水热法制备纳米ZrO_2粉体的条件
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摘要
采用ZrOCl_2·8H_2O、NH_3·H_2O为原料制备水热反应前驱物,以矿化剂(K_2O_3、KOH)溶液作为水热介质,PEG为分散剂,通过水热法合成纳米氧化锆粉末,利用XRD、SEM等分析测试手段对纳米ZrO_2粉末的物相组成、微观形貌、团聚现象等进行表征和分析.研究了PH值,水热反应温度,矿化剂含量,分散剂含量等对其物相组成、微观形貌、团聚现象的影响并提出相应解决方案.结果表明:在PH值为9、水热反应温度为230℃、分散剂(PEG)质量分数为1.5%、矿化剂(K_2O_3、KOH)比例K_(K_2O_3)/KOH=3:1的条件下,可制备出分散性良好,粉体粒径约为20 nm的纳米ZrO_2粉末.
Nano-sized ZrO_2 powders were synthesized by hydrothermal method using ZrOCl_2·8H_2O and NH_3·H_2O as hvdrotheraml precursor raw materials and(K_2O_3、KOH) water/mineralizer solutions as hydrothermalmedium;PEG as dispersant.The phase constitution、agglomerationand and physical properties of ZrO_2 powders were tested by the X-ray diffraction(XRD),Scanning electron microscope(SEM).The effects of PH value,hydrothermal reaction temperature and concentration of mineralizers and dispersant on the agglomeration of nano-sized ZrO_2 powders were investigated and some solutions were suggested accordingly.The result shows:well dispersed powder particle size of about 20 nm nano ZrO_2 powder can be prepared by the solution which PH value of 9,the hydrothermal reaction temperature is 230℃,dispersing agent(PEG) content of 1.5%,mineralizer(K_2O_3,KOH) ratio K_(K_2O_3/KOH) is 3:1.
Nano-sized ZrO_2 powders were synthesized by hydrothermal method using ZrOCl_2·8H_2O and NH_3·H_2O as hvdrotheraml precursor raw materials and(K_2O_3、KOH) water/mineralizer solutions as hydrothermalmedium;PEG as dispersant.The phase constitution、agglomerationand and physical properties of ZrO_2 powders were tested by the X-ray diffraction(XRD),Scanning electron microscope(SEM).The effects of PH value,hydrothermal reaction temperature and concentration of mineralizers and dispersant on the agglomeration of nano-sized ZrO_2 powders were investigated and some solutions were suggested accordingly.The result shows:well dispersed powder particle size of about 20 nm nano ZrO_2 powder can be prepared by the solution which PH value of 9,the hydrothermal reaction temperature is 230℃,dispersing agent(PEG) content of 1.5%,mineralizer(K_2O_3,KOH) ratio K_(K_2O_3/KOH) is 3:1.
引文
[1]YAMAMOTO O,ARATI Y,TAKEDA Y,et al.Electrical Conductivity or Stabilized Zirconia with Ytterbia and Scandia[J].Solid State Ionics 1995,79:137-142.
[2]LEE D S,KIM W S,CHOI S H,et al.Characterization of ZrO_2 codoped with Sc_2O_3 and CeO_2 Electrolyte for the Application of Inter-mediate Temperature SOFCs[J].Solid State Ionics,2005,176(1/2):33-39.
[3]李其连.等离子喷涂ZrO_2热障涂层热冲击破坏研究[J].中国表面工程,2004,3:17-25.
[4]Abd El-latif M M,SHOWMAN M S,IBRAHIM A M,et al.Optimizing the Preparation Parameters of Nanocrystalline Zirconia for Catalytic applications[J].Acta Metallurgica Sinica 2013,26(5):565-573.
[5]VOLLATH D,FISCHER F D,HAGELSTEIN M,et al.Phases and Phase Thansformation in Nanocrystaline ZrO_2[J].Journal of Nanoparticle Research,2006,8:1003-1016.
[6]Jun-Seop KIM,Dong-Hae LEE,Sung KANG,et al.Synthesis and microstructure of Zirconia Nanopowders by Glycothermal Processing[J].Transactions of Nonferrous Meters Society of China,2009,19:88-91.
[7]KHORRAMIE S A,BAGHCHESARA M A,Gohari D P.Fabrication of Aluminum Matrix Composites Reinforced with Al_2ZrO_5 nano Particulates Synthesized by sol-gel auto-combustion method[J].Transactions of Nonferrous Meters Society of China,2013,23:1556-1562.
[8]Lei YUAN,Dong Xiang,JING-kun Yu.Effect of solvents on the Properties of co-precipitated MgO-ZrO_2 Nano Powders[J].Journal of Ceramic Processing Research,2013,14(4):517-520.
[9]敖红敏,俞耀伦,龙志奇,等.超细锆基复合氧化物粉体制备方法概述[J].稀有金属,2013,37(2):302-311.
[10]PRAKASHBABU D,HARI KRISHNA R,NAGABHUSHANA B M,et al.Influence of precursors on Photoluminescence of hydrothermally derived ZrO_2[J].Journal of Chemical Engineering and Research,2014,2(1):105-111.
[11]李茹民,李占双,辛艳风,等.纳米二氧化锆制备方法进展[J].应用科技,2001,28(9):52-54.
[12]祝宝军,陶颖,邱玉婷等.水热法合成的纳米氧化锆结构[J].粉末冶金材料科学与工程,2008,13(2):111-114.
[13]ANANDAN K,RAJENDRAN V.A Low-temperature Synthesis and Characterization of Tetragonal-ZrO_2 Nanoparticles via Simple Hydrothermal Process[J].Journal of Physical Sciences,2013,17(28):49-52.
[14]AQIF A Chaudhry,Haixue Yan,Giuseppe Viola.Phase Stability and rapid Consolidation of Hydroxyapatite—zirconia Nano-coprecipitates Made using Continuous hydrothermal flow synthesis[J].J Biomater Appl,2013,28:448-461.
[15]SITI Machmudah,WIDIYASTUTI W,Okky Putri Prastuti,et al.Synthesis of ZrO_2 nano-particles by Hydrothermal Treatment[J].Journal of Chemical Engineering and Research,2012,21(4):38-42.
[16]Marcin Wysokowski,Mykhaylo Motylenko,Vasilii V.Bazhenov et al.Poriferan chitin as a Template for Hydrothermal Zirconia Deposition[J].Frontiers of Materials Science,2013,7(3):248-260.
[17]BEHBAHANI A,ROWSHANZAMIR S,ESMAEILIFAR A.Hydrothermal Synthesis of Zirconia Nanoparticles from Commercial Zirconia[J].Procedia Engineering2012,42:908-917.
[18]CAILLOT T,SALAMA Z,CHANUT N,et al.Hydrothermal synthesis and characterization of zirconia based catalysts[J].Journal of Solid State Chemistry,2013,203:79-85.
[19]唐勋海,顾华志,汪厚植,等.氯氧化锆前驱体制备纳米氧化锆的机理探讨[J].无机盐工业,2004,36(3):14-17.
[20]王焕英,国占生,刑广恩,等.不同工艺制备纳米氧化锆的研究[J].人工晶体学报,2006,35(4):753-757.
[2]LEE D S,KIM W S,CHOI S H,et al.Characterization of ZrO_2 codoped with Sc_2O_3 and CeO_2 Electrolyte for the Application of Inter-mediate Temperature SOFCs[J].Solid State Ionics,2005,176(1/2):33-39.
[3]李其连.等离子喷涂ZrO_2热障涂层热冲击破坏研究[J].中国表面工程,2004,3:17-25.
[4]Abd El-latif M M,SHOWMAN M S,IBRAHIM A M,et al.Optimizing the Preparation Parameters of Nanocrystalline Zirconia for Catalytic applications[J].Acta Metallurgica Sinica 2013,26(5):565-573.
[5]VOLLATH D,FISCHER F D,HAGELSTEIN M,et al.Phases and Phase Thansformation in Nanocrystaline ZrO_2[J].Journal of Nanoparticle Research,2006,8:1003-1016.
[6]Jun-Seop KIM,Dong-Hae LEE,Sung KANG,et al.Synthesis and microstructure of Zirconia Nanopowders by Glycothermal Processing[J].Transactions of Nonferrous Meters Society of China,2009,19:88-91.
[7]KHORRAMIE S A,BAGHCHESARA M A,Gohari D P.Fabrication of Aluminum Matrix Composites Reinforced with Al_2ZrO_5 nano Particulates Synthesized by sol-gel auto-combustion method[J].Transactions of Nonferrous Meters Society of China,2013,23:1556-1562.
[8]Lei YUAN,Dong Xiang,JING-kun Yu.Effect of solvents on the Properties of co-precipitated MgO-ZrO_2 Nano Powders[J].Journal of Ceramic Processing Research,2013,14(4):517-520.
[9]敖红敏,俞耀伦,龙志奇,等.超细锆基复合氧化物粉体制备方法概述[J].稀有金属,2013,37(2):302-311.
[10]PRAKASHBABU D,HARI KRISHNA R,NAGABHUSHANA B M,et al.Influence of precursors on Photoluminescence of hydrothermally derived ZrO_2[J].Journal of Chemical Engineering and Research,2014,2(1):105-111.
[11]李茹民,李占双,辛艳风,等.纳米二氧化锆制备方法进展[J].应用科技,2001,28(9):52-54.
[12]祝宝军,陶颖,邱玉婷等.水热法合成的纳米氧化锆结构[J].粉末冶金材料科学与工程,2008,13(2):111-114.
[13]ANANDAN K,RAJENDRAN V.A Low-temperature Synthesis and Characterization of Tetragonal-ZrO_2 Nanoparticles via Simple Hydrothermal Process[J].Journal of Physical Sciences,2013,17(28):49-52.
[14]AQIF A Chaudhry,Haixue Yan,Giuseppe Viola.Phase Stability and rapid Consolidation of Hydroxyapatite—zirconia Nano-coprecipitates Made using Continuous hydrothermal flow synthesis[J].J Biomater Appl,2013,28:448-461.
[15]SITI Machmudah,WIDIYASTUTI W,Okky Putri Prastuti,et al.Synthesis of ZrO_2 nano-particles by Hydrothermal Treatment[J].Journal of Chemical Engineering and Research,2012,21(4):38-42.
[16]Marcin Wysokowski,Mykhaylo Motylenko,Vasilii V.Bazhenov et al.Poriferan chitin as a Template for Hydrothermal Zirconia Deposition[J].Frontiers of Materials Science,2013,7(3):248-260.
[17]BEHBAHANI A,ROWSHANZAMIR S,ESMAEILIFAR A.Hydrothermal Synthesis of Zirconia Nanoparticles from Commercial Zirconia[J].Procedia Engineering2012,42:908-917.
[18]CAILLOT T,SALAMA Z,CHANUT N,et al.Hydrothermal synthesis and characterization of zirconia based catalysts[J].Journal of Solid State Chemistry,2013,203:79-85.
[19]唐勋海,顾华志,汪厚植,等.氯氧化锆前驱体制备纳米氧化锆的机理探讨[J].无机盐工业,2004,36(3):14-17.
[20]王焕英,国占生,刑广恩,等.不同工艺制备纳米氧化锆的研究[J].人工晶体学报,2006,35(4):753-757.