CN101859046A - Preparation method of polyvinylpyrrolidone-based solid electrolyte - Google Patents
Preparation method of polyvinylpyrrolidone-based solid electrolyte Download PDFInfo
- Publication number
- CN101859046A CN101859046A CN201010184820A CN201010184820A CN101859046A CN 101859046 A CN101859046 A CN 101859046A CN 201010184820 A CN201010184820 A CN 201010184820A CN 201010184820 A CN201010184820 A CN 201010184820A CN 101859046 A CN101859046 A CN 101859046A
- Authority
- CN
- China
- Prior art keywords
- solid electrolyte
- electrolyte
- solution
- pvp
- lithium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920000036 polyvinylpyrrolidone Polymers 0.000 title claims abstract description 42
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 title claims abstract description 42
- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 41
- 239000001267 polyvinylpyrrolidone Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003792 electrolyte Substances 0.000 claims abstract description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 12
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 12
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 230000008020 evaporation Effects 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 239000011255 nonaqueous electrolyte Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- -1 lithium tetrafluoroborate Chemical compound 0.000 claims description 8
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 5
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 5
- HZNVUJQVZSTENZ-UHFFFAOYSA-N 2,3-dichloro-5,6-dicyano-1,4-benzoquinone Chemical compound ClC1=C(Cl)C(=O)C(C#N)=C(C#N)C1=O HZNVUJQVZSTENZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 3
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 2
- 230000002441 reversible effect Effects 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 6
- 239000005518 polymer electrolyte Substances 0.000 description 6
- 238000004061 bleaching Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 238000004040 coloring Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000011244 liquid electrolyte Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 4
- 239000004926 polymethyl methacrylate Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000004984 smart glass Substances 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920003169 water-soluble polymer Polymers 0.000 description 2
- 241000195940 Bryophyta Species 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000795 conjunctiva Anatomy 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000118 hair dye Substances 0.000 description 1
- 239000008266 hair spray Substances 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 235000011929 mousse Nutrition 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 231100000344 non-irritating Toxicity 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Conductive Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
一种聚乙烯吡咯烷酮基固体电解质的制备方法，1)将2.5-14g锂盐或钾盐溶解于去离子水中，配成浓度为0.5-2mol/L的溶液；或将2.5-10g锂盐或钾盐溶解于有机溶剂PC和丙酮中，配成浓度为0.5-1mol/L的溶液。2)将30-130g PVP粉末溶解于上述溶液中，得到粘稠电解质，所用PVP的分子量介于8000-1300000；在所得粘稠电解质中，PVP所占的百分含量为：在含水型电解质中占45-55％；在非水型电解质中占25-35％；3)将所得粘稠电解质涂敷或填充至相应器件中，在室温下蒸发后形成固体电解质。本发明工艺简单、操作简便、成本低，可以根据不同需求制备含水型与非水型固体电解质。
A preparation method of a polyvinylpyrrolidone-based solid electrolyte, 1) dissolving 2.5-14g lithium salt or potassium salt in deionized water to form a solution with a concentration of 0.5-2mol/L; or dissolving 2.5-10g lithium salt or potassium salt The salt is dissolved in the organic solvent PC and acetone to form a solution with a concentration of 0.5-1mol/L. 2) Dissolving 30-130g of PVP powder in the above solution to obtain a viscous electrolyte, the molecular weight of the PVP used is between 8000-1300000; in the obtained viscous electrolyte, the percentage of PVP is: in the aqueous electrolyte Accounting for 45-55%; accounting for 25-35% in non-aqueous electrolytes; 3) coating or filling the obtained viscous electrolyte into corresponding devices, and forming a solid electrolyte after evaporation at room temperature. The invention has the advantages of simple process, convenient operation and low cost, and can prepare water-containing and non-aqueous solid electrolytes according to different requirements.
Description
技术领域technical field
本发明涉及一种固体电解质。特别是涉及一种电化学性能稳定和机械性能良好的多用途的聚乙烯吡咯烷酮基固体电解质的制备方法。The invention relates to a solid electrolyte. In particular, it relates to a method for preparing a multipurpose polyvinylpyrrolidone-based solid electrolyte with stable electrochemical performance and good mechanical performance.
背景技术Background technique
液体电解质已被广泛应用于移动通讯、电动交通工具、电子表的电池和超级电容器，以及用作电致变色器件的电解质。但是这些使用液体电解质的电子器件具有很多的缺点：如器件封装困难；电池易产生气胀、漏液等问题，易造成电子器件的腐蚀和损坏；可能出现起火和爆炸等事故；应用于大面积的电致变色智能窗等大型器件中，液体电解质是一个很大的安全隐患。而采用聚合物固体电解质，则可有效克服液体电解质的上述缺陷。同时，由于聚合物良好的粘结性能，使得组装的器件牢固可靠，安全性能显著提高，从而可应用于对安全性要求较高的电动交通工具、电致变色智能窗、航天器和军事等领域。Liquid electrolytes have been widely used in batteries and supercapacitors for mobile communications, electric vehicles, electronic watches, and as electrolytes for electrochromic devices. However, these electronic devices using liquid electrolytes have many disadvantages: such as difficult device packaging; batteries are prone to gas inflation, leakage and other problems, which are easy to cause corrosion and damage to electronic devices; accidents such as fire and explosion may occur; In large devices such as electrochromic smart windows, liquid electrolytes are a big safety hazard. The use of polymer solid electrolytes can effectively overcome the above-mentioned defects of liquid electrolytes. At the same time, due to the good bonding performance of the polymer, the assembled device is firm and reliable, and the safety performance is significantly improved, so it can be applied to electric vehicles with high safety requirements, electrochromic smart windows, spacecraft and military fields. .
聚合物电解质一般由聚合物基体和无机盐组成，具有离子导电能力，可用于电池、超级电容器和电致变色等器件。当用于电致变色器件时，可同时起到电解质和隔膜的作用。它除了提供电致变色材料所需的补偿离子(如Li+，Na+，K+等)外，还需要有较高的离子电导率、机械强度，同时还必须具有良好的透光率。聚氧化乙烯(PEO)是目前研究最多的聚合物电解质基体材料。但是，室温下PEO与碱金属盐的络合物结晶度很高，所得电解质的电导率很低，不能满足当前对快速充放电电池、超级容器和快速响应电致变色器件的使用要求。以聚甲基丙烯酸甲酯(PMMA)为基体的聚合物电解质具有较高的离子电导率，与金属锂电极的界面稳定性和相容性较好，再加上PMMA原料丰富、价格低廉、制备简单，从而引起了研究者们的兴趣。然而，PMMA基聚合物电解质的机械强度较差，限制了它的应用。聚偏氟乙烯(PVDF)聚合物也具有较高的离子电导率、良好的机械强度和化学稳定性，近来研究较多，但其单体的制备用到剧毒的氟化氢，生产过程危险。聚乙烯吡咯烷酮(PVP)是一种水溶性的聚合物，具有很强的粘接能力，易获得牢固稳定的全固态电子器件。它具有优良的生理惰性和生物相容性，不参与人体的新陈代谢，对皮肤、粘膜、眼睛等无刺激。PVP已广泛用于制造定型液、喷发胶及摩丝的定型剂、护发剂的遮光剂、香波的泡沫稳定剂及染发剂中的分散剂和亲合剂，纸张、纺织印染等工业中用作分散剂、成膜剂及乳化剂等助剂。PVP的生产工艺简单、安全、成本低。PVP具有优良的溶解性和明显的溶胀作用，溶于水中可以使溶液的体积达到所用溶剂体积的两倍。溶胀后的溶液中含有PVP高分子长链形成的网络结构，失去部分水分后形成聚合物凝胶，同时表面结膜。PVP的这种性质使其网络结构可容纳大量的导电离子，同时又具有较高的机械强度，非常适合用作锂离子电池、超级电容器和电致变色器件的电解质基体。因此，PVP基聚合物电解质的开发具有重要意义。然而，目前还未见任何有关PVP用于聚合物电解质的文献报道。Polymer electrolytes are generally composed of polymer matrix and inorganic salts, have ion conductivity, and can be used in devices such as batteries, supercapacitors, and electrochromics. When used in an electrochromic device, it can act as both an electrolyte and a separator. In addition to providing the compensation ions (such as Li + , Na + , K + , etc.) required by electrochromic materials, it also needs to have high ionic conductivity, mechanical strength, and good light transmittance. Polyethylene oxide (PEO) is currently the most studied polymer electrolyte matrix material. However, the complexes of PEO and alkali metal salts have high crystallinity at room temperature, and the resulting electrolytes have low conductivity, which cannot meet the current requirements for fast charge-discharge batteries, supercapacitors, and fast-response electrochromic devices. The polymer electrolyte based on polymethyl methacrylate (PMMA) has high ionic conductivity, good interface stability and compatibility with lithium metal electrodes, and PMMA is rich in raw materials, low in price and easy to prepare Simple, which has aroused the interest of researchers. However, the poor mechanical strength of PMMA-based polymer electrolytes limits its applications. Polyvinylidene fluoride (PVDF) polymer also has high ionic conductivity, good mechanical strength and chemical stability, and has been studied more recently, but its monomer preparation uses highly toxic hydrogen fluoride, and the production process is dangerous. Polyvinylpyrrolidone (PVP) is a water-soluble polymer with strong bonding ability, and it is easy to obtain firm and stable all-solid-state electronic devices. It has excellent physiological inertia and biocompatibility, does not participate in the metabolism of the human body, and is non-irritating to the skin, mucous membranes, and eyes. PVP has been widely used in the manufacture of styling liquid, hairspray and mousse styling agent, hair sunscreen agent, shampoo foam stabilizer, and dispersant and affinity agent in hair dye. It is used as a dispersant in paper, textile printing and dyeing industries. Agents, film formers and emulsifiers and other additives. The production process of PVP is simple, safe and low in cost. PVP has excellent solubility and obvious swelling effect. Dissolving in water can make the volume of the solution reach twice the volume of the solvent used. The swollen solution contains a network structure formed by long chains of PVP polymers, and after losing part of the water, a polymer gel is formed, and the conjunctiva is formed on the surface. This property of PVP makes its network structure capable of accommodating a large number of conductive ions while having high mechanical strength, making it ideal for use as an electrolyte matrix for lithium-ion batteries, supercapacitors, and electrochromic devices. Therefore, the development of PVP-based polymer electrolytes is of great significance. However, there has not been any literature report on the use of PVP in polymer electrolytes.
发明内容Contents of the invention
本发明所要解决的技术问题是，提供一种操作简便、成本低、电化学性能稳定和机械性能良好的多用途的聚乙烯吡咯烷酮基固体电解质的制备方法。The technical problem to be solved by the present invention is to provide a method for preparing a multi-purpose polyvinylpyrrolidone-based solid electrolyte with simple operation, low cost, stable electrochemical performance and good mechanical performance.
本发明所采用的技术方案是：一种聚乙烯吡咯烷酮基固体电解质的制备方法，包括如下步骤：The technical scheme adopted in the present invention is: a preparation method of polyvinylpyrrolidone-based solid electrolyte, comprising the following steps:
1)将2.5-14g锂盐或钾盐溶解于去离子水中，配成浓度为0.5-2mol/L的溶液；或将2.5-10g锂盐或钾盐溶解于有机溶剂PC和丙酮中，配成浓度为0.5-1mol/L的溶液。1) Dissolve 2.5-14g of lithium salt or potassium salt in deionized water to make a solution with a concentration of 0.5-2mol/L; or dissolve 2.5-10g of lithium salt or potassium salt in organic solvent PC and acetone to make a solution A solution with a concentration of 0.5-1mol/L.
2)将30-130g PVP粉末溶解于上述溶液中，得到粘稠电解质，所用PVP的分子量介于8000-1300000；在所得粘稠电解质中，PVP所占的百分含量为：在含水型电解质中占45-55％；在非水型电解质中占25-35％；2) Dissolve 30-130g of PVP powder in the above solution to obtain a viscous electrolyte, the molecular weight of the PVP used is between 8000-1300000; in the obtained viscous electrolyte, the percentage of PVP is: in the aqueous electrolyte 45-55%; 25-35% in non-aqueous electrolytes;
3)将所得粘稠电解质涂敷或填充至相应器件中，在室温下蒸发后形成固体电解质。3) Coating or filling the obtained viscous electrolyte into corresponding devices, and forming a solid electrolyte after evaporation at room temperature.
所述的锂盐是高氯酸锂、四氟硼酸锂、硫酸锂或氯化锂中的一种。The lithium salt is one of lithium perchlorate, lithium tetrafluoroborate, lithium sulfate or lithium chloride.
所述的钾盐是氯化钾、硫酸钾、四氟硼酸钾和六氟磷酸钾中的一种。The potassium salt is one of potassium chloride, potassium sulfate, potassium tetrafluoroborate and potassium hexafluorophosphate.
本发明的聚乙烯吡咯烷酮基固体电解质的制备方法，具有如下优点与有益效果：The preparation method of the polyvinylpyrrolidone-based solid electrolyte of the present invention has the following advantages and beneficial effects:
1)采用水溶性的聚合物PVP为固体电解质的基体材料，既可溶于水也可溶于有机溶剂，可以根据不同需求制备含水型与非水型固体电解质。含水型的固体电解质成本更低、更环保，是一种环境友好型固体电解质。1) The water-soluble polymer PVP is used as the matrix material of the solid electrolyte, which is soluble in both water and organic solvents, and aqueous and non-aqueous solid electrolytes can be prepared according to different needs. The aqueous solid electrolyte has lower cost and is more environmentally friendly, and is an environmentally friendly solid electrolyte.
2)PVP无臭、无味、物理化学性质稳定；原料来源广泛、易得；粘接能力强、机械性能优良；具有成膜性；具有优良的生理惰性和生物相容性，对皮肤、粘膜、眼等无任何刺激。2) PVP is odorless, tasteless, and has stable physical and chemical properties; raw materials are widely available and easy to obtain; strong bonding ability, excellent mechanical properties; film-forming properties; excellent physiological inertia and biocompatibility No irritation to eyes etc.
3)所得固体电解质离子电导率高，用于电致变色器件中显示出快速响应的电致变色性能。3) The obtained solid electrolyte has high ionic conductivity and exhibits fast-response electrochromic performance when used in electrochromic devices.
4)多种无机、有机的锂盐和钾盐均可用作导电电解质。4) A variety of inorganic and organic lithium salts and potassium salts can be used as conductive electrolytes.
5)工艺简单、操作简便、成本低。5) The process is simple, the operation is simple and convenient, and the cost is low.
附图说明Description of drawings
图1a是本发明所制备的固体电解质驱动的小型电致变色器件着色的可逆颜色变化的效果图；Figure 1a is an effect diagram of the reversible color change of the small electrochromic device driven by the solid electrolyte prepared in the present invention;
图1b是本发明所制备的固体电解质驱动的小型电致变色器件漂白的可逆颜色变化的效果图；Figure 1b is an effect diagram of the reversible color change of the bleached small electrochromic device driven by the solid electrolyte prepared by the present invention;
图2a是本发明所制备的固体电解质驱动的大面积电致变色器件着色的可逆颜色变化效果图；Figure 2a is a reversible color change effect diagram of the coloring of a large-area electrochromic device driven by a solid electrolyte prepared by the present invention;
图2b是本发明所制备的固体电解质驱动的大面积电致变色器件漂白的可逆颜色变化效果图；Figure 2b is a reversible color change effect diagram of bleaching of a large-area electrochromic device driven by a solid electrolyte prepared in the present invention;
图3是本发明所制备的固体电解质的电致变色器件着色/漂白过程中电流随时间的变化曲线图。Fig. 3 is a graph showing the variation of current with time during the coloring/bleaching process of the solid electrolyte electrochromic device prepared in the present invention.
具体实施方式Detailed ways
下面结合实施例和附图对本发明的聚乙烯吡咯烷酮基固体电解质的制备方法做出详细说明，但本发明的内容不仅仅局限于下面的实施例。The preparation method of the polyvinylpyrrolidone-based solid electrolyte of the present invention will be described in detail below with reference to the examples and accompanying drawings, but the content of the present invention is not limited to the following examples.
本发明的聚乙烯吡咯烷酮基固体电解质的制备方法，包括如下步骤：The preparation method of polyvinylpyrrolidone-based solid electrolyte of the present invention, comprises the steps:
1)将2.5-14g锂盐或钾盐溶解于去离子水中，配成浓度为0.5-2mol/L的溶液；或将2.5-10g锂盐或钾盐溶解于有机溶剂PC和丙酮中，配成浓度为0.5-1mol/L的溶液；1) Dissolve 2.5-14g of lithium salt or potassium salt in deionized water to make a solution with a concentration of 0.5-2mol/L; or dissolve 2.5-10g of lithium salt or potassium salt in organic solvent PC and acetone to make a solution A solution with a concentration of 0.5-1mol/L;
所述的锂盐是高氯酸锂、四氟硼酸锂、硫酸锂或氯化锂中的一种；The lithium salt is one of lithium perchlorate, lithium tetrafluoroborate, lithium sulfate or lithium chloride;
所述的钾盐是氯化钾、硫酸钾、四氟硼酸钾和六氟磷酸钾中的一种；The potassium salt is one of potassium chloride, potassium sulfate, potassium tetrafluoroborate and potassium hexafluorophosphate;
2)将30-130g PVP粉末溶解于上述溶液中，得到粘稠电解质，所用PVP的分子量介于8000-1300000；在所得粘稠电解质中，PVP所占的百分含量为：在含水型电解质中占45-55％；在非水型电解质中占25-35％；2) Dissolve 30-130g of PVP powder in the above solution to obtain a viscous electrolyte, the molecular weight of the PVP used is between 8000-1300000; in the obtained viscous electrolyte, the percentage of PVP is: in the aqueous electrolyte 45-55%; 25-35% in non-aqueous electrolytes;
3)将所得粘稠电解质涂敷或填充至相应器件中，在室温下蒸发后形成固体电解质。3) Coating or filling the obtained viscous electrolyte into corresponding devices, and forming a solid electrolyte after evaporation at room temperature.
图1a、图1b是使用本发明所制备的固体电解质驱动的小型(长2厘米、宽1.5厘米)电致变色器件着色/漂白的可逆颜色变化，如图所示，从蓝色到无色的可逆颜色转变说明该固体电解质具有良好的电化学性能，同时器件显示出良好的机械性能。Fig. 1a, Fig. 1b are the reversible color changes of coloring/bleaching of small (long 2 centimeters, wide 1.5 centimeters) electrochromic devices driven by the solid electrolyte prepared by the present invention, as shown in the figure, from blue to colorless The reversible color transition demonstrates the good electrochemical performance of the solid electrolyte, while the device exhibits good mechanical properties.
图2a、图2b是使用本发明所制备的固体电解质驱动的大面积(长20厘米、宽18厘米)电致变色器件着色/漂白的可逆颜色变化，如图所示，显示出用于电致变色智能窗的潜力。Fig. 2a, Fig. 2b are the reversible color changes of coloring/bleaching of large area (
图3是使用本发明所制备的固体电解质的电致变色器件着色/漂白过程中电流随时间的变化曲线，如图所示，电流在短时间内从最大到趋于零，说明本发明所制备的固体电解质离子导电率高、该电解质驱动的电致变色器件响应速度快。Fig. 3 is the change curve of electric current with time in the coloring/bleaching process of the electrochromic device using the solid electrolyte prepared by the present invention, as shown in the figure, the electric current tends to zero from the maximum in a short time, illustrating that the present invention prepares The solid electrolyte has high ionic conductivity, and the electrochromic device driven by the electrolyte has a fast response speed.
实施例1：Example 1:
一种聚乙烯吡咯烷酮基固体电解质的制备方法，是由如下步骤完成：A preparation method of polyvinylpyrrolidone-based solid electrolyte is completed by the following steps:
1)将11g氯化钾溶解于100mL去离子水中，得到浓度为1.1mol/L的溶液。1) Dissolve 11 g of potassium chloride in 100 mL of deionized water to obtain a solution with a concentration of 1.1 mol/L.
2)将125g PVP加入上述溶液，在室温或加热下搅拌使其溶解，得到粘稠溶液。2) Add 125g of PVP to the above solution, stir at room temperature or under heating to dissolve it, and obtain a viscous solution.
3)将所得粘稠溶液转移到相应器件中，在室温下蒸发后得到固体电解质。3) The resulting viscous solution was transferred to the corresponding device to obtain a solid electrolyte after evaporation at room temperature.
实施例2Example 2
一种聚乙烯吡咯烷酮基固体电解质的制备方法，是由如下步骤完成：A preparation method of polyvinylpyrrolidone-based solid electrolyte is completed by the following steps:
1)将8g高氯酸锂溶解于100mL去离子水中，得到0.8mol/L的溶液。1) Dissolve 8 g of lithium perchlorate in 100 mL of deionized water to obtain a 0.8 mol/L solution.
2)将95g PVP加入上述溶液，在室温或加热下搅拌使其溶解，得到粘稠溶液。2) Add 95g of PVP to the above solution, stir at room temperature or under heating to dissolve it, and obtain a viscous solution.
3)将所得粘稠溶液转移到相应器件中，在室温下蒸发后得到固体电解质。3) The resulting viscous solution was transferred to the corresponding device to obtain a solid electrolyte after evaporation at room temperature.
实施例3Example 3
一种聚乙烯吡咯烷酮基固体电解质的制备方法，是由如下步骤完成：A preparation method of polyvinylpyrrolidone-based solid electrolyte is completed by the following steps:
1)将4g高氯酸锂溶解于50mL PC中，得到0.7mol/L的溶液。1) Dissolve 4g lithium perchlorate in 50mL PC to obtain a 0.7mol/L solution.
2)将35g PVP加入上述溶液，再加入20mL丙酮，将容器密封后，在室温或加热下搅拌使其溶解，得到粘稠溶液。2) Add 35g of PVP to the above solution, then add 20mL of acetone, seal the container, stir it at room temperature or under heating to dissolve it, and obtain a viscous solution.
3)将所得粘稠溶液转移到相应器件中，在室温下蒸发后得到固体电解质。3) The resulting viscous solution was transferred to the corresponding device to obtain a solid electrolyte after evaporation at room temperature.
实施例4Example 4
一种聚乙烯吡咯烷酮基固体电解质的制备方法，是由如下步骤完成：A preparation method of polyvinylpyrrolidone-based solid electrolyte is completed by the following steps:
1)将7g六氟磷酸钾溶解于50mL PC中，得到0.8mol/L的溶液。1) Dissolve 7g of potassium hexafluorophosphate in 50mL of PC to obtain a 0.8mol/L solution.
2)将35g PVP加入上述溶液，再加入20mL丙酮，将容器密封后，在室温或加热下搅拌，得到粘稠溶液。2) Add 35g of PVP to the above solution, then add 20mL of acetone, seal the container, and stir at room temperature or under heating to obtain a viscous solution.
3)将所得粘稠溶液转移到相应器件中，在室温下蒸发后得到固体电解质。3) The resulting viscous solution was transferred to the corresponding device to obtain a solid electrolyte after evaporation at room temperature.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010184820A CN101859046A (en) | 2010-05-27 | 2010-05-27 | Preparation method of polyvinylpyrrolidone-based solid electrolyte |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010184820A CN101859046A (en) | 2010-05-27 | 2010-05-27 | Preparation method of polyvinylpyrrolidone-based solid electrolyte |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101859046A true CN101859046A (en) | 2010-10-13 |
Family
ID=42945036
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010184820A Pending CN101859046A (en) | 2010-05-27 | 2010-05-27 | Preparation method of polyvinylpyrrolidone-based solid electrolyte |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101859046A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102569702A (en) * | 2012-01-19 | 2012-07-11 | 常州大学 | Ion selective membrane used by non-solid-state electrode and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1426543A (en) * | 2000-12-27 | 2003-06-25 | 索尼公司 | Electrochromic display device and electrodeposition display device |
| CN1624952A (en) * | 2004-09-30 | 2005-06-08 | 浙江大学 | Polymer Template Method for Preparation of Fluoropolymer Separators for Li-ion Batteries |
-
2010
- 2010-05-27 CN CN201010184820A patent/CN101859046A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1426543A (en) * | 2000-12-27 | 2003-06-25 | 索尼公司 | Electrochromic display device and electrodeposition display device |
| CN1624952A (en) * | 2004-09-30 | 2005-06-08 | 浙江大学 | Polymer Template Method for Preparation of Fluoropolymer Separators for Li-ion Batteries |
Non-Patent Citations (4)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库》 20051115 孔旭新 固体核磁共振在一些高分子复合体系结构研究中的应用 A005-56 1-3 , 2 * |
| 《材料导报》 20020415 何秋星等 固体高聚物电解质研究进展 , 第04期 2 * |
| 《电池》 20081225 刘建生等 锂离子电池用P(VDF-HFP)基凝胶聚合物电解质的进展 , 第06期 2 * |
| 《电源技术》 20011027 黄拥理等 聚合物锂离子蓄电池技术与市场 , 第05期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102569702A (en) * | 2012-01-19 | 2012-07-11 | 常州大学 | Ion selective membrane used by non-solid-state electrode and preparation method thereof |
| CN102569702B (en) * | 2012-01-19 | 2015-01-14 | 常州大学 | Ion selective membrane used by non-solid-state electrode and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US12237460B2 (en) | Composite material, preparation method thereof and lithium ion battery | |
| US8765309B2 (en) | Electrochemical device | |
| CN104538670B (en) | A kind of full solid state polymer electrolyte, its preparation method and application | |
| CN109935476A (en) | Amphoteric gel polymer electrolyte with good properties and its preparation and application | |
| CN103500845B (en) | The application of a kind of cross-linked polymer base all solid state electrolyte material and cross linked polyoxyethylene ether | |
| JP6964768B2 (en) | Electrochemical device containing carbon quantum dot ion compound electrolyte | |
| CN106898811A (en) | A kind of solid electrolyte with dual diversion sub-network and preparation method thereof | |
| CN109037686A (en) | Ionomer for aqueous electrode slurry | |
| CN114721197B (en) | High-performance carbon-nitrogen compound/polyoxometallate composite electrochromic device | |
| Zhou et al. | Sulfonic acid-and lithium sulfonate-grafted poly (vinylidene fluoride) electrospun mats as ionic liquid host for electrochromic device and lithium-ion battery | |
| Cai et al. | Polyacrylamide gel electrolyte for high-performance quasi-solid-state electrochromic devices | |
| CN108306046A (en) | A kind of all-solid-state composite polymer electrolyte and preparation method thereof | |
| Lai et al. | A simple low-cost method to prepare gel electrolytes incorporating graphene oxide with increased ionic conductivity and electrochemical stability | |
| CN105826543A (en) | Aluminum-polyaniline secondary battery | |
| Du et al. | Transparent dual ionic (Zn2+-Al3+) hydrogel with high conductivity for self-chargeable Zn//WO3-x electrochromic devices | |
| Zhu et al. | Ionic crosslinked polymer as protective layer in electrochromic supercapacitors for improved electrochemical stability and ion transmission performance | |
| Li et al. | Recent progress in structural modification of polymer gel electrolytes for use in solid-state zinc-ion batteries | |
| Liu et al. | All-natural hydrogel electrolytes prepared by a universal strategy for supercapacitors | |
| Guo et al. | High-performance electrochromic device based on poly acrylamide gel polymer electrolyte containing hypromellose | |
| Wang et al. | Research progress in polymer electrolytes for electrochromic devices | |
| CN111525187A (en) | Sulfonated polyvinyl alcohol solid polymer electrolyte membrane for lithium battery and preparation method thereof | |
| CN101859046A (en) | Preparation method of polyvinylpyrrolidone-based solid electrolyte | |
| Eh et al. | Advances in polymer electrolytes for electrochromic applications | |
| CN117374405A (en) | Double-ion battery based on dimethyl sulfone eutectic electrolyte | |
| CN113737241B (en) | Ionic liquid doped water-soluble polythiophene composite film and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20101013 |