Browse > Article
http://dx.doi.org/10.9713/kcer.2019.57.1.133

Synthesis and Characterization of High Surface Area of Zirconia: Effect of pH  

Jeong, Ye-Seul (Department of Chemical Engineering, Chungbuk National University)
Shin, Chae-Ho (Department of Chemical Engineering, Chungbuk National University)
Publication Information
Korean Chemical Engineering Research / v.57, no.1, 2019 , pp. 133-141 More about this Journal
Abstract
High specific surface area zirconia with acid-basic property was synthesized by precipitation using reflux method or hydrothermal synthesis method using ammonium hydroxide solution as precipitant in the range of pH of Zr solution from 2 to 10. The prepared zirconia was characterized by the nitrogen adsorption, X-ray diffraction (XRD), isopropanol temperature programmed desorption (IPA-TPD), scanning electron microscopy and X-ray photoelectron spectroscopy, and the catalytic activity in the IPA decomposition reaction was correlated with the acid-basic properties. When using reflux method, high pH of Zr solution was required to obtain high fraction of tetragonal zirconia, and pure tetragonal zirconia was possible at pH 9 or higher. High pH was required to obtain high specific surface area zirconia, and the hydrous zirconia synthesized at pH 10 had high specific surface area zirconia of $260m^2g^{-1}$ even after calcination at $600^{\circ}C$. However, hydrothermal synthesis with high pressure under the same conditions resulted in very low specific surface area below $40m^2g^{-1}$ and monoclinic phase zirconia was synthesized. High pH of the solution was required to obtain high specific surface area tetragonal phase zirconia. In hydrothermal synthesis requiring high pressure, monoclinic zirconia was produced irrespective of the pH of the solution, and the specific surface area was relatively low. Zirconia with high specific surface area and tetragonal phase was predominantly acidic compared to basicity and only propylene, which was observed as selective dehydration reaction in IPA decomposition reaction, was produced.
Keywords
Zirconia; PH effect; High specific surface area; Acidity; IPA decomposition;
Citations & Related Records
Times Cited By KSCI : 1  (Citation Analysis)
연도 인용수 순위
1 Ren, T.-Z., Yuan, Z.-Y. and Su, B.-L., "Hierarchical Microtubular Nanoporous Zirconia with an Extremely High Surface Area and Pore Volume," Chem. Phys. Lett., 388, 46-49(2004).   DOI
2 Sim, H.-I., Park, J.-H., Cho, J. H., Ahn, J.-H., Choi, M.-S. and Shin, C.-H., "The Effect of the Crystalline Phase of Zirconia for the Dehydration of Iso-Propanol," Korean Chem. Eng. Res., 51, 208-213(2013).   DOI
3 Stichert, W. and Schuth, F., "Influence of Crystallite Size on the Properties of Zirconia," Chem. Mater., 10, 2020-2026(1998).   DOI
4 Hong, E., Baek, S. W., Shin, M., Suh, Y.-W. and Shin, C.-H., "Effect of Aging Temperature During Refluxing on the Textural and Surface Acidic Properties of Zirconia Catalysts," J. Ind. Eng. Chem., 54, 137-145(2017).   DOI
5 Liu, S., Wu, X., Tang, J., Cui, P., Jiang, X., Chang, C., Liu, W., Gao, Y., Li, M. and Weng, D., "An Exploration of Soot Oxidation over $CeO_2$-$ZrO_2$ Nanocubes: Do More Surface Oxygen Vacancies Benefit the Reaction?," Catal. Today, 281, 454-459(2017).   DOI
6 Shuang, L., Xiaodong, W., Duan, W. and Rui, R., "Ceria-Based Catalysts for Soot Oxidation: A Review," J. Rare Earths, 33, 567-590(2015).   DOI
7 Fino, D., Bensaid, S., Piumetti, M. and Russo, N., "A Review on the Catalytic Combustion of Soot in Diesel Particulate Filters for Automotive Applications: From Powder Catalysts to Structured Reactors," Appl. Catal. A: Gen., 509, 75-96(2016).   DOI
8 Liu, A., Nyavor, K., Li, Z. and Egiebor, N. O., "Effects of Composition and Calcination Temperature on Morphology and Structure of Barium Modified Zirconia Nanoparticles," Mater. Sci. Eng. A, 366, 66-73(2004).   DOI
9 Asadikiya, M. and Zhong, Y., "Oxygen Ion Mobility and Conductivity Prediction in Cubic Yttria-Stabilized Zirconia Single Crystals," J. Mater. Sci., 53, 1699-1709(2018).   DOI
10 Duwez, P., Odell, F. and Brown Jr, F. H., "Stabilization of Zirconia with Calcia and Magnesia," J. Am. Ceram. Soc., 35, 107-113 (1952).   DOI
11 Ma, H., Kong, Y., Hou, W. and Yan, Q., "Synthesis of Ordered Hexagonal Porous Tin-Doped Zirconium Oxides with a High Surface Area," Microp. Mesop. Mater., 7, 241-243(2005).
12 Li, P., Chen, I. W. and Penner-Hahn, J. E., "Effect of Dopants on Zirconia Stabilization-an X-Ray Absorption Study: I, Trivalent Dopants", J. Am. Ceram. Soc., 77, 118-128(1994).   DOI
13 Jung, K. T. and Bell, A. T., "The Effects of Synthesis and Pretreatment Conditions on the Bulk Structure and Surface Properties of Zirconia," J. Mol. Catal. A: Chem., 163, 27-42(2000).   DOI
14 Li, P., Chen, I. W. and Penner-Hahn, J. E., "Effect of Dopants on Zirconia Stabilization-an X-Ray Absorption Study: II, Tetravalent Dopants," J. Am. Ceram. Soc., 77, 1281-1288(1994).   DOI
15 del Monte, F., Larsen, W. and Mackenzie, J. D., "Stabilization of Tetragonal $ZrO_2$ in $ZrO_2$-$SiO_2$ Binary Oxides," J. Am. Ceram. Soc., 83, 628-634(2000).   DOI
16 Pyen, S., Hong, E., Shin, M., Suh, Y.-W. and Shin, C.-H., "Acidity of Co-Precipitated $SiO_2$-$ZrO_2$ Mixed Oxides in the Acid-Catalyzed Dehydrations of Iso-Propanol and Formic Acid," Mol. Catal., 448, 71-77(2018).   DOI
17 Yamaguchi, T., "Application of $ZrO_2$ as a Catalyst and a Catalyst Support," Catal. Today, 20, 199-217(1994).   DOI
18 Kim, T. W., Park, S., Oh, J., Shin, C.-H. and Suh, Y. W., "Hydrogenation of the LOHC Compound Monobenzyl Toluene over $ZrO_2$-Supported Ru Nanoparticles: A Consequence of Zirconium Hydroxide's Surface Hydroxyl Group and Surface Area," ChemCatChem, 10, 3406-3410(2018).   DOI
19 Miura, N., Sato, T., Anggraini, S. A., Ikeda, H. and Zhuiykov, S., "A Review of Mixed-Potential Type Zirconia-Based Gas Sensors," Ionics, 20, 901-925(2014).   DOI
20 Kouva, S., Honkala, K., Lefferts, L. and Kanervo, J., "Monoclinic Zirconia, Its Surface Sites and Their Interaction with Carbon Monoxide," Catal. Sci. Technol., 5, 3473-3490(2015).   DOI
21 Kijenski, J. and Baiker, A., "Acidic Sites on Catalyst Surfaces and Their Determination," Catal. Today, 5, 1-120(1989).   DOI
22 Kisi, E. H. and Howard, C., "Crystal Structures of Zirconia Phases and Their Inter-Relation," Key Eng. Mater., 153-154, 1-36(1998).   DOI
23 Guisnet, M. R., "Model Reactions for Characterizing the Acidity of Solid Catalysts," Acc. Chem. Res., 23, 392-398(1990).   DOI
24 Aramendiia, M. A., Borau, V., Jimenez, C., Marinas, J. M., Marinas, A., Porras, A. and Urbano, F. J., "Synthesis and Characterization of $ZrO_2$ as Acid-Basic Catalysts: Reactivity of 2-Methyl-3-Butyn-2-Ol," J. Catal., 183, 240-250(1999).   DOI
25 Li, Y., He, D., Zhu, Q., Zhang, X. and Xu, B., "Effects of Redox Properties and Acid-Base Properties on Isosynthesis over $ZrO_2$-Based Catalysts," J. Catal., 221, 584-593(2004).   DOI
26 Zhang, H., Ng, C. F. and Lai, S. Y., "Catalytic Decomposition of Chlorodifluoromethane (HCFC-22) over Platinum Supported on $TiO_2$-$ZrO_2$ Mixed Oxides," Appl. Catal. B: Environ., 55, 301-307 (2005).   DOI
27 Hong, E., Kim, C., Lim, D.-H., Cho, H.-J. and Shin, C.-H., "Catalytic Methane Combustion over $Pd/ZrO_2$ Catalysts: Effects of Crystalline Structure and Textural Properties," Appl. Catal. B: Environ., 232, 544-552(2018).   DOI
28 Guerrero, S., Araya, P. and Wolf, E. E., "Methane Oxidation on Pd Supported on High Area Zirconia Catalysts," Appl. Catal. A: Gen., 298, 243-253(2006).   DOI
29 Park, J.-H., Cho, J. H., Kim, Y. J., Kim, E. S., Han, H. S. and Shin, C.-H., "Hydrothermal Stability of $Pd/ZrO_2$ Catalysts for High Temperature Methane Combustion," Appl. Catal. B: Environ., 160, 135-143(2014).   DOI
30 Pecchi, G., Reyes, P., Gomez, R., Lopez, T. and Fierro, J., "Methane Combustion on $Rh/ZrO_2$ Catalysts," Appl. Catal. B: Environ., 17, L7-L13(1998).   DOI
31 Yue, Y., Zhao, X., Hua, W. and Gao, Z., "Nanosized Titania and Zirconia as Catalysts for Hydrolysis of Carbon Disulfide," Appl. Catal. B: Environ., 46, 561-572(2003).   DOI
32 Afanasiev, P., Thiollier, A., Breysse, M. and Dubois, J., "Control of the Textural Properties of Zirconium Oxide," Top. Catal., 8, 147-160(1999).   DOI
33 Chuah, G., Jaenicke, S. and Pong, B., "The Preparation of High-Surface-Area Zirconia: II. Influence of Precipitating Agent and Digestion on the Morphology and Microstructure of Hydrous Zirconia," J. Catal., 175, 80-92(1998).   DOI
34 Chuah, G. and Jaenicke, S., "The Preparation of High Surface Area Zirconia-Influence of Precipitating Agent and Digestion," Appl. Catal.: A Gen., 163, 261-273(1997).   DOI
35 Stöcker, C. and Baiker, A., "Zirconia Aerogels: Effect of Acid-to-Alkoxide Ratio, Alcoholic Solvent and Supercritical Drying Method on Structural Properties," J. Non-Cryst. Solids, 223, 165-178(1998).   DOI