一步固相法合成四钛酸钾片晶的研究
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摘要
采用一步固相法制得四钛酸钾片晶(K_2Ti_4O_9,KTO)。通过加镁诱导以及熔盐量的调控促使KTO朝二维方向生长,实现对片晶形貌的控制。用X射线衍射仪(XRD)、场发射扫描电子显微镜(FESEM)、热重分析仪(TG-DSC)以及粒度仪研究了诱导剂和KCl的量对KTO晶相结构、形貌演变和粒径大小的影响,并对其反应机理进行了初步的探讨。结果表明:熔盐量会对产物的组成产生影响,当原料中加入质量分数50%的KCl后,产物组成为KTO;随着诱导剂镁源的加入,KTO的形貌由一维生长的晶须向二维方向的片晶转变,当Mg(OH)_2的添加量为4. 3 wt%,此时形貌为片状、分布均匀的KTO即可生成,粒径范围1-10μm,D_(50)为2. 7μm。
Plate-like potassium tetratitanate was synthesized by one-step solid phase method. The morphology of tetratitanate was controlled by the magnesium and molten salt.Regulating the content of magnesium oxide and potassium chloride made tetratitanate grow in two-dimensional direction.X-ray diffraction( XRD),field emission scanning electron microscopy( FESEM),thermogravimetric analyzer( TG-DSC) and particle size analyzer were used to study the influence of MgO and KCl addition on the phase structure and morphology evolution of KTO.The mechanism of reaction was explored preliminarily.The results showed that KCl addition could affect the composition of crystals.When the content of KCl was 50%( mass fraction),the product composition was KTO.With the addition of MgO,the growth direction of KTO evolved from one dimension to two dimension.When Mg( OH)_2amount reached to 4. 3wt%,the KTO with platy morphology and uniform distribution was prepared.The particle size range was 1-10 μm,and D_(50) was 2. 7μm.
Plate-like potassium tetratitanate was synthesized by one-step solid phase method. The morphology of tetratitanate was controlled by the magnesium and molten salt.Regulating the content of magnesium oxide and potassium chloride made tetratitanate grow in two-dimensional direction.X-ray diffraction( XRD),field emission scanning electron microscopy( FESEM),thermogravimetric analyzer( TG-DSC) and particle size analyzer were used to study the influence of MgO and KCl addition on the phase structure and morphology evolution of KTO.The mechanism of reaction was explored preliminarily.The results showed that KCl addition could affect the composition of crystals.When the content of KCl was 50%( mass fraction),the product composition was KTO.With the addition of MgO,the growth direction of KTO evolved from one dimension to two dimension.When Mg( OH)_2amount reached to 4. 3wt%,the KTO with platy morphology and uniform distribution was prepared.The particle size range was 1-10 μm,and D_(50) was 2. 7μm.
引文
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[2]Zhou Y X,Liu C,He M,et al.Spliting behavior and structural transformation process of K2Ti6O13whiskers under hydrothermal conditions[J]. J Mater Sci,2008,43(1):155-163.
[3]韩世启,司乃潮,殷恒波,等.偏钛酸为原料制备六钛酸钾晶须机理研究[J].功能材料,2012,14(43):1829-1832.
[4]Tomas S M,Alexander G,Jose I E. Molten salt synthesis and characterization of potassium polytitanate ceramic precursors with varied Ti O2/K2O molar ratios[J]. J Am Ceram Soc,2008,91(9):3054-3064.
[5]Izawa H,Kikkawa S,Koizumi M.Ion exchange and dehydration of layered titanates,Na2Ti3O7and K2Ti4O9[J].J Phys Chem,1982,86(25):5023-5026.
[6]刘浩,商少明,赵贝贝,等.钛酸锂钾制备六钛酸钾片晶及过程控制[J].化学研究与应用,2017,29(9):1411-1416.
[7]Tersea Z.Investigation on synthesis and microstructure of potassium tetratitanate[J]. J Therm Anal Calorim,2008,91(3):911-913.
[8]张盼盼,李谦,黄金亮,等.微波合成四钛酸钾晶须[J].河南科技大学学报(自然科学版),2016,37(1):1-4.
[9]吴事江,吉晓莉.四钛酸钾纤维的反应机制研究[J].纳米科技,2013,10(6):62-66.
[10]Bao N Z,Feng X,Shen L.Calcination syntheses of a series of potassium titanates and their morphologic evolution[J].Cryst Growth Des,2002,2(5):437-442.
[11]Ishihara Y,Kyono H,Kohyama N,et al.Effects of surface characteristics of potassium titanate whisker samples on acute lung injury induced by a single intratracheal administration in rats[J].Inhal Toxicol,2002,14(5):503-519.
[12]邹新建,李亮.钒钛产品生产工艺与设备[M].北京:化学工业出版社,2014:173-177.
[13]钱清华,柏扬,周雪锋,等.溶胶-凝胶法制备纳米平整度的四钛酸钾薄膜[J].无机材料学报,2007,22(4):749-753.
[14]王菊,李春,梁斌.高浓KOH水溶液中低温合成六钛酸钾前驱体的研究[J].化工新型材料,2006,34(12):23-26.
[15]Song N,Liu Y,Liu B W,et al. Controlled synthesis of platy potassium titanates from potassium magnesium titanate[J].RSC Adv,2013,3(22):8326-8330.
[16]Takenaka T.Grain orientation effect on electrical properties of bismuth layer-structured ferroelectric ceramics[J].J Ceram Soc Jpn,2002,85(6):1461-1466.
[17]Fukuchi K T. Effect of potassium concentration on the grain orientation in bismuth sodium potassium titanate[J].J Am Ceram Soc,2002,85(6):1461-1466.
[18]刘浩,赵贝贝,商少明,等.煅烧工艺对熔盐法合成钛钾镁片晶的影响[J].应用化学,2017,34(10):1195-1201.
[19]宋旎.片状钛酸镁钾的制备及其处理溶液中铜离子的研究[D].长沙:中南大学粉末冶金研究院,2013.
[20]Yasuyoshi S.Alkali metal-containing niobate-based piezoelectric material composition and a method for producing the same[P].US20000511316,2002-05-14.