FIBRE ARCHITECTURE DESIGN,

PROCESSING AND TESTING OF HIGH

TEMPERATURE COMPOSITES

BY

SHINGADE VIJAYRAJ N., Sc’D’

HIGH TEMPERATURE COMPOSITES CENTRE

ADVANCED SYSTEMS LABORATORY, HYDERABAD
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What is Composite ?

 Tailored heterogeneous compound

material in which two or more than
material come together to form a structure
for a specific application.

 Consisting binder (matrix) and the

reinforcement fibres.

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 Basic difference between a Composite &
an Alloy

COMPOSITES ALLOYS

 MIXTURE OF MOSTLY NON  MIXTURE OF MOSTLY

METALS WITH NON METALS / METALS WITH METALS / NON
METALS. METALS.

 ANISOTROPIC  ISOTROPIC

 MACROSCOPICALLY  MACROSCOPICALLY
HETEROGENEOUS HOMOGENEOUS

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Classification of Composites

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Types of Composites

 Reinforcement

 Matrix binder

 Temperature capability

 Application

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 Types of Composites …

 Polymer Matrix Composites (PMC) 350O°C

 Metal Matrix Composites (MMC)

280O°C
 Ceramic Matrix Composites (CMC)
120O°C
 Ultra High Temp. Composites (UHTC)

 Carbon Carbon Composites (CCC)

800°C

350°C

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 Types of Composites …
CERAMICS
> 1000°C
CARBON

USE TEMPERATURE RANGES DEG. C

CMC
CMC CARBON-CARBON 3000 CARBON
3500 °C
SiC-SiC
1400
Si3N4/SiC

MCC
PPM
PO

MM
LS C

MC
L
< Y ME TA NiAl Ni-ALLOYS

M
M 800 °
E 1200

C
35
0 RS 400
- LAS/SiC
°C 1000
TiAl

DENSITIES 800
SiC FRG
Ti-ALLOYS
5.00 600
UHTC Al-ALLOYS
DENSITY (gm/cc)

4.00 CMC 400

MMC CPRP
200
3.00 0 2 4 6 8 10

PMC CCC DENSITY g/cm 2

2.00 THERMAL PROTECTION SYSTEMS

TPS
1.00
PASSIVE TPS ACTIVE TPS
0.00 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 • HOT STRUCTURES
C/POLYIMIDES C/Ti C-SiC SiC/ZrB2-SiC C/C CAPABLE OF
QUARTZ/SILICONE C/Al SiC/SiC CARRYING LOADS
C /PHENOLIC SiC/Ti SiO2/SiO2 • TPS FOR LOAD
BEARING VEHICLES
SiC/Al 7/51
 Types of Composites …

SINGE SHOT USE RE USABLE

• THERMO-STRUCTURAL • THERMO-STRUCTURAL
INTEGRITY INTEGRITY
• REUSABILITY
• THERMAL SHOCK
• SAFE ATTACHMENT
• SHAPE STABILITY SCHEMES
• LOW MAINTENANCE
• LIGHT WEIGHT
• LIGHT WEIGHT

HIGH SPEED FLIGHT ENVIRONMENT

CARBON FIBRES
10000 • EXTREME TEMPERATURES
( HOT AND COLD )
SiC/SiC
1000 • LOCALISED HEATING DURING
CARBON-CARBON
TENSILE STR N/mm2

FLIGHT MANEUVERS
100 K/E C/E
CARBON PHENOLIC • THERMALLY INDUCED STRESSES
• HIGH AERODYNAMIC, ACOUSTIC
LOADS/ SEVERE VIBRATION
100 200 300 400 500 1000 2000 3000

TEMPERATURE (°C)
• MATERIAL EROSION

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Composites in Missiles / Space Applications
AGNI

NAG

PRITHVI

BRAHMOS
TRISHUL

AKASH

INTERCEPTOR LAUNCH VEHICLE

MISSILE
9/51
 Composites in Aerospace Applications
5 – 6 % of airframe is composite
45% of air frame is Composites • Radome
• Fuselage
• Wings
TEJAS • FIN/ Rudder
• Drop Tanks
22,000 Parts Vs 8,000 Parts • C/C Brake Discs
SARAS

DROP TANKS- LCA ALH

85-90%of air frame

is composites HANSA
DHRUV
AIRBUS A380 BOEING 787

50% composite
25% composite • ALL COMPOSITE FUSELAGE
• ELIMINATION OF 50,000 FASTENERS 10/51
 High Temp. Composites for Aerospace & Defence
• EXTREME TEMPERATURES
MATERIAL AND STRUCTURES
( HOT AND COLD )
• LOCALISED HEATING DURING
FLIGHT MANEUVERS •• PERFORMANCE
PERFORMANCE
• THERMALLY INDUCED STRESSES •• RELIABILITY
RELIABILITY
• HIGH AERODYNAMIC, ACOUSTIC
•• COST
COST EFFECTIVENESS
EFFECTIVENESS
LOADS/ SEVERE VIBRATION
• MATERIAL EROSION SPACE SHUTTLE

SRE
HSTDV
DRDO
RLV- TD

ISRO
Bold major development
Ballistic reentry in the technology of
AGNI-V
Ballistic maneuvering re-entry human space flight
Orbital maneuvering re-entry
11/51
 High Temp. Composites in Indian Systems
TEJAS SUKHOI

C/C BRAKE DISCS NOSETIP

RECS
JET VANE

ENDO
INTERCEPTOR HSTDV
CC THROAT / NOZZLES 12/51
 Composites in Indian Systems

Lattice Cylinder
Flex Nozzles

Radomes
Drop Tanks

Composite Rocket Motor Casing Composite Canister 13/51

All Carbon Composite Re-entry Vehicle

RVS NOSETIP

THERMAL TESTS
MULTI-DIRECTIONAL
C- C COMPOSITES

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CARBON CARBON
COMPOSITES

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 Structure of Carbon

GRAPHITE
DIAMOND
HEXAGONAL UNIT CELL
FULLERENE

EFFECT OF HEAT TREATMENT

ON CARBON STRUCTURE
GRAPHITIZING PARTLY
GRAPHITIZING °C

GLASSY CARBON

CARBON FIBERS
16/51
 Carbon Fibres

 Fibrous carbon materials with carbon content

more than 90%.
 Transformed from organic matter by heat
treatment @ 1000° - 1500° C.
 First commercially produced carbon fibre for
incandescent lamp filament from cellulose precursor
in 1879 by Thomas Alva Edison.

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 Carbon Fibres …

 Precursor : Any fibrous material with carbon as

back bone which would yield carbonaceous residue
upon heat treatment.

 Viscose Rayon (Cellulose)

 Pitch
 PAN (Poly Acrylo Nitrile)

18/51
 Carbon Fibres (Manufacturing)

Polymerization
Acrylo Nitrile Spinning PAN fibres

HS fibre Pyrolysis Stabilization

1500°C 200 – 300°C
N2, Ar, HCl Air, Tension

Post Heat Treatment HM Carbon Fibres

> 2500°C
CrO, MgO2, VO2

19/51
 Carbon Fibres & Fabric

Untwisted Fibre Bundle

Woven roving Plain Weave 8HS Weave

Twisted Fibre Bundle

Knitted fabric Braided fabric

Continuous Chopped strand
strand roving 20/51
 Basic Fibre Architecture Design

1-D (Unidirectional) 3-D (Orthogonal) 3-D (Cylindrical)

2-D (Bidirectional) 4-D (In Plane) 4-D (Pyramidal)

21/51
 Multidirectional Fibre Architecture

SALIENT FEATURES
 NEAR ISOTROPY
 DELAMINATION FREE
 LOWER THERMAL STRESSES
 SHAPE STABILITY
 LOW & UNIFORM EROSION

 WEAVE CONFIGURATION
 WEAVE SPACINGS
 UNIT CELL VOLUME
 FIBRE VOLUME FRACTION

22/51
 Carbon Carbon Composites

CARBON FIBRE
REINFORCEMENTS

CARBON-CARBON
COMPOSITES
CARBON MATRIX

CARBON FIBRE CARBON MATRIX

• PAN BASED • PITCHES
• RAYON BASED • RESINS
• PITCH BASED • HYDROCARBON GASES
23/51
 Important Properties of Carbon Carbon
Composites

• HIGH SPECIFIC STRENGTH AND MODULUS

• RETENTION OF MECHANICAL PROPERTIES
AT ELEVATED TEMPERATURES
• HIGH SPECIFIC HEAT
• HIGH THERMAL CONDUCTIVITY & LOW THERMAL
EXPANSION. HENCE GOOD RESISTANCE TO THERMAL SHOCK
• BIO-COMPATIBILITY, FATIGUE, CORROSION
AND WEAR RESISTANCE
• GOOD AND STABLE FRICTIONA CO-EFFICIENT
• TAILORABILITY TO SUIT SPECIFIC APPLICATIONS

24/51
 Carbon Composites Fabrication
Acrylonitrile
(Petroleum product)
Polymer Synthesis
Polyacrylonitrile (PAN)
Process Technology
Spinning
Special Acrylic Fibre (SAF)
Process Technology Process Technology
Carbonisation Carbonisation
Carbon Fibre
Various T800-grade T300-grade
Chemicals
Formulated Woven Cloth
Resin
+ Resin
Process Technology
Impregnation Prepreg Filament
Winding

Carbon Fibre Composites

25/51
 Carbon Carbon Composites Fabrication
PIERCING INSERTION OF
BY NEEDLE PULTRUDED RODS

LOOM PLATE

CARBON FABRIC
STACK
3D ARCHITECTURE
330

MOULD TOOL
250

4D PREFORM

3D STITCHED
PREFORM

3D RECS for A2 3D C/C

BRAKES for
4D NOSE TIP for AGNI SUKHOI NOZZLE 26/51
 Carbon Carbon Composites Processing
PRECURSOR CARBON FIBRE / FABRIC
FIBRE

REINFORCEMENT (2D, 3D, 4D, .. nD )

PRECURSOR
MATRIX RESIN PITCH HYDROCARBON

IMPREGNATION IMPREGNATION CHEMICAL VAPOUR

n times
INFILTRATION (CVI)

PROCESS CARBONIZATION CARBONIZATION MACHINING

HIGH TEMPERATURE HEAT TREATMENT

PRODUCT CARBON CARBON COMPOSITES 27/51

 Carbon
CARBON- Carbon
CARBON Composites
PROCESSING Processing
TECHNOLOGIES
MULTIDIRECTIONAL DENSIFICATION
RIGIDIZATION
CARBON FIBRE WEAVING
IMPREGNATION
REINFORCEMENT
I M/C
HS, HM, IM, UHM
HIP,
FORMS CARBONISATION
MOULDING 800 °C, 1000 BARS
TOW FABRIC, 1000°C
FELT, CSM, MF GRAPHITIZATION
2750 °C
MULTIPLE CYCLES
MATRIX
PRECURSORS
* RESIN FINAL PRODUCT
* PITCH

IMPREGNATOR

CARBONISER GRAPHITIZER

HIP
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 C/C EXTENDIBLE
NOZZLE EXIT CONE
(ENEC) TECHNOLOGY

29/51
 ENEC : Introduction

ENEC IS THE STATE-OF-

THE-ART TECHNOLOGY

FOR EXPANDING EXHAUST

GASES TOWARDS HIGH

EXIT VELOCITIES AT HIGH

ALTITUDE

30/51
 ENEC : Concept

FIXED
FIXEDNOZZLE
NOZZLEINCREASES….
INCREASES….

----TOTAL
TOTALVEHICLE
VEHICLELENGTH
LENGTH

---- VEHICLE
VEHICLEBENDING
BENDINGMOMENT
MOMENT

---- INTERSTAGE
INTERSTAGESTRUCTURE
STRUCTUREWEIGHT
WEIGHT

ADVANTAGES
ADVANTAGESOF
OFENEC
ENEC

 HIGHER
HIGHERAREA
AREARATIO
RATIOAT
ATHIGH
HIGHALTITUDE.
ALTITUDE.

 INCREASE
INCREASEIN
INSPECIFIC
SPECIFICIMPULSE.
IMPULSE.

 REDUCING
REDUCINGTHE
THEOVERALL
OVERALLVEHICLE
VEHICLELENGTH
LENGTH&&
WEIGHT
WEIGHTOF
OFUPPER
UPPERSTAGE
STAGEOF
OFSPACE
SPACEVEHICLE
VEHICLE&&MISSILES
MISSILES

31/51
 ENEC : Prototype Configuration

RETAINER COMPLIANCE MOVABLE

CP LINER RING FIXED RING CONE
CONE

THROAT

BACKUP RING

METAL ACTUATORS
DOME

32/51
 ENEC : Density & Process selection

C/C COMPONENT DENSITY REQ. PROCESS

(g/cc) ROUTE
4D THROAT INSERT 1.9 HIPIC

3D FIXED & MOVABLE NOZZLES 1.6 I + C +G

2D LATCHING FINGERS 1.9 HIPIC

2D THROAT BACKUP RING 1.6 HIPIC

NPP M6 FASTENERS 1.9 HIPIC

33/51
 ENEC : Product development
V
4D THROAT INSERT W

 NEAR ISOTROPY Z

1.8
 LOW EROSION U

 SHAPE STABILITY CIRCULAR 2.07

ROD CARBON FIBRE

4D CONFIGURATION
350

320
MACHINED
THROAT INSERT
4D CARBON PREFORM 4D C/C DENSIFIED BILLET
34/51
 ENEC : Product development…

3D C/C NOZZLES
 NEAR NET SHAPE
 HIGH IN PLANE SHEAR
 DELAMINATION FREE Stitching Thread Border Thread

 LOW EROSION
3D FIBRE
ARCHITECTURE
Fabric Lay Up

3D STITCHED PREFORM 3D C/C FIXED NOZZLE 3D C/C MOVABLE NOZZLE

35/51
 ENEC : Product development…

2D C/C THROAT BACKUP 2D C/C LATCHING FINGERS

 LOW THERMAL CONDUCTIVITY  HIGH STRENGTH
 LOW DENSITY  DELAMINATION FREE
 DELAMINATION FREE  HIGH DENSITY

END
CENTRE CYLINDRICAL
PLATE
ROD MANDREL

FIXTURE ASSEMBLY

2D LATCHING FINGERS
WITH NPP M6 C/C BOLTS

DENSIFIED HOLLOW MACHINED RING

CYLINDER (2D C/C) 36/51
C/C PRODUCT TESTING

37/51
 ENEC : Composite testing
 C/C SAMPLE TESTING (RT – 2500°C)

TYPES OF TEST
MECHANICAL TENSILE
MATERIAL
(STRENGTH / COMPRESSION
MODULUS)  3D STITCHED LAMINATES
RT SHEAR  4D C/C
1000ºC, 1500ºC BENDING
2000ºC, 2500ºC POISSON’S RATIO & CTE
THERMAL THERMAL CONDUCTIVITY
RT - 2500ºC

3D C/C STITCHED LAMINATES 4D C/C BILLET

38/51
 ENEC : Composite testing
 C/C SAMPLE TESTING (RT – 2500°C) …
MACHINE : INSTRON
CRITICALITY 1196
 PREPARATION OF TEST SPECIMENS
WITH INTEGRAL NO. OF UNIT CELLS TEMP. RANGE : RT –
2800°C
IN GAUGE CROSS SECTION.
HEATING RATE : RT to
 DAMAGE TO COMPOSITE (FIBRE 2500°C in 25 sec
PULL OUT, CHIP OFF ETC.) COOLING TIME : 2500°C
to 100°C in 30 sec SAMPLE
ENVIRONMENT : ARGON

140
2000°
2500° 1500°
120
RT 1000°

100 GRAPHITE HEATERS

DURING TEST
STRESS (MPa)

80

60

40

20

0
0.00 0.05 0.10 0.15 0.20 0.25 0.3
STRAIN (%)

TYPICAL TEST SAMPLES TYPICAL TEST GRAPHS

39/51
 ENEC : Product testing
 THREADED JOINT EVALUATION

Threaded Joint for 4D Throat Insert to 3D

Fixed Cone
 Size : M105 x 4
(Buttress Thread profile as per IS 4696 PART 3)
 Length of Engagement : 30 mm
 No. of Specimens : 5

40/51
 ENEC : Product testing
 THREADED JOINT EVALUATION …

4D C/C LOAD 3D C/C

TYPICAL THREADED SAMPLES TEST SET UP

40
Buttress
35
Knuckle
Property BT Results (Avg) KT Results (Avg) 30
Screw
25
Thread Shear Failure 35.6 22.0 20

Load (KN)
Load (KN) 15
Thread Shear 7.5 5.4 10
Strength (MPa) stdev = 0.5 5
Design requirement 1.47 0
0 0.5 1 1.5 2 2.5 3
(MPa) Displacement (mm)
TYPICAL GRAPHS

41/51
 ENEC : Product testing
 THREADED JOINT : TORQUE & LEAK TEST

 EXTENDED ARM TORQUING

 5 Nm INCREMENT
 MAX. TORQUE CAPABILITY – 240 Nm
It was recommended based on the above
 REQUIRED TORQUE FOR
experiments to tighten the C/C threads with a
LEAK PROOFNESS – 140 Nm torque value of 140 N-m
42/51
 ENEC : Product testing
 C/C NOZZLE : PRESSURE & LEAK TEST

Schematic of Pressure & Leak test of Cone C/C Cone after Resin Impregnation

• The maximum pressure acting in the Fixed C/C cone is

6 bar at the cone inlet.
• Proposed to qualify the C/C nozzle by pressure testing
at 1.5 times the maximum pressure.
• C/C Nozzle was subjected to 9 bar pressure and the
pressure drop was observed with respect to time.
• No appreciable leak was observed.
• No damage to the component was observed.
43/51
 ENEC : Product testing
 C/C LATCHING FINGERS : BENDING & COMPRESSION TEST

LATCHING FINGERS
ASSEMBLY WITH C/C BOLTS
BENDING TEST COMPRESSION TEST

Description Result (Avg)

Bending Load (N) 67.5 (62 - 70) stdev = 3.8
Compression Load (N) 2079 (1626 - 2395) stdev = 329.1
Design Requirements 6.64 N (Bending), 105 N (Comp.)

44/51
ENEC : Static firing test

MOTOR THRUST (ACTUAL Vs PREDICTED)

ENEC NOZZLE INTEGRATED WITH
ROCKET MOTOR AT TEST BED

MOTOR THRUST (ACTUAL Vs BACK

CALCULATED FROM PRESSURE)

45/51
QUALIFICATION TESTING
OF C/C PRODUCTS

 Thermal testing
 Structural testing

46/51
 Thermal testing of C/C Nose Tip for Agni

 NOSE TIP EXPERIENCES SEVERE AERO

T10
THERMAL LOADS DURING RE-ENTRY
-
T1, T2

T-11
T-2
T-10
T-1 T-9
T7, T8
T-7

T-6
31mm
T-4
T-5

50mm
T-3
120 mm
T-8

Test condition T5 T6
Thermal Load : 1W/mm2
for 53 sec.

THERMOCOUPLE POSITION TEMPERATURE PLOT

OF THERMAL TEST

MAX. TEMPERATURE °C
LOCATION PREDICTED MEASURED
SURFACE 729 680
50 mm deep 172 135
31 mm deep 107 106
47/51
 Structural testing of C/C Nose Tip for Agni
 SEVERE FLIGHT STRESSES
F  SIMULATION OF FLIGHT CONDITIONS
 STRESS & STRAIN MEASUREMENT
Ø250

Load in
Sl No Remarks
Tones
5
7
0
4

1 4
9
9

2 8
2
15

Ø236.3 3 16.85 Design Load

4 18.95 Proof Load
5 22.4 Ultimate Load
LOADING SCHEME 6 25.2 Maximum Load

AL SECTION AL LOADING BLOCK QT & FLIGHT STRESS 48/51

 Structural testing of C/C RECS Fin for A2

LOADING
FIXTURE

C/C
RECS LVDT C/C RECS RECS ASSEMBLY

TEST SETUP

POSITION DESIGN LOAD ULTIMATE LOAD

1360 Kg 1808 Kg
PREDICTED ACTUAL ACTUAL

RECS TIP 17.5 22.4 31.2

FORK 4 5.2 7.2

SHAFT

DEFLECTION
49/51
 Testing of C/C Brake Discs
STATIC TORQUE
BRAKE FUNCTIONS
BLOCK 1
BLOCK-2 BLOCK-3 BLOCK-4 BLOCK-5
 PROVIDES DRAG 9 N.E.+1 O.L.

 ABSORBS K.E. STRUCTURAL RTO WET NORMAL

TORQUE
 HOLDS A/C STATIONARY DYNAMOMETER TEST PLAN AS PER MIL - 5013

STATOR ROTOR HEAT PACK FOR HEAT PACK FOR

TEJAS (A/F) SUKHOI

ASL DYNAMOMETER HAL DYNAMOMETER

- DOD TEST FIXTURE DOD BRAKE
TEST - TYRE, WHEEL & ASSEMBLY
- TWO DISCS BRAKE UNIT
- SINGLE INTERFACE - 7 Nos. OF DISCS
- 6 INTERFACES
50/51
THANK YOU