CN102097212A - Composite polymer gel electrolyte and preparation method thereof - Google Patents
Composite polymer gel electrolyte and preparation method thereof Download PDFInfo
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- CN102097212A CN102097212A CN 201110005424 CN201110005424A CN102097212A CN 102097212 A CN102097212 A CN 102097212A CN 201110005424 CN201110005424 CN 201110005424 CN 201110005424 A CN201110005424 A CN 201110005424A CN 102097212 A CN102097212 A CN 102097212A
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Abstract
The invention relates to composite polymer gel electrolyte and a preparation method thereof, which belong to the technical field of electrolyte for supercapacitors in energy materials. The composite polymer gel electrolyte is characterized by containing a composite compound, wherein the composite compound at least consists of polyvinyl alcohol and a titanium-containing compound; and the electrolyte also contains a non-aqueous polar organic compound solvent and a compound ionizable in the solvent. The electrolyte can be obtained by the method comprising the following steps of: dissolving the polyvinyl alcohol and the ionizable compound in the mixed solution of raw materials, and standing the mixed solution of the raw materials until gel is formed, wherein the polyvinyl alcohol, the titanium-containing compound, the non-aqueous polar organic solvent and the compound ionizable in the solvent coexist in the mixed solution of the raw materials. The electrolyte preparation method provided by the invention is simple and easy; and the prepared electrolyte has the high conductivity of 9.4*10<-3> S/cm and relatively stronger mechanical strength, and is difficult to damage in manufacturing and use, free of leakage, safe and reliable.
Description
Technical field
The present invention relates to a kind of polymer composition polymer gel electrolyte and preparation method thereof, belong to the electrolytical technical field of ultracapacitor in the energy and material.
Background technology
Capacitor is a kind of electric energy storing device.The basic principle of general electric capacity is: utilize two parallel and battery lead plate store charges that separate with dielectric, with electrical power storage among the electric field between pole plate.The pass of its capacitance C and voltage U and electric weight Q is:
And electrical power storage amount E is:
The maximum that can find the capacitor stores energy thus is:
The conclusion that can be drawn by following formula is: improve the electrical power storage amount of capacitor, need to improve its capacitance C and can bear maximum voltage U
Max
The influencing factor of the capacitance of general capacitor can be by following formulate:
ε is a medium dielectric constant between pole plate in the formula, S be pole plate over against area, k is the electrostatic force constant, and d is a polar plate spacing.
Can find that the method that improves capacitance has: increase pole plate area S, reduce polar plate spacing d, and the medium that between pole plate, uses high-k ε.But the capacitance of general capacitor is very low.This only just can reflect from the unit of weighing its capacitance, the international standard of capacitance (SI system) unit is faraday (F), 1F is equivalent to can store the electric weight of 1 coulomb (C) under the internal electrical potential difference of 1 volt (V), and the unit that is used to weigh the ordinary capacitor capacitance is μ F (10
-6F) and pF (10
-12F), this efficiency far for energy storage is not enough.And the capacitance of ultracapacitor (Supercapacitor) can directly use F to weigh as unit, and this just makes capacitor really have energy storage capacity that can be comparable with battery.
Electric double layer type ultracapacitor (Electric Double-Layer Capacitor, design EDLC) is different from general capacitor, and it is made up of electrolyte between two pole plates and pole plate and barrier film (solid electrolyte does not then need barrier film).If from the superficial phenomenon analysis, ultracapacitor only is that the dielectric between two pole plates is changed to electrolyte.But actual difference is more complicated.If wish from ultracapacitor, to seek and seek counter element with ordinary capacitor, actual lastblock ultracapacitor is to adopt electrolyte solution to be in series by two ordinary capacitor, and these two ordinary capacitor all are to be covered in the film that its surperficial electrolyte ion forms by a common pole plate and one deck to constitute, and this structure is called as electric double layer (Electric Double-Layer).According to the electric double layer theory of stem electric double layer model and renewal, form between the bilayer " electrode " of capacitor and separate, or the solvent molecule that is adsorbed on electrode surface is separated mutually with repulsion effect between molecule (ion).If contrast ordinary capacitor capacitance formula, its polar plate spacing d only is in same order with molecule (ion) size, this also just this type of ultracapacitor have one of reason far above the capacitance of other types capacitor.And on the other hand, the electrode material that this type of ultracapacitor uses generally has the complex surfaces structure, and specific area can reach 1000～2000m
2/ g, this just makes that also the S in the capacitance influencing factor also is greatly improved, and has improved capacitance from another angle.
The electrical power storage principle of oxidation-reduction type ultracapacitor then has bigger difference, in fact its principle is more similar to battery, the redox reaction that is to use electrode material and electrolyte to take place is converted into chemical energy with electric energy and stores, so this type of capacitor be otherwise known as dummy capacitor or fake capacitance device (pseudocapacitor).
Two class ultracapacitors all have very high capacitance C, but its U
MaxOrdinary capacitor has been subjected to bigger restriction relatively, for ordinary capacitor, its operating voltage only is subjected to the influence of dielectric breakdown voltage, generally be at least hundreds of volts, and have electrolyte in the ultracapacitor, if electrolyte is the aqueous solution, because of the water decomposition voltage limit, it can tolerate ceiling voltage only for about 1V, and if use nonaqueous solvents, also only decomposition voltage can be brought up to about 3V.Improve the capacitor working voltage, can only connect a plurality of capacitors, but capacitance even less than the capacitance of single electric capacity after the capacitors in series, and formula is:
This depresses the electric weight that can store even is lower than monolithic capacitor after showing capacitors in series outside identical, be undoubtedly the huge restriction for capacitor function.Therefore, the electrolyte of research and development high de-agglomeration voltage is made the more monolithic capacitor of high working voltage thus, is the important content in the capacitor research.
In addition, from the principle analysis actual inner conductive that is used to ultracapacitor of electrolyte as can be seen, so its conductivity becomes the key factor that influences capacitor performance.The electrolyte of low conductivity will consume more electric energy in discharging and recharging, and will reduce capacitor charging/discharging speed.This makes electrolytic conductivity become the important indicator in the research.
Electrolytical fail safe also is a big factor that influences the ultracapacitor performance.For improving the electrolyte withstand voltage, a lot of ultracapacitors have used nonaqueous solvents as electrolyte solvent, and the electrolyte ion type is also more and more, and these materials have toxicity mostly, in case leak the heavy damage environment.Also just therefore, the research and development with solid electrolyte of better mechanical stability become an important content in the ultracapacitor research.
The capacitance of electric double layer type ultracapacitor (EDLC) is not ideal enough, an important reasons is that electrolyte is not good for the wet face state of electrode surface, this just can explain from aforementioned EDLC principle: the electrical power storage of this type of capacitor relies on extremely low polar plate spacing d, but if electrolyte can not directly contact with electrode surface, low polar plate spacing just is in no position to take possession of, and the carbon electrode that EDLC uses has the complex surfaces structure, and this has strengthened the infiltration difficulty.This problem obviously will become even more serious when using solid electrolyte.
Comprehensive above the analysis, high de-agglomeration voltage, high conductivity, high mechanical stability and the electrolyte that can better soak into electrode surface are the targets that the ultracapacitor research staff seeks.Therefore polymer dielectric becomes an important research direction.
The preparation method of gel-form solid polymer electrolyte adds the salting liquid of a large amount of organic solvent dissolutions and liquid plasticizer in the polymeric matrix, forms the stable gel with polymer body structure.It has fully improved conductivity, but has reduced the mechanical strength of film, and makes electrolyte increase the corrosion activity of metal electrode.And composite polymer electrolyte (Compositepolymer electrolyte, CPE) be the compound electrolyte system of a kind of two-phase, it is that inorganic (pottery)/organic filler Dispersion of Particles of a small amount of micrometer/nanometer size is made in conventional solid polymer electrolyte.Common so electrolytical conductivity, mechanical performance and the interfacial activity of can making improved fully.And the size of filler and corresponding specific area just become the key influence factor of electrolyte performance.This class electrolyte has been subjected to extensive concern because of its performance of being optimized and with the correlation of nano science research.
(Sampath S, the Choudhury N A such as Sampath of Indian Inst Scient in 2009; Shukla A K.Journal ofChemical Sciences, 2009,121 (5): 727-734.) studied the electrolytical ultracapacitor of use polyvinyl alcohol (PVA) aqueous gel.And 2010, (Chatterjee J, Liu T, Wang B, etal.SolidState Ion., 2010,181 (11-12): 531-535.) studied PVA, LiCF such as Chatterjee of U.S. high performance material research institute
3SO
3With organic solvent N-N-methyl-2-2-pyrrolidone N-(n-methyl-2-pyrrolidone, NMP) the organogel electrolyte of Zu Chenging.But still find no the report that closes PVA base composite polymer electrolyte and preparation method thereof at present both at home and abroad.
Summary of the invention
The invention provides a kind of PVA-based composite polymer electrolyte and manufacture method thereof.
This electrolytical being characterised in that is contained complex chemical compound, and described complex chemical compound is a constituent with polyvinyl alcohol and titanium-containing compound at least, and contains non-aqueous polar organic compound solvent and ionogenic compound in this solvent.This electrolyte can obtain by the following method: polyvinyl alcohol, titanium-containing compound, non-aqueous polar organic solvent are arranged and in this solvent in the raw material mixed liquor of ionogenic compound in coexistence, after making the dissolving of polyvinyl alcohol and ionizable compound, the raw material mixed liquor left standstill until gel form.
In actual manufacture process, electrolytical manufacturing has following raw material to choose and processing mode:
1, at first prepares a kind of raw material mixed liquor, use non-aqueous polar organic solvent, wherein the polyvinyl alcohol quality accounts for 5～20% of mixed liquor gross mass, cation in the ionizable compound is 1: 2～1: 10 with the amount of substance of vinyl alcohol units ratio, titanium-containing compound accounts for 0.3～10% of mixed liquor gross mass, then by the raw material mixed liquor being heated to 100～180 ℃ and stirring, after making the dissolving of polyvinyl alcohol and ionizable compound, the raw material mixed liquor is left standstill, or the raw material mixed liquor carried out curtain coating on glass plate, leave standstill again until gel afterwards and form;
2, non-aqueous polar organic solvent can be N-methyl pyrrolidone or N, dinethylformamide, ionizable compound can be salt or the quaternary ammonium salt that contains alkali metal ion or ammonium radical ion, titanium-containing compound can be titanium dioxide or titanium dioxide hydrates, this titanium-containing compound obtains by the following method: the aqueous solution that contains titania powder and hydroxide ion is heated to 110～200 ℃ under enclosed environment, keep neutralization after 12～48 hours, filter out titanium-containing compound solid wherein and it is carried out drying, the titanium-containing compound characteristics of this method preparation are to form the tubulose or the wire pattern of certain radius and length, can improve electrolytical mechanical strength with this as inorganic compound particles;
The present invention is with respect to the advantage of traditional liquid electrolyte system, can not produce liquid and leak, need not to use barrier film, simplify processing step, and the capacitor impact of making vibrations tolerance is strong, can be because of the fluctuation of vibrations generation capacity or voltage.And, electrolyte manufacture method provided by the invention is simple, the electrolyte of making can either keep not the high conductivity of plural gel can have again enough mechanical strengths with guarantee its in manufacture process, the capacitor assembling and use in breakage does not take place, safe and reliable.For example, the electrolytic conductivity of making by embodiment 3 can reach 9.4 * 10
-3S/cm, and with respect to not compound PVA base gel electrolyte, mechanical strength has obtained significant raising.
Embodiment
PVA-based composite polymer electrolyte provided by the invention and manufacture method thereof are as described in the summary of the invention part.The present invention will further illustrate substantive distinguishing features of the present invention and marked improvement by the description of following embodiment, and still, the present invention only is confined to following embodiment.
In concrete enforcement, titanium-containing compound can obtain by the following method:
I, directly buy commercially available titanium dioxide, grind, cross behind 300 mesh sieves dry;
II, the solidliquid mixture to the titania powder of the aqueous solution that contains 10.5mol/L KOH and mass fraction 6% under enclosed environment are heated to 110 ℃, keep neutralization after 12 hours, filter out titanium-containing compound solid wherein and it is carried out drying;
III, the solidliquid mixture to the titania powder of the aqueous solution that contains 10mol/L NaOH and mass fraction 4% under enclosed environment are heated to 180 ℃, keep neutralization after 48 hours, filter out titanium-containing compound solid wherein and it is carried out drying;
IV, the solidliquid mixture to the titania powder of the aqueous solution that contains 9mol/L NaOH and mass fraction 5% under enclosed environment are heated to 200 ℃, keep neutralization after 48 hours, filter out titanium-containing compound solid wherein and it is carried out drying;
Prepare on the basis practicable following examples at above raw material:
Embodiment 1
The polyvinyl alcohol that gross mass of accounting for 5% is arranged in coexistence, 0.3% titanium-containing compound I, the amount of substance ratio of lithium ion amount of substance and vinyl alcohol units is 1: 2 a trifluoromethanesulfonic acid lithium, and remainder is N, in the raw material mixed liquor of dinethylformamide as solvent, by mixed liquor being heated to 100 ℃ and kept two hours, make the dissolving of polyvinyl alcohol and trifluoromethanesulfonic acid lithium after, pour the raw material mixed liquor into culture dish, under dry environment, leave standstill afterwards and form until gel.
Embodiment 2
The polyvinyl alcohol that gross mass of accounting for 15% is arranged in coexistence, 3% titanium-containing compound II, the amount of substance ratio of lithium ion amount of substance and vinyl alcohol units is 1: 3 a lithium perchlorate, and remainder is in the raw material mixed liquor of N-N-methyl-2-2-pyrrolidone N-as solvent, by mixed liquor being heated to 180 ℃ and kept one hour, after making the dissolving of polyvinyl alcohol and lithium perchlorate, the raw material mixed liquor is carried out curtain coating at smooth glass surface, under dry environment, leave standstill afterwards and form until gel.
Embodiment 3
The polyvinyl alcohol that gross mass of accounting for 15% is arranged in coexistence, 3% titanium-containing compound III, the amount of substance ratio of lithium ion amount of substance and vinyl alcohol units is 1: 5 a lithium perchlorate, and remainder is in the raw material mixed liquor of N-N-methyl-2-2-pyrrolidone N-as solvent, by mixed liquor being heated to 150 ℃ and kept one hour, after making the dissolving of polyvinyl alcohol and lithium perchlorate, the raw material mixed liquor is carried out curtain coating at smooth glass surface, under dry environment, leave standstill afterwards and form until gel.
Embodiment 4
The polyvinyl alcohol that gross mass of accounting for 20% is arranged in coexistence, 10% titanium-containing compound IV, the amount of substance ratio of tetraethyl ammonium radical ion amount of substance and vinyl alcohol units is 1: 16 a tetraethylammonium tetrafluoroborate, and remainder is in the raw material mixed liquor of N-N-methyl-2-2-pyrrolidone N-as solvent, by mixed liquor being heated to 120 ℃ and kept two hours, after making the dissolving of polyvinyl alcohol and tetraethylammonium tetrafluoroborate, the raw material mixed liquor is carried out curtain coating at smooth glass surface, under dry environment, leave standstill afterwards and form until gel.
From above-mentioned all embodiment as can be seen, as long as use listed raw material in the claim, and various parameters in the assurance preparation process, as polyvinyl alcohol, titanium-containing compound, non-aqueous polar organic solvent and in this solvent the proportioning of ionogenic compound in the listed scope of claim, can produce effective electrolyte finished product.In concrete implementation process, those skilled in the art can both carry out concrete enforcement according to the prescribed limit of each technological parameter, does not exceed with the given the foregoing description of the present invention.
By above-mentioned specific embodiment the present invention is described in detail, those skilled in the art are to be understood that, in the scope that does not exceed spirit of the present invention and essence, certain modification and distortion to the present invention makes still can realize result of the present invention.
Claims (6)
1. gel-form solid polymer electrolyte, it is characterized in that, contain complex chemical compound, described complex chemical compound is a constituent with polyvinyl alcohol and titanium-containing compound at least, and contains non-aqueous polar organic compound solvent and ionogenic compound in this solvent.
2. gel-form solid polymer electrolyte, it is characterized in that, described complex chemical compound obtains by the following method: polyvinyl alcohol, titanium-containing compound, non-aqueous polar organic solvent are arranged and in this solvent in the raw material mixed liquor of ionogenic compound in coexistence, after making the dissolving of polyvinyl alcohol and ionizable compound, the raw material mixed liquor left standstill until gel form.
3. gel-form solid polymer electrolyte as claimed in claim 2, it is characterized in that, by the raw material mixed liquor being heated to 100～180 ℃ and stirring, make the dissolving of polyvinyl alcohol and ionizable compound, in the raw material mixed liquor, the polyvinyl alcohol quality accounts for 5～20% of gross mass, and the cation in the ionizable compound is 1: 2～1: 16 with the amount of substance of vinyl alcohol units ratio, and the titanium-containing compound quality accounts for 0.3～10% of electrolyte gross mass.
4. as claim 2 or 3 described gel-form solid polymer electrolytes, wherein, non-aqueous polar organic solvent is N-methyl pyrrolidone or N, dinethylformamide, ionizable compound is salt or the quaternary ammonium salt that contains alkali metal ion or ammonium radical ion, titanium-containing compound is titanium dioxide or titanium dioxide hydrates, this titanium-containing compound obtains by the following method: the aqueous solution that contains titania powder and hydroxide ion is heated to 110～200 ℃ under enclosed environment, keep after 12～48 hours neutralization, filter out titanium-containing compound solid wherein and it is carried out drying.
5. the manufacture method of a gel-form solid polymer electrolyte, it is characterized in that, polyvinyl alcohol, titanium-containing compound, non-aqueous polar organic solvent are arranged and in this solvent in the raw material mixed liquor of ionogenic compound in coexistence, after making the dissolving of polyvinyl alcohol and ionizable compound, the raw material mixed liquor left standstill until gel form.
6. the manufacture method of a kind of gel-form solid polymer electrolyte as claimed in claim 5, it is characterized in that, the polyvinyl alcohol quality accounts for 5～20% of mixed liquor gross mass in the raw material mixed liquor, cation in the ionizable compound is 1: 2～1: 10 with the amount of substance of vinyl alcohol units ratio, and titanium-containing compound accounts for 0.3～10% of mixed liquor gross mass, then by the raw material mixed liquor being heated to 100～180 ℃ and stirring, after making the dissolving of polyvinyl alcohol and ionizable compound, the raw material mixed liquor is left standstill, or the raw material mixed liquor carried out curtain coating on glass plate, leave standstill again until gel afterwards and form.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102354620A (en) * | 2011-10-25 | 2012-02-15 | 中国科学院过程工程研究所 | All-solid-state supercapacitor and manufacturing method thereof |
| CN110211808A (en) * | 2019-05-16 | 2019-09-06 | 湖南艾华集团股份有限公司 | A kind of aluminium electrolutic capacitor of vibrationproof and preparation method thereof |
| CN115410836A (en) * | 2022-08-26 | 2022-11-29 | 华南理工大学 | Integrally-formed hydrogel solid-state supercapacitor and preparation method thereof |
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| CA2367290A1 (en) * | 2002-01-16 | 2003-07-16 | Hydro Quebec | High stability polymer electrolyte > 4 volts as electrolyte for a hybrid supercondenser and electrochemical generator |
| CN101350253A (en) * | 2008-09-17 | 2009-01-21 | 中国振华（集团）新云电子元器件有限责任公司 | Solid electrolyte capacitor with ultra-low equivalent series resistance and manufacturing method thereof |
| JP2009283748A (en) * | 2008-05-23 | 2009-12-03 | I Cast:Kk | Low-impedance loss line |
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2011
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| CA2367290A1 (en) * | 2002-01-16 | 2003-07-16 | Hydro Quebec | High stability polymer electrolyte > 4 volts as electrolyte for a hybrid supercondenser and electrochemical generator |
| JP2009283748A (en) * | 2008-05-23 | 2009-12-03 | I Cast:Kk | Low-impedance loss line |
| CN101350253A (en) * | 2008-09-17 | 2009-01-21 | 中国振华（集团）新云电子元器件有限责任公司 | Solid electrolyte capacitor with ultra-low equivalent series resistance and manufacturing method thereof |
Non-Patent Citations (1)
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102354620A (en) * | 2011-10-25 | 2012-02-15 | 中国科学院过程工程研究所 | All-solid-state supercapacitor and manufacturing method thereof |
| CN102354620B (en) * | 2011-10-25 | 2014-06-04 | 中国科学院过程工程研究所 | All-solid-state supercapacitor and manufacturing method thereof |
| CN110211808A (en) * | 2019-05-16 | 2019-09-06 | 湖南艾华集团股份有限公司 | A kind of aluminium electrolutic capacitor of vibrationproof and preparation method thereof |
| CN115410836A (en) * | 2022-08-26 | 2022-11-29 | 华南理工大学 | Integrally-formed hydrogel solid-state supercapacitor and preparation method thereof |
| CN115410836B (en) * | 2022-08-26 | 2023-09-08 | 华南理工大学 | Integrally formed hydrogel solid super capacitor and preparation method thereof |
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