Carbon 43 (2005) 741747 www.elsevier.

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Electrical conductivity of carbon blacks under compression

nchez-Gonza lez a, A. Mac as-Garc a a, J. Sa b mez-Serrano M.F. Alexandre-Franco , V. Go
a

b,*

rea de Ciencia de Materiales e Ingenier a Metalu rgica, Escuela de Ingenier as Industriales, Universidad de Extremadura, 06071 Badajoz, Spain A b mica Inorga nica, Facultad de Ciencias, Universidad de Extremadura, Badajoz 06071, Spain Departamento de Qu Received 13 January 2004; accepted 25 October 2004 Available online 9 December 2004

Abstract A study was made of the electrical conductivity of six commercial carbon blacks under compression. The inuence of the applied pressure, sample volume, mechanical work, and density of the carbons was investigated. The conductivity was measured at room temperature by impedance spectroscopy over the frequency range 20106 Hz with a voltage of 1 V. The decrease in volume under compression depended signicantly on each particular carbon and on the applied pressure, and for a larger number of carbons it was only important at low pressures. The patterns of variation of the conductivity with pressure and mechanical work were similar. Of the pressure and volume eects comprised in the inuence of mechanical work on the conductivity, that of the pressure appeared to predominate. The increase in conductivity with decreasing sample volume was greater for the carbons in which the volume under compression was smaller. The total increase in conductivity was greater for the densest carbons and least for the lightest one. Both the conductivity and its variation under compression were positively related to the density of the carbons. 2004 Elsevier Ltd. All rights reserved.
Keywords: A. Carbon black; D. Electrical properties

1. Introduction Carbon black is the accepted generic name for a family of small particle size carbon pigments which are formed in the gas phase by thermal decomposition of hydrocarbons. Carbon blacks are currently sold in the form of hundreds of commercial grades which vary in particle size, aggregate size and shape, porosity, and surface chemistry. Their most important properties for inks, coatings, and plastics are related to the nal product appearance (e.g., blackness, tone, and tint), UV protection, and electrical conductivity [1]. The conductivity is also important for other applications of carbon

Corresponding author. Tel.: + 34 24 289300 9040; fax: + 34 24 289395. mez-Serrano). E-mail address: vgomez@unex.es (V. Go 0008-6223/$ - see front matter 2004 Elsevier Ltd. All rights reserved. doi:10.1016/j.carbon.2004.10.045

blacks, such as their use in electronic components, cables, electrodes, electrode additives, and so on [28]. The electrical applications of carbon materials including carbon black have been reviewed recently by Chung [8]. Since the establishment of the contact theory by Mrozowski and Holm [9,10], it has become clear that the electrical conductivity of a carbon black depends on the particles separation distance [1117] and on their average size [18,19]. It also depends to a certain extent on the level and nature of impurities on the carbon surface and on the presence of certain functional groups [18]. For thermal carbon blacks the conductivity generally increases with decreasing concentration of surface oxygen and sulfur functional groups, and is well correlated with the polyaromatic character [20]. Of the many factors inuencing the electrical conductivity of carbon black, electron tunneling is by far the most important as it involves the ability of electrons to

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jump the gaps between closely spaced carbon black aggregates. Since narrowing the gaps and increasing interaggregate contact should have important eects in increasing the electrical conductivity, there have been many studies of the electrical conductivity of carbon black under compression [19,2123]. Indeed, measurements of the electrical conductivity of compressed particles have been used to characterise granular and powdered materials [2427], in particular carbons [28 30]. The electrical conductivity shown by compressed carbon black particles is the result of a combination of a number of factors, including the electrical conductivity of the individual particles, the degree of contact between the particles, and their packing. A more appropriate factor than the particle size itself is the number of contacts between particles, as this establishes the number of channels available for the transport of electric current. Nevertheless, using the packing factor allows one to compare the eect of the various surface morphologies of the particles for dierent types of carbons. A number of theoretical studies have been carried out in order to estimate both the degree of contact and the packing of particles during compression, although only ideal situations considering the particles to be equal or roughly equal spheres have been reported [3133]. Real situations are considerably more complicated as they involve simultaneously not only the particle size distribution but also the possible morphological changes which may occur during the compacting step. A recent study by Celzard et al. [27] categorised a large number of powdery carbonaceous materials belonging to six morphology classes, including a carbon black consisting of spherical particles, into two major classes depending on the way their grains were packed, i.e., materials with roughly spherical interparticle voids and powders which were more densely packed, having attened voids. Under compression it is clear that the electrical conductivity of a carbon black will not only depend on its intrinsic morphological properties, which will determine the degree of packing of the material and hence the change in density, but also on such extrinsic factors as the applied pressure. The contact resistances, for instance, are pressure dependent. Thus, according to Holms standard text [10], the conductance is four times the contact area divided by the sum of the resistivities of the two materials in contact, i.e., G = 4a/(r1 + r2). Given these facts therefore, in the present study the inuence of the applied pressure, volume change under compression, mechanical work, and density on the electrical conductivity is investigated for a broadly varied series of six commercial carbon blacks. There has been a recent study in the same line of the electrical properties of ve carbon blacks of dierent origin (plasma, partial combustion, and activated) by Probst and Grivei [34].

2. Experimental 2.1. Materials and surface area The carbon blacks used, Sterling V (SV), Vulcan 3 (V3), Vulcan 6 (V6), Black Pearls 880 (BP880), Black Pearls 1300 (BP1300), and Black Pearls 2000 (BP2000), were provided by Cabot Corp. (Spain). The materials as received were sized, and the fraction of diameter less than 0.32 mm was chosen. The particle size and structure of the carbons [35] are listed in Table 1. The overall resistivity of carbon black is obtained from the sum of all the aggregate resistances and interaggregate resistances [36]. Essentially, the resistance is a function of the matter-free space in the carbon sample. This space comprises not only the interaggregate voids but also the porosity corresponding to the intraaggregate and particle voids. For porous solids, such as carbon black, the microporosity (pores of width less than 2 nm [37]) has usually the greatest contribution to the surface area. But, together with the surface area, the surface chemistry and topology of carbon blacks also inuence their electrical properties [38]. In the present study, the specic surface area of the carbons (SBET) was estimated by applying the Brunauer, Emmett and Teller equation [39] to the N2 adsorption isotherms measured at 196 C, using a Micromeritics ASAP 2000 surface area analyser [40]. The values of SBET are listed in Table 1. 2.2. Electrical conductivity measurements Following a standard procedure [20,41], the electrical conductivity (r) was measured at room temperature by impedance spectroscopy over the frequency range 20 106 Hz with a voltage of 1 V, using the experimental arrangement schematised in Fig. 1 [27]. The masses of carbon used, after oven-drying at 100 C overnight, ranged between 0.0408 g for BP2000 and 0.0989 g for V6 (Table 1). A much smaller mass of BP2000 was used because of its lower density and hence greater volume. Each sample was placed in a hollow glass cylinder (inner

Table 1 Properties of the carbon blacks and sample masses Carbon SV V3 V6 BP880 BP1300 BP2000 SBET (m2 g1) 37 80 114 224 511 1443 Particle size (nm) 50 27 22 16 13 15 Structurea Medium-low Medium Medium-high Low High High m (g) 0.0924 0.0947 0.0989 0.0944 0.0977 0.0408

a The number of particles making up the primary aggregate gives the structure: the greater the number of particles per aggregate, the bulkier the aggregate, and thus the higher the structure of the carbon black.

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0.030

743

0.025

Volume (cm 3 )

0.020

0.015

0.010

Fig. 1. Apparatus to measure the conductivity.

0.005

SV V3 V6 BP880 BP1300 BP2000

0 100 200 300 400 500 600 700 800

0.000

diameter = 0.8 cm), and compressed in air between two commercial brass pistons forming the electrodes, the upper one movable and the lower one xed. The pressures were varied between 6.15 and 742 kPa by placing dierent loads on the upper piston. A cathetometer was used to measure the small changes produced in the height of the carbon bed. The conductivity was measured using an LCR meter (Quadtech, model 1920). After a series of preliminary tests, 15 min were allowed prior to making the conductivity measurements to avoid any transient eect of sample relaxation. The dielectric response (i.e., the complex impedance), from which the electric conductivity was obtained, was determined in the frequency range between 20 Hz and 1 MHz. The four probes, IL, IH, VL, and VH, were connected to the electrodes as shown in Fig. 1. Conduction was Ohmic, so that the electrical conductivity was given by r l=RA 1 where R is the electrical resistance in X, A the area of the piston surface in m2, and l the distance between the two pistons in the chamber in cm [30]. The electrical conductivity of the high-surface-area carbon black BP2000 has been measured before by microwave techniques [42]. The volume and density of the compressed sample were determined from a measurement of the height of the carbon column.

Pressure (kPa)
Fig. 2. Volume versus applied pressure.

3. Results and discussion 3.1. Change in the sample volume under compression

Similar behaviour to that exhibited by BP2000 has been observed recently for another activated carbon black with a high specic surface area [34]. Therefore, the extent of surface area of the carbons is not the predominant factor in the magnitude of the change in V produced by compression. Neither is it the microporosity of the carbons, since for porous solids the surface area is concentrated largely in the micropores. Perhaps the mesoporosity and the macroporosity of the carbons play a more important role. In fact, the mesopore volume, the macropore volume, and the total pore volume are as a rule higher for V6 and BP2000 than for the rest of the carbons [40]. Also, how close the packing comes to the ordered stacking of hard spheres will also inuence the evolution of V. In connection with the degree of occupancy in carbon black, it should be noted that values of 0.342 g cm3 for the apparent density of uncompacted powder and of 0.80 g cm3 for the apparent density of its particles have been reported [27]. The particle size is smaller for V6 than for V3 and SV, and somewhat larger for BP2000 than for BP1300. Finally, the aggregate structure is medium-high for V6 and high for BP2000 (Table 1). At high P values, V varied in the sequence SV < BP1330 < V3 < BP880 < V6 < BP2000. 3.2. Study of the electrical conductivity

Fig. 2 shows the variation of the sample volume (V) with applied pressure (P). It is seen that for most carbons the variation in V is only important at low P values, below 25 kPa. At such P values V was smaller as follows: SV  BP1300 < V3  BP880 < V6 < BP2000. At higher pressures, the decrease in V with increasing P was more signicant for BP2000 and V6. The carbons BP2000 and V6 have a very dierent degree of development of their surface area (see Table 1) as SBET is equal to 114 m2 g1 for V6 and to 1443 m2 g1 for BP2000.

Table 2 lists the values of the electrical conductivity (r) measured for the carbons at two P values, P = 25 kPa (r1) and P = 742 kPa (r2). One notes that r1 was much lower for BP2000 than for the rest of the carbons. Also, the value of r2 was high for SV and BP1300 and low for BP2000, with V3, V6, and BP880 presenting intermediate values. The table also gives the percentage increase in the electrical conductivity (PIEC), dened as (r2 r1)/r1 100.

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Table 2 Electrical conductivity of the carbon blacks at two pressure valves Carbon SV V3 V6 BP880 BP1300 BP2000
a

r1/(X m)1P = 25 kPa 21.2 38.0 26.2 32.0 34.1 7.0

r2/(X m)1 P = 742 kPa 214.6 157.6 115.4 151.3 251.2 44.7

PIECa 912 315 340 373 637 539

Table 2. These range from 315 for V3 to 912 for SV. The order of the variation is SV > BP1300 > BP2000 > BP880 > V6 > V3. The plots of r divided by the density against P for the various carbons were almost identical to those of r against P in Fig. 3. They have therefore been omitted for the sake of brevity. 3.2.2. Variation of r with volume The volume of the sample under compression can be regarded as an intrinsic property of each carbon. One observes in Fig. 4 that r was more sensitive to the volume change for BP1300 and SV than for the other carbons, especially for BP2000. The evolution of r with decreasing volume was similar for BP1300 and SV. However notice that at a given volume the increase in r was usually signicantly greater for SV than for BP1300. The values of r at intermediate volumes for V3, V6, and BP880 were close to each other. Figs. 3 and 4 show that the relative magnitude of r depends as a rule on whether the plot is against P or V. For example, r is signicantly higher for BP1300 than for SV over a wide P range, whereas the opposite is the case for these carbons over a wide V range. For V3 and BP880, r is nearly identical over almost the entire P range, but higher for V3 or BP880 according to the value of V. 3.2.3. Variation of r with mechanical work The opposing eects of P and V on r can be combined and analysed together by plotting r against the mechanical work (MW). To this end, MW was estimated using the expression [34] MW
i X j 1

Percentage increase in electrical conductivity.

3.2.1. Variation of r with pressure Fig. 3 shows plots of r against the extrinsic factor P. The electrical conductivity varied in the order: BP1300 > SV > V3  BP880 > V6 > BP2000 over a wide P range. Because the measured volume of sample at low pressures was signicantly smaller for SV and BP1300 than for BP2000 and V6 and similar for V3 and BP880, the electrical conduction was favoured in these carbons by a smaller volume. Indeed, a good linear relationship has been observed between the specic volume and the electrical resistivity of furnace blacks [43]. The conductivity r was markedly inuenced by the applied pressure. At low values of P, up to P  50 kPa, r was low and similar in value for most of the carbons. For BP2000, however, r was signicantly lower than for the rest of the carbons. At higher P, up to 100200 kPa, the greatest increase in r occurred for SV and BP1300. Since for a number of carbons, especially SV and BP1300, the volume change was greater at P < 25 kPa, the results indicate that only after the carbons have undergone an initial volume reduction is further compression more eective in increasing their electrical conductivity. The eect of the increase in P on r was very strong for all six carbons, as is shown by the PIEC values in

p j A h j 1 h j

300

Electrical conductivity ( -1m-1)

Electrical conductivity ( -1m-1)

200

SV V3 V6 BP880 BP1300 BP2000

300

250

200

150

SV V3 V6 BP880 BP1300 BP2000

100

100

50

0 0 200 400 600 800

0 0.012

0.016

0.020

0.024

0.028

Pressure (kPa)
Fig. 3. Electrical conductivity versus pressure.

V(cm )
Fig. 4. Electrical conductivity versus volume.

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745

where A is the piston surface area, and pj is the pressure required to cause the change in height hj1 hj in the carbon bed. The value of MW represents the resistance presented by the carbon bed to the reduction in volume by compression. Expression (2) is fully valid for a homogeneous medium. For non-homogeneous media, however, its applicability may be called into doubt as it does not take into account the eects of orientation of the grains and of pressure inhomogeneities in the carbon bed. Such eects depend on the kind of carbonaceous material (e.g., coconut shell active carbon, pinewood active carbon, articial graphite, or carbon black), the bed height, and the applied compacting pressure [27]. For carbon black, in particular, there appears a conductivity maximum at low values of the height that is better dened at high pressures. In the present study, for the results to be comparable, only a narrow range of initial heights of the powder column between 3.5 and 5.5 cm were used, and the pressure range was the same for all six carbons. Fig. 5 depicts the variation of r with MW. For each carbon, the rMW plot closely resembles the rP plot (Fig. 3) but not the rV plot (Fig. 4), indicating that the applied pressure rather than the volume of the sample is the predominant factor in the variation of r with MW. This is attributable to the fact that a large increase in P is needed to produce a small decrease in the volume of the sample. Nevertheless, it should be noted that the rMW plot for BP880 is situated signicantly above that of V3, whereas the rP plots for these carbons (Fig. 3) lie close to each other, with that for BP880 being even slightly below that for V3. These results show that r is more sensitive to the increase in MW than in P, and that therefore the discrimination between the carbons is better when MW is used. The greater r for BP880 as compared to V3 is likely connected to the dependence of r on V, since, as one infers from

Fig. 4, for a given value of V below approximately 0.023 cm3, r is noticeably greater for BP880 than for V3. 3.2.4. Variation of r with density The density is another intrinsic property of each carbon. Fig. 6 shows the conductivity versus density. This density, as measured, must be regarded as an estimate of the bulk density, since not even at the highest P value can one be sure that the total void space between the carbon particles has been entirely excluded from the volume of the sample. Obviously then, this density is lower than the apparent density (i.e., that measured using mercury [44]), and increases with increasing pressure to approach the latter. Fig. 6 shows that the total variation in r with the increase in density by compression of the samples depends strongly on the density of the carbons. Roughly, the increase in r is in the order BP1300, SV > V3, V6, BP880 > BP2000. Furthermore, the increase in r usually attens out after reaching a certain density. This occurs at lower densities for V6 than for V3 and BP880, and at similar densities for SV and BP1300. For BP2000, however, the variation of r is somewhat more marked at the highest densities, as shown by the increasing slope of the plot in Fig. 6. Carbon black morphology is usually described in terms of particles and aggregates. An aggregate is a discrete, rigid colloidal entity that is the smallest dispersible unit; it consists of extensively coalesced particles. A carbon black particle is a small spheroidal, paracrystalline, non-discrete component of an aggregate; it is separable from the aggregate only by fracturing [36]. The electrical conductivity and its variation with increasing density of the carbons may be explained on the basis of the morphology of carbon black, as seen below. The electrical conductivity depends on the number of eective electrical contacts that are established between the carbon particles. If one assumes that the mean

300

300

Electrical conductivity ( -1m-1)

Electrical conductivity ( -1m-1)

250

200

150

SV V3 V6 BP880 BP1300 BP2000

200

SV V3 V6 BP880 BP1300 BP2000

100

100

50

0 0.000

0
0.004 0.008 0.012 0.016

0.0

0.2

0.4

0.6
-3

0.8

Mechanical work (J)

Fig. 5. Electrical conductivity versus mechanical work.

Density (g cm )
Fig. 6. Electrical conductivity versus density.

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atomic mass of the constituent elements (i.e., mostly carbon and hydrogen and heteroatoms such as oxygen) is similar for all the carbons, then the number of electrical contacts is primarily a function of just the density of the carbons, since the greater the density, the closer the carbon particles and the less void space between the particles, or electrical resistance. Under compression, the number of electrical contacts increases due to the forced approach of the particles belonging to neighbouring aggregates. Again, the likelihood of contact between the carbon particles is greater for the denser carbons. For such carbons, since the carbon particles are closer, a smaller increase in density would result in a larger increase in electrical conduction. In the carbon blacks, the mass per volume unit is concentrated in particles of dierent sizes and these particles conform aggregates of dierent structures (Table 1). This means that not only the density of the carbons but also their morphology inuences their electrical conductivity (as is well known, the density depends on the orderliness of the packing of the aggregates, and this should be greater when the particle size and aggregate structure are smaller). Larger particle size and higher aggregate structure must favour the electrical conductivity since the probability of contact between the carbon particles should be greater in both cases. From the evolution of r with density (Fig. 6) for SV (large particles, medium-low structure) and BP1300 (small particles, high structure), the aggregate structure appears to be a stronger factor than the particle size. For the pair of carbons V3 and BP880, in which the morphological dierences are less pronounced than in SV and BP1300, the two eects may cancel out so that the variation of r is similar over a certain density interval. The smaller increase in r with increasing density at high densities for most carbons (Fig. 6) denotes that either the inter-penetration of aggregates or the contact between particles is no longer eective at increasing the electrical conduction. Because this plateau eect of a slower rise in r commences at a lower density for V6 than for V3 and BP880, and since the aggregate structure is higher for V6, the structural eect seems to be responsible for the weaker change in r. In fact, V6 possesses a particle size practically intermediate between the V3 and BP880 sizes. For SV and BP1300, the slope of the plots showing the slow-down in the increase of r at the highest densities is almost identical, the size and structure eects appear to compensate each other. The much weaker eect of compression on r for BP2000, even though this carbon is highly structured, is attributable to its low density, and hence the dispersion of the aggregates. In other words, although the aggregates are large in size, they do not make contact eectively due to the low density of the carbon. Also, the small size of the particles may hinder contact

between particles of dierent aggregates, except for the highest applied pressures. Other factors that are likely to aect the electrical conductivity of carbon blacks, but have not been investigated here, are the particle morphology [27] and the surface chemistry and topology [38]. In connection with the morphology, it should be kept in mind that a concentration of the mass of the carbon particles in the compression direction should facilitate their contact with particles of neighbouring aggregates and hence increase the electrical conductivity of the carbon. Contact will also be facilitated by the roughness of the particle surface. Moreover, since the presence of pores in the carbons will act as an electrical resistance, as was noted above, the electrical conductivity should decrease as the pore volume increases. Compression may crush pores, so that opposite pore walls make contact, thereby increasing the conductivity. Finally, as was noted in Section 3.2.3, orientation of the grains and the resulting pressure inhomogeneity may also inuence the electrical conductivity of the carbons.

4. Conclusion The volume change under compression was only important at low pressures for a larger number of carbons. There was a similar pattern in the variation of the conductivity with pressure and mechanical work. Of the opposing eects of pressure and volume involved in the dependence of the conductivity on the mechanical work, the eect of pressure appeared to predominate. The inuence of the decrease in the sample volume under compression on the conductivity was more marked for the carbons in which the volume was smaller. The increase in conductivity with increasing density was greater for the densest carbons, and least for the lightest carbon. The conductivity and its variation under compression were directly related to the density of the carbons.

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