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J O U R N A L O F M A T E R I A L S S C I E N C E 5 (1970) 9 4 5 - 9 5 0

The Tensile Properties of Nickel-Coated
Carbon Fibres
A. J. PERRY, E. de L A M O T T E , K. P H I L L I P S
Brown Boveri Research Center, 5401 Baden, Switzerland

The tensile properties of nickel-coated Grafil "HT"carbon fibres were studied as a function
of the coating thickness, taking into account the diameter-dependence of the properties of
the fibres themselves. The stress-strain curve exhibited three stages, following from an
initially elastic coating which yields and then extends plastically before failure of the fbre.
The behaviour could be described by a simple law of mixtures and the grain size of the

1. Introduction handling damage, thus making the measured
In a previous paper [1 ] we presented the results ultimate tensile stress (UTS) subject to error.
of a study concerned with the dependence of the The diameter and coating thickness of all
mechanical properties of Grafil " H T " carbon tested fibres was measured by mounting them in
fibres on their diameter. We now discuss the plastic, sectioning transversely and projecting the
influence of a thin metal coating on these proper- image on to the calibrated screen of a projection
ties. As a model system we have chosen nickel microscope.
because it can be readily electroplated in a
nominally stress-free condition. However, nickel 3. Results
is known [2] to degrade the fibre properties fol- We showed previously [1] that both the U T S
lowing heat-treatment at moderate temperatures and Young's modulus of uncoated fibres depend
and this fact limits the usefulness of the model upon their diameter. It was also found that a
system. dispersion of values was obtained (fig. 3) at a
given diameter. We have therefore referred the
2. Experimental present data to the average values obtained
The carbon fibres were electroplated in a sulpha- previously at a given fibre diameter.
mate bath by two suppliers. The nickel coatings A stress-strain curve of an as-received coated
were analysed (using an electron microprobe fibre is compared in fig. 2 with the average
analyser) to show a cobalt content in the range 8 properties of the uncoated ones of the same fibre
to 11 wt ~. This has the effect [3] of increasing diameter. The following stages are evident:
tensile strength and reducing ductility of the (I): elastic fibre and coating,
nickel but ensures that it can be heat-treated transition (I)-(II): yielding of the coating,
without embrittlement. (II): elastic fibre and plastic coating
The absence of an attack of the fibres by the (the slope being the so-called
nickel coating was confirmed (fig. 1), first by secondary modulus),
etching back the nickel coating and studying the 0II): fracture.
fibre surface, and second by checking a fracture These are the stages normally observed in a
surface as done previously by Jackson and composite material containing brittle fibres [5].
Marjoram [2]. Some specimens fractured before the transition
The fibres were separated and tested in simple reflecting variations in the fibre U T S as men-
tension with an Instron machine using the tioned above.
window technique [4], all specimens being 5 cm The interpretation of stage (II) was verified by
in gauge length. Considerable difficulty was two observations. First we noted stress relaxation
experienced in separating fibres with thicker before, but not after, the transition (I)-(II). Second,
coatings which consequently suffered more from classical work-hardening was evidenced by the
9 1970 Chapman and Hail Ltd. 945
A. J. P E R R Y , E. de L A M O T T E , K. P H I L L I P S


kg//mm 2

100 lli

I I 1 I ~ I
0 02 0-4 0.6 0.8 1-0 1-2

Strain %
Figure 2 The effect of a volume fraction of 39.1~/o nickel
(curve B) on the average properties of uncoated carbon
fibres [1] of the same 989~.m diameter (curve A). Curve C
shows the effect of a heat-treatment of 1 h at 600~ C;
volume fraction 45.g~/o nickel, fibre diameter g Fm. The
three stages observed in tensile experiments on coated
fibres are indicated.

raised yield point following loading beyond the
transition, unloading and reloading.
In fig. 3a-c are given the UTS, Young's and
secondary modulus, and the fracture strain of as-
received coated fibres of a given typical diameter
as a function of the volume fraction of nickel in
the coated fibre. A histogram of the data obtained
previously [1 ] for uncoated specimens is included
on the ordinate of each graph.
The microstructure of the nickel coating was
examined, as shown in fig. 4a, and found to be
fine-grained with a grain size comparable with
that reported by Saleem et al [6] in nickel also
deposited from a sulphamate bath. The nickel
could be readily recrystallised (fig. 4b) by heat-
treating for I to 2 h at 600 ~ C, following K/Sster
[7]. From the results given by Jackson and
Marjoram [2], this treatment was expected to be
too short for the nickel-carbon fibre interaction
discussed by them; while we noted a slight drop
in Young's modulus (some 10 %), this interaction
does not affect the yield point of the nickel
which is the aspect of interest to us.
Figure 1 Scanning electron micrographs of as-received The effect ofrecrystallisation on the mechanical
nickel-coated c~rbon fibres: (a) a transverse section from
properties is included in fig. 2; graph C in this
which the nickel has been partially etched away (• 1850),
(b) a fracture surface (• 1420), showing the lack of effect
figure indicates both the lowered yield point and
of the nickel on the surface or interior structure of the
also the retention of its ductility by the nickel
fibres. Also shown, in (c), is the effect of heat-treatment (presumably because of its cobalt content as
at 600 ~ C ( • 1470). mentioned above).


O *
[ Fracture
Fracture ~OUJ 0.sStrain
Stress E %

~00 ~
kg/mm 2 -'~ "A 9 0-6

y5 04

Z 0.2
I. I
O) 9 A 9
& I I 1 i
z 0
0 20 40 60 8o 100
Nickel vo,../.

I I i i
20 40 60 80 100
Nickel ,ot."/. Figure 3 The mechanical properties of nickel-coated
carbon fibres as typified by 989 diameter fibres tested
at 10-2 min -1. The data are: (a) fracture stress; the full and
3 open symbols refer to samples in which the coating did
Young's and did not yield beforefracture, respectively, (b) Young's
Modulus and secondary modulus (full and open symbols) (c)
E fracture strain; full symbols refer to samNes which
x 10-~ exhibited stage II, as a function of the volume fraction of
nickel. The straight lines in (a) and (b) are least-square
kg / mmz fits calculated including the data for uncoated fibres
obtained previously [1]. The square datum in (a) is the
fracture stress of electrodeposited nickel according to
K6ster [7]. Included on each ordinate are the histograms
from earlier work [1l appropriate to uncoated fibres of 9~-
/~m diameter.

line which extrapolates to 1.23 • 104 kg/mm 2 at
'0 100 % Ni (averaged over all fibre diameters). The
0 4 60 80 100
Nickel ,ot,'/.
line is a least squares fit calculated with the
(b) inclusion of the data which compose the histo-
gram of uncoated fibres. If the data are analysed
excluding the uncoated results, then the derived
4. D i s c u s s i o n modulus for nickel is 1.46 • 104 kg/mm 2. These
4.1. Stage I values can be compared with the range 1.5 to
The Young's modulus of coated fibres for thin 2.1 • 104 kg/mm 2 given in the A S M handbook
coatings (i.e. C2 <~ 1) is given by the relation [9] for massive nickel; it might be remarked that
derived from the linear tfieory of elasticity [8]" D'Antonio et al [10] concluded that the modulus
E E, + E 2 (v~--v~) 2 of (fine-grained) vapour-deposited thin nickel I
E l a w of mixtures
= - -
E1 1 P22
. C~ (1)
- - -
films does not differ from that of bulk nickel.

where E, v and C are Young's modulus, Poisson's 4.2. Stage II
ratio and volume fraction and the suffixes i and 2 It is apparent that the nickel coating retains the
refer to the carbon fibre and nickel coating facility to be work-hardened because the
respectively. Equation 1 predicts little deviation observed values for the secondary modulus Exi
from the law of mixtures, independently of the extrapolate to a finite value at 100 % nickel, this
value of v~ which has not been determined to date. value being the work-hardening rate [11].*
The data in fig. 3b adhere quite closely to a straight However the paucity of experimental data
*(EI1)e = E i V I -~" ,ue/(~)e,~ Vm, referring to strain value 111].

A. J. P E R R Y , E. de L A M O T T E , K . P H I L L I P S

Figure 4 Optical micrographs x 1500 of nickel coatings (a) as-received and (b) after 1 h at 600 ~ C, The annular
,super-structure" of the nickel coating in (a) is also apparent infig, la.

renders very approximate any analysis to give a
value to the work-hardening rate. Nevertheless
1 o8I
the value is clearly quite high and corresponds to
the rate immediately after yielding and at very
low plastic strain. It does not correspond to the
work-hardening rate of bulk nickel strained 1104- - ~ "~
several per cent, which is of the order E/100.
It is interesting to contrast the present coatings I IO2" ~
with vapour deposited films which show [10]
little capacity for work-hardening and, because
cobalt does not affect this [12], we attribute the 100 ' ~ ~
C2 0,5 "~.0
difference to a grain-size effect. A value of the
latter was not reported by D'Antonio et a l [10] 0-91~
but discussion of their later work [13] by Tarshis
Figure 5 The ratio of the yield stress of the coating o* to
and Wilshaw [14] implies a value of about its yield stress in simple tension oy as a function of coating
1000 A, which is smaller than the 0.3 to 1 Fm in thickness calculated from (2) for a range of values of v 1.
the present work. The values of v2, E2 and Et were set respectively to -~,
1.46 x 104 kg/mm 2 (from the present work) and 2.4 X 104
4.3. T r a n s i t i o n I-II kg/mm = (as appropriate to 9/~m diameter fbres [1]). Note
The transition I-II is attributed to the yielding of that if v 1 = 89 the curve coincides with the abscissa.
the nickel coating. The yield stress of the coating
a* is related to the yield stress in simple tension, series of Poisson's ratios. It is evident that
ay, through the relation derived from the linear relatively little change in the yield point is
theory of elasticity coupled with the yon Mises anticipated, hence this effect has been neglected
yield criterion: in the present discussion.
cr* (C~E~ + C~E~) 1 4- (1 -- 2v~)(C~ 4- QC~) (2)
(1 4-v2)
cry E2 ~/3(vl -- v2)e + {(1 + v2) 4- (1 -- 2v~)[(1 4- vl) 4- Q(1 4- vz)Cz]} z
with The yield point of the coating deduced from
the present data (by taking the m e a n Young's
(1 - 2~1)(1 + ~1) E~ modulus at each fibre diameter to account for
Q = (1 - 2v2)(1 4- v2) the load carried by the fibres themselves) is given
where a difference in Poisson's ratio is necessary in fig. 6 as a function of (coating thickness) -v2.
to affect the yield point. As remarked above, the This form of presentation was selected to allow
ratio is not known for the carbon fibres, hence comparison with the Petch relation [15]
equation 2 has been evaluated (fig. 5) for a oy : % 4- k d -a/2

where d is the grain diameter. No experimental problems experienced with the thicker coatings,
investigation of the Petch relation for nickel was the scatter of data is comparable with that of
found in the literature, hence we proceeded in the uncoated fibres (see the histogram on the
following way. A straight line of slope k equal to ordinate of fig. 3c). Fracture is thus considered
0.08 • 10-a mml/2 • /x (F being the shear as being initiated in the fibres and is not affected
modulus) as indicated for the f.c.c, metals by the coating. The latter retains its ductility as
copper, aluminium and silver [16] was adopted can be seen in fig. lb.
and applied to data on nickel from Macherauch
and V0ringer [17]. The increase in yield point 5. C o n c l u s i o n s
caused by cobalt was introduced by taking a line The mechanical properties of nickel-coated
parallel to the above in accordance with data carbon fibres in simple tension have been
cited by Parker and Hazlett [12]. studied. It has been shown:
The adoption of the mean modulus of the (l) The Young's modulus (i.e. before yielding of
fibres themselves at the appropriate diameters the coating) can be described by a law-of-
introduces a serious approximation into our mixtures relation.
analysis, which is more significant at lower coat- (2) The high yield point of the nickel coating can
ing thickness and probably accounts for the wide be explained in terms of its grain-size.
scatter of data. A comparison between our (3) The fracture of the coated fibres is governed
results and the constructed Petch curve can only by the fibres themselves and is unaffected by the
be regarded as semiquantitative at best, but metal coating.
nevertheless the present yield point values appear
to be too high. The discrepancy is attributed to Acknowledgements
handling damage coupled with the ability to
The equations 1 and 2 were derived by Dr B.
work-harden the coating remarked previously.
Biirgel of this laboratory, and we wish to express
In an attempt to confirm the latter point we
our obligation to him. We also wish to thank
heat-treated coated fibres at 600 ~ C for 1 and 2 h
Messrs H. Beutler and M. Villat of Sulzer
in order to recrystallise the coating (fig. 3). The
Brothers Ltd, Winterthur, for their participation
yield strain was thus reduced (fig. 2) and the in the study.
yield stress of about 25 kg/mm 2 agrees reason-
Finally we acknowledge firstly the stimulating
ably with that predicted by the Petch curve in
discussions with Professor J. S. L. Leach, Dr T.
fig. 6 at a grain size in the region of 1 Fro.
R. Wilshaw and Dr H. R. Killias, and secondly
correspondence with Professor N. J. Petch; these
150 contributed materially to our understanding of
Yield some features of the research.
Stress v v
kg/mm z References
,7 v
9 v
I. E. DE LAMOTTEand A. J. PERRY, Fibre Sci. Teeh.,
50 " ,~ ~ ~ " to be published.
2. P . W . J A C K S O N a n d J. R . M A R J O R A M , J. Mater. Sci.
. . . . __" .... , .... , , , 5 (1970) 9.
3. K . C. B E L T , J. A. C R O S S L E Y ~
0 10 20 30 40 50
Proe. 7th Int. Metal Finishing Conf., Hannover, 1968,
Diameter 2, Thickness 2 mml/2 p. 222.
Figure 6 A superposition of the present yield point data as 4. Grafil Test Methods, Courtaulds, Coventry, 1969.
a function of (coating thickness) -~ on a Petch plot 5. A. KELLY, "Strong Solids" (Clarendon Press,
derived as discussed in the text; the full and dashed lines Oxford, 1966).
are the nickel and nickel/10 w t % cobalt respectively.The 6. M. S A L E E M , D . A. ]BROOK, and j. w. C U T H B E R T S O N

square data points are taken from Macherauch and Electrochim. Acta 12 (1967) 553.
V~ringer [17J. The open and full symbols refer to speci- 7. w. K6STER,Z. Metallk. 31 (1939) 168.
mens taken from tows plated by the two suppliers. 8. I. S. S O K O L N I K O F F , "Mathematical Theory of
Elasticity" (2nd Ed., McGraw-Hill, 1956).
4.4. S t a g e III 9. "Metals Handbook" vol. I, 8th Edition (Amer. Soc.
Metals, 1961)p. 1118.
The fracture strain values are shown in fig. 3c for 10. C . D ' A N T O N I O , J . H I R S C F I H O R N , a n d L. T A R S H I S ,
one fibre diameter. Allowing for the handling Trans. Met. Soe. A I M E 2 2 7 (1963) 1346.
A . J. P E R R Y , E. de L A M O T T E , K . P H I L L I P S

11. A. KELLY a n d G. J. DAVIES, Metallurgical Reviews 15. N. J. PETCH, J. It'oH • Steel bzst. (LondotO 25 (1953)
10 (1965) 1. 174.
12. E. R. PARKER a n d R. ft. HAZLETT, " R e l a t i o n of 16. R. A R M S T R O N G , I . C O D D , R. M. D O U T H W A I T E , a n d
Properties to M i c r o s t r u c t u r e " (Amer. Soc. Metals, N. J. PETCrI, Phil. Mag. 7 (1962) 45.
Cleveland, 1953) p. 30. 17. E. MACHERAUCH a n d o . V O R I N G E R , Phys. Stat.
13. R. L. G R U N E S , C. D ' A N T O N I O , a n d E. K . K I E S , J~ Sol. 6 (1964) 491.
Appl. Phys. 36 (1965) 2735.
14. L. A. T A R S H I S a n d T. R. WlLSHAW, ibid 37 (1966) Received 28 July a n d accepted 7 September 1970.