‘I 2, ’1

I I 1 I Aerogel

Commer alization Pilot Project

ARPA Technology Reinvestment Project

Deployment Activity

GENCORP

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DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof. nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or use- fulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any spe- cific commercial product, process, or service by trade name, trademark, manufac- turer, or otherwise does not necessarily constitute or imply its endorsement, recom- mendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof.

DISCLAIMER

Portions of this document may be illegible electronic image products. Images are produced from the best available original document.

FINAL PROGRAM REPORT

ARPA TECHNOLOGY REINVESTMENT PROJECT

DEPLOYMENT ACTIVITY

Aerogel Commercialization Pilot Project:

GenCorp Aerojet

2/13/96

Executive Summary: Aerogels are extremely light weight, high surface area, very insulative materials that offer many potential improvements to commercial products. Aerogels have been the subject of extensive research at Department of Energy Laboratories and have been considered one of the technologies most ready for commercialization. However, commercialization of the technology had been difficult for the National Laboratories since end users were not interested in the high temperature and high pressure chemical processes involved in manufacturing the raw material. Whereas, Aerojet as a supplier of rocket fuels, specialty chemicals and materials had the manufacturing facilities and experience to commercially produce aerogel-type products. Hence the TRP provided a link between the technology source (National Laboratories), the mmfacturing (Aerojet) and the potential end users (other TRP partners). The program successfblly produced approximately 500 tt2 of organic aerogel but failed to make significant quantities of silica aerogel. It is significant that this production represents both the largest volume and biggest pieces of organic aerogel ever produced. Aerogels, available fiom this program, when tested in several prototype commercial products were expected to improve the products performance, but higher than expected projected production costs for large scale manufacture of aerogels has limited continued commercial interest fiom these partners. Aerogels do, however, offer potential as a specialty material for some high value technology and defense products.

TABLE OF CONTENTS

GENCORP AEROJET COMPANY HISTORY ......................................................................................... 5

COMMERCIALIZATION OF AEROGEL MATERIALS ......................................................................... 6

Program Progress .................................................................................................................................. 8

Evaluation and Transfer ofthe Two Aerogel Technologies .................................................................... 8

Silica Aerogels vs . Organic Aerogels: ................................................................................................ 8

Organic Aerogels. ............................................................................................................................ 11 Silica Aerogels: ............................................................................................................................... 21

RF AEROGEL COSTS ........................................................................................................................... 22

TRP PARTNER TESTING AND COOPERATION ................................................................................ 24

TECHNOLOGY OUTREACH PROGRAMS .......................................................................................... 26 APPENDIX 1 .......................................................................................................................................... 28 APPENDIX 2 .......................................................................................................................................... 29 APPENDIX 3 .......................................................................................................................................... 30

APPENDIX 4 .......................................................................................................................................... 31

LIST OF FIGURES

Figure 1 .Low denstiy silica aerogel ........................................................................................................... 4

Figure 2 . Aerojet aerogel pilot plant ........................................................................................................ 13

Figure 3 . Aerogel materials produced by this pro gram ............................................................................. 15 Figure 4 . Aerogel production process schemes ......................................................................................... 18

Figure 5 . Mass production cost estimates for aerogels .............................................................................. 23

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PROJECT OBJECTIVE

Aerogel materials are the lowest density tnmmar enf solids ever made (figure 1). Aerogels can be cold cast from a variety of organic and inorganic starting components

with various densities from 0.05 to >l.Ogm/cc. The thermal insulation characteristics of

the silica aerogel range fkom 3-10 times that of conventional organic foams or mineral

wool’s with a fraction of the weight. Aerogel performs extremely well as an insulation

allowing up to R36 values to be achieved per inch under mild vacuum conditions.

The purpose of this TRP is to create a facility and capability to manufacture si@cant

quantities of large aerogel monolithdpanels. While the initial aerogel processing steps

involve relatively simple sol-gel chemistry (mixing three components), subsequent

processing (casting, de-molding, solvent exchange and supercritical drying) is both labor

intensive and highly sensitive to even minor processing changes when conducted at a

commercial scale. Since aerogels have never been produced in a commercial environment,

a major challenge of the program will be to convert laboratory methods conducted by

Ph.D. scientists to a process well-defined enough to be conducted by chemical plant

operators. The program has three technical thrusts: 1) initial process process definition,

scale-up and production of large aerogel monoliths, 2) chemical modifications and processing changes to reduce aerogel production costs and 3) aerogel material supply to

specific end-users for applications testing. End-user prototype testing will be important in

establishing the commercial viability of aerogel production. Members of the TRP Aerogel

Commercialization Pilot Project are: GenCorp Aerojet (lead), General Motors

Corporation, Benteler Industries, Maytag Refiigeration Products, Boeing Commercial

Aircraft, Giacier Bay, Inc., Lawrence Livermore National Laboratory, Lawrence Berkeley

National Laboratory, California Manufacturing Technology Center, Michigan Energy

Research and Resource Agency, and the Federal Aviation Administration.

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Figure 1.

“Low” density open cell silica aerogel at approximately 0.08gdcc. The amber reflection of light is fiom the Raleigh scattering of light by the largest pores (>0.5pm) of the aerogel.

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This TRP also tested the technology transfer process fiom National Laboratories to industry. The intent of this program was not to establish a commercial research program

on the properties of aerogels but to leverage prior Government investment at the National

Laboratories to rapid commercial application. It was also a stated purpose of the TRP

program to assist companies in the process of defense conversion, for the economic

growth of the nation.

GENCORP AEROJET COMPANY HISTORY

Aerojet is the defense/aerospace segment of GenCorp, a Fortune 500 company that trades

on the New York Stock Exchange with the symbol GY. In addition to Aerojet's defense

business, GenCorp has major positions in automotive and polymer products. For this

program the automotive and polymer product divisions of GenCorp were considered to be

ideal potential distribution networks for aerogels. For example, GenCorp currently

supplies reinforced body panels to the automotive industry (including GM) and door seal

gaskets to refrigerator manufacturers, both potential users of aerogel as acoustic and

thermal insulation. This fit for aerogel materials within GenCorp's commercial products

provided broad based internal support for this defense conversion activity at Aerojet.

Aerojet maintains operations in seven states with major facilities in Sacramento, CA

(Propulsion), Azusa, CA (Electronics) and Jonesborough, TN (Ordinance). Major Aerojet

Propulsion products include: Titan ld and 2& stage engines, Delta 2"6 stage engines,

Minuteman 2" stage motors, Hawk motors, the Space Shuttle Orbital Maneuvering

Engine, solid, liquid and gelled rocket propellants and specialty chemical and bulk

pharmaceutical synthesis. Major Aerojet Electronics products include: Infrared (IR) and

Millimeter wave sensors for the Defense Support Program (DSP), Defense

Meteorological Satellite Program (DMSP) and boost phase satellite systems, and Sense

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I ’ ‘ and Destroy Armor (SADARMJ smart munitions. Ordinance products are concentrated in

depleted uranium heavy armor penetrating projectiles in numerous sizes. Recent

Department of Defense @OD) spending cut backs along with the cancellation of

Peacekeeper, Small ICBM and the Space Shuttle Advance Solid Rocket Motor have

caused significant force reductions at Aerojet. However, these same reductions have also

fieed large amounts of pre-existing manufacturing space and facilities for new ventures,

such as the aerogel project. In particular, the defense draw down and lost programs at the

Aerojet Sacramento plant idled 100,000 sq. ft. of chemical manufacturing plants and

caused massive employee lay-offs (SO% to date). In the Winter of ‘92, Aerojet

undertook an aggressive defense conversion activity to evaluate company strengths as they

relate to commercial products. Chemical productdadvanced material manufacturing,

thermal control systems, structural composites, and sensors were considered the areas

with the most commercialization potential for Aerojet. As of this report, only the

chemical products area has been commercially successll and profitable. -

COMlMERCIALIZATION OF AEROGEL MATERIALS

The commercialization of aerogels has been slow do in part to the “chicken and the egg”

syndrome. The National Laboratories have had a great deal of interest fiom companies

interested in using aerogel in a wide variety of products. However, upon learning of the

complex nature of the manufacturing process none of these “user” companies was interested in making aerogel. At the same time, companies in the business of

manufacturing bulk commodities are not in the business of introducing new materials into

an unproved market/application. This TRP program was designed to address four major

issues which inhibited the commercialization of Aerogel and these are:

Production of Material Has Been Size Limited

Production of Material Has Been Quantity Limited

1.

2.

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3.

4.

Material Standing Alone is Not Robust

Cost of Material (Due to Limited Production)

Fundamentally, commercialization progress has been slow since laboratory production of aerogels has not been able to provide materials for prototype applicationdproducts. In

particular the largest aerogel samples typically seen have been limited to a few inches in

diameter and even the quantity of these samples is extremely limited. Obviously,

industries wishing to make prototype products need sufficient quantities of aerogel for

testing. This program has been able to supply over 300 ft2 of RF aerogel to partners for

prototype application tests. However, as noted later in the RF aerogel discussion the

propagation of cracks, bubbling and warping caused significant reduction in anticipated

yields. Such yield problems are not typically seen in the production of small laboratory

aerogel samples and can only be assessed in a pilot plant operation such as those

conducted in this TRP.

In some cases, potential applications require much more material strength than is provided

by aerogel. With aerogel provided by this program, team members will have the

opportunity (and material) to test approaches such as: - Wrapped or Laminated

- Reinforced

- Powdered

For aerogels to be commercially accepted, they must have the extremely fiagile stigma

erased by a robust packaging method($. Any packaging methods for aerogels must be

both inexpensive and flexible enough to accommodate a variety of shapes and products.

The cost of aerogel has also been extremely high (thousands of dollars a sq. fi.) and this

has precluded serious commercial consideration. Furthermore lab scale “production data”

is inadequate to predict commercial production costs or just@ major capital investment. A

major portion of this project is to determine the cost drivers associated with the

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production of aerogels based on industrial pilot scale plant operations data. Aerogel costs

will ultimately determine marketplace use and acceptance.

Program Progress

The scale up of aerogel manufacturing from small laboratory operations to a pilot scale

industrial facility was a complex test of technology transfer fiom the National Laboratory

system to industry. Initially, both industry and the Laboratories considered their own knowledge and expertise to be superior for the design of the pilot scale facility. Early on Aerojet and the Laboratories tended to work very independently with only minimal

technology transfer being conducted. As the program proceeded the Laboratories and

Aerojet came to understand that both groups had very different skills to contribute.

In March 94, Aerojet took the lead and began design of a facility using an abandoned

pressure chamber fiom rocket testing. However, by May 94 this effort was halted when

costs to OSHA certifj, the pressure vessel using X-ray tomography were expected to

exceed $25K and take at least three months without any certainty of certification.

Previously, LLNL had acquired a 22” x 72” CO, autoclave fiom the failed Thermalux

Company that had unsuccesshlly tried to market silica aerogels. However, LLNL did not

have finding to set up this autoclave and it was leased to Aerojet to conduct this project

in June 94.

Evaluation and Transfer of the Two Aerogel Technologies

Silica Aeropels vs. Organic AeroEels: Part of the commercialization of aerogels is the evaluation of the different aerogels

compositions for both their ease of manufacturing and end product performance. The

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TRP program would manufacture and evaluate both organic and silica aerogels with

LLNL and LBNL as lead laboratories respectively. Silica aerogels can be produced using

either the high temperature methanol or C02 supercritical extraction methods. Organic

aerogels can only be produced using the COz extraction process. Table 1 illustrates the

differences in process steps required for C02 supercritical extraction vs.methano1

processing.

Table 1. Process steps for methanol and COz extractioddrying of aerogels.

1 Mixing Mixing

2

6

7

8

Casting and cure (approx. 300 K oven

cure for organic aerogel only)

De-molding

Load into solvent exchange tubs

Ambient temperature diffusion exchange

Load into autoclave

Supercritical extraction

(@ >304O K; >7.3Mpa)

Remove and package

Cast and cure

De-molding

Load into autoclave

Supercritical extraction

(@ >553 K; >lOMpa)

Remove and package

n/a

n/a

In general, even with the additional processing steps, the lower temperatures, lower

pressures and non-toxic fluids associated with the C02 process make it more commercially

desirable than the methanol process. The extra processing time required for the C02

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process “solvent exchange” is offset commercially by having multiple batches in process so

that the autoclave always contains material being extracted.

Initially, it was planned that the first pilot plant run would be conducted with silica

aerogels. A small high temperature autoclave (1 liter volume) was set up at Aerojet and

successfilly produced silica aerogels using the “methanol process” transferred from

LLNL. However, the large autoclave for the pilot plant could not reach the temperature

and pressures required for methanol process. LLNL loaned Aerojet a small “Polaron”

(500ml volume) autoclave that could be used for lower temperature COz processing of

silica and organic aerogels. LBNL and LLNL then started the technology transfer of C02

processing of silica and organic aerogels.

With the end of the Aerojet fiscal year looming near, the decision was made to switch the

initial pilot plant run to the production of organic resorcinol formaldehyde (RF) aerogels

to allow 1994 finding to support a plant run.

The programmatic switch fiom C02 silica aerogels to RF aerogels was primarily based on

the greater probability for an initial success with RF aerogels. Discussions between

Aerojet and the Laboratories indicated that organic aerogels were a more robust material,

compared to silica aerogels. Additional licensing issues associated with silica aerogels

hrther suggested that a delay in a silica aerogel pilot plant run would be appropriate.

Some of the LBNL staff were involved in the dehnct Thermalux Company and still have

an interest in selling license rights and associated intellectual property. Prior to winning the

TRP award, Aerojet believed that DOE held patent rights to the silica aerogel C02 as the

work had been conducted at LBNL. Apparently, when the patent was tiled, DOE saw no

si@cant commercial application for the technology and released rights to the LBNL

authors. In both CRADAs and TRP-type technology transfer activities third party patent

rights created delays, conflicts of interest and added cost. License discussions with LLNL

Technical Transfer Office were painful, costly and extremely time consuming.

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Orpanic Aerwels:

Laboratory methods for making organic aerogels were successhlly transferred fiom

Lawrence Livermore National Laboratory to Aerojet. Aerojet then scaled-up the process

and constructed a pilot manufacturing plant shown in figure 2.

Aerojet started production of organic Resorcinol Formaldehyde aerogel monoliths in the

new pilot scale production plant in early November ‘94. This plant produced the largest

pieces of organic resorcinol formaldehyde (RF) aerogel ever made. Additionally, this was

the first time organic aerogels have been produced commercially. During the operation of

this pilot facility Aerojet collected detailed data on process conditions in the supercritical

reactor (figure 3). In all, twelve autoclave runs were completed with yields varying fiom

nearly zero to 100%. The results of each RF batch are given in Table 2.

A simplified process flow is given in figure 4, with the generalized conditions for aerogel

manufacturing. A more detailed process flow diagram of the aerogel pilot plant is given in

Appendix 1. Initial difliculties encountered with the panels sticking to the molds. Various

release agents were tested including silicon grease, “Pam,’ , Vaseline, cooking oil, etc.

with limited success. It was determined that using aluminum foil liners provided the best

solution to the sticking problem. Delicate handling of the cast RF gels was required in

transferring the panels fiom the casting tray to the drying rack. The panel transfer

operation had to be completed while submerged in acetone, to prevent premature drying

(non-supercritical) of the aerogel panels. After the solvent exchange, batches of 60

panels, approximately 12” x12” x 5/8” each were moved to the autoclave for

extractioddrying of the acetone with supercritical COZ.

It should be noted that each successive batch did not necessarily provide improved results.

Warping and cracking of the organic aerogel panels occurred sporadically throughout the

manufacturing cycle. If additional budget had been available numerous sensors to

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monitor temperature and fluid flow variations could have been installed within the

autoclave. However, these sensors had not been planned at the time of the proposal due

to Aerojet's belief that the technology was mature..

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Figure 2. Aerogel pilot production plant at Aerojet, Sacramento California for the TRP. Autoclave in center (above the drum) is used for supercritical COZ extractioddrying of aerogel monoliths. Approximately sixty board feet of aerogel can be made in each batch.

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Figure 2 (cont.) Top left: Computerized control console for the aerogels pilot plant; Top right: oven for curing RF aerogels, in operation, the yellow duct provides environmentdsafkty ventilation; Middle: tanks for solvent exchange for wet gels, including circulation and safkty systems; Bottom: open pressure vessel prior to loading

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Figure 3. One of the RF aerogels monolith produced at Aerojet as part of the TRP. These RF aerogel monoliths are the largest ever produced. The wire is a thermal couple lead used to gather process data &om within an aerogel sample during the supercritical COZ step. (Note: the thermal couple is not used in production aerogel samples.) D

Figure 3 (cont.) Top: Failed RF aerogel panel (warped and cracked); Middle: interior section of a Med RF aerogel panel, with opaque band through the center due to insufEicient removal of water prior to supercritical drying. Bottom: failed silica aerogel panel fiom first batch.

1 1 I 1 I I I 1 I

Table 2. Production results of the aerogel pilot plant on RF compositions.

1 R-200

12/20 Panels on bottom rack were I unsuccessful due to uneven Additional heating coils were added to autoclave to I heating during supercritical I better distribute heat.

phase of process 2 50/60 Various release agentdfoils

R-150 evaluated

3 20/60 40 tiles warped and R-200 cracked, potentially due to

non-uniform CO2 flow through vessel

4 2/60 Most panels were opaque. R- 100 Suspect insufficient water

removal prior to drying.

5 R-150

54/60 90% good panels, but many 1-3mm bubbles on bottom surface. Some contamin- ation from unknown yellow dust.

Aluminum foil was found to release best. Most panels were acceptable. All fittings rechecked and cleaned.

Water analyses to be performed on all sub- sequent batches prior to drying All reactors and solvent storage tanks cleaned and rechecked for contamination.

6 R-150

57/60 A few broken tiles, but mostly successfbl. Some 1” thick panels included, which appeared cloudy (incomplete solvent ex- change).

A subsequent panels were cast no thicker than 0.75”.

R- 7 1 150 57/60 Slight bubbling and a few none. I broken, but a good run I

R-150 8 1 3 9/60 17 in lower section of 1 Recommend installing I autoclave had small opaque additional flow/pressure/ - -

regions in corners. Remainder were excellent available.

temp. sensors iffbnding

9 59/60 A nearly perfect run none

10 2/60 Most were broken or Cause unclear without R-150 cracked additional internal sensors

11 -5 8/60 All panels slightly opaque Assumed water present R-150 before drying.

12 59/60 A nearly perfect run none

R-150

R-120

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Product l3 - Aerogel T T ) (TJ

Basic Process Steps for RF Aerogels

Pre-mix/Mix e Resorcinol, formaldehyde, catalyst, water

Cast & Cure . Cast into molds at room temperature . Cure for 24 hours at 8OoC

Solvent Wash Exchange acetone for reaction water 24 hour diffusion controlled

. C02 extraction & Supercritical Drying

C02 extraction of acetone three times then supercritical drying C02 at 1200 psi, 5OoC

Figure 4. Basic processing steps for the production of RF aerogel. Some process steps are dfision controlled and, therefore, strongly time-dependent on sample thickness. (cont.)

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Evaporati

Sol

Pressure

Temperature

Figure 4. (cont.) Schematic of the supercritical extraction process used in making aerogels. Failed supercritical extraction produces a xerogel, which is a closed-cell porous

material with a much higher density than aerogels.

M e r completion of the fist batch it was determined that the bottom of the autoclave was

not reaching supercritical conditions due to a shortage of heating coils. Several days were

required to add the additional heating coils and re-insulate the autoclave. Subsequent to

the installaton of the additional heating coils, aerogels were successfidly produced

throughout the entire volume of the autoclave. As noted in table 1 above, RF aerogel

panels did not always come out as expected, cracking and bubbling were common problems that could not necessarily be correlated to any particular cause. Without data

fiom internal real-time sensors, it is impossible to determine what really went wrong with

particular batches. It is speculated, however, that tiles may occasionally float within their

holding racks and, in some cases, disrupt solvent circulation.

Also problematic was the commercial necessity to process aerogel batches in parallel and

thereby reduce labor down time and maximize autoclave usage. Running aerogel batches

in parallel is also commercially sensible since the plant must be manned by at least two

workers, 24 hours a day because of the high pressure operations (OSWunion

requirement). Figure 5 illustrates a typical run sequence for the aerogel pilot plant. It

should be noted that even when a problem is found, two other batches are already in

process and may have already been damaged. We attempted to duplicate normal

commercial operating conditions as closely as possible to obtain realistic data for

projecting mass production costs and to maximize the amount of material which could be

produced given available TRP funding.

5 complete autoclave run solvent exch. demold

6 complete autoclave run solvent exch.

7 complete autoclave run

8 complete

9

Figure 5 . Parallel sequence of processing aerogel batches. Note that it takes four full days

for the pilot plant to reach full capacity. Also notice that batches 2 and 3 are already in

progress before the results of batch 1 are known.

The program then supplied vacuum-packaged (0.1 atm) RF aerogel to the end-user

members of the TRP (General Motors Corporation, Benteler Industries, Maytag

Refigeration Products, Boeing Commercial Aircraft, Glacier Bay, Inc.). Applications and

results of these prototype applications are discussed under “Commercialization” and in

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individual appendices. Companies were requested to provide stand-alone sections on

results so as not to compromise any proprietary information regarding applications.

Samples of the RF aerogel monoliths of three different densities prepared in this project

were delivered to LBNL for thermal conductivity testing. These tests showed that the

Aerojet-prepared materials pedormed as expected in their insulating ability. R- values of nearly R-13hch were measured at ambient pressure. At modest vacuum, the materials

showed values of up to R-27/inch. This is in accordance with theoretical predictions and

previous laboratory measurements on similar density materials. This also demonstrates

that the supercritical extraction procedures were performed correctly and the materials

were truly aerogels.

Silica Aerosrels:

Aerojet then transitioned to making silica aerogels in early ‘95. This effort was less

successhl than the production of RF aerogel. The high costs unexpectedly encountered in

the early stages of the program (that were due inpart to the expensive installation costs

associated with what was thought to be a “turnkey” sysytem), left fbnding for only one

attempt to produce large silica aerogel monoliths. Five batches of gels were prepared

concurrently over a ten day period. One of the major costs associated with the large scale

production of aerogels results from the labor involved in pouring gels into molds, and

subsequently removing the set gels from the molds for aging and drying. Aerojet spent

considerable effort on improving these procedures during the RF aerogel runs and, in

consultation with LBNL, developed a similar system that worked well for silica gels. To

keep cost down, Aerojet planned an aging/demolding schedule for these gels that was

similar to that used successfblly for RF aerogels. LBNL could not assure Aerojet that this

schedule would be adequate, as a similar molding system had not been tried at the

Laboratories. In practice, this schedule lead to an inadequate curing of the gels. This was

apparent only when the gels were removed from the supercritical extractor. The gels were

mostly opaque, with significant shrinkage and cracking. These effects point to an unsuccessfbl curing process and a generally weak gel. The curing process for RF aerogels

relies on thermal effects, while the process for silica aerogels is chemical. Therefore, while

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it is acceptable to leave the RF gels in their molds while curing, this causes an uneven cure

in silica aerogels. When this was observed in the first batch of gels, attempts were made

to correct the problem in the remaining batches by adjusting the curing procedures in

terms of time and pH for the remaining batches. Specifically, the pH of the solution used

to cover the gel was increased. This improved the gels slightly, but again, the effects were

non-uniform. The outer surface of the gel that was exposed to the aging solution was

strengthened, while the inner surface (still against the mold) was not. Therefore, the inner

surface showed an increased shrinkage that warped and cracked the gel.

Aerojet and LBNL agreed that this failure could be avoided in future runs by slightly

modifLing the process schedule. Specifically, removal of the gels fkom the molds prior to aging. This could lead to more broken gels during demolding, but would result in an overall yield that is much higher. However, as the attempt to prepare silica aerogels

occurred at the end of the project and funding had been exhausted, another attempt to

prepare silica aerogel drawing on this experience could not be made.

RF AEROGEL COSTS After completing the successfbl RF aerogel pilot run Aerojet undertook a “scale-uphhould

cost” study. Results of this study indicated much higher costs for RF aerogels than had

been reported in two previous LLNL studies. The major difference between the cost

estimates for large scale RF aerogel production was the exclusion of waste disposal cost

fiom the LLNL estimates. Figure 5 illustrates the relative contributions of a variety of

cost elements to the productions costs as estimated by LLNL and Aerojet. The cost of

labor was another serious difference between Aerojet and LLNL cost estimates for

commercial aerogel production. While details of Aerojet’s estimates remain confidential to

the company, some general discussion will be useful. The LLNL cost estimate for labor

was probably low for two reasons. First the skill level and pay rate of commercial chemical

plant operators is not much less than that of a Ph.D. scientist. These chemical plant

operators work in a demanding environment, where there is little room for error.

Secondly, OSHA requires plants conducting hazardous operation be staffed 24 hours a

day, with at least two workers for safety reasons. This 24 hour staf€ing requires swing and

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weekend st&g which requires additional compensation (union rate is at least time and a

w-

LLNL AIEROJEF

Materials, Solvents Waste Disposal

Energy I Labor CI Capitol Emense

Figure 5. Pie charts comparing the cost components for RF aerogel production at large scale (> 188,008 Board Feet/yr.),

Neither capital nor waste disposal costs were included in the LLNL aerogel cost estimates.

Capital costs are significant for chemical plants conducting hazardous high-pressure

operations. It is also noteworthy that with additional capital expense, labor can be reduced

to some extent. Aerojet’s cost model assumed a moderate degree of automation within the

aerogel plant. A higher level of automation would only reduce labor by 10-15%, relative

to completely manual operations, yet increase start-up costs by up to 58%. Excess costs

during new operations start-ups are generally kept to a minimum by industry, with

additional automation added as the plant becomes profitable. Industrial waste disposal

costs are always higher than expected. For organic aerogels, the hazardous wastes

produces are: formaldehyde-contaminated acetone. Potentially formaldehyde-

contamhated solids fiom mold cleaning, and activated carbon fiom vapor stripping

systems. Other factors not included in either the LLNL or Aerojet cost estimates are

breakage and batch loses. These would probably increase costs an additional 10-15%.

The Aerojet projected cost for the production of RF aerogel is approximately $13 per

board foot (12” x 12” x 1”) or about 10 times the value projected by LLNL (Calson et al.

3: Non Cyst. SoZih, 186 1995). Even making very optimistic estimates of half the

current labor rate for Aerojet the RF cost is still over $9 a board foot. This high cost

directly effects the commercial acceptance of the RF aerogel material as will be discussed

later.

Program costs for this project can be found in Appendix 2.

TRP PARTNER TESTING AND COOPERATION

The coordination with the TRP partner end users was very difficult to manage for several

reasons. Many of the partner companies had never worked on a government contract

before and were very frustrated with the 8 month lag time between contract award and

implementation. This was not entirely due to the TRP program itself, but the DOE CRADA arrangement with LLNL and LBNL managed by the University of California

(UC). Normal Federal Government indemnification language was not used in the UC

CRADAdlicences which caused both lengthy negotiations and delays. Additionally,

ARPA assigned management of this new TRP program to DOE, so many new protocols

had to be established, firther slowing the start of the program.

These long delays affected the internal finding and interest of the TRP end-user partners.

In industry, as in government, fiscal year finding schedules and actual project schedules

do not always coincide. Shifting IR&D finds committed one year to another is not a

simple matter. When the program was delayed and material production was behind

schedule, the partners needed to shift finding to other programs. Boeing, for example

dropped their galley cart development project completely. Another problem encountered

with the management of the TRP end users was that their aerogel development work was

proprietary. Both Boeing and General Motors were particularly sensitive to this aspect of

24

the agreement. In order to provide for this product/use sensitivity, Aerojet twice requested

(August and December 1995) stand-alone appendices be provided by the end-users for

inclusion in this report. Information provided by the companies is given in Appendix 3. In order to protect proprietary information no attempt will be made by Aerojet to describe in

detail any development activity by the TRP end-user partners. The general results of end

user testing are given below.

Aerogel commercial prototypes being evaluated by TRP partners.

I Automotive Exhaust System I I ThermaVAcoustic Insulation Acoustic TBD

G WCadllac RF Panels Thermal Acoustic Insulation Products TBD Testing in Progress Maytag RF Panels 2 Refrigerators in Construction (July 1995)

Glacier Bay RF Panels 2 Marine Refrigerators in Construction (July 1995) Boeing RF Panels ThermaVAcoustic

G WCadllac RF Panels Thermal Acoustic Insulation Products TBD Maytag RF Panels 2 Refrigerators in Construction

Glacier Bay RF Panels 2 Marine Refrigerators in Construction Boeing RF Panels ThermaVAcoustic

Acoustic TBD

Boeing: Boeing was originally interested in using aerogels in a newly designed galley cart

for commercial aircraft. The advantage of an aerogel insulated cart would be that hot

food could be loaded onto the aircraft and served directly to passengers. However, early

in the program it was determined by Boeing that the entire infrastructure of aircraft galley

carts would need to be changed at a very high cost and the concept was dropped. Boeing

then considered the aerogel material as a possible fuselage insulation material however, the

aerogel material was considered both too heavy and too costly compared to current

fiberglass insulation as shown below:

Current fiberglass Aerogel @ O.OSgm/cc

1.50 lb/ft3 high noise areas 6.2 wfi3

0.42 lb/ft3 all other areas

Even with aerogel’s 5 fold increase in insulating value, it would still be significantly

heavier than fiberglass. Also since most insulation is used in the fixed space between

fbselage spars, there would be no space savings. A further discussion on aerogel can be

found in Appendix 4 (supplied by this TRP partner).

25

Benteler: The application for this partner was exhaust systems and was considered very

competition-sensitive. A further discussion on aerogel can be found in the Appendix 4

(supplied by this TRP partner).

GWCadillac never disclosed there intended use for aerogel but sound and thermal

protection were of the greatest interest. A fbrther discussion on aerogel can be found in

the Appendix 4 (supplied by this TRP partner).

Maytag constructed two test refiigerators out of the RF aerogel supplied and reports

results in Appendix 4.

Glacier Bay was to construct a marine refigerator out of the material supplied. During

this program Glacier Bay also tested a high vacuum powder supplied by another company

at a lower cost. A further discussion on aerogel can be found in the Appendix 4 (supplied

by this TRP partner).

TECHNOLOGY OUTREACH PROGRAMS

This program included two technology outreach symposia. The first of these was held on

June 28, 1995 in Ann Arbor, Michigan. This symposium was sponsored by MERRA and

consisted of technical and commercial presentations from Aerojet, LBNL, and LLNL. About fifty industrial and academic researchers attended the presentations and the

subsequent break-out sessions. Interest in aerogel technology seemed high, with at least

one potential collaboration (LBNL and T/J Technologies) resulting from this event.

The second outreach program was held on September 11, 1995 in Long Beach, CA and

was sponsored by the California Manufacturing Technology Center (CMTC). Again, this

symposium consisted of technical and commercial presentations from Aerojet, LBNL, and

LLNL and subsequent break-out sessions. Unfortunately, although CMTC had sent out

approximately 10,000 fliers promoting this event, the turnout for this symposium was

disappointing. Approximately, twelve researchers attended this symposium. Interest in

aerogels among those in attendance did not seem high. It was assumed that the low

26

attendance of the California symposium reflected the geographic differences in the

industrial base of southern California relative to Michigan (where many local industries

have potential applications for aerogels).

27

I

I

I I

I I 1 I I I

APPENDIX 1

Process Flow Diagram for RF-Aerogels

28

WATER WET CURED GEL -----

P-9 c

AEROGEL PROCESS FLOW DIAGRAM

1 0 0 V-14 A & B nun P-14 A & B

) A.B,C FRESH OR Q RECYCLABLE SOLVENT

I

RECYCLABLE SOLVENT

AEROGELS PILOT PLANT

SOLVENT EXTRACTION

= = - -I=

AEROGEL PROCESS FLOW DIAGRAM

R - 3 8 9 SOL n i x REACTOR se GRL, G/L

u- I2 u- 1 GEL RACK ASSEMBLY RACK L I F T CRANE CS RACK, COVER l00e L B S C a i n )

6-306 ~ - 3 8 9

i se SCFM. 1 HP 19 r i 2 , CLRSS VENT BLOUER SOLVENT CONOENSER

V - 3 0 2 CONOENSATE R E C E I V E R i e e GAL, WL

7-2 C 0 2 STG TANK ~ e e e GAL. (RENTAL )

1 VENT TO R-216 I 21 i 1

I 1 r r i - l I N

SOLVENT

01 URTER 3y CN I -

I I I I I I I I

i I ! I I ! I I ! I I ! 1 I ! I I ! I

( R E N T A L PACKAGE0 SYSTEM)

________________________________ I I

I REFER. I

I

I I I I

S Y S

P - 2 HP TBO

+ BRS

JI sc

SOLVENT TO R - 2 1 6 i e SB

c uc I I

REROCEL P I L O T P L A N T

AEROGEL PROCESS FLOW DIAGRAM

R-216 E-216 V - 9 VENT CONDENSER S . C . E X T R R C T O R / D R Y E R

see GAL. 3 0 ~ s I00 (12 . 316SS

C 0 2 E X T R A C T l O N L

P-216 ie CPM se'

I !

I % I I ! I I ! I

W

I , r @ CRUDE AEROGEL ! 1 r BAR

N2 I I !

!

i !

-9 ; ! ! ! ! ! !

I

I

I

- S U P E R C R I T I C A L D R Y I N G

PFS2-GEL.DCZ -

AEROGEL PROCESS FLOW DIAGRAM

R - 2 3 8 SPENT SOLVENT HOLD TRNK

i UCR

!PENT SOLVENT ./ R - 2 1 6

f---i R - 2 3 E

SCR-310 VENT SCRUBBER SYSTEM

I l l I l l - 1 H P-310

REROCEL '-PRODUCT

-e PFS3.0422 I . . _ _ _ _ _ I

APPENDIX 2

Program Costs

Initial Cost FY 94

Commitments (actual) Partner Sharing Espenditures

U.S. DOE $1,025,000

Propulsion 294,800 408,691

Benteler 23 3.500 n.a.

Aerojet

Systems Plant

GWCadillac 330,000 n.a. Boeing 56,000 n.a. Maytag 24,715 n. a.

Glacier Bay 50,000 n. a. M E m 27,843 n. a. CMTC 25,000 n.a.

FY 95

(actual) Expenditures Expenditures Total

$1,025,000

2 13,367 622,05 8*

3 1,700

n.a. 10,341 n.a. not reDorted

Total = $1,69 1,549

* Sufficient to meet matching requirement for DOE outlays to Aerojet ($545,000).

29

APPENDIX 3

Aerogel Material delivered to Industrial Partners

Aerogel samples shipped to partners for testing

Boeing :

Glacier Bay

General Motors

Admiral (Maytag)

Benteler

M E m

cmc LLNL

LBNL

Total

30 resorcinol-formaldehyde aerogel monoliths

40 resorcinol-formaldehyde aerogel monoliths

60 resorcinol-formaldehyde aerogel monoliths

120 resorcinol-formaldehyde aerogel monoliths

6 liters of silica aerogel and carbon aerogel powders

10 resorcinol-formaldehyde aerogel monoliths

10 resorcinol-formaldehyde aerogel monoliths

10 resorcinol-formaldehyde aerogel monoliths

assorted silica aerogel and carbon aerogel powc,zrs an^, resorcinol-

formaldehyde aerogel monoliths

280 panels shipped to partners for testing

30

APPENDM 4

Industrial TRP Partner Reports

Note: On August 16,1995, Aerojet requested a no cost extension for the Aerogel Commercialization Pilot Program (see attached letter, next page) to complete the final program tasks and coordinate the final program close-out. Shortly thereafter, Aerojet requested that the end-user partners provide summaries of their development activities and program costs. This was done to allow the partners to protect their intellectual property. The same request was made in writing on December 16, 1995 (see sample letter {Boeing) following page). Mormation received from the partners by 2/7/96 is included here.

31

GENCORP

16 August, 1995

P 0 Box 13222 Sacramento CA 9581 3-6000

Joanne M h o U. S . Department of Energy Idaho Field Office 785 DOE Place IdahoFalls, ID 83402

Dear Joanne,

On behalf of the Aerogel Commercialization Pilot Project TRP, I request a no cost program extension through the end of December 1995. As you are aware we encountered unexpected problems associated with the production of silica aerogel and end user testing has been delayed significantly. The program will also use this additional time to more hl ly complete the technology outreach task.

Please contact me if there are any problems or questions associated with this request for extension. I will assume that since there is no request for additional funds, this extension should be granted quickly. The contract offices at both LLNL and LBL have requested notification of this extension ASAP, so that funding can be carried over into FY 96.

Sincerely, / I

Dr. Wayne N. Sawka Aerogel TRP Program Manager

Dr. Michael Ayers Aerojet Corp. P.O. Box 13222 Sacramento, CA 9 16-3 55-5763 916-355-4936(fa~)

12/ 12/95 H. H. PfeSer Boeing Comercial Airplane Group P.O. Box 3707 Seattle, WA 98 124-2207

Dear Sir:

Aerojet is currently preparing the final program report for the ARPA-TRP Aerogel Commercialization Pilot Program, in which your company participated. The program close-out procedures require that your company submit a brief description of the development activities performed by your company, the results of these activities, and an accounting of the matching h d s provided to this project. We believe that having you supply this information will avoid any inadvertant disclosure of your company’s proprietary information by Aerojet.

If your company feels that it can not comply with these requirements, Aerojet will note this in its report to DOE.

The final report to DOE is due at the end of January, therefore, we would appreciate your assistance with this matter at your earliest convenience.

Sincerely,

Michael Ayers Project Manager-Aerogels

32

I I

e e

..

1

1

Maytag Corp. Results summarized on next page

33

MAYTAG REFRIGERATOFU FREEZER EVALUATION OF AEROGEL INSULATION

Report by G. Jeffrey Haworth and Dr. R Shrikanth

ABSTRACT

Special aerogel insulation panels approximately 11.375" x 10.5" x .7" were obtained from Aerojet - General as part of an ARPA -TRP Commercialization Pilot Program. These samples were subsequently packaged in plastic and evacuated for use as vacuum insulation for refrigerator / freezers. The vacuum panels were placed on the outer side walls of the refrigerator / freezers and further insulated with an HCFC- 14 1 B blown polyurethane foam. Energy usage was measured and compared to units only foam insulated. A total DOE energy improvement of 9.54 % was obtained with 5 1 % coverage of the exterior walls. This is similar to earlier test results with Thermalux aerogels and Degussa powder vacuum panels on the same cabinet with CFC-11 blown foam. An R-factor of around 20 per inch was measured and is in agreement with the energy usage improvement level observed.

BACKGROUND

During the past several years the household refrigerator / freezer manufacturers have been increasingly pressed by EPA, DOE and others to eliminate CFC's and reduce energy consumption to conserve energy resources and reduce global warming. The DOE energy usage standards for 1990 represented an average reduction of 25% and in 1993 a further average reduction of 30% was required. These energy reductions were obtained by manufacturers as result of a combination of several small changes such as component efficiencies, improved gasket sealing designs, improved foam insulations (low k-factor) and small changes in insulation wall thicknesses where they would not affect the marketability of the product. CFC- 1 1 blown polyurethane foams that were used typically provided insulation k-factors on the order of. 1 15 to .125 (BTU x Inch / Hour x Sq.Ft. x Deg.F). These foams have largely been replaced since 1994 by HCFC- 14 1 B (largest percentage), HCFC-22, HCFC-142B and blends of all three with typical k-factors from .125 to .137. Additional improved eficiencies in other components were frequently required to maintain the 1993 DOE standards level of performance.

By law the DOE could have proposed new standards for 1998 (5 years fiom the last standard) but they also needed to publish the final ruling three years ahead of the implementation date. Although a working group that included appliance manufacturers, environmental interests, large power generating companies and state energy agencies made a landmark joint proposal based on LBL calculations in September of 1994, the DOE did not develop a final standard in 1995. At this point in time, the earliest a new standard could be implemented is 1999 and 2000 is more likely in light of the one year moratorium proposed by the U.S.Congress (10/95 to 10/96).

In addition, the HCFC-14 1 B foam blowing agent currently used by most refrigerator / freezer manufacturers is due to be phased out by Jan~my 1 , 2003. All of the currently known alternates

such as HFC's 134a, 236ea, 245fa, 356mffm, 365mfc and hydrocarbons such as cyclopentane have k-factors of. 140 and above.

In short, the appliance industry faces the prospect of a DOE standard for an additional 20 to 30% reduction in energy after the year 2000 while facing the prospect of increased energy usage of as much as 10 percent or more due to a change in foam blowing agent. The possibilities for increased wall thickness are limited by access space in existing residential kitchens. The smaller models may be able to be made slightly larger but the larger higher value added models can not. This is where the use of vacuum insulations might be considered where improved insulation will allow thinner walls or larger internal volumes. These large, high feature models offer more opportunity for recovery of the high cost of vacuum insulation particularly when there are energy rebates offered by municipalities and power companies.

With all of the above factors in mind, Maytag - Galesburg Refrigerator Products (formerly Admiral Refrigeration) has had a long term development effort to evaluate alternate advanced insulations. Beginning with the original SEN (Solar Energy Research Institute, Golden, CO) test of CVI and continuing with the EPA sponsored evaluations of Thennalux aerogels, OCF "AURA" panels, Alladin metal panels and Degussa plastic encapsulated powder panels. All of these evaluations were performed on a standard 19 cubic foot top freezer model. Over the years of these evaluations the product energy has been steadily improving but the basic geometry of the cabinet has not changed and makes an excellent baseline for such studies. This also is the standard model that has been used for alternate blowing agent comparisons.

EXPERIMENTAL

Panel Fabrication

The Aerojet Resorcinol-Formaldehyde aerogel panels (hereafter called R/F panels) were provided as 1 1.5" x 10.5" x .70" castings with rounded corners on one side and sharp edges on the other side. Although the original plan was to fabricate larger composite panels (as was done for the Thermalux test units) the irregular shape and brittle nature of the panels made this impossible. It was decided to use the panel size delivered.

Early experimentation with evacuated panels indicated a pressure rise over time not typical of the packaging material when previously used with evacuated powder panels. After discussion with Aerojet it was decided to bake the samples before evacuation. The panels were placed in a TYVEC pouch to protect them in the oven and especially to protect the vacuum system. The final encapsulation was with a sealed VECAT pouch. Our sub-contractor has provided a tabulation of panel weight loss on baking for the I 16 panels processed which showed an average weight loss of about 12% with some panels changing by as much as 18% ( table 1). The sub- contractor has also provided measurement of the vacuum level on 12 of these samples by a proprietary non-destructive test as well as k-factor measurement at a 75 degrees F mean temperature for 4 of the samples (table 2). The reported vacuum levels are more than adequate to develop optimum k-factor.

Cabinet selection

The refrigerator / freezer model selected for this test is a 19 cubic foot (approximately 540 liter) standard top freezer design without special energy components (not a rebate model). This is a very popular model/size and easily scheduled for test runs. In addition, this particular model has been used as a test vehicle for various alternate foams as well as vacuum insulations [l]. With 1.88 inch refrigerator side walls and 2.38 inch freezer side walls, vacuum panels as thick as 314 inch to 1 inch can be used without any major flow problems (resulting in voids). The current version of this model has 2 inch thick foamed doors compared to the 1.5 inch doors used in earlier studies.

Panel Placement

A total of 28 panels were used on each cabinet as follows: 9 for each of the two side walls, 4 for the top and 6 on the cabinet back. These were attatched with a 1 " wide x 1/32" foam tape with adhesive on both sides. This neccessary to hold the panels in position during the foaming process. The freezer doors each had 2 panels and the refrigerator doors each had 4 panels.

Panel Area Coverage and Thickness - Because of the use of the standard 1 1.375" x 10.5" x 0.7" panels the area coverage was not as high as the earlier Thermalux and Degussa tests previously reported particularly in the doors. The cabinet side walls area coverage is calculated to be 55% compared to the earlier tests. The doors area coverage was only 38% compared to over 67% for the earlier tests. In addition, the sample thickness at around .70 inch average for the current Aerojet aerogel panels compares unfavorably to most of the earlier work done with 1 inch panels. Running a double thickness of Aerogel panels would not leave sufficient room for foam flow.

Foam Materials and Process

A polyurethane foam formulation blown with HCFC-141B blowing agent was injected into a single pour hole in the cabinet bottom. The reacting liquid sprayed to the cabinet top and flows back to the bottom as an expanding frothy mass where cavity air is vented through special breather holes that contain the almost reacted foam. The doors were poured with a similar formulation on a horizontal dual conveyor line which seals the expanding foam,

Energy Measurement Test (DOE)

The standard energy test for refigerator/freezers is called the DOE energy test, which is named after the Department of Energy. The test is performed at a 90" F ambient temperature with the cabinet operating, the doors closed, and the defrost cycle turned on for the test. The test cabinets are operated at two control point settings in order to be above or below a 5 O F freezer temperature, and the data is interpolated for a 5 OF freezer. In the case where electric anti-sweat heaters are used, the test is conducted with the heaters both on and off and the results averaged. Energy test results for this report will be compared directly to the average of the HFCF- 14 1 B

foam baseline cabinets, which are defined to be 100%.

K-factor Measurement

Single temperature (75 F) measurements at Maytag are on the Holometrix Rapid-K with 12" x 12" samples. K-factor versus temperature measurement has been done on the LaserComp Fox300, which also uses 12" x 12" samples. The upper plate was set as the cold plate, and the lower plate was set as the warm plate. Samples were exposed to the following pairs of temperatures: -1 5/15,0/30, 15/45,30/60,45/75,60/90 and 75/105 O F to obtain sample mean temperatures of 0,15,30,45,60,75 and 90°F. K-factors are calculated for the upper and lower plates using two separate heat flow meters and averaged.

REFRIGERATOR / FREEZER ENERGY TEST RESULTS

Percent Relative DOE Enerw Compared to the Baseline Cabinets Average

Baseline Cabinet A with HCFC-141B blown only in Cabinets and Doors Baseline Cabinet B with HCFC-141B blown only in Cabinets and Doors Baseline Cabinet C with HCFC-141B blown only in Cabinets and Doors

Baseline Cabinets Average

Aerogel Test Cabinet D with Vacuum Panels only in the Cabinet Only Aerogel Test Cabinet E with Vacuum Panels only in the Cabinet Only Aerogel Test Cabinet F with Vacuum Panels only in the Cabinet Only

Aerogel Panels in the Cabinet Only Average

Aerogel Test Cabinet D with Vacuum Panels in the Cabinet and Doors Aerogel Test Cabinet E with Vacuum Panels in the Cabinet and Doors Aerogel Test Cabinet F with Vacuum Panels in the Cabinet and Doors

Aerogel Panels in the Cabinet and Doors Average

99.09 99.81

101.10

100.00

93.19 94.95 89.12

92.42

88.85 91.98 90.56

90.46

Energy Test Discussion

The total energy improvement of nearly 10 percent is approximately what would be expected for the panel area coverage and thicknesses used. Slightly more improvement might have been obtained with the doors if higher area coverage could have been used. The use of 1 inch panels except on the refrigerator back could have added another 3 to 4%. All things considered, the aerogels gave equivalent performance to what would have been expected if comparable panels of the precipitated silica (Degussa) had been used. Slightly higher improvement levels are usually observed for tests with higher k-factor foams such as HCFC-141 B compared to CFC- 1 1 foams.

AEROGEL PANEL K-FACTOR TEST RESULTS

K-factor vs. Temperature Measurement

Two panels were measured early in the program and resGILs were reported at the November, 1994 meeting at Aerojet and shown on figure 1. Further testing of this kind was not possible since the Lasercomp tester needs to have a flat panel and the irregular nature of the Aerojet panels put the test plates in a bind. Based on subsequent 75 F k-factor measurements on the Holometrix tester by Maytag and our sub-contractor the R150 BA2 samples to be more representative of the panels tested in the cabinets.

K-factor (75 F) and Vacuum Measurement on Sample Panels

The sub-contractor provided measurement of the vacuum level on 12 of these samples by a proprietary non-destructive test as well as k-factor measurement at a 75 degrees F mean temperature for 4 of the samples (table 2). The reported vacuum levels are more than adequate to develop optimum k-factor. One of the vacuum panels was brought back to ambient pressure and had a measured k-factor of .0894 (Winch = 1 1.185)

CONCLUSIONS

The use of the Aerojet Resorcinol / Formaldehyde Aerogel in a vacuum panel appears to produce comparable energy improvement to earlier testing done with silica aerogel and precipitated silica vacuum panels. Current estimated costs for these insulations, however, do not look promising for early implementation in household refXgerator freezers. Opportunities for special rebate models may materialize in the future but near term prospects are not good as long as comparable energy improvement levels can be attained by less costly component replacements.

PROJECT COST SUMMARY

Item OriPinal Forecast Actual Cost

W r t L . Manpower Cost $18,615 !Ky44 5,450 d J ’ 3 q Total Man-hours 604 247

Travel Cost $2,100 $2,041 >l lJ lClL W- Materials Cost $4,000 $1,740 Sub-contractor Fabrication of Panels $1,070 Total Project Cost $24,7 15 $rn

%3V\ Tasks 6 through 12 were not completed due to competing priorities for the test facilities and the observation that these insulations were not dramatically different from those tested earlier.

0 e Table 1: Panel Weights Before and After Oven Drying (with TYVEK)

74 .48 .43 75 .32 .28

Table 2:

# 9

# 16

# 59

# 60

# 66

# 77

# 102

# 105

# 110

# 11

# 113

# 117

Pressure and K Factor on Panels That Were Tested

0.3 TORR .054 K FACTOR

0.9 TORR

0.9 TORR .057 K FACTOR

0.5 TORR

1.0 TORR

1.2 TORR

1.0 TORR .048 K FACTOR

1.6 TORR

0.9 TORR

0.6 TORR

1.0 TORR .055 K FACTOR

1.0 TORR

0.068

0.066

0.064

0.062

0.060

0.058

0.056

0.054

0.052

0.050

0.048

0.046

0.044

. .

-e R200 BA3 3.5 TORR.

~ n m m n m u - - - - n n m n - m w m K-FACTOR VS. TEMPERATURE FOR ORGANIC AEROGEL SAMPLES FROM

AEROJET-GENERAL (11121194) MEASURED AS VACUUM PANEL INSULATION

+ R150 BA2 2.8 TORR. . _ _ _ I_ - . .

. . . ...

.. .

lr^l 17:1 1-* 1L.l

0 I O 20 30 40 50 60 70 80 90

SAMPLE MEAN TEMPERATURE - F

I - 1

AEROJETI . X L S Itvt avg figure 1 HAWORTH 20196

Boeing Corp.

Did not respond to requests for program results

34

GWCadillac

Did not respond to requests for program results

35

Benteler Industries

Results summarized on next page.

36

i 1 . Pr ram/Pro ea IEentdlearmn NO. 3. Repomng Perm 6k-FCOd-94ID13291 . mercialization Pilot Project 7 r 9 4 mrough 1 W95

t Name and Address Bentekr Industries 3 721 Hagen Drive Gmid Rapids, Mi 49548 6. Conorem Oate I8 __

I I I

Benreler determined rhe dyno durability and insulating integrity of aerogel powder in the air gap of exhaust duwnpipes was questionable. We discovered it wits difficuit to contain and seal it fiom escape. Our sccond application of aerogel, in air gap exhaust manifolds, have additional escape routes to seal. Therefore, the assembly, testing and development of aerogel in manifolds was cancelled.

Performance V m c e s . kamptisnments, or PfOPt8ms

I i a None

c I -

Benteler spending to date: lTEM OyaNTTTY RATE i%i COST f $1

i Travel to Acrvjet 4 people 1,50O/ptrson 6,000 Engineering Labor 203 hours SOhour 10,150 Matcrials/Protorypes 4 downpipes t ,000 each 4,000 Dyno Testing 154 hours 75hour 1 I , S O Totat - - 3 1,700

I 1)9

10. Status Asbessmenr and foreca$f

Aerojet estimated the cost of aerogel microspheres to be approx. $lOO/fG, while currently avaiiabte ceramic fibers cost i apprvx. $j/fi3. Also, Benteler demonstrated zlerogtI had negligible bcnefit to heatshielding, sound intensity and hear-up time compared 10 ceramic fibers. At a 20 t h e s greater costhenefit ratio compared to ceramic fibers, continued R&D of 1 this aerogel application is not recommended. 1

I I i 1 1 1 I

Glacier Bay

Results summarized on next page.

37

FINAL REPORT ARPA-TRP AEROGEL COMMERCIALIZATION PILOT PROJECT

Purpase The purpose for Glacier Bay's involvement in this project was to determine the suitability of aerogels for use as an insulation material for thermal storage refrigerators and freezers in shipboard (marine) applications. The ultimate goal being that of space savings by providing a reduction in the required thickness d t h e insulated walls.

TMting The testing pameters were established cooperatively with Glacier Bay, Inc. and Lawrence Livermore National Laboratory and presented in detail in the Joint Program SoIicitarion No: SOL 93-29, July 21,1993. This provided that Glacier Bay, Inc. wouid design, fabricate. test and evaluate the performance of a two (2) prototype cabinets each utilizing 72 board fcet of aerogel material. Sufficient quantity of aerogel was not made available to Glacier Bay, Inc. to complete even one of this test cabinets therefore these tests we not performed. Glacier Ray, Inc. was eventually provided with 24 board feet of resorcinol-formaldehyde aerogel monolith. The material was of variable quality and the quantity was inadequate to perform any of the testing p h d , Although information made available to Glacier Bay, Inc. indicated that a hydrophobic variation of low density silica aerogel may be best for our application, no such material was ever made available.

Cooperation and Consultation Although the Joint Program Solicitation clearly stated that cooperation and mutual assistance would be provided to end-user participants by the Pilot Project Proposers (LLNL, LBL, Aerojet) virtually none was available. Attempts to interface with LLNL and LBL werc made after we received our first samples of material. However, we were told that all of the money they had received to perform their obligations had essentially rn out and that there was no assistance which could be provided.

Conclusion The funding committed and provided by ARPA and the end-user participants should easily have been adequate to meet the obligations a p e d to in the Joint Program Solicitation. From our perspective the entire project achieved little if anything due to almost unbelievablc poor management by, and continued disagreements among, the proposal presenters (LLNL, LBL, Aerojet) .

G. Kevin Alston, President Date