Effect of Carbon fiber on the Physico-Chemical Properties of Conductive Butyl-Rubber Composite

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1 Egypt. J. Sl., Vl. (23), N. (1), (2000) 167 Effect f Carbn fiber n the Physic-Chemical Prperties f Cnductive Butyl-Rubber Cmpsite F.S. Deghaidy Department f Chemistry, Faculty f Science, Suez Canal University, Ismailia - Egypt This study fcuses n the effect f the carbn fiber (CF) cncentratin n the physic-chemical prperties f Isbutylene and Isprene Butyle Rubber (IIR) cmpsites. The kinetic parameters fr the vulcanizatin prcess f IIR/CF cmpsites were calculated and discussed. The swelling mechanisms were identified; whereas, relative humidity and resistance during swelling as a functin f carbn fiber cntent were measured. The effects f carbn fiber cntents n sme electrical and mechanical prperties were investigated. SEM was used t supprt the bserved trends. It was demnstrated that carbn fiber accelerates the vulcanizatin prcess by acting as a catalyst and imprves the physic-chemical prperties f IIR cmpsites fr practical applicatins.

2 F.S. Deghaidy 168 Intrductin Recently there has been a grwing interest in plymer cmpsites, where different fillers were used t imprve the characteristics f the cmpsite [1-13]. In spite f the fact that plymer exhibits gd insulatin prperties, its electrical cnductivity is imprtant in many applicatins. In general, the electrical cnductin prcess in carbn black plymer cmpsites is cmplicated and depends n large number f parameters, mainly n filler cncentratin. As Carbn fibers (CF) filler has its wn attractive prperties, this study fcuses n the effect f the carbn fiber (CF) cncentratin n the physic-chemical prperties f Isbutylene and Isprene Butyle Rubber (IIR) cmpsites. In additin t the amunt f lading CF, particle size and structure, filler matrix interactins, swelling and prcessing techniques are key factrs in determining the physical prperties [2,4]. Analysis f the mechanisms f swelling in plymeric systems has received cnsiderable attentin in recent years because f the imprtance f the applicatins f plymers in bimedical, envirnmental and agricultural engineering and thers [3,14]. Experimental Prcedure All rubber mixtures were prepared n a tw-rll mill f 170 mm diameter, wrking distance 300 mm, speed f slw 18 rpm and gear rati The varius rubbers used in this wrk were prepared accrding t the recipes given in Table (1), where Plyacrylnitrile based CF was used. The average diameter f a single filament f the CF was 6 µ m while the CF density was 1800 kg/cm 3. Phsphric acid (H 3 PO 4 ) was used fr inhibitin and/r retardatin f CF xidatin during vulcanizatin prcess. An verall mixing time f 1 hur at 20 0 C befre adding CF was allwed t ensure hmgeneity f cnductive particles. Vulcanizatin was carried ut between stainless steel platens at 175 C and pressure 300 kn/m 2 fr dwelling time 30 min. Thin brass electrde was embedded int samples during vulcanizatin prcess. A circuit used fr electrical cnductivity measurements during vulcanizatin prcess was described elsewhere [4,13]. Mechanical prperties f the samples were measured by the Shimadzu AGS-IKNA Tensiln. The mrphlgy was studied by scanning electrn micrscpy (SEM), The crsslinking density (CD) was calculated accrding t the equatin, [12]: ( m t m ) CD = (1) mr m where m t is the mass f the swllen plymer at time t, m is the mass f dry plymer at time 0, and m r is the mass f rubber used in phr. The vlume fractin f rubber (V r ) was calculated accrding t the equatin [13]:

3 Egypt. J. Sl., Vl. (23), N. (1), (2000) 169 ( mt λ m ) mt λ m β V r = / ( + ) ρ ρ ρ r where λ is the mass fractin f the insluble cmpnent in rubber sample, ρ r and ρ s are the densities f IIR and kersene respectively and β is the mass f the bserved slvent (kersene) crrected fr swelling increment. Table (1): Frmulatin f the recipes. Ingrediants (phr) F0 F3 F6 F9 F1 Butyl rubber (IIR) Stearic acid Zinc xide Prcessing il (HAF) black a TMTD b Carbn fiber (CF) H 3 PO Sulfur (a)high abrasin furnace black, (b)tetramethyl thiuran disulfide. Results and Discussin Effect f Carbn Fiber n Vulcanizatin Kinetics f IIR cmpsites The vulcanizatin time versus electrical cnductivity f IIR cmpsites with different cncentratins f CF at P = 300 kn/m 2 and T = C are shwn in Fig. (1), (at this temperature slid sulfur transfrms t liquid sulfur cnsisting f S 8 ring mlecules and chain mlecules with an average mlecular weight f mre than 10 5 ) [15]. It is clear that the vulcanizatin begins during heating and depends n CF cncentratin. The vulcanizatin prcess shws an S-shaped prfile shifted t shrter time scales with increasing CF cntents. The behavir f vulcanizatin prcess can be divided int tw regins: in the first ne, the electrical cnductivity increases rapidly. This may be attributed t rdering f the cnductive phases and thermal activatin causing rapid crsslinking density [13]. In the secnd stage, the cnductivity slightly increases and then remains steady with time fr abut five hurs. This plateau crrespnds t cmpletin f the vulcanizatin prcess [5]. It was fund that the separatin distance between cnductive aggregates, (calculated accrding the equatins given by Ref. [6]), decreases with increasing CF cntent {Table (2)}.This reflects the fact that the CF enhances the crsslinking density and increases the interfacial bnding f the fiber and matrix. r s (2)

4 F.S. Deghaidy 170 The characteristic time cnstant (τ ) as a functin f CF cntents can be estimated by the empirical frmula: ( σ -t/τ -σ ) = ( σ m -σ ) (1- e ) (4) where σ m and σ are the maximum and initial cnductivity f the tested samples respectively and τ is the characteristic time cnstant depending n CF cncentratin. The values f characteristic time cnstant as a functin f CF cntent are listed in Table (2). In Table (2), the characteristic time decreases with increasing CF; this implies that the CF accelerates the driving frce during vulcanizatin prcess and increases the reactin kinetics rate [5]. The mass transprt f vulcanizatin can be estimated accrding t the empirical frmula: σ = t n AC (5) where, σ / t is the rate f cnductivity during vulcanizatin, A is the verall rate cnstant f cnductivity and is an incrprating characteristics f the aggregatin distributin and CF cntent, C is the cncentratin f CF (phr), and n is the diffusin expnent, which is indicative f the transprt mechanism during vulcanizatin prcess. The value f n fr bth stages f IIR cmpsites with different cncentratins f CF are listed in Table (2). The values f n in Table (2) indicate that, tw main vulcanizing stages are defined. The first ne with n 1 indicates the mechanism f rdering f the cnductive particles. The secnd stage with n 0.5 indicates that the grain bundary f aggregates diffusin leads t ptimum vulcanizatin prcess [6]. The vulcanizatin parameter ( σ / σ ) is time dependent because f the systematic decrease f the prsity f the cmpact sample and increase f the crsslinking with the vulcanizing time. The activatin energy f vulcanizatin prcess (Q) as a functin f CF cntent can be estimated by the fllwing equatin, [7]: σ = A exp( Qn / KTt ) (6) σ where Q is the activatin energy fr mass transprt during vulcanizatin, K is the Bltzmann cnstant and T is the Kilven Temperature. The values f Q f

5 Egypt. J. Sl., Vl. (23), N. (1), (2000) 171 IIR cmpsites during vulcanizatin as a functin f CF cntent are recrded in Table (2). It is cnsidered that the activatin energy decreases with increasing CF cntent which may indicate the slwer rate f kinetic reactin during vulcanizatin prcess f samples having lwer cntent f CF [8]. Table (2): Separatin distance befre (ω ) and afterω (t) swelling, characteristic time cnstant during vulcanizatin (τ ), diffusin expnent (n) and activatin energy during swelling (Q) as a functin f CF cntent f IIR cmpsites. Sample ω batch ( A) ω (t) ( A) τ (min) First Stage (n) Secn d stage (n) (Q) (ev) F F F F F Fig (2) shws the relatinship between crsslinking density (CD) and vlume fractin f rubber (Vr) against CF cntent. It is clear that, the CD and Vr increase with CF cntent. The CD and Vr clearly prnunce that the CF imprves the cntiguity links between cnductive aggregate [16]. Electrical Resistance During Swelling and Mass Swelling Of IIR /CF Cmpsites Fig (3) shws the effect f CF n the electric resistance f IIR cmpsites during swelling in kersene at 20 C. It is nted that at lw cntent f CF the resistance increases linearly while at higher cntent the resistance slightly increases quasi-cnstant. It is clear that the swllen behavir f IIR cmpsites strngly depends n the aggregatin structure and the mlecular mbility f the slvent, in ther wrds n the degree f rdering. Thereby, the increase f resistance at lw CF cntent is ascribed t the kersene mlecules, which frm a layer structure and/r bimlecular lamellae with rubber matrix [9] especially samples F0 and F6. SEM phtgraph in Fig. (4a,b) shws that there is a black hle inside a rubber matrix due t the reactin f kersene mlecules with mlecules f rubber cmpsites fr sample (F0), while sample (F6) is nt affected by slvent mlecules. The mass swelling [% S(m)] f the IIR /CF cmpsites can be estimated accrding t equatin:

6 F.S. Deghaidy 172 m m % S (m) = x100 (7) m Fig (5) shws that mass swelling is increasing with time, but after certain perid becmes cnstant. The Mass equilibrium Swelling (MES) can be calculated by the empirical frmula: t -N/τ ( S - S ) = ( S - S ) (1- e ) (8) where S m and S 0 are the maximum and initial swelling f IIR cmpsites respectively, and N is the characteristic swelling time cnstant which crrespnds t MES at N = t. Therefre, the mlecules f rubber will expand due t netwrk structure change. While at high cntent f CF the mlecules f kersene cannt penetrate int chains f rubber matrix. Table (3) represents the change f MES (%) with CF cntent. A decrease in the MES values with increasing the CF cntent is bserved. This may be attributed t penetratin f the kersene mlecules int the chains f the rubber matrix at lw CF cntent (i.e. samples F0 and F3). Therefre, the mlecules f rubber will expand due t net wrk structural change. While at high cntent f CF the mlecules f kersene can nt penetrate int the chains f the rubber matrix. Thereby, it is cncluded that CF imprves the micrstructure cre and rdering the rubber matrix. Table (3): Mass Equilibrium Swelling (MES) values f IIR/CF cmpsites Sample batch F0 F3 F6 F9 F12 MES % m Effect f Relative Humidity n Resistance f IIR cmpsites as a functin f CF cntent Fig. (6) shws the relatinship between relative humidity f IIR cmpsites and electric resistance as a functin f CF cntent. It was fund that fr lw cntent f CF, especially samples F0 and F3, the resistance increases linearly with increasing humidity, while at higher CF (i.e. samples F6, F9 and F12), the electric resistance slightly increases with humidity. This is because at lw CF cntent the resistance increases due t the frmatin f liquid film with cnductive aggregates which acts like membrane. It is cncluded that the IIR - CF cmpsites can be used as humidity sensr and shielding.

7 Egypt. J. Sl., Vl. (23), N. (1), (2000) 173 Effect f CF n Tensile strength - Mdulus, Elngatin and Hardness f IIR cmpsites Fig. (7 a, b) tensile strength and tensile mdulus f IIR cmpsites as a functin f CF cntent. It is clear that tensile strength and mdulus are increasing with CF cntent. Fig. (8 a, b) shws ptimum elngatin and hardness f IIR cmpsites at different CF cntent. It is clear that the elngatin and hardness increase with CF cntent. These results suggest that, CF imprves the hmgeneity by cnnective linkage amng aggregates and refines the micrstructure stability f IIR cmpsite [15]. Cnclusins CF acts as a catalyst, reduces the curing time, accelerates the driving frce, reactin kinetic rate during vulcanizatin prcess and imprves the micrstructral netwrk f IIR cmpsites. CF inhibits the swelling and the mechanism f diffusin which is f nn-fickian type. IIR cmpsites at lw CF cntent can used as humidity sensr while at high CF cntent can be used as humidity shielding. The electrical prperties are strngly affected by CF cntent. CF imprves the tensile strength - mdulus, elngatin and hardness f IIR cmpsites. Acknwledgment The authr is very grateful t Dr. F.El-Tantawy, Suez Canal University, Faculty f Science, Department. f Physics, fr his help during the experimental measurements and useful discussins. References 1. G. Wu, Plymer Jurnal, 29(9), 705, (1997). 2. D. Ch, Plymer Jurnal, 29(12), 959, (1997). 3. T. G. Gpakumar, Plymer Jurnal, 29(11), 884, (1997). 4. W. Hpark, Plymer Jurnal, 28(5), 672, (1996). 5. D. Saraydin, Plymer Jurnal, 29(8), 631, (1997). 6. J. Shan, Plymer Jurnal, 29(7), 580, (1997). 7. M. kazaki, Plymer Jurnal, 31(8), 672, (1999). 8. H. Tagachi, Physica B, 270, 325, (1999). 9. E. Iguchi, Physica B, 270, 332, (1999). 10. L. Karasek, Plym. J., 28(2), 121, (1996) 11. D. Ma, Slid state Cmmun., 112, 251, (1999).

8 F.S. Deghaidy H. H. Hassan, E. M. Abdel Barry, A. M. El-Lawindy, M. Ab-assy and F. El-Tantawy,Plymer Internatinal,30(3),371,(1993) 13. F. El-Tantawy and F. S.Deghaidy, Plymer Internatinal, 49,1-6(2000) 14. A.A. Hashem, J. f Applied plymer Sci., 42, 1082, (1991). 15. A. licea Claerei and F. J. U. Carrill, Plymer Testing, 16(5), 445, (1997). 16. K.M. Sumita, J. Material Sci., 31, 281, (1996). Appendix Fig.(1):The vulcanizatin time versus electrical cnductivity f IIR cmpsites with different cncentratins f CF at P = 300 kn/m2 and T = 175 C. Fig.(2):Shws the relatinship between crsslinking density (CD) and vlume fractin f rubber (Vr) against CF cntent.

9 Egypt. J. Sl., Vl. (23), N. (1), (2000) 175 Fig.(3): Shws the effect f CF n the electric resistance f IIR cmpsites during swelling in kersene at 20 C. Fig.(4): SEM phtgraph fr sample (F0) and sample (F6) after swelling in kersene fr 5 days.

10 F.S. Deghaidy 176 Fig.(5): Shws the mass swelling f IIR cmpsite as a functin f CF cnstant. Fig.(6): Shws the relatinship between relative humidity f IIR cmpsites and electric resistance as a functin f CF cntent.

11 Egypt. J. Sl., Vl. (23), N. (1), (2000) 177 (a) (b) Fig.(7): Tensile strength and tensile mdulus f IIR cmpsites as a functin f CF cntent. (a) (b) Fig.(8): Optimum elngatin and hardness f IIR cmpsites at different CF cntent.

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