CN112500160A - 一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷及制作工艺 - Google Patents

一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷及制作工艺 Download PDF

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CN112500160A
CN112500160A CN201910871743.9A CN201910871743A CN112500160A CN 112500160 A CN112500160 A CN 112500160A CN 201910871743 A CN201910871743 A CN 201910871743A CN 112500160 A CN112500160 A CN 112500160A
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龚文
吴超峰
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Tongxiang Qingfeng Technology Co ltd
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Abstract

本发明提出一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷及制作工艺，采用锑、钡、锆和钛元素进行掺杂取代，通过复合添加的方法，实现价态和空位补偿，提高其压电性能，使之满足于压电雾化片的性能要求。本发明采用铌酸钾钠基无铅压电陶瓷取代传统的含铅压电材料作为压电雾化片的核心元件，绿色环保，可有效避免压电陶瓷材料在生产、使用和废弃过程中带来的铅污染，减少对人类健康和环境的损害。

Description

一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷及制作工艺
技术领域
本发明涉及无铅压电陶瓷技术领域，尤其涉及一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷及其制作工艺。
背景技术
压电陶瓷雾化片因具有体积小、重量轻、无触点、无噪音、功耗低、高可靠、长寿命、可以适应恶劣的工作环境等特点，被广泛应用于环境工程、医疗器械、汽车工业、舞台设备以及家用电器等领域。目前使用的压电雾化片都是采用锆钛酸铅（PZT）基压电材料制造的。而在锆钛酸铅材料中，铅（Pb）元素约占材料总重量的70％，这类陶瓷材料在生产、使用以及废弃处理过程中都会给人类健康和生态环境造成十分严重的损害。
发明内容
针对以上问题，本发明提出一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷及制作工艺，采用锑、钡、锆和钛元素进行掺杂取代，通过复合添加的方法，实现价态和空位补偿，提高其压电性能，使之满足于压电雾化片的性能要求。
为实现以上目的，本发明通过以下技术方案来实现：一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷，化学组成为：(1-x)(K0.4Na0.6)Nb1-ySbyO3+xBaZr0.5Ti0.5O3；所述x，y为摩尔百分比，0≤x≤0.4，0.01≤y≤0.2。
进一步地，其原料包括：碳酸钾、碳酸钠、五氧化二铌和辅料，所述辅料为三氧化二锑、碳酸钡、二氧化锆和二氧化钛。
本发明在合成铌酸钾钠基无铅压电陶瓷的过程中，采用掺杂改性和复合添加的方法，活化了压电微区，有效提高了铌酸钾钠基无铅压电陶瓷的压电常数及机电耦合系数。
一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷的制作工艺，包括以下步骤：
（1）原料预处理：将碳酸钾、碳酸钠、五氧化二铌、三氧化二锑、碳酸钡、二氧化锆和二氧化钛放入培养皿，置于烘箱内，在120-150℃下保温3-6h；
（2）称料混合：按所述化学组成配比称量预处理后的原料，分散于无水乙醇中，混合均匀后烘干，粉碎过筛，制成预混粉；
（3）预烧：将预混粉置于箱式炉中连续升温至850-1000℃，保温4-8h，降温至室温后粉碎过筛，得到预烧粉；
（4）烧结：将预烧粉干压成型为生坯，在气氛烧结炉中于1100-1300℃下保温6-12h，得到致密的压电陶瓷片；
（5）后处理：将烧结好的压电陶瓷片加工成所需形状，在两侧镀上银层，标注正负极后极化老化得到所述铌酸钾钠基无铅压电陶瓷。
进一步地，步骤（2）所述预处理后的原料分散于无水乙醇后通过球磨机湿磨混合均匀，所述球磨机的转速为300-600rpm，湿磨时间为24-48h。
进一步地，步骤（4）所述气氛烧结炉的烧结气为空气或氧气，气压为0.1-0.5MPa。
进一步地，步骤（5）所述镀银过程为：在陶瓷片的两表面用丝网涂上厚度为0.01mm的银浆，在150℃下烘干，随后在箱式炉中升温至550-650℃，保温60min后降温至室温，得到被银陶瓷片。
进一步地，步骤（5）所述极化老化过程为：将标注有正负极的被银陶瓷片放入装有硅油的极化装置中，油浴加热至60-100℃，在3-5kV/mm的电压下极化30min，然后在室温下放置24h老化，得到所述铌酸钾钠基无铅压电陶瓷。
本发明采用直接干压成型、气氛烧结的方式，制备成了致密度高、电性能好的铌酸钾钠基无铅压电陶瓷，该压电陶瓷的压电常数在350pC/N以上，平面机电耦合常数为0.48-0.52，完全可以满足压电雾化片对于压电陶瓷材料的需求。
本发明采用铌酸钾钠基无铅压电陶瓷取代传统的含铅压电材料作为压电雾化片的核心元件，绿色环保，可有效避免压电陶瓷材料在生产、使用和废弃过程中带来的铅污染，减少对人类健康和环境的损害。将本发明得到的铌酸钾钠基无铅压电陶瓷制备成直径20毫米的雾化片用于压电雾化装置，出雾量可达300-400mL/h，使用寿命在3000小时以上，表明该无铅压电雾化片具有好的出雾能力，达到作为雾化器件的应用要求。
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具体实施方式
本具体实施方法仅仅是对本发明的解释，并不是对本发明的限制。本领域技术人员在阅读了本发明的说明书之后所做出的任何改变，只要在权利要求书的范围内，都将受到专利法的保护。
实施例1：
一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷，包含以下原子百分比的化学组成，90%的(K0.4Na0.6)Nb0.9Sb0.1O3和10%的BaZr0.5Ti0.5O3，制备方法包括以下步骤：
（1）原料预处理：将碳酸钾、碳酸钠、五氧化二铌、三氧化二锑、碳酸钡、二氧化锆和二氧化钛放入培养皿，置于烘箱内，在120℃下保温5h；
（2）称料混合：按所述化学组成配比称量预处理后的原料，分散于无水乙醇中，放入球磨机湿磨，球磨机的转速为450rpm，湿磨时间为24h，湿磨结束后取出放入烘箱烘干，用玛瑙研钵磨碎，过80目筛，制成干粉；
（3）预烧：将预混粉置于箱式炉中连续升温至850℃，保温8h，降温至室温后粉碎过筛，得到预烧粉；
（4）烧结：将预烧粉干压成型为生坯，在0.1MPa氧气气氛烧结炉中于1200℃下保温6h，得到致密的压电陶瓷片；
（5）后处理：将烧结好的压电陶瓷片加工成所需形状，在两侧镀上银层，烧银温度为600℃；在被银陶瓷片两侧电极分别标注正负极，放入装有硅油的极化装置中，油浴加热至80℃，在3kV/mm的电压下极化30min，然后在室温下放置24h老化，得到所述铌酸钾钠基无铅压电陶瓷。
将所述铌酸钾钠基无铅压电陶瓷制作成直径20mm的压电雾化片，并用于压电雾化装置，出雾量可达350mL/h，使用寿命在3500小时以上。
实施例2：
一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷，包含以下原子百分比的化学组成，92%的(K0.4Na0.6)Nb0.85Sb0.15O3和8%的BaZr0.5Ti0.5O3，制备方法包括以下步骤：
（1）原料预处理：将碳酸钾、碳酸钠、五氧化二铌、三氧化二锑、碳酸钡、二氧化锆和二氧化钛放入培养皿，置于烘箱内，在150℃下保温3h；
（2）称料混合：按所述化学组成配比称量预处理后的原料，分散于无水乙醇中，放入球磨机湿磨，球磨机的转速为400rpm，湿磨时间为36h，湿磨结束后取出放入烘箱烘干，用玛瑙研钵磨碎，过80目筛，制成干粉；
（3）预烧：将预混粉置于箱式炉中连续升温至900℃，保温6h，降温至室温后粉碎过筛，得到预烧粉；
（4）烧结：将预烧粉干压成型为生坯，在0.1MPa空气气氛烧结炉中于1200℃下保温10h，得到致密的压电陶瓷片；
（5）后处理：将烧结好的压电陶瓷片加工成所需形状，在两侧镀上银层，烧银温度为600℃；在被银陶瓷片两侧电极分别标注正负极，放入装有硅油的极化装置中，油浴加热至80℃，在3kV/mm的电压下极化30min，然后在室温下放置24h老化，得到所述铌酸钾钠基无铅压电陶瓷。
将所述铌酸钾钠基无铅压电陶瓷制作成直径20mm的压电雾化片，并用于压电雾化装置，出雾量可达400mL/h，使用寿命在3000小时以上。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (6)

1.一种用于压电雾化片的铌酸钾钠基无铅压电陶瓷，其特征在于：所述铌酸钾钠基无铅压电陶瓷的化学组成为：(1-x)(K0.4Na0.6)Nb1-y Sb y O3+xBaZr0.5Ti0.5O3；所述x，y为摩尔百分比，0≤x≤0.4，0.01≤y≤0.2。
2.一种如权利要求1所述的铌酸钾钠基无铅压电陶瓷的制作工艺，其特征在于，包括以下步骤：
（1）原料预处理：将碳酸钾、碳酸钠、五氧化二铌、三氧化二锑、碳酸钡、二氧化锆和二氧化钛放入培养皿，置于烘箱内，在120-150℃下保温3-6h；
（2）称料混合：按所述化学组成配比称量预处理后的原料，分散于无水乙醇中，混合均匀后烘干，粉碎过筛，制成预混粉；
（3）预烧：将预混粉置于箱式炉中连续升温至850-1000℃，保温4-8h，降温至室温后粉碎过筛，得到预烧粉；
（4）烧结：将预烧粉干压成型为生坯，在气氛烧结炉中于1100-1300℃下保温6-12h，得到致密的压电陶瓷片；
（5）后处理：将烧结好的压电陶瓷片加工成所需形状，在两侧镀上银层，标注正负极后极化老化得到所述成品铌酸钾钠基无铅压电陶瓷。
3.根据权利要求2所述的一种铌酸钾钠基无铅压电陶瓷的制作工艺，其特征在于：步骤（2）所述预处理后的原料分散于无水乙醇后通过球磨机湿磨混合均匀，所述球磨机的转速为300-600rpm，湿磨时间为24-48h。
4.根据权利要求2所述的一种铌酸钾钠基无铅压电陶瓷的制作工艺，其特征在于：步骤（4）所述气氛烧结炉的烧结气为空气或氧气，气压为0.1-0.5MPa。
5.根据权利要求2所述的一种铌酸钾钠基无铅压电陶瓷的制作工艺，其特征在于：步骤（5）所述镀银过程为：在陶瓷片的两表面用丝网涂上厚度为0.01mm的银浆，在150℃下烘干，随后在箱式炉中升温至550-650℃，保温60min后降温至室温，得到被银陶瓷片。
6.根据权利要求2所述的一种铌酸钾钠基无铅压电陶瓷的制作工艺，其特征在于：步骤（5）所述极化老化过程为：将标注有正负极的被银陶瓷片放入装有硅油的极化装置中，油浴加热至60-100℃，在3-5kV/mm的电压下极化30min，然后在室温下放置24h老化，得到所述铌酸钾钠基无铅压电陶瓷。
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