CN110452481A - 一种综合性能优异的0-3型压电复合薄膜 - Google Patents
一种综合性能优异的0-3型压电复合薄膜 Download PDFInfo
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Abstract
本发明涉及0‑3型压电复合薄膜制备技术领域，且公开了一种综合性能优异的0‑3型压电复合薄膜，包括以下重量份数配比的原料：40～50份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒、40～50份的平均粒径38um的聚偏氟乙烯(PVDF)粉、1～2份的平均粒径6.5um的微米铜(Cu)粉、8～9份微米级的聚乙烯醇(PVA1799)粉或/和乙酸纤维素粉；其制备包括：先通过球磨混合的方法使上述原料混合均匀，再将分散均匀的复合体系在温度为200℃、压力为150MPa的钢制模具中保持热压，得到0‑3型压电复合材料薄膜。本发明解决了目前现有的0‑3型压电复合薄膜，由于其主要基体PVDF的成膜性能很差，不适合制备大面积薄膜器件，难以制备得到综合性能优异的大面积0‑3型压电复合薄膜的技术问题。
Description
技术领域
本发明涉及0-3型压电复合薄膜制备技术领域，具体为一种综合性能优异的0-3型压电复合薄膜。
背景技术
压电材料是实现机械能(包括声能)与电能之间转换的重要功能材料，其特别是在信息的检测、转换、处理和储存等传感器领域占有非常重要的地位。压电复合材料是将压电陶瓷和其他基体材料按一定的连通方式复合而成的一类新型压电功能材料，其中，0-3型压电复合材料表示压电陶瓷颗粒(0维)均匀分布在3维连通的聚合物中形成的复合体系。而0-3型压电复合材料以成型加工容易(只需将压电陶瓷粉末和聚合物混合在一起，通过聚合物加工方法就可以得到成品)、柔韧性好、容易制得大面积传感器、综合压电性能好等优点而倍受青睐。
要得到综合性能优异的0-3型压电复合材料，关键是复合材料的极化。诸多错综复杂的影响因素制约着压电复合材料的充分极化。因此，在设计和制备压电复合材料时总是遇到很多矛盾和困难。其中较为突出的问题是：难以制得综合性能很好的大面积压电薄膜。目前电学综合性能最好的压电复合材料一般是通过热压工艺制备，而热压方法制备的压电薄膜面积受到限制，而且不适合复合材料的现场制备(如结构器件的安全监控传感器等)。0-3型压电复合材料的主要基体PVDF的成膜性能很差，不适合制备大面积薄膜器件。用流延法和轧膜法可以得到面积稍大的压电薄膜材料，但同样不适合有些构件的现场实施。选用其它聚合物，用喷涂或涂覆的方法有望解决大面积压电薄膜制备的问题。但这类复合材料的致密度较低，而且聚合物本身的介电常数不及PVDF及其共聚物，复合材料的极化更加困难。因此，要制得综合性能很好的大面积压电薄膜仍然很困难。
发明内容
(一)解决的技术问题
针对现有技术的不足，本发明提供了一种综合性能优异的0-3型压电复合薄膜，解决了目前现有的0-3型压电复合薄膜，由于其主要基体PVDF的成膜性能很差，不适合制备大面积薄膜器件，难以制备得到综合性能优异的大面积0-3型压电复合薄膜的技术问题。
(二)技术方案
为实现上述目的，本发明提供如下技术方案：
一种综合性能优异的0-3型压电复合薄膜，包括以下重量份数配比的原料：40～50份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒、40～50份的平均粒径38um的聚偏氟乙烯(PVDF)粉、1～2份的平均粒径6.5um的微米铜(Cu)粉、8～9份微米级的聚乙烯醇(PVA1799)粉或/和乙酸纤维素粉；
上述0-3型压电复合薄膜的制备方法包括以下步骤：先通过球磨混合的方法使上述原料混合均匀，再将分散均匀的复合体系在温度为200℃、压力为150MPa的钢制模具中保持热压，得到0-3型压电复合材料薄膜。
优选的，所述聚乙烯醇(PVA1799)粉的平均粒径为10um。
优选的，所述乙酸纤维素粉的平均粒径为10um。
优选的，所述0-3型压电复合薄膜还包括以下重量份数配比的原料：1份的平均粒径6.5um的石墨粉。
(三)有益的技术效果
与现有技术相比，本发明具备以下有益的技术效果：
本发明通过将成膜性能极好的聚乙烯醇(PVA1799)粉或/和乙酸纤维素粉、电学性能极优异的微米铜(Cu)粉或/和石墨粉，与基体材料聚偏氟乙烯(PVDF)粉、功能增强相锆钛酸铅(PZT)陶瓷颗粒进行复合，得到压电常数d33为42～46pC/N、介电损耗tanδ为0.016～0.018、介电常数εr为205～211、电导率σ为10-5S/m的综合性能优异、且适合制备大面积薄膜器件的0-3型压电复合薄膜。
具体实施方式
以下实施例与对比例中所使用的原料如下：
锆钛酸铅(Pb(Ti0.48Zr0.52)O3，PZT)陶瓷颗粒，平均粒径3um，压电系数>400pC/N、介电常数>1600、介电损耗<0.005、电导率10-7S/m；
聚偏氟乙烯(PVDF)粉、平均粒径38um；
微米铜(Cu)粉，平均粒径6.5um；
石墨粉，平均粒径6.5um；
聚乙烯醇(PVA1799)粉，平均粒径10um；
乙酸纤维素粉，平均粒径10um。
实施例一：
0-3型压电复合薄膜包括以下重量份数配比的原料：45份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒、45份的平均粒径38um的聚偏氟乙烯(PVDF)粉、1.5份的平均粒径6.5um的微米铜(Cu)粉、8.5份的平均粒径10um的聚乙烯醇(PVA1799)粉；
上述0-3型压电复合薄膜的制备方法包括以下步骤：
步骤一：将45份的平均粒径38um的聚偏氟乙烯(PVDF)粉、8.5份的平均粒径10um的聚乙烯醇(PVA1799)粉与100mL无水乙醇一起放置在不锈钢球磨容器内，并置于球磨仪上进行球磨，调整球磨转速为300r/min，每球磨30min间歇5min，球磨时间为2h，得到一次球磨产物；
步骤二：将1.5份的平均粒径6.5um的微米铜(Cu)粉加入到一次球磨产物中，调整球磨转速为400r/min，球磨时间为2h，每球磨30min间歇10min，得到二次球磨产物；
步骤三：将45份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒加入到二次球磨产物中，调整球磨转速为500r/min，球磨时间为4h，每球磨30min间歇20min，得到三次球磨产物；
步骤四：将三次球磨产物放置在温度80℃的烘箱内进行干燥，直至复合体系内不含有无水乙醇为止，得到分散均匀的复合体系；
步骤五：将分散均匀的复合体系在温度为200℃、压力为150MPa的钢制模具中保持热压4h，温度降至室温时脱模，得到φ12mm、厚200～300um的0-3型压电复合材料薄膜。
实施例二：
0-3型压电复合薄膜包括以下重量份数配比的原料：50份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒、40份的平均粒径38um的聚偏氟乙烯(PVDF)粉、1份的平均粒径6.5um的微米铜(Cu)粉、6份的平均粒径10um的聚乙烯醇(PVA1799)粉、3份的平均粒径10um的乙酸纤维素粉；
上述0-3型压电复合薄膜的制备方法包括以下步骤：
步骤一：将40份的平均粒径38um的聚偏氟乙烯(PVDF)粉、6份的平均粒径10um的聚乙烯醇(PVA1799)粉与100mL无水乙醇一起放置在不锈钢球磨容器内，并置于球磨仪上进行球磨，调整球磨转速为300r/min，每球磨30min间歇5min，球磨时间为2h；
将3份的平均粒径10um的乙酸纤维素粉加入到上述球磨产物中，调整球磨转速为350r/min，每球磨30min间歇5min，球磨时间为2h，得到一次球磨产物；
步骤二：将1份的平均粒径6.5um的微米铜(Cu)粉加入到一次球磨产物中，调整球磨转速为400r/min，球磨时间为2h，每球磨30min间歇10min，得到二次球磨产物；
步骤三：将50份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒加入到二次球磨产物中，调整球磨转速为500r/min，球磨时间为4h，每球磨30min间歇20min，得到三次球磨产物；
步骤四：将三次球磨产物放置在温度80℃的烘箱内进行干燥，直至复合体系内不含有无水乙醇为止，得到分散均匀的复合体系；
步骤五：将分散均匀的复合体系在温度为200℃、压力为150MPa的钢制模具中保持热压4h，温度降至室温时脱模，得到φ12mm、厚200～300um的0-3型压电复合材料薄膜。
实施例三：
0-3型压电复合薄膜包括以下重量份数配比的原料：40份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒、50份的平均粒径38um的聚偏氟乙烯(PVDF)粉、2份的平均粒径6.5um的微米铜(Cu)粉、8份的平均粒径10um的乙酸纤维素粉；
上述0-3型压电复合薄膜的制备方法包括以下步骤：
步骤一：将50份的平均粒径38um的聚偏氟乙烯(PVDF)粉、8份的平均粒径10um的乙酸纤维素粉与100mL无水乙醇一起放置在不锈钢球磨容器内，并置于球磨仪上进行球磨，调整球磨转速为300r/min，每球磨30min间歇5min，球磨时间为2h，得到一次球磨产物；
步骤二：将2份的平均粒径6.5um的微米铜(Cu)粉加入到一次球磨产物中，调整球磨转速为400r/min，球磨时间为2h，每球磨30min间歇10min，得到二次球磨产物；
步骤三：将40份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒加入到二次球磨产物中，调整球磨转速为500r/min，球磨时间为4h，每球磨30min间歇20min，得到三次球磨产物；
步骤四：将三次球磨产物放置在温度80℃的烘箱内进行干燥，直至复合体系内不含有无水乙醇为止，得到分散均匀的复合体系；
步骤五：将分散均匀的复合体系在温度为200℃、压力为150MPa的钢制模具中保持热压4h，温度降至室温时脱模，得到φ12mm、厚200～300um的0-3型压电复合材料薄膜。
实施例四：
0-3型压电复合薄膜包括以下重量份数配比的原料：45份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒、45份的平均粒径38um的聚偏氟乙烯(PVDF)粉、1份的平均粒径6.5um的微米铜(Cu)粉、4份的平均粒径10um的聚乙烯醇(PVA1799)粉、4份的平均粒径10um的乙酸纤维素粉、1份的平均粒径6.5um的石墨粉；
上述0-3型压电复合薄膜的制备方法包括以下步骤：
步骤一：将45份的平均粒径38um的聚偏氟乙烯(PVDF)粉、4份的平均粒径10um的聚乙烯醇(PVA1799)粉、4份的平均粒径10um的乙酸纤维素粉与100mL无水乙醇一起放置在不锈钢球磨容器内，并置于球磨仪上进行球磨，调整球磨转速为300r/min，每球磨30min间歇5min，球磨时间为2h，得到一次球磨产物；
步骤二：将1.5份的平均粒径6.5um的微米铜(Cu)粉、1份的平均粒径6.5um的石墨粉加入到一次球磨产物中，调整球磨转速为400r/min，球磨时间为2h，每球磨30min间歇10min，得到二次球磨产物；
步骤三：将45份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒加入到二次球磨产物中，调整球磨转速为500r/min，球磨时间为4h，每球磨30min间歇20min，得到三次球磨产物；
步骤四：将三次球磨产物放置在温度80℃的烘箱内进行干燥，直至复合体系内不含有无水乙醇为止，得到分散均匀的复合体系；
步骤五：将分散均匀的复合体系在温度为200℃、压力为150MPa的钢制模具中保持热压4h，温度降至室温时脱模，得到φ12mm、厚200～300um的0-3型压电复合材料薄膜。
性能测试：
采用精密阻抗分析仪对实施例中的0-3型压电复合材料薄膜进行电容和介电损耗(tanδ)测试，并计算出介电常数εr，采用准静态测量仪测量实施例中的0-3型压电复合材料薄膜的压电常数d33，采用电导率测试仪测量实施例中的0-3型压电复合材料薄膜的电导率σ，测试结果见表1。
表1
Claims (4)
1.一种综合性能优异的0-3型压电复合薄膜，其特征在于，包括以下重量份数配比的原料：40～50份的平均粒径3um的锆钛酸铅(PZT)陶瓷颗粒、40～50份的平均粒径38um的聚偏氟乙烯(PVDF)粉、1～2份的平均粒径6.5um的微米铜(Cu)粉、8～9份微米级的聚乙烯醇(PVA1799)粉或/和乙酸纤维素粉；
上述0-3型压电复合薄膜的制备方法包括以下步骤：先通过球磨混合的方法使上述原料混合均匀，再将分散均匀的复合体系在温度为200℃、压力为150MPa的钢制模具中保持热压，得到0-3型压电复合材料薄膜。
2.根据权利要求1所述的0-3型压电复合薄膜，其特征在于，所述聚乙烯醇(PVA1799)粉的平均粒径为10um。
3.根据权利要求1所述的0-3型压电复合薄膜，其特征在于，所述乙酸纤维素粉的平均粒径为10um。
4.根据权利要求1所述的0-3型压电复合薄膜，其特征在于，所述0-3型压电复合薄膜还包括以下重量份数配比的原料：1份的平均粒径6.5um的石墨粉。
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