CN106915965B - 锆酸铅基反铁电多层电容器及其制备方法 - Google Patents
锆酸铅基反铁电多层电容器及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种锆酸铅基反铁电多层电容器及其制备方法,用于制备锆酸铅基反铁电多层电容器的锆酸铅基反铁电材料的化学通式为(Pb0.92‑xBa0.05La0.02Dyx)(Zr0.68Sn0.27Ti0.05)O3;其中,x的取值范围为:0<x≤0.06。本发明的锆酸铅基反铁电多层电容器,用掺杂了Dy的锆酸铅基反铁电材料制备的电容器,在外加电场的作用下,会随Dy含量的增加反铁电相越稳定,能够获得较大的反铁电到铁电转变电场(EAFE‑FE),EAFE‑FE与铁电到反铁电转变电场的差值ΔE逐渐降低,提高了多层电容器的储能密度和储能效率。
Description
技术领域
本发明属于电子功能材料与器件技术领域,具体涉及一种锆酸铅基反铁电多层电容器及其制备方法。
背景技术
人类文明的进步和科学技术的飞速发展在无形中增加了自能源的利用和探索,但是由于能源的大量消耗,能源问题逐渐成为21世纪的人们所面临的主要难题之一。故而增加传统能源在实际应用中的利用率和不断创新去探索新能源代替传统能源逐步成为世界各国研究者的追求目标。其中人们对电子产品方便、简单、快捷的要求,促使相应的电子电路向着集成化、微型化、简洁化发展,给电子元器件设定了新的要求,对于高储能器件和高储能材料的基础性研究首当其冲成为了各大高校、研究机构的研究内容和重点。
锆酸铅基反铁电材料是典型的钙钛矿相结构,反铁电到铁电相发生相变时伴随着巨大的相变电流,其方向与外加场强的方向一致,从宏观上去看电荷沿着电场方向移动,当施加反向电压时,铁电体相向反铁体转变此时电荷被储存,这是其作为储能电容的理论基础。电子技术、信息技术和控制技术的发展,以及器件的小型化和集成化趋势对材料提出了新的要求。
因此,研制储能材料与新型储能技术是关系到我国电子技术发展的紧迫任务之一。
发明内容
本发明的一个目的在于提出一种锆酸铅基反铁电材料。
本发明的锆酸铅基反铁电材料,其化学通式为(Pb0.92-xBa0.05La0.02Dyx)(Zr0.68Sn0.27Ti0.05)O3;其中,x的取值范围为:0<x≤0.06。
根据本发明实施例的锆酸铅基反铁电材料,通过在锆酸铅基反铁电材料中掺杂Dy,提高了锆酸铅基反铁电材料的储能密度,提高了储能效率。用掺杂了Dy的锆酸铅基反铁电材料制备的电容器,在外加电场的作用下,会随Dy含量的增加反铁电相越稳定,能够获得较大的反铁电到铁电转变电场(EAFE-FE),EAFE-FE与铁电到反铁电转变电场(EFE-AFE)的差值ΔE逐渐降低,提高了多层电容器的储能密度和储能效率。
本发明的另一个目的在于提出所述的锆酸铅基反铁电材料的制备方法,包括如下步骤:S101:将四氧化三铅、氧化钡、氧化镧、氧化镝、氧化锆、氧化锡和氧化钛按照摩尔比(0.92-x):0.05:0.02:x:0.68:0.27:0.05混合,得到混合物,然后将所述混合物放入球磨罐中,再加入酒精和氧化锆球球磨2h~6h后烘干;S102:将所述步骤S101得到的产物加热至910℃~1100℃并保温2h~6h;S103:将所述步骤S102得到的产物放入球磨罐中,再加入酒精和氧化锆球球磨3h~6h后烘干,得到锆酸铅基反铁电材料。
另外,根据本发明上述实施例的锆酸铅基反铁电材料的制备方法,还可以具有如下附加的技术特征:
作为本发明优选的实施方式,在所述步骤S101中,烘干的温度为80℃~100℃,烘干的时间为3h~6h;在所述步骤S103中,烘干的温度为80℃~100℃,烘干的时间为3h~6h;在所述步骤S101中,所述混合物与所述酒精和所述氧化锆球的质量比为1:1.5:1;在所述步骤S103中,所述步骤S102得到的产物与所述酒精和所述氧化锆球的质量比为1:1.5:1;所述氧化锆球的直径为2mm~10mm。
本发明的另一目的在于提出一种锆酸铅基反铁电厚膜的制备方法。
所述的锆酸铅基反铁电厚膜的制备方法,包括如下步骤:S201:将锆酸铅基反铁电材料与甲苯-乙醇溶剂和磷酸三丁酯混合后球磨,得到第一浆料;其中,所述锆酸铅基反铁电材料的重量份数为63份~65份,所述甲苯-乙醇溶剂的重量份数为35份~40份,所述磷酸三丁酯的重量份数为0.5份~1份;S202:向所述第一浆料中加入聚乙二醇、邻苯二甲酸丁酯、PVB、环乙酮,然后球磨得到第二浆料;其中,所述聚乙二醇的重量份数为1.5份~2份,所述邻苯二甲酸丁酯的重量份数为1.5份~2份,所述PVB的重量份数为3份~4份,所述环乙酮的重量份数为0.3份~0.8份,所述甲苯-乙醇溶剂中,甲苯与乙醇的体积比为3:(0.8~1.2);S203:通过真空除泡法除去所述第二浆料中的气泡,然后通过流延机流延,得到厚度为20μm~80μm的流延膜生带,然后干燥,得到锆酸铅基反铁电厚膜。
作为本发明的优选的实施方式,在所述步骤S202后,所述步骤S203前,还包括如下步骤:利用冷等静压设备在100MPa~200MPa压强下,保压25min~35min。
本发明的再一个目的在于提出上述的方法制备得到的锆酸铅基反铁电厚膜。
本发明的再一个目的在于提出一种锆酸铅基反铁电多层电容器的制备方法。
所述的锆酸铅基反铁电多层电容器的制备方法,包括如下步骤:S301:通过切片机将锆酸铅基反铁电厚膜切片,然后通过丝网印刷法在所述切片上印刷电极,再将多层所述印刷有电极的切片重叠后热压,得到多层膜;S302:将所述多层膜在500℃~600℃温度下保温5h~6h,然后在800℃~1000℃温度下保温1h~3h,得到锆酸铅基反铁电多层电容器。
作为本发明的优选的实施方式,在所述步骤S301中,所述切片的面积为2.25cm2,所述电极的面积为0.225cm2。
作为本发明的优选的实施方式,在所述步骤S301中,多层所述印刷有电极的切片为10层。
本发明的再一个目的在于提出上述的方法制备得到的锆酸铅基反铁电多层电容器。
本发明的附加方面和优点将在下面的描述中部分给出,部分将从下面的描述中变得明显,或通过本发明的实践了解到。
附图说明
图1是本发明提供的锆酸铅基反铁电多层电容器的XRD图谱;
图2是本发明提供的锆酸铅基反铁电多层电容器在300kV/cm下的P-E图谱;
图3是本发明提供的反铁电到铁电的转变电场以及电滞宽度随Dy含量变化的图谱;
图4是本发明提供的锆酸铅基反铁电多层电容器的能密度和储能效率随着Dy含量变化图谱。
具体实施方式
下面详细描述本发明的实施例,所述实施例的示例在附图中示出,其中自始至终相同或类似的标号表示相同或类似的元件或具有相同或类似功能的元件。下面通过参考附图描述的实施例是示例性的,旨在用于解释本发明,而不能理解为对本发明的限制。
实施例1
实施例1提出了一种(Pb0.90Ba0.05La0.02Dy0.02)(Zr0.68Sn0.27Ti0.05)O3多层电容器,所述的(Pb0.90Ba0.05La0.02Dy0.02)(Zr0.68Sn0.27Ti0.05)O3多层电容器的制备方法包括如下步骤:
(一)(Pb0.90Ba0.05La0.02Dy0.02)(Zr0.68Sn0.27Ti0.05)O3材料的制备
(1)将四氧化三铅,氧化钡,氧化镧,氧化镝,氧化锆,氧化锡和氧化钛按照摩尔比0.90:0.05:0.02:0.02:0.68:0.27:0.05混合,得到混合物,然后将所述混合物放入球磨罐中,再根据混合物、氧化锆球和酒精的质量比为1:1.5:1加入酒精和氧化锆球,以500转/分转速球磨2h使其均匀混合,然后将其放入干燥箱中以80℃下保温4h烘干,其中,所述氧化锆球的直径为2mm。
(2)将步骤(1)得到的产物置于坩埚内,然后将坩埚放入马弗炉,在910℃下保温4h预烧结。
(3)将步骤(2)得到的产物放入球磨罐中,根据步骤(2)得到的产物、氧化锆球和酒精的质量比为1:1.5:1加入酒精和氧化锆球,以500转/分转速球磨2h使其充分研磨,然后将将其放入干燥箱中,在80℃温度下保温3h烘干,得到(Pb0.90Ba0.05La0.02Dy0.02)(Zr0.68Sn0.27Ti0.05)O3粉体。
(二)(Pb0.90Ba0.05La0.02Dy0.02)(Zr0.68Sn0.27Ti0.05)O3厚膜的制备
(1)将重量份数为63份的(Pb0.90Ba0.05La0.02Dy0.02)(Zr0.68Sn0.27Ti0.05)O3粉体与重量份数为40份的甲苯-乙醇溶剂和重量份数为0.5份的磷酸三丁酯在500转/分转速下辊磨12h,得到第一浆料,其中,甲苯-乙醇溶剂中,甲苯与乙醇的体积比为3:0.8。
(2)向第一浆料中加入重量份数为2份的塑性剂聚乙二醇、重量份数为1.5份的邻苯二甲酸丁酯重量份数为3份的粘结剂PVB和重量份数为0.8的均质剂环乙酮,然后在500转/分转速下球磨6h,得到第二浆料,再利用冷等静压设备在100MPa压强下,保压35min。
(3)通过真空除泡法除去所述第二浆料中的气泡,然后通过流延机以30cm/min的流延速率进行流延,得到厚度为40μm的流延膜生带,烘干后得到(Pb0.90Ba0.05La0.02Dy0.02)(Zr0.68Sn0.27Ti0.05)O3厚膜生带,其中,烘干的温度为80℃,烘干的时间为6h。
(三)(Pb0.90Ba0.05La0.02Dy0.02)(Zr0.68Sn0.27Ti0.05)O3多层电容器的制备
(1)将干燥好的流延膜生带,通过切片机在80℃温度下均匀切成面积为2.25cm2的膜片,然后通过丝网印刷法在切好的膜片上印刷面积为0.225cm2的Pd-Ag电极,取10片膜片叠片后在模具中热压得到10层多层膜。
(2)将多层膜放入管式炉中,加热至500℃后保温6h进行排胶处理,然后在1000℃烧结温度下保温2h得到(Pb0.90Ba0.05La0.02Dy0.02)(Zr0.68Sn0.27Ti0.05)O3多层电容器。
实施例2
实施例2提出了一种(Pb0.88Ba0.05La0.02Dy0.04)(Zr0.68Sn0.27Ti0.05)O3多层电容器,所述的(Pb0.88Ba0.05La0.02Dy0.04)(Zr0.68Sn0.27Ti0.05)O3多层电容器的制备方法包括如下步骤:
(一)(Pb0.88Ba0.05La0.02Dy0.04)(Zr0.68Sn0.27Ti0.05)O3材料的制备
(1)将四氧化三铅,氧化钡,氧化镧,氧化镝,氧化锆,氧化锡和氧化钛粉按照摩尔比0.88:0.05:0.02:0.04:0.68:0.27:0.05混合,得到混合物,然后将所述混合物放入球磨罐中,再根据混合物、锆球和酒精的质量比1:1.5:1加入酒精和氧化锆球,以200转/分转速球磨6h使其均匀混合,然后将其放入干燥箱中以80℃下保温4h下烘干,其中,所述氧化锆球的直径为10mm。
(2)将步骤(1)得到的产物置于坩埚内,然后将坩埚放入马弗炉,在1200℃下保温2h预烧结。
(3)将步骤(2)得到的产物放入球磨罐中,根据步骤(2)得到的产物、氧化锆球和酒精的质量比为1:1.5:1加入酒精和氧化锆球以200转/分转速球磨4h使其充分研磨,然后将将其放入干燥箱中,在100℃温度下保温6h烘干,得到(Pb0.88Ba0.05La0.02Dy0.04)(Zr0.68Sn0.27Ti0.05)O3粉体。
(二)(Pb0.88Ba0.05La0.02Dy0.04)(Zr0.68Sn0.27Ti0.05)O3厚膜的制备
(1)将重量份数为65份的(Pb0.88Ba0.05La0.02Dy0.04)(Zr0.68Sn0.27Ti0.05)O3粉体与重量份数为35份的甲苯-乙醇溶剂和重量份数为1份的磷酸三丁酯在500转/分转速下辊磨24h,得到第一浆料,其中,甲苯-乙醇溶剂中,甲苯与乙醇的体积比为1:0.4。
(2)向第一浆料中加入重量份数为1.5份的塑性剂聚乙二醇、重量份数为2份的邻苯二甲酸丁酯重量份数为4份的粘结剂PVB和重量份数为0.3的均质剂环乙酮,然后在200转/分转速下球磨12h,得到第二浆料,再利用冷等静压设备在200MPa压强下,保压25min。
(3)通过真空除泡法除去所述第二浆料中的气泡,然后通过流延机以40cm/min的流延速率进行流延,得到厚度为60μm的流延膜生带,烘干后得到(Pb0.88Ba0.05La0.02Dy0.04)(Zr0.68Sn0.27Ti0.05)O3厚膜生带,其中,烘干的温度为100℃,烘干的时间为3h。
(三)(Pb0.88Ba0.05La0.02Dy0.04)(Zr0.68Sn0.27Ti0.05)O3多层电容器的制备
(1)将干燥好的流延膜生带,通过切片机在100℃温度下均匀切成面积为2.25cm2的膜片,然后通过丝网印刷法在切好的膜片上印刷面积为0.225cm2的Pd-Ag电极,取10片膜片叠片后在模具中热压得到10层多层膜。
(2)将多层膜放入管式炉中,加热至600℃后保温5h进行排胶处理,然后在800℃烧结温度下保温3h得到(Pb0.88Ba0.05La0.02Dy0.04)(Zr0.68Sn0.27Ti0.05)O3多层电容器。
实施例3
实施例3提出了(Pb0.86Ba0.05La0.02Dy0.06)(Zr0.68Sn0.27Ti0.05)O3多层电容器,所述的(Pb0.86Ba0.05La0.02Dy0.06)(Zr0.68Sn0.27Ti0.05)O3多层电容器的制备方法包括如下步骤:
(一)(Pb0.86Ba0.05La0.02Dy0.06)(Zr0.68Sn0.27Ti0.05)O3材料的制备
(1)将四氧化三铅,氧化钡,氧化镧,氧化镝,氧化锆,氧化锡和氧化钛粉按照摩尔比0.86:0.05:0.02:0.06:0.68:0.27:0.05混合,得到混合物,然后将所述混合物放入球磨罐中,再根据混合物、锆球和酒精的质量比1:1.5:1加入酒精和氧化锆球,以300转/分转速球磨2h使其均匀混合,然后将其放入干燥箱中以90℃下保温4h下烘干,其中,所述氧化锆球的直径为6mm。
(2)将步骤(1)得到的产物置于坩埚内,然后将坩埚放入马弗炉,在1200℃,保温2h预烧结。
(3)将步骤(2)得到的产物放入球磨罐中,根据步骤(2)得到的产物、氧化锆球和酒精的质量比为1:1.5:1加入酒精和氧化锆球以300转/分转速球磨4h使其充分研磨,然后将将其放入干燥箱中,在100℃温度下保温6h烘干,得到(Pb0.86Ba0.05La0.02Dy0.06)(Zr0.68Sn0.27Ti0.05)O3粉体。
(二)(Pb0.86Ba0.05La0.02Dy0.06)(Zr0.68Sn0.27Ti0.05)O3厚膜的制备
(1)将重量份数为64.2份的(Pb0.86Ba0.05La0.02Dy0.06)(Zr0.68Sn0.27Ti0.05)O3粉体与重量份数为37.67份的甲苯-乙醇溶剂和重量份数为0.8份的磷酸三丁酯在300转/分,18h的转速下辊磨得到第一浆料,其中,甲苯-乙醇溶剂中,甲苯与乙醇的体积比为28:9.67。
(2)向第一浆料中加入重量份数为1.6份的塑性剂聚乙二醇、重量份数为1.6份的邻苯二甲酸丁酯重量份数为3.3份的粘结剂PVB和重量份数为0.5的均质剂环乙酮,然后在300转/分转速下球磨9h,得到第二浆料,再利用冷等静压设备在150MPa压强下,保压30min。
(3)通过真空除泡法除去所述第二浆料中的气泡,然后通过流延机以35cm/min的流延速率进行流延,得到厚度为80μm的流延膜生带,烘干后得到(Pb0.86Ba0.05La0.02Dy0.06)(Zr0.68Sn0.27Ti0.05)O3厚膜生带,其中,烘干的温度为90℃,烘干的时间为4h。
(三)(Pb0.86Ba0.05La0.02Dy0.06)(Zr0.68Sn0.27Ti0.05)O3多层电容器的制备
(1)将干燥好的流延膜生带,通过切片机在90℃温度下均匀切成面积为2.25cm2的膜片,然后通过丝网印刷法在切好的膜片上印刷面积为0.225cm2的Pd-Ag电极,取10片膜片叠片后在模具中热压得到10层多层膜。
(2)将多层膜放入管式炉中,加热至550℃后保温5.5h进行排胶处理,然后在900℃烧结温度下保温1h得到(Pb0.86Ba0.05La0.02Dy0.06)(Zr0.68Sn0.27Ti0.05)O3多层电容器。
对比例
对比例提出了一种(Pb0.92Ba0.05La0.02)(Zr0.68Sn0.27Ti0.05)O3多层电容器,所述的锆酸铅基反铁电多层电容器的制备方法包括如下步骤:
(一)(Pb0.92Ba0.05La0.02)(Zr0.68Sn0.27Ti0.05)O3材料的制备
(1)将四氧化三铅,氧化钡,氧化镧,氧化镝,氧化锆,氧化锡,和氧化钛粉按照摩尔比0.92:0.05:0.02:0.68:0.27:0.05混合,得到混合物,然后将所述混合物放入球磨罐中,再根据混合物、锆球和酒精的质量比1:1.5:1加入酒精和氧化锆球,以300转/分的转速球磨2h使其均匀混合后烘干,烘干的温度为90℃,烘干的时间为4h;其中,所述氧化锆球的直径为6mm。
(2)将步骤(1)的产物置于坩埚内,然后将坩埚放入马弗炉,加热至1200℃,保温2h预烧结。
(3)把步骤(2)的产物放入球磨罐中,根据步骤(2)得到的产物、氧化锆球和酒精的质量比为1:1.5:1加入酒精和氧化锆球以300转/分转速球磨18h使其充分研磨,然后在100℃温度下保温6h烘干,得到(Pb0.92Ba0.05La0.02)(Zr0.68Sn0.27Ti0.05)O3粉体。
(二)(Pb0.92Ba0.05La0.02)(Zr0.68Sn0.27Ti0.05)O3厚膜的制备
(1)将重量份数为64.2份的(Pb0.92Ba0.05La0.02)(Zr0.68Sn0.27Ti0.05)O3粉体与重量份数为37.67份的甲苯-乙醇溶剂和重量份数为0.8份的磷酸三丁酯在200转/分,12h的转速下辊磨得到第一浆料,其中,甲苯-乙醇溶剂中,甲苯与乙醇的体积比为28:9.67。
(2)向第一浆料中加入重量份数为1.6份的塑性剂聚乙二醇,重量份数为1.6份的邻苯二甲酸丁酯,重量份数为3.3份的粘结剂PVB,重量份数为0.5份的均质剂环乙酮,然后在300转/分转速下辊磨6h,得到第二浆料。
(3)通过真空除泡法除去所述第二浆料中的气泡,然后通过流延机以35cm/min的流延速率进行流延,烘干后得到(Pb0.92Ba0.05La0.02)(Zr0.68Sn0.27Ti0.05)O3厚膜生带,其中,烘干的温度为80℃,烘干的时间为6h。
(三)(Pb0.92Ba0.05La0.02)(Zr0.68Sn0.27Ti0.05)O3多层电容器的制备
(1)将干燥好的流延膜生带,通过切片机在90℃温度下均匀切成面积为2.25cm2的膜片,然后通过丝网印刷法在切好的膜片上印刷面积为0.225cm2的Pd-Ag电极,取10片膜片叠片后在模具中热压得到10层多层膜。
(2)将多层膜放入管式炉中,加热至550℃后保温5.5h进行排胶处理,在900℃烧结温度下保温2h得到(Pb0.92Ba0.05La0.02)(Zr0.68Sn0.27Ti0.05)O3多层电容器。
对上述四种铅基反铁电薄膜进行分析:
参照图1,即对比例、实施例1、实施例2、实施例3的工艺制得的四个组分反铁电多层电容器介电层的XRD图谱,从图中可以看出,对比例、实施例1、实施例2、实施例3反铁电薄膜均形成了单一的钙钛矿相结构,除衬底峰外,并且没有其他杂峰,表明Dy的加入,对PZ基结构未产生明显影响。
参照图2,即对比例、实施例1、实施例2、实施例3的工艺制得的四个组分反铁电多层电容器介电层在300kV/cm下的P-E图谱。从此图中可以看出各个组分的电滞回线均表现出典型的反铁电特性,随Dy含量的增加饱和极化强度是降低的,而相转变电场是增加的。可以说明,添加Dy能够对铅反铁电多层电容器的储能行为产生积极的影响,有利于提高储能密度和储能效率。
参照图3,明显的发现对比例、实施例1、实施例2、实施例3制得的四个组分反铁电到铁电的转变电场以及电滞宽度随Dy含量变化的图谱,由图可知随Dy含量的增加反铁电到铁电的转变电场(EAFE-FE)逐渐增加,电滞宽度逐渐降低,有利于提高储能密度和储能效率。
参照图4明显的发现对比例、实施例1、实施例2、实施例3制得的四个组分反铁电厚膜多层电容器储能密度和储能效率随着Dy含量变化图谱,由图可知随Dy含量的增加储能密度升高当x=0.04时,储能密度达到最大。随Dy含量的增加储能效率增大。
综上,本发明实施例的锆酸铅基反铁电多层电容器,通过在锆酸铅基反铁电材料中掺杂Dy,提高了锆酸铅基反铁电材料的储能密度,提高了储能效率。用掺杂了Dy的锆酸铅基反铁电材料制备的电容器,在外加电场的作用下,会随Dy含量的增加反铁电相越稳定,能够获得较大的反铁电到铁电转变电场(EAFE-FE),EAFE-FE与铁电到反铁电转变电场(EFE-AFE)的差值ΔE逐渐降低,提高了多层电容器的储能密度和储能效率。
在本说明书的描述中,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征。在本发明的描述中,“多个”的含义是两个以上,除非另有明确具体的限定。
在本说明书的描述中,参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不必须针对的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任一个或多个实施例或示例中以合适的方式结合。此外,在不相互矛盾的情况下,本领域的技术人员可以将本说明书中描述的不同实施例或示例以及不同实施例或示例的特征进行结合和组合。
尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。
Claims (10)
1.一种锆酸铅基反铁电材料,其特征在于,所述锆酸铅基反铁电材料的化学通式为(Pb0.92-xBa0.05La0.02Dyx)(Zr0.68Sn0.27Ti0.05)O3;其中,x的取值范围为:0<x≤0.06。
2.权利要求1所述的锆酸铅基反铁电材料的制备方法,其特征在于,包括如下步骤:
S101:将四氧化三铅、氧化钡、氧化镧、氧化镝、氧化锆、氧化锡和氧化钛按照元素铅、钡、镧、锆、锡、钛的摩尔比(0.92-x):0.05:0.02:x:0.68:0.27:0.05混合,得到混合物,然后将所述混合物放入球磨罐中,再加入酒精和氧化锆球球磨2h~6h后烘干;
S102:将所述步骤S101得到的产物加热至910℃~1100℃并保温2h~6h;
S103:将所述步骤S102得到的产物放入球磨罐中,再加入酒精和氧化锆球球磨3h~6h后烘干,得到锆酸铅基反铁电材料。
3.根据权利要求2所述的锆酸铅基反铁电材料的制备方法,其特征在于,在所述步骤S101中,烘干的温度为80℃~100℃,烘干的时间为3h~6h;在所述步骤S103中,烘干的温度为80℃~100℃,烘干的时间为3h~6h;
在所述步骤S101中,所述混合物与所述酒精和所述氧化锆球的质量比为1:1.5:1;在所述步骤S103中,所述步骤S102得到的产物与所述酒精和所述氧化锆球的质量比为1:1.5:1;
所述氧化锆球的直径为2mm~10mm。
4.一种锆酸铅基反铁电厚膜的制备方法,其特征在于,包括如下步骤:
S201:将权利要求1所述的锆酸铅基反铁电材料与甲苯-乙醇溶剂和磷酸三丁酯混合后球磨,得到第一浆料;其中,所述锆酸铅基反铁电材料的重量份数为63份~65份,所述甲苯-乙醇溶剂的重量份数为35份~40份,所述磷酸三丁酯的重量份数为0.5份~1份;
S202:向所述第一浆料中加入聚乙二醇、邻苯二甲酸丁酯、PVB、环乙酮,然后球磨得到第二浆料;其中,所述聚乙二醇的重量份数为1.5份~2份,所述邻苯二甲酸丁酯的重量份数为1.5份~2份,所述PVB的重量份数为3份~4份,所述环乙酮的重量份数为0.3份~0.8份,所述甲苯-乙醇溶剂中,甲苯与乙醇的体积比为3:(0.8~1.2);
S203:通过真空除泡法除去所述第二浆料中的气泡,然后通过流延机流延,得到厚度为20μm~80μm的流延膜生带,然后干燥,得到锆酸铅基反铁电厚膜。
5.根据权利要求4所述的锆酸铅基反铁电厚膜的制备方法,其特征在于,在所述步骤S202后,所述步骤S203前,还包括如下步骤:利用冷等静压设备在100MPa~200MPa压强下,保压25min~35min。
6.权利要求4或5所述的方法制备得到的锆酸铅基反铁电厚膜。
7.一种锆酸铅基反铁电多层电容器的制备方法,其特征在于,包括如下步骤:
S301:通过切片机将权利要求6所述的锆酸铅基反铁电厚膜切片,然后通过丝网印刷法在所述切片上印刷电极,再将多层所述印刷有电极的切片重叠后热压,得到多层膜;
S302:将所述多层膜在500℃~600℃温度下保温5h~6h,然后在800℃~1000℃温度下保温1h~3h,得到锆酸铅基反铁电多层电容器。
8.根据权利要求7所述的锆酸铅基反铁电多层电容器的制备方法,其特征在于,在所述步骤S301中,所述切片的面积为2.25cm2,所述电极的面积为0.225cm2。
9.根据权利要求7所述的锆酸铅基反铁电多层电容器的制备方法,其特征在于,在所述步骤S301中,多层所述印刷有电极的切片为10层。
10.根据权利要求7-9任一项所述的方法制备得到的锆酸铅基反铁电多层电容器。
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