CN115612145B - 一种pvdf压电薄膜及其制备方法 - Google Patents
一种pvdf压电薄膜及其制备方法 Download PDFInfo
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- 239000002033 PVDF binder Substances 0.000 title claims abstract description 156
- 229920002981 polyvinylidene fluoride Polymers 0.000 title claims abstract description 156
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000012528 membrane Substances 0.000 claims abstract description 12
- 238000004528 spin coating Methods 0.000 claims abstract description 11
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical class [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 claims description 46
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000003929 acidic solution Substances 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 230000010287 polarization Effects 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 229920000767 polyaniline Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MMCPOSDMTGQNKG-UHFFFAOYSA-N anilinium chloride Chemical compound Cl.NC1=CC=CC=C1 MMCPOSDMTGQNKG-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 2
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229940113088 dimethylacetamide Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920006126 semicrystalline polymer Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
本发明涉及压电材料技术领域,具体公开了一种PVDF压电薄膜的制备方法,包括以下步骤:将PVDF溶于有机溶剂中得到PVDF溶液,将PVDF溶液在玻璃基板上涂膜,烘干,冷却得到PVDF膜片;对PVDF膜片进行单向拉伸,极化,得到极化的PVDF薄膜;将PEDOT:PSS水溶液真空旋转涂覆在的PVDF薄膜上,真空旋转涂覆工艺参数为:第一级转速600~800rpm,运行时间为5~10s,第二级转速为2500~3000rpm,运行时间为6~12s;70~100℃烘干,得到PVDF压电薄膜。本发明的PVDF压电薄膜的制备方法中,在PVDF压电薄膜旋涂一层PEDOT:PSS膜,提高PVDF压电薄膜的压电性能,同时保持PVDF压电薄膜的柔韧性和强度,并且制备工艺简单、操作方便,有利于推动PVDF压电薄膜在柔性压电传感器中应用。
Description
技术领域
本发明属于压电材料技术领域,特别涉及一种PVDF压电薄膜及其制备方法。
背景技术
锆钛酸铅、钛酸钡、氧化锌和聚偏氟乙烯(PVDF)作为压电材料在许多领域中得到了应用,钛酸钡、锆钛酸铅压电陶瓷材料,具有价格低、易合成、压电系数高等优点,但是由于其成型温度较高、不易制得复杂形状、脆性高等不足限制了在快速发展的柔性电子器件领域的应用;而聚偏氟乙烯具有其他压电材料所没有的柔性、机械强度高、生物兼容性、易于加工成型大面积和复杂形状等优点,克服了陶瓷压电材料硬而脆、难于加工等困难,具有广阔的应用前景。
聚偏氟乙烯是一种具有优良压电性能的半晶聚合物,PVDF可以有五种不同的结晶相(α、β、γ、δ和λ相),具有非极性。聚偏氟乙烯优良的压电性能来自于TTTT构象即β相同,其中CH2和CF2基团的分子结构沿聚合物主链相反方向排列。由于分子间立体和静电相互作用的限制,聚合物结晶使多数晶体结构趋向一种低能构型,即α晶相或与其相近的γ晶相。因此一般的工艺条件下易形成α晶相,α晶相没有压电性能,α晶相通过极化可转变为β晶相。由于聚偏氟乙烯(PVDF)的压电系数相对较低,基于PVDF传感器等电子器件的性能仍处于较低水平,制约了其在现代高科技领域的应用范围。因此,如何提高PVDF的压电性能对于推动PVDF传感器的应用具有重要意义。
发明内容
本发明的目的在于PVDF压电薄膜的制备方法,克服PVDF材料压电性能不足的缺陷。
为实现上述目的,本发明提供了一种PVDF压电薄膜的制备方法,包括以下步骤:
(1)将PVDF溶于有机溶剂中得到PVDF溶液,将PVDF溶液在玻璃基板上涂膜,烘干,冷却得到PVDF膜片;
(2)对步骤(1)制得的PVDF膜片进行单向拉伸,极化,得到极化的PVDF薄膜;
(3)将PEDOT:PSS水溶液真空旋转涂覆在步骤(2)得到的PVDF薄膜上,真空旋转涂覆工艺参数为:第一级转速600~800rpm,运行时间为5~10s,第二级转速为2500~3000rpm,运行时间为6~12s;70~100℃烘干,得到PVDF压电薄膜。
优选的,上述的PVDF压电薄膜的制备方法中,所述步骤(1)中,PVDF溶液中PVDF的质量分数为10~15%;在95~120℃烘干,冷却方式为水冷,有机溶剂为N-甲基吡咯烷酮或二甲基乙酰胺。
优选的,上述的PVDF压电薄膜的制备方法中,所述步骤(2)中,单向拉伸和极化的具体步骤为:将PVDF膜片在温度为80~110℃、拉伸速度为5~20cm/min条件下,单向拉伸4~5倍,然后升温至120~125℃保温20~30min,自然冷却至室温得到PVDF薄膜;然后把PVDF薄膜夹在一对平面电极之间,浸入在硅油中,加热升温至80~90℃,在两电极之间施加电压50~80kV/cm条件下极化20~60min,然后恒定电压下冷却至室温。
优选的,上述的PVDF压电薄膜的制备方法中,所述PEDOT:PSS水溶液的质量百分比浓度为1~2%。
优选的,上述的PVDF压电薄膜的制备方法中,所述步骤(1)中,在PVDF溶液中加入钛酸铋钠(Bi0.5Na0.5TiO3),所述钛酸铋钠的加入量为所述PVDF重量的5~20%。
优选的,上述的PVDF压电薄膜的制备方法中,所述钛酸铋钠为改性钛酸铋钠,所述改性钛酸铋钠由以下方法制备而成:
①将硅烷偶联剂、去离子水和无水乙醇搅拌混合0.5~1h,得到混合溶液;将钛酸铋钠粉末加入混合溶液中,超声振荡0.5~1h,得到混悬液;
②在冰水浴条件下,将苯胺的酸性溶液滴加入步骤①得到的混悬液中,苯胺滴加完毕后,再滴加过硫酸铵的酸性溶液,在冰水浴中搅拌24~48h,然后过滤得到沉淀,洗涤,烘干,得到改性钛酸铋钠。采用硅烷偶联剂对钛酸铋钠进行表面改性,然后在钛酸铋钠表面修饰聚苯胺层得到改性的钛酸铋钠,改性的钛酸铋钠能够均匀分散在PVDF压电薄膜中,同时聚苯胺与PVDF相互作用,能够大大提高PVDF压电薄膜的压电性能。
优选的,上述的PVDF压电薄膜的制备方法中,所述步骤①中,硅烷偶联剂、去离子水与无水乙醇的重量比为1:50~60:30~40;钛酸铋钠粉末与混合溶液的重量比为1:20~45。
优选的,上述的PVDF压电薄膜的制备方法中,所述步骤②中,苯胺的加入量为所述钛酸铋钠重量的5~15%,苯胺与过硫酸铵的摩尔比为1:0.5~1,酸性溶液为盐酸,盐酸浓度为0.5~2mol/L。
上述的PVDF压电薄膜的制备方法制备得到的PVDF压电薄膜。
上述的PVDF压电薄膜在制备压电传感器中的应用。
与现有的技术相比,本发明具有如下有益效果:
1.本发明的PVDF压电薄膜的制备方法中,在PVDF压电薄膜旋涂一层PEDOT:PSS膜,提高PVDF压电薄膜的压电性能,同时保持PVDF压电薄膜的柔韧性和强度,并且制备工艺简单、操作方便,有利于推动PVDF压电薄膜在柔性压电传感器中应用。
2.本发明的PVDF压电薄膜的制备方法中,通过在PVDF加入钛酸铋钠,进一步提高PVDF压电薄膜的压电性能;同时通过钛酸铋钠进行改性,提高钛酸铋钠的分散性,与PVDF相互作用,显著增强压电薄膜压电常数D33,表现出优异的压电性能,同时维持PVDF压电薄膜的较好的柔韧性和强度。
具体实施方式
下面对本发明的具体实施方式进行详细描述,但应当理解本发明的保护范围并不受具体实施方式的限制。
实施例1
一种PVDF压电薄膜的制备方法,包括以下步骤:
(1)将PVDF溶于N-甲基吡咯烷酮中得到PVDF溶液,PVDF溶液中PVDF的质量分数为10%,将PVDF溶液在玻璃基底上涂膜,在100℃烘干2h,水冷得到PVDF膜片;
(2)对步骤(1)制得的PVDF膜片放入专用拉伸机中进行单向拉伸,在温度为105℃、拉伸速度为15cm/min条件下,单向拉伸4倍,然后升温至120℃保温20min,自然冷却至室温,得到厚度约为53μm的PVDF薄膜;然后把PVDF薄膜夹在一对平面电极之间,浸入在硅油中,加热升温至90℃,在两电极之间施加电压50kV/cm条件下极化30min,然后恒定电压下自然冷却至室温,得到极化的PVDF薄膜;
(3)将质量百分比浓度为1%的PEDOT:PSS水溶液真空旋转涂覆在步骤(2)得到的极化PVDF薄膜上,真空旋转涂覆工艺参数为:第一级转速800rpm,运行时间为5s,第二级转速为3000rpm,运行时间为6s;80℃烘干20min,得到PVDF压电薄膜。
实施例2
一种PVDF压电薄膜的制备方法,包括以下步骤:
(1)将PVDF溶于N-甲基吡咯烷酮中得到PVDF溶液,PVDF溶液中PVDF的质量分数为10%,在PVDF溶液中加入表面改性的钛酸铋钠粉末,钛酸铋钠粉末的加入量为PVDF重量的10%,在功率为600W条件下超声分散1h得到混合液;将混合液在玻璃基板上涂膜,在100℃烘干2h,水冷得到PVDF膜片;
(2)对步骤(1)制得的PVDF膜片放入专用拉伸机中进行单向拉伸,在温度为105℃、拉伸速度为15cm/min条件下,单向拉伸4倍,然后升温至120℃保温20min,自然冷却至室温得到厚度约为53μm的PVDF薄膜;然后把PVDF薄膜夹在一对平面电极之间,浸入在硅油中,加热升温至90℃,在两电极之间施加电压50kV/cm条件下极化30min,然后恒定电压下自然冷却至室温,得到极化的PVDF薄膜;
(3)将质量百分比浓度为1%的PEDOT:PSS水溶液真空旋转涂覆在步骤(2)得到的极化PVDF薄膜上,真空旋转涂覆工艺参数为:第一级转速800rpm,运行时间为5s,第二级转速为3000rpm,运行时间为6s;80℃烘干20min,得到PVDF压电薄膜。
表面改性的钛酸铋钠粉末的制备过程为:将γ-甲基丙烯酰氧基丙基三甲氧基硅 烷、去离子水和无水乙醇按照1:55:35搅拌混合1h,得到混合溶液;将粒径为0.5~1μm钛酸铋钠粉末加入混合溶液中,钛酸铋钠粉末与混合溶液的重量比为1:40,在功率为600W条件下超声振荡1h,然后过滤、用去离子水洗涤3次、真空100℃干燥3h,得到表面改性钛酸铋钠粉末。
实施例3
一种PVDF压电薄膜的制备方法,包括以下步骤:
(1)将PVDF溶于N-甲基吡咯烷酮中得到PVDF溶液,PVDF溶液中PVDF的质量分数为10%,在PVDF溶液中加入改性钛酸铋钠粉末,改性钛酸铋钠粉末的加入量为PVDF重量的10%;在功率为600W条件下超声分散1h得到混合液;将混合液在玻璃基板上涂膜,在100℃烘干2h,水冷得到PVDF膜片;
(2)对步骤(1)制得的PVDF膜片放入专用拉伸机中进行单向拉伸,在温度为105℃、拉伸速度为15cm/min条件下,单向拉伸4倍,然后升温至120℃保温20min,自然冷却至室温得到厚度约为53μm的PVDF薄膜;然后把PVDF薄膜夹在一对平面电极之间,浸入在硅油中,加热升温至90℃,在两电极之间施加电压50kV/cm条件下极化30min,然后恒定电压下自然冷却至室温,得到极化的PVDF薄膜;
(3)将质量百分比浓度为1%的PEDOT:PSS水溶液真空旋转涂覆在步骤(2)得到的极化PVDF薄膜上,真空旋转涂覆工艺参数为:第一级转速800rpm,运行时间为5s,第二级转速为3000rpm,运行时间为6s;80℃烘干20min,得到PVDF压电薄膜。
改性钛酸铋钠由以下方法制备而成:
①将γ-甲基丙烯酰氧基丙基三甲氧基硅烷、去离子水和无水乙醇按照1:55:35搅拌混合1h,得到混合溶液;将粒径为0.5~1μm钛酸铋钠粉末加入混合溶液中,钛酸铋钠粉末与混合溶液的重量比为1:40,在功率为600W条件下超声振荡1h,得到混悬液;
②在5℃以下冰水浴条件下,将苯胺盐酸溶液滴加入步骤①得到的混悬液中,苯胺盐酸溶液为苯胺与盐酸体积比为1:1进行混合得到,盐酸的浓度为1mol/L,苯胺的加入量为钛酸铋钠重量的12%;苯胺滴加完毕后,再缓慢滴加过硫酸铵的盐酸溶液,过硫酸铵与苯胺的摩尔比为1:1,过硫酸铵的盐酸溶液为过硫酸铵与盐酸质量体积比为0.6g:1mL进行混合溶解得到;在冰水浴中搅拌24h,然后过滤得到沉淀,用去离子水洗涤,真空100℃干燥3h,得到改性钛酸铋钠。
实施例4
本实施例同实施例3,不同之处在于:改性钛酸铋钠制备过程中苯胺的加入量为钛酸铋钠重量的8%。
实施例5
本实施例同实施例3,不同之处在于:改性钛酸铋钠制备过程中苯胺的加入量为钛酸铋钠重量的15%。
对比例1
一种PVDF压电薄膜的制备方法,包括以下步骤:
(1)将PVDF溶于N-甲基吡咯烷酮中得到PVDF溶液,PVDF溶液中PVDF的质量分数为10%,将PVDF溶液在玻璃基底上涂膜,在100℃烘干2h,水冷得到PVDF膜片;
(2)对步骤(1)制得的PVDF膜片放入专用拉伸机中进行单向拉伸,在温度为105℃、拉伸速度为15cm/min条件下,单向拉伸4倍,然后升温至120℃保温20min,自然冷却至室温得到PVDF薄膜;然后把PVDF薄膜夹在一对平面电极之间,浸入在硅油中,加热升温至90℃,在两电极之间施加电压50kV/cm条件下极化30min,然后恒定电压下自然冷却至室温,得到PVDF压电薄膜。
对比例2
本实施例同实施例3,不同之处在于:改性钛酸铋钠制备过程中苯胺的加入量为钛酸铋钠重量的3%。
对比例3
本实施例同实施例3,不同之处在于:改性钛酸铋钠制备过程中苯胺的加入量为钛酸铋钠重量的20%。
对实施例1~5和对比例1~3制备的PVDF压电薄膜进行拉伸性能测试,采用拉伸试验机进行测试。在PVDF压电薄膜两侧面涂膜银浆层,采用准动态测试法-冲击试验测定压电系数d33,具体步骤参照“严伏明等,高分子压电材料压电常数d33的测定”,测试结果如表1所示。
由表1可知,相比对比例1,实施例1、实施例2和实施例3制备的PVDF压电薄膜的压电系数d33分别提高了57.8%、100%和142.8%,实施例1的PVDF压电薄膜拉伸强度和断裂伸长率与对比例1相当,实施例2和实施例3的PVDF压电薄膜拉伸强度和断裂伸长率相较于对比例1有小幅度下降,但仍维持较好的强度和柔韧性。以上结果表明,相较于纯的PVDF压电薄膜,本申请制备的PVDF压电薄膜压电性能提高显著,并且能够维持PVDF压电薄膜的强度和柔韧性。同时由表1可知,加入改性钛酸铋钠的PVDF压电薄膜的压电性能显著提高,通过优化改性钛酸铋钠中聚苯胺的含量实现对压电性能的提高,聚苯胺过高或者过低,压电性能的提升效果不明显。
表1 PVDF压电薄膜的性能数据
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式,并且很显然,根据上述教导,可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用,从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。本发明的范围意在由权利要求书及其等同形式所限定。
Claims (8)
1.一种PVDF压电薄膜的制备方法,其特征在于,包括以下步骤:
(1)将PVDF溶于有机溶剂中得到PVDF溶液,将PVDF溶液在玻璃基板上涂膜,烘干,冷却得到PVDF膜片;在PVDF溶液中加入改性钛酸铋钠,所述改性钛酸铋钠的加入量为所述PVDF重量的5~20%;
(2)对步骤(1)制得的PVDF膜片进行单向拉伸,极化,得到极化的PVDF薄膜;
(3)将PEDOT:PSS水溶液真空旋转涂覆在步骤(2)得到的PVDF薄膜上,真空旋转涂覆工艺参数为:第一级转速600~800rpm,运行时间为5~10s,第二级转速为2500~3000rpm,运行时间为6~12s;70~100℃烘干,得到PVDF压电薄膜;
所述改性钛酸铋钠由以下方法制备而成:
①将硅烷偶联剂、去离子水和无水乙醇搅拌混合0.5~1h,得到混合溶液;将钛酸铋钠粉末加入混合溶液中,超声振荡0.5~1h,得到混悬液;
②在冰水浴条件下,将苯胺的酸性溶液滴加入步骤①得到的混悬液中,苯胺的加入量为钛酸铋钠重量的5~15%,苯胺滴加完毕后,再滴加过硫酸铵的酸性溶液,在冰水浴中搅拌24~48h,然后过滤得到沉淀,洗涤,烘干,得到改性钛酸铋钠。
2.根据权利要求1所述的PVDF压电薄膜的制备方法,其特征在于,所述步骤(1)中,PVDF溶液中PVDF的质量分数为10~15%;在95~120℃烘干,冷却方式为水冷,有机溶剂为N-甲基吡咯烷酮或二甲基乙酰胺。
3.根据权利要求1所述的PVDF压电薄膜的制备方法,其特征在于,所述步骤(2)中,单向拉伸和极化的具体步骤为:将PVDF膜片在温度为80~110℃、拉伸速度为5~20cm/min条件下,单向拉伸4~5倍,然后升温至120~125℃保温20~30min,自然冷却至室温得到PVDF薄膜;然后把PVDF薄膜夹在一对平面电极之间,浸入在硅油中,加热升温至80~90℃,在两电极之间施加电压30~80kV/cm条件下极化20~60min,然后恒定电压下冷却至室温。
4.根据权利要求1所述的PVDF压电薄膜的制备方法,其特征在于,所述PEDOT:PSS水溶液的质量百分比浓度为1~2%。
5.根据权利要求1所述的PVDF压电薄膜的制备方法,其特征在于,所述步骤①中,硅烷偶联剂、去离子水与无水乙醇的重量比为1:50~60:30~40;钛酸铋钠粉末与混合溶液的重量比为1:20~45。
6.根据权利要求1所述的PVDF压电薄膜的制备方法,其特征在于,所述步骤②中,苯胺与过硫酸铵的摩尔比为1:0.5~1,酸性溶液为盐酸,盐酸浓度为0.5~2mol/L。
7.根据权利要求1~6任一项所述的PVDF压电薄膜的制备方法制备得到的PVDF压电薄膜。
8.根据权利要求7所述的PVDF压电薄膜在制备压电传感器中的应用。
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