CN112028622A - 一种将硬团聚大颗粒BaTiO3转变为纳米及亚微米级颗粒的方法 - Google Patents

一种将硬团聚大颗粒BaTiO3转变为纳米及亚微米级颗粒的方法 Download PDF

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CN112028622A
CN112028622A CN202010898072.8A CN202010898072A CN112028622A CN 112028622 A CN112028622 A CN 112028622A CN 202010898072 A CN202010898072 A CN 202010898072A CN 112028622 A CN112028622 A CN 112028622A
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符小艺
周嘉会
陈志武
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South China University of Technology SCUT
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Abstract

本发明属于无机功能粉体材料领域，尤其涉及一种将硬团聚大颗粒BaTiO3转变为纳米及亚微米级颗粒的方法。本方法是采用熔盐刻蚀的方法，将团聚大颗粒BaTiO3粉体和熔盐充分混合在高温下进行熔盐刻蚀，得到纳米级和亚微米级BaTiO3粉体。具有操作简单、反应物可回收利用、所制备的BaTiO3颗粒具有结晶性增加、团聚减少、平均粒径减小且均匀性增加等优点。可以用来解决目前部分BaTiO3粉体粒径大，团聚严重，以及生产过程中环境污染等各种问题。

Description

一种将硬团聚大颗粒BaTiO3转变为纳米及亚微米级颗粒的 方法
技术领域
本发明属于无机功能粉体材料领域，尤其涉及电子陶瓷用四方相BaTiO3粉体的制备方法，具体涉及一种将硬团聚大颗粒BaTiO3转变为纳米及亚微米级颗粒的方法。
背景技术
钛酸钡基陶瓷材料因具有优异的介电性能，良好的铁电、压电以及热释电性能和绝缘性能，是制备多层陶瓷电容器(MLCC)、埋入式电容器、光记忆和电光器件等的主要材料，被认为是电子陶瓷的基石。国内可以大量生产BaTiO3粉体，但产品质量多数处于中低端，对于目前高端电子元器件所需要的高质量的BaTiO3粉体，仍大量需要进口。高端BaTiO3粉体对形貌和晶相有严格的要求，比如颗粒尺寸为亚微米级；分散度良好；四方相等等，而目前大量的中低端粉体为团聚的粉体，分散度差，尺寸多为微米级且均匀性差。此外，由于环保政策日趋严格，对于生产过程中的环境污染也有严格的规定，这必然导致了制备方法受限。比如，可以合成小尺寸和均匀性良好的液相法通常会带来环境污染问题，而环保也必然导致产品成本的大幅上升，限制了这些方法的大规模应用。因此，开发工艺简单，避免环境污染的高质量BaTiO3粉体的制备以满足社会发展的需要，具有重要的意义。
传统的固相法是将等物质的量的钡化合物和钛化合物混合，研磨，挤压成型，然后在1200℃进行煅烧，然后在粉碎湿磨压滤干燥研磨之后，得到BaTiO3粉末。通常固相法具有工艺、设备简单，原料易得的优点，但是制备出的BaTiO3颗粒尺寸不均，化学组分多、粉体粒径较大等缺点，当对BaTiO3粉体质量要求不高时，可以采用固相法合成(SMIRNOV A D,KHOLODKOVA A A,DANCHEVSKAYA M N,PONOMAREV S G,et al.Method of producingbarium titanate based ceramics has micron powder is obtained by solid phasesynthesis from equimolar mixture of barium carbonate and titanium dioxide:Russian.RU2706275-C1[P].2018-12-21.)。
熔盐法是近年来制备纳米材料的新型方法。熔融盐是盐的熔融态液体，形成熔融态的无机盐其固态大部分为离子晶体，在高温下熔化后形成离子熔体。熔盐法制备BaTiO3粉体已经有文献报道。这些文献大多是采用TiO2和钡的前驱体。例如BaCO3和TiO2与NaCl-KCl混合盐混合，经过高温反应生成BaTiO3粉体。目前大部分的熔盐法合成BaTiO3粉体的形貌为线状，而在电子陶瓷用粉料里，粒状用量最大要求最高。
发明内容
为解决上述技术问题，本发明的目的是提供一种将硬团聚大颗粒BaTiO3转变为纳米及亚微米级颗粒的方法。
该法是指在高温下采用熔盐刻蚀法制备出粒径小、分布窄、四方晶相含量高、均匀性和分散性好的高纯BaTiO3粉体。此法有效解决了高质量BaTiO3粉体生产过程工艺复杂，环境污染和成本问题，具有良好的工业生产与应用前景。与采用钛钡前驱体经化学反应合成钛酸钡不同，采用大尺寸或团聚的BaTiO3粉体作为原料，利用高温下熔盐刻蚀原理，将其转变为小尺寸BaTiO3粉体是高品质BaTiO3粉体制备的新思路。采用这种方法，一方面克服了液相法合成BaTiO3粉体容易造成环境污染且成本高的缺点，另一方面，也解决了传统固相法制备BaTiO3粉体易团聚和尺寸大的问题。
本发明提出了一种将硬团聚大颗粒BaTiO3转变为纳米及亚微米级颗粒的方法，将团聚大颗粒BaTiO3粉体和熔盐充分混合，然后在高温下进行熔盐刻蚀，得到纳米或亚微米级BaTiO3粉体。具体制备方法如下所述：
S1、称取硬团聚大颗粒BaTiO3粉体和熔盐，研磨使其充分混合；
S2、将S1制备的混合物置于坩埚中，高温下处理一段时间后冷却到室温；
S3、将S2高温处理后的混合物用热水洗涤，至洗涤液检测不到Cl-，得到湿的BaTiO3粉体；
S4、将湿的BaTiO3粉体用乙醇超声分散；
S5、将S4得到的BaTiO3粉体干燥，得到目标BaTiO3粉末。
进一步的，上述步骤S1中所述的硬团聚大颗粒BaTiO3粉体的平均粒径为0.2-10μm的BaTiO3粉体，S1中采用的熔盐为NaCl、KCl以及NaCl-KCl混合熔盐中的一种。
进一步优选的，上述步骤S1中采用的BaTiO3粉体是固相法和液相法制备的平均粒径为0.5～10μm的微米级BaTiO3粉体。
进一步的，上述步骤S1中所述将硬团聚大颗粒BaTiO3粉体和熔盐混合研磨时间是20min～40min。
进一步的，上述步骤S1中所述的硬团聚大颗粒BaTiO3粉体与熔盐质量比为1：5～1：100。
进一步的，上述步骤S2中所述高温处理的温度为600℃～900℃。
进一步的，上述步骤S2中高温处理时间为30min～10h。
进一步的，在高温刻蚀后，混合物需要热水洗涤。
进一步的，上述步骤S3洗涤后的上层清液直至0.5mol/L的AgNO3溶液没有白色沉淀。
进一步的，上述步骤S4所述湿的BaTiO3粉体在无水乙醇中超声分散30min。
进一步的，上述步骤S5所述干燥操作为90℃的环境中干燥12h。
进一步的，上述步骤S5所述得到的BaTiO3粉末平均粒径为50～800nm，成分和晶相与原料微米级BaTiO3粉体相同。
借由上述方案，本发明至少具有以下优点:
1)操作简单；
2)本发明制备的BaTiO3颗粒与原料相比具有团聚少，粒径减小且均匀性增加等优点；
3)本发明使用的熔盐，可以回收利用，减少环境污染。
附图说明
图1a为实施例3的BaTiO3粉体原料的SEM图。
图1b为实施例3的经熔盐刻蚀法处理后的粉体的SEM图。
图2a为实施例3的BaTiO3粉体原料的平均粒径分布图。
图2b为实施例3的经熔盐刻蚀法处理后的粉体的平均粒径分布图。
图3a为实施例3的BaTiO3粉体原料以及经熔盐刻蚀法处理后的粉体的XRD图。
图3b为图3a的40-55°的XRD图。
具体实施方式
下面将结合实施例对本发明的实施方案进行详细描述，但是本领域技术人员将会理解，下列实施例仅用于说明本发明，而不应视为限定本发明的范围。
实施例1
称取固相法制备的平均粒径为5μm微米级BaTiO3粉体和NaCl以质量比为1：30置于研钵，研磨30min使其充分混合；将制备的混合物置于Al2O3坩埚中，在900℃下处理30min后冷却到室温；将高温处理后的混合物用热水洗涤以去除Cl-；洗涤至采用0.5mol/L的AgNO3溶液检测不到AgCl白色沉淀；将得到湿的BaTiO3粉体在无水乙醇中超声分散30min，放在90℃的环境中干燥12h，得到干燥的粉末。
经SEM表征分析可知，原料BaTiO3粉体和处理后的样品形貌为不规则圆形，经统计，经过熔盐处理后的样品的平均粒径为200nm。与原料相比，处理后的样品具有良好的均一性和分散性，团聚减少，平均粒径减小。经XRD表征分析可知，经过处理的BaTiO3粉体结晶性增加，在熔盐刻蚀过程中，BaTiO3粉体的晶相不变。
实施例2
称取实施例1熔盐处理后的BaTiO3粉体，和NaCl以质量比1:30置于研钵，研磨30min使其充分混合；将制备的混合物置于Al2O3坩埚中，在900℃下处理30min后冷却到室温；将高温处理后的混合物用热水洗涤以去除NaCl；洗涤至采用0.5mol/L的AgNO3溶液检测不到AgCl白色沉淀；将得到湿的BaTiO3粉体在无水乙醇中超声分散30min，放在90℃的环境中干燥12h，得到干燥的粉末。
经SEM表征分析可知，经过二次刻蚀的样品形貌依然为不规则圆形，经统计，经过二次熔盐处理后的样品的平均粒径为50nm。与原料相比，二次处理后的样品比一次处理的BaTiO3粉体均一性和分散性更好，平均粒径减小。经XRD表征分析可知，经过处理的BaTiO3粉体结晶性增加，在熔盐刻蚀过程中，BaTiO3粉体的晶相不变。
实施例3
称取固相法制备的平均粒径为1.8μm的微米级BaTiO3粉体和NaCl以质量比为1：5置于研钵，研磨20min使其充分混合；将制备的混合物置于Al2O3坩埚中，在800℃下处理3h后冷却到室温；洗涤至采用0.5mol/L的AgNO3溶液检测不到AgCl白色沉淀；将得到湿的BaTiO3粉体在无水乙醇中超声分散30min，放在90℃的环境中干燥12h，得到干燥的粉末。
经SEM表征分析可知(图1a、图1b)，BaTiO3粉体形貌依然为不规则圆形，经统计(图2a、图2b)，经过熔盐处理后的BaTiO3粉体平均粒径为800nm，与原料相比，处理后的样品团聚减少，均一性增加。经XRD表征分析可知(参考附图3a、图3b)，经过处理的BaTiO3粉体结晶性增加，在熔盐刻蚀过程中，BaTiO3粉体的晶相不变。
实施例4
称取固相法制备的平均粒径为10μm的BaTiO3粉体和NaCl-KCl以质量比为1：60(NaCl-KCl的摩尔比为1:1)置于研钵，研磨40min使其充分混合；将制备的混合物置于Al2O3坩埚中，在600℃下处理5h后冷却到室温；将高温处理后的混合物用热水洗涤以去除NaCl-KCl；洗涤至采用0.5mol/L的AgNO3溶液检测不到AgCl白色沉淀；将得到湿的BaTiO3粉体在无水乙醇中超声分散30min，放在90℃的环境中干燥12h，得到干燥的粉末。
经SEM表征分析可知，处理后的BaTiO3粉体形貌为不规则四方形，经统计，经过处理后的样品平均粒径为300nm，与原料相比，处理后的BaTiO3粉体均一性增加，平均粒径小，团聚减少。经XRD表征分析可知，经过处理的BaTiO3粉体结晶性增加，在熔盐刻蚀过程中，BaTiO3粉体的晶相不变。
实施例5
称取水热法制备的平均粒径为0.5μm的亚微米级BaTiO3粉体和NaCl以质量比为1：100置于研钵，研磨30min使其充分混合；将制备的混合物置于Al2O3坩埚中，在700℃下处理10h后冷却到室温；将高温处理后的混合物用热水洗涤以去除NaCl；洗涤至采用0.5mol/L的AgNO3溶液检测不到AgCl白色沉淀；将得到湿的BaTiO3粉体在无水乙醇中超声分散30min，放在90℃的环境中干燥12h，得到干燥的粉末。
经SEM表征分析可知，BaTiO3粉体形貌由四方形转变为不规则圆形，经统计，经过处理后BaTiO3粉体的平均粒径为100nm，与原料相比，处理后的样品具有良好的均一性和分散性，平均粒径减小，团聚减少。经XRD表征分析可知，经过处理的BaTiO3粉体结晶性增加，在熔盐刻蚀过程中，BaTiO3粉体的晶相不变。
虽然本发明已以较佳实施例公开如上，但其并非用以限定本发明，任何熟悉此技术的人，在不脱离本发明的精神和范围内，都可做各种的改动与修饰，因此本发明的保护范围应该以权利要求书所界定的为准。

Claims (9)

1.一种将硬团聚大颗粒BaTiO3转变为纳米及亚微米级颗粒的方法，其特征在于，包括以下步骤：
S1、称取原料硬团聚大颗粒BaTiO3粉体和熔盐研磨，使其充分混合；
S2、将S1制备的混合物置于坩埚中，高温下处理一段时间后冷却到室温；
S3、将S2高温处理后的混合物用热水洗涤，至洗涤液没有Cl-检出，得到湿的BaTiO3粉体；
S4、将S3得到的湿BaTiO3粉体用乙醇超声分散；
S5、将S4得到的BaTiO3粉体干燥，得到目标BaTiO3粉末。
2.根据权利要求1所述的方法，其特征在于，步骤S1中所述的硬团聚大颗粒BaTiO3粉体的平均粒径为0.2～10μm的BaTiO3粉体，S1中所述的熔盐为NaCl、KCl以及NaCl-KCl混合熔盐中的一种。
3.根据权利要求1所述的方法，其特征在于，步骤S1中所述将硬团聚大颗粒BaTiO3粉体和熔盐混合研磨时间是20min～40min。
4.根据权利要求1所述的方法，其特征在于，步骤S1中所述硬团聚大颗粒BaTiO3粉体与熔盐的质量比是1：5～1：100。
5.根据权利要求1所述的方法，其特征在于，步骤S2中所述高温处理温度为600℃～900℃，所述高温下处理时间是30min～10h。
6.根据权利要求1所述的方法，其特征在于，步骤S3中所述洗涤液用0.5mol/L的AgNO3溶液检测，没有AgCl白色沉淀。
7.根据权利要求1所述的方法，其特征在于，步骤S4所述湿的BaTiO3粉体在无水乙醇中超声分散30min。
8.根据权利要求1所述的方法，其特征在于，步骤S5所述干燥操作为90℃的环境中干燥12h。
9.根据权利要求1所述的方法，其特征在于，步骤S5所述得到的BaTiO3粉末平均粒径为50～800nm，成分和晶相与原料微米级BaTiO3粉体相同。
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