dual core manual

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CD2.01-002 DUAL SPINDLE

CORE DEPOSITION SYSTEMREFERENCE MANUAL

ASI/SILICA MACHINERY, LLC.Head Office

515 Loring Avenue

Los Angeles, CA 90028

United States of America

Manufacturing Facility

1210 East 223rd Street

Carson CA 90745

United States of America

PH: +1 (818) 920 1962 FAX: +1 (818) 920 1792

www.asisilica.com

PH:+1 (310) 835 3368 FAX: +1 (310) 835 3378

www.asisilica.com


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CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC 2

Table of Contents

1.0 Safety........................................................................................................................................... 7

2.0 Material Safety Data Sheets.................................................................................................. 8

2.1 MSDS OXYGEN ...................................................................................................................................9

2.2 MSDS HYDROGEN ...........................................................................................................................19 2.3 MSDS NITROGEN .............................................................................................................................27

2.4 MSDS SILICON TETRACHLORIDE...............................................................................................35

2.5 MSDS HYDROGEN CHLORIDE .....................................................................................................44

2.6 MSDS GERMAINIUM TETRACHLORIDE.....................................................................................53

2.7 MSDS ACETYLENE ..........................................................................................................................59

3.0 System Requirements........................................................................................................... 68

3.1 Space Requirements............................................................................................................. 68

4.0 Core Deposition Operating Procedure............................................................................. 69

4.1 Materials/Tools needed for the process .............................................................................................694.2 How to set up and load mandrel assembly ........................................................................................69

4.3 Checklist for an OVD Core run .........................................................................................................72

4.4 Loading a recipe ..................................................................................................................................74

4.5 Editing a Recipe ..................................................................................................................................75

4.6 Running a Recipe ................................................................................................................................78

4.7 OVD Core Run Characteristics .........................................................................................................79

4.8 Shutdown Procedure ...........................................................................................................................82

4.9 Preparation for sintering ....................................................................................................................83

4.10 Materials Usage Totals .......................................................................................................................84

5.0 Core Deposition Software.................................................................................................... 85

5.1 Startup.................................................................................................................................................85

5.2 Function Screens .............................................................................................................................85

5.2.1 Configuration Screen ..................................................................................................................... 86

5.2.2 Configuration Screen ..................................................................................................................... 86

D/A output controls (Blue) ....................................................................................................................................... 87

A/D input indicators (Green) ................................................................................................................................... 87

DIO Out (Orange) .................................................................................................................................................... 87

DIO In (Gray)........................................................................................................................................................... 87

5.2.3 Motor Screen ..................................................................................................................................... 88

5.2.4 Scales and Controllers Screen .................................................................................................... 90

5.2.5 Image Configuration Screen ...................................................................................................... 90


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5.2.6 Monitor Screen ............................................................................................................................... 91

5.2.7 Monitor Mode Controls and Indicators.................................................................................................. 92

5.2.8 Recipe Editor Screen ..................................................................................................................... 94

5.2.9 Manual Torch Screen .................................................................................................................... 95

5.2.10 MFC Sizing Screen ..................................................................................................................... 98

5.2.11 Information Screen ...................................................................................................................... 98

5.2.12 Alarm Screen .............................................................................................................................. 99

5.2.13 Auto Zero Screen ..................................................................................................................... 101

5.2.14 Gas Usage Screen ................................................................................................................... 102

6.0 ASI GeCl4 Vaporizer System............................................................................................. 104

6.1 GeCl4 Vaporizer System Description........................................................................................104

6.2 GeCl4 Vaporizer System Fume Stream ....................................................................................107

6.3 GeCl4 Vaporizer System Operation...........................................................................................108

6.4 GeCl4 Vaporizer System Process Mode ..................................................................................109

6.5 GeCl4 Vaporizer System Purge Mode.......................................................................................109

6.6 GeCl4 Vaporizer System Start Up ..............................................................................................109

6.7 How To Fill The GeCl4 Vaporizer System ................................................................................110 6.7.1 Pre-requisites............................................................................................................................................. 110

6.7.2 Instructions................................................................................................................................................. 110

6.8 Warming Up the Vaporizer (and Burp the Vaporizer During Heat Up ..........................111

6.8.1 Pre-requisites............................................................................................................................................. 111

6.8.2 Instructions................................................................................................................................................. 111

6.9 GeCl4 Vaporizer System Controlled Fume Production........................................................111

6.9.1 Pre-requisites............................................................................................................................................. 111

6.9.2 Start Up Sequence .................................................................................................................................... 112

6.9.3 Shut Down Sequence............................................................................................................................... 112

6.10 GeCl4 Vaporizer System Maintenance .....................................................................................113 6.10.1 How to Swap Out a GeCl4 Mass Flow Controller (MFC) ............................................................ 113

6.10.1.1 Pre-Requisites ............................................................................................................................. 113

6.10.1.2 Pre-Requisites ............................................................................................................................. 113

6.10.2 Method .................................................................................................................................................... 113

6.10.2.1 Purge MFC to be Changed ....................................................................................................... 113

6.10.2.2 Cool Down the GeCl4 Vaporizer ............................................................................................. 113

6.10.2.3 Warm Up the GeCl4 Vaporizer................................................................................................. 114


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6.10.3 Replacing the (BARITRON) Pressure Sensor And/OR Rupture Disc ..................................... 114

6.10.3.1 Pre-Requisites ............................................................................................................................. 114

6.10.3.2 Equipment Needed ..................................................................................................................... 114

6.10.3.3 Method ........................................................................................................................................... 114

Appendix 1 - Full State Table .............................................................................................................. 116

7.0 Dual Spindle Clad Deposition System Maintenance.................................................. 117

7.1 Maintenance & Lubrication of Linear Positioning Tables ...................................................117

7.1.1 Drive Mechanisms .................................................................................................................................... 117

7.1.2 Acme Screws ............................................................................................................................................. 117

7.1.3 Ball Screws ................................................................................................................................................. 117

7.1.4 Lubrication (Acme Screws) .................................................................................................................... 117

7.1.5 Lubrication (Ball Screws)........................................................................................................................ 118

7.2 Trouble Shooting the End Burner Flame .................................................................................119

7.3 Applying Heating Tape .................................................................................................................120

7.4 Torch Alignment .............................................................................................................................121

7.4.1 Torch Position Relative to Mandrel Centerline ................................................................................. 1217.5 Emptying Vaporizer Tank and Preheater .................................................................................123

7.6 Maintenance & Lubrication of Linear Positioning Tables ...................................................131

7.7 Temperature Controller Setup ....................................................................................................132

8.0 Dual Spindle Clad Deposition System Maintenance.................................................. 137

8.1 Load Cell Readout and Load Cell Calibration ........................................................................137

8.1.1 Scale Readout Screen.............................................................................................................................. 137

8.1.2 Dual Spindle Scale Readout Screen Descriptions ........................................................................... 137

8.1.2.1 Zero ..................................................................................................................................................... 137

8.1.2.2 Mode ................................................................................................................................................... 137

8.1.2.3 Tare ..................................................................................................................................................... 1388.1.2.4 Print..................................................................................................................................................... 138

8.1.2.5 _/Test/Clr............................................................................................................................................ 138

8.1.2.6 1/Tare/Val ........................................................................................................................................... 138

8.1.2.7 2/Status/Bar....................................................................................................................................... 139

8.1.2.8 3/Lb/Kg ............................................................................................................................................... 139

8.1.2.9 4/......................................................................................................................................................... 139

8.1.2.10 5/....................................................................................................................................................... 139

8.1.2.11 6 Setpoint............................................................................................................................................. 139

8.1.2.12 7 Option............................................................................................................................................... 140

8.1.2.13 8/Cal..................................................................................................................................................... 1408.1.2.14 9/......................................................................................................................................................... 140

8.1.2.15 0/Exit.................................................................................................................................................... 140

8.1.2.16 Enter .................................................................................................................................................... 140

8.1.3 Dual Spindle Scale Calibration Procedure (Hard Calibration)....................................................... 141

8.1.4 Setting The Zero Calibration Value ...................................................................................................... 141

8.1.4.1 To zero the scales ................................................................................................................................ 143

8.1.5 Setting The Span Calibration Value ..................................................................................................... 144


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8.1.6 Checking the Weight of the System. .................................................................................................... 145

8.1.7 Tare and Zero the Scale Read Outs. .................................................................................................... 145

8.1.8 Trouble Shooting the Scale Readout. .................................................................................................. 145

9.0 Spindle Leg Chiller Connection....................................................................................... 146

9.1 Uncrating and Mechanical Installation .....................................................................................146

9.2 Electrical Installation PDU ...........................................................................................................148

9.3 Programming and Temperature Setting...................................................................................149

9.3.1 Selecting the Sensor Type...................................................................................................................... 149

9.3.2 UM4300 Controller Temperature Settings .......................................................................................... 150

9.4 Chiller Programming Chart..........................................................................................................151

10.0 Trouble-Shooting For Deposition & Sintering & Process Activities...................... 152

10.1 Process Activities ..........................................................................................................................152

10.1.1 Introduction ........................................................................................................................................... 152

10.1.1.1 Ideal Refractive Index Profile ........................................................................................................... 152

10.1.1.2 Various modes in the recipe............................................................................................................... 153

1. Mandrel Flame Polish Mode ......................................................................................................................... 1532. Carbon Coating Mode ................................................................................................................................... 153

3. Carbon Flame Polish Mode........................................................................................................................... 153

4. Centerline Mode (SiCl4 only) ......................................................................................................................... 153

5. Core A Mode (SiCl4 + GeCl4)........................................................................................................................ 153

6. Core B Mode (SiCl4 + GeCl4)........................................................................................................................ 153

7. Clad Mode Oscillation 1 (SiCl4 only) ......................................................................................................... 153

8. Clad Mode Oscillation 2 (SiCl4 only) ......................................................................................................... 153

10.1.2 Tuning centerline refractive index ................................................................................................... 154

10.1.3 Tuning Refractive Index Delta ........................................................................................................... 154

10.1.4 Examples of Index Profiles and Methods of Tuning ................................................................... 15510.1.4.1 Profile with a high dip........................................................................................................................ 155

10.1.4.2 Delta with slanted slopes .................................................................................................................... 155

10.1.4.3 Delta Height Adjustment ................................................................................................................... 156

10.1.5 Changing SiCl4 and GeCl4 flows in the recipe............................................................................. 157

10.1.6 Oscillations at the Delta ..................................................................................................................... 158

10.1.7 How To Calculate Core Weight Given a Core/Clad Diameter Ratio ......................................... 159

10.1.8 Measurement Diffraction Type Problem......................................................................................... 160

10.1.8.1 Example 1: Power loss in the center ................................................................................................ 160

10.1.8.2 Example 2: Power loss at the edges................................................................................................... 160

10.1.9 How To Do A Manual Density Profile .............................................................................................. 16110.1.10 Troubleshooting Torch Buildup. ...................................................................................................... 163

10.1.11 Flow Analysis ........................................................................................................................................ 165

10.1.12 Recipe Command Spreadsheet ........................................................................................................ 167

10.1.13 Sudden Change in Index Profile (delta/shape) Between Preforms ......................................... 170

10.2 PHYSICAL TUNING / CONTROL .................................................................................................170

10.2.1 Surface Smoothness (ripples) .......................................................................................................... 170

10.2.2 Density Control ..................................................................................................................................... 170


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10.2.3 Deposition Rate .................................................................................................................................... 171

1) Traverse Speed .......... ........... .......... ........... .......... ........... .......... ........... .......... ........... .......... ........... .......... ....... 171

2) Temperature/ heat (hydrogen flow) ............................................................................................................... 171

3) SiCl4 flow rate ............................................................................................................................................... 171

4) Cleanliness of fume tubes .............................................................................................................................. 171

5) Makeup flow rate ........................................................................................................................................... 171

6) Alignment ...................................................................................................................................................... 17110.2.4 Diameter Variation ............................................................................................................................... 172

10.2.5 Soot Cracking at Handle Interface ................................................................................................... 173

10.2.6 Splits........................................................................................................................................................ 173

10.2.7 Warts ....................................................................................................................................................... 174

10.2.8 Core/Clad Cracking After Sintering ................................................................................................. 174

10.3 FIBER TUNING/CONTROL ...........................................................................................................175

10.3.1 Modefield Diameter Out of Specification ....................................................................................... 175

10.3.2 Cutoff Wavelength Out of Specification ......................................................................................... 176

10.3.3 Core/Clad Concentricity ..................................................................................................................... 177

10.3.4 High Attenuation................................................................................................................................... 17810.3.5 Gas Bubbles .......................................................................................................................................... 180


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1.0 Safety

Forward

In common with all manufacturing equipment, the ATMOSPHERIC CHEMICAL VAPOR CORE SYSTEMcontains potential hazards to the operator.

Warning

In order to avoid serious injury or death and or damaging the equipment, it is very important that onlyqualified and properly trained people should be allowed to operate these equipment.

The ACVC system runs on chemicals and gases that could be:

Extremely corrosive, and or simple asphyxiant.

Therefore:

All piping connecting these chemicals to the system must be tested for leaks and certified prior tooperation.

Piping materials must be compatible with the commodity to be handled.

The site must be equipped with gas detectors that are capable of detecting any leaks in the area, andshutting down the supply at the source.

The equipment must be connected to a pollution control system that is capable of handling the type ofchemicals used and generated.

The ducting connecting the equipment to the pollution control system must be capable of handling heatand corrosion.

Material Safety Data Sheets are provided in this section for the various chemicals used and generated;operators of this equipment should take the time and familiarize themselves with the information provided inthese data sheets, and follow the safety guidelines and the handling procedures they contain.


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2.0 Material Safety Data Sheets

The following section contains the material safety data sheets for the material used with the ACVC02Dual Spindle Core Deposition System.


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2.1 MSDS OXYGEN


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2.2 MSDS HYDROGEN


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2.3 MSDS NITROGEN


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2.4 MSDS SILICON TETRACHLORIDE


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2.5 MSDS HYDROGEN CHLORIDE


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2.6 MSDS GERMAINIUM TETRACHLORIDE

1.6.1. PRODUCT AND COMPANY IDENTIFICATION

Product Identifier: Germanium TetrachlorideGeneral Use: Telecommunications fiber productionProduct Description: High purity inorganic chloride

MANUFACTURER:

Eagle-Picher Technologies, LLCElectro-Optic MaterialsP. O. Box 737Hwy. 69A EastQuapaw, OK 74363

EMERGENCY TELEPHONE NUMBERS:

Eagle-Picher EOM (01) 918/673-1650 (USA) 8 am-4:30 pm CST M-FINFOTRAC 800/535-5053 24 hours everyday

1.6.2. COMPOSITION/INFORMATION ON INGREDIENTS

CAS # CHEMICAL NAME % VOLUME EINECS#10038-98-9 Germanium Tetrachloride 100 233-166-7Chemical Formula : GeCl4Hazard Symbols: CRisk Phrases: 14 34

OSHA REGULATORY STATUS:

While this material is not classified as hazardous under OSHA regulations, this MSDS contains valuableinformation critical to the safe handling and proper use of the product. This MSDS should be retained andavailable for employees and other users of this product.

1.6.3. HAZARDS IDENTIFICATION

EMERGENCY OVERVIEW:

Warning! Water reactive, producing toxic and corrosive fumes. Causes eye and skin irritation. Causesirritation of the digestive and respiratory tracts. Fumes in moist air. May form hazardous decompositionproducts which may cause irritation and possible burns. Vapors can cause eye irritation.

TARGET ORGANS:None known

POTENTIAL HEALTH EFFECTS:

ROUTES OF ENTRY:

Skin Contact: Yes Skin Absorption: No Ingestion: YesEye Contact: Yes Inhalation: Yes

HEALTH EFFECTS:

Irritant: Yes Sensitization: NoTeratogen: No Reproductive Hazard: No


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EXPOSURE LIMITS:

PEL-OSHA: None ListedTLV-ACGIH: None ListedNIOSH: None Listed

INHALATION:

Irritating to upper and lower respiratory tracts. Symptoms may include coughing, labored breathing andexcessive salivary and sputum formation. Excessive irritation of the lungs causes acute pneumonitis andpulmonary edema which could be fatal.

EYE CONTACT:Lacrymator. May cause irritation and possible burns.

SKIN CONTACT:May cause irritation, and possible burns, especially if skin is wet or moist. .

INGESTION:May cause severe gastrointestinal tract irritation and possible burns.

CHRONIC:May cause liver and kidney damage.

NFPA Hazard Codes System HMIS Hazard Codes Ratings

Not Published Not Published 0 = No Hazard1 = Slight Hazard2 = Moderate Hazard3 = Serious Hazard4 = Severe HazardSee Section 8 for Personal Protection information.See Section 11 for Toxicological information.

POTENTIAL ENVIRONMENTAL EFFECTS:

The ecotoxicity and environmental fate of Germanium Tetrachloride is currently not available.

1.6.4. FIRST AID MEASURES

INHALATION:

Remove victim of exposure to fresh air immediately. If not breathing, give artificial respiration. If breathingis difficult, give oxygen. Seek medical aid immediately.

EYE CONTACT:

Immediately flush eyes, including under eyelids, with large amounts of water for at least 15 minutes. Seekmedical aid immediately.

SKIN CONTACT:

Remove contaminated clothing (including shoes) as soon as possible. Flood skin with large amounts ofwater for at least 15 minutes. Seek medical aid immediately.


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INGESTION:

If swallowed, DO NOT induce vomiting. Never give anything by mouth to an unconscious person.If conscious, have victim rinse mouth liberally with water. Seek medical aid immediately.

1.6.5. FIRE FIGHTING MEASURES

Flashpoint and Method: None / Not Applicable

Flammable Limits: Not Flammable

Autoignition Temperature: None

LEL (%): None UEL (%): None

HAZARDOUS COMBUSTION PRODUCTS: None

Sensitivity to Mechanical Shock: NoneSensitivity to Static Discharge: NoneNFPA Rating: Not Published

FIRE FIGHTING INSTRUCTIONS:

Germanium Tetrachloride REACTS VIOLENTLY WITH WATER OR STEAM TO PRODUCEHYDROCHLORIC ACID.

FIRE FIGHTING EQUIPMENT:

Use normal firefighting procedures which include wearing NIOSH/MSHA approved self-containedbreathing apparatus in pressure-demand. Wear MSHA/NIOSH approved, flame and chemical resistantclothing; hats, boots and gloves. If without risk, remove material from fire area. EXTINGUISHING MEDIA:Use media appropriate for surrounding materials. Product reacts with water to form corrosive fumes.

1.6.6. ACCIDENTAL RELEASE MEASURES

Evacuate personnel from affected area. Use proper personal protective equipment as indicated in Section8.

SPILLS / LEAKS: Absorb spill with inert material then place into a chemical waste container.

Provide ventilation. Refer to section 13 for disposal considerations.

1.6.7. HANDLING AND STORAGE

HANDLING:

Use only in a well ventilated area. Do not allow water to get into container because of violent reaction.

Avoid contact with eyes, skin and clothing. Avoid ingestion and inhalation. Wash thoroughly after handling.Remove contaminated clothing and wash before reuse.

STORAGE:

Store in tightly closed container in a cool , dry, well ventilated area away from incompatible substances(See Section 10).


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1.6.8. EXPOSURE CONTROLS/PERSONAL PROTECTION

EXPOSURE LIMITS:PEL-OSHA : None ListedTLV-ACGIH: None ListedNIOSH: None Listed

ENGINEERING CONTROLS:

The use of local exhaust forced ventilation is recommended to prevent accumulation above the exposurelimits of hydrochloric acid. Provide mechanical ventilation of confined spaces. Use explosion-proofventilation equipment in accordance with electrical codes.

PERSONAL PROTECTION:

RESPIRATOR:

NIOSH/MSHA approved respirator with an organic vapor cartridge. Follow OSHA regulations in 29 CFR1910.134 or European Standard EN 149 as appropriate. Always use a NIOSH or European Standard EN149 approved respirator when necessary. Positive pressure air line with full face mask and escape bottleor self-contained breathing apparatus should be available for emergency use.

PROTECTIVE CLOTHING:

Protective Safety Glasses or Chemical safety goggles as described by OSHA regulations in 29 CFR1910.133 or European Standard EN166 as appropriate. Rubber gloves, lab coat and apron, flame andchemical resistant coveralls as appropriate. Other / General: Safety Shower and Eyewash fountainavailable.

1.6.9. PHYSICAL AND CHEMICAL PROPERTIES

Parameter Value Units

Vapor Pressure: 72 Not Applicable

Specific Gravity (H2O=1): 1.844 g/cm3Solubility in Water: Hydrolyzes Not ApplicablepH: Not Available Not ApplicableBoiling Point: 82 - 84 C @ 760.00 mm HgDecomposition Temperature: Not Available Not ApplicableViscosity: Not Applicable Not ApplicableVapor Density (Air=1): Not available Not ApplicableEvaporation Point: Not Available Not ApplicableFreezing / Melting Point: -49.5 COdor: Acrid, irritating Not ApplicableOdor Threshold: Not Available Not ApplicableAppearance: Colorless Not ApplicablePhysical State: Fuming Liquid Not Applicable

Molecular Formula: GeCl4 Not ApplicableMolecular Weight: 214.4 Not Applicable

1.6.10. STABILITY AND REACTIVITY

CHEMICAL STABILITY:

Stable under normal temperatures and pressures.


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INCOMPATIBLE MATERIALS AND CONDITIONS TO AVOID:

Rapidly reacts with water or steam to form hydrochloric acid, which reacts to most metals and manyorganic materials with the evolution of heat and hydrogen gas. Incompatible materials, contact with wateror exposure to moist air.

HAZARDOUS DECOMPOSITION PRODUCTS:

Hydrochloric acid.Hazardous Polymerization: Will not occur.

1.6.11. TOXICOLOGICAL INFORMATION

RTECS# : LY5225000LD50/LC50: LC50=44 gm/m3/2H (inhalation, mouse)Carcinogenicity: Not listed by ACGIH, IARC, NIOSH, or OSHAEpidemiology: Not AvailableTeratogenicity: Not AvailableReproductive Effects: Not AvailableNeurotoxicity: Not AvailableMutagenicity: Not Available

Other: Not AvailableSee Section 3 for Potential Health Effects.

1.6.12. ECOLOGICAL INFORMATION

Ecotoxicity: Not AvailableEnvironmentl Fate: Not availablePhysical / Chemical: Not AvailableOther: Not Available

1.6.13. DISPOSAL CONSIDERATIONS

Return to supplier or dispose of in accordance with all current local, State and Federal Regulations.

RCRA D-Series Manimum Concentration of Contaminants: None ListedRCRA D-Series Chronic Toxicity Reference Levels: None ListedRCRA F-Series: None ListedRCRA P-Series: None ListedRCRA U-Series: None Listed

1.6.14. TRANSPORT INFORMATION

Shipping Name Hazard Class UN Number Packing Group DGC

US DOT Corr Liq, Acidic, Inorg, N.O.S.* 8 3264 II --IMO Corr Liq, Acidic, Inorg, N.O.S. 8 3264 II --IATA Corr Liq, Acidic, Inorg, N.O.S.* 8 3264 II --RID/ADR Corr Liq, Acidic, Inorg, N.O.S. 8 3264 II 8 (66B)Can. TDG Corr Liq, Acidic, Inorg, N.O.S. 8 (9.2) UN3264 II --


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1.6.15. REGULATORY INFORMATION

US FEDERAL:

TSCA (Toxic Substance Control Act): Listed on the TSCA inventory.Health Safety Reporting List: Not listed.Chemical Test Rules: Not listed.Section 12b: Not listed

TSCA Significant New Use Rule: No SNUR under TSCASARA:Section 302 (RQ): No RQSection 302 (TPQ): No TPQSection 313: Not Reportable.Clean Air Act: Does not contain any hazardous air pollutants.Does not contain any Class 1 Ozone Depletors.Does not contain any Class 2 Ozone Depletors.Clean Water Act: Not listed as hazardous Substance under the CWA.Not listed as Priority Pollutants under the CWA.Not listed as Toxic Pollutants under the CWA.OSHA: Not considered highly hazardous by OSHA.STATE: Germanium Tetrachloride is not present on State lists from CA, PA, MN, MA, FL, or NJ.

California No Significant Risk level: Not listed.European / International : European labeling in accordance with EC Directives:Hazard Symbols: CRisk Phrases: R 14 Reacts violently with water.R 34 Causes BurnsSafety Phrases: S 25 Avoid contact with eyes.S 36/37/39 Wear suitable protective clothing, gloves, andeye/protection.S 45 In case of accident or if you feel unwell, seek medicaladvice immediately (Show the label where possible).S 8 Keep container dry.WGK (Water Danger / Protection): No information available.Canada: Is listed on Canadas DSL/NDSL List.

Does not have a WHMIS Classification.Is not listed on Canadas Ingredient Disclosure List.Exposure Limits: OEL-RUSSIA : STEL 1 mg/m3

1.6.16. OTHER INFORMATION

MSDS Creation Date: September , 1979MSDS Revision Date: February, 2001THE STATEMENTS CONTAINED HEREIN REPRESENT THE BEST INFORMATION CURRENTLYAVAILABLE TO US, AND IS OFFERED FOR INFORMATIONAL PURPOSES ONLY. THISINFORMATION IS INTENDED TO BE FOLLOWED BY PERSONS HAVING RELATED TECHNICALSKILLS AND AT THEIR OWN DISCRETION AND RISK. SINCE CONDITIONS AND MANNER OF USEARE OUTSIDE OUR CONTROL, WE MAKE NO WARRANTIES, EXPRESS OR IMPLIED, AND ASSUME

NO LIABILITY IN CONNECTION WITH ANY USE OF THIS INFORMATION.


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2.7 MSDS ACETYLENE


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3.0 System Requirements

3.1 Space Requirements

FRONT OF MACHINE

441 CM

200 cm

BLOWER CHILLERVAPORISERS AND

WATER BATH

DEPOSITION MACHINECTRLCABIN

MAIN

GAS

PANEL


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4.0 Core Deposition Operating Procedure

4.1 Materials/Tools needed for the process

MandrelHandle

Three O-rings: 75 Vinton; Size 2.4 x 7.6V block inserts (replace if deteriorated)

Teflon PlugGases and Chemicals (Hydrogen, Oxygen, Nitrogen, Acetylene, GeCl4, SiCl4)

Isopropanol and clean-room wipers

Igniter (to light up the torch)Allen wrench (to tighten cap onto chuck)

4.2 How to set up and load mandrel assembly

Clean the mandrel thoroughly with alcohol and appropriate wiper.

Slide two O-rings (75 Viton; Size 0.312ID x 0.5) into the mandrel so that they are about 200mm

and 250mm from the end with a bigger diameter. The mandrel will be pulled out after deposition,

so it is designed to be tapered, with diameter of one end bigger than the other.

1) Slide the handle into the mandrel from the end that has a smaller diameter.


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4) Slide the handle all the way so that the o-rings are inside the handle as shown on the picturebelow. Leave about 35mm-40mm of mandrel length behind the handle.

Notice that the 2 O-rings have rolled towards the left when the handle is being slid through. The O-

rings need to be located at a maximum of 130mm from the wide end of the handle. Too close to theend burner flame will cause the O-rings to burn and melt.

5) Insert the hollow Teflon plug through the mandrel from the left end and push in firmly to helpsecure the handle on the mandrel.

6) Put in the chuck cap and an o-ring into the mandrel at the handle end, leaving about 1 cm ofmandrel length behind.

7) Insert that end into the left chuck and lay the other end onto the Teflon V-block. (Replace V-block inserts if deteriorated)


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8) Secure the mandrel by tightening the two screws, which hold the cap to the chuck.

9) Adjust the handle position so that the distance between the tip of the handle and the end of thechuck cap is 273mm +/- 2mm.


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4.3 Checklist for an OVD Core run

1. SiCl4 delivery system ready? Valves open?

2. SiCl4 tank level is high enough?

3. GeCl4 delivery system ready? Valves open?

4. Pushing Oxygen has a pressure of 30psi-35psi?

5. GeCl4 tank level is high enough?

6. Acetylene delivery system ready?

7. Are exhaust flows about 2300 ft/min for the center and800 ft/min for the sides?

8. Chamber and filters are clean?

9. Temperatures of chemlines, makeup lines, SiCl4 vaporizertank and SiCl4 vaporizer chamber are close/ equal to set points?

10.SMR temperature and pressure and hotbox temperature of the GeCl4vaporizer system close/equal to set points?

11.Re-zero GeCl4 and SiCl4 mfcs?

12.Replace V block inserts? (If the original ones deteriorated)

13.Scrubber is on?


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After loading in the mandrel and completing the items on the startup checklist, the user is now ready touse the program and start a run.

In all times ASI software, Core Version X.X should be running, if this is not so, click on the

desktop. After configuration, the program should be on standby/ready mode, showing the main screen

as below.

The user can access various functions of the program by using the icons on the top of the screen.


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4.4 Loading a recipe

In order to run a recipe, that recipe has to be loaded first by clicking on icon on the top of themain screen. Then the recipe editor screen will be shown as below.

Click on the icon on the top left corner. A directory will appear, select the

appropriate recipe. You can only load a recipe with a seq extension. The selected recipe will beshown in a spreadsheet format called recipe editor. The first column displays a description of what thestep does. The second column contains action commands and the third column displays input

parameters, which are to be passed to the corresponding commands. The last column shows the units

of the parameters, these units do not have any impact on recipe execution. After loading a recipe, youmay click on

to return to the main screen.


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4.5 Editing a Recipe

Editing a recipe is also being done on the recipe editor screen. A complete reference of the functionsand arguments available to use in the sequence editor is provided. The sequence looks like an Excel

spreadsheet, but you cannot type in the cells directly. To create or modify a recipe, use the Recipe

Editing tools:

The test name and units are comment fields that they do not get executed and are present to make the

recipe steps more clear. The VI name is a ring list of all the commands available to the sequence editor.

The input buffer contains the arguments that will be passed to the selected function. The number ofarguments will depend on the particular function. The delete button deletes an entire row. Use of the

other controls will be illustrated in the following examples:

To modify an existing line:

In this example, we want to change MFC 4 setpoint from 15 to 20 lpm.

Select the row and click


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The current parameters arenow displayed in the text

boxes. The comma (,) is

always used as the fielddelimiter. Select the desired

field in the input buffer.

Change to the desired

setting, 20.

Click on

The new values is updated:

To create a new line, the process is similar. For example, we want to add a 1 second delay between row

54 and 55:

Select either row 54 or 55. You can insert a new row above or below the selected row. In this case we

will select row 55. Click on

Click on and select a VI from the ring list:


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Then fill (overwrite) the other fields of the editing tool.

Click on .

The new row is now inserted.

Note: If row 54 was selected previously, should be used.

One can also insert a blank line by using and with empty editing cells.

To copy and paste a line, click on the line that is to be copied, and then click on ,editing cells will then be filled with by the copied values. Click on the line that is to be pasted and

click .

Before exiting, save changes you might want by clicking on icon.

To proceed, click on the icon. This will set the current recipe into the computers memory.This action will also return to the main screen.


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4.6 Running a Recipe

After loading a recipe, click on the monitor mode icon, for starting a run based on the loadedrecipe. The following screen will be shown.

Then

different actions will be taken according to the recipe. The left upper window shows the status and

which command is being executed. After some initialization of motors, controllers communication,etc, a dialog will show up as below:


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This dialog prompts for operators name, performs ID, carbon coating length, perform length, initialweight of the mandrel with handle setup, core weight, final weight (core plus clad weight) and data file

name. The core weight determines when the program switches core mode (depositing both SiCl4 and

GeCl4) to clad mode (SiCl4 only). The final weight determines when the run will be terminated. Thedata file name is the name of the file where all the process variables will be written. After entering

information into the dialog box, click on OK and the program will continue to run according to the

sequence in the recipe.

If for any reasons that the run needs to be aborted, click onto the icon on the

upper right hand corner of the monitor mode screen. Another option is to press on the EMO button onthe machine. This will shut down the whole machine including power.

4.7 OVD Core Run Characteristics

This system is able to run continuously while monitoring and controlling the process. Since each run isa significant investment, any shut down must be avoided. The operator must make sure that the

machine and process will have all the chemical resources that it needs prior to the start of the run.

In addition:

Constant supply of N2 is required for purging when the unit is not in run mode.

100-PSI gas is required to operate the Nupro valves in the vaporizer and gas cabinet.

Sufficient push gas pressure for both GeCl4 and SiCl4 delivery.

Then sequence of events take place as follows, according to a standard recipe:

Data acquisition begins.

HEPA blower turns on. SiCl4 vaporizer tank temperature ramps to set point.

Preform rotation initiates.

Traverse and end burner move to their starting positions.

Tare scales.

Ignite torches and end burners. The operator will need a flame starter.

During ignition of the left torch, the program will ask if operator is ready to ignite. When OK is

clicked, hydrogen will start flowing. Use a flame starter with a tip at least 5 inches long to start the

flame. As a safety measure, the computer will ask for confirmation of ignition. If the computer doesnot receive a confirmation, it will shut off hydrogen and start the ignition sequence over again.

After the left torch is ignited. The process will go through different modes. A typical ASI core-making

recipe includes seven modes in a run.

1. Mandrel Flame Polish Mode2. Carbon Coating Mode3. Carbon Flame Polish Mode4. Centerline Mode (SiCl4 only)


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5. Core A Mode (SiCl4 + GeCl4)6. Core B Mode (SiCl4 + GeCl4)7. Clad Mode-Oscillation 1 (SiCl4 only)8. Clad Mode-Oscillation 2 (SiCl4 only)

Depending on the recipe, the operator will often asked to confirm ignition and move torches in at thetransition of the first 5 modes. Before doing so (clicking ok), make sure that all gases and chemicalsflows are close to their set points.

When SiCl4 starts flowing out from the torches, the flames should immediately turn bright and whiteand have a well-defined shape, similar to the images below.

Flame with GeCl4 only is not bright and white like flame with SiCl4. There is only a very minor

brightness difference between flame with and without GeCl4. One way to test is to place a piece of

glass on top of the torches to see if there is any chemical deposited on it.

During the run, operator should make sure that the process parameters behave in a normal fashion.

From the monitor screen, observe the following for the SiCl4vaporizer:

Tank pressure:The pressure and tank temperature for the vaporizer is directly related. Therefore as

tank temperature is increasing, tank pressure will also increase and vice versa. The

normal operating tank temperature is 770C-79

0C. This line normally has a cyclic

pattern due to on/off SiCl4 refill. Every refill will bring down the tank temperature by

a few degrees. The tank then slowly heats up back to the set temperature, then another

refill lower the temperature again and so on. If the tank pressure continues to increase

(line is going up), this is a sign of running out of SiCl4, i.e., no refill. This might due toempty SiCl4 source tank or insufficient push gas pressure.


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Loadcell: The vaporizer has been programmed to refill whenever the level drops below 3.5V andstop filling when the level has reached 3.8V, as shown on the right most indicator

above the monitor.

Normal Exit Sequence

When the current preform weight exceeds target weight, the program will commence the exit routine.

Cut gases and chemicals to the torches.

Cut gases to the end burners.

End traverse oscillations.

Prompt to stop rotation.

Return to main screen.

Put SMR back to purge state.

Put Vaporizer tank to standby stage.


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4.8 Shutdown Procedure

In the event that a situation arises where the operator deems it necessary to shut down the process, clickon the button located monitor screen.

In doing so, the program will do the following:

Cut off all gases and SiCl4 (and GeCl4) flow so that the torch and end burners are extinguished.

Put SMR to purge state.

Put the vaporizer tank temperature controller in standby mode.

Prompt operator to stop preform rotation.

Return to main screen.

The computer will take about 5 to 10 seconds from the time the button is toggled to respond. Once pressed,there is no going back.

Emergency Shutdown

If the program does not respond, the EMO switch may be used. The EMO will immediately cut allpower to every circuit in the system. The EMO is the red button located on top of the left door panel

of the deposition cabinet.


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Caution

The EMO should be avoided unless absolutely necessary because it may damage the

computers hard drive as well as corrupt the scale and temperature controllers.

If the EMO is used, refer to the RESTART procedure. The EMO is the red button located on top of

the left door panel of the deposition cabinet.

Restart after an EMO shutdown

1. Press the RESTART button. (Green button next to the EMO red button)

2. During the computers boot up sequence the operator will be asked to run the utility SCANDISK.Select OK and the program will check the hard drive for damage. Usually the program will check

the file allocation system and repair a file. If the program goes into a sector-by-sector surface scan,it could be a sign that the hard disk is about to fail.

3. When Windows 2000 is running, click on the clad icon, labeled Core x.x version.

4. ASI software will start running, configuring and return to the standby/main screen.

4.9 Preparation for sintering

After the exit sequence, the program will return to the main screen. Use the motor screen and move

preform to the left almost. Let the preform cool down a little and then move it back to the middle.

Start a slow rotation and by using a knife, trim off loose soot at both ends, so the ends are

flat and hard, as shown as below.

The reason to trim away loose soot is that the soot density difference causes differentshrinkage and might add some bending to the preform upon sintering.

Take out the preform from the deposition cabinet. Place it in a safe place and let it cooldown before pulling out the mandrel. One way to speed up the cooling process is to blow

Nitrogen through the mandrel to speed up cooling. Be Careful of the Nitrogen coming out

of the mandrel, which is very hot. When the outgoing Nitrogen gets to about room

temperature, mandrel can be pulled out.


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To pull out the mandrel, wear gloves, hold the handle and land the preform vertically on the floor, put

some cushion in between for protection.

Very carefully, tap the preform on the floor but do not break the mandrel. Be cautious; do not smash

the bottom part of the soot preform on the floor. When the mandrel pops up through the handle, pull it

out upwards. Be careful that the mandrel may be still hot.

4.10Materials Usage Totals

User can obtain data of material consumed after each run. To analyze the materials usage for a

particular run, use the main screen and click on the gas usage icon . Refer to software section onhow to use the Gas Usage Screen.

When mandrel is taken out the

soot core preform is ready to besintered. Hang preform onto

core sinter coupler and refer to

sinter process manual forsintering procedure.


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5.0 Core Deposition Software

5.1 Startup

Start the program by double clicking on , labeled Core x.x version.

The program will configure the motors and solenoids then initialize the communications with the scale,

gas panel, HEPA blower, temperature controllers and SiCl4 and GeCl4 vaporizers.

5.2 Function Screens

At the top of the main screen are icons that allow the operator to access the various parts of the

program. Below is an explanation and descriptions of each icon.


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5.2.1 Configuration Screen

It allows the user to set the communication parameters to the temperature controllers and scale, thescaling factors to the motors and the file path of the recipe and data file. This does not need to be

modified unless new hardware is installed.

5.2.2 Configuration Screen

This screen is normally used for troubleshooting and maintenance. It allows the user to control all the

MFCs, valves and relays of the system and verify if they are functioning normally.


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D/A output controls (Blue)

These are digital controls for oxygen, hydrogen, acetylene, SiCl4 and GeCl4 MFCs and HEPA blower.The input range is 0-5 volts for oxygen, hydrogen and GeCl4 MFCs; this range covers the whole

capacity of the MFC itself. HEPA blower has a range of 0-10V and the four SiCl4 vaporizer MFCs are

4.8-12mA.

A/D input indicators (Green)

These are indicators of actual output flows of various MFCs and HEPA. Clicking on other variableslike vaporizer load cell, pressure sensor, etc, will show their current values.

DIO Out (Orange)

The three orange columns are DIOs that turn on relays/solenoids. Buttons labeled with GPV# means

gas panel valve #, these numbers corresponds to the MFC numbers on D/A and A/D columns. AV#and SMR# are valves on the SiCl4 and GeCl4 vaporizer systems. Other buttons turn on certain

devices/functions as labeled; refer to the I/O signal chart for more specifics on the conversions and

explanation. In addition, as a safety feature, the enable bit must be ON for the machine to

function. On the other hand, the neg enable bit will disable the machine if it switched on.

DIO In (Gray)

The last column includes DIO In. If description on the buttons label is true, the button will be turned

on (green).

WarningOpening or closing the wrong vaporizer valves could cause contamination and tank

overfills. Leaving an oxygen or hydrogen line open without lighting it is a serious

explosion hazard.


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5.2.3 Motor Screen

The motor system has three axes, which can be manually controlled by this screen.

Axis 1 Rotational

Motor (upper

left window)Axis 2 Right

End Burner

Motor (upperright window)

Axis 3

Traverse Motor

(lower left

window)

For Axis 1,user is able to

set the velocity

(rpm) andacceleration

(rpm2) for

preformrotation.

Similarity, the

velocity (mm/min), direction, distance (mm) and acceleration (mm/min2) for Axis 2 and Axis 3 canalso be specified. Left and right limits indicators will be on (red) if the corresponding limits are hit.

Start Initiate motionStop Stop the motor

Quit - Return to the main function screen

E-Stop Stop all the motors.

Set Zero Set encoder reading to zero.Home Send right end burner or traverse back to home positions.

The traverse can be set to oscillate through Oscillation Traverse (lower right) window.Enter desired traverse distance (mm) for each pass and set the starting direction from Axis 3, lower left

window. V1 is the speed for initial direction and V2 is the speed for the other direction. Offset and

total offset are extra distances ran by the traverse aimed to reduce ripples on preform surface. Forexample, with L=distance, initial direction set to left, offset = 1 and total offset = 3, the traverse will

move left and right in a pattern described below.


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L+3

L

L-1

L

L-1

L

L-1

L

L+3

The total offset can be any number as long as it can be divided by interlace offset and gives a whole

number. Click on to initiate oscillation.


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5.2.4 Scales and Controllers Screen

This function can be used to read and send set points to the temperature and pressure controllers. The

program can read the weight and tare the scales. Scale E is the sum of Scale A and Scale B. This

screen is useful in verifying that serial communication between the instrument and PC is working

properly. Note that communication enabled buttons (located on the right top corner of the screen) haveto be clicked on for communications.

The blocks on the screen represent temperature and pressure controllers. Each of them shows the

current process value, PV and current set values, SV. PV and SV should read the same as on the

controllers themselves when communication is functioning properly. New set points can be inputted

by entering them in the SP window and then click on .

5.2.5 Image Configuration Screen

This screen is used to calibrate the camera so that the diameter can be obtained. The procedure is

explained in the maintenance section.


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5.2.6 Monitor Screen

This function is used to do a preform run in recipe mode. The screen is as shown below.

There are two types of display objects. One is control and the other is indicator.

The program will read a control and a change in an input parameter will occur. Controls can haveseveral forms such as digital, knob and slide. Digital controls have increment buttons.

The other type of display object is an indicator. An indicator simply displays a process variable andcannot be used to affect a change in input.


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5.2.7 Monitor Mode Controls and Indicators

The following Controls and Indicators are outlined below along with an explanation as to what these particularicons control or indicate.

This icon should be used if the operator wishes to abort a run. The gases to the torch and

end burners will be cut off, the traverse will be sent home and the system will be putback in standby mode. If you choose to abort, you cannot continue where you left off,

you must start over again.

This is an on/off switch which turns on the water pump of the vaporizer. It is not

normally used during operation, it is provided as a redundancy in case the tanktemperature controller fails and there is a temperature runaway in the tank.

Shows the alarm screen that allows the user to silence the alarm, check which parameters

trigger the alarm and to do alarm setup. Refer to alarm screen for details.

Shuts down GeCl4 flows.

Pulls out motor screen. User can enter control parameters through it to override settings

from the recipe being run.

Shows the alarm screen that allows alarm settings. Refer to alarm screen for details.

Pulls out scale and temperature control screen. User can input new set

values/temperatures to the controllers, overwriting what is on the recipe being run.

Indicates the starting time of the run in AM/PM format.

Shows the elapsed time since the start time inHR:MIN:SECformat.

Shows the elapsed time since the torch was moved into position in HR:MIN:SEC format.

Shows the current recipe being executed.

Shows the Preform ID of the preform being deposited.


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The following controls can be used to make changes to various process parameters. It is not necessary to usethese features because the recipe already incorporates desirable settings for these process parameters. Thesecontrols are not normally used during a run, but add a degree of flexibility to the user.

Warning

Using these controls improperly may cause an entire production run to be wasted and severe

damage to the system could occur.

Echoes the final desired weightclad + core) that the operator entered in the beginning of

the recipe. This value may be changed during the run should the operator find thisnecessary. The exit sequence for reaching the final weight is different than the abort exit. If

a change is made, be certain the value you enter is greater than the current weight. Or else,the run will be stop immediately.

Echoes the final desired core weight that the operator entered in the beginning of the recipe.

This value may be changed during the run (core mode) should the operator find this

necessary. This weight determines when to switch from core to clad mode. If a change ismade, be certain the value you enter is greater than the current weight.

The process can be closely monitored by the above indicators. Density, diameter and mass are physical data ofthe preform being deposited. Tank volume and tank pressure are used to monitor any abnormal activities within

the silica tetrachloride tank, like overfilling, low level, etc. The second column tells the what mode is theprocess currently in and also the position of the traverse. The third column shows parameters useful for runmonitoring and troubleshooting.

This is the main readout/control cluster provides the current process information as well as the abilityto manipulate all of the MFCs in the OVD core system. The readouts are grouped by left torch and

right torch.


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The two columns in the middle under ACT shows the actual output flows of the MFCs. The twocolumns to next to them, under SET show the flows set points. These set points come from the

recipe being run and can be overwritten. To do so, click on the square (under columns named OVR)

next to the set point window, overwrite the desired flow on that window and press ENTER. The colorof the window should turn red to indicate that it was modified. Unchecking the square will change the

set point back to the value recipe is calling for.

All flows for the hydrogen, oxygen and acetylene are in liters/min. For SiCl 4 and GeCl4 vapor, the unitsare grams/minute. If a variable is overwritten, the color of the window will turn red to indicate that it

was modified.

Flows and other process variables are also recorded on a chart during the run. This serves as a good

tool in tracing and monitoring any abnormal activities with the process.

5.2.8 Recipe Editor Screen

This screen is used to load and edit recipe. Refer the to the operation section for instructions.


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5.2.9 Manual Torch Screen

This is a very useful screen/function for diagnostics and testing. It can also be used to deposit apreform with manual control instead of recipe control.

All the gas and chemical vapor flows controls are grouped by left and right torches and end burners.They are color-matched with the torch top view diagram on the upper left of the screen.

The GeCl4 SMR Control block allows user to select the desired SMR stage.

Normal mode for the SMR with MFCs being purged with Nitrogen.

When selected, SMR to ready to deliver GeCl4 and there is no flow through

MFCs

Has to be selected for GeCl4 flows. It opens the guarding valves after theMFCs.


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The Vaporizer Control block is used for refilling SiCl4 (manually and automatically) when running innon-recipe mode.

SiCl4 MFCs are normally being purged at all times, this button, when clicked, willswitch off the purge and have the MFCs ready to output SiCl4.

Allows the user to select between auto and manual refilling of vaporizer tank.

For manual refilling only. This button turns on and shuts down SiCl4 filling into thetank.

Turns cooling water circulation on when clicked; used

when tank is overheated.

Turns on tank heater relay. This has to be on when auto

tank temperature control (below) is being used.

Auto vaporizer tank temperature control. SiCl4 flowsnormally require a tank temperature of 770C.

Vaporizer tank volume and pressure indicators formonitoring purpose.

The upper section of this manual torch screen includes functions (green buttons) that are useful for

depositing a preform in a non-recipe mode and are used to set alarms and exit.

Allows user the set oscillation parameters. Upon clicking, a

pop-up screen will be shown:

Starts oscillation using the parameters inputted through the

screen above.


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Moving the torches in/out.

Start and Stop acquiring manual run data.

When clicked, motor screen will pop. Return to manual torchscreen by clicking quit or EXIT on the motor screen.

Show temperature and scale control screen when clicked. To

return to manual torch screen, click on the EXIT.

Reset the pass # counter.

Get a diameter measurement (that will be shown on the diameter

window) whenever this button is clicked.

Take diameter measurement every 10 seconds when turned on

by clicking.

Turns camera light on and off when toggling.

OrShow either run notes or preform picture on the window in the

middle of this screen upon toggling the button.

This button will appear when the window is showing run notes.

Click to save notes entered.

Shut down all flows and valves; reset set values to zero.


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OR

Both buttons will show the following alarm screen when clicked.

Refer the alarm screen section on how to setup the alarm.

Should the alarm go on when using manual torch screen, click

on Alarm Occurrence and the above screen will be shown.This screen allows user to silence the alarm and so informs user

which parameter triggers the alarm, those parameter will then

be in red instead of green.

5.2.10 MFC Sizing Screen

This screen allows user to enter different conversion factor for different MFC capacities. This screen is

reversed for ASI/Silica Machinery.

5.2.11 Information Screen

This is the About ASI software screen, which shows the version of the software.


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5.2.12 Alarm Screen

This screen allows the user the silence any alarm and to set up the alarm system.

Alarms can be set up for deviation in various process variables as labeled on the three columns of

buttons on the screen.

Alarms that are disabled will be shown in gray. When an alarm is set, the corresponding button is ingreen.

In any cases, should the alarm be triggered, user should go to this screen through main, monitor

mode or manual torch screen to silence to alarm. Any deviation that triggers alarm will turn thebutton red. Operator can ignore the alarm for the rest of the run by clicking on that particular red

button; this will change the color from red to white.


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To disable or set up an alarm click on , an alarm setup screen will appear as below:

To set up or disable an alarm, first select the process parameter from , a

pull-down menu will be shown:

Then enter the deviation on and delay time (seconds). If a process variable is above

or below set + value for over a delay time, then the alarm will turn on.

To disable an alarm, choose . After editing the alarm settings, user can choose either

or to return to the main alarm screen.


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5.2.13 Auto Zero Screen

This screen allows user to do an auto-zeroing on the four SiCl4 vaporizer mfcs.

User can either choose cancel or ok. Upon clicking ok, the system will run a zeroing routine. This can

prevent the MFCs from drifting but does not need to be run for every fun, approximately once a weekis recommended.

Note: Every time ASI software is started, this screen will appear on top of the main screen, asking if

auto-zeroing SiCl4 MFCs needs to be done as a reminder.


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5.2.14 Gas Usage Screen

This screen provides data on material used for a particular run. The material usage program is a postrun operation that reads and processes data from file. The benefit of streaming data to disk and

processing it later is an enormous saving in processor and memory load.

In order for the program to recognize the data properly, it must be in the same format as it was

originally written to. If the spreadsheet data is manipulated, then the file should be saved under a

different file name. The usage for the oxygen, hydrogen and acetylene are calculated by data from the

respective MFCs and presented in liters per minute. GeCl4 usage is calculated from MFCs data. Theusage for silicon tetrachloride is calculated from the load cell data as we have found that to be a little

more reliable parameter than the SiCl4 MFCs. Silicon tetrachloride usage is presented in grams/min.

The screen appears as followed:

The actual data recorded for the MFCs and load cell are displayed in spreadsheet form. Each rowrepresents a 10-second interval. Underneath the spreadsheet are the totals for each channel. There are

two indicators showing the combined oxygen and hydrogen usage.

To load a file to analyze, click on the load icon, .

The following dialog will appear.


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Select the file to load and click on

The program will parse the incoming data and fill the rows and columns automatically. The whole

process will take a few seconds.

If the operator wishes to look at the usage immediately after the conclusion of a run, then click on the

icon. By using this step, the program will use the path of the last data file in memory.


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6.0 ASI GeCl4 Vaporizer System

6.1 GeCl4 Vaporizer System Description

The GeCl4 vaporizer is a compact unit which when full contains approximately 1 litre of material. The unit is aself- metering design which uses a valve and float arrangement to allow a constant flow of material equal to the

amount of material which is being vaporised at any one time to replace a liquid being lost to the process.

Figure 1 GcCl4 Vaporizer

The inlet GeCl4 supply is attached to the Manual Valve M1 and must be pressurised so that it is 15 -25 psiabove the operating pressure of the vaporizer. The vaporizer operates at an absolute pressure of about 1100Torr (mmHg), which is approximately equal to 7 psig. The final set point value will depend upon prevailingconditions that will be determined during commissioning. Based on current experience this means that theGeCl4 supply pressure must be between 22 -32 psi.

Failure to do this will mean that the vapour stream will be insufficient to keep up with the flows rates required bythe process and this will lead to a potential loss of end product i.e. core rods.

The vaporizer flow streams are left and right handed as per the torches. The GeCl4 fume stream is mixed withthe make up oxygen before this mixture is merged with the main SiCl4 stream.


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Figure 2 GeCl4 Vaporizer P&ID


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Below is a picture of the GeCl4 Vaporiser Enclosure that is supplied with ASI Core Machines:

Legend:

AV-1 = Automatic Valve (AV) N2 Supply AV-2 = O2 Supply

AV-3 = Drying Gas AV-4 = GeCl4 Vapour

AV-5 = GeCl4 Out LHS AV-6 = MFC Purge Valve

AV-7 = GeCl4 Out RHS AV-8 = Vessel PurgeAV-9 = Purge Supply AV-10 = GeCl4 Supply Valve

AV-11 = Upper Sight Tube Isolation Valve

AV-12 = Lower Sight Tube Isolation Valve

MV-1 = Liquid GeCl4 Isolation valve

R1 = Purge Regulator R2 = Solenoid Regulator


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6.2 GeCl4 Vaporizer System Fume Stream

The Vaporizer fume streams are handed left and right as per the main Torches. The GeCl4 fume streams areinjected into their respective Make-up oxygen flows, which are then merged with their respective SiCl4 streams.

The pressure of each mixture will be monitored during the Preform production process and may be used tocharacterise the combined flow. The combined flow is then burnt in the torch flame as it leaves the fume tube.

GeCl4

Vaporizer

SiCl4

Vaporizer

Make-

up

Torch

P

Figure 4 - Combined Fume Stream


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6.3 GeCl4 Vaporizer System Operation

The general GeCl4 vaporizer unit has three basic modes of operation:

1. Standby (and Shutdown)

2. Process mode3. Purge mode

Here Is the State table for the GeCl4 Vaporizer system:

VaporizerFunctions

AV1 AV2 AV3 AV5AV6(NO)

AV7 AV8 AV9 AV4 AV10 AV11 AV12 MV1

Standby Mode 0 0 0 0 1 0 0 0 0 0 0 0 1

Process M

dual core manual

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