CN105591022B - 铌酸钠钾纤维基复合材料的柔性纳米发电机的制备方法 - Google Patents
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- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000002131 composite material Substances 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 21
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 13
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- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 32
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 12
- 239000010955 niobium Substances 0.000 claims description 9
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 8
- 239000004744 fabric Substances 0.000 claims description 8
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 8
- -1 polydimethylsiloxane Polymers 0.000 claims description 5
- 238000009987 spinning Methods 0.000 claims description 5
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 4
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- 239000012298 atmosphere Substances 0.000 claims description 4
- 230000005684 electric field Effects 0.000 claims description 4
- 235000011056 potassium acetate Nutrition 0.000 claims description 4
- 239000001632 sodium acetate Substances 0.000 claims description 4
- 235000017281 sodium acetate Nutrition 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 claims description 3
- PNCDAXYMWHXGON-UHFFFAOYSA-N ethanol;niobium Chemical compound [Nb].CCO.CCO.CCO.CCO.CCO PNCDAXYMWHXGON-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
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- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical class OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 abstract description 11
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 abstract description 10
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 abstract description 10
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 abstract description 9
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- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 4
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- 239000012362 glacial acetic acid Substances 0.000 description 3
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
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- 239000003795 chemical substances by application Substances 0.000 description 2
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- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical group [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect 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
- 238000006243 chemical reaction Methods 0.000 description 1
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000003022 phthalic acids Chemical class 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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Abstract
本发明公开了铌酸钠钾纤维基复合材料的柔性纳米发电机的制备方法,该铌酸钠钾的化学通式为:0.96(K0.48Na0.52)(Nb0.95Sb0.05)O3‑0.04Bi0.05(Na0.82K0.18)0.05ZrO3(KNNS‑BNKZ),应用溶胶凝胶法配置前驱体溶胶,通过静电纺丝法制备纤维,经过热处理将纤维粉碎,与PDMS(聚二甲基硅氧烷)混合后用涂膜器刮涂在溅射了铜的PET(聚对苯二甲酸类塑料)基底上,引出铜导线,上面覆盖同样的溅射了铜的PET(聚对苯二甲酸类塑料),然后用PDMS(聚二甲基硅氧烷)封装,固化,极化后即得到无铅的柔性纳米发电机。该方法简单可靠,工艺重复性好,可操作性强。本发明制备的纳米发电机变形后能产生高达10V的电压,能实现能量的收集与存储,可用自供电于无线无源传感器网络。
Description
技术领域
本发明涉及铌酸钠钾纤维基复合材料的柔性纳米发电机的制备方法,具体是一种0.96(K0.48Na0.52)(Nb0.95Sb0.05)O3-0.04Bi0.05(Na0.82K0.18)0.05ZrO3(简称KNNS-BNKZ)溶胶的制备,静电纺丝及热处理以及纳米发电机的制备。
背景技术
纳米发电机是在微纳尺度能够进行力-电能量转换的器件,在生物医学、军事、无线通信和无线传感方面都将有广泛的重要应用。目前研究最多的是锆钛酸铅(PZT)基压电式纳米发电机,然后铅对环境及人体的危害阻碍了它的应用。0.96(K0.48Na0.52)(Nb0.95Sb0.05)O3-0.04Bi0.05(Na0.82K0.18)0.05ZrO3基无铅压电材料以优越的压电性能(d33~490pc/N,Tc~220℃)和环境友好性而成为最有可能替代锆钛酸铅(PZT)的压电材料之一。将KNNS-BNKZ纤维与PDMS(聚二甲基硅氧烷)复合,刮涂大面积无孔隙、无裂纹、均匀度一致性的薄膜同时具有高分子材料的柔性与压电材料的压电效应,能够有效克服压电陶瓷硬,脆的缺点,轻松的实现变形并将机械能转化为电能。现在传感器网络节点都是使用化学电池为传感器供电,无法长期提供电能,需要经常性更换电池,浪费大量人力与资源。本发明可以用于无线传感器供电,支撑起传感器网络。
目前通过溶胶法和静电纺丝法制备KNNS-BNKZ纤维以及将其与PDMS(聚二甲基硅氧烷)复合后制备纳米发电机方法未有报道。
发明内容
技术问题:本发明提供了一种铌酸钠钾纤维基复合材料的柔性纳米发电机的制备方法,该方法简单可靠,工艺重复性好,可操作性强。
技术方案:本发明的铌酸钠钾纤维基复合材料的柔性纳米发电机的制备方法,采用溶胶法制备前驱体溶胶和静电纺丝法制备纤维,然后组装纳米发电机,包括如下步骤:
该制备方法包括配制溶胶,将该溶胶通过静电纺丝法制备纤维,然后制备纤维基纳米发电机,所述的溶胶是0.96(K0.48Na0.52)(Nb0.95Sb0.05)O3-0.04Bi0.05(Na0.82K0.18)0.05ZrO3, 简称KNNS-BNKZ,具体包括以下步骤:
步骤1、以所述的溶胶化学通式中的比例依次称取药品,配置KNNS-BNKZ溶胶;
步骤2、将KNNS-BNKZ溶胶在静电纺丝机上纺丝,得到KNNS-BNKZ纤维;
步骤3、将步骤2得到的KNNS-BNKZ纤维进行热处理;
步骤4、将步骤3得到的纤维粉碎,与聚二甲基硅氧烷PDMS混合,在溅射了铜的聚对苯二甲酸类塑料PET基底上涂膜,引出铜导线,然后在该膜的上面覆盖同样的溅射了铜的聚对苯二甲酸类塑料PET,封装,固化,极化后即得到KNNS-BMKZ基纳米发电机。
其中:
步骤1中以化学通式0.96(K0.48Na0.52)(Nb0.95Sb0.05)O3-0.04Bi0.05(Na0.82K0.18)0.05ZrO3为依据,按化学计量比依次称取乙酸钾、乙酸钠、乙酸锑、乙酰丙酮锆,五水合硝酸铋,溶于冰醋酸、乙二醇甲醚和乙酰丙酮的混合溶剂中,制得前驱体A;按照化学通式称取乙醇铌,溶解在乙二醇甲醚中,注意在干燥气氛中称量溶解制备前驱体B;将前驱体A与前驱体B混合搅拌,最后加入按照体积称量0.06g/mLPVP作为溶胶稳定剂并增加黏度以便静电纺丝,搅拌10h-24h后即得到黄色澄清透明的KNNS-BNKZ溶胶。
步骤2中,静电纺丝工艺参数为:注射泵注射速率为0.001-0.015mL/min,高压电场为0.2kV/cm-1kV/cm,取下得到的织物,在80℃干燥10h-24h。
步骤3所述KNNS-BNKZ纤维的热处理过程为:先以5℃/min的速度升温至100℃,保温30min,再以5℃/min的速度升温至430℃,保温30min,再以5℃/min的速度升温至700℃,保温60min,自然冷却至室温。
有益效果:本发明提供了一种铌酸钠钾纤维基复合材料的柔性纳米发电机的制备方法,将KNNS-BNKZ纤维与PDMS(聚二甲基硅氧烷)复合,刮涂大面积无孔隙、无裂纹、均匀度一致性的薄膜同时具有高分子材料的柔性与压电材料的压电效应,能够有效克服压电陶瓷硬,脆的缺点,轻松的实现变形并将机械能转化为电能。该方法简单可靠,工艺重复性好,可操作性强。
具体实施方式
下面结合实施例对本发明做更进一步的解释。下列实施例仅用于说明本发明,但并不用来限定发明的实施范围。
步骤1、以化学通式0.96(K0.48Na0.52)(Nb0.95Sb0.05)O3-0.04Bi0.05(Na0.82K0.18)0.05ZrO3为依据,按化学通式中的比例依次称取乙酸钾、乙酸钠、乙酸锑、乙酰丙酮锆,五水合硝酸铋,溶于冰醋酸、乙二醇甲醚和乙酰丙酮的混合溶剂中,制得前驱体A;按照化学通式称取乙醇铌,溶解在乙二醇甲醚中,注意在干燥气氛中称量溶解制备前驱体B;将步骤1与步骤2制备的前驱体混合搅拌,然后按照体积称量0.06g/mL的PVP溶解在前驱体中,搅拌24h后即得到黄色澄清透明的KNNS-BNKZ溶胶。
步骤2、将KNNS-BNKZ溶胶在静电纺丝机上纺丝,注射泵注射速率为0.001-0.015mL/min,高压电场为0.2-1kV/cm,之后揭下得到的织物,在80℃干燥10h-24h。
步骤3、将步骤2得到的织物进行热处理,先以5℃/min的速度升温至100℃,保温30min,再以5℃/min的速度升温至430℃,保温30min,再以5℃/min的速度升温至700℃,保温60min,自然冷却至室温。
步骤4、将步骤3得到的织物粉碎,与PDMS(聚二甲基硅氧烷)按照1:5~1:10的质量比混合,用涂膜器在溅射了铜的PET(聚对苯二甲酸类塑料)基底上刮涂薄膜,引出铜导线,上面覆盖同样的溅射了铜的PET(聚对苯二甲酸类塑料),然后用PDMS(聚二甲基硅氧烷)封装,固化,极化后即得到KNNS-BMKZ基纳米发电机。
实施例1
步骤1、以化学通式0.96(K0.48Na0.52)(Nb0.95Sb0.05)O3-0.04Bi0.05(Na0.82K0.18)0.05ZrO3为依据,按化学通式中的0.01molKNNS-BNKZ的质量依次称取乙酸钾、乙酸钠、乙酸锑、乙酰丙酮锆,五水合硝酸铋,溶于冰醋酸4mL、乙二醇甲醚10mL和乙酰丙酮4mL的混合溶剂中,制得前驱体A;按照化学通式称取乙醇铌,溶解在10mL乙二醇甲醚中,注意在干燥气氛中称量溶解制备前驱体B;将步骤1与步骤2制备的前驱体混合搅拌,然后按照体积称量0.06g/mL的PVP溶解在前驱体中,搅拌24h后即得到黄色澄清透明的KNNS-BNKZ溶胶。
步骤2、用针管抽取步骤1制备的KNNS-BNKZ溶胶,用导管连接到滚筒式静电纺丝机的喷头,将针管固定在注射泵上,用铝箔包裹住滚筒,进行纺丝,注射泵注射速率为0.015mL/min,喷头与滚筒收集器之间距离为20cm,电压为20kV,滚筒转速为700rpm,之后取下铝箔,揭下得到的织物,在80℃干燥24h。
步骤3、将步骤2得到的织物进行热处理,先以5℃/min的速度升温至100℃,保温30min,再以5℃/min的速度升温至430℃,保温30min,再以5℃/min的速度升温至 700℃,保温60min,自然冷却至室温。
步骤4、将步骤3得到的织物粉碎,与PDMS(聚二甲基硅氧烷)按照1:5~1:10的质量比混合,(PDMS(聚二甲基硅氧烷):固化剂:己烷以10:1:1的质量比预混合),用涂膜器在用涂膜器在溅射了铜的PET(聚对苯二甲酸类塑料)基底上刮涂10μm厚的薄膜,引出铜导线,上面覆盖同样的溅射了铜的PET(聚对苯二甲酸类塑料),然后用PDMS(聚二甲基硅氧烷)封装,在100℃下固化,在1kV/mm的电场下极化3h后即得到KNNS-BMKZ基纳米发电机。
Claims (1)
1.一种铌酸钠钾纤维基复合材料的柔性纳米发电机的制备方法,其特征在于,该制备方法包括配制溶胶,将该溶胶通过静电纺丝法制备纤维,然后制备纤维基纳米发电机,所述的溶胶是0.96(K0.48Na0.52)(Nb0.95Sb0.05)O3-0.04Bi0.05(Na0.82K0.18)0.05ZrO3,简称KNNS-BNKZ,具体包括以下步骤:
步骤1、以所述的溶胶化学通式中的比例依次称取药品,配置KNNS-BNKZ溶胶;
步骤2、将KNNS-BNKZ溶胶在静电纺丝机上纺丝,得到KNNS-BNKZ纤维;
步骤3、将步骤2得到的KNNS-BNKZ纤维进行热处理;
步骤4、将步骤3得到的纤维粉碎,与聚二甲基硅氧烷PDMS混合,在溅射了铜的聚对苯二甲酸类塑料PET基底上涂膜,引出铜导线,然后在该膜的上面覆盖同样的溅射了铜的聚对苯二甲酸类塑料PET,封装,固化,极化后即得到KNNS-BMKZ基纳米发电机;
其中,
步骤1中以化学通式0.96(K0.48Na0.52)(Nb0.95Sb0.05)O3-0.04Bi0.05(Na0.82K0.18)0.05ZrO3为依据,按化学计量比依次称取乙酸钾、乙酸钠、乙酸锑、乙酰丙酮锆,五水合硝酸铋,溶于冰醋酸、乙二醇甲醚和乙酰丙酮的混合溶剂中,制得前驱体A;按照化学通式称取乙醇铌,溶解在乙二醇甲醚中,注意在干燥气氛中称量溶解制备前驱体B;将前驱体A与前驱体B混合搅拌,最后加入按照体积称量0.06g/mLPVP作为溶胶稳定剂并增加黏度以便静电纺丝,搅拌10h-24h后即得到黄色澄清透明的KNNS-BNKZ溶胶;
步骤2中,静电纺丝工艺参数为:注射泵注射速率为0.001-0.015mL/min,高压电场为0.2kV/cm-1kV/cm,取下得到的织物,在80℃干燥10h-24h;
步骤3所述KNNS-BNKZ纤维的热处理过程为:先以5℃/min的速度升温至100℃,保温30min,再以5℃/min的速度升温至430℃,保温30min,再以5℃/min的速度升温至700℃,保温60min,自然冷却至室温。
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