CN119161184B - 高机电耦合系数无铅压电陶瓷材料及其制备方法和应用 - Google Patents
高机电耦合系数无铅压电陶瓷材料及其制备方法和应用 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 60
- 230000008878 coupling Effects 0.000 title claims abstract description 43
- 238000010168 coupling process Methods 0.000 title claims abstract description 43
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000919 ceramic Substances 0.000 claims abstract description 58
- 239000011159 matrix material Substances 0.000 claims abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 27
- 229910052709 silver Inorganic materials 0.000 claims description 27
- 239000004332 silver Substances 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 25
- 239000002002 slurry Substances 0.000 claims description 22
- 238000000227 grinding Methods 0.000 claims description 20
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 18
- 238000005266 casting Methods 0.000 claims description 17
- 238000005303 weighing Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 12
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-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
- 230000010287 polarization Effects 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
- 239000002994 raw material Substances 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 10
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 6
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 6
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 6
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical group CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000009694 cold isostatic pressing Methods 0.000 claims description 6
- 230000005684 electric field Effects 0.000 claims description 6
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 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
- 239000000203 mixture Substances 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 239000013530 defoamer Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- -1 naNbO 3 template Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 12
- 231100000614 poison Toxicity 0.000 abstract description 4
- 239000003440 toxic substance Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 description 15
- 238000001816 cooling Methods 0.000 description 12
- 229910052726 zirconium Inorganic materials 0.000 description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 9
- 229920002799 BoPET Polymers 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 239000011734 sodium Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000007650 screen-printing Methods 0.000 description 5
- 230000033228 biological regulation Effects 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 238000003475 lamination Methods 0.000 description 3
- 239000012856 weighed raw material Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
本发明涉及压电陶瓷材料技术领域，具体为高机电耦合系数无铅压电陶瓷材料及其制备方法和应用。所述的高机电耦合系数无铅压电陶瓷材料，由以下基体制备：(0.99‑x)(K0.5Na0.5)(Nb0.96Sb0.04)O3‑0.01BaZrO3‑xBi0.5(Ag0.5Li0.5)0.5HfO3。本发明高机电耦合系数无铅压电陶瓷材料具有优异的电学性能，其KP可以达到57%，d33可以达到462 pC/N，使得本发明的压电陶瓷具备在工业中应用的条件。本发明高机电耦合系数无铅压电陶瓷材料制备过程更具有安全性，不含铅元素及甲苯等有毒物质。
Description
技术领域
本发明涉及压电陶瓷材料技术领域，具体为高机电耦合系数无铅压电陶瓷材料及其制备方法和应用。
背景技术
压电陶瓷具有电能和机械能相互转换的特性，在蜂鸣器、雾化器、传感器和换能器等多种功能器件中广泛应用。Pb(Zr，Ti)O3(PZT)基陶瓷体系自发明以来凭借其优异的电学性能在压电应用领域占据主导地位。然而，铅基压电陶瓷中含有大量铅元素，在陶瓷制备和废弃处理过程中会对环境造成严重危害，现阶段无铅压电材料已成为当前压电材料发展的主要趋势。
铌酸钾钠基压电陶瓷可以通过相结构调控产生优异压电性能的同时还能保持较高居里温度的特点，被认为是取代PZT基陶瓷最有前途的压电陶瓷体系之一。然而，铌酸钾钠基陶瓷虽然性能优异，但是在陶瓷制备过程中钾和钠元素易挥发、成瓷性差等问题严重限制了其实际化应用。针对上述问题，研究人员采用组元调控、离子掺杂以及织构化工艺等方式对铌酸钾钠基压电陶瓷进行系统性调控，制备出烧结特性良好、性能优异的无铅压电陶瓷样品。目前国内外铌酸钾钠基压电陶瓷产品性能仍然无法达到铅基压电陶瓷性能指标，主要原因在于电学性能优异的无铅压电陶瓷配方中组元调控与离子掺杂十分精细，实际生产过程中无法保证陶瓷配方化学计量比的精确性。织构化工艺是指通过添加模板诱导陶瓷中的晶粒向某一方向进行取向生长，烧结后的陶瓷具有与单晶类似的各向异性，其压电性能显著提升。当前无铅压电陶瓷的织构化工艺仍处于实验室阶段，存在织构浆料部分配方中存在甲苯等毒性物质、制备样品规格较小且无法批量制备等问题，距其取代铅基压电陶瓷进行实际化应用仍有较大差距。
发明内容
根据以上现有技术中的不足，本发明的目的是提供一种高机电耦合系数无铅压电陶瓷材料，具有优异的电学性能，其KP可以达到57%，d33可以达到462 pC/N，使得本发明的压电陶瓷具备在工业中应用的条件。
本发明的另一个目的在于提供一种高机电耦合系数无铅压电陶瓷材料的制备方法，成本较低且制备方法简单易行，可以满足工业化生产的要求。
本发明的第三个目的在于提供一种高机电耦合系数无铅压电陶瓷材料的应用，用于能量收集器、换能器或传感器。
本发明是采用以下的技术方案实现的：
所述的高机电耦合系数无铅压电陶瓷材料，由以下基体制备：(0.99-x)(K0.5Na0.5)(Nb0.96Sb0.04)O3-0.01BaZrO3-xBi0.5(Ag0.5Li0.5)0.5HfO3；
所述的基体中，x的取值可以为0.01、0.02、0.03或0.04中的一种。
所述的高机电耦合系数无铅压电陶瓷材料的制备方法，包括以下步骤：
（1）按照高机电耦合系数无铅压电陶瓷材料基体化学通式中元素的化学计量比称取K2CO3、Na2CO3、Nb2O5、Sb2O3、BaCO3、ZrO2、Bi2O3、Ag2O、Li2CO3、HfO2原料，经球磨、烘干、过筛后获得粉体基料；
（2）称取粉体基料、NaNbO3模板、溶剂、增塑剂、消泡剂和粘结剂进行辊磨混合，获得流延浆料；
（3）将所述流延浆料进行流延、干燥、切割，叠片、烘烤、冷等静压、冲片和排胶，获得陶瓷生坯；
（4）将所述陶瓷生坯进行烧结，并对成品进行加工，加工成尺寸为直径16mm，厚度为0.7mm的圆片，获得无铅压电陶瓷材料；
（5）将步骤（4）得到的无铅压电陶瓷材料陶瓷片，涂覆银浆并进行烧结，获得具有银电极的压电陶瓷；
（6）将步骤（5）得到的具有银电极的压电陶瓷进行极化，得到高机电耦合系数无铅压电陶瓷材料。
圆片参考国家标准GB/T 2414.1-1998制备。步骤（5）中，涂覆银浆均采用丝网印刷，厚度为10-30μm。
球磨时，采用锆球与原料的重量比为2:1，溶剂为无水乙醇，其与原料的重量比为2-2.2:1。
所述的步骤（2）中的溶剂为乙酸丁酯与无水乙醇按质量比1:（0.8-1.2）的混合物，增塑剂为邻苯二甲酸二辛酯，消泡剂为正丁醇，粘结剂为聚乙烯醇缩丁醛；粉体基料、NaNbO3模板、溶剂、增塑剂、消泡剂和粘结剂的质量比为10:0.3:9:0.3:0.25:0.9；混合时间为10-12h。
所述的步骤（3）中流延时，刮刀高度为100-200μm。
所述的步骤（3）中烘烤条件为室温升高至100℃，之后保温30-60min。
所述的步骤（3）中排胶条件为：以0.5℃/min的速度升温至180℃，保温6h后，再以0.2℃/min的速度升温至570℃，保温4h后，随炉冷却。
所述的步骤（4）中烧结条件为：使用埋烧法将四组分圆片以5℃/min的速度从室温升温至900℃，再以3℃/min的速度升温至1190℃，保温1min后，以10℃/min的速度冷却至1110℃，保温6h后，随炉冷却。
所述的步骤（6）中极化温度为25-60℃，极化电场为15-20kV/cm，极化时间为20-30min。
所述的高机电耦合系数无铅压电陶瓷材料的应用，用于能量收集器、换能器或传感器。
与现有技术相比，本发明的有益效果是：
(1) 本发明高机电耦合系数无铅压电陶瓷材料具有优异的电学性能，其KP可以达到57%，d33可以达到462 pC/N，使得本发明的压电陶瓷具备在工业中应用的条件。
(2) 本发明高机电耦合系数无铅压电陶瓷材料制备过程更具有安全性，不含铅元素及甲苯等有毒物质。
(3) 本发明高机电耦合系数无铅压电陶瓷材料可以采用工业用原料制备，成本较低且制备方法简单易行，可以满足工业化生产的要求。
附图说明
图1为高机电耦合系数无铅压电陶瓷材料实物图。
图2为实施例1无铅压电陶瓷材料的阻抗、相位角与频率示意图。
图3为实施例2无铅压电陶瓷材料的阻抗、相位角与频率示意图。
图4为实施例3无铅压电陶瓷材料的阻抗、相位角与频率示意图。
图5为实施例4无铅压电陶瓷材料的阻抗、相位角与频率示意图。
图6为对比例1无铅压电陶瓷材料的阻抗、相位角与频率示意图。
具体实施方式
为了使本发明目的、技术方案更加清楚明白，对本发明作进一步的详细说明。
实施例1
具有高机电耦合系数无铅压电陶瓷材料的制备方法，采用以下步骤：
（1）按0.98(K0.5Na0.5)(Nb0.96Sb0.04)O3-0.01BaZrO3-0.01Bi0.5(Ag0.5Li0.5)0.5HfO3分别称量烘干后的K2CO3、Na2CO3、Nb2O5、Sb2O3、BaCO3、ZrO2、Bi2O3、Ag2O、Li2CO3、HfO2原料，称量后的原料共计40.51g，放入球磨罐中并加入80g无水乙醇，在行星式球磨机上球磨18h，将球磨后的浆料与锆球分离后放入烘箱中并在80℃下烘干，烘干后使用玛瑙研钵将样品磨成粉体，倒入坩埚中并用研磨棒压实，在850℃下保温5h；预烧后的粉料使用玛瑙研钵磨成粉体并放入球磨罐中，加入80g无水乙醇后进行二次球磨，时间为48h，球磨后的浆料与锆球分离后放入烘箱中在80℃下烘干；将烘干后的基料研磨并过200目筛后即可得到粉体基料；
（2）称取20g粉体基料，然后分别加入0.6g的NaNbO3模板、18g溶剂(溶剂为乙酸丁酯与无水乙醇的混合物，质量比为1：0.8）、0.6g邻苯二甲酸二辛酯、0.5g正丁醇和1.8g聚乙烯醇缩丁醛后，在辊磨机上辊磨10h，转速为180r/min，得到粘结剂与浆料混合均匀的流延浆料；
（3）流延浆料通过刮刀的作用在PET膜上流延成膜(刮刀高度为100μm)，待湿膜自然干燥后，用刀片将样品膜从PET膜上刮下；刮下的膜切割成大小为2×2cm的正方形膜进行叠片，膜总层数保持在40层，得到压制前的坯体。将坯体放入烘箱中由室温升高至100℃下保温30min后取出，进行冷等静压(压力为200MPa)。取出压好的样品冲片后，以0.5℃/min的速度升温至180℃，保温6h后，再以0.2℃/min的速度升温至570℃，保温4h后，随炉冷却进行排粘，得到陶瓷生坯；
（4）将生坯在马弗炉中利用两步烧结法进行烧结：从室温升至900℃(升温速率为5℃/min)，再以3℃/min的速度升温至1190℃，保温1min后快速冷却(冷却的速率为10℃/min)到1110℃，并在此温度下保温6h，制备出无铅压电陶瓷材料，烧结后的陶瓷采用磨床加工成尺寸为直径16mm，厚度为0.7mm的圆片；
（5）将以上圆片超声清洗后涂覆银浆，涂覆银浆均采用丝网印刷，厚度为10μm，烧银后获得具有银电极的压电陶瓷；
（6）将具有银电极的压电陶瓷进行极化，极化温度为25℃，极化电场为15kV/cm，极化时间为20min，得到高机电耦合系数无铅压电陶瓷材料。所得高机电耦合系数无铅压电陶瓷材料的阻抗、相位角与频率示意图见图2。所得高机电耦合系数无铅压电陶瓷材料的实物图见图1。
实施例2
具有高机电耦合系数无铅压电陶瓷材料的制备方法，采用以下步骤：
（1）按0.97(K0.5Na0.5)(Nb0.96Sb0.04)O3-0.01BaZrO3-0.02Bi0.5(Ag0.5Li0.5)0.5HfO3分别称量烘干后的K2CO3、Na2CO3、Nb2O5、Sb2O3、BaCO3、ZrO2、Bi2O3、Ag2O、Li2CO3、HfO2原料，称量后的原料共计40.89g，放入球磨罐中并加入80g无水乙醇，在行星式球磨机上球磨18h，将球磨后的浆料与锆球分离后放入烘箱中并在80℃下烘干，烘干后使用玛瑙研钵将样品磨成粉体，倒入坩埚中并用研磨棒压实，在850℃下保温5h；预烧后的粉料使用玛瑙研钵磨成粉体并放入球磨罐中，加入80g无水乙醇后进行二次球磨，时间为48h，球磨后的浆料与锆球分离后放入烘箱中在80℃下烘干；将烘干后的基料研磨并过200目筛后即可得到粉体基料；
（2）称取20g粉体基料，然后分别加入0.6g的NaNbO3模板、18g溶剂(溶剂为乙酸丁酯与无水乙醇的混合物，质量比为1：1.2）、0.6g邻苯二甲酸二辛酯、0.5g正丁醇和1.8g聚乙烯醇缩丁醛后在辊磨机上辊磨12h，转速为200r/min，得到粘结剂与浆料混合均匀的流延浆料；
（3）流延浆料通过刮刀的作用在PET膜上流延成膜(刮刀高度为200μm)，待湿膜自然干燥后，用刀片将样品膜从PET膜上刮下；刮下的膜切割成大小为2×2cm的正方形膜进行叠片，膜总层数保持在60层，得到压制前的坯体。将坯体放入烘箱中由室温升高至100℃下保温60min后取出，进行冷等静压(压力为200MPa)，取出压好的样品冲片后，以0.5℃/min的速度升温至180℃，保温6h后，再以0.2℃/min的速度升温至570℃，保温4h后，随炉冷却进行排粘，得到陶瓷生坯；
（4）将生坯在马弗炉中利用两步烧结法进行烧结：从室温升至900℃(升温速率为5℃/min)，再以3℃ /min的速度升温至1190℃，保温1min后快速冷却(冷却的速率为10℃/min)到1110℃，并在此温度下保温6h，制备出无铅压电陶瓷材料。烧结后的陶瓷采用磨床加工成尺寸为直径16mm，厚度为0.7mm的圆片；
（5）将以上圆片超声清洗后涂覆银浆，涂覆银浆均采用丝网印刷，厚度为30μm，烧银后获得具有银电极的压电陶瓷；
（6）将具有银电极的压电陶瓷进行极化，极化温度为55℃，极化电场为20kV/cm，极化时间为30min，得到高机电耦合系数无铅压电陶瓷材料。所得高机电耦合系数无铅压电陶瓷材料的阻抗、相位角与频率示意图见图3。
实施例3
具有高机电耦合系数无铅压电陶瓷材料的制备方法，采用以下步骤：
（1）按0.96(K0.5Na0.5)(Nb0.96Sb0.04)O3-0.01BaZrO3-0.03Bi0.5(Ag0.5Li0.5)0.5HfO3分别称量烘干后的K2CO3、Na2CO3、Nb2O5、Sb2O3、BaCO3、ZrO2、Bi2O3、Ag2O、Li2CO3、HfO2原料，称量后的原料共计41.27g，放入球磨罐中并加入80g无水乙醇，在行星式球磨机上球磨18h，将球磨后的浆料与锆球分离后放入烘箱中并在80℃下烘干，烘干后使用玛瑙研钵将样品磨成粉体，倒入坩埚中并用研磨棒压实，在850℃下保温5h；预烧后的粉料使用玛瑙研钵磨成粉体并放入球磨罐中，加入80g无水乙醇后进行二次球磨，时间为48h，球磨后的浆料与锆球分离后放入烘箱中在80℃下烘干；将烘干后的基料研磨并过200目筛后即可得到粉体基料；
（2）称取20g粉体基料，然后分别加入0.6g的NaNbO3模板、18g溶剂(溶剂为乙酸丁酯与无水乙醇的混合物，质量比为1：1）、0.6g邻苯二甲酸二辛酯、0.5g正丁醇和1.8g聚乙烯醇缩丁醛后，在辊磨机上辊磨10h，转速为180-200r/min，得到粘结剂与浆料混合均匀的流延浆料；
（3）流延浆料通过刮刀的作用在PET膜上流延成膜(刮刀高度为160μm)，待湿膜自然干燥后，用刀片将样品膜从PET膜上刮下；刮下的膜切割成大小为2×2cm的正方形膜进行叠片，膜总层数保持在50层，得到压制前的坯体。将坯体放入烘箱中由室温升高至100℃下保温30min后取出，进行冷等静压(压力为200MPa)。取出压好的样品冲片后，以0.5℃/min的速度升温至180℃，保温6h后，再以0.2℃/min的速度升温至570℃，保温4h后，随炉冷却进行排粘，得到陶瓷生坯；
（4）然后将生坯在马弗炉中利用两步烧结法进行烧结：从室温升至900℃(升温速率为5℃/min)，再以3℃/min的速度升温至1190℃，保温1min后快速冷却(冷却的速率为10℃/min)到1110℃，并在此温度下保温6h，制备出无铅压电陶瓷材料。烧结后的陶瓷采用磨床加工成尺寸为直径16mm，厚度为0.7mm的圆片；
（5）将以上圆片超声清洗后涂覆银浆，涂覆银浆均采用丝网印刷，厚度为20μm，烧银后获得具有银电极的压电陶瓷；
（6）将具有银电极的压电陶瓷进行极化，极化温度为25℃，极化电场为20kV/cm，极化时间为25min，得到高机电耦合系数无铅压电陶瓷材料。所得高机电耦合系数无铅压电陶瓷材料的阻抗、相位角与频率示意图见图4。
实施例4
具有高机电耦合系数无铅压电陶瓷材料的制备方法，采用以下步骤：
（1）按0.95(K0.5Na0.5)(Nb0.96Sb0.04)O3-0.01BaZrO3-0.04Bi0.5(Ag0.5Li0.5)0.5HfO3分别称量烘干后的K2CO3、Na2CO3、Nb2O5、Sb2O3、BaCO3、ZrO2、Bi2O3、Ag2O、Li2CO3、HfO2原料，称量后的原料共计41.65g，放入球磨罐中并加入80g无水乙醇，在行星式球磨机上球磨18h，将球磨后的浆料与锆球分离后放入烘箱中并在80℃下烘干，烘干后使用玛瑙研钵将样品磨成粉体，倒入坩埚中并用研磨棒压实，在850℃下保温5h；预烧后的粉料使用玛瑙研钵磨成粉体并放入球磨罐中，加入80g无水乙醇后进行二次球磨，时间为48h，球磨后的浆料与锆球分离后放入烘箱中在80℃下烘干；将烘干后的基料研磨并过200目筛后即可得到粉体基料；
（2）称取20g粉体基料，然后分别加入0.6g的NaNbO3模板、18g溶剂(溶剂为乙酸丁酯与无水乙醇的混合物，质量比为1：1）、0.6g邻苯二甲酸二辛酯、0.5g正丁醇和1.8g聚乙烯醇缩丁醛后，在辊磨机上辊磨10h，转速为180-200r/min，得到粘结剂与浆料混合均匀的流延浆料；
（3）流延浆料通过刮刀的作用在PET膜上流延成膜(刮刀高度为180μm)，待湿膜自然干燥后，用刀片将样品膜从PET膜上刮下；刮下的膜切割成大小为2×2cm的正方形膜进行叠片，膜总层数保持在60层，得到压制前的坯体。将坯体放入烘箱中由室温升高至100℃下保温30min后取出，进行冷等静压(压力为200MPa)。取出压好的样品冲片后，以0.5℃/min的速度升温至180℃，保温6h后，再以0.2℃/min的速度升温至570℃，保温4h后，随炉冷却进行排粘，得到陶瓷生坯；
（4）将生坯在马弗炉中利用两步烧结法进行烧结：从室温升至900℃(升温速率为5℃/min)，再以3℃/min的速度升温至1190℃，保温1min后快速冷却(冷却的速率为10℃/min)到1110℃，并在此温度下保温6h，制备出无铅压电陶瓷材料。烧结后的陶瓷采用磨床加工成尺寸为直径16mm，厚度为0.7mm的圆片；
（5）将以上圆片超声清洗后涂覆银浆，涂覆银浆均采用丝网印刷，厚度为30μm，烧银后获得具有银电极的压电陶瓷；
（6）将具有银电极的压电陶瓷进行极化，极化温度为45℃，极化电场为20kV/cm，极化时间为25min，得到高机电耦合系数无铅压电陶瓷材料。所得高机电耦合系数无铅压电陶瓷材料的阻抗、相位角与频率示意图见图5。
对比例1
一种无铅压电陶瓷材料的制备方法，包括以下步骤：
制备方法同实施例3，区别在于步骤（2）中不添加NaNbO3模板。所得无铅压电陶瓷材料的阻抗、相位角与频率示意图见图6。
实施例1-4和对比例1的测试数据见表1。
表1实施例1-4和对比例1的测试数据
表1中所列的机电耦合系数KP是由附图中谐振与反谐振频率计算得出，计算公式如下：
；
其中，fr为谐振频率；fa为反谐振频率。
从表1中数据可以看出，随着组元掺杂量的不断提升，陶瓷的压电性能呈现出先增加后降低的趋势，表明适当的组元掺杂可以调控陶瓷在室温下的相结构进而影响陶瓷性能，促进陶瓷压电性能的提升。从实施例3与对比例1的性能对比中可以看出，织构工艺对陶瓷压电性能的提升是十分显著的，其d33和KP分别提升了64%和39%，性能优于当前市场中用于制备蜂鸣片的无铅压电陶瓷。本发明不仅在组元调控和织构工艺的基础上对陶瓷压电性能进行了优化，而且对织构陶瓷制备流程的安全性(无甲苯和铅元素等有毒物质)和可行性(成本低，工艺简单)进行了调整，能够满足批量化生产要求。
Claims (7)
1.一种高机电耦合系数无铅压电陶瓷材料，其特征在于，由以下基体制备：(0.99-x)(K0.5Na0.5)(Nb0.96Sb0.04)O3-0.01BaZrO3-xBi0.5(Ag0.5Li0.5)0.5HfO3；
所述的基体中，x的取值为0.01、0.02、0.03或0.04中的一种；
所述的高机电耦合系数无铅压电陶瓷材料的制备方法，包括以下步骤：
（1）按照高机电耦合系数无铅压电陶瓷材料基体化学通式中元素的化学计量比称取K2CO3、Na2CO3、Nb2O5、Sb2O3、BaCO3、ZrO2、Bi2O3、Ag2O、Li2CO3、HfO2原料，经球磨、烘干、过筛后获得粉体基料；
（2）称取粉体基料、NaNbO3模板、溶剂、增塑剂、消泡剂和粘结剂进行辊磨混合，获得流延浆料；
（3）将所述流延浆料进行流延、干燥、切割，叠片、烘烤、冷等静压、冲片和排胶，获得陶瓷生坯；
（4）将所述陶瓷生坯进行烧结，并对成品进行加工，加工成尺寸为直径16mm，厚度为0.7mm的圆片，获得无铅压电陶瓷材料陶瓷片；
（5）将步骤（4）得到的无铅压电陶瓷材料陶瓷片，涂覆银浆并进行烧结，获得具有银电极的压电陶瓷；
（6）将步骤（5）得到的具有银电极的压电陶瓷进行极化，得到高机电耦合系数无铅压电陶瓷材料；
所述的步骤（2）中的溶剂为乙酸丁酯与无水乙醇按质量比1:（0.8-1.2）的混合物，增塑剂为邻苯二甲酸二辛酯，消泡剂为正丁醇，粘结剂为聚乙烯醇缩丁醛；粉体基料、NaNbO3模板、溶剂、增塑剂、消泡剂和粘结剂的质量比为10:0.3:9:0.3:0.25:0.9；混合时间为10-12h。
2.根据权利要求1所述的高机电耦合系数无铅压电陶瓷材料，其特征在于，所述的步骤（3）中流延时，刮刀高度为100-200μm。
3.根据权利要求1所述的高机电耦合系数无铅压电陶瓷材料，其特征在于，所述的步骤（3）中烘烤条件为室温升高至100℃，之后保温30-60min。
4.根据权利要求1所述的高机电耦合系数无铅压电陶瓷材料，其特征在于，所述的步骤（3）中排胶条件为：以0.5℃/min的速度升温至180℃，保温6h后，再以0.2℃/min的速度升温至570℃，保温4h后，随炉冷却。
5.根据权利要求1所述的高机电耦合系数无铅压电陶瓷材料，其特征在于，所述的步骤（4）中烧结条件为：使用埋烧法将四组分圆片以5℃/min的速度从室温升温至900℃，再以3℃/min的速度升温至1190℃，保温1min后，以10℃/min的速度冷却至1110℃，保温6h后，随炉冷却。
6.根据权利要求1所述的高机电耦合系数无铅压电陶瓷材料，其特征在于，所述的步骤（6）中极化温度为25-60℃，极化电场为15-20kV/cm，极化时间为20-30min。
7.一种权利要求1所述的高机电耦合系数无铅压电陶瓷材料的应用，其特征在于，用于能量收集器、换能器或传感器。
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