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7 Article history: Poly(maleic acid) (PMA) was investigated as an anionic long chain dispersant for the preparation of highly
8 Received 13 April 2013 loaded aqueous alumina slurry. Suspensions with 1 wt% alumina powder were prepared through varia-
9 Received in revised form 13 May 2013 tion of PMA concentrations at pH 9 to assess its dispersion efficacy in aqueous medium. Addition of PMA
10 Accepted 16 May 2013
increased the stability of 1 wt% alumina suspensions as evidenced by higher zeta potential and RSH (rel-
11 Available online xxx
ative suspension height). 55 vol% alumina slurries were prepared with different PMA concentrations at
12
pH 9. Based on the rheological studies, 3.8 mg of PMA per gram of alumina was obtained as the optimized
13 Keywords:
dispersant amount at pH 9. All the slurries had shear thinning behavior and the slurry with optimum
14 Alumina
15 Dispersant dispersant amount had insignificant thixotropy. Further, adsorption of dispersant was evident by Fourier
16 Zeta-potential transform infrared spectroscopy (FTIR) analysis and thermogravimetric analysis (TGA). The slurry at pH Q3
17 Thixotropy 9 with optimum dispersant amount had lowest viscosity and easy flowability. Microstructure of bisque
18 Viscosity fired and sintered body by SEM microscopy revealed homogeneous particle distribution and uniform
19 Microstructure grain growth with sintered density of 3.94 g/cm3 . The mechanical property evaluation revealed that the
samples prepared with optimum dispersant amount had the flexural strength of 483 ± 22 MPa.
© 2013 The Ceramic Society of Japan and the Korean Ceramic Society. Production and hosting by
Elsevier B.V. All rights reserved.
22 Colloidal processing techniques have been widely used in near In aqueous colloidal processing of ceramics, the nature and 37
23 net shape forming of ceramics for diverse applications due to dif- amount of dispersant are important in order to obtain stable and 38
24 ficulty in controlling the microstructure by melt processing [1–3]. uniform dispersed system [11–13]. Well dispersed slurry with easy 39
25 High powder loading is important for slurry based colloidal pro- flowability is achieved by optimum concentration of the dispersant. 40
26 cessing to obtain high packing density of the green body facilitating Optimum amount of dispersant provides highest surface charge 41
27 minimum drying and sintering shrinkage which eventually reduces resulting in a homogeneous and well-stabilized suspension. It was 42
28 the warpage of the final components [4]. However, high powder reported that ceramic suspensions containing insufficient or excess 43
29 loading is difficult to achieve for fine powders due to high tendency amounts of dispersant than those with optimum show a rela- 44
30 of agglomeration. During slurry based colloidal processing, disper- tively higher viscosity [14]. The increase in viscosity with less than 45
31 sant has important role in the preparation of ceramic green body optimum dispersant concentration is due to insufficient surface 46
32 with uniform green density and homogeneous particle distribution coverage of the particles which facilitates formation of agglom- 47
33 [5–9]. A stable and well-dispersed colloidal suspension facilitates erates in the suspension through bridging flocculation. While in 48
34 high packing density in the green body. Uniform green density case of dispersant amount above the optimum concentration, the 49
Q2 ∗ Corresponding author. Tel.: +91 9434701616. In the context of slurry processing [15], Yasuda et al. [16] 53
E-mail addresses: sdhara@smst.iitkgp.ernet.in, santanudhara@gmail.com reported that the quantity of polymer dispersant has major 54
(S. Dhara). influence on microstructure and mechanical properties of bulk 55
Peer review under responsibility of The Ceramic Society of Japan and the Korean
hydroxyapatite during colloidal processing. Actually, high viscos- 56
Ceramic Society.
ity of the slurry will render difficulty in removal of air bubbles 57
Please cite this article in press as: S. Mohanty, et al., Poly(maleic acid) – A novel dispersant for aqueous alumina slurry, J. Asian Ceram.
Soc. (2013), http://dx.doi.org/10.1016/j.jascer.2013.05.005
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64 Among various dispersant types, anionic electrosteric disper- highly loaded slurries. Fourier transform infrared spectroscopy 129
65 sant such as poly(acrylic acid) [20], poly(methacrylic acid) [21], (FTIR) analysis and thermogravimetric analysis (TGA) were per- Q4 130
66 pyrophosphate [22], citric acid [23], etc. are mostly studied for formed to validate adsorption of the PMA on alumina powder 131
67 preparation of highly loaded ceramics (alumina, zirconia, silica, sil- surface. Density, microstructure and mechanical properties of the 132
68 icon carbide, etc.) based colloidal suspensions. The performance of sintered alumina prepared using 55 vol% slurry were evaluated for 133
69 the polyelectrolyte [24] dispersants is mainly influenced by sev- optimized dispersant amount at pH 9. 134
74 ries. Chain length and number of carboxylic groups per unit length
75 of poly anionic dispersant have influence on dispersion efficacy Alumina powder (RG 4000, Almatis Alumina Private Limited, 137
76 during slurry preparation. The carboxylic acid groups attached to Falta, India; d50 ∼ 0.7 m; surface area, 7 m2 /g) based aqueous slur- 138
77 the polymer chain are deprotonated at pH above pKa value, result- ries were prepared using PMA (PM-200, Aquapharm Chemicals 139
78 ing in an increase of surface charge of alumina in the suspension Pvt. Ltd., Pune, India) for dispersion and tetramethyl ammonium 140
79 due to adsorption of the negatively charged dispersant. At optimum hydroxide (25% solution, Merck, Mumbai, India) was used for pH 141
85 pension. was added to distilled water for the preparation of 1 wt% alumina 145
86 It is reported by Hanaor et al. [26] that small quantity of car- suspension at pH 9. The suspensions with different dispersant con- 146
87 boxylic acid reagent imparted high negative zeta potential values centrations (Table 1) were ultrasonicated for 10 min to breakdown 147
88 and stabilized ZrO2 suspension electrosterically over a wide pH the agglomerates. The suspensions were poured into graduated 148
89 range. Hidber et al. [27] successfully used citric acid as dispersant cylinder and were placed vertically for over a period of one month 149
90 for the deflocculation of concentrated alumina slurries. The interac- followed by measurement of turbidity and sediment height at dif- 150
91 tion of citric acid with alumina powder particles leads to adsorption ferent time intervals. Further, zeta potentials of all the suspensions 151
92 of citrate ions on the hydroxylated alumina powder surface result- with different dispersant amounts were measured by Zetasizer 152
93 ing in development of negative charge. The three carboxylic groups (Malvern instrument, Malvern, UK) at pH 9. 153
98 preparation of high solid loading ceramic slurries using ammonium ous alumina slurries, PMA was added initially to a poly(propylene) 156
99 polyacrylate as electrosteric dispersant at alkaline pH. Cesarano bottle containing predetermined amount of distilled water and alu- 157
100 and Aksay [29] described the dispersion of sufficiently highly con- mina powders were added in steps. In the present study, 55 vol% 158
101 centrated (>50 vol%) ␣-alumina powder (particle size 0.2–1.0 m) alumina slurries were prepared by addition of alumina in three 159
102 slurries using sodium poly(methacrylic acid) and poly(acrylic acid) steps in presence of varied amount of PMA and slurries were 160
103 at different pH for the fabrication of dense ceramic components. adjusted at pH 9. The slurries were milled by roll mill with addition 161
104 Poly(acrylic acid) is widely used dispersant in ceramic processing of 1:1 ratio of powder to ZrO2 milling media (3 mm diameter) at 162
105 due to its eletrosteric stabilization. 40 rpm. Finally, the slurries were filtered using sieve to separate the 163
106 In this context, poly(maleic acid) (PMA), being a poly car- milling media. For deairing of slurries, 100 l of n-octanol per 100 g 164
107 boxylic anionic macromolecules, is adsorbed on metallic oxides slurry was added followed by rolling at 20 rpm for 30 min using the 165
108 (like Goethites), carbonates (calcites) and forms a Langmuir mono- procedure discussed by Dhara et al. [18]. The deaired slurries were 166
109 layer as reported by Wang et al. [30] and Euvrard et al. [31]. It has ready for rheological measurement and casting. 167
110 also been utilized for boiler treatment as it stabilizes gypsum par- The effect of slurry pH on suspension stability was evaluated for 168
111 ticles in aqueous solution and inhibits crystal growth by adhering a constant dispersant concentration. Based on optimization study, 169
112 to the surface [32]. There are few preliminary reports on improve- 55 vol% alumina slurries with 3.8 mg PMA per gram of alumina 170
113 ment of rheology and zeta potential in chalcocite slurries even at powder were prepared at three different pH levels (viz., 6, 9 and 171
114 very high powder loading by addition of PMA [33]. Interestingly, 12, respectively). Flow behavior test of these slurries was carried Q5 172
115 PMA has similar structure to poly(acrylic acid) and this polymer has out to evaluate influence of slurry pH on viscosity at constant shear 173
116 double charge density than that of poly(acrylic acid) per unit chain rate. Further, slurries were diluted to 1 wt% by adding deionized 174
117 length owing to presence of one carboxylic acid group in each car- water and final suspension pH was maintained at their native pH 175
118 bon atom in the main back bone of the polymer chain. Maleic acid using TMAH and HCl. The zeta potentials of these suspensions were 176
119 has pKa values within 1.8–6 (pK1 = 1.83; pK2 = 6.07) [34,35] and its also measured to evaluate surface charge of alumina with constant 177
120 macromolecule (PMA) highly ionizes above pH 7 (pKa between 5 dispersant concentration at the above mentioned pH. 178
121 and 7) in aqueous medium [36]. This polymer has the potential to
122 disperse oxide ceramics for the preparation of colloidal suspension 2.4. Rheological measurement 179
125 for the stabilization of highly loaded alumina slurry. Dispersion poured into cylindrical cup of the rotational viscometer (Visco Elite, 181
126 ability of the PMA was primarily evaluated by RSH (relative sus- Fungilab, UK) along the wall and a spindle was placed carefully to 182
127 pension height), zeta potential measurement. Optimization of avoid entrapment of air bubbles. To prevent water loss during mea- 183
128 dispersant dose was carried out through rheological studies of surement, 5 drops of n-octanol were added on top the slurries. Prior 184
Please cite this article in press as: S. Mohanty, et al., Poly(maleic acid) – A novel dispersant for aqueous alumina slurry, J. Asian Ceram.
Soc. (2013), http://dx.doi.org/10.1016/j.jascer.2013.05.005
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Table 1
Effect of PMA concentrations on RSH, zeta potential and viscosity of alumina powders in aqueous medium at pH 9.
RSH (%) after one month Zeta potential (mV) Viscosity (Pa s) at (5.6 s−1 )
185 to measurement, the slurries were subjected to stirring by rotat- out and amount of PMA dispersant adsorbed on the surface of alu- 229
186 ing the spindle at 100 rpm to maintain similar condition prior to mina powder for suspensions with different PMA concentrations 230
187 measurement. Viscosity of the slurries was measured at different was calculated by the percentage weight loss during decomposition 231
188 shear rates ranging from 0.14 and 16.8 s−1 at 25 ◦ C from upward of organics by heat treatment. 232
surface of bisque fired samples was gold coated and analyzed via 237
194 ( ) at constant shear rate during downward ( ) and upward SEM (SEM; EVO ZEISS, Carl Zeiss SMT AG, Germany) at an accelerat- 238
(ῃdw) ing voltage of 10–20 kV for particles distribution in the green body. 239
Further, the green samples were also sintered at 1550 ◦ C for 2 h in 240
195 ( ) viscosity against shear rate measurement.
air by a chamber furnace (Bysakh, Kolkata, India) for microstructure 241
219 2.7. Thermogravimetric analysis were prepared using different concentrations of PMA at pH 9 and 266
220 TGA was carried out for analyzing quantitative adsorption of ferent shear rates. The shear rate sweep measurement of all the 268
221 PMA on alumina surface by Thermo-gravimetric analyzer (Perkin slurries indicated non-Newtonian flow behavior (shear thinning) 269
222 Elmer Pyris Diamond Model, MA) using alumina crucible under air owing to their high powder loading (Fig. 1a). It was also found that 270
223 atmosphere in the temperature range of 50–650 ◦ C with a heat- viscosities of the slurries were strongly influenced by the amount 271
224 ing rate of 10 ◦ C/min. Different slurries were diluted to 1 wt% using of PMA. As viscosity is function of shear rate, while viscosity values 272
225 deionized water and centrifuged to collect the precipitate. The alu- of all slurries were plotted against different PMA amounts at con- 273
226 mina precipitates after centrifugation and the as received alumina stant shear rate, all the curves passed through a minima at 3.8 mg 274
227 powders were vacuum dried at 40 ◦ C for a period of 24 h in a vacuum of polymer/g of alumina (Fig. 1b). At this PMA concentration, vis- 275
228 oven. Thermal degradation behavior of all the samples was carried cosity of the slurry was 1.6 Pa s at 5.6 s−1 shear rate. Further, above 276
Please cite this article in press as: S. Mohanty, et al., Poly(maleic acid) – A novel dispersant for aqueous alumina slurry, J. Asian Ceram.
Soc. (2013), http://dx.doi.org/10.1016/j.jascer.2013.05.005
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Fig. 1. Flow behavior and change in viscosity of 55 vol% alumina slurries (at pH 9) (a) at different shear rates; (b) with different PMA concentrations.
277 this dose, viscosity of the slurries increased gradually with increase showed shear thinning behavior against shear rate sweep mea- 302
278 in polymer concentrations. surement at room temperature. Viscosities of all the slurries were 303
279 The pseudoplastic behavior of highly loaded slurries was due to strongly influenced by pH with same dispersant concentration. 304
280 formation of inter-particle network at relatively lower shear rate. Among all the slurries, minimum viscosity was evident for slurry 305
281 With gradual increase in shear rate, this inter-particle network was prepared at pH 9. The slurry with pH 6 showed highest viscos- 306
282 transformed into small flowable clusters and resulted in reduction ity, whereas moderate viscosity was obtained for slurry with pH 307
283 of slurry viscosity. For different PMA concentrations, viscosity of the 12. The viscosity values of the slurries at pH 6, 9, and 12 were 308
284 slurries reduced gradually with increase in polymer concentrations 3.18 Pa s, 1.34 Pa s, and 2.46 Pa s, respectively, at constant shear rate 309
285 up to 3.8 mg/g of alumina mainly due to increase in zeta potential of 5.6 s−1 . This result was also supported by lower zeta potential 310
286 value associated with higher surface coverage. At lower concen- value of suspension prepared at pH 9 (Fig. 2a). Thixotropic behavior 311
287 tration of PMA, there is actually incomplete coverage of polymer of highly loaded alumina slurries (55 vol%) was strongly depen- 312
288 molecules leading to strong network formation via inter-particle dent on PMA concentrations (Fig. 3). In this study, three different 313
289 adsorption of long chain molecules. At 3.8 mg of PMA/g of alu- PMA concentrations, such as 2.3 mg (below optimum), 3.8 mg (opti- 314
290 mina, the suspended powder surface had the highest surface charge mum) and 5.3 mg (above optimum) per gram of alumina, were 315
291 (−55 mV) owing to monolayer coverage of polymers. Beyond this chosen to investigate their effect on thixotropic behavior. From the 316
292 amount, the excess un-adsorbed polymer molecules remained in plot in Fig. 3, it is evident that the slurry with optimum amount of 317
293 the aqueous solution and their counter ions minimized the sur- dispersant showed minimum thixotropy in comparison to below 318
294 face charge by compression of the double layers which resulted and above the optimum amount of dispersant. However, the slurry 319
295 in reduction of zeta potential value. From this fact, it can be con- with less than optimum amount of dispersant had pronounced 320
296 cluded that 3.8 mg of PMA/g of alumina is the optimum amount of thixotropy in comparison to more than optimum amount, even 321
297 dispersant for preparation of highly loaded slurry. These data are with same magnitude of deviation from the optimum dispersant 322
298 also supported by RSH and zeta potential values. concentration. Actually, tendency of inter-particle network forma- 323
299 Further, 55 vol% slurries with 3.8 mg/g of alumina were also tion is more with less than optimum amount of dispersant owing 324
300 prepared at different pH (6, 9 and 12) to evaluate effect of pH to their less surface coverage with respect to optimum and above 325
301 on flowability (Fig. 2b). All the slurries prepared at different pH optimum dispersant concentrations. However, slurry with more 326
Fig. 2. Influence of pH on (a) zeta potential and (b) viscosity of 55 vol% alumina slurries prepared using optimum amount of dispersant (3.8 mg PMA/g alumina).
Please cite this article in press as: S. Mohanty, et al., Poly(maleic acid) – A novel dispersant for aqueous alumina slurry, J. Asian Ceram.
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Fig. 3. Thixotropy of 55 vol% alumina slurries expressed as difference in viscosity Fig. 5. TGA–DTA of vacuum dried alumina powder and powder residues of dis-
persed alumina slurries with different concentrations of PMA, viz. below optimum,
(ῃuw)
optimum and above optimum.
1636 cm−1 is mainly associated with physisorbed water on the sur- 338
327 than optimum amount of dispersant had lowering of zeta potential face, and the peaks at 1401 cm−1 and 1384 cm−1 are due to surface 339
328 which facilitated relatively higher inter-particle interaction due to hydroxide [39]. For FTIR spectra of alumina with different amount 340
329 compression of double layer. of PMA, the peak at ∼1636 cm−1 and additional peak at ∼1573 cm−1 341
330 FTIR spectra of dried PMA, as received alumina and alumina are associated with asymmetric stretching vibration of carboxylate 342
331 with different PMA concentrations were plotted under transmit- ions [23] of the adsorbed PMA. There were also two more peaks 343
332 tance mode as shown in Fig. 4. Being a polycarboxylic acid, PMA has at 1401 cm−1 and 1384 cm−1 associated with symmetric stretch- 344
333 major characteristic peak at 1723 cm−1 for C O stretching vibra- ing vibration of carboxylate ion [23]. However, carbonyl stretching 345
334 tion of free molecules [38]. Additionally for COO− group, peaks at vibration peak at 1723 cm−1 for dried PMA was absent in case of 346
335 1633 cm−1 and 1557 cm−1 were assigned for asymmetric stretch- alumina containing adsorbed PMA. It is noteworthy that the peaks 347
336 ing vibration and peaks at 1487 cm−1 and 1400 cm−1 appeared due associated to carboxylate symmetric and asymmetric vibrations 348
were broadened for optimum and above optimum (3.8 mg/g and 349
Fig. 5 shows weight loss profile of vacuum dried alumina with 352
received alumina powder, 0.1% weight loss was evident mainly due 355
ance of two endothermic peaks at ∼100 ◦ C and ∼400 ◦ C was mainly 357
dispersant. Specifically, percent weight loss of 0.68, 0.98 and 1.0 362
was evidenced for below optimum, optimum and above optimum 363
that there was a significant increase in %weight loss with increase 365
whereas the increase in %weight loss was insignificant with beyond 367
the optimum level. Actually, with addition of more than optimum 368
Further, presence of exothermic peak in DTA curve was also evident 371
slurry into silicone rubber mold with optimum PMA concentra- 375
Fig. 4. FTIR spectra of (a) freeze dried PMA; (b) vacuum dried alumina powder;
vacuum dried powder residues from alumina slurries with (c) below optimum, (d) tion (3.8 mg/g) at pH 9. The vacuum dried samples were ready for 376
optimum and (e) above optimum amount of PMA (at pH 9), respectively. sintering and did not have any visual crack on the surface. All the 377
Please cite this article in press as: S. Mohanty, et al., Poly(maleic acid) – A novel dispersant for aqueous alumina slurry, J. Asian Ceram.
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Fig. 6. SEM micrographs of fracture surface of (a) green, (b) bisque fired and (c) sintered alumina at pH 9 with optimum dispersant amount.
378 samples were polished and sintered at 1550 ◦ C for 2 h. The sintered Conflict of interest statement 424
379 alumina prepared using optimum slurry did not develop any sig-
380 nificant warpages or cracks during sintering. All the samples had The authors declare that there are no conflicts of interest. 425
405 mina suspensions in presence of different PMA concentrations [17] C. Zha and H. Sun, J. Colloid Interface Sci., 162, 52–58 (1994). 453
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408 increase in zeta potential. Highly loaded alumina slurries with Uematsu, J. Eur. Ceram. Soc., 20, 389–395 (2000). 457
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462
412
(1996). 463
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Soc. (2013), http://dx.doi.org/10.1016/j.jascer.2013.05.005
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Please cite this article in press as: S. Mohanty, et al., Poly(maleic acid) – A novel dispersant for aqueous alumina slurry, J. Asian Ceram.
Soc. (2013), http://dx.doi.org/10.1016/j.jascer.2013.05.005