CN107056291A - 一种亚微米晶尺度压电能量收集材料及其制备方法 - Google Patents
一种亚微米晶尺度压电能量收集材料及其制备方法 Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 7
- 238000002360 preparation method Methods 0.000 title abstract description 7
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 15
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 9
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 claims abstract description 9
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Abstract
一种亚微米晶尺度压电能量收集材料及其制备方法，属于压电陶瓷材料领域。该陶瓷材料的基体化学组成为0.2Pb(Zn1/3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3，晶粒尺寸在亚微米级。以Pb3O4、ZnO、Nb2O5、ZrO2和TiO2为原料，采用湿磨、烘干、高能球磨、压制成型、烧结步骤。本发明应用于压电能量收集器件，可以在实现器件小型化的同时，有效地回收再利用环境中废弃的振动能，具有显著的经济和社会价值。
Description
技术领域
本发明属于压电陶瓷材料领域，具体涉及一种可应用于小型化压电能量收集器件的具有亚微米晶粒尺寸、高压电应变常数和低介电常数的压电陶瓷材料及其制备方法。
背景技术
近年来，随着能源问题的日益严重，如何将环境中废弃的振动能回收再利用成为各国研究的重点。将振动能转化为可以使用的电能无疑是最好的选择，压电能量收集器件基于压电材料的正压电效应可以实现这一功能。
为了满足压电能量收集器件的要求，压电陶瓷必须具有高的能量密度:
能量密度u可用如下公式表示：
d：压电应变常数 g：压电电场常数
F：作用力 A：面积
通过公式可以看出，高的能量密度主要由大的换能系数(d×g)来决定。又因为g＝d/(ε0×εr)，所以具有高的换能系数(d×g)的材料可以通过高的压电应变常数d和低的介电常数εr获得。
此外，压电能量收集器件的微型化发展趋势需要其核心压电陶瓷材料在保持高换能系数的同时，还应具有亚微米尺度的晶粒结构，以便实现器件的轻薄化。但是，前人的研究工作发现，许多压电陶瓷的晶粒尺寸由微米级减小到亚微米级时，材料压电应变常数的下降幅度远大于介电常数的下降幅度，不利于获得高的换能系数。
综上所述，为了满足压电能量收集器件微型化的要求，在本专利中，以PZN-PZT为目标体系，通过高能球磨法免煅烧制备纳米级前驱粉体并进行致密化烧结工艺调控，在获得亚微米晶粒尺寸实现微型化的同时，陶瓷材料具有高的换能系数。设计并制备这一关键亚微米晶材料对于推进压电能量收集器件的微型化及相关小型高效电源制造具有重大的意义。
发明内容
本发明的目的在于提供一种可应用于微型压电能量收集器件的压电陶瓷材料及其制备方法，在降低晶粒尺寸实现微型化的同时，陶瓷材料具有高的换能系数。
本发明的压电陶瓷特征在于具有亚微米尺度的晶粒尺寸和高的换能系数。
为实现上述目的，本发明采取以下技术方案。
本发明提供一种应用于微型压电能量收集器件的压电陶瓷材料，其特征在于，晶粒尺寸在亚微米级，基体化学组成为：0.2Pb(Zn1/3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3。进一步优选晶粒尺寸为0.33μm。
本发明上述具有亚微米晶粒尺寸的压电能量收集材料的制备方法，其特征在于，选择高能球磨法免煅烧制备纳米尺度的PZN-PZT前驱粉体，并通过优化烧结工艺制备得到亚微米晶粒尺度的高换能系数压电陶瓷，具体包括以下步骤：
(1)将Pb3O4、ZnO、Nb2O5、ZrO2和TiO2按化学摩尔计量比称量，将称量好的原料放入球磨罐中，以无水乙醇为介质置于行星球磨机中球磨12h，然后100℃条件下烘干；
(2)将干燥后的粉体采用直径为3mm的碳化钨磨球，球料比20:1，进行高能球磨90min；
(3)不需要添加粘结剂，将粉体直接在800MPa的压力下成型，然后在850-1050℃烧结，保温120min，即得到目标陶瓷材料。
烧结后的陶瓷片，经过抛光处理之后进行微结构观测，然后被上银电极，在120℃的硅油中，于30kV·cm-1的直流高压下极化30min。然后对样品进行电性能的测试。
其中，最佳样品为：通过高能球磨90min得到的纳米级前驱粉体，在烧结温度为950℃、保温120min时得到的0.2Pb(Zn1/3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3陶瓷，其晶粒尺寸为0.33μm,性能可达到：d33＝315pC/N，εr＝1405，d33×g33＝7980×10-15m2/N，可以满足微型压电能量收集器件的要求。
在本发明中，选择高能球磨法得到的纳米尺度的粉体作为PZN-PZT前驱粉体，制备得到亚微米尺度的PZN-PZT陶瓷。
与现有技术相比较，本发明具有以下优点：
本发明提出的方法可用于构建满足微型化压电能量收集器件要求的具有高换能系数的亚微米晶压电陶瓷。现有常规技术采用普通高温煅烧工艺合成前驱粉体，制备出的粉体不仅由于高温下PbO等物质的挥发造成环境污染与材料计量比失配，而且合成产物粉体颗粒粗大，无法进一步用于烧结制备亚微米晶压电陶瓷。本发明技术上通过高能球磨法免煅烧制备得到纳米级前驱粉体，结合烧结工艺优化，从而实现了将陶瓷的晶粒尺寸从微米级降低到亚微米级(0.33μm)，在满足能量收集器件微型化的同时，也具有高的换能系数(d33×g33)。
附图说明
图1为混合粉末在机械化学处理90min后的微观结构细节，(a)纳米粉末TEM形貌图，(b)HRTEM图，(c)选区电子衍射(SAED)图和(d)EDS能谱；
图2为本发明成分在(a)850℃，(b)900℃，(c)950℃，(d)1000℃，(e)1050℃下烧结2h的XRD图谱；
图3为本发明成分在(a)850℃，(b)900℃，(c)950℃，(d)1000℃，(e)1050℃下烧结2h的PZN-PZT样品抛光和热蚀后的断面SEM照片及(f)陶瓷的相对密度随烧结温度的变化曲线。
具体实施方式
以下将通过实施例对本发明进行详细描述，这些实施例只是出于示例性说明的目的，而非用于限定本发明。
本发明提供一种具有亚微米尺寸可应用于微型压电能量收集器件的压电陶瓷材料，其特征在于，该陶瓷材料具有亚微米尺度的晶粒尺寸，其化学组成通式为：0.2Pb(Zn1/ 3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3。组成原料为：Pb3O4、ZnO、Nb2O5、ZrO2和TiO2。具体制备方法为，首先，将称量好的原料放入球磨罐中，以无水乙醇为介质置于行星球磨机中球磨12h。球磨后所得浆料在100℃下烘干，然后将干燥后的粉体采用直径为3mm的碳化钨磨球，球料比20:1，高能球磨90min；将得到的粉体不需要添加粘结剂，直接在800MPa的压力下成型，然后在850-1050℃烧结，保温2h，得到陶瓷材料。烧结后的陶瓷片，印刷并烧渗银电极，在120℃的硅油中，在30kV·cm-1的电压下极化30min。然后对样品进行电性能的测试。本发明通过测定的压电常数d33和介电常数εr，经过简单计算就可以得出机电转换系数d33×g33。
下面通过实施例进一步阐明本发明的实质性特点和显著优点。应该指出,本发明决非仅局限于所陈述的实施例。
实施例1：
按化学式0.2Pb(Zn1/3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3称量Pb3O4、ZnO、Nb2O5、ZrO2和TiO2，并在乙醇中球磨12h。混合物经烘干后，干燥后的粉体采用高能球磨90min，将高能球磨得到的粉体直接在800MPa下压制成型，并在850℃下烧结2h得到陶瓷。
实施例2：
按化学式0.2Pb(Zn1/3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3称量Pb3O4、ZnO、Nb2O5、ZrO2和TiO2，烧结温度为900℃。其它同实施例1。
实施例3：
按化学式0.2Pb(Zn1/3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3称量Pb3O4、ZnO、Nb2O5、ZrO2和TiO2，烧结温度为950℃。其它同实施例1。
实施例4：
按化学式0.2Pb(Zn1/3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3称量Pb3O4、ZnO、Nb2O5、ZrO2和TiO2，烧结温度为1000℃。其它同实施例1。
实施例5：
按化学式0.2Pb(Zn1/3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3称量Pb3O4、ZnO、Nb2O5、ZrO2和TiO2，烧结温度为1050℃。其它同实施例1。
表1上述实施例性能对比表
Claims (4)
1.一种应用于小型化压电能量收集器件的亚微米晶压电陶瓷材料，其特征在于，压电陶瓷材料的化学组成为：0.2Pb(Zn1/3Nb2/3)O3–0.8Pb(Zr1/2Ti1/2)O3，晶粒尺寸在亚微米级。
2.按照权利要求1所述的一种应用于小型化压电能量收集器件的亚微米压电陶瓷材料，其特征在于，晶粒尺寸为0.33μm。
3.制备权利要求1所述的压电陶瓷材料的方法，其特征在于，通过采用高能球磨法得到的纳米级前驱粉体，通过普通烧结工艺制备得到亚微米晶粒尺度的压电陶瓷，具体包括以下步骤：
(1)将Pb3O4、ZnO、Nb2O5、ZrO2和TiO2按化学摩尔计量比称量，将称量好的原料放入球磨罐中，以无水乙醇为介质置于行星球磨机中球磨12h，然后100℃条件下烘干；
(2)将干燥后的粉体采用直径为3mm的碳化钨磨球，球料比20:1，进行高能球磨90min；
(3)不需要添加粘结剂，将粉体直接在800MPa的压力下成型，然后在850-1050℃烧结，保温120min，即得到目标陶瓷材料。
4.按照权利要求1或2所述的压电陶瓷材料用于小型化压电能量收集器件。
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