CN111646797A - 一种多层无铅压电陶瓷驱动器及其制备方法 - Google Patents
一种多层无铅压电陶瓷驱动器及其制备方法 Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 26
- 238000000498 ball milling Methods 0.000 claims description 26
- 239000002994 raw material Substances 0.000 claims description 22
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims description 17
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
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- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Inorganic materials O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 6
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 6
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Abstract
本发明涉及一种多层无铅压电陶瓷驱动器及其制备方法，化学分子式为:(1‑a)(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07‑aCaZrO3‑bCuO,其中a＝0.01～0.05,b＝0.1‑2％。采用传统的固相法合成压电陶瓷粉体，将粉体配制浆料，然后利用流延成型法制备压电陶瓷薄片，进而通过印刷电极，采用三步烧结法共烧，制成叠层驱动器。该方法工艺简单，可广泛应用于压电陶瓷驱动器等高精度位移控制器方面。
Description
技术领域
本发明属于电子信息功能材料与元器件领域，尤其是涉及一种多层无铅压电陶瓷驱动器及其制备方法。
背景技术
驱动器是智能结构中的核心部件之一，并且驱动器被认为是影响电子元器件寿命的主要因素，而在多数驱动器中，陶瓷驱动器因其具有优异的性能而受到广泛的关注。
多层压电陶瓷驱动器是利用压电陶瓷的逆压电效应，在多层压电陶瓷驱动器上施加电压后产生位移，是一种小型化、集成化的电子元器件。多层压电陶瓷驱动器以其转换效率高、位移精度高、低能耗、响应速度快等特点已经广泛应用于激光光路调整、扬声器、机床伺服刀头位移控制、线性马达等领域。
目前市场上应用的主要是铅基多层压电陶瓷驱动器，然而铅基压电陶瓷中PbO含量高达60wt％以上，由于氧化铅是一种易挥发的有毒物质，使得PZT材料在使用和废弃处理过程中给人类和环境带来极大的危害。目前国内采用制备多层压电陶瓷驱动器都是高温共烧技术，高温共烧中采用的多为钯含量高于80％的内电极，钯为贵金属，成本较高，会限制企业的发展。因此很有必要探索一种可以调控多层无铅压电陶瓷驱动器低温烧结的烧结方法。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种工艺简单、成本低其具有实用性的多层无铅压电陶瓷驱动器制备方法。
本发明的目的可以通过以下技术方案来实现：
一种多层无铅压电陶瓷驱动器及其制备方法，化学分子式为:(1-a)(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-aCaZrO3-bCuO，其中a＝0.01～0.05，b＝0.1-2％。
多层无铅压电陶瓷驱动器及其制备方法，采用以下步骤：
(1)选取纯度大于99％的Na2CO3,K2CO3,Li2CO3,Nb2O5,Sb2O5,CaCO3,ZrO2和CuO作为铌酸钾钠基无铅压电陶瓷的原料；
(2)按照配方组成称量原料、混合、球磨、烘干；
(3)烘干后的原料在850℃下预烧，保温时间6h；
(4)预烧后的粉料加入CuO进行二次球磨，烘干；
(5)将混合制得的粉料置于球磨罐中，加入溶剂，辊磨8-12小时，再加入粘结剂继续辊磨5-8小时，制得浆料；
(6)取出制得的浆料，使用流延机在玻璃基板上进行流延，流延后将玻璃基片平放、静置，形成膜片，将膜片从玻璃基板上刮下，切割后叠片，丝网印刷上内电极后热压成型，将成型后的坯体排胶；
(7)排胶后的坯体于1000～1050℃下进行第一步烧结，升温速度为3℃/min,保温0min；
(8)将第一步1000～1050℃的烧结温度快速升温到1100～1150℃，保温0～5min，进行第二步烧结；
(9)快速降温到700～1000℃，保温2～10h，进行第三步烧结；自然冷却到室温；
(10)将烧结成瓷的样品两侧抛光，被上外电极，600℃，保温10-30min，自然冷却到室温，得到铌酸钾钠基无铅压电陶瓷多层驱动器。
与现有技术相比，本发明采用三步烧结法制备多层无铅压电陶瓷驱动器，有效地降低了烧结温度，该方法对于多层无铅压电陶瓷驱动器体系可以重复烧结工艺，是一种工艺简单、成本低其具有实用性的多层无铅压电陶瓷驱动器制备方法。
附图说明
图1为实施例1制得的无铅压电陶瓷的XRD图谱；
图2为实施例1-4制得的铌酸钾钠基无铅压电陶瓷的d33随烧结温度变化图谱；
图3为实施例3制得的铌酸钾钠基无铅压电陶瓷的S-E图谱；
图4为实施例4制得的铌酸钾钠基无铅压电陶瓷的S-E图谱；
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。
实施例1
多层无铅压电陶瓷驱动器及其制备方法，采用以下步骤：
(1)按照化学分子式为:(1-a)(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-aCaZrO3-bCuO的化学计量比称取原料Na2CO3,K2CO3,Li2CO3,Nb2O5,Sb2O5,ZrO2和CaCO3，其中a＝0.04,装入球磨罐中进行混料，球磨介质为无水乙醇和氧化锆球，混合原料与氧化锆球的质量比为1:1.2，与无水乙醇的质量比为1:1.5；混合原料在360r/min的速度下球磨24h，100℃烘干后，装入刚玉坩埚中，加盖，在850℃下保温6h，升温速率为3℃/min；
(2)将步骤(1)得到的粉料在研钵中研细，加入bCuO进行二次球磨,其中b＝0.5％，得到0.96(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-0.04CaZrO3-CuO混合粉料；
(3)将步骤(2)得到的粉料加入浓度为8wt％的PVA溶液进行造粒，并在100MPa压力下压制成直径为10mm的陶瓷坯体，其中，PVA溶液占混合粉料与PVA溶液总质量的5％；
(4)将步骤(3)得到的陶瓷坯体在600℃下保温5h以除去粘合剂(PVA)，得到排胶坯体；
(5)将步骤(4)得到的排胶坯体放置在装有锆粉的坩埚中，埋烧；按升温速度3℃/min于1000℃下保温0min进行第一次烧结；然后以10℃/min快速升温至1100℃，保温1min进行第二步烧结；再以10℃/min快速降温至900℃，保温5h进行第三步烧结，随后随炉自然冷却至室温，得到铌酸钾钠基无铅压电陶瓷。
(6)将步骤(5)得到的铌酸钾钠基无铅压电陶瓷抛光被上银电极，在120℃的硅油中，40kV/cm电压下极化30min。
图1为的实施例1所制得的无铅压电陶瓷XRD图谱，结果如图1所示，制备的压电陶瓷为典型单一的钙钛矿结构，烧结温度的不同并没有引起晶体结构的变化。与传统烧结方法相比，采用三步烧结法制备的CuO掺杂铌酸钾钠压电陶瓷能有效降低烧结温度，同时不会改变原来的钙钛矿结构。
实施例2
多层无铅压电陶瓷驱动器及其制备方法，采用以下步骤：
(1)按照化学分子式为:(1-a)(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-aCaZrO3-bCuO的化学计量比称取原料Na2CO3,K2CO3,Li2CO3,Nb2O5,Sb2O5,ZrO2和CaCO3，其中a＝0.04,装入球磨罐中进行混料，球磨介质为无水乙醇和氧化锆球，混合原料与氧化锆球的质量比为1:1.2，与无水乙醇的质量比为1:1.5；混合原料在360r/min的速度下球磨24h，100℃烘干后，装入刚玉坩埚中，加盖，在850℃下保温6h，升温速率为3℃/min；
(2)将步骤(1)得到的粉料在研钵中研细，加入bCuO进行二次球磨,其中b＝0.5％，得到0.96(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-0.04CaZrO3-CuO混合粉料；
(3)将步骤(2)得到的粉料加入浓度为8wt％的PVA溶液进行造粒，并在100MPa压力下压制成直径为10mm的陶瓷坯体，其中，PVA溶液占混合粉料与PVA溶液总质量的5％；
(4)将步骤(3)得到的陶瓷坯体在600℃下保温5h以除去粘合剂(PVA)，得到排胶坯体；
(5)将步骤(4)得到的排胶坯体放置在装有锆粉的坩埚中，埋烧；按升温速度3℃/min于1000℃下保温0min进行第一次烧结；然后以10℃/min快速升温至1100℃，保温1min进行第二步烧结；再以10℃/min快速降温至800℃，保温5h进行第三步烧结，随后随炉自然冷却至室温，得到铌酸钾钠基无铅压电陶瓷。
(6)将步骤(5)得到的铌酸钾钠基无铅压电陶瓷抛光被上银电极，在120℃的硅油中，40kV/cm电压下极化30min。
图2为的实施例2所制得的无铅压电陶瓷高温图谱，结果如图2所示，介电峰的位置并无明显变化，表明不同烧结温度并没有改变居里温度。
实施例3
多层无铅压电陶瓷驱动器及其制备方法，采用以下步骤：
(1)按照化学分子式为:(1-a)(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-aCaZrO3-bCuO的化学计量比称取原料Na2CO3,K2CO3,Li2CO3,Nb2O5,Sb2O5,ZrO2和CaCO3，其中a＝0.04,装入球磨罐中进行混料，球磨介质为无水乙醇和氧化锆球，混合原料与氧化锆球的质量比为1:1.2，与无水乙醇的质量比为1:1.5；混合原料在360r/min的速度下球磨24h，100℃烘干后，装入刚玉坩埚中，加盖，在850℃下保温6h，升温速率为3℃/min；
(2)将步骤(1)得到的粉料在研钵中研细，加入bCuO进行二次球磨,其中b＝0.5％，得到0.96(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-0.04CaZrO3-CuO混合粉料；
(3)将步骤(2)得到的粉料置于球磨罐中，加入溶剂，辊磨8-12小时，再加入粘结剂继续辊磨5-8小时，制得浆料；
(4)将步骤(3)得到的浆料，使用流延机在玻璃基板上进行流延，流延后将玻璃基片平放、静置，形成膜片，将膜片从玻璃基板上刮下，切割后叠片，丝网印刷上内电极后热压成型，将成型后的坯体排胶；
(5)将步骤(4)中排胶后的坯体于1000～1050℃下进行第一步烧结，升温速度为3℃/min,保温0min；
(6)将步骤(5)中第一步1000～1050℃的烧结温度快速升温到1100～1150℃，保温0～5min，进行第二步烧结；
(7)将步骤(6)中快速降温到700～1000℃，保温2～10h，进行第三步烧结；自然冷却到室温；
(8)将步骤(7)烧结成瓷的样品两侧抛光，被上外电极，600℃，保温10-30min，自然冷却到室温，得到铌酸钾钠基无铅压电陶瓷多层驱动器。
图3为实施例3所制得的铌酸钾钠基无铅压电陶瓷SEM图谱，结果如图3所示，陶瓷叠层驱动器单层厚度为50μm，其内电极比较均匀，并无明显渗透到陶瓷中的痕迹。表明三步烧结法制备压电陶瓷多层驱动器是一种有效的制备方法，并能够获得优异的性能。
实施例4
多层无铅压电陶瓷驱动器及其制备方法，采用以下步骤：
(1)按照化学分子式为:(1-a)(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-aCaZrO3-bCuO的化学计量比称取原料Na2CO3,K2CO3,Li2CO3,Nb2O5,Sb2O5,ZrO2和CaCO3，其中a＝0.04,装入球磨罐中进行混料，球磨介质为无水乙醇和氧化锆球，混合原料与氧化锆球的质量比为1:1.2，与无水乙醇的质量比为1:1.5；混合原料在360r/min的速度下球磨24h，100℃烘干后，装入刚玉坩埚中，加盖，在850℃下保温6h，升温速率为3℃/min；
(2)将步骤(1)得到的粉料在研钵中研细，加入bCuO进行二次球磨,其中b＝0.5％，得到0.96(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-0.04CaZrO3-CuO混合粉料；
(3)将步骤(2)得到的粉料置于球磨罐中，加入溶剂，辊磨8-12小时，再加入粘结剂继续辊磨5-8小时，制得浆料；
(4)将步骤(3)得到的浆料，使用流延机在玻璃基板上进行流延，流延后将玻璃基片平放、静置，形成膜片，将膜片从玻璃基板上刮下，切割后叠片，丝网印刷上内电极后热压成型，将成型后的坯体排胶；
(5)将步骤(4)中排胶后的坯体于1000～1050℃下进行第一步烧结，升温速度为3℃/min,保温0min；
(6)将步骤(5)中第一步1000～1050℃的烧结温度快速升温到1100～1150℃，保温0～5min，进行第二步烧结；
(7)将步骤(6)中快速降温到700～1000℃，保温2～10h，进行第三步烧结；自然冷却到室温；
(8)将步骤(7)烧结成瓷的样品两侧抛光，被上外电极，600℃，保温10-30min，自然冷却到室温，得到铌酸钾钠基无铅压电陶瓷多层驱动器。
图4为实施例4所制得的无铅压电陶瓷叠层驱动器的位移随电压变化曲线，测试的频率为5Hz，插图为当电压为150V时的位移变化曲线。从插图中可以看出当电压为150V时，最大位移量为136nm，可以达到目前已报道的铌酸钾钠基无铅压电陶瓷多层驱动器的最大位移量水平，但是采用本方法制备的陶瓷驱动器工艺简单，工艺稳定性好，节约成本。
Claims (9)
1.一种多层无铅压电陶瓷驱动器，其特征在于，化学分子式为:(1-a)(K0.5Na0.5)0.95Li0.05Nb0.93Sb0.07-aCaZrO3-bCuO，其中，a和b均为摩尔分数，a＝0.01～0.05，b＝0.1-2％。
2.如权利要求1中所述的多层无铅压电陶瓷驱动器的制备方法，其特征在于，该方法采用以下步骤：
(1)选取纯度大于99％的Na2CO3,K2CO3,Li2CO3,Nb2O5,Sb2O5,CaCO3,ZrO2和CuO作为铌酸钾钠基无铅压电陶瓷的原料；
(2)按照配方组成称量原料、混合、球磨、烘干；
(3)烘干后的原料在850℃下预烧，保温时间6h；
(4)预烧后的粉料加入CuO进行二次球磨，烘干；
(5)将混合制得的粉料置于球磨罐中，加入溶剂，辊磨8-12小时，再加入粘结剂继续辊磨5-8小时，制得浆料；
(6)取出制得的浆料，使用流延机在玻璃基板上进行流延，流延后将玻璃基片平放、静置，形成膜片，将膜片从玻璃基板上刮下，切割后叠片，丝网印刷上内电极后热压成型，将成型后的坯体排胶；
(7)排胶后的坯体于1000～1050℃下进行第一步烧结，升温速度为3℃/min,保温0min；
(8)将第一步1000～1050℃的烧结温度快速升温到1100～1150℃，保温0～5min，进行第二步烧结；
(9)快速降温到700～1000℃，保温2～10h，进行第三步烧结；自然冷却到室温；
(10)将烧结成瓷的样品两侧抛光，被上外电极，600℃，保温10-30min，自然冷却到室温，得到铌酸钾钠基无铅压电陶瓷多层驱动器。
3.根据权利要求2所述的多层无铅压电陶瓷驱动器的制备方法，其特征在于，两次球磨均在球磨机中进行，球磨过程中加入氧化锆球及无水乙醇作为研磨介质。
4.根据权利要求3所述的制备方法，其特征在于，待研磨的物料与氧化锆球的质量比为1:1.2～1:1.5，待研磨的物料与无水乙醇的质量比1:1.2～1:1.5。
5.根据权利要求2所述的多层无铅压电陶瓷驱动器的制备方法，其特征在于，两次球磨的转速为300～400r/min，时间为12～24h，步骤(2)及步骤(4)中烘干的温度为80～120℃。
6.根据权利要求2所述的多层无铅压电陶瓷驱动器的制备方法，其特征在于，步骤(5)中溶剂的加入量为每10g混料的总重量对应加入5-7g无水乙醇和4-7g甲苯；本体系优选无水乙醇6-3g，甲苯5-7g；溶剂的加入量为每10g混料的总重量对应加入3.5-6.5g粘结剂，优选5.2g。
7.根据权利要求2所述的多层无铅压电陶瓷驱动器的制备方法，其特征在于，步骤(5)中加入溶剂进行辊磨，转速为70r/min，辊磨时间为12h,加入粘结剂进行辊磨，转速为50r/min，辊磨时间为4h；加入的粘结剂为用于制备流延浆料的市售LS粘合剂。
8.根据权利要求2所述的多层无铅压电陶瓷驱动器的制备方法，其特征在于，步骤(6)中流延刮刀与玻璃板的高度为200μm，流延的速度为6cm/s，流延后玻璃板平放静置3h；热压成型是将流延静置后的膜切成1.15cm×1.15cm的片，将一定数量的这些片叠加到一定的高度，然后放入模具中，并且在模具外套上一个可以调控温度的加热装置，然后置于压片机下，加热到70℃,压力大小是70Mpa,反复进行4次，保温保压时间为1h；步骤(6)中所述的内电极为银钯浆料。
9.根据权利要求2所述的多层无铅压电陶瓷驱动器的制备方法，其特征在于，还包括极化处理步骤，将制备得到的铌酸钾钠基无铅压电陶瓷被上银电极，在室温～120℃的硅油中，30～40kV/cm电压下极化30～40min。
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