27th HIGH TEMPLE WORKSHOP 2007 12-15 February 2007, Sedona, Arizona

Presentation Title: “High Thermal Conductivity Polymer Matrix Composites (PMC) for Advanced Space Radiators” Authors: E. Eugene Shin1, Cheryl Bowman, Duane Beach, et. al. --- NASA Glenn Research

Center, 21000 Brookpark Rd., Cleveland, OH 44135; 1 Ohio Aerospace Institute Submitted by: E. Eugene Shin

NASA Glenn Research Center - OAI 21000 Brookpark Rd., MS 49-1 Cleveland, Oh 44135 Tel: 216-433-2544, Fax: 216-977-7132 E-mail: Euy-sik.E.Shin@nasa.gov

Sponsoring Organization: NASA

ABSTRACT High temperature polymer matrix composites (PMC) reinforced with high thermal conductivity (~ 1000 W/mK) pitch-based carbon fibers are evaluated for a facesheet/fin structure of large space radiator systems. Significant weight reductions along with improved thermal performance, structural integrity and space durability toward its metallic counterparts were envisioned. Candidate commercial resin systems including Cyanate Esters, BMIs, and polyimide were selected based on thermal capabilities and processability. PMC laminates were designed to match the thermal expansion coefficient of various metal heat pipes or tubes. Large, but thin composite panels were successfully fabricated after optimizing cure conditions. Space durability of PMC with potential degradation mechanisms was assessed by simulated thermal aging tests in high vacuum, 1-3×10-6 torr, at three temperatures, 227 °C, 277 °C, and 316 °C for up to one year. Nanocomposites with vapor-grown carbon nano-fibers and exfoliated graphite flakes were attempted to improve thermal conductivity (TC) and micro-cracking resistance. Good quality nanocomposites were fabricated and evaluated for TC and durability including radiation resistance. TC was measured in both in-plan and thru-the-thickness directions, and the effects of microcracks on TC are also being evaluated. This paper will discuss the systematic experimental approaches, various performance-durability evaluations, and current subcomponent design and fabrication/manufacturing efforts. KEY WORDS: High temperature polymer composite, Pitch-based carbon fiber, Facesheet/Fin, Space Radiator, Thermal conductivity, Thermal expansion, Space durability, Nano-composites

https://ntrs.nasa.gov/search.jsp?R=20070010454 2020-01-27T02:15:33+00:00Z

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72

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/GRC:

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MC

ND

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aci

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gest

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Chris

Bur

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GRC:

The

rmal

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ling

test

of

radi

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sub

-pan

els

Don

Jaw

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RC:

R

adia

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test

ing

Tim

Ubi

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velle

, SLI

/GRC:

PMC

mac

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ng &

tes

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fab

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hn, U

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PM

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.:

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o fo

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d co

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epre

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pane

l fab

ricat

ion

E. E

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in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

73

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ject

Mat

ter

Back

grou

ndPM

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iato

r Pa

nel D

esig

n &

Mat

eria

l Sel

ectio

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cesh

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Des

ign

and

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PMC

Perf

orm

ance

& F

easi

bilit

y Ev

alua

tion

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mal

con

duct

ivity

and

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mpo

site

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rack

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cuum

the

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agi

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hard

ness

PMC

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rap

co-c

ure

vs. 2

ndar

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alua

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mar

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d Fu

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k pl

an

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ugen

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in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

74

Bac

kgro

und

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ter I

cy M

oons

Orb

iter (

JIMO)

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lora

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er a

rea,

sig

nific

ant

mas

s dr

iver

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er r

ange

of

tem

pera

ture

s (2

00 –

550°

F)So

phis

ticat

ed d

eplo

ymen

t, p

ossi

bly

sim

ilar

to I

SS

PMC

with

hig

h th

erm

al c

ondu

ctiv

ity c

arbo

n fib

ers

(Coa

l tar

pitc

h-ba

sed

w/

up t

o 10

00 W

/mK)

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ighe

r po

tent

ial!

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ion

Surfa

ce P

ower

(FSP

)

E. E

ugen

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in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

75

Pol

ymer

Mat

rix

Com

posi

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PER

TIES

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h s

peci

fic

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fnes

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str

engt

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) Le

ast

expe

nsi

ve c

ompo

site

for

m(+

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ilora

ble

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, th

erm

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ity,

m

ech

anic

al p

rope

rtie

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) Es

tabl

ish

ed m

anu

fact

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ng

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(-)

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rabi

lity

insu

ffic

ien

tly

char

acte

rize

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oor

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ess

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ndu

ctiv

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(-)

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hly

an

isot

ropi

c pr

oper

ties

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) B

ondi

ng

chal

len

ges

w/

met

al H

P/H

T

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RT

Den

sity

(g

/cm

3)

--~1

~4

0

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s.

--1

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TE (μm

/mK

)

400

590

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ulu

s (G

Pa)

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2St

ren

gth

(G

Pa)

300

600

RT

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duct

ivit

y (W

/mK

)

0°±

30°

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alK

11

00

/pol

ymer

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10

0/p

olym

er6

0%

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er V

ol6

0%

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er V

ol

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S A

ND

CO

NS

PRO

S A

ND

CO

NS

DES

CR

IPTI

ON

DES

CR

IPTI

ON

Varie

ties o

f mat

erial

choi

ces;

fibe

rs, r

esin

sCo

mm

only

used

for s

pace

craf

t stru

ctur

al m

embe

rs an

d lo

wer t

empe

ratu

re ra

diat

ors

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rent

ly lo

w re

sin th

erm

al co

nduc

tivity

; bu

t im

prov

ed b

y the

use

of n

ano-

filler

s tra

nsfe

rabl

e to

cont

inuo

us fi

ber P

MCs?

Res

in G

lass

Tra

nsiti

on T

empe

ratu

res

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in G

lass

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nsiti

on T

empe

ratu

res

Toug

hene

d Ep

oxy

Toug

hene

d Ep

oxy

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ate

Cyan

ate

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rEs

ter

BMI

BMI

BMI

BMI

Poly

imid

ePo

lyim

ide Poly

imid

ePo

lyim

ide

300

350

400

450

500

550

600

650

Temp (K)

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

76

Bac

kgro

und

Tech

nolo

gy D

evel

opm

ent

Req

uire

d fo

r PM

CLo

w t

hru-

thic

knes

s th

erm

al c

ondu

ctiv

ityEf

fect

of

crac

king

def

ects

on

ther

mal

con

duct

ivity

Tem

pera

ture

lim

its f

or lo

ng-t

erm

app

licat

ion

Com

pone

nt s

peci

fic f

iber

arc

hite

ctur

e op

timiz

atio

nCo

mpo

nent

spe

cific

des

ign

data

and

fab

ricat

ion

expe

rienc

e

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

77

PM

C R

adia

tor

Pan

el D

esig

ns PMC

mat

eria

lH

T m

ater

ial;

Al,

SS, T

iH

T ra

dius

PMC

f/s

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knes

sA

dhes

ive

mat

eria

l

Sand

wich

Over

wrap

Bond

ed

PMC

mat

eria

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ddle

mat

rl&

des

ign

Adh

esiv

e m

ater

ial

Cor

e m

ater

ial &

type

Varia

bles

PMC

mat

eria

lH

T m

ater

ials

; Al,

SS, T

iA

dhes

ive

mat

eria

lA

dhes

ive

thic

knes

s

Bal

ance

of

ther

mal

per

form

ance

an

d st

ruct

ura

l in

tegr

ity

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

78

PM

C M

ater

ial S

elec

tion

Mat

rix m

ater

ials

:RS9

(Cy

anat

ees

ter)

, YLA

EX15

51 (

Cyan

ate

este

r), B

ryte

Cyco

m52

50-4

(Bi

smal

eim

ide)

, Cyt

ec

HFP

E-II

-52

(6-F

pol

yim

ide)

, Mav

eric

k

Pitc

h-ba

sed

carb

on f

iber

s: K

13D

2U (

Mits

ubis

hi)

and

K110

0 (A

moc

o/Cy

tec)

in 2

K to

w80

0~10

00 W

/mK

in-p

lane

vs.

~20

W/m

Kou

t-pl

ane

TC

Axia

l CTE

~ -

1.5

ppm

/°C;

elo

ngat

ion

to f

ailu

re <

0.4

%

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

79

PM

C F

aces

heet

Des

ign

–C

TE

mat

chin

g

PMC

f/s

lay-

up c

onfig

urat

ions

to

mat

ch C

TE o

f m

etal

HP/

HT

via

vario

us

anal

ytic

al s

olut

ions

bas

ed o

n la

min

atio

n th

eory

: [

0/15

/-15

] nfo

r al

umin

um

vs. [

0/25

/-25

] nfo

r st

ainl

ess

stee

l vs.

[0/

30/-

30] n

for

Tita

nium

-505101520253035

010

2030

4050

6070

80

Angl

e of

Off

Axis

Plie

s, α

90° CTE of PMC Laminate, ppm/°C

53%

FV, E

2=5G

Pa; U

DRI

53%

FV, E

2=12

GP

a; U

DRI

60%

FV, E

2=5G

Pa; U

DRI

60%

FV, E

2=9G

Pa; G

RC-

ICAN

60%

FV, E

2=12

GP

a; U

DRI

60%

FV, E

2=?;

ATK

53%

FV, E

2=?;

ATK

Hea

t Pip

e A

xis

= 90

°

10.9

5.7

12.7

19.3

10

5.4

15.8

9.9

11.4

17.1

5101520

2324

2526

2728

2930

3132

CTE

of H

P/H

TTi

=

~ 9

ppm

/°CSS

= ~

16 p

pm/°C

Al

= ~

24 p

pm/°C

Lay-

up C

onfig

urat

ion:

[0, +

α, -α

] 1S

HFP

E/K

1100

50%

FVF

RS9

D/K

1100

56%

FVF

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

710

PM

C F

aces

heet

Fab

rica

tion

Hot

-mel

t pr

epre

ggin

g (Y

LA);

12

”w

ide,

37w

% r

esin

, 67

gsm

FAW

0.

0025

inch

thi

ck a

fter

cur

e, 6

0 v%

FVF

tar

gete

d

Pane

l fab

(GRC

or C

anyo

n);

Han

d la

y-up

(12

”x12

”or

24”

x36”

or 3

6”x4

4”;

6-pl

y)

optim

ized

vac

uum

bag

ging

auto

clav

e cu

rew

/

C-sc

an a

nd Q

C te

stin

g (G

RC)

RS-

9D c

ure

Appl

y 28

in/H

g va

c&

80

psi P

Hea

t to

390

°F

@ 3

–5

°F/m

inH

old

at 3

90 °

F fo

r 12

7 m

inCo

ol t

o RT

@ ~

3°F

/min

Post

cure

at

600

°F f

or 4

hrs

fr

ee s

tand

ing

in a

ir

HFP

E-II

-52

cure

B-st

agin

g @

400

ºF f

or 1

hr

Post

cure

@ 7

00°F

for

16

hrs

in a

ir

0

10

0

20

0

30

0

40

0

01

20

24

03

60

48

06

00

72

08

40

96

0

Part Pressure, psi / Vacuum, inHg

Vacu

um

44

0m

in

65m

in

20

0m

in

0

10

0

20

0

30

0

40

0

50

0

60

0

70

0

80

0

01

20

24

03

60

48

06

00

72

08

40

96

0T

ime

, m

in

Part Temperature, ºF

14

0m

in

1.0

ºF/m

in

5.0

ºF/m

in

2.9

ºF/m

in

60

min

110

min

70m

in55

min

5.0

ºF/m

in

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

711

The

rmal

con

duct

ivit

y an

d N

ano-

com

posi

tes

-Mat

eria

l Sel

ecti

ons

Hig

h th

erm

al c

ondu

ctiv

ity n

ano

fille

rs s

tudi

ed;

Vapo

r gr

own

carb

on n

ano

fiber

s (V

GCN

F)--

-hi

gh

tem

pera

ture

gra

de:

PR24

HH

T, A

SIde

nsity

= ~

1.8

g/cc

, a t

ube

stru

ctur

e of

gra

phite

w/

varia

ble

mor

phol

ogy

and

dens

ities

Aver

age

diam

eter

= ~

100

nm (

10 n

m -

500

nm in

di

strib

utio

n), a

spec

t ra

tio =

~50

0

Exfo

liate

d gr

aphi

te f

lake

s (E

xGf)

---

exfo

liate

d by

UD

RI

pate

nted

pro

cess

RS-

9D C

yana

tees

ter

resi

n (Y

LA)

+ K

13D

2U C

-fib

er

(Mits

ubis

hi)

com

posi

te s

yste

m

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

712

130º

F

Dia

mon

d Po

lyU

nwin

d 4

Top

Pap

erT

ake-

up 2

Top

Pap

er L

et-O

ffU

nwin

d 3

Fabr

ic L

et-O

ffU

nwin

d 2

Bot

tom

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erLe

t-Off

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ind

1

Nip

s

Idle

rs

Idle

rs

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r

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ber

Rol

lSl

itter

s

Prod

uct

Win

d-up

Chill

Plat

eHo

t Plat

e

Hig

h C

onc.

PM

R-I

I-50

Mon

omer

Sol

utio

n (~

80%

)

64"

Rem

oval

of E

xces

s So

lven

t @ h

igh

Vac

uum

, ~12

0ºF

Roo

m te

mp.

Res

in a

mou

nt in

pre

preg

co

ntro

lled

by•g

ap b

etwe

en n

ip r

olle

rs•r

olle

r te

mpe

ratu

re•r

olle

r rp

m

130º

F

Dia

mon

d Po

lyU

nwin

d 4

Top

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erT

ake-

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Top

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er L

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nwin

d 3

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ic L

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ffU

nwin

d 2

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tom

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s

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rs

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itter

s

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uct

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t Plat

e

Hig

h C

onc.

PM

R-I

I-50

Mon

omer

Sol

utio

n (~

80%

)

64"

Rem

oval

of E

xces

s So

lven

t @ h

igh

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uum

, ~12

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Roo

m te

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Res

in a

mou

nt in

pre

preg

co

ntro

lled

by•g

ap b

etwe

en n

ip r

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olle

r te

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Nan

o fil

ler-

resi

n m

ixin

g, c

ompo

undi

ng (

20w

t% f

iller

) by

U

DRI/

Nan

oSpe

rse/

MRI

for

optim

um d

ispe

rsio

nU

ni-t

ape

PMC

prep

reg

by H

ot-m

elt

proc

ess

at Y

LA (

10w

t% f

iller

) co

mpo

site

pan

el f

abric

atio

n w

the

opt

imiz

ed c

ure

cycl

es a

t G

RC

(12”

x12”

) an

d Ca

nyon

(24

”x36

”)

YLA

P

repr

eggi

ng

Set-

up

The

rmal

con

duct

ivit

y an

d N

ano-

com

posi

tes

-Pro

cess

es

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

713

The

rmal

con

duct

ivit

y an

d N

ano-

com

posi

tes

-Pre

limin

ary

Res

ults

12-p

ly, [

0/+

30/-

30/-

30/+

30/0

] 1S

to m

atch

CTE

of

Ti h

eat

pipe

(H

P);

12”x

12”x

0.02

8”

Cure

d @

380

°F,

80p

si, 2

8 in

/Hg

vacu

um f

or 2

hrs

w/

optim

ized

bag

ging

Po

stcu

red

at 6

00 °

F fo

r 4

hour

s

C-sc

an N

DE

Stra

ight

resin

Resin

+ V

GCNF

(10w

t%)

Resin

+ VG

CNF

(5wt

%)

+ Ex

Gf(5

wt%

)

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

714

RS-

9D+V

GC

NF

/K13

D2U

RS-

9D/K

13D

2U

RS-

9D+V

GC

NF

+ Ex

Gf/K

13D

2U

Typi

cal S

EM m

icro

grap

hs o

f RS-

9D/K

13D

2U P

MC

in t

erm

s of

nan

o-m

odifi

catio

n sh

owin

g fib

er/f

iller

dis

trib

utio

n-co

nnec

tivity

and

def

ects

The

rmal

con

duct

ivit

y an

d N

ano-

com

posi

tes

-Pre

limin

ary

Res

ults

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

715

410

423

368

57.3

Stra

ight

resi

n

410

413

330

46.0

Res

in+V

GC

NF+

ExG

f40

841

130

954

.2R

esin

+VG

CN

F

Tan δ

G' o

nset

Td, °

C

(TG

A in

N2)

Tg, °

C (b

y D

MA

)F.

V.F

*, %

Pro

perti

esP

MC

Lam

inat

e ty

pe

* F.

V.F

was

det

erm

ined

by

optic

al im

age

anal

ysis

in K

eyen

ce h

igh

pow

er (

500x

) di

gita

l mic

rosc

ope

syst

em (

Not

e: n

ano

fille

r vo

lum

e co

unte

d in

res

in v

olum

e)

The

rmal

con

duct

ivit

y an

d N

ano-

com

posi

tes

-Pre

limin

ary

Res

ults

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

716

METZ

SCH

LFA

447 1.44

1.37

1.42

0.62

0.78

1.00

Z-di

r.47

5159

2029

4290

°20

624

029

988

138

212

1.34

1.00

0.81

1.75

0°

1.47

1.43

1.30

0.66

0.86

1.09

Z-di

r.37

4223

3590

°16

618

019

874

108

166

1.32

0.98

0.70

1.70

0°RS-

9D+V

GC

NF+

ExG

f/K13

D2U

lam

inat

e1.

511.

461.

360.

610.

791.

01Z-

dir.

4550

5618

2742

90°

213

223

241

8612

117

91.

451.

080.

791.

720°R

S-9D

+VG

CN

F/K

13D

2U la

min

ate

RS-

9D S

trai

ght/K

13D

2U la

min

ate

300 °

C15

0 °C

20 °C

300 °

C15

0 °C

20 °C

300 °

C15

0 °C

20 °C

g/cc

Cond

uctiv

ity, W

/mK

Diffu

sivity

, mm

2 /sec

Spec

ific h

eat c

apac

ity, J

/g °C

Dens

ity

* Th

erm

al d

iffus

ivity

by

Lase

r Fl

ash

Anal

ysis

(LF

A 44

7), Δ

Cp b

y m

DSC

, den

sity

by

dim

.

The

rmal

con

duct

ivit

y an

d N

ano-

com

posi

tes

-Pre

limin

ary

Res

ults

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

717

1.47

1.43

1.30

0.66

0.86

1.09

1.32

0.98

0.70

1.70

RS-

9D+V

GC

NF+

ExG

f/K13

D2U

lam

inat

e

Z-di

r.

1.44

1.37

1.42

0.62

0.78

1.00

Z-di

r.1.

341.

000.

811.

75

2.08

1.90

2.28

1.16

1.44

1.98

Z-di

r.1.

330.

980.

861.

34

HFP

E-II-

52 P

olyi

mid

e/K

13D

2U la

mia

nte

1.51

1.46

1.36

0.61

0.79

1.01

Z-di

r.1.

451.

080.

791.

72R

S-9D

+VG

CN

F/K

13D

2U la

min

ate

RS-

9D S

trai

ght/K

13D

2U la

min

ate

300 °

C15

0 °C

20 °C

300 °

C15

0 °C

20 °C

300 °

C15

0 °C

20 °C

g/cc

Cond

uctiv

ity, W

/mK

Diffu

sivity

, mm

2 /sec

Spec

ific h

eat c

apac

ity, J

/g °C

Dens

ity

The

rmal

con

duct

ivit

y an

d N

ano-

com

posi

tes

-Pre

limin

ary

Res

ults

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

718

Eff

ects

of

Mic

rocr

acks

-Pre

limin

ary

Res

ults

Ther

mal

spi

king

pre

cond

ition

ing

expe

rimen

ts (

Prai

rie V

iew

A&

M f

acili

ty)

RS-9

D/K

13D

2U:

[0/

30/-

30]1

s vs

[0/3

0/-3

0/-3

0/30

/0]1

s vs

[0/6

0/-6

0/-6

0/60

/0]2

s LN

2⇔

177

°C (

350°

F)D

ensi

ty o

f m

icro

crac

k

mea

sure

d, #

/mm

TC m

easu

rem

ents

in t

hru-

thic

knes

s di

rect

ion,

W/m

K

Obj

ecti

ve:

Det

erm

ine

effe

cts

of m

icro

crac

ks o

n t

her

mal

con

duct

ivit

y

1.93

7±0.

071.

975±

0.13

12-p

ly1.

404±

0.02

1.73

9±0.

1924

-ply

1250

cyc

les

0 cy

cle

7.0±

0.5

7.6±

1.9

6.9±

1.2

4.4±

1.7

24-p

ly6.

1±1.

45.

0±1.

43.

0±1.

812

-ply

1250

cyc

les

950

cycl

es75

0 cy

cles

450

cycl

es

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

719

Eff

ects

of

Mic

rocr

acks

-Cur

rent

Wor

k P

lan

RS-

9D/K

13D

2U v

s. R

S-9X

1 (V

GCN

F-PR

24H

HT)

/K13

D2U

vs

. RS-

9X2

(VG

CNF+

ExG

f)/K

13D

2U

Also

, eff

ects

of

nano

-mod

ifica

tion

on m

icro

crac

king

All 1

2-pl

y [0

/30/

-30/

-30/

30/0

]1s

Ther

mal

spi

king

pre

cond

ition

ing

expe

rimen

ts

(Pra

irie

View

A&

M f

acili

ty)

LN2 ⇔

up t

o 23

2 °C

(45

0°F)

, aut

omat

ed c

ycle

@ 4

cy

cles

/hr

up t

o 2,

000

cycl

es

TC m

easu

rem

ents

: 0

°an

d 90

°in

-pla

ne d

irect

ions

vs.

th

ru-t

hick

ness

dire

ctio

n

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

720

To a

sses

s PM

C sp

ace

dura

bilit

y by

the

acc

eler

ated

the

rmal

ag

ing

unde

r hi

gh v

acuu

m in

sim

ulat

ing

spac

e en

viro

nmen

tsTo

dow

n-se

lect

mos

t du

rabl

e PM

C ca

ndid

ate

syst

emTo

iden

tify

PMC

degr

adat

ion

mod

es a

nd m

echa

nism

s

232

-28

8~

349

C: R

S-9D

/K13

D2U

~ 3

1640

4B:

HFP

E/K1

100

~ 3

1639

0A:

HFP

E/K1

3D2U

>28

8~

371

F: R

S-9X

2 (V

GCN

F+Ex

Gf)

/K13

D2U

>28

8~

366

E: R

S-9X

1 (V

GCN

F)/K

13D

2U

232

-28

836

1D

: RS-

9D/K

1100

Max

. use

T, °

CD

ry T

g, °

CP

MC

Can

dida

tes

Vac

uum

The

rmal

Agi

ng

All

test

pan

els:

6-p

ly [0

, +30

, -30

] 1S

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

721

Vac

uum

The

rmal

Agi

ng-E

xper

imen

tal s

et-u

p

22

7 v

s 2

77

vs

31

6°C

(4

40

vs

53

1 v

s6

00

°F)

10

-6to

rrU

p to

10

,00

0 h

rs -

--0

; 5

0;

15

0;

25

0;

41

7 d

ays

Tota

l 4

8 3

"x3

"; 1

8 6

"x4

"; 1

8 4

"x6

" ar

ran

ged

for

radi

atio

n h

eat

ΔW

t, T

g, T

d, C

p, C

TE, T

C, F

VF,

voi

d co

nt,

FT-

IR, d

amag

e ev

olu

tion

, an

d ax

ial &

tra

nsv

erse

ten

sile

pro

pert

ies

to b

e m

onit

ored

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

722

Vac

uum

The

rmal

Agi

ng-I

niti

al R

esul

ts

PMC

Cou

pon

Tem

pera

ture

s (4

)-Vac

uum

Log

0

100

200

300

400

500

600

010

0020

0030

0040

0050

00Ag

ing

time,

hrs

Temperature, °F

02468101214

Vacuum, x 10E-6 torr

50-d

aysh

ut d

own

150-

day

shut

dow

n Re

pair

shut

dow

n -7-6-5-4-3-2-10

050

010

0015

0020

0025

0030

0035

0040

00

Agin

g Ti

me,

hrs

% Weight Change

HFP

E/k

13D

2U

HFP

E/K

1100

RS9

D/K

13D

2U

RS9

D/K

1100

RS9

X1/K

13D

2U

RS9

X2/K

13D

2U

Sign

ifica

nt o

utga

ssin

g fr

om C

yana

tees

ter

syst

ems

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

723

RS-

9##/

K13

D2U

com

posi

tes,

6-p

ly [0

, +30

, -30

] 1S

pane

ls

5678910 Modulus, GPa

Stra

ight

Re

sinVG

CNF

mod

ified

VGCN

F+Ex

Gf

mod

ified

+11%

+0.3

%

30405060 Strength, MPa

Stra

ight

Re

sinVG

CNF

mod

ified

VGCN

F+Ex

Gf

mod

ified

+16%

+3%

0.5

0.6

0.7

0.8

0.9

1.0

Strain-to-failure, %

Stra

ight

Re

sinVG

CNF

mod

ified

VGCN

F+Ex

Gf

mod

ified

+19%

+24%

Tran

sver

se (9

0°) T

ensi

le P

rope

rties

(Not

nor

mal

ized

by

F.V

.F)

Bas

elin

e co

ntro

l at R

T @

t=0

Vac

uum

The

rmal

Agi

ng-I

niti

al R

esul

ts

Posi

tive

effe

cts

of n

ano-

mod

ifica

tions

on

mec

hani

cal p

rope

rty

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

724

Bas

elin

e co

ntro

l pro

perti

es a

t RT

@ t=

0(T

ested

by M

ateria

l Inno

vatio

ns In

c (MI

I); N

ot no

rmali

zed b

y F.V

.F)

RS-

9D+V

GC

NF+

ExG

f/ K

13D

2U la

min

ate

RS-

9D+V

GC

NF/

K

13D

2U la

min

ate

RS-

9D S

trai

ght/

K13

D2U

lam

inat

e

PMC

Lam

inat

e typ

e and

test

dire

ctio

n

1.2

1.2

1.3

Z-di

r.84

8891

90°

300

322

345

0°

2.1

2.2

2.2

Z-di

r.77

7983

90°

281

297

322

0°1.

61.

71.

7Z-

dir.

8890

9390

°30

432

634

60°

150

°C10

0 °C

30 °C

Con

duct

ivity

*, W

/mK

*MII

inte

rnal

Ste

ady

Stat

e Th

erm

al C

ondu

ctiv

ity M

etho

d

Vac

uum

The

rmal

Agi

ng-I

niti

al R

esul

tsR

S-9#

#/K

13D

2U c

ompo

site

s, 6

-ply

[0, +

30, -

30] 1

Spa

nels

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

725

PM

C R

adia

tion

Har

dnes

s

Hig

h en

ergy

rad

iatio

n ca

n le

ad t

o ch

ain

scis

sion

(so

ften

ing)

or

cros

s-lin

king

(ha

rden

ing)

in p

olym

ers

Elec

tron

Bea

m (β

part

icle

) is

a c

ost

effe

ctiv

e &

saf

e w

ay t

o su

rvey

the

rad

iatio

n se

nsiti

vity

of

mat

eria

ls &

com

pone

nts

PMCs

exp

osed

to

20, 2

00, &

400

Mra

dfr

om 4

.5 M

eVe-

beam

A:H

FPE/

K13D

2U, C

:RS-

9D/K

13D

2U, F

:RS-

9X (

VGCN

F+Ex

Gf)

/K13

D2U

Expo

sure

led

to n

o m

easu

rabl

e w

eigh

t lo

ss, a

goo

d in

dica

tion

that

th

ere

was

no

sign

ifica

nt c

hang

es in

che

mis

try

Oth

er e

valu

atio

ns (

e.g.

, Tg,

Td,

Cp,

CTE

, TC,

axi

al &

tra

nsve

rse

tens

ile

prop

ertie

s, F

VF, a

nd v

oid

cont

ent

etc)

are

und

erw

ay

PMC

A-0

.046

±0.

053

-0.1

06±

0.19

0-0

.013

±0.

086

C0.

131

±0.

102

0.01

9±

0.31

00.

194

±0.

218

F0.

053

±0.

112

-0.0

89±

0.38

60.

134

±0.

208

200

Mra

d40

0 M

rad

20 M

rad

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

726

PM

C R

adia

tor

Sub

-Pan

el F

abri

cati

on-O

verw

rap

Con

cept

: Co-

cure

d

Bene

fits:

Larg

er c

onta

ct a

rea

to H

T/H

P, t

hus

mor

e ef

ficie

nt h

eat

tran

sfer

Mor

e ro

bust

str

uctu

re, b

ette

r pr

otec

ted

HT/

HP

Chal

leng

es:

Britt

lene

ss o

f pi

tch-

base

d C-

fiber

s, li

mite

d be

nd r

adiu

s of

2.0

inch

?Po

tent

ially

hea

vier

wei

ght

pena

ltyG

reat

er C

TE m

ism

atch

bet

wee

n H

T/H

P an

d f/

sin

tra

nsve

rse

dire

ctio

nVa

cuum

bag

ging

and

cur

e co

nditi

ons

optim

ized

to

min

imiz

e re

sin

sque

eze-

out

and

to r

educ

e CT

E m

ism

atch

Cure

@ 1

77°C

for

3 h

rs, t

hen

post

cure

d @

204

°C f

or 6

hrs

RS-

9D/K

13D

2U P

MC

f/s

Alu

min

um H

TH

T ra

dius

?PM

C f/

sTh

ickn

ess?

RS-

4A fi

lm A

dhes

ive

CTE

mism

atch

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

727

PM

C R

adia

tor

Sub

-Pan

el F

abri

cati

on-O

verw

rap

Con

cept

: Co-

cure

d[0

/15/-1

5/0]–

HT(R

1.75”

)–[0

/15/-1

5/0]

[0/15

/-15/0

] 1S–H

T(R1

.5”)–

[0/15

/-15/0

] 2S

IR T

herm

o-gr

aphs

; Da

rker

area

slo

wer c

oolin

g cr

acks

, dela

m,

or d

ebon

ding

etc.

Crac

ks d

ue t

o CT

E m

ism

atch

, not

by

HT

curv

atur

e si

nce

both

sid

e cr

acke

dPo

or b

ondi

ng d

ue t

o la

ck o

f re

sin

+

CTE

mis

mat

ch

Crac

ks o

n fr

ont

8-pl

y f/

s, a

lso

dela

min

ated

and

/or

debo

nded

16

-ply

Cr

ack-

free

and

goo

d bo

ndin

g!Rol

e of

HT

curv

atur

e?

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

728

PM

C R

adia

tor

Sub

-Pan

el F

abri

cati

on-O

verw

rap

Con

cept

: Co-

cure

d[0

/15/-1

5/0] 2S

–HT(

R1.5”

)–[0

/15/-1

5/0] 1S

[0/15

/-15/0

] 2S–[

RS4A

] 2-HT(

R1.0”

)–[R

S4A]

2-[0/1

5/-15

/0]2S

Cure

d

Pos

tcur

edCu

red

P

ostc

ured

No

crac

ks o

n 16

-ply

des

pite

of

curv

atur

e,

but

debo

nded

aft

er P

C du

e to

cur

vatu

re

Crac

ks o

n 8-

ply

due

to C

TE m

ism

atch

, an

d lo

caliz

ed d

elam

and/

or d

ebon

ding

Thin

sin

gle

crac

k on

bot

h 16

-ply

f/s

Addi

tiona

l cra

ck &

loca

lized

del

am/d

ebon

daf

ter

PC o

n fr

ont

f/s

due

to c

urva

ture

Stro

ng/r

igid

adh

esiv

e bo

nd c

ause

d gr

eate

r CT

E m

ism

atch

?

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

729

PM

C R

adia

tor

Sub

-Pan

el F

abri

cati

on-A

dhes

ive-

Bon

ding

Con

cept

Bene

fits:

Easi

er f

abric

atio

n, L

ight

er, a

nd g

ood

man

ufac

tura

bilit

y

Chal

leng

es:

Thru

-thi

ckne

ss t

herm

al c

ondu

ctiv

itySt

rong

and

rob

ust

bond

ing

Vacu

um b

aggi

ng a

nd c

ure

cond

ition

s (a

utoc

lave

) op

timiz

ed t

o m

inim

ize

resi

n sq

ueez

e-ou

t an

d to

red

uce

CTE

mis

mat

ch

PMC

f/s

cure

d @

193

°C f

or 2

hrs

st

and.

Sur

face

pre

p H

T bo

nded

&

cure

d @

177

°C f

or 3

hrs

al

lpos

tcur

ed @

204

°C f

or 6

hrs

RS-

9D/K

13D

2U P

MC

f/s

HT

mat

eria

ls: S

S vs

. Al

RS-

4A fi

lm A

dhes

ive

(0.0

31 p

sf)

Adh

esiv

e th

ickn

ess?

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

730

PM

C R

adia

tor

Sub

-Pan

el F

abri

cati

on-A

dhes

ive-

Bon

ding

Con

cept

SS H

T-[R

S4A]

1-[0/2

5/-25

/0]1S

Cure

d-po

stcu

red

pane

ls

No

visu

al d

amag

e on

PM

C f/

san

d re

ason

able

bon

ding

reg

ardl

ess

of H

T ty

pe o

r bo

ndlin

e th

ickn

ess

3-la

yer

adhe

sive

m

ore

resi

n fil

let

form

ed a

t H

T ed

ges

SS H

T-[R

S4A]

3-[0/2

5/-25

/0]1S

AL H

T-[R

S4A]

3-[0/2

5/-25

/0]1S

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

731

PM

C R

adia

tor

Sub

-Pan

el F

abri

cati

on-T

herm

al P

erfo

rman

ce: 4

3°C

⇔-1

53°C

, 10-

20 c

ycle

sSS

HT-

[RS4

A]1-[

0/25/-

25/0]

1S

SS H

T pa

nels

und

er s

ever

er t

herm

al c

yclin

g 1-

laye

r ad

hesi

ve f

aile

d,

but

3-la

yer

surv

ived

w o

nly

edge

deb

ondi

ng10

0% a

dhes

ive

failu

re o

n PM

C f/

sU

nder

con

trol

led

rate

, AL

HT

w 3

-laye

r ad

hesi

ve s

urvi

ved

20+

cyc

les

SS H

T-[R

S4A]

3-[0/2

5/-25

/0]1S

AL H

T-[R

S4A]

3-[0/2

5/-25

/0]1S

Heat

ing/

cool

ing

rate

not

cont

rolle

d10

°C/m

in

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

732

PM

C R

adia

tor

Sub

-Pan

el F

abri

cati

on-H

T-P

MC

bon

ding

eva

luat

ion

Sub-

pane

l to

be s

ectio

ned

into

~0.

6”w

ide

test

cou

pons

−Bo

th o

verw

rap

and

adhe

sive

-bo

nded

pan

els

−O

ptim

ized

sec

tioni

ng w

/ a

low

sp

eed

diam

ond

saw

not

to

dam

age

bond

line

Test

ed in

lap-

shea

r m

ode;

Te

st f

ixtu

res

desi

gned

and

fa

bric

ated

Test

ed a

t RT

and

177°

C (3

50°F

)

Back

ing

plat

e (S

teel

)w

/ gr

it bl

aste

d fin

ish

Adhe

sive

Har

dene

d th

read

ed r

od

Low

er g

rip p

late

(St

eel)

Hol

ding

pla

te (

Stee

l)

R2.

0″

1.0″

1.5″

1.25

″

1.5″

1.0″

0.75

″0.5″

0.2″

thic

k

0.2″

thic

k

Test

cou

pon

(6”

x 0.

6”)

1.0″

2.0″

2.0″

PMC

HT

(ove

rwra

pped

or b

onde

d

Back

ing

plat

e (S

teel

)w

/ gr

it bl

aste

d fin

ish

Adhe

sive

Har

dene

d th

read

ed r

od

Low

er g

rip p

late

(St

eel)

Hol

ding

pla

te (

Stee

l)

R2.

0″

1.0″

1.5″

1.25

″

1.5″

1.0″

0.75

″0.5″

0.2″

thic

k

0.2″

thic

k

Test

cou

pon

(6”

x 0.

6”)

1.0″

2.0″

2.0″

PMC

HT

(ove

rwra

pped

or b

onde

d

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

733

Sum

mar

yD

esig

n an

d ca

ndid

ate

mat

eria

l sel

ectio

n w

ere

mad

e fo

r PM

C ra

diat

or

deve

lopm

ent;

an

d de

sign

and

fab

ricat

ion

of P

MC

f/s

pane

ls w

ere

com

plet

ed

Nan

o-co

mpo

site

s w

/ tw

o co

nduc

tive

nano

fill

ers

wer

e ev

alua

ted

for

TC

enha

ncem

ent,

but

the

impr

ovem

ent

was

ver

y lim

ited

yet

Perf

orm

ance

and

dur

abili

ty e

valu

atio

ns o

f PM

C f/

sin

clud

ing

vacu

um t

herm

al

agin

g, r

adia

tion

hard

ness

, and

mic

rocr

ack-

TC r

elat

ion

wer

e in

itiat

edFo

r ov

erw

rap

conc

ept,

the

rad

ius

of H

T cu

rvat

ure

shou

ld b

e gr

eate

r th

an 4

.45

cm

(1.7

5 in

).

PMC

face

shee

t sh

ould

be

16 p

lies

or h

ighe

r on

bot

h fr

ont

and

back

si

de o

f th

e H

T ov

erw

rap

sect

ion.

The

n, w

eigh

t sa

ving

con

cern

? M

icro

slo

ts o

r ho

les

to r

educ

e w

eigh

t of

HT

Com

bina

tion

of o

verw

rap

and

adhe

sive

bon

ding

is s

till p

ursu

able

opt

ion,

but

m

ore

duct

ile/s

oft

adhe

sive

sys

tem

s w

ith r

easo

nabl

e bo

nd s

tren

gth,

goo

d th

erm

al

cond

uctiv

ity, a

nd h

igh

tem

pera

ture

cap

abili

ty, e

.g.,

cond

uctiv

e na

no-m

odifi

ed

silic

on b

ased

adh

esiv

e w

ould

be

mor

e su

itabl

e fo

r th

e ap

plic

atio

n?Fo

r th

e ad

hesi

ve-b

ondi

ng c

once

pt, t

he R

S-4A

Cya

nate

este

r fil

m a

dhes

ive

perf

orm

ed w

ell f

or b

oth

SS a

nd A

l HT

with

RS-

9D/K

13D

2U P

MC

f/s.

Thic

ker

adhe

sive

laye

r, ~

0.04

cm

(0.

016

in),

was

rec

omm

ende

d fo

rth

e ad

hesi

ve-

bond

ing

optio

n ba

sed

on t

herm

al p

erfo

rman

ce, a

nd s

izab

le r

esin

fill

et f

orm

ed a

t th

e ed

ges

of H

T w

ould

impr

ove

bond

ing

inte

grity

HT-

PMC

f/s

bond

ing

inte

grity

will

be

quan

titat

ivel

y ev

alua

ted

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

734

Futu

re W

ork

Pla

n

Com

plet

e va

cuum

the

rmal

agi

ng a

t al

l thr

ee T

sCo

mpl

ete

mic

rocr

ack-

TC r

elat

ions

Com

plet

e bo

nd s

tren

gth

eval

uatio

n D

own-

sele

ct a

nd o

ptim

ize

mat

eria

l, de

sign

and

pr

oces

s D

evel

op f

abric

atio

n-m

anuf

actu

ring

spec

ifica

tions

for

a

full-

size

com

pone

nt s

cale

PM

C ra

diat

or p

anel

sCo

ntin

ue n

ano-

mod

ifica

tion

for

thru

-thi

ckne

ss T

C im

prov

emen

t ba

sed

on “

cock

tail

Des

ign”

appr

oach

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

735

Max

imiz

e/op

timiz

e th

e th

ru-t

hick

ness

the

rmal

con

duct

ivity

of

cont

inuo

us f

iber

re

info

rced

PM

C, s

peci

fical

ly f

ocus

ing

onSy

ner

gist

ic c

hem

ical

, ph

ysic

al, a

nd

stru

ctu

ral m

odif

icat

ion

s fr

om

mol

ecu

lar

leve

l to

nan

o, m

icro

, an

d m

acro

sca

les

incl

udi

ng,

Sele

ctio

n of

hig

h TC

con

stitu

ent

Mat

eria

ls,

Mol

ecul

ar m

odifi

catio

ns o

f m

atrix

res

in s

yste

m

Hig

h TC

fill

er r

einf

orce

men

t bu

t vi

a co

ckta

il de

sign

fro

m n

ano

to m

acro

sca

le t

o m

axim

ize

conn

ectiv

ity/a

rchi

tect

ural

inte

ract

ions

Fille

r lo

adin

g ra

tio o

ptim

ized

in t

erm

s of

con

nect

ivity

, pro

cess

abili

ty, a

nd w

eigh

t/de

nsity

co

ntro

l

Mat

eria

l-pro

cess

sel

ectio

n ba

sed

on p

erfo

rman

ce p

redi

ctio

n/th

eore

tical

mod

elin

gO

ptim

izin

g m

ater

ial p

roce

ssin

g (m

ixin

g/di

sper

sing

) an

d st

ruct

ure

(des

ign

and

fabr

icat

ion)

O

ptim

izin

g fil

ler

surf

ace

trea

tmen

t fo

r im

prov

ed w

ettin

g an

d bo

ndin

g w

/ m

atrix

re

sin

Mul

ti-fu

nctio

naliz

atio

n; in

add

ition

to

high

TC,

impr

ove

elec

tric

al c

ondu

ctiv

ity a

nd

EMI

shie

ldin

g as

wel

l as

good

mec

hani

cals

Futu

re W

ork

-“C

ockt

ail D

esig

n”A

ppro

ach

E. E

ugen

e Sh

in, 2

7th

Hig

h T

empl

e W

orks

hop

Feb

12-1

5, 0

736

Coc

ktai

l Mod

ifica

tion

Con

cept

for

Z-

Ther

mal

Con

duct

ivity

Impr

ovem

ent

Dim

ensi

ons

Fibers:

K13

D2U

or K

1100

: ~10

µm

dia

M40

J &

M60

J: 5

µm

dia

Matrix:

Mol

ecul

ar m

odifi

catio

ns fo

r hig

h TC

; Ep

oxie

s, C

yana

tees

ters

, Pol

yim

ides

Fillers:

Met

al F

lake

s/Fi

bers

/Sph

eres

(MF)

etc

:~

1 m

m L

x ~

0.5

mm

W x

~25

µm

Th

Cho

pped

Fib

ers

(CF)

: 3

–5

µm Ø

x ~

50 µ

m L

Car

bon

Bla

cks

(CB

): ~

3 –

8 µm

ØEx

folia

ted

Gra

phite

Fla

kes

(EG

f):

~ 30

µm

L x

~ 1

0 µm

W x

sub

-µm

Th

Car

bon

Nan

o Fi

ber (

CN

F):

~ 0.

02 µ

m Ø

x ~

5 -1

0 µm

LN

ano-

part

icul

ates

(NP;

met

allic

/cer

amic

): ~

10 –

100

nm Ø

e.g.

, Com

posi

te w

/ 60

% F

VF+

tot

al u

p to

20

wt%

Fill

er lo

adin

g

CB

CN

F

EG

f

CF

orM

F

NP

Opt

imiz

e fi

ller

load

ing

rati

os, s

hap

e fa

ctor

s, a

nd

tota

l am

oun

t in

ter

ms

of

ther

mal

con

duct

ivit

y, p

roce

ssab

ility

, an

d co

mpo

site

per

form

ance

an

d pr

oper

ties

Futu

re W

ork

-“C

ockt

ail D

esig

n”A

ppro

ach