基于Al(OH)3的熔盐法制备片状α-Al2O3工艺参数优化
Optimization of Process Parameters for Preparation of Flaky α-Al2O3 by Molten Salt Method with Al(OH)3
摘 要
以Al(OH)3为前驱体,采用熔盐法制备片状α-Al2O3,通过正交试验结合单因素方法研究了Al(OH)3与熔盐(NaCl+Na2SO4)的质量比(1:1,1:2,1:3)、添加剂Na3PO4质量分数(0.1%,1%,2%)、添加剂TiOSO4质量分数(0.5%,1%,3%)、烧结温度(900,1 050,1 200 ℃)以及保温时间(1,3,5 h)对Al2O3形貌的影响,获得最优工艺参数。结果表明:由正交试验得到对片状α-Al2O3形貌的影响由大到小依次为烧结温度、Al(OH)3与熔盐质量比、Na3PO4含量、保温时间,结合单因素方法得到最优工艺参数为烧结温度1 050 ℃、Al(OH)3与熔盐质量比1:2、Na3PO4质量分数1%、TiOSO4质量分数1%、保温时间3 h;在优化工艺条件下获得平均直径为15.413 μm、厚度为0.765 μm、径厚比为20.147的形状规则的片状α-Al2O3,且Al2O3纯净、无杂质。
片状α-Al2O3
熔盐法
正交试验
形貌
Al(OH)3
flaky α-Al2O3
molten salt method
orthogonal experiment
morphology
Abstract
The flaky α-Al2O3 was prepared by the molten salt method with Al(OH)3 as precursor. The effects of the mass ratio of Al(OH)3 to molten salt (NaCl+Na2SO4) (1:1,1:2,1:3), the mass fraction of Na3PO4 additive (0.1%, 1%, 2%), the mass fraction of TiOSO4 additive (0.5%, 1%, 3%), the sintering temperature (900,1 050,1 200 ℃) and the holding time (1,3,5 h) on the Al2O3 morphology were investigated by orthogonal experiment combined with single factor method,and the optimal process parameters were obtained. The results show that the factors influencing the morphology of flaky α-Al2O3 in descending order were sintering temperature, mass ratio of Al(OH)3 to molten salt, Na3PO4 content, and holding time. Combined with the single factor method, the optimal process parameters were sintering temperature of 1 050 ℃, Al(OH)3 to molten salt mass ratio of 1:2, Na3PO4 mass fraction of 1%, TiOSO4 mass fraction of 1%, and holding time of 3 h. Under the optimized process conditions, the flaky α-Al2O3 had the average diameter of 15.413 μm, thickness of 0.765 μm, and radius to thickness ratio of 20.147; the Al2O3 was pure and free of impurities.
中图分类号 TB383.1 DOI 10.11973/jxgccl202305008
所属栏目 新材料 新工艺
基金项目 贵阳市科技计划项目(筑科合同[2021] 1-10);贵阳市工信局创新能力平台建设项目(2018-01)
收稿日期 2022/10/20
修改稿日期 2023/3/31
网络出版日期
作者单位点击查看
备注龙开琳(1989-),男,贵州天柱人,讲师,硕士
引用该论文: LONG Kailin,LIU Fengkun,HUANG Yi,CUI Bowen,ZHU Huaqiang,LANG Xianzhong. Optimization of Process Parameters for Preparation of Flaky α-Al2O3 by Molten Salt Method with Al(OH)3[J]. Materials for mechancial engineering, 2023, 47(5): 47～54
龙开琳,刘风坤,黄毅,崔博文,朱化强,郎咸忠. 基于Al(OH)3的熔盐法制备片状α-Al2O3工艺参数优化[J]. 机械工程材料, 2023, 47(5): 47～54
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【4】黄世娥,吴华忠,洪蕾,等.以单晶片状氧化铝为基材包覆二氧化钛银白珠光颜料的制备[J].陶瓷学报,2018,39(1):48-52. HUANG S E,WU H Z,HONG L,et al.Preparation of silver white pearlescent pigment by coating single crystal flaky alumina substrate with titanium dioxide[J].Journal of Ceramics,2018,39(1):48-52.
【5】于闽.新型片状氧化铝材料的合成及在珠光颜料中的应用[D].上海:复旦大学,2010. YU M.Preparation of novel flaky alumina and its application in pearlescent pigment[D].Shanghai:Fudan University,2010.
【6】徐敬尧,周小丽,卿培林.高温固相法制备片状α氧化铝粉体的工艺研究[J].广东化工,2021,48(15):18-19. XU J Y,ZHOU X L,QING P L.Study on the preparation technology of flake α alumina by high temperature solid state method[J].Guangdong Chemical Industry,2021,48(15):18-19.
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【10】王莉玮,袁占辉,林棋.新型片状氧化铁的合成以及在珠光颜料中的应用[J].闽江学院学报,2013,34(2):113-118. WANG L W,YUAN Z H,LIN Q.Synthesis of late-model flaky iron oxide and its application on pearlescent pigment[J].Journal of Minjiang University,2013,34(2):113-118.
【11】苏周.熔盐法合成片状氧化铝粉体的研究[D].长沙:中南大学,2004. SU Z.Preparation of flaky alumina powder by molten salt synthesis method[D].Changsha:Central South University,2004.
【12】张集发,程小苏,曾令可.用于珠光颜料的片状氧化铝制备[J].中国陶瓷工业,2014,21(6):1-5. ZHANG J F,CHENG X S,ZENG L K.Preparation of flaky aluminum oxide for pearlescent pigment[J].China Ceramic Industry,2014,21(6):1-5.
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【16】孙春晖,朱玲玲,李赛,等.前驱体预处理及卤化铵添加剂对α-氧化铝微粉颗粒形貌的影响[J].无机盐工业,2018,50(9):19-23. SUN C H,ZHU L L,LI S,et al.Effect of pretreated precursor and halogenated ammonia additives on the morphology of α-Al2O3 powders[J].Inorganic Chemicals Industry,2018,50(9):19-23.
【17】赵燕禹,胡兴兰,张志鸿,等.高温固相法制备片状氧化铝及表征[J].无机盐工业,2014,46(4):46-48. ZHAO Y Y,HU X L,ZHANG Z H,et al.Preparation and characterization of flaky alumina by high temperature solid phase method[J].Inorganic Chemicals Industry,2014,46(4):46-48.
【18】申亚强,李冬云,徐扬,等.氟化铵对片状高纯氧化铝粉体的组成和形貌的调控机制探究[J].陶瓷学报,2021,42(1):84-89. SHEN Y Q,LI D Y,XU Y,et al.Mechanism of ammonium fluoride to regulate the composition and morphology of high-purity flaky alumina powder[J].Journal of Ceramics,2021,42(1):84-89.
【19】贾春燕,李东红,刘永鹤.以氢氧化铝为原料制备亚微米级α-Al2O3粉体[J].机械工程材料,2015,39(2):42-44. JIA C Y,LI D H,LIU Y H.Preparation of sub-micron α-Al2O3 powders using aluminium hydroxide as raw material[J].Materials for Mechanical Engineering,2015,39(2):42-44.
【20】LIU Q, WANG Y, ZHU Q G, et al.Synthesis of thin alpha alumina platelets with a large aspect ratio[J].Ceramics International,2021,47(1):252-259.
【21】ZHU L H , HUANG Q W.Morphology control of α-Al2O3 platelets by molten salt synthesis[J].Ceramics International,2011,37(1):249-255.
【22】SOUMAVO S,SATYANARAYANA S,BEHERA SHANTANU K, et al.Effect of processing parameters on the development of anisotropic α-Al2O3 platelets during molten salt synthesis[J].Ceramics International,2022,48(8):11145-11154.
【23】孙敬会,卿培林.熔盐法制备片状氧化铝粉体的研究[J].广州化工,2021,49(16):46-48. SUN J H,QING P L.Preparation of flake alumina powder by molten salt method[J].Guangzhou Chemical Industry,2021,49(16):46-48.
【24】吴宇峰,张铁军,张家萌,等.α-Al2O3相变机理及制备工艺研究进展[J].人工晶体报,2021,50(1):199-208. WU Y F,ZHANG T J,ZHANG J M,et al.Research progress on phase transition mechanism and preparation technology of α-Al2O3[J].Journal of Synthetic Crystals,2021,50(1):199-208.
【25】张倩影,朱丽慧,刘伟,等.添加剂在熔盐法合成片状α-Al2O3中的作用[J].材料研究学报,2008,22(2):205-208. ZHANG Q Y,ZHU L H,LIU W,et al.Influence of additives on the morphology control of α-Al2O3 platelets synthesized in molten salt[J].Chinese Journal of Materials Research,2008,22(2):205-208.
【26】WANG W L, BI J Q, QI Y Q, et al.Preparation of micrometer-sized α-Al2O3 platelets by thermal decomposition of AACH[J].Powder Technology,2010,201(3):273-276.
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