CN104681295B - Method for preparing polymer electrolytes - Google Patents
Method for preparing polymer electrolytes Download PDFInfo
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- CN104681295B CN104681295B CN201510033112.1A CN201510033112A CN104681295B CN 104681295 B CN104681295 B CN 104681295B CN 201510033112 A CN201510033112 A CN 201510033112A CN 104681295 B CN104681295 B CN 104681295B
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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Abstract
A kind of polymer dielectric, it is characterised in that including mixture A, organic solvent B, the I that molar ratio is 1:5~1:102/ KI oxidation-reduction pair, crosslinking agent and plasticizer；The mixture A includes the polyoxyethylene and vinylidene fluoride-hexafluoropropylene copolymer that weight ratio is 1:4~4:1；The organic solvent B includes the propene carbonate and glycol dimethyl ether that volume ratio is 1:8~8:1；The weight of the crosslinking agent is the 25%~125% of mixture A total weight, and the crosslinking agent is the aprotic solvent for the thiocarbamide that concentration is 0.05g/ml~0.10g/ml.In this polymer dielectric; the synergistic effect of plasticizer and crosslinking agent can effectively improve electrolyte ion conductivity; to improve the short circuit current of dye sensitized nano crystal salar battery; and it is coordinated to form protective layer with light anode titanium dioxide; reduce dark reaction reaction ratio; improve open-circuit voltage, the final photoelectric conversion efficiency for improving battery.
Description
Technical field
The present invention relates to a kind of electrolyte more particularly to a kind of polymer dielectrics, and the invention further relates to a kind of polymer
Electrolyte preparation method and its application.
Background technique
Although the dye sensitized nano crystal salar battery based on liquid electrolyte achieves higher photoelectric conversion efficiency,
But liquid electrolyte is easily revealed, volatilizees, and it is difficult to cause the cell sealing assembled, and in long-term practical application under performance
Drop, reduced service life.Through known to a large amount of practical studies: in order to solve the problems, such as that liquid electrolyte exists, solid electricity can be used
Solution matter substitution liquid electrolyte uses gel electrolyte, to develop solid-state or quasi- solid state solar cell.
Have in the selection of material, design and synthesis using high molecular polymer as the quasi-solid electrolyte of matrix flexible
Property, and preparation process is relatively simple, and the dye sensitized nano crystal salar battery assembled can get higher
Photoelectric conversion efficiency.But polymer dielectric ionic conductivity is low, ionic diffusion coefficient is small and contacts between working electrode
Property it is poor, cause to be lower than using the photoelectric conversion efficiency of the dye sensitized nano crystal salar battery of polymer dielectric based on liquid
The dye sensitized nano crystal salar battery of electrolyte.
The raising of short circuit current helps to improve the photoelectric conversion efficiency of dye sensitized nano crystal salar battery, therefore,
The raising of short circuit current is realized by adding auxiliary agent into polymer dielectric at present.
For example, Chinese invention patent " the polymer-modified electrolysis of solar battery of Patent No. ZL201210057963.6
Matter and preparation method and application " (Authorization Notice No. CN102543451B) disclose a kind of polymer-modified electricity of solar battery
Xie Zhi, including polyoxyethylene and the inclined hexafluoropropylene mixture of polytetrafluoroethylene (PTFE), Nano particles of silicon dioxide, oxidation-reduction pair,
Amide and organic solvent.Because the oxygen atom of the amide in the invention easily reacts with the K+ in electrolyte, be conducive to electronics
Transmission, to improve the short circuit current of polymer dielectric, finally can be improved battery efficiency.But the electrostrictive polymer of the invention
After Xie Zhizhong is added to amide, the photoelectric conversion effect of battery cannot be significantly increased in the limitation that short circuit current improves
Rate.
For another example " dye sensitized nano crystal salar battery is quasi- for the Chinese invention patent of Patent No. ZL201210058165.5
Solid electrolyte and its preparation method and application " quasi-solid electrolyte packet disclosed in (Authorization Notice No. CN102543447B)
It includes: polyoxyethylene and the inclined hexafluoropropylene mixture of polytetrafluoroethylene (PTFE), Nano particles of silicon dioxide, oxidation-reduction pair, bis- (trifluoros
Sulfonyloxy methyl imines) lithium and organic solvent.Wherein bis- (trifluoromethanesulp-onyl -onyl imide) lithiums play a part of plasticizer, are conducive to mention
The ionic conductivity of high quasi-solid electrolyte, the final raising for promoting dye sensitized nano crystal salar battery efficiency.But it should
The photoelectric conversion efficiency of battery cannot be equally significantly increased in the limitation that plasticizer improves short circuit current.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of to improve dyestuff simultaneously for the above-mentioned state of the art
The short circuit current of sensitized nanocrystalline solar battery and the polymer dielectric of open-circuit voltage.
Another technical problem to be solved by this invention is to provide a kind of method for preparing polymer electrolytes.
Another technical problem to be solved by this invention is to provide a kind of application of polymer dielectric.
The technical scheme of the invention to solve the technical problem is: a kind of polymer dielectric, including mixture
A, organic solvent B, the I that molar ratio is 1:5~1:102/ KI oxidation-reduction pair, plasticizer and crosslinking agent；
The mixture A includes the polyoxyethylene and vinylidene fluoride-hexafluoropropylene copolymer that weight ratio is 1:4~4:1, institute
The total weight for stating mixture A is the 2%~10% of organic solvent B weight；
The organic solvent B includes the propene carbonate and glycol dimethyl ether that volume ratio is 1:8~8:1；
The I2O in K and polyoxyethylene in/KI oxidation-reduction pair meets, and K/O molar ratio is 0.6~0.8；
The weight of the plasticizer is the 10%~30% of mixture A total weight；
The weight of the crosslinking agent is the 25%~125% of mixture A total weight, and the crosslinking agent is that concentration is 0.05g/
The aprotic solvent of the thiocarbamide of ml~0.10g/ml.
Preferably, the aprotic solvent is 4- tert .-butylpyridine, dimethyl sulfoxide, dimethylformamide, dioxanes, six
One of methyl phosphamide and tetrahydrofuran are a variety of.
As an improvement, the polymer dielectric of above-mentioned technical proposal further includes dehydrated alcohol, the plasticizer and anhydrous second
The proportion of alcohol is 0.02g/ml~0.1g/ml.
Preferably, the plasticizer is Nano particles of silicon dioxide.In polymer dielectric, Nano particles of silicon dioxide
Play a part of solid plasticizer, the ionic conductivity of polymer dielectric can be effectively improved.
A kind of method for preparing polymer electrolytes, includes the following steps:
1. weighing polyoxyethylene and vinylidene fluoride-hexafluoropropylene copolymer, mixing composition mixing by weight 1:4~4:1
Object A, 1:8~8:1 measures propene carbonate and glycol dimethyl ether, mixing composition organic solvent B, by mixture A by volume
It is added into organic solvent B, the total weight of mixture A is the 2%~10% of organic solvent B weight, and 60 DEG C~100 DEG C are lauched
Plasticizer is added until being completely dissolved in bath, and the weight of the plasticizer is the 10%~30% of mixture A total weight, obtains height
Molecule nano mixed liquor；
2. the I that molar ratio is 1:5~1:10 is added into step 1. resulting high molecular nanometer mixed liquor2/ KI oxidation is also
Former electricity is right, obtains polymer electrolyte matrix, the I2O in K and polyoxyethylene in/KI oxidation-reduction pair meets, K/O
Molar ratio is 0.6~0.8；
3. crosslinking agent is added into 2. polymer electrolyte matrix that step obtains, persistently stirs while being stirred continuously
It mixes to being uniformly mixed, obtains the polymer dielectric based on crosslinking agent, the weight of the crosslinking agent is mixture A total weight
25%~125%, the crosslinking agent is the aprotic solvent for the thiocarbamide that concentration is 0.05g/ml~0.10g/ml.
The step 1. in, the plasticizer is first dissolved in dehydrated alcohol, is added to mixture A and organic solvent B
In mixed liquor, the proportion of the plasticizer and dehydrated alcohol is 0.02g/ml~0.1g/ml.
The aprotic solvent is 4- tert .-butylpyridine, dimethyl sulfoxide, dimethylformamide, dioxanes, hempa
One of amide and tetrahydrofuran are a variety of.
Preferably, the plasticizer is Nano particles of silicon dioxide.
The polymer dielectric of above-mentioned technical proposal can be particularly applicable in dye sensitized nano crystal salar battery.
Compared with the prior art, the advantages of the present invention are as follows: after being added to crosslinking agent in polymer dielectric, oxidation is also
Former electricity is to I2/I3 -Big ionic group can be formed by complexation reaction with crosslinking agent, this big ionic group is more advantageous to ion
Transport.In addition, the synergistic effect of plasticizer and crosslinking agent can effectively improve electrolyte ion conductivity, to improve dye sensitization
The short circuit current of nano-crystalline solar battery, and be coordinated to form protective layer with light anode titanium dioxide, reduce dark reaction reaction
Ratio improves open-circuit voltage, the final photoelectric conversion efficiency for improving battery.
In addition, the crosslinking agent in the present invention is the aprotic solvent of thiocarbamide, since thiocarbamide can be formed with iodide ion
Coordination to improve ion transport capacity, and the titanium in the aprotic solvent and titanium dioxide of such as 4- tert .-butylpyridine from
Son forms coordination, to reduce dark reaction ratio, improves open-circuit voltage, and then improve the transfer efficiency of battery.
Specific embodiment
Present invention is further described in detail with reference to embodiments.
Embodiment 1
By weight polyoxyethylene (PEO)/vinylidene fluoride-hexafluoropropylene copolymer (P (VDF- for weighing 0.2g for 2:3
HFP the organic solvent of propene carbonate (PC) and glycol dimethyl ether (DME) that 6g volume ratio is 7:3)) is mixed at 80 DEG C
In, it continues stirring until dissolution completely, 0.02g SiO is then added2Nano particle and dehydrated alcohol, SiO2Nanoparticle with it is anhydrous
Ethanol solution is according to following proportions: 0.02g/ml~0.1g/ml, and continuing heating stirring is uniformly mixed it, obtains high score
Sub- nanometer mixed liquor.Nano particles of silicon dioxide is as high molecular solid plasticizer, the anhydrous second of Nano particles of silicon dioxide
Alcohol is dissolved and is added in mixture.
0.057g I is added into high molecular nanometer mixed liquor2Oxidation-reduction pair is constituted with 0.25g KI, is polymerize
Object electrolyte matrix, I2Molar ratio with KI is I2: the O in KI=1:7, K and PEO meets: K/O molar ratio is 0.8, under room temperature
Stirring 4~8 hours uniform to being blended.
The 4- tert-butyl that 0.05g concentration is 0.05g/ml thiocarbamide is added into polymer electrolyte matrix while agitating
Pyridine solution persistently stirs 12~24 hours.Dye sensitization will be added drop-wise to by the modified quasi-solid electrolyte system of crosslinking agent
On nanometer crystal film, it is horizontally arranged in baking oven and is persistently toasted 1~3 hour in the environment of 70 DEG C, cover platinum to electrode.
In room temperature environment, xenon lamp simulated solar irradiation, light intensity 95.53mW.cm are used-2(light intensity: use silicon photoelectric diode
Calibration) under the conditions of, measuring dye sensitized nano crystal salar battery, (effective illuminating area is 0.16cm2) short circuit current be
12.83mA.cm-2, than the quasi-solid electrolyte solar battery short circuit current for being not added with crosslinking agent of comparative example 1
(12.46mA.cm-2) improve 0.37mA.cm-2；Its open-circuit voltage is 638.2mV, than the not added friendship of comparative example 1
The quasi-solid electrolyte solar energy open-circuit voltage (601.6mV) of connection agent improves 36.6mV；Its photoelectric conversion efficiency is 4.63%,
Quasi-solid electrolyte solar battery efficiency (4.13%) than the not added crosslinking agent of comparative example 1 improves about
0.50%.
Embodiment 2
This embodiment differs from embodiment 1 in that: in oxidation-reduction pair, I2Molar ratio with KI is I2: KI=1:
10, K meet with the O in ethylene oxide: K/O molar ratio is 0.8.
(effective illuminating area is the dye sensitized nano crystal salar battery assembled by the polymer dielectric
0.16cm2) short circuit current be 12.6mA.cm-2, than the quasi-solid electrolyte sun for being not added with crosslinking agent of comparative example 1
It can battery short circuit electric current (12.46mA.cm-2) improve 0.14mA.cm-2；Its open-circuit voltage is 620.8mV, compares comparative example
The quasi-solid electrolyte solar energy open-circuit voltage (601.6mV) of 1 not added crosslinking agent improves 19.2mV；Its photoelectric conversion
Efficiency is 4.59%, than the quasi-solid electrolyte solar battery efficiency (4.13%) for being not added with crosslinking agent of comparative example 1
Improve about 0.46%.
Embodiment 3
This embodiment differs from embodiment 1 in that: 0.10g crosslinking agent is added into polymer electrolyte matrix ---
The 4- tert .-butylpyridine solution of thiocarbamide, concentration 0.05g/ml.
(effective illuminating area is 0.16cm to the dye sensitized nano crystal salar battery assembled by the polymer dielectric2)
Short circuit current be 14.20mA.cm-2, shorter than the quasi-solid electrolyte solar battery for being not added with crosslinking agent of comparative example 1
Road electric current (12.46mA.cm-2) improve 1.74mA.cm-2；Its open-circuit voltage is 650.8mV, than comparative example 1 without
The quasi-solid electrolyte solar energy open-circuit voltage (601.6mV) of addition crosslinking agent improves 49.2mV；Its photoelectric conversion efficiency is
5.02%, the quasi-solid electrolyte solar battery efficiency (4.13%) than the not added crosslinking agent of comparative example 1 improves
About 0.89%.
Embodiment 4
This embodiment differs from embodiment 1 in that: 0.25g crosslinking agent is added into polymer electrolyte matrix ---
The 4- tert .-butylpyridine solution of thiocarbamide, concentration 0.1g/ml.
(effective illuminating area is 0.16cm to the dye sensitized nano crystal salar battery assembled by the polymer dielectric2)
Short circuit current be 13.21mA.cm-2, shorter than the quasi-solid electrolyte solar battery for being not added with crosslinking agent of comparative example 1
Road electric current (12.46mA.cm-2) improve 0.75mA.cm-2；Its open-circuit voltage is 630.5mV, than comparative example 1 without
The quasi-solid electrolyte solar energy open-circuit voltage (601.6mV) of addition crosslinking agent improves 28.9mV；Its photoelectric conversion efficiency is
4.81%, the quasi-solid electrolyte solar battery efficiency (4.13%) than the not added crosslinking agent of comparative example 1 improves
About 0.68%.
Comparative example 1:
By weight be 2:3 weigh 0.2g PEO/P (VDF-HFP) be mixed at 80 DEG C PC that 6g volume ratio is 7:3 with
In the organic solvent of DME, continues stirring until dissolution completely, 0.02g SiO is then added2Nanoparticle and dehydrated alcohol continue
Heating stirring is uniformly mixed it.
0.057g I is added into mixed solution2With 0.25g KI, oxidation-reduction pair, I are constituted2Molar ratio with KI is
I2: the O in KI=1:7, K and ethylene oxide meets: K/O molar ratio is 0.8.It stirs 4~8 hours and is extremely blended uniformly under room temperature.
The quasi-solid electrolyte system for being not added with crosslinking agent is added drop-wise on dye sensitized nano crystal film, baking is horizontally arranged
It is persistently toasted 1~3 hour in the environment of 70 DEG C in case, covers platinum to electrode.
In room temperature environment, xenon lamp simulated solar irradiation, light intensity 95.53mW.cm are used-2(light intensity: use silicon photoelectric diode
Calibration) under the conditions of, measuring dye sensitized nano crystal salar battery, (effective illuminating area is 0.16cm2) short circuit current be
12.46mA.cm-2, open-circuit voltage 601.6Mv, photoelectric conversion efficiency 4.13%.
Comparative example 2
With comparative example 1 the difference is that: crosslinking agent be 0.05g thiocarbamide.
(effective illuminating area is the dye sensitized nano crystal salar battery assembled by the polymer dielectric
0.16cm2) short circuit current be 13.58mA.cm-2, open-circuit voltage 605.8mV, photoelectric conversion efficiency 4.27%.
Comparative example 3
With comparative example 1 the difference is that: crosslinking agent be 0.05g 4- tert .-butylpyridine.
(effective illuminating area is the dye sensitized nano crystal salar battery assembled by the polymer dielectric
0.16cm2) short circuit current be 10.43mA.cm-2, open-circuit voltage 653.3mV, photoelectric conversion efficiency 4.45%.
Shown in the battery performance parameter of above-described embodiment table specific as follows:
By above table this it appears that: the battery efficiency highest of embodiment 3, at this time I2Molar ratio with KI is I2:KI
=1:7, the weight of plasticizer Nano particles of silicon dioxide are 0.02g, crosslinking agent 0.1g, only meet these three simultaneously
Part, can be only achieved the optimal dye sensitized nano crystal salar battery of performance, photoelectric conversion efficiency also highest, it can be seen that,
Above-mentioned three kinds of proportions between component and component are an indivisible entirety, and this is also that crosslinking agent cooperates with work with plasticizer
Result.
4- tert .-butylpyridine in above-described embodiment can also use dimethyl sulfoxide, dimethylformamide, dioxanes, pregnancy
Base phosphamide and tetrahydrofuran substitute, and the trend of presentation is as being same as above table.
Claims (1)
1. a kind of method for preparing polymer electrolytes, it is characterised in that include the following steps:
1. weighing polyoxyethylene and vinylidene fluoride-hexafluoropropylene copolymer by weight 1: 4~4: 1, composition mixture A is mixed,
Measure propene carbonate and glycol dimethyl ether at 1: 8~8: 1 by volume, mixture A is added mixing composition organic solvent B
Into organic solvent B, the total weight of mixture A is the 2%~10% of organic solvent B weight, water-bath at 60 DEG C~100 DEG C, directly
To being completely dissolved, plasticizer is added, the weight of the plasticizer is the 10%~30% of mixture A total weight, obtains macromolecule
Nanometer mixed liquor；
2. the I that molar ratio is 1: 5~1: 10 is added into step 1. resulting high molecular nanometer mixed liquor2/ KI redox electricity
It is right, obtain polymer electrolyte matrix, the I2O in K and polyoxyethylene in/KI oxidation-reduction pair meets, and K/O moles
Than being 0.6~0.8；
3. crosslinking agent is added into 2. polymer electrolyte matrix that step obtains, continues stirring until while being stirred continuously
Be uniformly mixed, obtain the polymer dielectric based on crosslinking agent, the weight of the crosslinking agent be mixture A total weight 25%~
125%, the crosslinking agent is the aprotic solvent for the thiocarbamide that concentration is 0.05g/ml~0.10g/ml；
4. the polymer dielectric based on crosslinking agent is added drop-wise on dye sensitized nano crystal film, it is horizontally arranged in baking oven 70
It is persistently toasted in the environment of DEG C 1~3 hour, covers platinum to electrode；
The aprotic solvent is in dimethyl sulfoxide, dimethylformamide, dioxanes, hexamethyl phosphoramide and tetrahydrofuran
It is one or more；The plasticizer is Nano particles of silicon dioxide.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102800479A (en) * | 2012-08-06 | 2012-11-28 | 宁波大学 | Dye sensitization nanocrystalline solar cell polymer electrolyte as well as preparation method and applications thereof |
| CN103839688A (en) * | 2014-03-05 | 2014-06-04 | 宁波大学 | Polymer electrolyte, preparation method and application |
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- 2015-01-23 CN CN201510033112.1A patent/CN104681295B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102800479A (en) * | 2012-08-06 | 2012-11-28 | 宁波大学 | Dye sensitization nanocrystalline solar cell polymer electrolyte as well as preparation method and applications thereof |
| CN103839688A (en) * | 2014-03-05 | 2014-06-04 | 宁波大学 | Polymer electrolyte, preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| Effect of thiourea incorporation in the electrolyte on the photovoltaic performance of the DSSC sensitized with pyridyl functionalized porphyrin;G.D.Sharma等;《Electrochimica Acta》;20130410;第102卷;第459-465页 * |
| Unusual enhancement of photocurrent by incorporation of Bronsted base thiourea into electrolyte of dye-sensitized solar cell;Mi-Jeong Kim等;《The Journal of Physical Chemistry C》;20101029;第114卷(第46期);全文 * |
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