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Materials Science and Engineering A343 (2003) 243 /250 www.elsevier.com/locate/msea

Fragmentation study of interfacial shear strength of single SiC ber reinforced Al after fatigue
Yongning Liu a,1,1, Wei Kang a, Jiawen He a, Zuming Zhu b
b

State Key Laboratory for Mechanical Behavior of Materials, Xian Jiaotong University, Xian 710049, Peoples Republic of China State Key Laboratory for Fatigue and Fracture of Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110015, Peoples Republic of China Received 4 January 2002; received in revised form 17 May 2002

Abstract The interfacial shear strength of SiC fiber reinforced aluminum composite has been studied by the fragmentation test of single fiber reinforced model specimens after a number of fatigue cycles. The result shows that apparent stiffness of the testing machine is influenced by cyclic loading, which will affect the calculation of fiber strength by Cloughs model. An extracting test in which fragmented fiber was extracted out by dissolving the matrix material in NaOH water solution indicated that the fiber strength did not lose via vacuum hot press treatment. This result contradicts the Cloughs model. The experimental result showed that the critical length of the fiber increases a little after a few cycles of fatigue loading and thus, the interfacial shear strength decreases. The reason for this is that the thermal residual stress around the fiber developed during fabrication decreases in cyclic loading. # 2002 Elsevier Science B.V. All rights reserved.
Keywords: Fragmentation; Composite materials; Fracture; Fatigue

1. Introduction The fiber reinforced metal matrix composites (MMC) have been subjected to intensive researches for their good merits such as high stiffness, high strength, high damping and high fatigue crack propagation resistance. The interface between fibers and matrix plays a very important role in transferring load and turn out to be a key factor in the mechanical properties of MMC [1 /3]. There are several ways to measure the interfacial strength such as push out, pull out and fragmentation for single fiber reinforced model specimen. Each method is characterized with its way of measurement and the results are different. [4 /6]. For MMC, push out and fragmentation are two methods used often [6 / 10]. In the fragmentation test, both fiber strength and interfacial shear strength can be obtained [9 /11].
1 Corresponding author. Tel.: '/86-29-266-9071; fax: '/86-29-2663453 E-mail address: ynliu@mail.xjtu.edu.cn (Y. Liu). 1 Now as a visiting scholar in Institute of Composite Materials, Shanghai Jiaotong University.

Clough [11] developed a model which can calculate the fiber strength in the fragmentation test. However, the calculated results are much smaller than that of the intrinsic strength of the fiber [11]. As a result a few papers still followed the way to do the experiments and released the data [12,13]. According to Clough way, it seems that the fibers were damaged in the fabrication process. However, some published data [6,7] did not agree with the results. The thermal exposure test of a SiC reinforced aluminum [6] indicated that the fiber strength did not reduce even at 600 8C for 700 h. This is a problem which needs to be clarified. Further more, many research efforts have been aimed at the study of the interfacial shear strength via different fabrication technologies [5 /7,14,15], little work has been done to examine the fatigue effects on the interfacial shear strength of fiber reinforced MMC [16,17]. Research showed that the interfacial shear friction stress between SiC fiber and titanium alloy matrix measured by the push out method decreased after fatigue loading [18]. The reason was explained as (1) asperity wear of the SCS coating layer, and (2) relaxation of radial residual thermal stress in the matrix. There are two interesting

0921-5093/02/$ - see front matter # 2002 Elsevier Science B.V. All rights reserved. PII: S 0 9 2 1 - 5 0 9 3 ( 0 2 ) 0 0 3 6 3 - 5

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questions: (1) whether this phenomenon will occur also in SiC reinforced aluminum matrix, (2) whether this phenomenon can be repeated by fragmentation test because there is no asperity wear effect in the test. This work is going to study these problems by fragmentation testing single fiber reinforced aluminum matrix model specimens.

sf 0

N DsuL A2 s Af kLDN

(2)

where Ds 0 DP=As ; DP is the magnitude of the load drop, As is the cross section area of the specimen, Af is the cross section area of the fiber, uL is the macro work hardening rate at the gage length L , k is the stiffness of the test machine, N is the total number of the fibers fractured, DN is the number of repeated fracture in one drop, which can be obtained by DN $ DP DP (3)

2. Experimental procedure The model specimens were prepared by vacuum hot press. The fiber is SiC with diameter 90 mm and provided by the Institute of Metals, Sinica Academy. The fiber is a pure SiC with no any surface treatment. The matrix is pure aluminum plate of thickness of 1 mm. The hot press process is conducted at temperature of 600 8C with constant pressure of 40 MPa for 2 h. The plate specimen was cut into a size of 5 mm in width, 1.8 mm in thickness and 20 mm in gage length. The tensile and fatigue tests were conducted in a computer controlled screw driving testing machine with capacity 10 kN. In order to study the effect of cyclic loading on interfacial strength, the fatigue test was performed using the pulsating method at a stress ratio of smin/smax 0/0. The maximum stress is about 0.8 to /0.9 of the yield stress of the material. All force and displacement signals were recorded and processed by a computer. In this test the fiber will break during tensile process. There is a critical length of fiber, beyond it the fiber will not break anymore. An important result is to obtain the critical length. So an acoustic emission detector AE-02 was used to monitor the fiber fracture during the tensile test [11]. To obtain the number of fiber fractures after the tensile test, the fractured fibers were extracted out by dissolving the matrix material in NaOH water solution. So the critical fiber length can be obtained. The critical length was obtained by a statistical result given by Kelly and Tyson [20] lc 0 1 0:75 Lc (1)

is the average of all load drops, DP is one where DP load drop. Calculated DN is 2 for Figs. 1 and 2. The stiffness of the test machine can be calculated by the following equation [13,19]  (1 v l k0 ( (4) (dP=dt)max As Es where v is the crosshead velocity of the machine, (dP / dt )max is the maximum slope of the load versus time curve at the elastic part. l , As and Es are gage length, cross-section area and Youngs modulus of the specimen, respectively. The interfacial shear strength can be calculated by the Kelly and Tyson [20] approach when the critical length and fracture strength of fiber are known ti 0 sf d 2l c (5)

where ti is the interfacial shear strength, d is the diameter of fibers. Putting Eq. (1) into Eq. (5), it yields [21 /23] 3 d ti 0 sf 8 Lc (6)

3. Experimental result Figs. 1 and 2 are a set of tensile and acoustic emission signal curves. Fig. 1 shows the result of virgin specimen and Fig. 2 is after ten cycles fatigue loading. In order to show the load drops during tensile test, the part of the curves with a number of load drop peaks has been magnified as in Figs. 1b and 2b. Each load drop is corresponding to the acoustic emission signal in Figs. 1c and 2c. The signals at the beginning of the acoustic emission are produced by tightening between the specimen and grips, which are basically in the non-linear region at the initial part of the tensile curves of Figs. 1a and 2a. The fiber fracture usually occurs after the bulk yielding of the specimen and results in a load drop, yet

where lc is critical length, Lc is fragmentation length and can be obtained by an average of the fiber length in gage span divided by the number of the fractures. To examine the fiber strength calculated by Clough equation and measurement, the fiber was tested by gluing the fiber onto two steel plates at two sides of the fiber. The steel plates were clamped by grips of the testing machine. The stress and strain were recorded and process by a computer system. The fracture strength of the fiber can be calculated by the Clough equation in term of load drop and number of fractures [11].

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Fig. 1. The tensile curves and corresponding acoustic emission signals of specimen without fatigue. (a) Load and time curve of tensile test. (b) Local high magnication of A. (c) Acoustic emission signals.

Fig. 2. Tensile curve after 10 cycle fatigue loading and corresponding acoustic emission signals. (a) Tensile curve. (b) Local high magnication of A. (c) Acoustic emission signals.

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the duration time and load drop magnitude are different. This fact indicates that more than one fracture could be involved in one load drop and this was confirmed by the extraction test. For instance, the specimen of Fig. 1 showed eight fractures according to the accounts of acoustic emission signal and load /time curve, however, the extraction test exhibited 13 times of fracture. For the specimen in Fig. 2, the accounting number by acoustic emission and tensile curve was 10, however, the extraction result was 15. In order to make a precise measurement of the number of fractures and the critical length in this study, we are based on the counted using the extraction test. From Figs. 1 and 2, it is obvious that there is a great difference in dP /dt in the elastic regions for the specimen before and after fatigue. Because the geometry of the specimen is the same, from Eq. (4) the stiffness will deviate according to the difference in dP /dt . The measurement of (dP /dt )max and the calculations of stiffness are shown in Table 1. The values in Table 1 indicate that (dP /dt )max is the main factor in determination of k. The geometry of the specimen and the Youngs modulus in the second term of Eq. (4) would not change much, thus, one order magnitude difference in (dP /dt )max before and after fatigue will lead to the same order of difference in the calculated stiffness. Putting different stiffnesses in Eq. (2), the calculated fiber strengths are shown in Fig. 3. The remarkable difference in fiber strength is by no means due to the specimen being fatigued 10 /100 cycles. The strength of the fibers should be determined by the manufacturing technology, the composite process and the chemical reaction at the interface. It should not depend so strongly on the process of physical loading.

Fig. 3. Fiber fracture strength calculated by Cloughs relationship with cycle loading number.

U 0 Um ' Us ' Uo

(7)

where Um is the displacement caused by machine such as elastic deformation of machine columns, gaps between the screw threads. Us is the displacement caused by deformation of the specimen. Uo is the displacement arisen from slippage. Differentiating above equation dU dt 0 dUm dt ' dUs dt ' dUo dt (8)

where dU /dt is the crosshead velocity of the test machine and can be expressed by v and dUo/dt is slippage rate and is simplified as vo. dUm/dt is the elastic deformation rate of the test machine and can be expressed by om Lm and dUs/dt is the deformation rate of the specimen and can be expressed by os l : om and os are the strain rates of the test machine and specimen. Lm and l are the rod lengths of the columns between the crossheads of the test machine and the gage length of the specimen respectively. Then, v 0 om Lm ' os l ' vo (9)

4. Discussion 4.1. Stiffness The stiffness k is a very important parameter and will affect the calculation of fiber strength sf with Eq. (2). Table 1 shows that the difference in k before and after fatigue is great. This difference real does not come from machine stiffness while comes from slippage between specimens and grips of testing machine. Suppose the displacement between two crossheads could be written
Table 1 Stiffness k and (dP /dt )max with and without cyclic treatments No cycle (dP /dt )max (N min( 1) k (kN m ( 1) 256.0 257.8 10 cycles 3180.8 3480.6 100 cycles 3064.8 3340.3

The elastic deformation is calculated by Hookes law o0 1 dP EA dt (10)

Putting Eq. (10) into Eq. (9)   Lm l dP v0 ' v0 ' Em Am Es As dt then dP dt 0 v ( v0 Lm l ' Em Am Es As 

(11)

(12)

This equation indicates that the slippage v0 in tensile test will decrease dP /dt . In the first loading as shown in Fig. 1, there is slippage effect. After several cycles of

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fatigue loading, the specimens had been tighten and the slippage had been diminished. Clough [11] did not mention this effect in the stiffness measurement. However, It had been recommended by international standard IOS 2573 [24], that one should first apply and remove a force at least as great as the maximum load used in the determination of the compliance of the test system. 4.2. Fiber strength The calculation of fiber strength using Eq. (1) indicates that there is a great difference using the stiffness measured before and after fatigue. The calculated sf seem to be a reasonable, around 2300 MPa, if the stiffness before fatigue is used. Otherwise, sf is quite small, around 150 MPa, if we use the stiffness after the fatigue, which would be much approaching the correct stiffness, see Fig. 3. It is questionable if the fiber strength is so low, how can it reinforce the matrix materials? Some published data showed similar magnitude values of fiber strength by using Clough model, paper [12] reported that sf 0/494 MPa for fiber SiC, sf 0/715 MPa for SiO/2 treated SiC, and sf 0/567 MPa for carbon treated SiC. Paper [11] reported sf 0/798 to /340 MPa for carbon treated SiC. All these strength values are around the strengths of aluminum alloys or medium carbon steels and there would have been a great loss of the fiber strength in comparison with the original strength, 3500 MPa [7,25], during hot press process. If so great a loss of the fiber strength is true, it would be impossible to use the fiber reinforced composites. In order to clarify this problem, several specimens which were subjected to the same hot press technology and fatigue pre-loading were dissolved in NaOH water solution. The fibers were taken out and the strengths were measured again. The result is shown in Fig. 4. In this figure, 1 presents as received state, 2 presents the hot pressed state and 3 presents the hot pressed and fatigued state. There is no substantial loss of the fiber strength after the hot pressing and fatigue pre-treatment.

This result agrees with many published results [6,17,26] but disagrees with Cloughs [11,13] data. If we make a close look at Eq. (2), Clough adopted an assumption that the crosshead displacement was much smaller than that of the specimen in a load drop, that is v dt &/dus, see Appendix A in Ref. [11]. So v dt could be omitted. Since no data had been shown in his publication to prove this assumption, we did the measurements in this test. In Table 2, six load drops have been measured for two specimens on the tensile curves. The sketch of this measurement is shown in Fig. 5. For one load drop, the starting point marked 1 and the end point 2, the displacement, x , time, t and load, p , at different sites can be obtained by computer acquisition. Because the velocity of the crosshead is a constant, the crosshead displacement can be obtained by v dt 0/v (t2(/t1). Concerning the specimen displacement, for a tensile system, the displacement of the crosshead should be   1 1 x0 ' P (13) km ks where km is the stiffness of the testing machine and ks is the stiffness of the specimen. Because the stiffness of test machine is a constant, when a fiber breaks, the stiffness of the specimen will be changed by Dks, then     1 1 1 1 x2 ( x1 0 P( P ' ' km ks ' Dks km ks   1 1 0 P (14) ( ks ' Dks ks This means the displacement between crosshead is mainly caused by fiber breaking and can be treated as the specimen displacement. Thus, Us 0 x2 ( x1 (15)

The results in Table 2 indicate that the specimen displacements Us and the crosshead displacement are in

Fig. 4. Fiber strength after dissolving the matrix aluminum.

Fig. 5. A high magnication of a local region of the tensile curve to show the load drop and the values which can be measured on this drop.

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Table 2 The measurements of the displacements of crosshead and specimens in load drops Specimen 1 Us (mm) V dt (mm) Specimen 2 Us (mm) v dt (mm) 1 0.0153 0.0137 1 0.0084 0.0140 2 0.0089 0.0063 2 0.0123 0.0090 3 0.0093 0.0085 3 0.0054 0.0050 4 0.0004 0.0076 4 0.0046 0.0090 5 0.0045 0.0069 5 0.0073 0.0076 6 0.0110 0.0029 6 0.0083 0.0140

the same order and no rule of v dt &/dus was exhibited. Even more, there are some values of v dt larger than that of specimens. The measurements indicate that the presumption in Cloughs theory is not true. 4.3. Interfacial shear stress and its changes with fatigue If the strength of the fibers does not change remarkably after hot pressure, the critical length of the fibers can be obtained by dissolving aluminum after tensile test. The result is shown in Fig. 6. The critical length increases as the number of fatigue loads increase. Taking these results into Eq. (6), the interfacial shear strength can be calculated and the result is shown in Fig. 7. Contrary to the change of the critical length, the interfacial strength decreases as the number of fatigue loading increases. The result is in agreement with a push out experiments of SiC fiber-reinforced titanium alloy [18]. Guo and Kagawa [18] ascribed the effect of fatigue on the interfacial shear strength to asperity wear and residual stress. In fragmentation test, there is no asperity wear influence. Concerning the residual stress effect, there is an experimental fitting equation [18]
T sT (bT (N 5 100) 11 N ) r (N ) 0 sr (0)exp( T T ( N ) 0 0 : 65 s ( 0 )exp( ( b N (N ] 100) sT 12 ) r r

Fig. 7. Interfacial shear strength vs cyclic loading number.

coefficients and larger than zero. This equation indicates that the residual stress will decrease with the increase of the number of fatigue loads. The initial radial thermal stress sT r (0) is approximately given by [26]
DT

sT r ( 0) 0 b1 and b1 0

g (a ( a )dT
f m 0

(17)

(16a) (16b)

rEm Ef Em (1 ( nf ) ' Ef (1 ' nm )

(18)

where sT r (0) is the initial residual thermal compressive T stress of the composite and bT 11 and b12 are the numerical

where Ef, Em, nf and nm are Youngs modulus and Poissons ratio of the fiber and matrix, respectively, af and am are thermal expansion coefficient of the fiber and the matrix in the radial direction, respectively, DT is the temperature difference over which the residual thermal stress develops in the composite, and r is an adjustment factor for the effect of fiber volume fraction. r is equal to unity for an infinite single composite and is less than unity in usual case [26]. Here, in calculation of sT / r (0); the fiber volume fraction can be neglected and r 0/1 [18], the calculated sT ( 0 ) / 0/( /890 MPa. The conr stants used in the calculation are shown in Table 3. In the push out test, the interfacial shear frictional stress, t; is written as [18] t 0(msr (sr B 0) (19)

Fig. 6. Fiber critical length vs cyclic loading number.

where m is friction coefficient and sr is the average

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Y. Liu et al. / Materials Science and Engineering A343 (2003) 243 /250 Table 3 The constants of ber and aluminum matrix Aluminum matrix constants Youngs modulus, Em Poissons ratio nm Thermal expansion coefficient, am Fiber constants Youngs modulus, Ef Poissons ratio nf Radial thermal expansion coefficient, af 249

80 GPa 0.3 23.6 ) 10 ( 6 K ( 1 400 GPa 0.17 2.6 ) 10 ( 6 K ( 1

compressive stress acting on perpendicular to the sliding interface. The friction coefficient m can be calculated by [18] m0 P(0) 2phRf sr (0) (20)

where P (0) is the maximum load in push out test at initiation state, h is the thickness of the push out slice, Rf is the radius of the fiber and sr/(0) is the compressive stress perpendicular to the sliding interface. A push out test of SiC fiber reinforced aluminum composite was carried out by Yang [27] and the results were P (0) 0/0.65 N, h 0/0.17 mm, Rf 0/4.57 mm. Putting these values and the compressive stress calculated above into Eq. (20), the calculated friction coefficient m 0/0.149, which is a little smaller than that of titanium alloy [18]. Then, from Eq. (19), the calculated the interfacial shear friction stress is 132.6 MPa. Comparing the values in Fig. 7 at pristine case, which is around 75 MPa, the agreement in the order of magnitude is reasonable. The difference mainly comes from two different measurement systems as mentioned at the beginning of the paper and in fabrication technology of samples making. The sample used by Yang [27] is made by casting while here is made by vacuum hot press of aluminum plates. Anther factor is that there is asperity wear effect in push out test. If putting Eq. (16a) into Eq. (19), we get ti 0(msT (bT 11 N ) r (0)exp( (21)

the test machine will influence greatly the calculation of the fiber strength. There is significant slippage between the grips and plate specimen at the first tensile loading. One to two times pre-loading is required before the formal measurement of stiffness. By dissolving the matrix aluminum and testing the remaining SiC fiber, it is found that the fiber strength is not changed after the hot pressure at 600 8C in vacuum furnace for 2 h. This fact against to the Cloughs data remarkably. The measurements of the displacements of the crosshead and the specimen during load drops on load vs time curves of tensile test did not prove the Cloughs assumption that the crosshead motion is much smaller than that of specimen during fiber breaking in the fragmentation test. After 10 /100 cycles fatigue loading, the fiber critical length increases a little and the interfacial shear strength decreases with fatigue loading. That the interfacial shear stress of SiC fiber reinforced composite decrease with fatigue cyclic number is mainly due to the thermal residual stress between the fiber and the matrix, which decrease with fatigue cyclic loading.

Acknowledgements This research is a part work of NSFC project: evaluation of the interfacial properties of aluminum matrix lamella composite and its relationship with fatigue (no: 59731020). Authors are also grateful for the support by Visiting Program of Chinese Education Ministry as a visiting scholar in State Key Lab. Of Composite Materials, Shanghai Jiaotong University.

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It is clear that the interfacial shear stress decrease with increasing of fatigue loading number. Thermal residual compression stress around the fiber decreases during fatigue. This makes the interfacial shear strength decreases also. The Fig. 6 indicates that the fiber critical length increases with fatigue loading. This phenomenon related to the interfacial shear stress, from Eq. (5), when interfacial shear stress decreases, the critical length will increase.

5. Conclusions When Cloughs model is used in the fragmentation test of single fiber reinforced specimen, the stiffness of

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