CN109369173B - 一种四方相钛酸钡粉体的制备方法及产品 - Google Patents

一种四方相钛酸钡粉体的制备方法及产品 Download PDF

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CN109369173B
CN109369173B CN201811530238.XA CN201811530238A CN109369173B CN 109369173 B CN109369173 B CN 109369173B CN 201811530238 A CN201811530238 A CN 201811530238A CN 109369173 B CN109369173 B CN 109369173B
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barium
hydroxide
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朱归胜
徐华蕊
章秋晨
钱浩宇
赵昀云
张秀云
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Guilin University of Electronic Technology
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Abstract

本发明涉及一种四方相钛酸钡粉体的制备方法及产品，属于介电陶瓷材料技术领域，该方法中，首先将钡盐或钡的氢氧化物和钛的氧化物或氢氧化物分开球磨或砂磨，分别获得钡盐或钡的氢氧化物浆料和钛的氧化物或氢氧化物浆料，然后将两种浆料在20‑40℃下混匀后进行喷雾干燥，获得混合粉体，再向该混合粉体中加入混合粉体总质量5‑90％的陶瓷材料，再次混匀后进行微波处理，最终制得粉体晶粒细小，粒径均匀，分散性良好的四方相钛酸钡粉体。该制备方法工艺简单，易操作，且成本低，适合工业化生产。

Description

一种四方相钛酸钡粉体的制备方法及产品
技术领域
本发明属于压电陶瓷材料技术领域，具体涉及一种四方相钛酸钡粉体的制备方法及产品。
背景技术
钛酸钡作为重要的电子基础材料，广泛应用于积层电容元件(MLCC)、压电元件、限流保护、消磁、启动、发热元件(PTC)、发光材料等领域。随着MLCC介质层厚度的不断减少，对钛酸钡粒径的要求也越来越细，因此对超细纳米钛酸钡的需求与日增多。
当前，制备钛酸钡主要可分为液相法和固相法两大类。液相生产方法主要有：草酸法、水热法、溶胶－凝胶法和微波水热法。通过液相法生产的钛酸钡，虽然粒径细小，但成本过高，工艺流程复杂，产能有限，并且粉体内含大量反应所生成的羟基，在后续陶瓷化过程容易带入缺陷，导致电容介电常数、损耗等电性能的波动。通过固相法生产制备钛酸钡是目前通用的方法，此法工艺技术成熟，原料来源广泛且价格便宜，可大量生产，最关键的是合成的钛酸钡晶粒完整，缺陷较少，但在球磨过程中，原料与介质碰撞会产生局部高温，从而造成钛酸钡晶核的产生，进而影响最终制备的钛酸钡的均匀性，并且在高温合成中，会出现晶粒长大和团聚，因此难以生产粒径小的超细钛酸钡粉体。因此，急需一种能够制备出粉体晶粒细小，粒径均匀，分散性良好的相钛酸钡粉体的固相法。
发明内容
有鉴于此，本发明的目的之一在于提供一种四方相钛酸钡粉体的制备方法；目的之二在于提供一种四方相钛酸钡粉体。
为达到上述目的，本发明提供如下技术方案：
1、一种四方相钛酸钡粉体的制备方法，所述方法包括如下步骤：
(1)按Ba和Ti的摩尔比为1.02-1.05:1称取钡盐或钡的氢氧化物和钛的氧化物或氢氧化物，然后将所述钡盐或钡的氢氧化物和钛的氧化物或氢氧化物分别进行球磨或砂磨处理，获得钡盐或钡的氢氧化物浆料和钛的氧化物或氢氧化物浆料；
(2)将步骤(1)中获得的钡盐或钡的氢氧化物浆料和钛的氧化物或氢氧化物浆料在20-40℃下混匀，然后进行喷雾干燥，获得混合粉体，再向所述混合粉体中加入所述混合粉体总质量5-90％的陶瓷材料，再次混匀后进行微波处理，所述微波处理具体为以20-100℃/min的升温速率升至600-1100℃后，保温0.5-4h。
优选地，步骤(1)中，所述Ba和Ti的摩尔比为1.03:1。
优选地，步骤(1)中，所述钡盐为BaCO3，所述钡的氢氧化物为Ba(OH)2。
优选地，步骤(1)中，所述钛的氧化物为TiO2，所述钛的氢氧化物Ti(OH)4。
优选地，步骤(2)中，所述喷雾干燥时进风温度为200℃，出风温度为100℃，雾化器转速为15000-33000rpm。
优选地，步骤(2)中，再向所述混合粉体中加入所述混合粉体总质量25-50％的陶瓷材料。
优选地，所述陶瓷材料是粒径为20-1000μm的微粒。
优选地，所述陶瓷材料为SiC、ZrO2或Al2O3中的至少一种。
优选地，步骤(2)中，所述微波处理具体为以30-50℃/min的升温速率升至800-1000℃后，保温1-2h。
2、由所述的方法制备的四方相钛酸钡粉体。
本发明的有益效果在于：本发明提供了一种四方相钛酸钡粉体的制备方法及产品，在制备过程中将钡盐或钡的氢氧化物和钛的氧化物或氢氧化物分开球磨或砂磨，从而有效地避免了球磨或机磨过程中，因原料间的碰撞产生的局部高温或能量传递而产生的非均相成核，生成少量钛酸钡晶种或晶核，极大影响钛酸钡粉体粒径均匀性的缺陷，保证了最终制备的钛酸钡的均匀性。另外，后期混入陶瓷材料后结合微波处理，一方面利用了陶瓷材料良好的微波吸收性，在其与粉体的充分混合后，形成微区均匀加热，克服了BaTiO3微波吸收性不好的缺陷，另一方面，在利用微波加热快速、均匀的特性的同时，通过限定微波处理的工艺条件，不但能够缩短合成时间，还能有效避免晶粒长大和团聚，相比于传统固相法，所制备出的粉体晶粒细小，粒径均匀，分散性良好。该制备方法工艺简单，易操作，且成本低，适合工业化生产。
附图说明
为了使本发明的目的、技术方案和有益效果更加清楚，本发明提供如下附图进行说明：
图1为实施例1至实施例8中制备的四方相钛酸钡粉体的XRD图；
图2为实施例1至实施例4中制备的四方相钛酸钡粉体的SEM图。
具体实施方式
下面将对本发明的优选实施例进行详细的描述。
实施例1
制备四方相钛酸钡粉体
(1)按Ba和Ti的摩尔比为1.02:1称取BaCO3和TiO2，按球:料:水的质量比例为2:1:1的比例分别将BaCO3和TiO2加入到两个球磨罐中，然后以300rpm的速度球磨4h，分别获得BaCO3浆料和TiO2浆料；
(2)将步骤(1)中获得的BaCO3浆料和TiO2浆料在25℃下混匀，然后在进风温度为200℃，出风温度为100℃，雾化器转速为20000rpm的工艺条件下进行喷雾干燥，获得混合粉体，再向该混合粉体中加入混合粉体总质量5％的陶瓷材料(由SiC微粒和Al2O3微粒按质量比1:1混合而成，且SiC微粒和Al2O3微粒的平均粒径均分布在50-100μm)，再次混匀后进行微波处理，微波处理具体为以60℃/min的升温速率升至600℃后，保温4h，制得四方相钛酸钡粉体。
实施例2
制备四方相钛酸钡粉体
(1)按Ba和Ti的摩尔比为1.03:1称取Ba(OH)2和Ti(OH)4，按球:料:水的质量比例为2:1:1的比例分别将Ba(OH)2和Ti(OH)4加入到两个球磨罐中，然后以150rpm的速度球磨1.5h，分别获得Ba(OH)2浆料和Ti(OH)4浆料；
(2)将步骤(1)中获得的Ba(OH)2浆料和Ti(OH)4浆料在30℃下混匀，然后在进风温度为200℃，出风温度为100℃，雾化器转速为15000rpm的工艺条件下进行喷雾干燥，获得混合粉体，再向该混合粉体中加入混合粉体总质量15％的陶瓷材料(平均粒径分布在100-150μm的SiC微粒)，再次混匀后进行微波处理，微波处理具体为以80℃/min的升温速率升至700℃后，保温3.5h，制得四方相钛酸钡粉体。
实施例3
制备四方相钛酸钡粉体
(1)按Ba和Ti的摩尔比为1.05:1称取BaCO3和Ti(OH)4，按球:料:水的质量比例为2:1:1的比例分别将BaCO3和Ti(OH)4加入到两个球磨罐中，然后以200rpm的速度球磨3h，分别获得BaCO3浆料和Ti(OH)4浆料；
(2)将步骤(1)中获得的BaCO3浆料和Ti(OH)4浆料在35℃下混匀，然后在进风温度为200℃，出风温度为100℃，雾化器转速为25000rpm的工艺条件下进行喷雾干燥，获得混合粉体，再向该混合粉体中加入混合粉体总质量15％的陶瓷材料(由ZrO2微粒和Al2O3微粒按质量比1:1混合而成，且ZrO2微粒和Al2O3微粒的平均粒径均分布在150-200μm)，再次混匀后进行微波处理，微波处理具体为以45℃/min的升温速率升至800℃后，保温3h，制得四方相钛酸钡粉体。
实施例4
制备四方相钛酸钡粉体
(1)按Ba和Ti的摩尔比为1.02:1称取Ba(OH)2和TiO2，按球:料:水的质量比例为2:1:1的比例分别将Ba(OH)2和TiO2加入到两个球磨罐中，然后以250rpm的速度球磨2h，分别获得Ba(OH)2浆料和TiO2浆料；
(2)将步骤(1)中获得的Ba(OH)2浆料和TiO2浆料在30℃下混匀，然后在进风温度为200℃，出风温度为100℃，雾化器转速为33000rpm的工艺条件下进行喷雾干燥，获得混合粉体，再向该混合粉体中加入混合粉体总质量25％的陶瓷材料(由SiC微粒和Al2O3微粒按质量比2:1混合而成，且SiC微粒和Al2O3微粒的平均粒径均分布在500-1000μm)，再次混匀后进行微波处理，微波处理具体为以50℃/min的升温速率升至850℃后，保温2h，制得四方相钛酸钡粉体。
实施例5
制备四方相钛酸钡粉体
(1)按Ba和Ti的摩尔比为1.04:1称取BaCO3和TiO2，按料:水的质量比例为1:1的比例分别将BaCO3和TiO2以2000rpm的速度砂磨1h，分别获得BaCO3浆料和TiO2浆料；
(2)将步骤(1)中获得的BaCO3浆料和TiO2浆料在30℃下混匀，然后在进风温度为200℃，出风温度为100℃，雾化器转速为28000rpm的工艺条件下进行喷雾干燥，获得混合粉体，再向该混合粉体中加入混合粉体总质量25％的陶瓷材料(平均粒径分布在500-800μm的SiC微粒)，再次混匀后进行微波处理，微波处理具体为以20℃/min的升温速率升至900℃后，保温2h，制得四方相钛酸钡粉体。
实施例6
制备四方相钛酸钡粉体
(1)按Ba和Ti的摩尔比为1.05:1称取Ba(OH)2和Ti(OH)4，按料:水的质量比例为1:1的比例分别将Ba(OH)2和Ti(OH)4以1500rpm的速度砂磨1.5h，分别获得Ba(OH)2浆料和Ti(OH)4浆料；
(2)将步骤(1)中获得的Ba(OH)2浆料和Ti(OH)4浆料在37℃下混匀，然后在进风温度为200℃，出风温度为100℃，雾化器转速为22000rpm的工艺条件下进行喷雾干燥，获得混合粉体，再向该混合粉体中加入混合粉体总质量50％的陶瓷材料(由SiC微粒和Al2O3微粒按质量比3:1混合而成，且SiC微粒和Al2O3微粒的平均粒径均分布在500-700μm)，再次混匀后进行微波处理，微波处理具体为以100℃/min的升温速率升至950℃后，保温1.5h，制得四方相钛酸钡粉体。
实施例7
制备四方相钛酸钡粉体
(1)按Ba和Ti的摩尔比为1.04:1称取BaCO3和Ti(OH)4，按料:水的质量比例为1:1.2的比例分别将BaCO3和Ti(OH)4以3000rpm的速度砂磨0.5h，分别获得BaCO3浆料和Ti(OH)4浆料；
(2)将步骤(1)中获得的BaCO3浆料和Ti(OH)4浆料在35℃下混匀，然后在进风温度为200℃，出风温度为100℃，雾化器转速为20000rpm的工艺条件下进行喷雾干燥，获得混合粉体，再向该混合粉体中加入混合粉体总质量90％的陶瓷材料(平均粒径分布在800-1000μm的ZrO2微粒)，再次混匀后进行微波处理，微波处理具体为以65℃/min的升温速率升至1000℃后，保温1h，制得四方相钛酸钡粉体。
实施例8
制备四方相钛酸钡粉体
(1)按Ba和Ti的摩尔比为1.03:1称取Ba(OH)2和TiO2，按料:水的质量比例为1:0.8的比例分别将Ba(OH)2和TiO2以2200rpm的速度砂磨1h，分别获得Ba(OH)2浆料和TiO2浆料；
(2)将步骤(1)中获得的Ba(OH)2浆料和TiO2浆料在20℃下混匀，然后在进风温度为200℃，出风温度为100℃，雾化器转速为15000rpm的工艺条件下进行喷雾干燥，获得混合粉体，再向该混合粉体中加入混合粉体总质量60％的陶瓷材料(由SiC微粒、ZrO2微粒和Al2O3微粒按质量比0.5:0.5:1混合而成，且SiC微粒、ZrO2微粒和Al2O3微粒的平均粒径均分布在400-450μm)，再次混匀后进行微波处理，微波处理具体为以90℃/min的升温速率升至1100℃后，保温0.5h，制得四方相钛酸钡粉体。
实施例1至实施例8中制备的四方相钛酸钡粉体的XRD图，由图1可知，实施例1至实施例8中的方法均可以获得具有四方相的钛酸钡粉体，且晶型完整，不存在其它杂相。
图2为实施例1至实施例4中制备的四方相钛酸钡粉体的SEM图，由图2可知，实施例1至实施例4中制备的钛酸钡粉体分散性良好，晶粒生长完整，粒径尺寸在200-400nm，且性能指标重复性好。
最后说明的是，以上优选实施例仅用以说明本发明的技术方案而非限制，尽管通过上述优选实施例已经对本发明进行了详细的描述，但本领域技术人员应当理解，可以在形式上和细节上对其做出各种各样的改变，而不偏离本发明权利要求书所限定的范围。

Claims (7)

1.一种四方相钛酸钡粉体的制备方法，其特征在于，所述方法包括如下步骤：
(1)按Ba和Ti的摩尔比为1.02-1.05:1称取钡盐或钡的氢氧化物和钛的氧化物或氢氧化物，然后将所述钡盐或钡的氢氧化物和钛的氧化物或氢氧化物分别进行球磨或砂磨处理，获得钡盐或钡的氢氧化物浆料和钛的氧化物或氢氧化物浆料；
(2)将步骤(1)中获得的钡盐或钡的氢氧化物浆料和钛的氧化物或氢氧化物浆料在20-40℃下混匀，然后进行喷雾干燥，所述喷雾干燥时进风温度为200℃，出风温度为100℃，雾化器转速为15000-33000rpm，获得混合粉体，再向所述混合粉体中加入所述混合粉体总质量5-90％的陶瓷材料，所述陶瓷材料为SiC、ZrO2或Al2O3中的至少一种，再次混匀后进行微波处理，所述微波处理具体为以20-100℃/min的升温速率升至600-1100℃后，保温0.5-4h。
2.如权利要求1所述的方法，其特征在于，步骤(1)中，所述Ba和Ti的摩尔比为1.03:1。
3.如权利要求1所述的方法，其特征在于，步骤(1)中，所述钡盐为BaCO3，所述钡的氢氧化物为Ba(OH)2。
4.如权利要求1所述的方法，其特征在于，步骤(1)中，所述钛的氧化物为TiO2，所述钛的氢氧化物Ti(OH)4。
5.如权利要求1所述的方法，其特征在于，步骤(2)中，再向所述混合粉体中加入所述混合粉体总质量25-50％的陶瓷材料。
6.如权利要求5所述的方法，其特征在于，所述陶瓷材料是粒径为20-1000μm的微粒。
7.如权利要求1-6任一项所述的方法，其特征在于，步骤(2)中，所述微波处理具体为以30-50℃/min的升温速率升至800-1000℃后，保温1-2h。
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