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TM04533

28 MAY 1993

ASRM DEVELOPMENT TEST PLAN

HUMIDITY EFFECTS ON SOLUBLE CORE

MECHANICAL AND THERMAL PROPERTIES

VOLUME H

(NASA-CP-193B93) HUMIDITY EFFECTS

ON SJLUgLE CORE MECHANICAL AND

THERMAL PROPERTIES (PgLYVINYL

ALCOHOL/MICROBALLOON COMPOSITE)

TYPE CG EXTFNDOSPHERES, VOLUME 2

Final Report (tiber Materials)

314 p

N94-2422_

Uncl3s

G3/24 0204200

Contract No. NAS8-37800

DR-TM04

WBS 1.3.2.4

TYPE 3THIS DCCUMENTAVAILABLE FROM

ASRM DATA MANAGEMENTYELLOW CREEK. MS

ASOF:7'-/5"-7,_ _ ,,

https://ntrs.nasa.gov/search.jsp?R=19940019751 2018-04-29T16:44:46+00:00Z

EMTL-FINAL REPORT NO. 1539

F,M_I-EMTL-W/A NO. 3111

FINAL REPORT

HUMIDITY EFFECTS ON SOLUBLE COREMECHANICAL AND THERMAL PROPERTIES

(POLYVINYL ALCOHOI./MICROBALLOON COMPOSITE)TYPE "CG" EXTENDOSPHERES

BY

THE ENERGY MATERIALS TESTING LABORATORY

A DMSION OF FIBER IdATERIALS INC.

5 MORIN STREET

BIDDEFORD, MAINE 04005

PREPARED FOR:

AEROJET ASRM DIVISION

1 NASA DRIVE, BUILDING 1000

IUKA, MS 38852-8998

ATI'N: ROD M. BIZZELL/0954

MANUFACTURING ENGINEER

PURCHASE ORDER NO. 100345

MAY 28,1993

A OivurdoN OF IqiE/t MATEmALL INC.BIOOEFORD INO4LJ4FrIMALPAIU(., EIOOI[FQ4_O, ME. 040_

F_RWARD

This effort was performed by the Energy Materials Testing

laboratory (EMTL) , a division of Fiber Materials, Inc. (FMI) , 5

Morin Street, Biddeford Industrial Park, Biddeford, Maine 04005.

Technical questions regarding the report can be dire__ed_" "_o thefollowing:

Technical: Glenn M. Vaillancourt

Principle Investigator, Project Engineer

Technical: Darrell R. Dunn

Manager, Mechanics and Structures Lab

Technical: Stephen A. Michaud

Manager, Thermophysical Properties Lab

Technical: Paul A. Pelton

Manager, Analytical Chemistry and Morphology LabDivision Manager, EMTL

Contract Administrator: David R. Audie.

ORI_NP, t, PAGE IS

OF P<_R QUALITY

THIS DOCUMENT WAS REVIEWED

BY S. SKLADANEK

____ _/ //-(

SYS/_qgIS ENGINEERING

Designee

REVIEWED BY FLIGHT HARDWARE

SAFETY& RELIABILITY

S.T. PEACE, LMSC S&R

Designee

Section

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

i0.0

ii.0

12.0

13.0

14.0

15.0

16.0

17.0

F!7_

I.,_R_L_ ION ......................

OBJECTIVE .......................

PURPOSE .........................

PASS/'FAIL CRITERIA ...................

SCOPE ........................ 2

SPECIMEN MIXING .................... 4

SPECIMEN MOLDS .................... 5

FILLING AND PACKING OF THE MOLDS ........... 5

SPECIMEN CURING .................... i0

STORAGE AND AGING OF SPECIMENS ............ 12

TENSILE AND COMPRESSIVE TEST APPARATUS ........ 13

TENSILE AND COMPRESSIVE TEST PROCEDURES ........ 17

TENSILE AND COMPRESSIVE DATA REDUCTION ........ 21

TENSILE AND COMPRESSIVE TEST RESULTS ......... 22

THERMAL EXPANSION MEASUREMENTS AND RESULTS ...... 37

MICROSCOPIC EXAMINATION OF FRACTURE SURFACES ..... 45

DISCUSSION/OBSERVATIONS ................ 48

FIGURE

1

2

3

4

LIST OF FIGURES

5

6

7

8

i0

ii

12

13

14

15

16

17

18

19

Tensile Specimen Mold Drawing .............

Compressive Specimen Mold Drawing ...........

CTE Specimen Mold Drawing ...............

Photograph Tensile and Compression Molds, Mixing of the

Binder solution, and the Curing Oven ..........

Photo Tensile and Compressive Test Facility ......

Close Up View of Tensile and Compressive Setups ....

Tensile Test Fixture Drawing ..............

Graphical Summary of the Effect of Humidity and Loading

Rate on Tensile and Compressive Strength ........


Rate on Tensile and Compressive Modulus .........


Rate on Tensile and Compressive Poisson's Ratio ....

CTE facility ......................

NIST Standard Reference Test ..............

Graphical Summary of Thermal Expansion Measurements

Microscopic Photographs of Fracture Surfaces ......

Typical Tensile and Compression Specimen Failure Modes

Strength Using Type SG vs CG Extendospheres ......

Modulus Using Type SG vs CG Extendospheres .......

Poisson's Using Type SG vs CG Extendospheres ......

CTE Using Type SG vs CG Extendospheres .........

PAGE

9

14

15

16

23

24

25

38

39

40

46

47

52

53

54

55

ii

LIST IF T'-_-'-S

1 Tensile and Compressive Aging Conditions/Test Matrix

2 Thermal Expansion Aging Conditions and Test Matrix

3 Drying Oven Evaporation Rate Determination ...... i0

4 Effect of Humidity and Loading Rate on Tensile

Strength, Modulus and Poisson's Ratio ......... 26

5 Effect of Humidity and Loading Rate on Compressive

Strength, Modulus and Poisson's Ratio ......... 26

6-14 Individual Tensile Properties ........... 27-31

15-23 Individual Compressive Properties ......... 32-36

24 Effect of Humidity on CTE Measurement ......... 41

25-29 Individual CTE Measurements ............ 42-44

30 Tensile Properties Using SG vs CG Extendospheres 56

31 Compressive Properties Using SG vs CG Extendospheres 56

32 CTE Properties Using SG vs CG Extendospheres ..... 57

Appendix

Microballon Certificate of Analysis ............. 60

Individual Batch Formulation Data .............. 62

Individual Curing/Aging Date and Time Summaries ....... 64

High Humidity Aging Wet and Dry Bulb Measurements ...... 75

Laboratory Ambient Humidity Strip Charts .......... 78

Individual Dimensional Measurements . . . . . . . . . . . . 81

Curing and Drying Temperature vs Time Strip Charts ..... 90

Tensile and Compression Strain Measurement Qualification i01

Individual Tensile and Compressive Stress vs Strain Curves

(Raw Data) ........................ 104

Individual CTE curves (Raw Data) ............. 204

iii

This Jccu:ent constitutes the final reFcrt fcr the study ofhum!!ity effects anJ loading rate on soluble core (PVA/MB

composite naterial) mechanical and thermal properties under

Contract No. 100345. This report describes test results,

procedures employed, and any unusual occurrences or specificobservations associated with this test program.

Note: The test methods used in this program were exactly as used

during the conduct of Purchase Order #100364 and reported in EMTL

report #1491, dated 5 January 1993. The only difference between

these two programs was a change from type "SG,, extendospheres totype "CG" extendospheres, as requested in the SOW.

2.0 OBJECTIVE

The primary objective of this work was to determine if cured

soluble core filler material regains its tensile and compressive

strength after exposure to high humidity conditions and followinga drying cycle. Secondary objectives include measurements of

tensile and compressive modulus, and Poisson's ratio, and

coefficient of thermal expansion (CTE) for various moistureexposure states. I

A third objective was to compare the mechanical and thermal

properties of the composite using "SG" and "CG" typeextendospheres.

3.0 PURPOSE

The proposed facility for the manufacture of soluble cores at the

Yellow Creek site incorporates no capability for the control of

humidity. Recent physical property tests performed with the

soluble core filler material showed that prolonged exposure to

high humidity significantly degradates in strength. The purpose

of these tests is to determine if the product, process or

facility designs require modification to avoid imparting a highrisk condition to the ASRM. I

4.0 PASS/FAIL CRITERIA

The material tensile and compressive ultimate strength shall

return to within one standard deviation of the baseline ultimate

strength after exposure to high humidity conditions followed by adrying cycle at comparable cross-head speeds. CTE measurements

are required to support engineering analyses. I

ORIGINAL, PAGE I$

OF POOR QUALITY

5.0 SCO_E

In summary, EMTL performed the following tasks:

o Purchased the required materials for specimen fabrication.

o Fabricated molds and test fixturing.

o Mixed, molded, and cured the tensile, compressive and CTE

specimens.

o Aged the test specimens.

o Tested the specimens.

o Submitted final test report.

Tensile and compressive test were conducted to determine the

effects of high humidity (90%) and strain rates (0.05, 0.25, 2.0

in/min) on the tensile and compressive strength, modulus and

Poisson's ratio of the material. These test also determined if

cured soluble core filler material regains its tensile and

compressive strength, modulus and Poisson's ratio after exposure

to high humidity conditions and following a drying cycle. The

drying cycle of 16±2 hours represents the soluble core barrier

cure cycle presently incorporated into the process.

EMTL conducted 32 tensile and 32 compressive tests at room

temperature after high humidity aging, after high humidity aging

then drying, and immediately after cure test conditions. Table 1

specifies the aging temperature, humidity level, drying time,

rate of testing, and number of tests that were conducted at each

condition.

EMTL also conducted 40 CTE tests after high humidity aging, after

high humidity aging then drying, immediately after cure, and

after a week under laboratory ambient conditions. Table 2

specifies the aging temperature, humidity level, drying time,

method of testing, and number of tests that were conducted ateach condition.

Thermal expansion measurements were performed over the range 70°F

to 250°F. Thermal Expansion was measured continuously over this

range.

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2

2

8

4

4

4

2

2

TE_

2

2

8

4

4

4

2

2

AG:NG IG;NG AGIwG Db_ATrON CQzlwG T:ME _T

9%5 90:10 120:12

90-5_ 90,I0. 120:12

90*5 90-10 120_12

90Z5 90-_10 120-_12

9_s <;_I0 Izo.,_I_

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I SPEZD ('_.'m'n)

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16:2 0.05

16_2 0.25

16_2 2.0

0.05

0.25

2.0

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CTE

8

8

8

8

8

TABLE 2

THERMAL EXPANS:CN SPECIMEN AGING CONDITIONS AND TEST MATRIX

I AGING AGING AGING ::1JRATION DRYING TIME AT SPECIMENTEMP (OF) RH (_) (HRS) 180°F (MRS) SIZE

90_5 90-10 120-I_ NONE 7"L x.75"0

90:5 16_2 7"L x.75"0

70*5

90:10

<50 7"L x. 75"D

7'% x. 75"0

2"L x.25"SO

3

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The specimen PVA/MB mixture was formulated by weight in the

following percentages from the following materials.

75%

10%

10%

5%

Microballoons - Extendospheres CG - Hollow Microspheres,

from PQ Corp. See appendix for certificate of analysis.Water

Ethanol - Alcohol, Anhydrous, Reagent• Specially DenaturedAlcohol Formula 3A, from VWR.

Polyvinyl Alcohol - Airvol 205, from Air Products.

Several replicate 5.5 ib batches of this mixture were made duringthe course of the program. The binder solution for the mixture

was made by combining 250±5 grams of tap water with 250Z5 grams

of denatured ethanol in a liter beaker. This water ethanol

mixture was heated to 130 ° ± 5°F and agitated on a magnetic

stirring hot plate. 125±2 grams of polyvinyl alcohol (PVA)

crystals were slowly added to the heated mixture and agitated

until the PVA crystals were fully dissolved.

1875±25 grams of microballoons were pre-measured and placed intoan airtight, i0 liter, wide mouth container. The microballons

were slowly stirred by hand, with a spatula, while the binder

solution was added. Hand mixing continued for approximately 5

minutes until a homogeneous PVA/MB consistency was obtained. If

the mixture was not immediately pressed into molds, it was sealed

in the air tight container and used within two weeks after mixingor discarded.

Presented in the appendix are the various batch numbers and their

corresponding formulation weights.

7.0 SPECIMEN HOLDS

All specimens were cast from PVC or aluminum molds dependent cn

the specimen type. The internal surfaces of all molds were

sprayed with several coats of FREKOTE NO.I mold release

manufactured by the Dexter Corporation. The top of all molds

were kept open to provide a vapor path for the water/ethanol.

Each mold was firmly packed using a low density tamper (glass

phenolic or wood rod), and compressing approximately two to three

times the volume of PVA/MB material into the molds.

The tensile mold was made of aluminum as per EMTL's drawing

EMC-3915. Reference Figure 1 for the tensile mold drawing.

The compression molds were made of PVC pipe, 3"Z0.0625" diameter

by 7" long faced off to length so that the centerline of the pipe

was perpendicular to the bottom edge of the pipe. One end of the

pipe was covered with a solid flat plate and the opposite end of

the pipe was covered with a plate that had a 3" cylindrical hole.

The pipe was held between these plates with 4 bolts. The hole in

the top plate allowed filling and packing of the mold. This

compression mold assembly was easily assembled and disassembled

easing the filling, packing, and specimen removal operation.

Reference Figure 2, EMTL DWG# EMC-3929, for the compressive mold

drawing.

The CTE molds were made of aluminum as per EMTL's drawing # EMC-

3925. Reference Figure 3 for the CTE mold drawing.

Reference Figure 4 for a photograph of the tensile and

compressive molds, mixing of the binder solution, and the curing

oven.

8.0 FILLING AND PACKING OF THE MOLDS

The method used to prepare uniformly compacted compression

specimens was to add the loose PVA/MB mix to the mold in

approximately 200 ml portions. Each portion was tamped and

compacted before the next was added. This process was continued

until the mold was completely filled.

The tensile and CTE samples were prepared in the same manner as

the compression samples except the loose PVA/MB mix was added to

the molds in smaller amounts (=25 ml portions) due to the smallermold volume.

Great care was taken to obtain tightly packed samples of uniform

density since we knew from previous work, with this PVA/MB

material, that the degree and uniformity of compaction has a

direct effect on the properties of the composite. The

difficulties encountered in creating uniformly compacted

laboratory size samples underscores the difficulty to be expected

when creating large solid rocket motor molds.

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9.0 SPECIMEN CURING

All samples were cured in the same oven at 250=F. The tensile

_nd CTE samples were cured for a minimum of 6 hours. The

compression samples were cured for a minlmum of 9 hours. Strip

chart records of cure temperature vs time relating to specimen

type and number are presented in the appendix. Tabulations of

the date and time the specimens were placed into and removed from

the curing oven are summarized in the appendix.

The specifications for the drying oven were outlined in a sub-

specification of ASTM C495, ASTM C88. The oven was to be capable

of being continually heated at 230Z9°F for 4 hours and the rate

of evaporation, at this range of temperature, was to be at least

25g/hr. The rate determined for this oven was 27.6g/hr. Thisrate was determined from the water loss from five 1 liter low-

form beakers, each containing 500g of water at 70±3°F, placed at

each corner and the center of the oven. The results of this

evaporation determination are presented in Table 3.

TABLE 3

DRYING OVEN EVAPORATION RATE DETERMINATION PER ASTM C88

BEAKER WEIGHT WEIGHT WEIGHT AFTER 4 EVAPORATION

NO. EMPTY FULL HRS AT 230°F (g) RATE (g/hr)

(g) (g)

1 303.1 803.6 695.3 27.1

2 309.1 809.3 662.9 36.6

3 297.1 797.8 693.7 26.0

4 409.5 909.6 802.6 26.8

5 408.8 908.9 800.2 27.2

Note: Evaporation rate must be >25g/hr. AVE = 26.7g/hr

Date: 4/20/92, Time in 13:05, Time out 17:05

Ol_ PC/OR QLJ_,LITY

I0

Each specimen, as it was removed ...... :he ms':s ,as assianed a

unique identification. The specimen ile=tlfls_tien system that

was emp!c'/ed in this program was as fcilc_s:

TEN-75_F-90 -0.05-1

ReD!icate ._:umber

Crosshead Soeed (in/min)

0.05

0.25

2.0

N/A for CTE

Aqinq Humidity Level (%]

5O

90

Dry

Test Temp (°F)75

N/A for CTE

Type of Evaluation

TEN-Tension

CMP-Compression

CTE-Thermal Expansion

After the compression specimens were removed from the molds, the

end of the samples corresponding to the open end of the mold

required machining to remove the rough surfaces left by the

filling process. All compression samples were ground in the FMI

machine shop to their final dimensional requirements. Finish

machined specimens were weighed, and the post cured gravimetric

density in air calculated per ASTM-C559 to an accuracy of 1% or

better. The tensile and CTE specimens did not require any

machining after removal from the molds. The tensile and CTE

specimens were also dimensioned and weighed.

All of the samples underwent visual inspection for cracks, voids,

discolorations, inclusions, irregularities, and surface porosity.

Flawed specimens were excluded from further processing.

II

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Baseline Post Cured, Dry! Sannles:

After the cure cycle, the baseline compression samples were

cooled in a desiccated, sealed chamber at ambient temperature for

6 hours mlnimum prior to final machining. After machining the

ends of the specimens flat and parallel, these samples were

reheated to 250°F for 4 hours to remove any moisture that might

have been absorbed during the time they were out of the

desiccator. After the redrying cycle, the baseline compression

samples were cooled again in a desiccated, sealed chamber at

ambient temperature for 6 hours minimum prior to testing.

Testing was conducted within five minutes after removal of the

specimens from the cool-down chamber.

After the cure cycle, the baseline tensile and CTE samples were

cooled in a desiccated, sealed chamber at ambient temperature for

6 hours minimum prior to testing. Unlike the compression

samples, these tensile and CTE samples required no further

preparation. Testing was conducted within five minutes after

removal of the specimens from the cool-down chamber.

High Humidity Aged Samples:

High humidity aging at 90%RH, 90°F was accomplished with a

humidity chamber. The humidity level and temperature inside the

chamber was monitored daily through the use of dry and wet bulb

thermometer measurements. Tables of the humidity level, wet and

dry bulb measurements and dates are in the appendix. These

samples were weighed immediately after removal from the humidity

chamber to determine the wet density of the samples after high

humidity conditioning. Testing was conducted within five minutes

after removal of the specimens from the humidity chamber.

High Humidity Aged/Dried Samples:

After high humidity aging, some of the samples were to be dried

at 180°F for 16Z2 hours. This was accomplished with the same

oven used for curing the samples. After the drying cycle, these

samples were cooled in a desiccated, sealed chamber at ambient

temperature for 6 hours minimum prior to test. Testing was

conducted within five minutes after removal of the specimens fromthe cool-down chamber.

12

i._.., Tz..,-e''_-._- A:;D CCMTRESSI','E TEST .:-.P:'-:'-.-"S

-he =ecn]nisal test equipment consiste2 of the following:

o 20,000 !b Electro-Mechanical Test Machine Model 1113.

o I0,000 lo Load Cell, 2500 Series (Compression Tests).

o 1,000 Ib Load Cell, 2500 Series (Tension Tests).

o Load Cell Conditioner, No. LPM-700-000.

o Compressive Platens.

o Tensile Test Fixtures, DWG# EMC-3914.

o i0 Channel Strain Gage Conditioner, 2100 System.

o Strain Gages, No. EA-13-1OCBE-120, EA-13-250BG-120/LE.

o 12 Inch Vernier, 0.001" Resolution.

o Computerized Data Acquisition 386 System.

o High Humidity Chamber No. C08A-3-I0.

o Type K Thermocouples.

o I0 Channel Thermocouple Meter No. 650-KF-A-DSS

o Strip Chart Recorder No. 141/39/31/50

o Balance, 4000 gram range, No. GT4000.

o Balance, 160 gram range, No. RI60D.

Note: Two types of analog to digital (A/D) converters were used

for these tests. The A/D which provides the cleanest signal has

an operational limit of i0 Hz and was used for the testsconducted at 0.05 and 0.25 in/min. In order to acquire data at

25 Hz an A/D which does not take time to filter the signals

before transmitting was necessary. The jagged stress vs strain

curves, for the 2.0 in/min tests, are due to the use of this

"non-filtering" A/D converter.

Figure 5 is a photographic record of the mechanical test facility

and the high humidity aging chambers. Figure 6 is a close up view

of the tensile and compressive setups. Figure 7 is the tensile

test fixture drawing.

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16

L2,0 TE,';S-LE AND COMPRESSIVE TEST__ ?F3]EEL'-_ES

All test- -l..g was pe_fo_ed in accordance with the good engineer n_

practices established by the following accepted ASTM procedures

and the customers statement of work,

ASTM_ Title

C 31

C 39

C 307

C 495

C 469

E 4

E 6

E Iii

Method of Making and Curing Concrete test Specimens in the

Field.

Test Method for Compressive Strength of Cylindrical

Concrete Specimens.

Tensile Strength of Chemical-Resistant Mortar, Grouts, and

Monolithic Surfacing.

Compressive Strength of Lightweight Insulating Concrete.

Static Modulus of Elasticity and Poisson's Ratio of

Concrete in Compression.

Practices for Load Verification of Testing Machines.

Terminology Relating to Methods of Mechanical Testing.

Test Method for Young's Modulus.

Following is a brief description of the tensile and compressive

test procedures.

Compression Test Setup and Calibration

A I0,000 !b load cell and compression platens were installed in a

universal test machine. The crosshead displacement rate was set

at 0.05 in/min and verified with a dial indicator and a stop

watch. The load cell, strain gage, extensometer and LVDT signal

conditioners were connected to a data acquisition computer via an

analog to ffigital converter. These measurements were monitored

and recorded during testing at a sampling rate of 2 Hz for the

tests conducted at a crosshead speed of 0.05in/min, l0 Hz for the

test conducted at 0.25 in/min and 25 Hz for the tests conducted

at 2.0 in/nin. Once all data acquisition and test equipment was

setup it was calibrated before any tests were conducted. Theload cell was calibrated init_ally with a proofing ring traceable

to NIST. During this calibration, a shunt-calibration was also

determined. This shunt calibration was checked before each run

to ensure that the calibration did not change during the course

of the program. Additionally, calibrated dead weights were

placed on the load cell to verify the load cell response. The

strain gages signals were calibrated with a shunt resistor. The

extensometers were calibrated with an extensometer calibrator.

The LVDT was calibrated with a LVDT calibrator.

17

Prior to ]stu_i specimen testing, a graphite qua!if_saticnspecimen was tested to verify compressive platen alignment, ih=sspecimen was instrumented with axi_l 4 straln gages located at

90 _ to each sther around the specimens gage section. The

specimen was placed between the compression platens and loaded to

50% of its yield strength. The four gages were monitored during

testing. Their output signals were recorded and used to determine

the amount of bending, if any, induced into the specimen. This

compressive setup was adjusted until it introduced less than 5%

bending into the specimen.

This graphite specimen was also used to qualify the axialextensometers and the transverse LVDT that would be used to

measure strain on the PVA/MB samples. A transverse strain gage

was added to the graphite qualification sample. The two axial

extensometers were place 1800 to each other over two of the axial

strain gages. The transverse LVDT was positioned around the

circumference of the sample at mid height, near the transverse

strain gage. The graphite specimen was loaded to 50% of its

yield strength. The axial and transverse strain gage readings

were compared to the axial and transverse extensometer and LVDT

readings. All strain measurements were in agreement and the

results of this test are presented in the appendix.

PVA/MB Compression Specimen Testinq

The PVA/MB compression specimens were tested in accordance withASTM C495-86 and the statement of work. Two axial extensometers

were place on the specimen 180 ° from each other at the samples

mid height. The transverse LVDT was positioned around the

circumference of the sample just above the extensometers.

For the specimens conditioned at high humidity, compression

testing was conducted at room temperature within five minutes

after removal of the specimens from the high humidity chamber.

For the samples conditioned at high humidity, dried at 180°F,

then cooled to RT in a desiccated chamber, compression testing

was conducted at room temperature within five minutes after

removal of the specimens from the cool down chamber. For the

baseline specimens, after the redrying cycle following final

machining, the samples were cooled to RT in a desiccated chamber

for 6 hours minimum prior to testing. Compression testing was

conducted within five minutes after removal of the specimens from

the cool-down chamber.

Plots of stress vs strain were generated for each test and usedto calculate modulus and Poisson's ratio. The maximum load

obtained during testing was determined from the data printout

sheets and used to calculate ultimate compressive strength.

18

Tensile Test 5etun _nfl Calibration

A 1,000 ib i:ad cell and tensile test f=xtures were installed :n

a universal test machine. The crosshead displacement rate was

set at 0.05 in/min and verified with a dial indicator and a stcp

watch. The i9ad cell, strain gage, extensometer and LVDT signal

conditioners were connected to a data acquisition computer via an

analog to digital converter. These measurements were monitored

and recorded during testing at a sampling rate of 2 Hz for the

tests conducted at a crosshead speed of 0.05 in/min, I0 Hz for

the test conducted at 0.25 in/min and 25 Hz for the tests

conducted at 2.0 in/min. Once all data acquisition and test

equipment was setup it was calibrated before any tests were

conducted. The load cell was calibrated initially with a

proofing ring traceable to NIST. During this calibration, ashunt-calibration was also determined. This shunt calibration

was checked before each run to ensure that the calibration did

not change during the course of the program. Additionally,

calibrated dead weights were hung from the load cell to verify

the load cell response. The strain gages signals were calibratedwith a shunt resistor. The extensometers were calibrated with an

extensometer calibrator. The LVDT was calibrated with a LVDT

calibrator.

Prior to actual specimen testing, a graphite qualification

specimen was tested to verify tensile grip alignment. This

specimen was instrumented with axial 4 strain gages located at

90 ° to each other around the specimens gage section. The

specimen was placed in the fixtures and loaded to 50% of its

yield strength. The four gages were monitored during testing.

Their output signals were recorded and used to determine the

amount of bending, if any, induced into the specimen. This setup

was adjusted until it introduced less than 5% bending into the

specimen.

This graphite specimen was also used to qualify the axialextensometers and the transverse LVDT that would be used to

measure strain on the PVA/MB samples. A transverse strain gage

was added to the graphite qualification sample. The two axial

extensometers were place 180 ° to each other over two of the axial

strain gages. The transverse LVDT was positioned around the

circumference of the sample at mid height, near the transverse

strain gage. The graphite specimen was loaded to 50% of its

yield strength. The axial and transverse strain gage readings

were compared to the axial and transverse extensometer and LVDT

readings. All strain measurements were in agreement and the

results of this test are presented in the appendix.

19

P'.'A MB TensiZe Specimen TestLnq

The PVA/MB Tensile specimens were testel in acccrJance with the

statement of work. Two axial extensc=eters were place on the

specimen 180 o from each other at the samples mid height. The

transverse LVDT was positioned around the circumference of the

sample between the extensometer arms.

For the specimens conditioned at high humidity, tensile testing

was conducted at room temperature within five minutes after

removal of the specimens from the high humidity chamber. For the

samples conditioned at high humidity, dried at 180°F, then cooled

to RT in a desiccated chamber, tensile testing was conducted at

room temperature within five minutes after removal of the

specimens from the cool down chamber. For the baseline specimens,

after the redrying cycle following final machining, the samples

were cooled to RT in a desiccated chamber for 6 hours minimum

prior to testing. Tensile testing was conducted within five

minutes after removal of the specimens from the cool-downchamber.

Plots of stress vs strain were generated for each test and used

to calculate modulus and Poisson's ratio. The maximum load

obtained during testing was determined from the data printout

sheets and used to calculate ultimate tensile strength.

2O

!3.0 TE:;S_'- AND e_s<_qSl','E TEST _._.A FE:'UCT _;

The results that were calculated for mechanical tests included

Ultimate tensile and Compressive Strength, Modulus, and Pc[sscn's

Ratio.

o Ultimate Strength of the material was calculated from the

equation: US = P/A, where:

US = Ultimate Strength (psi)

P = Maximum load obtained during testing (ibs)

A = Cross-sectional area (in 2)

o Modulus of Elasticity was determined by drawing a tangent

line on top of the initial linear portion of the axial

stress/strain curve. The slope of this line represents themodulus of the material and was calculated from the

equation: E =Aa/AE, where:

E = Modulus of Elasticity (psi)

Aa = Linear Increase in Stress (psi)

AE = Linear Increase in Strain (_)

o Poisson's Ratio is equal to the ratio of transverse strain

to axial strain over the same increment of stress.

Note: Ultimate compressive strength was defined as the first

drop in load. Most of compression samples never loaded above the

first load drop value. All of the ultimate compressive strength

data was reported at the first drop in load value.

The density of the Samples is presented for reference only. In

order to reduce the number of tensile specimen measurements and

still provide a density value, the following method was used to

calculate an average mold (specimen) volume for all the tensile

samples.

Density 6061 aluminum = 0.098 lb/in 3.

Average weight of the 8 tensile molds = 1.725 ibs.

Therefore, volume of alum in the mold = 1.7251bs in 3 = 17.600 in 3

0.098 ibs

Volume of a solid mold based on surface dimensions is = 24.92 in 3

Therefore, the missing volume (volume of tensile specimen)= 24.92 in 3 - 17.600 in 3 = 7.32 in 3 =120.0 cm 3.

This 120.0 cm 3 value was used for all cure, wet, and dried

density calculations.

21

For the compression and CTE samples, pre.'ic_s reports _EMTL-14+I.

EMTL-1430) calculated "cured", "wet", anl "Jried" !enslties

based cn the cured dimensisns only. However, in this regort,

additional measurements were taken at the wet and dried

conditions and these measurements were used to calculate the wet

and dried densities of the compression and CTE samples. The

original method shows relatively larger increase and decrease in

densities, where as the second method does not. Original method

type density results can be obtained from tNis report's data by

simply using the cured dimensions for all density calculations.

Since these wet and dried measurements were for reference only,

it is left to the reader to decide which method is more useful.

14.0 TENSILE AND COMPRESSIVE TEST RESULTS

The effect of humidity and loading rate on tensile and

compressive properties is graphically summarized in Figures 8

through I0. The effects of humidity and loading rate are also

presented in tabular form in Tables 4 and 5. Tabulations of the

individual values are presented in Tables 6 through 23.

Tabulations of individual batch formulations, individual

cure/aging dates and times, individual dimensional measurements,

high humidity wet and dry bulb measurements, strip chart records

of cure temperature vs time, plots of the high humidity aging

conditions, drying cycle temperature vs time plots, and the

individual stress vs. strain curves are presented in the

appendix.

22

ORIGIN;,t i'.'_3E IS

OF POOR Q_ ,_LI'rY

cn

In

In

O

Sb%{MARY OF EFFECT OF }KfMIDITY AND LOADINGON TENSILE AND COMPRESSIVE STRENGTH

TYPE CG EXTENDOSPHERES

RATE

1500

1250

1000

750

5OO

250

0

= c--_ _ (Dm0

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VELOCITY, IN/MIN

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Energy MoterioleTeet.in@ Loborot.ory

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CROSSHEAD VELOCITY. IN/MIN

23

SUMMARY OF EFFECT OF HUMIDITY A_ND LOADLNGON TENSII_E AND COMPRESSIVE MODULUS


_ &,KSE-NE ,_RY) i

90_, 90%R_. THEN C)Ri_ !

g0_', 90%RHl

.4-

RATE

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CROSSHEAD VELOCITY, IN/MIN

24

Ii

i

2.0

O

E-

C_

SUMMARY OF EFFECT OF HUMIDITY A_ND LOADING RATEON TENSILE AND COMPRESSIVE POISSONS RATIO


.¢

BAS_NE {DRY) l_K)"_',_K)_r.RH._ DRIED

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v

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0.25

VELOCITY,

X X

2.0

IN/MIN

£

.5

.4.5

.¢

a,',SBJNC(OrgY)1_ eO_',eO'_. I"HIP_DRI_

o'x-'Am_,,r,_N74_

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Z0 .3

.25,--,0 _-

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Energy MaterlaleTeetlng Laboratory

0.25

CROSSHEAD VELOCITY, IN/_N

25

":S_E *

::;E--_" .S_ -ILIW!DI'Y AND L_IWG e_E 3N "E_S:.E 3A'_, wEAN *AL_ES

"Y_E IICSIIEw'EwDCSr''E;E S

I i i

Z_wCZ'IOW (:F) SPEED (,_,_n) I =EAw !cs_) J MEAw C"_) I:;ATIS

i

"ENS:SN 3ASE_TIE 7_ 0.05 _37 .25_ I .'27

SASE_:IE _ 0.25 _50 .2'5 .13_

BASE.:_E

90_.RM(_R IED)

90_,__ ('_i_IEl))

73

73

73

2.00

0.05

0.25

_37

_3_

z._8

.2_7

.26_

.259

• ',:.6

• 12,:,

.122

73 2.00 401 .2?3 .126

75 0.05 198 .0820 .329

0.25 229 .0776 .25690°F ;_J'_ 73

90°F ;_/_Ig_ 73 2.00 202 .0916 .252

TABLE 5

Err_CT OF HUMIDITY AND LOADING RATE ON COMPRESSIVE DATA, MEAN VALUES

TYPE "CG" EXTENDOSPHERES

TEST TYPE AGING TEST TEMP CRO_3SHEAD STRENGTH MOOULUS POISSON'S

CONDI':ON (OF) SPEED (in/min) MEAN (psi) MEAN (n_i) RATIO

COMPRESSIVE 8ASEL:_E ?3 0.05 1031 .333 .150

BASEL:_E

BASEL:IE

90%RwC:_IED)

90%RMC:_IED)

90%RM _.'_IED)

900F ).'%R_

90°P o_.,_

90°F _,,RN

73 0.25 1100 ,336 .150

73 2.00 1058 .309 .132

75 0.05 1066 .370 .144

?3

?3

73

?3

0.25

2.O0

0.05

0.25

2.00

1333

1312

673

6?3

768

.371 .I_I

.373 .152

.0756

.0693

.0787

.361

.332

.317

ONIG'IN;_,t_;.'.:._E .'._

-.. I ¢OF P_-_P {_)L;AL.T_

26

:wDIVIOCAL TENSILE PRv-_E_TY SLMMA_Y, T_;E -_" E_TE4CCSP_E_ES

AGED AT qCS_R_, ;_ °c, '.E4 SR'ED _' I_0 °r

$;E-'wEW NO. AGING TEST :ROSS_EA3 S:_ENGT_ W(]_ULJS PC ZSSCw'S

CONDITION TEuP SPEED (;_s_) (_'_i) RAT:O

(OF) ('m/m_n)

,Ew-_SF-QC_CDRTED)-O.C5-17 90t.RH(DRIED) 75 3._5 .._._ .233 .'O_

TEW-7_F-90%(DRIED)-O.C5-18 901_RH(DRIED) _ 0.05 ,37.1 .311 .'30

"EN-7_F-90%(DRIED)-0.05-19 901r.RH(DRIED) 7_j 0.05 427.7 .253 .!26

TEW-7_F-gO%(DRIED)-O.05-20 90_RH(ORIED) 75 0.05 392.3 .2_2 .I05

TEN-75F-90%(DRIED)-O.05-21 91)',I_M(DRIED) 7"5 0.05

TEN-75F-9_)%(DRIED)'O.05-22 90X,_H(DRIED 75 0.05

TEN-75F-90%(DRIED)-O.05-2.3 90'&RH(DRIED) 75 0.05

TEN-75F-90%(DRIED)'O.05"24

TEN-75F-90_(DRIED)'O.05-46

TEN-75F-90%(DRIED)-O.05-47

90%.RH(DRIED)

901{,RH(DRIED)

90%RH(DRIED)

75

73

75

0.05

0.05

0.05

AVE

SD

CV (%)

443.0 .2B_, .137

316.9 .238 .129

374.8

_TS.6

_89.0

539.7

_33.B

62.3

14.4

.258

.255

.276

.286

.26/..

.0249

9.4&

.120

.119

.120

.143

.12_

.0117

9.45

TABLE 7

INDIVIDUAL TENSILE PROPERTY SUMMARY, TYPE "CG" EXTENDOSPNERES

AGED AT 90%RN, 90°F, THEN DRIED AT 180°F

SPECIMEN NO.

TEN-75F-90%(DRIED)-0.25-25

TEN-75F-90%(DRIED)-0.25-26

TEN-75F-90%(DRIED)-O.25-27

TEN-75F-90%(DRIED)-O.25-2B

TEN-75F-90%(DRIED)-0.25-48

AGING

CONDITION

90%RH(DRIED)

9O%RM(DRIED)

9O_,RH(DRIED)

9O_IJIH(DRIED)

90_,RH(DRIED)

TEST

TEMP

(OF)

75

75

75

73

75

CROSSHEAD

SPEED

(in/min)

0.25

0.25

0.25

0.25

0.25

AVE

SO

CV (%)

STRENGTH

(psi)

_20.2

420.0

433.1

401.1

566.9

448.3

67.3

15.0

MOOULUS

(ms i)

.242

.250

.258

.228

.316

.259

.0338

13.1

POISSON'S

RATIO

.131

.104

.125

.0949

.155

.122

.0236

19.4

ORIGIN;:,L t:::,,.GE ISOF POOR QUALITY

27

SPEC:WEw _0.

"Ew-TSF-_C%C:RIE3)-2.SO-2_9

TEN-7_F-_;_]'4(DRIED)-2.00-30

TEN-7_F-_%(DRIED)-2.00-31

TEN-7'SF-90%(DRIED)-2.00-4.Z,

TEN-7'SF-90"Z,(DRIED)-2.00-45

AGING

CONDITION

9C_{,RH(DRIED)

(_O"/.,_H(DRIED)

;>O_{,RH(DRIED)

(;_'I,RM(ORIED)

9(]_RN(DRIED)

TEST

TEWP

(OF)

75

7"5

73

7"5

73

:RZSS-EAD

S_EED

(,_/m_ _ )

2.:0

2.C0

2.CO

2.00

2.00

AVE

SD

CV (%)

Cps_)

_80.3

259.2

583.1

239.0

_01.4

14836.9

.2,.3

.2_,5

.273

.308

•308

.27"5

.032811.9

'22

.132

.X33

.159

.126

.0216

17.2

OF POOR QUALITY

28

,N_,V,3CAL "E_S LE P_SPE_ T_ S_MM_" *'_E ":S E('E_2CS;-E_ES

S;E]:wEN _. AG:NG 'EST ::CSS-E_S , S'_E_5:_ W_l::bLwS cC:SSC_'SCSNDITION TEWP SPEED ] :cs_) (_"r_) _AT:O

(o_) C'" _:m:' i J

"EW-75F-D_Y-].35-1 BASELINE 75 0.3,5 -2'3.2 .223 .'29

TEN-75F-DRY-O.35-2 BASELINE ,'5 0.35 -C_,2 .233 ._30

TEN-TSF-DRY-O.05-3 BASELINE 7_ 0.05 _13.6 .261 .I_5

TEN-75F-DRY-O.05-4 BASELINE 75 0.05 _8x..I ,258 .12G

TEN-75F-DRY-O.05-5 BASELINE 75 0.05 _32.9 .259 .]3-¢,

TEN-75F-DRY-O.05-6 BASELINE 75 0.05 507.B .283 .118

TEN-75F-DRY-O.05-7 BASELINE 7_ 0.05 38L,.9 .258 .120

TEN-T_F-DRY-O.05-8 BASELINE 75 0.05 448.1 .261 .139

AVE _37.0 .254 .127

SD _1.4 .0185 .00892

CV (%) 9._7 7.27 7.04

TABLE 10

INDIVIDUAL TENSILE PROPERTY SUMMARY, TYPE "CG" EXTENDOSPMERES

BASELINE SAMPLES DRY

SPECIMEN NO. AGING TEST CROSSHEAD STRENGTH M(X)ULUS POISSON'S

CONDITION TEMP SPEED (psi) (ms i) RATIO

(o_) (in/min)

TEN-75F-DRY-0.25- 9 BASELINE 75 0.Z5 _89.0 .263 .151

TEN-_F-DRY-0.25- 10

TEN-75F-DRY-0.25- 11

TEN-TSF-DRY-0.25- 12

BASELINE

BASELINE

BASELINE

75

75

75

0.25

0.25

0.25

AVE

SD

CV (%)

453.7

428.9

_.30.5

450.5

28.0

6.22

.245

.236

.236

.245

.0127

5.20

.139

.144

.112

0.136

.0171

12.5

Off, G, ;..._: ,_;

29

£_'ENSCSP-E_ES

" i

];£Z:.E_ _Z. _5[NG T£ST Z_ZSS_E&3 $'_E_GT_ wCCULUS PGISSCw S

CONDITION TEwP SPEED :ps!) (r_1) RAT:O

; i

"EN-75F-;R_-2,30-13 BASELINE _ 2.'3 [ 307._ .225 ._50

TEN-7"_F-DRy-2,i30-1_ BASELINE 75 2.3 _53._ .2_8 ._32

TEW-7_F-DRY-2.00-15

TEN-75F-DRY-2.00-16

BASELINE

BASELINE 7'5

2.0

2.0

AVE

SD

CV (%)

500.I

_26.3

&37.0

55._

12.7

.234

.282

.2&T

.0250

10.1

.1.-2

• 160

.146

.0119

8.1_

OF PC'vOR QI.i/:_LI"I_"

30

"_SLE "2

i

SPEC:WEN NO. A&I4G TEST CRCSS.E_3 SrRE4GT_ NODuLeS ;OISSC,hq 5CCNDITION rEaP SPEED ,psi) C"r_) RATIO

(c;) (,r,_'-',

TE_.7_F._C%-3.,35-33 ;0%RM, ;Oa; 7'5 3.05 £C6.5 .C896 .36&

TEN-7'SF-90%-0.05-34 7'5 3.05 216.2 .08./,.2 .29&

TEN-75F-90%-O.05-35

TEN-75F-90%-O.05-41 90%RH, 90°;

TS

75

0.05

0.05

AVE

SD

CV (%)

176.2

198._

17.2

8._

.O779

.0764

.0820

•006O8

7.&I

.325

•334

.329

.0258

8.76

TABLE 13

INDIVIDUAL TENSILE PROPERTY SUMMARY, TYPE "CG" EXTENDOSPMERES

AGED AT 909&,qH, 90°F

SPECIMEN NO.

TEN-TSF-90%-0.25-37

TEN-75F-90%-0.25-38

AGING

CONDITION

90_RH, 90°r

90%,RH, 90°F

TEST

TEMP

(OF)

7"5

75

CROSSHEAD

SPEED

(inlmin)

0.25

0.25

AvE

SD

CV (%)

STRENGTH

(psi)

245.7

213.6

229.6

22.7

9._

MOOULUS

(msi)

.0769

.0783

• 0776

.000990

1.28

POISSON'S

RATIO

• 262

.251

.256

•00778

3.04

TABLE 14

INDIVIDUAL TENSILE PROPERTY SUMMARY, TYPE "CG" EXTENDOSPHERES

AGED AT 90%,RH, 90°F

SPECIMEN NO.

TEN-75F-90%'2.00"39

TEN-75F-90%-2.00-40

TEN-TSF-90%'2.00"42

TEN-'75F-90%-2.O0-43

AGING

CONDITION

90_RN, 90°F

TEST

TEMP

(OF)

90"ARN, 90°F

75

CROSSHEAD

SPEED

(inlmin)

2.00

STRENGTH

(psi)

257.3

MOOULUS

(ms i)

.0984

POISSON'S

RATIO

.259

90_,aM r 90°F 75 2.00 180.2 .0923 .271

90_RM, 90°F 75 2.00 112.6 .0811 .243

75 2.00 260.3 .0949 .237

AVE 202.6 .0916

SD 70.5 .00748

CV (%) 34.8 8.16

.252

.0154

6.13

0,Q6;%'i' ; :',_r ,e...... __

OF PC'-_'_ '_U_I%_"

31

'wC;v:DUAL C:_WP;ESS:,E _;.3r_ERF_ ;jwjwA;F T'CE 'Z_' E(TEwCCSP'E;ES

:; E- " W'E'w ',,C. TEST

TEWP

(3F)

i2_]SSHEAD

SPEED

, (!minim)

S';ENGT_

I

SwP- _F-_O%(_R IED ) -0 .,]5-21 <;_]_H(DR IED ) _ ].05 "2C0 .35; . I _,:,

CMP- 7_3F-gx:]%(DR iED ) - O. 95- 22 _H(DRIED) 75 0.,?,5 ;130 .3S5 '._2

CMP- _F- 9O%(DR I ED)- 0.05 - 23 _M(DRIED) 75 0.'35 ?,BO .369 . !30

CMP- 75 F- 91]%(DR I ED)- O. 05 - 24 O(TfJ_M (DR I ED ) _ 0.05 I0<_5 .385 .139

CMP- 7'5F-90_{(DR IED) - 0.05- 25 000{,RH (DR IED) _ 0.05 1372 .395 .'_.5

CMP- 75 F- 90"4(DR 1ED) -0.05- 26 90_H(DRIED 75 0.05 86,4 .357 .157

CMP- 75 F-qO_,(DR IED) - 0.05- 27 90"_g_H(OR IED ) 75 0.05 83g .379 .162

CMP- 75 F-90"/,(DR [ED) -O. 05- 28 90"/,RH(DR IED) 75 0.05 1003 .375 .138

CMP- 75 F- 90",_(DR I ED ) - 0.05 - 29 90_&RN(DR I ED) 75 0.05 976 .368 .147

CNP- 75 F-90%(DR IED)-O.05- 30 90_,RH(DR I ED) 75 0.05 1200 .357 .140

AVE 10_:_ .370 .144

SD 165 .0135 .00930

CV (%) 15.5 3.65 6.46

TABLE 16

INDIVIDUAL COMPRESSIVE PROPERTY SUMMARY, TYPE "CG" EXTENOOSPHERES

AGED AT 907,,RH, 90°F, THEN DRIED AT 180°F

SPECIMEN NO. AGING TEST CROSSHEAD STRENGTH MOOULUS POISSON' S

CONDITION TEMP SPEED (psi) (ms_) RATIO

(OF) (in/m_n)

CMP- 75F-90_,(DR I ED )- O. 25- 31 90Y, RM (DR I ED) 75 0.25 1273 .380 .146

CMP- 75F- 90%(DR I ED)- O. 25-32 90}',RH(DR I ED) 75 0.25 1330 .379 .139

CMP- 75F-90_(DR IED)- 0.25-33 90_RM(DR I ED) 75 0.25 1341 .365 .146

CMP- 75 F-90_(DR IED)-O. 25- 34 _N(DRIED) 75 0.25 1399 .364 .139

CMP- 75F- 90%(DR IED) -0,25-35 90_g_M(DR I ED ) 75 0.25 1322 .367 .137

AVE 1333 .371 . 141

SD 45. I . 00784 • 00428

CV (_) 3.38 2.11 3.03

ORIGI; _/-'L "" _;=""'"OF POOR QU_I.IIY

32

J

5_EC:MEw w_. A5Iw_ TEST ]RCSS,EA_ 3T_Ew_Tff I wOCUL_S ;C:SS_W'5

CONDITION TEMP SPEED C_s;) i (,_s_) _ATZ3(OF) (_,,_T_)i

i

CMP-7"SF-_C%C_IE_)-2.$0-36 90tr.RM(DRIED) I _ 2.00 " .3G6 ._5

CMP-TSF-QO%(CR!E_)-2.CO-37 90%.RM(DRIED) _ 2.00 " .w_7 .'57

CMP-7_F-90%(DRIED)-2.00-38 90_{,RM(DRIED) 7_ 2.00 " .3;5 .'55

CMP-73F-90%(DRIED)-2.00-39 90_,{I_M(DRIED) 75 2.00 • .37g .139

CMP-7_F-90%(DRIED)-2.00-L9 (]_:)%,RM(DRIED) 73 2.0 " .385 .I_I

CMP-_F-90%(DRIED)-2.00-51 _)_,RM(DRIED) 73 2.0 1303 .355 ._

CMP-7'SF-90_(DRIED)-2.00-52 O0_,RM(DRIED) 7'5 2.0 1073 .341 .134

CMP-7_F-90%(DRIED)-2.00-53 90_.RM(DRIED) 73 2.00 1207 .319 .17x_

AVE 1312 .3T3 .152

SD 128 .0325 .0152

CV (%) 9.T5 8.71 10.0

• Note: Load cell conclitioner over-ranged: 1400 _i/m_n value.

33

B_SE_:NE SAMPLES ::_'::

S_ZS:_EN 4C. _ AG;NG "ES: 3_CgS-£_3 I S'_EwGT_ wC_bL_S [ ;OISSON'S

] CONDIT:ON TE_P S;EED (;s_) C_s;) I _ATIO(s_) (,_ m'_)

I:Mp-_F-Dff_-].:5-_ BASELINE 7_ 0._5 ISC- .3_2 .139

CMP-7_F-DRY-O.05-2 BASELINE 7_J 3.05 1111 .380 _7_

CMP-75F-DRY-O.05-3 BASELINE 75 0.05 961.6 .333 .153

CMP-75F-DRY-O.05-4 BASELINE 75 0.05 1024 .328 .I_9

CMP-75F-ORY-O.05-11 BASELINE 75 0.05 1063 .316 .137

CMP-7_F-DRY-O.05-12 BASELINE T5 0.05 879 .379 .164

CMP-75F-DRY-O.O5-13 BASELINE 75 0.05 1014 .286 .144

CMP-75F-DRY-O.05-14 BASELINE 75 0.05 888.8 .300 .136

AVE 1031 .333 .150

AD 136 .0338 .0139

CV (%) 13.2 10.1 9.26

TABLE 19

INDIVIDUAL COMPRESSIVE PROPERTY SUMMARY, TYPE '°CG" EXTENDOSPHERES

BASELINE SAMPLES DRY

SPECIMEN NO. AGING TEST CROSSHEAD STRENGTH MOOULUS POISSON'S


(OF) (inlmin)

CMP-75F-DRY-0.25-5 BASELINE 75 0.25 1220 .376 .153

CMP-75F-DRY-0.25-6 BASELINE 75 0.25 1197 .360 .156

CMP-75F-DRY'0.25-7 BASELINE 75 0.25 1144 .334 .156

CMP-75F-DRY-0.25-15 BASELINE 75 0.25 757.6 .320 .160

7S 0.25 1188 .305CMP-TSF-DRY-0.25-16

CMP-7_F-DRY-0.25-17

BASELINE

BASELINE 7_ 0.25

AVE

SO

CV (%)

1095

1100

174

15.8

.319

.336

.0271

8.08

.142

.133

.150

.0103

6.89

34I_nO_:IOUALII'Y

:401V!_AL

T_3LE ZCEOWP_ESS:vE ;_CPE_ TY _J,_M_RY '':E

BASELI4E SAMPLES C_ _

'ZS' _'S43CS;-S;ES

SPECIWEW 4_.

CMP-_F-DRY-2.00-IOA

T

i TESTTEWP

S_P-7_F-Cq_-2.00-8 BASEL:WE

CMP-7_F-DRY-2.0_-gA BASELIWE 75

BASEL!WE 73

CMP-7_F-ORY-2.00-18 BASELINE 75

CMP-73F-ORY-2.00-19 BASELIWE 73

BASELIWE 7"5CMP- 7_ F - DRY - 2.00- 21:)

C_CSS_EAD

S;EED

('rlm,n)

2.3 "ZZ6 .27a .,_7

_5 .326 .135

_C85 .32_

2.0

2.0

927.92.0 .328

2.0 I0a5 .333 ._36

2.0 939.8 .270 ._12

.I09

AVE

SO

CV (%)

1058 .309 .132

111 .0290 .0209

10.5 9.37 15.8

" ,h

35

"-'5.S "'

rr j ,SPES:WEw _0. _GING TEST , :ROSS_EAD STRE_GT_ WOOUL_S =C[SSC_'S

CONDITISN "EwP J S;EE3 (ps,) (,n_s;) _AT:O

(OF) ] (ir/m!_)

CWP-7_F-90%-3.35-_I 91]',&RH,_0°_ 75 0.35 542 .37-7'_ .3"-2

CMP-7"SF-90%-O.05-42 75 0.05 624 .06J.I .350

CMP-7_F-90%-O.05-43 75 0.05 725 .0708 .311

CMP-75F-90%-O.05-44 90"wL_H, 90°F 75 0.05 700 .0901 .410

AVE 67"3 .0756 .361

SD 47.6 .0111 .0414

CV (X) 7.07 14.7 11.5

TABLE 22

INDIVIDUAL COMPRESSIVE PROPERTY SUMMARY, TYPE "CG" EXTENDOSPNERES

AGED AT 90X.RH, 90°F

SPECIMEN NO. AGING TEST CROSSHEAD STRENGTH M(X)ULUS POISSON'S


(OF) (in/min)

CMP-?SF-90%-0.25-45 90"/,RN, 90°F 75 0.25 792 .0833 .308

CMP-75F-?0%-0.25-46 90"w,RH, 90°F 75 0.25 640 .0721 .365

CMP-75F-90%-0.25-48 90_RH, 90°F 75 0.25 592 .0524 .322

AVE 675 .0693 .332

SD 104 .0156 .0297

CV (%) 15.5 22.6 8.95

TABLE 23

INDIVIDUAL COMPRESSIVE PROPERTY SUMMARY TYPE "CG" EXTENDOSPHERES

AGED AT 90_H, 90°F

SPECIMEN NO. AGING TEST CROSSHEAD STRENGTH MOOULUS POISSON'S


(OF) (in/min)

CMP-75F-90%-2.00-49 75 2.00 760 .0787 .315

CMP-75F-90%-2.00-50

90ZRH_ 90°F

90"/.RH, 90°F 75 2.00

AVE

SD

CV(%)

777 .0787

768 .078712.0 - -

1.56 - -

.319

.317

.00283

.892

36

°

5.0 ,__-_.-FZTZE"-".,, C'F TH m_''_.................=.'.--.-..,_ -".' _'E-='SUREM_'"_-.

Csefficient of The_m. al ExFansicn measurements were made us!ng the

..e ....a (F_gure 11) {n accordance w__nquartz Fush rod di!atometer - "_ " _ - "

Test Specification ASTM E-228 entitled "Linear The._m, al Expansicn

of solid Materials with a Vitreous Silica Dilatometer".

Sample heating and measurement was performed within the

isothermal zone of an insulated furnace, with controlled heating

rates that were limited to 5°F per minute. Sample temperature

was recorded with a Type K thermocouple, and length changes were

recorded with an linear voltage displacement transducer (LVDT).

Two sample sizes were used for this measurement, 2.00 inches in

length by 0.25 inches wide by 0.25 inches thick and samples 7.0

inches long with a 0.75 inch diameter.

Each specimen was tested over the range of room temperature to

250°F.

Prior to measurement of the PVA/MB samples, a calibration test

was performed using the NIST fused silica standard reference

material, SRM 739-i. The results are shown in Figure 12.

The average CTE results for the PVA/MB samples are shown in

Figure 13 and Table 24. Tabulations of the individual values are

presented in Tables 25 thru 29.

Tabulations of individual batch formulations, individual

cure/aging dates and times, individual dimensional measurements,

high humidity wet and dry bulb measurements, strip chart records

of cure temperature vs time, plots of the high humidity aging

conditions, drying cycle temperature vs time plots, and the

individual expansion vs temperature curves are presented in the

appendix.

Thermal expansion is presented in percent, and was calculated at

each temperature as;

% Expansion = _L/L o.

where:

_L = change in length (in)

L ° = original length (in)

37

C":E F._CZL _'_''_.

INERT GAS I

_LO_ iN Ji

QUARTZ PUS]_ ,_

RO0 II L

LVDT SIGNAL I I

CONDITIONER AND

FURNACE CONTROL ] I

QUARTZ

TU BE

Ii

X-Y

RECORDER

TIc

I SPECIMEN !

J

FURNACE

38

Z

Z

Z

L,.

Z

0

I,--I

O_

_v

|_!_

| ,

m •

0

1!o

q

i.,.q

_0

1

_o'.04

1

i 0 ,,,0

-i1

.4

-4.

,,- 00 r_ _ c_l 0 _ _ r_) 00 ,,'--• 0 0 0 0 0 0 0 0 ,"

I

I I I t

]uaa.Tacluo!su_3dx_ T_U_._aq,L

39

o _t

=_-_

_Oa.J_

L

Z0

;>-,_

i I ! 1_ I ! | I |

iI

L L I I I

(:Z:)o o o. o. o. o. o. o. I ":

I I I I I

_uoo_odUOTsu_dx_t l_m.xoqJ,

z

L O

_0,_

t ° ._O0

,_..j

_O"_- I_11--

_0

S_ARY 3_ _;;_Z" _ HbM[3['" ZN CTE _ATA

"EST 7,_E AGING

CONDITION

(_) E_PANSIO_ AT TEMPERATcRE (°F)

,"3 180 _0 '_0 253

CTE BASELINE 0 .312 .02& .337 .071

90%,RH(DRIED) 0 .012 .026 .041 .077

70°F 507,,IRH 0 .008 .0006 -.028 .016

90°F 90_,,RM 0 .007 -.015 .107 -.111

CORRELATION 0 .005 .002 .006 .0_4,

4t

":GLZ 25

:w,C:,_'.:,+ALT._£;'WAL EJ(PAWS:,CN (S'E) S,-,MMAR'_, "';E '::3" _'_:E_,CCSP-E:ZS

BASEL'",E SAMpi-.._S'_:R+:'

SPES:wEW _0. C%) ExPAN_::N AT "EwPERAr+RE (c;)

7_ !00 _J :_0 250

CTE-DRY-I BASELINE 0 .012 ._25 .038 .071

CTE-DRY-2 " 0 .012 .024 .038 .074

CTE-DRY-3 " 0 .012 .026 .041 .074

,, .011 .025 .037 .070CTE-DRY-4 0

CTE-DRY-5 " 0 .012

" 0 .010CTE-DRY-6

CTE-DRY-7 " 0 .011

CTE-DRY-8 " 0 .012

AVE

SO

CV (%)

.012

.0075

6.3

.027 .040 .076

.024 .036 • 067

.021 .034 .0(54

.024 .035 .071

.037

.0024

6.4

.071

.0039

5.6

.024

.0018

7.4

TABLE 26

INDIVIDUAL THERMAL EXPANSION (CTE) SUMMARY, TYPE "CG" EXTENDOSPHERES

AGED AT 90°F 90% RH

_PECIMEN NO. AGING

CONDITION

(%) EXPANSION AT TEMPERATURE (OF)

I75 I 100 140 180 250

CTE-90%-17 90°F 90_,RM 0 .009 .005 -.085 -.086

CTE-90%-18 " 0 .006 .013 -.090 -.097

CTE-90%-19 .001 - .035 - .142 -.141

CTE-90%-20 " 0 .007 -.009 -.091 -.110

CTE-90%-21 " 0 .009 -.016 -.129 -.131

CTE-90%-22 " 0 .008 -.013 -.I06 -.110

CTE-90%-23 " 0 .008 -.012 -.104 -.102

AVE .007 -.015 -.107 -.111

SD .003 .0096 .0214 .0192

CV (%) 40 64 20 17

Mote: CV(%) vatue is not retevsnt in this type of anatysis but is presented for reference. As the ther_t

expansion curve returns to zero percent expansion, CV(_) al:_Droaches infinity. A better indication of the

data spre_w:l is reftected in the SO vlh._S.

42il -IOF POOR Q,.A,.ITY

SPEC:.EW _0.

CTE-O0_ (DRIED)-32

(%) E_PANSICN AT TEw#E_ATCeE (or)

?00 ".3 _80 250

CTE-90% (DRIED)-25 90"_M (DRIED) 0 .012 .029 .0_6 .083

CTE-90% (DRIED)-26 • 0 .012 .029 .045 ._85

CTE-90% (DRIED)-27 - 0 .010 ,021 .030 .86._,

CTE-90% (DRIED)-28 " 0 .012 .025 .041 .080

CTE-90% (DRIED)-29 , 0 .011 .026 .041 .075

CTE-9OII& (DRIED)-30 - 0 .014 .029 .0_7 .083

CTE-90_ (DRIED)-31 " 0 .011 .026 .043 .080

• 0 .011 .021 .033 .06,B

AVE

SD

CV (%)

.012

.0012

9.9

.026

.0033

13

.041

.0062

15.0

.077

.0076

9.9

TABLE 28

INDIVIDUAL THERMJ_L EXPANSION (CTE) SUMMARY, TYPE "CG" EXTENDOSPHERES

AGED AT 70°F 50% RH

SPECIMEN NO. AGIWG

CONDITION

(%) EXPANSION AT TEMPERATURE (OF)

75 100 140 180 250

CTE-SO%-g 70°v 50_,RH 0 .008 -.004 -.037 -.028

CTE-5OZ-IO " 0 .009 .004 -.027 -.017

CTE-50%-11 " 0 .008 -.007 -.043 -.033

CTE-50_-12 w 0 .011 .008 -.019 -.009

CTE-50_-13 " 0 .008 .002 -.025 -.010

CTE-50"&-14 " 0 .009 .002 .025 -.010

CTE-50"&-15 = 0 .008 .006 -.017 -.007

CTE-SO'&-16 " 0 .007 -.006 -.034 -.012

AVE

SD

CV (%)

.008

.001

lS

.0006

.006

- .028

.0089

32

- .016

.0096

60

Note: CV(%) value is not re|evant in this type of analysis but is presented for reference. As the thermal

expansion curve returns to zero percent expansion, CV(%) approaches infinity. A better indication of the

data spread is reflected in the SO values.

43

"_BLE 29 Z:3wPAeE .I'_ "&BLE JS

I_DI,_DUAL T_E_MAL EXPINS[SW (C'E) SCMMA_z, "'_E 'SS" E_'E_CCSP-EeES

,SC)e_ELAT;CN SAMPLES (0.26" B_ ].ZS" 3_ 2.S" L3NG)

TESTED 3RY FCR COMPAR:SCN T3 .ARCER ;;ECZWEW SIZE

CTE-Dry-l-Smal[

AVE

SD

CV (%)

AGENG

CONDITION

CORRELATION

7"5

(%) E(PAWS:CN AT TEWPERATURE (o;1

100

.01&

- .001

.006

-. 005

• 009

_80

.020

- .001

- .014

25O

• O%

.02B

.012

.004

.001

.008

.007

.001

.005

.005

..

.004

.004

.O05

.004

- .001

.002

.007..

.010

.012

•O02

.0O9

.014

.OO6

.010

.041

.O40

.027

.034

.040

.034

.012

37

Note: CV(%) value is not relevant in this type of analysis b_t is presented for reference. As the thermal

expansion curve returns to zero percent expansion, CV(%) aporoaches infini[y. A petter indication of the

data spread is reflected in the SD values.

44

The inner and outer surfaces of sever31 specimens were

microsccpicaily examined to verify that the microballons were net

crushed during the molding operation. No evidence of crushed

microballons was observed on these surfaces. The flaky material

obse_¢ed on the very outer surface of the samples is the mold

release agent.

The machined surfaces of the compression specimens were examined,

and as expected, revealed that the grinding operation openedmicroballons on these surfaces.

The fracture surface of the specimens were also examined, and as

expected, these surfaces also contain open microballons. Therewas a noticeable difference in the microballon failures on the

fracture surfaces of the compression and tensile samples. The

microballons for the tensile samples were simply broken where-as

the microballons for the compression samples were crushed into a

dust.

Photomicrographs were also taken of the specimens subjected to

high humidity conditions to determine if these samples appeared

to be anomalous. These photomicrographs showed no anomalies.

This examination was conducted using an Olympus SZ40

stereomicroscope.

Reference Figure 14 for a representative sample of these

photomicrographs.

Figure 15 is a photograph of typical tensile and compressivefailure modes.

45

.- :Y.FE -4

ZE::-i iF..:.::H5 iF FF+:.2:-'_F:E 5+_i-F'. YI :

i"

o , -. I,

FRACTURE SURFACE: TEN-75F-DRY-2.0-15

i, • _ (• I +

FRACTURE/MOLDED SURFACE: CMP-75F-90%-0.25-46

46OR,GI ,,-.._F._,.}v !SOF P(_OI_QUALITY

_I23LF.E 2_

_.7

17.0 DISC__'SS]:N/ OBSERVATI3NS

Effect of HumiJitv _nd Loadinq Rate on Tensile and Csm<ress;','e

Pro:erties.

The primary objective of this work was to deter_,.ine if curedsoluble core filler material regains its tensile and compressive

strength after redrying following exposure to high humidity

conditions.

The pass/fail criteria was that the material's tensile and

compressive ultimate strength shall return to within one standarddeviation of the baseline ultimate strength after exposure to

high humidity conditions followed by a drying cycle.

Figure 8 in section 14.0, shows that the material does in fact

regain its tensile and compressive strength after high humidity

conditioning and redrying. Additionally, the conditioning cycletends to increase the tensile and compressive strength. Similar

responses were noted for modulus and Poisson's ratio.

One possible explanation for this is that the high humidity

conditioning further distributes the binder (PVA) around the

microballoons, providing additional bonding sites and greater dry

sample strength.

If this theory is true, then it may be inferred that storing a

pre-cured mixture in a sealed container for an extended period of

time, may improve the distribution of binder (PVA) around the

microballoons and provide stronger samples.

It might also be predicted that an increase in the amount of

binder (PVA) for a given mixture may increase the strength of the

samples.

The effect of mixture pre-cure storage time and PVA concentration

could be determined by testing samples where (i) The mixture pre-

cure storage time is varied and (2) The PVA concentration is

varied.

Figure 8 also shows that the samples conditioned at 90°F,90%RH

had lower tensile and compressive strengths than the dry samples,

indicating that high humidity condition is the primary factor

responsible for the large reductions in tensile and compressive

strength. Significant changes in modulus and Poisson's ratio

were also noted for increases in humidity level.

It was also determined that faster loading rates provided higher

ultimate tensile and compressive strengths. The impact of

loading rate on modulus and Poisson's ratio was minimal.

Tensile and Compression Failure Modes.

All of the tensile specimens failed in the reduced gage section

area of the specimen. The compression samples failed in what can

be described as either a "cone and split" or "simple flat

crushing" sample failure mode. Reference Figure 15 for a

photograph of typical tensile and compressive specimen failures.

48

?nermal Exoansicn

F=gure 13, in section 15, shows that moisture level has a

significant influence on the free theism-a! expansion response of

the soluble core material.

The samples tested with no humidity aging (baseline dry) expanded

in a linear manner.

The samples tested after conditioning at 90°F, 90%RH, and then

redried at I80°F, expanded in a linear manner, similar to the

baseline dry samples.

Samples which were tested after conditioning at 90°F, 90%RH,

contracted considerably before expanding. These samples were

saturated with water during the high humidity conditioning, which

caused the samples to swell. During testing, as the water was

driven out of the sample, the sample contracted. Once all of the

water was gone, the sample expanded.

Samples conditioned at 70°F, 50%RH, contracted to a lesser degree

than the high humidity samples, before expanding. These samples

absorbed some moisture, during the 7 day conditioning period,

causing the sample to swell. During testing, as the water was

driven out of the sample, the sample contracted. Once all of the

water was gone, the sample expanded.

The 2" long baseline dry correlation samples provided non-typical

results. These samples were expected to respond like the other

baseline dry samples. However, they behaved more like the 7"

long samples conditioned at 70°F, 50%RH. Several factors could

be responsible for this event.

i) This smaller sample configuration is more likely to contain

proportionally larger localized variations in density than the

larger sample, resulting in a greater effect on the CTE

measurement.

2) The anomalous readings might be a function of the contact

force of the LVDT. Although these tests are called "Free"

thermal expansion tests, there is a small force of =25 grams

which acts axially against the specimen. This small load may be

sufficient to affect the CTE measurement on 2" long, 1/4" by 1/4"

square cross-section samples. The cross-sectional area of the 2"

long (1/4" by 1/4" square) samples is 7 times smaller than the 7"

long (0.75" dia) samples.

3) The increased surface area to total volume ratio, 16:1

(small) vs 5:1 (large), may cause these small samples to absorb

proportionally larger amounts of moisture. Increased moisture

absorption would occur from the time they are removed from the

cure oven until they are placed into a desiccated chamber, and/or

from the time they are removed from the desiccator until they are

placed into the dilatometer.

49

With all processing and test parameters equal, any Jifferences =nmechanical and thermal properties must be attributed to the typeof microballoon used in the test specimens, "SG" vs "CG".Following is a comparison of the physical properties of theextendospheres as described on PQ corporation's certificate ofAnalysis.

DescriptionSieve Particle Size Distribution:Mean Particle Diameter:Appearance:Melting Point:Bulk Density:Specific Gravity:Moisture:

Extendosphere Type"SG"

10-425

140

Gray, FF

>2700°F

24.1

0.687

0.2%

"CG"

10-212 Microns

106 Microns

Gray, Free Flowing>2700°F

24.9 lbs/ft 3

0.757 g/cm 3

0.1%

In summarizing this table, it appears that the "CG" type

extendosphere is slightly smaller than its counterpart resulting

in a higher bulk density. Intuition tell us that the strengthand modulus of the material should rise with the increase in

density and smaller extendospheres. Figures 16 through 18

compare the mechanical properties of the composite using the two

types of extendospheres at various humidity levels. As suspected,

strength and modulus values did rise using the smaller "CG" type

extendospheres.

Figure 19 compares the thermal expansion response of the

composite using the two types of extendospheres at various

humidity levels. The SG and CG baseline dry and redried samples

all responded in a similar manner.

However, the CG type samples aged at 75°F, 50%RH and at 90°F,

90%RH responded with a greater percent of thermal expansion.

Several factors could be responsible for this event.

I) The higher density of the "CG" samples resulted from the use

of smaller microballoons. With more total microballoons in each

sample, there is more total microballoon surface area. With more

total surface area, there is more total binder in the sample. If

the binder is responsible for all of the water storage, there

would be more total water storage capacity. With more total

water storage capacity there is more water to drive off,

resulting in an increased shrinkage.

2) If moisture penetrates the microballoons, and with the

increased total quantity of microballoons in the "CG" samples,

there is more total water storage capacity. With more total

water storage capacity there is more water to drive off,

resulting in an increased shrinkage.

5O

3) Since tnese two types of samples were not conditioned at thesame exact ti=e, it is possible that there was a slightdifference if the humidity levels of the conditioning chamber.Since this composite material is very sensitive to moisturelevels, the differences could be attributed to small variationsin moisture content. To resolve this question for future tests,a few SG and CG type samples should be conditioned in the samehumidity chamber at the same time, before performing the CTEtests.

The 2" long samples are considered too small to make any accurateassessments between SG and CG type extendospheres.

General Observations

It was observed, during the weighing of the "90°F, 90%RH"

samples, that the moisture was evaporating off at a rate of

approximately 0.0001 grams/sec. Every effort was made to weigh

and test the "90°F, 90%RH" samples as soon as possible.

51

SUMMARYON

OF EFFECT OF HUMIDITY AND LOADINGTENSILE AND COMPRESSIVE STRENGTHTYPE SG VS CG EXTENDOSPI_RES

RATE

).05

_ °_

--_\\

,, ,= ....\\\x ,,-'\\ . //i X Z

\\ " / / _ _.._\xxX ,/ X--'\v,X N,. ,,',X N

0.25 2.0

CROSSHEAD VELOCITY, iN/_J.N

15O0

1250

I000

t

(_

r'_--_II0_',llOlllN.THI_ DRED:SG

750

500OQZ_Q

[_ 250

0

Enemy Mated=leTemtlnl I.abomtory

VN\ A

"_N\ V

r,,,\/N

NX_Z

O.25

Ir'_T-

122v'/

_,/

!_//'-

%_IA

_ XI v

N_IV

kX_VI/k

2.0

CROSSHEAD VELOCITY, IN/MIIN

52

SUMMARY OF EFFECT OF HUMIDITY AND LOAD_'G RATEON TENSI1.E AND COMPRESSIVE MODULUS

TYPE SG VS CG EXTENDOSPKERES


.5

.45t==4

r./l.4

r_ .35

.3

0 .25 _----_-x

.15 \\r._ NN

.I

H\'"NN

.05 \\

0 _x\

0.05

Ener_iy MaterlaleTeeting Loboratory

!t r-',n sAss_ (m_)__ CSe0._

r'x-'-_ _,,F, ;_mH, THE_ DR_Z)-.SG

r'7"_ gO,,f'._I.L.CG

v ....

VA

v

x

\\\\\t

i

\\\\

\X\X\X\\\X

\X\\

\\

;-,IT-

v_.-;

/X

g

g/X

0.25

\N

\N

\N


53

V

_-. -t 1

!N//NV

/N

& •2.0

O

ZOcn[23

O=.

cn

oL_

SUMMARY OF EFFECT OF HUMIDITY A_X) LOADING RATEON TENSILE AND COMPRESSIVE POISSONS RATIO

TYPE SG VS CG EXTENDOSPHERES

.5

.4-5

.4

.35

.3

.25

.2

.15

.1

.05

0

" /

/

F..

L6.,

i

0.05

7_

,,/,////,,,4

//1

,/

,/

\\, ,,,----4\\_ /_-- ,

Y\\, \,--,q

0.25

/',4,

CROSSHEAD VELOCITY,

_ (_0-_

r'z"'_ _10,_',_:x;

/

\'qi,. \'qE -,, \,q

X i\'4(_-:4, "_';

2.0

IN/MIN

Energy MoterlaleTeotlng Labor=tory

_ (_a_.._

_.__ _', _ [n,-:r'-_ O0,K O_

I

I

0.05 0.25 2.0

I\

I\I'k

CROSSHEAD VELOCITY, IN/_I_

54

L,

V

55

TEST TYPE

TENSIO0_

TABLE 30

EFFECT OF HUN IDITY AND LOADING RATE _ TENS:LE 0ATA, MEAN VALUESTYPE "SG" VS "CG u EXTENDOSP_EeES

AGING TEST CRO_SHEAO STRENGTH wCOULUS I_ISS_'S

CO_IO[TIC)_ TENP ._EED MEAN (psi) WEAN (_) RATIO

(OF) (in/min)

CG SG CG SG CG SG

BASELINE 75 0.05 437 31G .25G .235 .127 .112

BASELINE 75 0.25 450 323 .2_5 .229 .136 .122

BASELINE 75 2.00 637 326 .267 .228 .1_,6 .0919

9Ol_RH(DRIED) 75 0.05 434 382 .264 .228 .12_ .118

901_H(DRIED) 75 0.2S 648 476 .259 .282. .122 .120

90¢RN(DRIED) 75 2.00 401 445 .275 .270 .126 .112

900F 90_H 75 0.05 198 154 .0820 .0780 .329 .369

900F 90¢RN 75 0.25 229 175 .077'6 .0809 .256 .271

90°F 90_X 75 2.00 202 181 .0916 .09433 .252 .265

TABLE 31

EFFECT OF HUMIDITY AMO LOADING RATE O_ CONPRESSIV1E DATA, MEAN VALUESTYPE "SG" VS RES

TEST TYPE AGING TEST CROSSHEAD STRENGTH NOOULUS

CONDITION TENP SPEED NtEAfl (psi) MEAN (ms i)

C°F) (in/min)

COMPRESSIVE BASELINE

BASELINE

BASELINE

905QRH(DRIED)

905r,RH(DRIEO)

905QRN(ORIED)

90°F 9_glN

90°F 9(fl_H

90°F 90_N

CG SG

75 0.05 1031 911

75 0.25 1100 951

75 2.00 1058 921

75 0.05 1066 874

75 0.25 1333 1021

75 2.00 1312 1066

75 0.05 673 526

7_ 0.25 675 575

75 2.00 768 619

POISSO_'SRATIO

CG SG CG SG|

• 333 .282 .150 .141

• 336 .Z94 .150 .160

.309 .315 .132 .150

.370 .292 .164 .140

.371 .294 .161 .133

.373 .287 .152 .137

.0756 .0952 .361 .333

.0693 .0956 .332 .301

.0787 .09M .317 .304

56

TESTTYPE

CTE

m

AGING

CONDITION

73

CG

BASELIME 0

9O_RH(DRIED) 0

70°F 50"/.RH 0

90°F 90_N 0

CORRELATION 0

TABLE ]2

_IN_RY OF EFFECT OF _¢OZTY C_ CTE OATA

TYPE "SO" VS "¢q" _XT_e)OSP.E_E_

(_) EXPANS[OIII AT TENPERATUIRE (oF)

I00 140 180 250

SG CG SG CG SG CG SG CG SG

0 .012 .0110 .024 .0299 .037 .OZ,S9 .071 .07_3

0 .012 .0101 .026 .028_ .0_I .0._45 .077 .0773

0 .008 .0048 .0006 .0045 -.028 -.0093 -.016 -.0159

0 .007 .0039 -.015 -.0166 -.107 -.0670 -.111 -.07130

0 .005 -.0049 .002 .0006 .006 .0154 .034 .0393

57

AEROJET ASRM, "Process Development Test Plan", WBS No. 1.4. 3 .4,

DR-TM05, Type 3, page I.

58

M_CROBALLON C_RTIFICATE OF ANALYSIS

6O

CERT[¢_ CATE CF _NALY_,I$

CLISTdDPIER;

_:H'PPED TO'I. i

FIBER M_TERIAL5 IN':.FIBER MATERIAL9 INC.

DATEI Apri 1 21, 1995P.O. #: 72733PR00UCT CODE' AI

PRODUCT: CG

LOT NUMBER : A!

Tmst Me_hod _i$¢ription R_$ul ts

U,$. STANDARD $1EUE PARTICLE _,IZE C.I_,TRIBUTION; :0 - 21_ MICRONS

WT % OVER 9IEVE

Vl _' ,A,

N./A

WEI_MT PER

MEAEURED VOLUME

AIR PYCNOMETE_

% LO_9 OVEN

DRIED S_MPLE

MEAN PARTICLE DIAMETER:

_PPEARANCE :

MELTING POINT:

BULK DENSITYs

SFECIFIC GRAVITY :

M0I c'r'_R='

i06 MICRON_

_:_Y, TREE FLOWING

>2703 DEOREES

Z4,9 LBS/FT3

•75? G/CO

0.I %

S IGNED

QUALITY CONTI_OL TECHNICIAN

61

TO BEAPPROVt_D

DATE INITIAL

GP-

INDIVIDUAL BATCH FORMULATION DATA

62

AEROJET AS_M P_A/WO

FORMULATION OF SOLUBLE CC_E ulxTLa_E

T_PE "CG" ExTEwOO'SPwERES

BATCH _ N20 ETMAW(3(. PVA TOTAL BIWDER IIWOE! .|X# (g) (g) (g) (g) (g) TEMP (F) TIIqE (.in)

1 187'5.2 251.3 250.3 124.9 2422.1 135"F 6W} 5

2 1873.1 250.1 250.4 125.1 2430.2 135"F 50 5

3 187B.7 250.2 254.0 127.9 2461.0 135"F 60 5

4 18;'2.3 250.8 253.8 127.2 2433.3 13_B'F 65 5

5 187_.2 253.0 253.0 129.5 2453.6 132"F 60 5

6 1880.0 254.6 251.6 128.0 2454.6 130"F 6Q 5

? 187_.0 252.6 250.2 127.3 2431.4 139"F _) 5

8 1878.0 251.0 250.8 125,6 240(].2 130"F 65 5

9 1874.1 250.7 252.9 125.1 2419.3 135"F 60 5

10 18_.4 250.1 250.1 125.0 2431.2 130"F 60 5

11 187_.6 251.2 250.0 125.2 2406.0 130"F 6() 5

12 187_.3 251.4 250.2 125.1 2420.0 130"F 60 5

13 187_ 250.8 249.8 125.4 -- 135"F 60 5

14 18T_.2 250.3 250.5 126.2 2443.9 135"F 60 5

15 1874.1 251.3 253.0 125.8 2445.5 130"F 60 5

FILLER W/XIWG

Note: Following stetements aPplY for ILL batches.

Binder mix agitation spell: St|rrld binder slowly with megr_etic stirrer hot plate.

PVA acldtton rate: SLOWLy added PVA to microbeLlons by hind while et|rrinli.

Filler mixing speed: Slow mtx_l by hand.Mixed filter Itoroge tim: For otL canqDress|orl, there was no Itoroge tim. Att r.._Ipresei_ batches were

completely used or rai|ru:ler d|scarciod. For termites end CTE, itorllge time m Less th4m 2 weeks.

JAB mixed aLL batches.

pecked eLL specimens.

63

INDIVIDUAL CURING/AGING DATE AND TIME SUMMARIES

64

0 _

r,_, :|-_

• s •

I :

"2

aco

65

uJ _-j..

s • • z •

c-

p

_o

Q.

,- |

)- Z GO *

0 4L. 6_a

68

]E

mU

a o_u

U U U U ¢J_ _ _ _ _ _ _ _ _.

72

ic_

z z

...... _ _l .... °,o_ ¢_ o-.9- _; _, _"

• z • • • z •

C

;_, oo_, , , _ _. __._ ..= ..= _=

z z • •

z •

7

o

:11 • Iu

|

_°

73

m

al

74

HIGH HUMIDITY AGING WET AND DRY BULB MEASUREMENTS

75

SPECIMEN _3.

CNP #21-30 r

Chair

CTE #17-32

AE_OJET ASRN PVA/M8

HIGH _¢..IMXD]TY AGING U_T AI_ ORT 8_,JL8 NEAS_RE_IENT$

15:0(3, 5/05/93 90 87 9O

8:00, 5/06/93 90 87 90

8:00_ 5107193 90 87 90

8:00, 5110193 90 87 9_

AEROJET ASRM PVA,/M8

HIGH HL.INIDITY AGING t,_T AJdO ORY BULB MEASI.JRENENTS

TYPE mCGM EXTEMOOSPHERES

v

SPECIIEH NO.

OqP lr31-60

Ch_lDer

SPECIMEN NO.

CMP d_1-50

Chamdoer #2

DATE, TIME DRY BULB _,_T BULB RELATIV1ETENP (OF) TEIeP (OF) NUNIDITY (_)

15:00 r 5105193 90 87 90

8:00, 5106193 90 87 90

8:00 t 5/07193 90 87 90

8:00, 5110193 90 87 90

AEROJET ASRN PVA/MB

HIGH HUMIDITY AGING q_T AND DRY BULB MEASUREMENTS

TYPE "CG" _XTENOOSPHERES

DATE, TIME

8:001 5111193

8:00, 5112193

DRY BULBTEMP (OF)

_T IIULITEMP (OF)

87

RELATIVI[

HUMIDITY (Z)

8:00 r 5/07/93 90 90

8:00, 5110193 90 87 90

90 87 90

90 87 90

Note: Wet _ dry butb muwur_te _ty taken pertodicatty.

Hlgl_ I_Jid|ty ¢_mr rurw rettabty for months uithout Klju=tment is preset co.lit|at1.

76

SPECTNEM _0.

TEW #17 32, S_P _'-55

ChasTiser 81

SPECIMEN NO.

TEN tf33-40

ChemDer #I

SPECIMEN NO.

TEN _1-6_

Chlmber

AE_OvET ASRM PVA/NB

MIG_ _UNIDITY AGIWG _T A_D DRY @_JLB IQEASL_EWEW'S

TYPE "CG" EXTEWOOSPwEgES

DATE, TINE

8:00 z S/17193

8:00, 5118193

DRY BULBTEMP (Dr>

9O

9O

9_

9_

87

87

87

87

AEROJET ASRM PVA/MB

HIGH HUNIDITY AGING _T AMD DRY BULB MEASUREMENTS

TYPE "CG" EXTENDOSPHERES

DATE, TIME

8:&5 t 5/1&/93

8:00, 5117193

8:001 5/18/93

8:00, 5119193

DRY BULB

TEI_P (OF)

9O

9O

90

9O

WET BULB

TEMP (OF)

87

87

87

87

AEROJET ASRM PVA/M8

HIGH HUMIDITY AGING f,_T ANO DRY BULB I,QEASUREMENTS

TYPE "CG m [XT_NOOSPHERES

DATE, TIME

16:00f 5114/93

8:00, 5117193

DRT BULB

TE_ (OF)

90

90

WET BULB

TEkLO (OF)

87

87

IIEL_TIVE

9O

9_

9O

90

RELATIVE

HUMIDITY (_)

9O

9O

9(]

90

RELAT IV1E

HUMIDITY (_.)

9O

90

8:001 5118193 90 87 90

8:00, 5/19193 90 87 90

Note: 1Jet I_d dry buLb aemiureimnts onty taken periodicaLLy.

Nigh h_alidity chli_er _ rettabty for mnthl without idjultalnt me preset ccnditione.

77

LABORATORY AMBIENT HUMIDITY STRIP CHARTS

78

i

ECN NO. 2_3

I

?

80

INDIVIDUAL DIMENSIONAL MEASDq_EMENT$

81

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97

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