft X-Ray Multilayer MirrorCoatings by Jens Birch, Linkoping University.This talk was followed by five contributedpresentations: Advanced TCO and CIS Coatingsthrough the Pulsed-Magnetron Sputtering ofPowder Targets (Peter Kelly, University ofSalford), Flexible and High-ThroughputDeposition of Multilayer Optical Coatings UsingClosed-Field Magnetron Sputtering (Des Gibson,Applied Multilayers Ltd.), Reactive Low-VoltageIon Plating Plasma-Assisted Deposition: A NewPerspective for Optical Coatings (Carlo Misiano,Romano Film Sottili SRL), Multilayer ProtectiveCoatings for Polycarbonates Prepared byPlasma-Enhanced CVD (Zuzana Kucerova,Masaryk University, Czech Republic, a studentpresentation), and Improving Rate Control inElectron Beam-Evaporated Optical Coatings: theRole of Arcing and Controller Tuning (MichaelGevelber, Boston University).

The Tuesday afternoon session on OpticalFilters and Thin Film Systems opened with aninvited talk by Jerzy (George) Dobrowolski,National Research Council of Canada (retired),entitled, Developments in Materials andProcesses: Key to Advances in Thin Film Design.This was followed by four contributed presenta-tions: Broad-Band Antireflection Coating DesignRecommendations (Ron Willey, Willey Optical,Consultants), The Production of Ultra-Low-LossAR Coatings (Ian Stevenson, Denton VacuumLLC), Application of Ion Beam-Assisted ThinFilm-Deposition Techniques to the Fabricationof a Biosensor Chip with Fieldability Potentialfor Important Biohazard Detection Applications(Dale Morton, Denton Vacuum LLC), andManufacturable Filter for CWDMs (DavidCushing, 3M Precision Optics, Inc.)

The Wednesday afternoon session wasdevoted to Optical Metrology and New PhotonicsMaterials. The invited talk that introduced thesession was presented by Claude Amra, InstitutFresnel Marseille, and was entitled, LightScattering, Photothermal Microscopy, and LaserDamage of Optical Interference Coatings. It wasfollowed by seven contributed presentations:Optical Response from Single- and MultilayerMetal/Dielectric Nanocomposite Thin FilmSystems (Jean-Michel Lamarre, École




Polytechnique, a student presentation),Structural Characterization of Wurtzite AI1-xInxN (0.1<x<0.9) Grown by Dual Reactive DCMagnetron Sputter Deposition (Timo Seppänen,Linkoping University), Versatile ReactiveSputtering Batch Drum Coater with AuxiliaryPlasma (Mark George, Deposition Sciences,Inc.), High Reflectivity Protected Silver Coatingson Stainless Steel and Aluminum (FredericSabary, CEA Le Ripault), Optical and StructuralAnalysis of Annealed SiOx Thin Films Depositedby ECR-PECVD (Tyler Roschuk, McMasterUniversity), How to Have Clean Surfaces in anUnclean World (David Allred, Brigham YoungUniversity) and finally, the last talk of theoptical thin film sessions, Interface Engineeringof Porous/Dense Multilayers of Silicon Nitride: InSitu Real Time Spectroscopic Ellipsometry Study(Ludvik Martinu, École Polytechnique). Onceagain, it appeared that the audience was wellsatisfied with the offered program.

Ludvik Martinu, École Polytechnique, Montreal,Canada ([email protected]), is the OpticalCoating TAC Chair, and George Dobrowolski, NRC,Ottawa, Canada ([email protected]), is theOptical Coating TAC Assistant Chair.

Plasma Processing

This year’s Plasma Processing sessions werevery successful in attracting a diverse

selection of exciting and engaging technical

presentations. Our first invited speaker wasMark Sobolewski of the National Institute forStandard and Technology (NIST) whodemonstrated an experimental and theoreticalformalism for extracting detailed and sometimeselusive information pertaining to the ion energydistribution and the ion flux to a surface underplasma from rather well-characterized andcareful current and voltage measurements.Richard Van de Sanden of Eindhoven Universityof Technology showed us a novel plasma source,the expanding thermal plasma (ETP) and theexciting surface deposition possibilities it canprovide due to the unique fundamental proper-ties of the source. Both sessions were wellattended and the invited talks generated a greatdeal of post-session discussions.

In addition to our invited speakers, ourtalks emanated from academic, government, andindustrial laboratories. We were intrigued byinnovative applications of electron beam-generated plasmas to nitride steels forhardcoating. We heard talks that sought toemploy innovative two-dimensional magneticmodeling to optimize the design of magnetrons.We were impressed by the efforts made toinnovate, scale, and implement a chromiumcoating tool and process for the interior of canonbarrels! Four talks centered on the fundamentalunderstanding and application of high-powerimpulse magnetron sputtering (HIPIMS). Wewere delighted by a “real-world” application of

PECVD coating of SiOx and hard carbon films asfor diffusion barriers as a means to extend shelflife for soft drink and beer containers. Thespeaker even brought the bottles to the talk! Weheard many excellent plasma diagnosticspresentations consisting of pulsed absorptionspectroscopy; ion energy resolved in situ massspectrometry, and semi-quantitative opticalemission spectroscopy. Finally, our sessionsalways enjoy being a forum for the debut of anew or novel plasma source or process, and thisyear was no exception. We were treated to atleast three presentations that introduced anatmospheric pressure source for cleaning wires,a large area source for CVD diamond deposition,and a scaleable, modular ion source for surfacemodification.

Next year we hope to continue our traditionof bringing the highest-quality technical presen-tations to the Society with the introduction ofthe latest sources, diagnostic techniques,processes, and plasma science in the community.In fact, there was so much interest in HIPIMSthat we will have a special session devoted tothis promising and burgeoning processingtechnology (see announcement on page 12).

Finally, in addition to our growing areas oftechnical interest, we have three new membersof the Plasma Processing TAC. This TAC is theperfect vehicle for members who wish tocontribute to the manner and direction in whichSVC addresses plasma science and technology.

If you are interested in joining the SVC PlasmaProcessing TAC, please do not hesitate to callupon any of the members!

Vasgen A. Shamamian, Dow Corning Corporation([email protected]), is the PlasmaProcessing TAC Chair, and Scott G. Walton, NavalResearch Laboratory ([email protected]),and Falk Milde, VON ARDENNE ANLAGENTECHNIKGmbH ([email protected]), are the Assistant TACChairs.

Process Control &Instrumentation

The SVC Process Control & InstrumentationTAC focuses on the instruments, controls,

and methods that make thin film coatingspossible. This year's TechCon session provedboth interesting and informative in presentingsome new approaches to controlling thin filmdeposition processes.

The session started with our invited presen-tation, Modeling of Sputtering Equipment,Process, and Film Growth as an EngineeringTool: Building a Virtual Sputter Tool, by JacquesKools of Veeco Instruments. The presentationdescribed the use of computer modeling tosimulate the thin film process to reduce the trialand error, guesswork, and costs that oftenaccompany the development of thin film produc-tion tools and processes. Modeling techniqueswere applied to the deposition equipment, theprocess, and film growth to create a virtualsputter tool. This tool then becomes a practicaland cost-effective way to develop new thin films.As the cost of computing power continues tocome down, these modeling techniques areexpected to become more widely used in thinfilm development.

The second presentation was EffectiveClosed-Loop Control for Reactive SputteringUsing Two Reactive Gases, by Dan Carter ofAdvanced Energy Industries. Two-reactive-gassputtering is useful in producing binarycompound thin films, which are increasinglyused for electrical, optical, wear-resistant, and

many other functional coatings. But, thepresence of two reactive gases adds significantcomplexity to the process control because ofcompeting reactions. The presentation reviewedthe difficulties associated with controlling theseprocesses and offered a solution based on partialpressure signals to control the process and theresulting complex compound materials.

Our third presentation described reactivesputtering control from a different perspective.Victor Bellido-Gonzalez, of Gencoa Ltd.,presented Flexible Reactive Gas SputteringProcess Control. He described a high-speedcontrol algorithm for gas input control, usingplasma emission monitoring or target voltagemonitoring as the control input. Several alterna-tive process control structures were illustrated.

Our fourth presentation was Stabilizing RFGenerator and Plasma Interactions, by VictorBrouk of Advanced Energy Industries. Thispresentation investigated how the characteris-tics of the plasma process system interact withthe RF delivery system to influence the stabilityof the plasma. A means for quantifying thestability factor for the system was described, andsome methods were presented for configuringthe RF delivery and plasma process systems foroptimum and stable operation.

Our fifth presentation, Fundamentals ofFeedback Control for Batch Coating ReactiveSputtering Processes, was made by Mark Georgeof Deposition Sciences. The presentation charac-terized the non-linear hysteresis involved incontrolling a reactive sputtering process and thevarious methods employed to overcome thesechallenges. The presentation discussed controlsystem hardware and some control algorithmsthat achieve steady-state operating points in lessthan 500 msec on some drum coaters.

Our next presentation, by Werner Klug ofLeybold Optics, was High Accurate In-SituOptical Monitoring for Multilayer Coatings. Thepresentation described a single-wavelengthoptical monitor used to improve the accuracy oflayer thickness in a batch coater, resulting inimproved production yields. The device hasapplication in plasma-assisted evaporation andmagnetron sputtering and is useful for



John B. Fenn’s PlenarySpeech a Highlight ofthe 2004 TechConOne of the highlights of this year’s SVCTechnical Conference held in Dallas, TX, wasthe Plenary Speech given by Dr. John B. Fennof Virginia Commonwealth University. Dr.Fenn won the Nobel Prize in Chemistry in2002 for his pioneering work in the develop-ment of an analytical tool, called electrospray, that allows for the accurate measure-ment of masses for large complex moleculessuch as proteins. This technology, incombination with mass spectrometers, hashelped to revolutionize the biochemical andbiomedical industries.

The electro spray concept, which Dr.Fenn describes as helping molecularelephants to fly, allows for a single largemolecule to be put in the vapor state byevaporating the solvent off an ionicallycharged liquid droplet. This concept evolvedfrom his efforts in characterizing molecularbeams while working at Princeton and YaleUniversities. Once in the vapor state themass of the molecule can then be accuratelydetermined by using a mass spectrometer. Inhis speech, Dr. Fenn reviewed the history ofmolecular beams, which are basicallygenerated by using a small hole, called a gasnozzle, to emit gases into a large vacuumchamber. In total, 12 Nobel Prizes have beenawarded to people involved in the science ofmolecular beams. He peppered the technicalaspects of his presentation with personalstories and tales of his own experiences inthe field. All in all, it was a speech thatappealed to the entire audience, and aninteresting and enjoyable way to kick off the47th Annual SVC TechCon.

Nobel Prize winner Dr. John B. Fenn (left), andRic Shimshock, SVC Program Chair. Dr. Fennpresented the Plenary Speech at the OpeningCeremonies during the TechCon in Dallas.

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First Call For Papers for the 2005 TechConSpecial Session on High-Power Impulse MagnetronSputtering (HIPIMS)High-power impulse magnetron sputtering (HIPIMS) is a subject of growing interest that has found itsfirst applications in hard coatings, substrate pretreatment, low friction, and optical layers. The highionization of the HIPIMS plasma provides opportunities to develop novel and improved materials withunique microstructure and macroscopic properties. HIPIMS processing requires a fundamentalunderstanding of the dynamics in the plasma, on the target and the substrate surface as well as strongdevelopment of the hardware. The SVC’s Plasma Processing TAC is proud to invite you to discuss andhear about all these topics and more in a special session devoted to the HIPIMS technique. Pleaseplan to attend what should prove to be an engaging and informative technical session devoted to theburgeoning field. For information please contact the Plasma Processing TAC Chair, Dr. Vasgen A.Shamamian ([email protected]) or Dr. Artutiun P. Ehiasarian ([email protected]).


multilayer optical devices such as band passfilters, steep edge filters, and AR coatings.

The next presentation, Computer-AidedDesign and Analysis of Optical Transmittanceand Electromagnetic Shielding Efficiency onConductive Antireflective Coatings, was made byJen-chieh Yang of National Cheng KungUniversity. A computer-aided design model wasdescribed for analyzing thin film compositionfrom sputtering or evaporation,and predictingoptical and electromagnetic shielding properties.

Our final presentation, CombinationGauges: Responding to the TechnologicalChallenges, was made by Steve Smith of HelixTechnology. The presentation described some ofthe difficult challenges faced in making vacuummeasurements over the wide range of pressuresfound in thin film processes and described someof the novel solutions used to meet thoserequirements.

J. Grant Armstrong, Carberry Technologies([email protected]), and DavidChamberlain, MKS Instruments, Inc. ([email protected]), are the Process Control &Instrumentation TAC Co-Chairs:

Tribological &Decorative Coating

The Tribological & Decorative Coating sessionsconsisted of 11 contributed and 4 invited

presentations. Professor John Moore from the

Colorado School of Mines delivered an invitedpresentation on the development of a functionalsurface for die casting operations. The develop-ment of the functional surface included optimiza-tion of the substrate metallurgy and the deposi-tion of nanostructured coatings by pulsed-plasmareactive magnetron sputtering. The microstruc-

ture and properties of the coatings werecorrelated with characteristics of the plasmaproduced during the deposition process.

Mahmoud Taher of Caterpillar Inc.presented results of studies on metal-carbidereinforced diamond-like carbon coatings for gearapplications performed as part of a joint

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TRUMPF Group

Don McClure’s Lunchtime Tutorial entitled, “Web Coating for Fun and profit - Lessons from Two Decades ofMaking it Happen,” was one of the many popular seminars at the 2004 TechCon. Don McClure was also honoredthis year as the winner of the 2004 Nathaniel H. Sugerman Memorial Award (see page 17).

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program between Caterpillar, UnitedTechnologies, and the J. A. Woollam Company.

One focus of this program is to determinethe criticality of coating deposition parametersand to develop in situ means of monitoring thoseprocess parameters. Taher presented findingscorrelating in situ plasma diagnostics andspectroscopic ellipsometry with each other andwith the chemical composition of the diamond-like carbon matrix of the coatings.

Herb Gabriel from Plasma und VakuumTechnik presented an overview of refinementsand developments that have occurred in the areaof cathodic arc evaporation processes for thedeposition of hard, wear-resistant coatings. Inparticular, Gabriel discussed how developmentsin cathodic arc evaporation have spawned thecreation of coating deposition systems so largethat building structures are designed anderected around the deposition systems.

In his invited presentation, Roughua Weifrom Southwest Research Institute described theconceptualization and development of a metalplasma source to be used for metal plasmaimmersion ion implantation and deposition inthe same chamber. With this technology, aseamless transition between ion implantationand coating deposition can occur, offering thebenefits of enhanced corrosion resistance,

enhanced coating adhesion, and functionallygraded substrate and coating microstructures.

One highlight from the contributed talks wasHans-Joachim Scheibe’s (Fraunhofer Institute)presentation of novel concepts in the area of laserarc deposition of tetrahedrally bonded amorphouscarbon for wear-resistance applications. Scheibe’snovel process seems to be the first commerciallyviable process capable of making these technologi-cally valued coatings with minimum particulates.His presentation included brilliantly devisedcomputer generated animations of the processthat provided the audience a better grasp of thenovelty of the process.

Papken Hovsepian from Sheffield HallamUniversity presented methods in which Ti and Nbdeposited by PVD processes, then subsequentlytreated with anodic oxidation can be madevirtually any color desired. Many of these surfacetreatments were corrosion and wear resistant.

Ales Kolouch of the Technical University ofLiberec gave one of this year’s student presenta-tions. Kolouch discussed a comparison of thedeposition and characterization of titaniumoxide thin films produced by PVD and plasmaenhanced CVD processes.

Dale McIntyre, Vapor Technologies, Inc.([email protected]), is the Tribological &Decorative Coating TAC Chair, and Gary Doll,Timken Research ([email protected]), and RoelTietema, Hauzer Techno Coating BV([email protected]), are the Assistant TAC Chairs.



Vacuum Web Coating

The Vacuum Web Coating Technical AdvisoryCommittee (Web TAC) put together two

sessions for the 2004 TechCon, along with a jointsession in cooperation with the Optical TAC andthe Large Area TAC. Thank you to the membersof this committee who actively worked to makethis year’s Vacuum Web Coating sessions a greatsuccess. A special thanks to John Fenn, Jr., forcoordinating the Panel Workshop and Discussionon Vacuum Coated Flexible Webs for Use inDisplays.

The opening session, Substrates, CoatingMaterials, and Applications, was moderated byPeter Moulds of Ursa International Corporationand Craig Outten of Outten Technical Consulting.John Affinito of Helicon Research led off thisyear’s session with his invited presentation, ANew Class of Ultra Barrier Materials. With 165people in attendance, the interest in high-barrierflexible substrates and high-barrier encapsulationfor flexible displays is confirmed. MetallizedPolymer Films as Replacement for Aluminum Foilin Packaging Films was presented by WolfgangDecker of Toray Plastics America. His presenta-tion pointed out the advancement andadvantages in using metallized polymer films asan alternative to aluminum foil. Angelo Yializisof Sigma Technologies presented UV versusElectron Beam Radiation Curing of VacuumDeposited Polymer Leveling Coatings for Ultra-High-Barrier Applications. He discussed a cost-effective, promising technology for enhancing thegas and moisture barrier properties of polymerwebs used in a variety of applications, from foodto display packaging. Development of a PilotManufacturing Process for High-VolumeCatalyzation of Fuel Cell Electrodes waspresented by James Arps of the SouthwestResearch Institute. This presentation discusseda high-volume process for reducing the costs ofmembrane electrode assemblies for automotivefuel cell applications. As discussed in thecommittee meeting, the Web TAC would like toexpand the theme of energy generation for thenext technical conference.

The next presentation was Reactive SputterDeposition in the Manufacturing of an OpticalBiosensor by S. Schulz of SRU Biosystems. Hispresentation described the use of vacuum webprocessing in the manufacture of optical biosen-sors for label-free, high-throughput screeningapplications in the pharmaceutical industry. Thelast presentation of the session was an excellentone entitled, Ultra-High Barrier Coatings onPolymer Substrates for Flexible Optoelectronics:Water Vapor Transport and Measurement Systemsand was presented by Ahmet G. Erlat of GeneralElectric Global Research. Devices such as OLEDsrequire extreme water vapor transmission rates(WVTR). This presentation dealt with recentresults to address both barrier and measurementissues.

The final session was on Processes, ProcessControl & Packaging and was moderated by


Roger Kelly of Amcor Flexibles Camvac. Theinvited presentation for the session was given byBernard Henry from the University of Oxford, UK.The presentation, titled Gas Barrier Properties ofTransparent Metal Oxide Coatings on PET Film,was the latest in a series from the same group,and it reviewed the science to bring us all up todate and then went on to try to change thethinking on which materials should be used inbarrier coatings. Bernard ended his talk with abrief tribute to a colleague, Prof. Ron Howson, along time supporter of SVC, who died earlier thisyear. Along with sharing his knowledge, Howsonalso shared his enthusiasm and sense of fun withhis colleagues. This presentation was followedby Possible Future Trends for AluminumMetallizing, given by Charles A. Bishop of C.A.Bishop Consulting Ltd. that gave an insight intosome of the trends in metallizing and what mighthave to be done to make metallizing moreprofitable in the future.

The next presentation, Electron Beam WebCoating—Not only for Consumables? fromApplied Films GmbH & Co was presented byRainer Ludwig, who gave a positive view on thecost effectiveness of using electron beam deposi-tion for multilayer optical coatings as well as themore usual high-volume coatings. This wasfollowed by another presentation on electronbeam deposition given by Ekkehart Reinhold ofVON ARDENNE ANLAGENTECHNIK GMBH, HighSpeed EB-PVD Web Coating—A New CoaterConcept for New Applications. This presentationincluded results from a prototype web coaterthat was designed with some of the newermultilayer optical coatings in mind and based onlayers of titania and silica.

Rolf Rank of the Fraunhofer Institute forElectron Beam and Plasma Technologypresented the talk, Adhesion PromotionTechniques for Coating of Polymer Film. Thistopic continues to be of great interest as thematerials may change, but the need to controlthe adhesion never does. Increasing web speedsand changing plasma source design hasincreased the variations available, and thispresentation addressed these issues.

This was followed by a presentation thatdealt with another one of the problem areas ofvacuum coating. Buckling or Wrinkling of ThinWebs off a Drum was presented by Mike McCannof McCann Science, and it detailed howwrinkling occurs and showed why downgaugingcan be a problem and why using clean web andcleaning the deposition drum can help preventwrinkles.

The final presentation of the session wasgiven by Al Douglas, Jr., of Flex Products and wasentitled, The Application of Reliability CenteredMaintenance (RCM) to High Volume Thin-FilmCoaters. This presentation described what was anew (to most of the audience) method forreducing the amount of lost machine time due tomachine or process failures in a way that wasdemonstrably cost effective.

Roger S.A. Kelly, Amcor Flexibles Camvac([email protected]), and Peter J.Moulds, Ursa International Corporation([email protected]), are the 2004 TAC Co-Chairs. Charles Bishop, C.A. Bishop Consulting Ltd.,([email protected]) joins PeterMoulds as the new Web TAC Co-Chair for 2005.

Smart MaterialsSymposium

The Smart Materials Symposium took place onApril 28–29 as part of the 47th Annual SVC

Technical Conference. The Symposium included18 presentations by authors from Australia,Bulgaria, France, Japan, Portugal, Sweden,Turkey, and the United States. The interest inthe Symposium was encouraging, with theattendance usually between 50 and 100 peopleper talk.

The Smart Materials Symposiumdemonstrated, among other things, that theinterest in switchable glazings—capable ofvarying the throughput of light and solar energyin windows—is growing. This was emphasizedby Greg Sottile, Research Frontiers Inc., whopresented recent results of a study of theknowledge of this emerging technology byAmerican architects. New research results onelectrochromic materials for switchable glazings(often referred to as “smart windows”) werepresented by Nilgun Ozer of San Francisco StateUniversity, Kostadinka Gesheva of the BulgarianAcademy of Sciences in Sofia, Vasco Texeira ofthe University of Lisbon in Portugal, and others.

Technology for switchable glazings,especially the ones based on electrochromicmaterials, is commonly regarded as ready forwidespread market introduction and is currentlyworked on by a number of companies in theUnited States, Europe, and Japan, as surveyed byCarl Lampert, Star Science. Electrochromicautomotive sunroofs will be introduced on some

Elsevier Helps Make theSmart MaterialsSymposium PossibleThe Society of Vacuum Coaters wishes toacknowledge the support of Elsevier inorganizing this successful Smart MaterialsSymposium.

Thanks also are extended to members ofthe Organizing Committee: Carl M.Lampert, Star Science; Ric Shimshock,MLD Technologies; Claes G. Granqvist,Uppsala University, Sweden; LudvikMartinu, École Poytechnique, Canada; andPeter Martin, Battelle Pacific NorthwestLaboratory.

Plans to repeat this successful experimentare already underway for the 48th SVCAnnual Technical Conference in Denver.



European cars already in the summer of 2004, asdisclosed in an invited presentation by Jean-Christophe Giron of Saint Gobain SekuritDeutschland in Germany. Other applications,especially related to polymer-based eyewearsuch as ski goggles and variable-transmittancevisors for motorcycle helmets, were presented by

Claes Granqvist ofUppsala University andChromogenics, inSweden. Many of theapplications related toelectrochromics employthin films based ontungsten oxide. Aneconomic analysis ofthin film deposition bydifferent technologieswas given by PhilipHenderson of AirProducts andChemicals. An alterna-tive to electrochromicoxides in the future maybe electrochromicpolymers; research inthis rapidly developingfield was given by John

Reynolds of the University of Florida inGainesville.

Numerous other presentations were made,but only a few will be mentioned here. Aninvited presentation by Yoel Fink of theMassachusetts Institute of Technology pointedout the possibilities of integrating sophisticated

concepts such as photonic band gap structuresin optically functional textile yarns. Barrierfilms for food packaging is an important field,and the advantages of using a new high-densityplasma source were delineated by John Madocksof Applied Process Technologies. Surfacechemical properties are frequently of muchinterest for oxide coatings, and the role ofhydroxyl groups was emphasized by SatoshiTakeda of the Asahi Glass Company inYokohama, Japan. Vacuum windows, withsuperior thermal properties are criticallydependent on the out-gassing performance ofthe used materials; new results were presentedby Tetsuo Minaai of Nippon Sheet Glass in Kyoto,Japan. Further studies of such windows, relatedto the thermal and optical evolution, were givenin a presentation by Nelson Ng of the Universityof Sydney in Australia.

The field of Smart Materials is stronglylinked to vacuum coatings, as clearlydemonstrated by this Symposium. The field isnotable for being interdisciplinary andembracing several more-or-less interlinked areasof interest to science, technology, and business.

Claes G. Granqvist, Uppsala University ([email protected]), is one of theorganizers of the Smart Materials Symposium.

Panel members for the Workshop on “Vacuum Coated Flexible Webs for Use inDisplays” included Johannes Strümpfel, Hans-Georg Lotz, Charles Bishop, HassanMemarian, Robert Rustin, Steve Sargeant, and Don McClure (see pages 7 and 8).

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After three years of declining attendance since 2001, this year’s EducationProgram at the 2004 Technical Conference showed a healthy 27% increase

in registration from last year. Four new courses were offered:• C-212 Troubleshooting for Thin Film Deposition Processes• C-213 Introduction to Smart Materials• V-304 Cryogenic High Vacuum Pumps• V-305 Challenges and Changes in Vacuum Equipment for Vacuum

Coating ProcessingThese courses drew a large number of participants. The SVC Education Committee continues to reorganize its portfolio to

tune its course offerings to the current needs of the vacuum coating industry.Look for more new courses at the 2005 Technical Conference in Denver,Colorado.

During the coming months before the next TechCon, take advantage ofthe SVC On-Site Education Program through which many of our SVC coursescan be brought directly to your facility – thus saving travel expenses and timeaway from your company for your employees. Contact Vivienne Mattox, theSVC Executive Director at 505/856-7188 ([email protected]) for detailsconcerning this program.

Ismat Shah, University of Delaware ([email protected]) is the Education CommitteeChair, and Vasgen Shamamian, Dow Corning Corporation([email protected]), is the Education Committee Assistant Chair.

Don McClure Awarded this year’sNathaniel Sugerman AwardDon McClure received this year’s Nathaniel H. Sugerman Award during theOpening Ceremonies at the TechCon. Don has the spent the last 22 years in3M’s corporate research laboratory, where he has worked on a broad range ofprograms He recently joined a group developing flexible organic electronicmaterials and devices.

Don attended the SVC Conference for the first time in 1984. From 1990through 1996 he presented his “Workshop on Vacuum Web Coating” and hisfirst course, “Basics of Vacuum Web Coating,” has been part of the educationalprogram since 1994. He added his course on “Sputter Deposition onto FlexibleSubstrates” in 2003.

He was selected for the Board in 1991 and was elected Vice-President in1994, President in 1996, and was Past President in 1998. He became theinaugural Secretary to the Board in 2000, and served for four years.

For more about Don’s contributions to the SVC and the vacuum coatingindustry, go to http://www.svc.org/AW/AW_Nat.html.

Education Program Has 27%Increase in Attendance at theDallas TechCon!

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Vacuum coating professionals took advantage of Dave Glocker’s short course entitled,“Sputter Deposition in Manufacturing”. It was just one of over 30 short coursesoffered during the TechCon.


Vacuum Technology:In-Line Processing Systems

“In-line” processing systems use severalprocessing chambers connected together tosequentially process the substrates. Forexample, the system can clean the substrate,modify the substrate surfaces, and deposit filmsor otherwise build structures or devices withoutexposing the substrate to the ambient environ-ment between steps. An in-line system mayinvolve several different types of processing,such as Physical Vapor Deposition (PVD) andSub-Atmospheric Chemical Vapor Deposition(SA-CVD). The in-line systems are characterizedby having the substrates moving from chamber tochamber in one direction so that a fixture can beunder processing conditions in each module allthe time. This can give very high productthroughput of multi-process-built structures,particularly when the system is automated.Some in-line system designs have the capabilityof adding or changing process chambers withease; others do not.

The processing chambers can be operatingat different vacuums or they may use differentprocessing gases. The processing chambers canbe isolated from each other in several ways, asshown in Figure 1.

In the “Valve Isolation” system there is avalve between processing chambers. The fixtureis moved from one chamber to another, valvesclose, and the process is physically isolated fromthe other processing chambers. After processingis completed, the chamber may be pumped out toremove the processing gases (if any), the valve isopened, and the fixture is moved. Figure 1ashows a linear in-line system where it is relativelyeasy to change or add more processing stages.

In the "Pump Isolation" system there is anintermediate chamber ("tunnel") between theprocessing chambers. This intermediatechamber has a low conductance for gas flowbetween chambers and the region is activelypumped to prevent gases and vapors from onechamber getting into the other chamber. Anadvantage to this system is that one end of a longsubstrate can still be in one chamber while atthe other end it is entering the next chamber.This type of design is common in systems used tocoat architectural glass (10' x 12' panes) withsolar-control or low-E coatings. It is relativelyeasy to change or add more processing stages tothis type of equipment.

In the “Vacuum Transfer” system the fixtureis moved into and out of a transfer chamber thatcan be evacuated to a “rough” or even a “high”vacuum. The purpose of the transfer chamber isto prevent processing gases in one chamber fromentering another by rapidly pumping the transferchamber. In some cases the transfer chambercan be at a higher pressure than the processingchamber so that when the valve is opened, gasflow is into the processing chamber from thetransfer chamber to further prevent "backflow"of the residual processing gases. In one applica-tion using SA-CVD, the pressure in the transferchamber is 3 Torr when the valve is opened.

If the in-line system shown in Figure 1aused a separate chamber to separate and isolatetwo processing chambers, and not for processing,it would be called a vacuum transfer system.The system shown in Figure 1c uses a vacuumtransfer chamber that is common to all theprocessing modules. This configuration issometimes called a "Cluster In-Line" system. Inone application of this system, the coating ofauto headlight reflectors with aluminum, the

cycle time for each processingchamber is 30 seconds. It isnot possible to add moreprocessing stages to this typeof in-line system equipment.

In the “ControlledAtmosphere Transfer” systemthe transfer chamber is atatmospheric pressure, sohermetically sealed gloves canbe used. In the transferchamber, measurements andprocedures, such as maskalignment or C-V measure-ments, can be performedbetween processing steps.The gas in the transferchamber can be dry air if theproduct is moisture sensitiveor an inert gas such as argon

Sample Guide from the Collection ofEducation Guides to Vacuum Coating Processingby Donald M. MattoxSVC Technical Director

Load-LockChamber

AccessDoor

Fixture

#1 #2 #3 #4

External Valves Internal Valve

#1 #2 #3 #4

Vacuum Pump

Low-Conductance TunnelUnload

Chamber

Pump Isolation Systemb.

Vacuum Transfer (“Cluster”)c.

VacuumTransfer

Chamber

#1

#2

#3

#4

In-ProcessPosition

InternalValveLoad/Unload

Chamber

FixtureMotion

TransferPosition

Valve Isolation Systema.

Inert or DryTransfer Chamber

Gloves(Optional)

#1 #2 #3

Direct-LoadChamber

Load-LockChamber

Controlled Atmosphere Transferd.

Figure 1: In-line processing systems. 1a: Valve isolation system, 1b: Pumpisolation system, 1c: Vacuum transfer system, and 1d: Controlled atmospheretransfer system.

Order YourEducation

Guides Today!Written by Donald M. Mattox, SVCTechnical Director, this indispensiblepublication contains individual, stand-alone, two-page guides on differentaspects of the equipment and technologyassociated with vacuum coatingprocessing by physical vapor deposition.Titles of some of the sections include:

• Introduction to the Basics ofPVD Processing

• Materials Science

• Vacuum Technology

• Plasma Technology

• Surface Preparation

• Vacuum Evaporation

• Sputter Deposition

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Society of Vacuum Coaters71 Pinon Hill Place NEAlbuquerque, NM 87122-1914Telephone 505/856-7188Fax 505/856-6716E-mail [email protected] Site www.svc.org

or nitrogen if chemical reaction is a problem.The individual processing chambers can be of a“direct-load” design where the processingchamber is opened to the transfer chamberduring each cycle, or a "load-lock" design wherethere is a chamber between the transferchamber and the processing chamber. In thetransfer chamber the product may be packagedin an appropriate container before beingexposed to the ambient.

Several types of valves can be used in thein-line system. If one side of the valve is atatmospheric pressure while the other is at agood vacuum (“external” valve), the sealingpressure is from the pressure differential andthe valve can be a simple plate that seals againstan elastomer seal. These can be used for theload-lock chamber and for access doors toindividual chambers. Door movement should besuch that the sealing surfaces are pressed“metal-to-metal” on sealing. Common polymerseals and their recommended maximumoperating temperatures are: Buna-N (100°C),Viton (200°C), silicone (250°C), and spring-loaded Teflon™ (350°C).

The "internal" (isolation) valves have nolarge pressure differential during the processsequencing. They can be simple “flap-valves”that have little sealing pressure but just restrictthe conductance of gas flow between chambers;or they can be valves that have a positive sealingpressure provided by mechanical means. The

latter is desirable if the processing gases used inone process would be a contaminant if they getinto another processing chamber or if highvacuums are required for processing.

In-line systems are meant to operatecontinuously, so heat build-up is a consideration.If high temperatures are desired in theprocessing chamber it may be best to design avacuum oven using radiant heaters to heat thefixture and have water-cooled surfaces facing thechamber walls. Since there is no convectiveheating in the vacuum chamber, this willminimize heating of the chamber walls. It maybe desirable to actively cool seal areas if heatbuild-up is a concern. This can be done usingcooling coils on the exterior of the chamber. Ifthe fixture has attained a high temperatureduring processing it may be necessary to have anexit chamber that is actively cooled by flowinggas to reduce the temperature to an acceptablelevel before the fixture leaves the in-line system.

Generally each chamber is provided withan access door(s). This allows easy cleaning,maintenance, and repair. Processing hardware,such as sputtering cathodes or ion guns, can bemounted on the access door.

Vacuum pumping of each chamber can bedone with individual pumping "stacks," or thechambers may be joined to a common vacuummanifold. Often the chambers use a commonroughing manifold and each chamber has anindividual high-vacuum pump. This can result in

limitations on the use of the system. Forexample: If two chambers at different pressuresare opened to the roughing manifold at the sametime, gases from the higher-pressure chamberwill tend to enter the lower-pressure chamber.This may not be acceptable.

Transfer mechanisms are driven fromoutside the vacuum chamber by rotary-motionvacuum feedthroughs. The drive can be apositive mechanism, such as gear-and-sprocket,or it may be a friction drive, such as poweredrollers. For tall fixtures, such as a vertical palletfixture, it may desirable to stabilize the movingfixture by having a fixture guide at both top andbottom. Transfer mechanisms and drive trainsare often the operational weak points of an in-line system.

Sometimes a back-and-forth motion isdesirable in the processing chamber. Forexample, the fixture might need to have multiplepasses in front of a planar sputtering cathodeand a linear ion gun, both in the same chamber.This allows periodic "atomic peening" of thegrowing film structure by inert-gas ion bombard-ment to densify the film without requiring a biason the substrate. Use of reactive ions allowsreactive deposition by depositing a fewmonolayers of metal, followed by bombardmentwith a reactive species such as oxygen ornitrogen. A back-and-forth motion requires thenecessary chamber length, drive mechanism,


continued on page 24


SVC Exhibit is Well Received by TechCon Attendees!In spite of the slow economy and the struggles that other societies have with low exhibittraffic, the SVC Exhibit remains vibrant.

With over 200 booths in Dallas, a broadrange of exhibiting companies offeredtheir products and services to the

vacuum coating professional.Here are some quotes from our exhibitors

and conference attendees:“The quality of exhibitors was good – met

new ones I had never heard of.”“Well organized, compact, and well

attended by attendees.”“Good networking opportunities.”“Many of our crucial customers/vendors

were there.”“TechCon short courses draw a quality

crowd.”“Broad range of exhibiting companies.”TechCon sponsors of the Internet Café,

Beer Blast, and Coffee Breaks were highlightedwith balloon bouquets at their booth andacknowledged in the Final Program, throughoutthe TechCon signage, and on the Web Site. Thethree Internet Café stations in the back of theExhibit Hall were very popular and in constantuse – but with no one having to wait for morethan a few minutes.

The Program Committee scheduled thetechnical presentations to minimize conflict withthe Exhibit Open Hours. As an example, alltechnical sessions ended at 3:30 p.m. on Tuesdayso that everyone could visit the Exhibit and enjoythe Beer Blast. The afternoon break on Mondaywas almost an hour and two technical sessionsinstead of three sessions were scheduled for thistime frame. The expansion of the TechCon to fourdays this year has enabled the ProgramCommittee to really pay attention to scheduling

issues that allow the conference attendees tospend more time in the Exhibit Hall.

Having the Poster session boards in theExhibit Hall was also a well-conceiveddecision—conference attendees and exhibitorsalike found the location to be convenient. SVCused new methods to promote the TechCon andExhibit in 2004: a postcard mailing, E-mailblasts, and an On-line Visitor registrationprocess which was popular.

The SVC Exhibitor Pass system enabledexhibit booth personnel to attend technicalpapers of choice. The SVC wishes to acknowl-edge the invaluable assistance offered by HarryGrover of MeiVac, Inc. to all of our exhibitors.

We also welcome Lisa Robillard, with MKSInstruments, Inc. as our new Exhibit CommitteeChair.

If you have questions or comments(positive and negative), please do not hesitate tosend them to Vivienne Mattox, SVC ExecutiveDirector and Meeting Planner, at [email protected].

Ric Shimshock (right), Program Chair, awards Ludvik Martinu of École Polytechnique the $200 prize for “BestPoster” presentation in the Exhibit Hall during the 2004 TechCon. The Poster Session was set up in the ExhibitHall for extended viewing during the Exhibit.

The popular Internet Café was located in the ExhibitHall.

The Exhibit allows for one-to-one interaction betweenattendees and exhibitors.

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Abstract

Vacuum (sub-atmospheric) coating processeshave been the enabling technology in severalfields for a number of reasons. The vacuumcoating process has allowed a functional coatingto be deposited when no other technique can doso and sometimes has allowed the production ofa more functional coating than is available byother means. The use of a vacuum coating canprovide a more marketable product that isproduced at a low cost. In some cases thereproducibility of the process allows the produc-tion of very complex and demanding productssuch as multilayer diffraction gratings andbandpass filters. New markets have beengenerated due to the availability of vacuumcoating processes. In many, if not most cases, avacuum coating is a value-added process whoseprice and contributions to the economy and theenvironment is difficult to quantify. This presen-tation will address many of these subjects andcompare some vacuum-coated products to non-vacuum-coated products and processes. In thepast few years, plasma-based vacuum processeshave become important production techniquesand their use is expanding rapidly. Vacuum

coating technologies will continue to developand be an enabling technology for the foresee-able future.

Introduction

An “enabling technology” is one that allowssomething to be done on an industrial scale thatcould not be done otherwise. The first use ofvacuum coating (sputter deposition) on anindustrial scale was by T. Edison for making thesub-masters of his “Gold Moulded” cylinderrecords. However, the process was not an enablingtechnology because others were doing much thesame thing by making their wax masters electri-cally conductive using carbon powder.

The second early process that might beconsidered enabling was the zinc coating ofpaper for paper capacitors by R. Bosch (BoschCompany) in 1935. The use of metallized paper(roll coating) instead of metal foil allowed thesize of a capacitor to be reduced by about 50%.In 1940 Whiley (England) patented the use ofaluminum for web coating. Lead foil was usedfor early packaging to some extent but tin foilwas the first widely used flexible packaging foil.It was replaced by aluminum foil after 1910

when repeated rolling of aluminum was shown toprovide a cheaper foil product. Aluminum foilwas used to preserve “freshness” until well afterWWII when it was replaced by metallizedpolymer film prepared by vacuum coating.

Web coating went on to be an enablingtechnology for such processes as coatingpolymer with vapor barriers for flexible


Vacuum coating—An Enabling Technologyby Donald M. MattoxManagement Plus, Inc., Albuquerque, NM

In February 2004, the SVC Board ofDirectors honored Don Mattox by creatingThe Donald M. Mattox Tutorial Program, inrecognition of his many contributions tovacuum coating technology and the Society.Don was presented with a plaque at theAwards Ceremony in Dallas and was askedto prepare a presentation to kick-off theTutorial Program bearing his name. Hispresentation entitled “Vacuum Coating—AnEnabling Technology,” was the InauguralTutorial in The Donald M. Mattox TutorialProgram on April 26, 2004, at the TechCon.Don McClure of 3M Company, and CharlesBishop with C.A. Bishop Consulting Ltd.,also presented Tutorials in this program.


packaging. Multilayer coatings on webs began inthe IC industry to metallize flexible substrates.A major advance in web coating was the use ofsputter deposition for depositing compounds andmultilayers. For packaging this is leading to“see-through” freshness packaging. Magnetronsputter deposition on flexible webs was firstused by D. Charoudi in 1977.

The antireflection (AR) layer on old glasswas recognized in the early 1800s. In the latterpart of the 1800s all professional photographersknew that old lenses were better than newlenses because of the coating that formed onthem with age. There were numerous attempts(and patents) on the chemical treatment oflenses to form an AR coating on the surface.

In 1935, A. Smakula (Zeiss Company)discovered the use of vacuum coating to form

single-layer AR coatings on lenses but the patentwas considered to be a Military Secret until 1940[1]. In 1936 John Strong discovered the use ofvacuum coating for forming an AR coating onlenses and published it in the open literature.Again this might be considered an enablingtechnology even though chemical treatmentscan be used to formed AR coatings on surfaces.It is interesting to note that the Germans did notuse AR coatings on camera lenses until afterWWII. Single-layer AR coatings continued in usewell after WWII [2].

The first explanation of the effect of asingle-layer coating on antireflection was by Airyin 1832 [3]. He used classical ray and wavetechniques to show the effect. In 1939 usingchemical techniques (Langmuir-Blodgett films)to form layers of very precise thickness andvarying indices of refraction Blodgett showed theAR effect and equations for the relationshipbetween thickness and index of refraction in ARcoatings [4].

Multilayer AR coatings are another matter.Cartwright and Turner deposited 2-layer coatingsin 1939. There is one report that the Schott Co.(Germany) formed multilayer AR coatings (3-layer) on lenses during WWII by spray pyrolysis.Otherwise mutilayer AR and filter coatings were

not used until the late 1940s. It has been asserted that Monarch Cutler,

an undergraduate student at MIT, was the firstto calculate the effect of multi-coatings on theAR properties of a surface [5]. Mr. Cutler’ssenior thesis at MIT was entitled “Reflection ofLight From Multilayer Films” (May 1939). It isinteresting to note that in the acknowledgmentof his thesis Mr. Cutler acknowledged Dr.Cartwright and Dr. Turner “for informationconcerning their work in the production of colorfilms.” He also acknowledged Richard P.Feynman, also an undergraduate student at MIT,for his help in deriving the equations for thereflection and transmission of multilayer films.Dr. Feynman later received a Nobel Prize inPhysics (1965) for his work in quantum electro-dynamics (QED) and was considered one of thefinest physics lecturers of all time [6].

Feynman’s senior thesis at MIT was “Forcesand Stresses in Molecules.” In my research Ihave not found any other reference to a relation-ship between Dr. Feynman and Mr. Cutler’s 1939work. By 1946 several authors were involved incalculating the optical properties of multi-layerfilms [7].

The vacuum deposition of aluminumreflecting coatings on glass by vacuum deposi-tion can certainly be considered an enablingtechnology for the subject of astronomy. JohnStrong published the first work on aluminizinglarge mirrors in 1936 [8]. For about 100 yearsbefore that time chemical deposition was used.The “modern” techniques of deposition bychemical reduction began with Liebig in 1835[9]. There are two widely used methods ofchemical silvering. The “Brasher method” wasused to deposit thick coatings on front-surfacemirrors that could be subsequently polished fortelescope mirrors and the “Rochelle Saltsmethod”, that has a slower deposition rate, andwas used to deposit thin silver films such aswere used in partially silvered mirrors.

In 1920 at a discussion on “The Making ofReflecting Surfaces” R. Kanthack, in hisIntroduction, stated “Six weeks of bibliographyhunting have given me the impression that atthe present time—85 years after Liebig’sclassical discovery!—we have not evolved anymethod of chemical deposition on glass soscientific and practically perfect that it could beadopted officially” [10].

Polishing, which leaves minute scratches,reduces the resolution of the reflected light aswas shown in tests by Strong on the Hooker 100inch telescope on Mount Wilson in the mid-1930s. The Hooker telescope had used polishedchemical-silver coatings and had barely beenable to see the companion star (magnitude of 8)of the extremely bright star Sirius (magnitude ofminus 1.5). Strong’s vacuum evaporatedaluminum coating enabled the “Companion of

Sirius” to be resolved easily by the Hookertelescope. During WW II Heraeus (Germany)used the sublimation of a protective layer of SiOon the surface of aluminized mirrors. In 1946Turner addressed the effect of a single layerdielectric on mirror surfaces (“protected”surfaces) [11]. Today multilayer reflectingcoatings are used in all kinds of reflectingapplications. These include heat mirrors, coldmirrors, low-E window coatings, silver coatingson astronomical telescopes and many others.

Corrosion protection is one of the mostdemanding applications for coatings of any type.Electroplating on electrically conductingsubstrates was developed soon after the develop-ment of the Volta Cell in 1800 and has been usedto deposit corrosion protective coatings for manyyears. A problem with the electrodeposition ofmany materials from aqueous solutions is the co-deposition of hydrogen. This hydrogen can causeembrittlement of high strength steels (>200,000psi), particularly when they are under stress.The electroplating industry uses heating to try tooutgas the incorporated hydrogen but this can bedifficult to quantify. Vacuum deposited cadmium(VacCad) was formally accepted as a replace-ment for electrodeposited cadmium by themilitary in 1958 (Mil Spec. 8837) as a sacrificialcorrosion protective coating.

A major advance in corrosion resistantcoatings was the development of the “Ivadizing”process at McDonnell-Douglas in the late 1960s.The ivadizing process allowed adherentevaporated aluminum to be coated on steel andtitanium fasteners in a “barrel coater.” Thesecoated fasteners prevent galvanic corrosionwhen they are used in contact with aluminumsuch as on airplane “skin.” The process was laterjust called “ion vapor deposition” and is nowknown in the aerospace and military relatedindustries as IVD coating. The aluminumdeposited by IVD is often shot peened orburnished in order to seal pinholes that are a

Vacuum Coating—An Enabling Technologycontinued from page 21

Figure 1: RF sputter deposition of Cr and Cu on aKapton® web, (Morrill, Egan, Paszek, and Aronson)JVST 9(1)350 (1972)

Figure 2: American vacuum system for coating opticsduring WWII. Note the lack of a high vacuum valve.


problem with using vacuum coatings forcorrosion protection.

Vacuum coating for tribology, using low-shear-strength metals, was studied anddeveloped by NASA for use in vacuum in the late1960s. Their advantage is that they do not“creep” as oils and greases do. An example oftheir current use is in the coating of bearingsused on the rotating anode in x-ray tubes,

Vacuum deposition of electrical resistorsdidn’t come into real use until the age of the“integrated circuit” (IC) technology. The ICindustry began in the late 1950s. In ICtechnology tantalum was a material of greatinterest for making stable thin film conductorswith low temperature coefficient of resistivity(after annealing), thin film resistors made ofreactively sputter deposited TaN that couldeasily be “trimmed” to the correct resistancevalues by anodizing, and thin film capacitorsthat could be made by anodizing (oxidizing) thefilm surface to form a dielectric (Ta2O3). Forthe IC industry very high volumes of coatedsubstrates were needed.

The IC industry brought about theintroduction of high-volume coating systemssuch as the air-to-air in-line coater [12], theload-lock in-line coater, and the random-accessprocess chambers with a central vacuumchamber [13] that may be considered theforerunner of the modern cluster tool that iswidely used for processing wafers.

Sputter cleaning is an in situ cleaning

process that is often integral to obtaining goodadhesion of the deposited coating. Sputtercleaning was first used in ultrahigh vacuumtechnology in the field of Surface Science toobtain atomically clean surfaces. Sputtercleaning as a separate step in vacuum coating isoften not as successful as it could be because ofrecontamination of the surface betweenprocessing steps. An enabling technique wasintroduced in the early 1960s whereby thesputter cleaning was continued while the first ofthe coating material was applied by evaporation.As long as the deposition rate exceeded thesputtering rate a film was formed, essentially onan atomically clean surface.

SummaryThere are a number of developments in

vacuum coating technology that might be citedas “enabling technologies” but the followingwould certainly be included in any list.

1. Evaporation of aluminum from tungstenfilaments.

2. Deposition of single-layer and multilayeroptical coatings.

3. Development of electron beam (e-beam)evaporation techniques.

4. Use of concurrent bombardment duringdeposition to modify the properties of thedeposited material.

5. Integration of the sputter cleaningprocess with the deposition process togive a “clean” interface.

6. Development of reactive sputter deposition.7. Development of the in-line deposition

system (“tool”).8. Development of magnetron sputter

deposition technology.9. Development of plasma enhanced

chemical vapor deposition (PECVD)technology.

10. Development of arc vapor deposition.

AcknowledgementsThe author thanks Ric Shimshock for pointingout the very interesting relationship of RichardP. Feynman to Monarch Cutler and providing thetitle page of the Cutler thesis. Thanks are alsoextended to George Dobrowolski for calling

Figure 3: Patent for a vacuum system with a centralvacuum chamber and separate processing chamber.This may be considered the forerunner of the clustertool [13].


attention to the Russian work (Appendix I) thatdescribes 2-layer AR coatings and providing thetranslations given in Appendix 1.

ReferencesGeneral reference: Donald M. Mattox, TheFoundations of Vacuum Coating Technology,Noyes Publications (2003).

Additional references:1. J. Taimer, J. Opt. Soc. Amer., 36, 701 (1946)2. R.A. Denton and T.L. Scatchard, “Recent

Trends in Vacuum Deposition of PrecisionOptical and Electrical Thin Films,” p. 51 inVacuum Symposium Transactions (2nd),American Vacuum Society (1955)

3. G.B. Airy, Trans. Cambridge Phil. Soc., 4, 409(1832)

4. K.B. Blodgett, “Use of Interference toExtinguish Reflection of Light From Glass,”Phys. Rev., 55, 391 (1939); also Blodgett,Phys. Rev., 57, 921 (1940)

5. P. Baumeister, communication 20036. The Beat of a Different Drum: The Life and

Science of Richard Feynman, JagdishMehra, Oxford (1994); also RichardFeynman: A Life in Science, John & MaryGribbin, Dutton (1997); also Surely You’reJoking Mr. Feynman; also QED: the StrangeTheory of Light and Matter, Richard P.Feymen (Alix G. Mautner MemorialLectures), Princeton University Press(1985)

7. P. King and L.B. Lockhart, J. Opt. Soc. Am.,36, 513 (1946); also D.L. Caballero, J. Opt.Soc. Am., 36, 256 (1946); also H.D. Polster, J.Opt. Soc. Am., 350A (1946)

8. J. Strong, “The Evaporation Process and itsApplication to the Aluminizing of Large

Telescope Mirrors,” Astrophysical J. 83(5)401 (1936)

9. J. von Liebig, “Uber die Produkte derOxydation des Alkohols, Aldehyd,” Ann. D.Pharm., 14, 134 (1835).

10. R. Kanthack, p.5 in “The Making ofReflecting Surfaces,” A Discussion of ThePhysical Society of London and The OpticalSociety., 26th November (1920), FleetwayPress.

11. A.F. Turner, J. Opt. Soc. Am., 36, 711A(1946).

12. S.S. Charsan, R.W. Glenn and H. Westgaard,The Western Electric Engineer, 7, 9 (1963)

13. Joseph S. Mathias, Alfred A. Adomines,Richard H. Storck, and John McNamara“Evaporation System” U.S. Patent #3,404,661(Oct. 8, 1968) (filed Aug. 26, 1965)

Appendix IMay 3, 2004To: Don Mattox (by E-mail)From: George DobrowolskiBelow is the Russian original and the Englishtranslation of the contents of the title page ofthe book which I am also appending in the formof a file for your interest:

Academician I.V. Grebenshchikob, A.G. Vlasov,B.S. Neporent, N.V. Suikobskaya

The Antireflection Coating of Optics/Reduction ofthe Reflection of Light by the Surfaces of Glass(Prosvetlenie Optiki/ Umienshenie otrazheniyasveta poverchnost’yu stekla), edited byI.V.Grebenshchikov, published by GocudarstvennoeIzdatelstbo Technicko-Teoreticheskoi Literaturyi(State Publishers of Technical-TheoreticalLiterature) Moskva 1946 Leningrad

The book consists of 212 pages and is organizedin 9 chapters with headings:1. Physical basis for the antireflection effect2. Mathematical theory of the antireflection

effect of thin films3. Physical properties of antireflection

coatings and their control4. Antireflection coating of silicate glasses

using an etching method5. Antireflection of glasses by deposition of

silicon-organic solutions6. Deposition of antireflection coatings

through the deposition of fluoride vapors ina vacuum

7. Antireflection though the deposition ontothe surface of a glass of monomolecularlayers of organic materials

8. The manufacture of glasses with anenhanced reflection coefficient through thedeposition of titanium dioxide layers

9. Antireflection coating through the deposi-tion of two-layer coatings.

It contains 99 illustrations (some of equipment),tens of tables, and over a hundred references.Very impressive for a book which must have beenwritten during the Second World War, if it wasapproved for publication in March of 1946 andcame out later in the same year.

Vacuum Coating—An Enabling Technologycontinued from page 23

Sample Education Guide — Vacuum Technology: In-Line Processing Systemscontinued from page 19

and position sensors.Position sensors allow a “fail-safe"

operation of the transfer mechanism. Thefixture must be in the correct position for theprocess to begin or for a valve to close. Positionsensors may operate by optical, mechanical,electrical, or magnetic sensing.

Sensors in the system enable software to beprogrammed to allow automation of the motionand the processing. In high-throughput systems,movement of fixtures from one processingchamber to another or into or out of a transferchamber are often coordinated to maximizeefficiency. This can lead to an inflexibility insystem use. This can be important if the systemis also going to be used for development orprocess characterization. If this is a considera-tion, the software should be such that it can be

reprogrammed easily. It may even be desirableto run the system in a manual mode, yet leavethe "fail-safe" sensors operative.

In some modules, the substrates may beelectrically isolated ("floated") so a bias voltagecan be applied to the fixture/substrates or so auniform self-bias can be created on the surface ofa dielectric material. (Note: Often a dielectricsurface that is being subjected to a flux ofcharged particles and is being held in a groundedmetal fixture will have a different surfacepotential near the edges from that at the centerdue to surface-charge leakage. This effect can beminimized by electrically isolating the fixturefrom ground.) Electrical isolation can beprovided to the whole fixture and transferassembly or just to the part of the fixture thatholds the substrates. If the whole fixture and

transfer assembly are biased, the total area canbe very much greater than just the substratearea. This wastes power and may causeoperational problems. Electrical contact to justan area on the fixture that is electrically isolatedfrom the rest of the fixture and the transfermechanism can be done using brush-contacts ormechanically loaded make-break contacts thatrelease before the fixture is moved.

Sometimes redundant processing volumes,such as long processing chambers or dualcooling chambers, may be needed to allow formore processing time than is required by otherprocesses. The cycle-time-limiting processesneed to be carefully considered in the design ofthe in-line processing system.

Mark Your Calendar!Society of Vacuum Coaters

48th Annual Technical Conference

April 23–28, 2005Adam’s Mark Denver Hotel, Denver, CO

Deadline for Abstracts is October 1, 2004


Abstract

Reactive sputtering is becoming a more widelyaccepted practice for the deposition of manyuseful compound thin films. The use of closed-loop control for the deposition of such films isalso increasing in popularity. The closed-loopprocess for forming binary compounds, typicallyoxides or nitrides, is conveniently accomplishedusing one of several feedback mechanismscoupled to a high-speed reactive gas controlvalve. Optical emission, target voltage and massspectroscopy have all been successfully used toprovide feedback for such processes when usinga single reactive gas. The presence of tworeactive gases in a reactive sputtering processadds significant complexity and presents theissue of competing reactions. Since bothreactive gases can affect the state of the targetsurface and the plasma conditions, both alsoaffect common feedback control signals such asthe cathode voltage and optical emission.Modeling has shown that the way to control atwo-gas reactive sputtering process is to produceindividual control signals for each gas. In thisstudy, partial pressure signals for each reactivegas were used to control the deposition of SiOxNyand TiOxNy compounds. The results of this studyare presented here and shown to support themodeled behavior. The two-gas, closed-loopapproach is then demonstrated to provide astable, high rate solution for the deposition ofthese highly complex thin film materials.

Introduction

Oxide and nitride thin films are becomingincreasingly popular for their electrical, optical,wear resistant, and other functional properties.Driven by improvements in depositiontechniques, these thin film materials arebecoming commonplace in many vacuum coatingapplications. Reactive sputtering continues toemerge as one of the most economical methodsfor depositing these materials. With properlyconfigured power delivery and process controlmeasures, high rate, arc free deposition of manyoxides and nitrides is now possible. As reactivesputtering methods have matured, interest inextending the technique beyond simple binarycompounds has been growing. As materialcomplexity increases however, so do thechallenges of process control as we examine anddiscuss in this study.

Although the concept of reactive sputteringis quite simple, the art of employing it effectivelyto produce high quality insulating films atmaximum rates can be a real challenge. The

nature of forming insulating layers in a direct-current sputter deposition is inherently disrup-tive to the process. In recent years the issue ofarcing in reactive sputtering has been effectivelymanaged using one of several power deliverytechniques [1-4]. The most common of theseare pulsed-dc in a single magnetron system andlow frequency ac power in a dual magnetronsystem. In both cases a voltage reversal at thecathode is used to effectively eliminate chargebuild up on the target surface and thus avoid thebreakdown event. Many modern power suppliesalso possess arc detection and arc handlingcircuitry designed to quickly extinguish an arcshould one occur.

Target transition control is another majorchallenge in these processes. As the reacted,insulating deposit is formed on the work piece, italso forms on the target surface causing achange in its sputtering character. Increasingreactive gas flow to the sputtering processincreases conversion of the deposit to thedesired compound but also increases thecoverage percentage of the compound on thesurface of the target. At a critical point, anavalanche transition often occurs where fullcoverage of the target is experienced. Thischange in target condition, commonly calledpoisoning, has several detrimental effects on theprocess. Dramatic voltage swings, a decrease indeposition rate and an uncontrolled increase inprocessing pressure are all common results oftarget poisoning [5-7]. Further complicating thematter is the hysteresis character commonlybrought on by this behavior. Figure 1 shows atypical transition curve for reactively sputteredtitanium nitride showing how the poisoningprocess is not directly reversible by simplydecreasing reactive gas flow.

Reactive sputtering can be performed froma fully poisoned target but this approach resultsin low deposition rate and lack of compositioncontrol. Operation of these processes in thetransition region offers a significant rateadvantage [7-9] along with the ability to control

the composition of the produced film [9]. Thiswould be most advantageous in a two reactive gasprocess as the potential exists for a broad rangeof film properties by adjusting, for instance, theratio of oxygen and nitrogen incorporated in anoxynitride film. Compositional control inoxynitride depositions has been demonstratedusing CVD, PECVD and ion assisted evaporation[10-12] but these techniques tend toward highercomplexity and cost and often require more heattolerant substrates than most typical sputteringapplications.

Over the past two decades closed-loopcontrol systems have been developed for reactivesputtering processes [5,6]. These techniques,when properly implemented, allow for stablecontrol within the so-called transition region ofthe target. Process feedback is in the form ofoptical emission, mass spectrometry or targetvoltage [5,6,9] and control is derived by regula-tion of a single reactive gas through one or morehigh speed flow devices.

Adding a second reactive gas significantlycomplicates the process control challenge [13].With two reactive gases present, theindependent reactions compete with oneanother. Depending on the reactivity betweenthe metal and each gas, one reaction maydominate causing the process to become trappedin an undesirable state preventing incorporationof the less dominant reactive gas. This behaviorwas predicted in the Carlsson model and hassubsequently been demonstrated experimentally[14,15]. To prevent this, independent control ofboth reactions is necessary.

Control in one gas reactive depositions isoften achieved by managing the surfacecondition of the target. Target voltage is conven-ient when transition causes an impedancechange and optical emission of the sputteredspecies is effective when transition affectssputter yield. These methods, however, offer nomeans for discriminating the effects of multiplereactive gases. To accomplish such discrimina-tion the partial pressure of each reactive gasmust be measured. As compound formationconsumes a reactive gas, the partial pressure isaffected. During target transition, the consump-tion of reactive gas decreases due to reducedunreacted target surface and decreased metalflux to other surfaces. This behavior gives rise topartial pressure monitoring as a direct feedbackfor compound formation in such a process. Mostimportantly, partial pressure control offers thecritical advantage of being species dependent,thus allowing for independent monitoring andcontrol of multiple reactive species.

Depositions for this study were performed

Effective Closed-Loop Control for Reactive SputteringUsing Two Reactive Gasesby Dan Carter, Bill Sproul, and David ChristieAdvanced Energy Industries, Inc., Fort Collins, CO

Figure 1: Partial pressure hysteresis behavior typicalfor titanium nitride reactive sputtering.

Presented on April 29, 2004, at the 47th SVC TechConin the Process Control and Instrumentation Session.


in an open volume, batch style, cylindricalchamber measuring approximately 50 cm indiameter and 55 cm deep. An AngstromSciences 150 mm source was used with either asilicon or titanium metallic target. The chamberwas pumped to a base pressure of less than 1.33x 10-4 Pa (1.0 x 10-6 Torr) prior to each test andoperated with 0.4 Pa (3.0 x 10-3 Torr) argon. AnAdvanced Energy Pinnacle®Plus pulsed-dcpower supply was operated at 1000 watts pulsedat 100 kHz and 60 or 80% duty factor for alldepositions (depending on arc activity). AnAdvanced Energy IRESS reactive sputteringcontroller [16] equipped with an InficonTranspector 2 mass spectrometer was used toactively regulate reactive gas partial pressuresby providing control signals to Advanced EnergyAera® 980 series high-speed mass flowcontrollers. Glass slides and polished siliconslices were used as substrates and loaded onto ashuttered, rotating sample holder. A schematicof the test setup is shown in Figure 2.

Using partial pressure reactive gas controlwe first investigated single gas behaviors,depositing oxides and nitrides. We evaluatedtarget transition effects with each reactive gasand then showed how adding a second gas usingflow control only can lead to unwanted transi-tions and target trapping. The effect of addingpartial pressure control for the second reactivegas was then investigated demonstrating a meansfor stable control throughout a broad processingspace allowing access to a wide operating rangeand expansive compositional matrix.

ResultsTwo Gas Reactive Sputtering for SiliconOxynitrideOxide and nitride transition curves weregenerated in order to verify operation andbaseline the process in preparation for multi-gasprocesses. Figure 3 shows reactive gas partialpressure versus reactive gas flow for siliconoxide and silicon nitride formation. Partialpressure values are reported on a 0-10 volt scalerepresenting current collected on the Faradaycup in the mass spectrometer. These values areproportional to the actual pressure of each

constituent being measured. Pumping curves forboth reactive gases are also shown for reference.Noteworthy differences are the relatively higherpumping efficiency for nitrogen and increasedconsumption of oxygen to the reaction,especially at the lower partial pressures. Thisgives rise to a maximum flow value of oxygen atthe onset of target transition of approximately 15sccm. A maximum flow and indication of transi-tion are not observed for the nitrogen reaction.

With partial pressure control in place, allpoints on each curve in Figure 3 were availablefor stable operation. In addition, stable controlwas achieved by either starting in the metalmode or by beginning the process in thepoisoned or dielectric mode.

As nitrogen is added to the silicon oxideprocess the effect is to suppress the amplitude ofthe transition curve, or decrease the amount ofoxygen consumed in the process. Figure 4 showsthis effect in a family of curves generated withincreasing fixed nitrogen flow. In these curves,only oxygen is under partial pressure control. Theimportance of this distinction is discussed below.

Above approximately 12 sccm nitrogen, thetransition curves in Figure 4 become nearlylinear, suggesting that little if any oxygen isbeing incorporated in the reacted film. Despitethe significant change with increased nitrogenflow, stable process control throughout thetransition appears to be achieved in each case asthe smooth character in the transition ismaintained.

The corollary to Figure 4 is to operate thedeposition in nitrogen partial pressure control.Here oxygen is added at fixed flow values.

Figure 5 gives these results. Again, the curvature is suppressed as the

second gas is added indicating reduced nitrogenconsumption at higher oxygen flows. Throughoutthe range tested, the process appears to remainstable. This observation, however, is misleading.What is not shown in Figure 5 is the oxygenpartial pressure. For this test only nitrogen wasunder partial pressure control. In this caseoxygen was in fixed flow control leading to thebehavior shown in Figure 6.

Figure 6 illustrates the onset of targettrapping as described by Carlsson et.al. [13]. Atlow oxygen flows, consumption by the reactionkeeps oxygen partial pressures low throughoutthe tested nitrogen partial pressure range. Asthe oxygen flow is increased, the process beginsto poison, resulting in an uncontrolled increasein oxygen partial pressure. This behaviorindicates the presence of oxygen in excess ofwhat the deposition process can consume.

The trapping effect is more clearlyillustrated in Figure 7 where partial pressures ofboth nitrogen and oxygen were plotted alongwith target voltage. As before, nitrogen partialpressure is actively controlled and is incremen-tally increased over time to a predefinedmaximum. At this point the nitrogen partialpressure is decreased back to zero. As before,oxygen is introduced at a fixed flow and itspartial pressure is monitored but not directlycontrolled. The oxygen flow is 14 sccm here,chosen based on results from Figure 6.

As nitrogen partial pressure increases weinitially observe a gradual increase in oxygenpartial pressure. At just over three minutes into

Effective Closed-Loop Controlcontinued from page 25

Figure 2: Vacuum and control apparatus used fortwo gas reactive sputtering process.

Figure 3: Partial pressure transition curves for SiOxand SiNy. Pumping curves for each gas for compar-ison.

Figure 4: Fixed nitrogen flows and their effect onoxygen partial pressure transition curves forSiOxNy..

Figure 5: Fixed oxygen flows and their effect onnitrogen partial pressure transition curves forSiOxNy..

Figure 6: Oxygen partial pressure at fixed flows withnitrogen under partial pressure control.


the run, a poisoning event is experiencedcausing a rapid increase in oxygen partialpressure and a rapid decrease in sputteringvoltage. Once poisoned, the oxygen partialpressure remains relatively unchanged at a pointof saturation and the target remains in a trappedstate until both gases are removed from theprocess.

We found that trapping can be prevented byapplying partial pressure control to both reactivegases. Figure 8 gives results from the sameprocess sequence carried out in Figure 7, but

this time operated with partial pressure controlfor oxygen as well. In this case oxygen partialpressure was set to 50% the nitrogen partialpressure.

Similarly smooth transitions, not shownhere, were obtained across a broad range ofoxygen to nitrogen partial pressure ratios(O2:N2) from 0.05:1 to 4:1, operated with eithernitrogen or oxygen as the primary gas. None ofthese runs, operated with both gases in partialpressure control, showed any evidence ofuncontrolled target poisoning or trapping.

With stable control established, we testedthe ability to deposit intermediate oxynitridecompositions. Figure 9 gives rate and refractiveindex measurements for films deposited withvarying reactive gas partial pressure ratios. Ateither extreme in the chart we see resultsrepresentative of the binary process. SiOx filmsyielded RI ~ 1.45 at 1510 Å/min while SiNy gaveRI ~ 2.10 at 940 Å/min. Intermediate composi-tions provided values between the two extremes.These results demonstrate the ability to usesuch control to access intermediate composi-tions possessing properties between those of thepure oxide or nitride film.

Two Gas Reactive Sputtering for TitaniumOxynitride

The titanium oxynitride process showsmany similarities to the silicon process. Themost notable difference is a rise in cathodevoltage upon target transition opposed to the fallseen for silicon. Aside from this difference, mostother behaviors are quite similar. Titaniumoxide and nitride transition curves are shown inFigure 10. As was the case for silicon, the oxideprocess consumes more reactive gas and shows amore distinct target transition.

Target trapping was also observed fortitanium oxynitride depositions. Again, as wesaw for silicon, when one of the gases isregulated by flow only, the possibility for trappingexists. Figure 11 shows a case where wecontrolled the nitrogen partial pressure andoperated oxygen at a fixed flow of 7 sccm. Forthis test nitrogen partial pressure was increasedincrementally and then decreased. A poisoningevent is clearly shown at approximately 400seconds into the run. From this point the targetis trapped as indicated by both oxygen partialpressure and target voltage. Only when thereactive gases are removed does the target

transition out of the poisoned state.Partial pressure control of both reactive

gases was again shown to prevent this behavior.We tested a wide range of partial pressurecombinations and found stable, controlledoperation in all cases. Figure 12 is one exampleof such control. Here both oxygen and nitrogenare subjected to partial pressure control. Theresult was a smooth transition throughout theentire range tested for both reactive gases aswell as for target voltage.

Discussion

The presence of multiple reactive gases in anoxynitride reactive sputtering process addsvariables that can exceed the control capabilityof the typical single gas technique. The multi-gas process is complicated as the two reactivegases compete for available metal. The twosimultaneous reactions taking place do not actindependent of one another and, in fact, onereaction may dominate allowing the process tobecome poisoned and then trapped in anundesirable state preventing stable operation ofthe process.

To effectively prevent target trapping, aprocess control technique capable of differenti-ating the effects of individual reactive gases isneeded. We have demonstrated the occurrenceof target trapping in both silicon oxynitride andtitanium oxynitride reactive depositions. Wealso show the behavior to be effectivelyprevented by employing partial pressure controlfor both the oxygen and nitrogen reactive gasesduring deposition. By using such control, abroad range of operating conditions is availableproviding stable process performancethroughout.

Generating a composite summary of theoperating range tested, we can produce aprocess response surface for stable operation ofsuch depositions. One such response surface isshown in Figure 13 for the silicon oxynitridedeposition studied.

Using this surface one can visualize a vastrange of operating conditions available toperform the two gas reactive deposition. Westudied film properties from only a small portionof this surface. Points tested are indicated onthe chart and film data were presented earlier,in Figure 9.

Figure 7: Cathode voltage and reactive gas partialpressures during SiOxNy deposition resulting intarget trapping. Nitrogen is under partial pressurecontrol and oxygen fixed at 14 sccm.

Figure 9: Rate and refractive index for SiOxNydeposited by reactive gas partial pressure control.

Figure 10: Partial pressure transition curves for TiOxand TiNy..

Figure 8: Cathode voltage and reactive gas partialpressures during deposition of SiOxNy using partialpressure control of both gases. No target trapping isobserved.

Figure 11: Cathode voltage and reactive gas partialpressures during TiOxNy deposition resulting intarget trapping. Nitrogen is partial pressurecontrolled and oxygen is fixed at 7 sccm.

Figure 12: Cathode voltage and reactive gas partialpressures during deposition of TiOxNy using partialpressure control of both gases. No target trapping isobserved

Conclusion

Measuring the partial pressure of reactive gasesprovides a critical means for control of individualgases in a two reactive gas deposition. Withoutthe ability to differentiate the effects of eachreactive gas such processes are subject to aphenomenon called target trapping. Targettrapping can be effectively prevented by control-ling the partial pressure of the individualreactive gases in a multi-gas reactive sputteringprocess. With such control in place, reactivesputtering can be successfully used to produceoxynitride thin films with varying compositionsand properties.

References1. S. Schiller, K. Goedicke, J. Reschke, V.

Kirchhoff, S. Schneider, and F. Milde,“Pulsed magnetron sputter technology,”Surf. Coat. Technol., 61 (1993).

2. P. Kelly, P. Henderson, R. Arnell, G. Roche,D. Carter, “Reactive pulsed magnetronsputtering process for alumina films,” J.Vac. Sci. Technol., 18, 6, pp 2890-2896,(2000).

3. G. Este, and W.D. Westwood, “A quasi-direct-current sputtering technique for the deposi-tion of dielectrics at enhanced rates,” J.Vac. Sci. Technol., A 6 (3) 1988.

4. D.A. Glocker, “Influence of the plasma onsubstrate heating during low-frequencyreactive sputtering of AIN,” J. Vac. Sci.Technol. A 11, 2989 (1993).

5. W.D. Sproul, “High rate reactive sputteringprocess control,” Surf. Coat. Technol., 33,1987.

6. S. Schiller, U. Heisig, Chr. Korndorfer, G.Beister, J. Reschke, K. Steinfelder, and J.Strumpfel, “Reactive d.c. high ratesputtering as a production technology,”Surf. Coat. Technol., 33, 1987.

7. S. Berg, H-O. Blom, T. Larsson, and C.Nender, “Modeling of reactive sputtering ofcompound materials,” J. Vac. Sci. Technol.,A 5, 1987.

8. J.M. Schneider, W. D. Sproul, M.-S. Wong,and A. Matthews, “Very High Rate PulsedDC Sputter Deposition of AlOx Coatings,”Surf. Coat. Technol., 96 262 (1997).

9. K. Koski, J. Holsa, and P. Juliet, “Voltagecontrolled reactive sputtering process foraluminum oxide thin films,” Thin SolidFilms, 326, 1998.

10. Y. Ma and G. Lucovsky, “Deposition of singlephase, homogeneous silicon oxynitride byremote plasma-enhanced chemical vapor

deposition, and electrical evaluation inmetal-insulator-semiconductor devices,” J.Vac. Sci. Technol., B 12(4), 1994.

11. G.A. Al-Jumaily, T.A. Mooney, W.A. Spurgeon,and M. Dauplaise, “Ion assisted depositionof oxynitrides of aluminum and silicon,” J.Vac. Sci. Technol., A 7(3), May/June 1989.

12. J. Vuillod, “Preparation and characteriza-tion of plasma enhanced chemical vapordeposited silicon nitride and oxynitridefilms,” J. Vac. Sci. Technol., A 5(4), (1987).

13. P. Carlsson, C. Nender, H. Baránková, and S.Berg, “Reactive sputtering using tworeactive gases, experiments and computermodeling,” J. Vac. Sci. Technol., A 11(4),(1993).

14. H. Baránková, S. Berg, P. Carlsson, and C.Nender, “Hysteresis effect in the sputteringprocess using two reactive gases,” ThinSolid Films, 260, p. 181, 1995.

15. W.D. Sproul, D.J. Christie, D.C. Carter, S.Berg, and T. Nyberg, “Control of theReactive Sputtering Process Using TwoReactive Gases,” 47th Annual TechnicalConference Proceedings of the Society ofVacuum Coaters, 2003.

16. W. D. Sproul and B. E. Sylvia, “An IntegratedSolution for Reactive Sputtering,” Vac. Tech.and Coating, 2 No. 8, 32, 2001.

Effective Closed-Loop Controlcontinued from page 27

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Want to read more?We’ll be including more papers

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PSE 2004

Manufacturing Science and Technology; NanometerScale Science and Technology; Organic Films andDevices; Plasma Science and Technology;Semiconductors; Technology for Sustainability;Thin Films; Vacuum Technology. For details visitthe new AVS Web site at www.avs.org

SVC is a Cooperating Society for the OpticalInterference Coatings Ninth Topical Meetingand Tabletop Exhibit, June 27-July 2, 2004,Loews Ventana Canyon Resort & Spa, Tucson,Arizona. For more details visithttp://www.osa.org/meetings/topicals/oic/

The Association of Industrial Metallizers, Coatersand Laminators honored Celplast MetallizedProducts Ltd., Toronto, Ontario, with itsMetallized Product of the Year Award in Marchduring its Winter Management Meeting. Celplastmetallizes Cellofoil™ low-density polyethylene forbread bags used by Canada Bread Co. Ltd.,Etobicoke, Ontario, for its Dempster’s® brandwhite bread.

The SVC sponsored three promising studentsthrough its Student Sponsorship Program at thisyear’s TechCon. Zuzana Kucerova, a student atMasaryk University in the Czech Republic,presented a paper in the Optical Coating Sessionentitled, “Multilayer Protective Coatings forPolycarbonates Prepared by Plasma EnhancedCVD”. Jean-Michel Lamarre, a student at ÉcolePolytechnique in Montréal, Canada, presented hispaper in the Optical Coating Session entitled,“Optical Response from Single- and Multi-layerMetal/Dielectric Nanocomposite Thin FilmSystems”. Ales Kolouch, a student at theTechnical University of Liberec in the CzechRepublic, presented his paper entitled,“Comparison of Titanium Oxide CoatingsDeposited by PVD and PECVD” in the Tribologicaland Decorative Coating Session.

The SVC Student Sponsorship Program isdevoted to being a link between students andindustry professionals. For more informationabout student sponsorship, visithttp://www.svc.org/EP/EP_StudentProg.html.

For the first time, all Poster presentations at theSVC TechCon were eligible for a $200 BestPoster Award (see page 20), which resulted in atechnically and visually exciting session. ThePoster presentations were displayed side-by-sidein a highly visible area in the busy Exhibit Halland remained there until the end of the Exhibiton Tuesday afternoon. By extending the viewingtime and placing the Posters in the Exhibit Hall,more attendees were able to see the posters andtake part in the question and answer phasewithout missing any of the Exhibit.

The SVC plans to continue the “Best Poster”Award for the 2005 TechCon in Denver, CO, andreminds authors that the deadline for submittingabstracts is October 1, 2004.

The Society of Vacuum Coaters wishes toacknowledge Elsevier for their support in co-sponsoring the very successful Smart MaterialsSymposium held at the 2004 SVC AnnualTechnical Conference (see page 15). It isplanned to repeat this format and the extensionof the TechCon to four days in 2005 in Denver.

The SVC has created a new section of the WebSite called “In Memoriam” to honor thepassing of those who have been part of the SVCcommunity and who have served the Society.SVC Mentors, short course instructors, TACChairs, Board members, and those who havebeen interviewed for oral histories will beremembered. It is with regret that weannounce the passing of Ted Van Vorous inFebruary 2004.

Please visit our tribute to Ted at http://www.svc.org/AboutSVC/AS_Memoriam.html

The Society regretfully announces the passingof Professor Ron Howson of LoughboroughUniversity, UK. Ron helped initiate the IPATseries of international conferences and wasinvolved in the Coatings on Glass series ofconferences. He was a regular contributor tomany of the international vacuum coatingconferences across the world and part of his

legacy is the continued contribution to the fieldmade by so many of his past research students.In 1982 he and his research group won the BPNational Energy Research Prize, followed thenext year by the BP International Prize forEnergy Research.

The SVC Awards Committee announced theMentor Award recipients for 2004 at the SVCAnnual Business meeting held on April 25 inDallas: Harold Gadon, Providence MetallizingCompany, Inc. (retired); Russell J. Hill, VONARDENNE Coating Technology; and RichardSwisher, Sheldahl, Inc.

The new SVC Nominations Committee Chair,John Felts, welcomes suggestions frommembers for nominees for the position ofDirector. John can be reached [email protected]. The Board will haveseveral vacancies for Director to fill for the2005-2008 period. SVC Board policy is that theNominations Committee and Board of Directorshave members who represent the broadinterests of the different technologies associ-ated with the society.

SVC is pleased to announce several new SVCCommittee Chairs: Lisa Robillard, MKSInstruments, Inc. has accepted an appointmentas the SVC Exhibit Committee Chair. She can bereached at [email protected]. IsmatShah, University of Delaware, has accepted anappointment as the SVC Education CommitteeChair. Vasgen Shamamian, Dow CorningCorporation, has accepted an appointment as theSVC Assistant Education Committee Chair. Ismatand Vasgen can be reached at [email protected] [email protected] respectively.Lisa, Ismat and Vasgen all welcome your views onhow to move SVC forward in these areas.

SVC welcomes Charles Bishop, C.A. BishopConsulting Ltd.,([email protected]) as thenew Vacuum Web Coating TAC Co-Chair, andRoel Tietema, Hauzer Techno Coating BV,([email protected]) as the new Tribologicaland Decorative Coating TAC Chair.

The Society of Vacuum Coaters is co-sponsoringthe 5th International Conference on Coatingson Glass (ICCG) to be held July 4–8, 2004 inSaarbruecken, Germany. For details visitwww.iccg.de.

AVS 51st International Symposium &Exhibition will be held at the AnaheimConvention Center, Anaheim, CA on November14–19, 2004. Session topics include thefollowing: Advanced Surface Engineering;Applied Surface Science; Biomaterial Interfaces;Electronic Materials and Devices; High-KDielectrics; Magnetic Interfaces andNanostructures; MEMS and NEMS;

Society and Industry News


SVC Thanks TechConEvent SponsorsThe SVC would like to acknowledge thecompanies sponsoring many eventsduring the TechCon.

Beer Blast Sponsors:Dexter Magnetic Technologies, Inc.DynaVacEnglehard CorporationGeneral Vacuum EquipmentGlassman High Voltage, Inc.Heraeus, IncorporatedHuettinger Electronic, Inc.KDFMDC Vacuum Products CorporationRigaku/MSC Vacuum ProductsRohwedder, Inc.

Coffee Break Sponsors:MeiVac, Inc.Pfeiffer VacuumVarian Inc., Vacuum Technologies

Internet Cafe Sponsors:Advanced Energy Industries, Inc.General Vacuum EquipmentEnglehard CorporationMKS Instruments, Inc.MDC Vacuum Products Corporation

Heuréka! Post-Deadline Session:Advanced Energy Industries, Inc.

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Reserve Your Booth Early for the 2005 TechCon ExhibitApril 25th and 26th, 2005, at the Adam’s Mark Hotel, Denver, Colorado

Don’t wait until the last minute to reserve your booth in the only exhibit devoted entirely toVacuum Coating. This premier exhibit attracts thousands of professionals in every aspect ofvacuum coating, including engineers, manufacturers, technologists, scientists, andbusiness professionals. Year after year, the TechCon Exhibit succeeds in offering exhibitorsan array of opportunities to promote products, make contacts, and generate new businessin the vacuum coating industry. To reserve your booth or inquire about sponsorship,call 505/856-7188 or E-mail [email protected].

Join us in Denver, Colorado,in 2005!

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