CN106045499A - 掺锆掺镧钛酸钠铋‑钛酸钡陶瓷的制备方法 - Google Patents

掺锆掺镧钛酸钠铋‑钛酸钡陶瓷的制备方法 Download PDF

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CN106045499A
CN106045499A CN201610363715.2A CN201610363715A CN106045499A CN 106045499 A CN106045499 A CN 106045499A CN 201610363715 A CN201610363715 A CN 201610363715A CN 106045499 A CN106045499 A CN 106045499A
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樊慧庆
赵扬
董广志
彭彪林
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Abstract

本发明公开了一种掺锆掺镧钛酸钠铋‑钛酸钡陶瓷的制备方法，用于解决现有制备的钛酸钠铋‑钛酸钡陶瓷储能密度低的技术问题。技术方案是采用高温固相合成法，以碳酸钡、碳酸镧、碳酸钠、氧化铋、氧化钛和氧化锆为原料，按化学计量比称量，以酒精为介质、氧化锆球为磨球进行混料，待浆料干燥后将其过筛并轻压成块状坯体高温煅烧。煅烧后的块料研磨成细粉，压制成型后经过高温烧结，制得掺锆掺镧钛酸钠铋‑钛酸钡陶瓷。该材料弛豫弥散度得到增加，抗击穿强度高，获得了较高的储能密度。经测试，在56kV/cm的电场下，储能密度由背景技术的0.59J/cm3提高到0.77J/cm3，提高了31％。

Description

掺锆掺镧钛酸钠铋-钛酸钡陶瓷的制备方法
技术领域
本发明涉及一种钛酸钠铋-钛酸钡陶瓷的制备方法，特别是涉及一种掺锆掺镧钛酸钠铋-钛酸钡陶瓷的制备方法。
背景技术
对反铁电材料储能效应的研究主要集中在锆钛酸铅为基的含铅材料体系中，为响应欧盟ROHS/WEEE指令对电子产品中有害物质使用的限制，无铅反铁电储能材料的研究开始得到重视。但报道的该类材料存在储能密度较低的缺陷，难以满足应用需求。
文献“Energy-storage properties of 0.89Bi0.5Na0.5TiO3-0.06BaTiO3- 0.05K0.5Na0.5NbO3 lead-free anti-ferroelectric ceramics.J.Am.Ceram.Soc.2011,94(12):4382-4386”公开了一种钛酸钠铋-钛酸钡-铌酸钾钠陶瓷的制备方法。该方法采用氧化铋、碳酸钠、氧化钛、碳酸钡、碳酸钾和五氧化二铌为原料，混料之后经高温加热烧成陶瓷。该材料在56kV/cm的电场下，储能密度约为0.59J/cm3，并不理想。
发明内容
为了克服现有方法制备的钛酸钠铋-钛酸钡陶瓷储能密度低的不足，本发明提供一种掺锆掺镧钛酸钠铋-钛酸钡陶瓷的制备方法。该方法采用高温固相合成法，以碳酸钡、碳酸镧、碳酸钠、氧化铋、氧化钛和氧化锆为原料，按化学计量比称量，以酒精为介质、氧化锆球为磨球进行混料，待浆料干燥后将其过筛并轻压成块状坯体高温煅烧。煅烧后的块料研磨成细粉，压制成型后经过高温烧结，制得掺锆掺镧钛酸钠铋-钛酸钡陶瓷。该材料弛豫弥散度得到增加，抗击穿强度高，可获得较高的储能密度。
本发明解决其技术问题所采用的技术方案是：一种掺锆掺镧钛酸钠铋-钛酸钡陶瓷的制备方法，其特点是包括以下步骤：
步骤一、将分析纯的BaCO3、La2O3、Na2CO3、Bi2O3、TiO2和ZrO2置于烘箱中烘料2～5小时，烘料温度为100～120℃，随后按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti(1-x)ZrxO3(0≤x≤0.06)称量并配料；
步骤二、将配好的原料置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，制成浆料，混料时间为3～4小时；
步骤三、待浆料干燥后过筛并轻压成块状坯体在800～1100℃煅烧4～6小时。此后将煅烧后的块料研磨成细粉，再次球磨、烘干得到陶瓷粉料；
步骤四、将陶瓷粉料采用钢模手压成直径10～11mm、厚度约0.9～1.2mm的薄片，在300～350MPa下冷等静压成型后，以3～4℃/min的升温速率升至1100～1200℃保温4～6小时，随炉冷却至室温；
步骤五、将烧成的陶瓷薄片打磨抛光后涂覆银浆，在500～550℃保温20～40分钟，烧制银电极。
本发明的有益效果是：该方法采用高温固相合成法，以碳酸钡、碳酸镧、碳酸钠、氧化铋、氧化钛和氧化锆为原料，按化学计量比称量，以酒精为介质、氧化锆球为磨球进行混料，待浆料干燥后将其过筛并轻压成块状坯体高温煅烧。煅烧后的块料研磨成细粉，压制成型后经过高温烧结，制得掺锆掺镧钛酸钠铋-钛酸钡陶瓷。该材料弛豫弥散度得到增加，抗击穿强度高，获得了较高的储能密度。经测试，在56kV/cm的电场下，储能密度由背景技术的0.59J/cm3提高到0.77J/cm3，提高了31％。
下面结合具体实施方式对本发明作详细说明。
具体实施方式
实施例1。按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti(1-x)ZrxO3(0≤x≤0.06)称量并配料。当x＝0时，将分析纯的各原料置于烘箱中烘料5小时，烘料温度为100℃，之后按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]TiO3称量氧化铋10.6215g，碳酸钠2.4160g，碳酸钡1.1485g，氧化镧0.3258g，氧化钛7.9870g，氧化锆0g，置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，混料时间为4小时；待浆料干燥后将其过筛并轻压成块状坯体在1000℃煅烧5小时，此后将煅烧后的块料研磨成细粉，再次球磨、烘干得到陶瓷粉料；最后将陶瓷粉料采用钢模手压成直径10mm、厚度约1.2mm的样片，在300MPa下冷等静压成型后，以3℃/min的升温速率升至1100℃保温6小时，随炉冷却至室温，烧制成瓷。
实施例2。按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti(1-x)ZrxO3(0≤x≤0.06)称量并配料。当x＝0.02时，将分析纯的各原料置于烘箱中烘料4小时，烘料温度为110℃，之后按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.98Zr0.02O3称量氧化铋10.6215g，碳酸钠2.4160g，碳酸钡1.1485g，氧化镧0.3258g，氧化钛7.8272g，氧化锆0.2464g，置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，混料时间为3小时；待浆料干燥后将其过筛并轻压成块状坯体在900℃煅烧6小时，此后将煅烧后的块料研磨成细粉，再次球磨、烘干得到陶瓷粉料；最后将陶瓷粉料采用钢模手压成直径10.5mm、厚度约1.1mm的样片，在350MPa下冷等静压成型后，以3℃/min的升温速率升至1150℃保温6小时，随炉冷却至室温，烧制成瓷。
实施例3。按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti(1-x)ZrxO3(0≤x≤0.06)称量并配料。当x＝0.04时，将分析纯的各原料置于烘箱中烘料2小时，烘料温度为120℃，之后按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.96Zr0.04O3称量氧化铋10.6215g，碳酸钠2.4160g，碳酸钡1.1485g，氧化镧0.3258g，氧化钛7.6675g，氧化锆0.4928g，置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，混料时间为3小时；待浆料干燥后将其过筛并轻压成块状坯体在1100℃煅烧4小时，此后将煅烧后的块料研磨成细粉，再次球磨、烘干得到陶瓷粉料；最后将陶瓷粉料采用钢模手压成直径11mm、厚度约1mm的样片，在350MPa下冷等静压成型后，以3℃/min的升温速率升至1150℃保温5小时，随炉冷却至室温，烧制成瓷。
实施例4。按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti(1-x)ZrxO3(0≤x≤0.06)称量并配料。当x＝0.06时，将分析纯的各原料置于烘箱中烘料3小时，烘料温度为120℃，之后按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti0.94Zr0.06O3称量氧化铋10.6215g，碳酸钠2.4160g，碳酸钡1.1485g，氧化镧0.3258g，氧化钛7.5077g，氧化锆0.7393g，置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，混料时间为4小时；待浆料干燥后将其过筛并轻压成块状坯体在800℃煅烧6小时，此后将煅烧后的块料研磨成细粉，再次球磨、烘干得到陶瓷粉料；最后将陶瓷粉料采用钢模手压成直径10.5mm、厚度约0.9mm的样片，在300MPa下冷等静压成型后，以3℃/min的升温速率升至1200℃保温4小时，随炉冷却至室温，烧制成瓷。
经测试，本实施例制备的钛酸钠铋-钛酸钡陶瓷，在56kV/cm的电场下，储能密度为0.77J/cm3。

Claims (1)

1.一种掺锆掺镧钛酸钠铋-钛酸钡陶瓷的制备方法，其特征在于包括以下步骤：
步骤一、将分析纯的BaCO3、La2O3、Na2CO3、Bi2O3、TiO2和ZrO2置于烘箱中烘料2～5小时，烘料温度为100～120℃，随后按化学计量比[(Bi1/2Na1/2)0.9118Ba0.0582La0.02]Ti(1-x)ZrxO3(0≤x≤0.06)称量并配料；
步骤二、将配好的原料置于以酒精为介质、氧化锆球为磨球的尼龙罐中进行混料，制成浆料，混料时间为3～4小时；
步骤三、待浆料干燥后过筛并轻压成块状坯体在800～1100℃煅烧4～6小时；此后将煅烧后的块料研磨成细粉，再次球磨、烘干得到陶瓷粉料；
步骤四、将陶瓷粉料采用钢模手压成直径10～11mm、厚度约0.9～1.2mm的薄片，在300～350MPa下冷等静压成型后，以3～4℃/min的升温速率升至1100～1200℃保温4～6小时，随炉冷却至室温；
步骤五、将烧成的陶瓷薄片打磨抛光后涂覆银浆，在500～550℃保温20～40分钟，烧制银电极。
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CN107188555A (zh) * 2017-06-22 2017-09-22 广西大学 一种陶瓷靶材的制备方法
CN107935589A (zh) * 2017-12-14 2018-04-20 陕西科技大学 一种微量二氧化锆添加st‑nbt储能陶瓷及其制备方法
CN112225559A (zh) * 2020-09-25 2021-01-15 陕西科技大学 一种高储能高效率的Zr掺杂高熵钙钛矿氧化物陶瓷材料、制备方法及应用
CN114671681A (zh) * 2022-04-11 2022-06-28 北京科技大学 一种兼具高储能密度，高功率密度和高效率的钛酸钡基弛豫铁电陶瓷材料及其制备方法

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