CN104681295A - Polymer electrolyte and preparation method and application thereof - Google Patents
Polymer electrolyte and preparation method and application thereof Download PDFInfo
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- CN104681295A CN104681295A CN201510033112.1A CN201510033112A CN104681295A CN 104681295 A CN104681295 A CN 104681295A CN 201510033112 A CN201510033112 A CN 201510033112A CN 104681295 A CN104681295 A CN 104681295A
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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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- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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Abstract
The invention discloses polymer electrolyte which is characterized by comprising a mixture A, an organic solvent B, an I2/KI redox couple with the mole ratio of 1: 5-1: 10, a crosslinking agent and a plasticizer, wherein the mixture A comprises polyoxyethylene and a vinylidene fluoride-hexafluoropropylene copolymer according to the weight ratio of 1: 4-4: 1; the organic solvent B comprises propylene carbonate and glycol dimethyl ether according to the volume ratio of 1: 8-8: 1; the weight of the crosslinking agent is 25-125 percent of the total weight of the mixture A; the crosslinking agent is an aprotic solvent solution of thiocarbamide with the concentration of 0.05g/ml-0.10g/ml. According to the polymer electrolyte, under the synergistic effect of the plasticizer and the crosslinking agent, the ionic conductivity of the electrolyte can be effectively improved, so that a short circuit of a dye-sensitized nanocrystalline solar cell is enhanced, and a protection layer is formed by a photo-anode titanium dioxide ligand; therefore, the reaction proportion of dark reaction is reduced, open circuit voltage is increased, and the photoelectric conversion efficiency of the cell is finally improved.
Description
Technical field
The present invention relates to a kind of electrolyte, particularly relate to a kind of polymer dielectric, the invention still further relates to a kind of method for preparing polymer electrolytes and application thereof.
Background technology
Although the dye sensitized nano crystal salar battery based on liquid electrolyte achieves higher photoelectric conversion efficiency, but liquid electrolyte is easily revealed, volatilize, cause assemble cell sealing difficulty, and in long-term practical application hydraulic performance decline, useful life shorten.Known through a large amount of practical study: in order to solve liquid electrolyte Problems existing, can liquid electrolyte be substituted with solid electrolyte or adopt gel electrolyte, thus develop solid-state or accurate solid state solar cell.
Take high molecular polymer as the selection of quasi-solid electrolyte at material of matrix, design and synthesis have flexibility, and preparation technology is relatively simple, its dye sensitized nano crystal salar battery assembled can obtain higher photoelectric conversion efficiency.But polymer dielectric ionic conductivity is low, ionic diffusion coefficient is little and poor with work electrode Contact, cause the photoelectric conversion efficiency of the dye sensitized nano crystal salar battery adopting polymer dielectric lower than the dye sensitized nano crystal salar battery based on liquid electrolyte.
The raising of short circuit current contributes to the photoelectric conversion efficiency improving dye sensitized nano crystal salar battery, therefore, at present by adding the raising that auxiliary agent achieves short circuit current in polymer dielectric.
Such as, the patent No. is that the Chinese invention patent " solar cell modified polymer electrolyte and preparation method and application " (Authorization Notice No. is CN102543451B) of ZL201210057963.6 discloses a kind of solar cell modified polymer electrolyte, comprises polyoxyethylene and the inclined hexafluoropropylene mixture of polytetrafluoroethylene, Nano particles of silicon dioxide, oxidation-reduction pair, acid amides and organic solvent.Because the K+ of oxygen atom easily and in electrolyte of the acid amides in this invention reacts, be conducive to the transmission of electronics, thus improve the short circuit current of polymer dielectric, finally can improve battery efficiency.But after with the addition of acid amides in the polymer dielectric of this invention, the limitation that its short circuit current improves, can not improve the photoelectric conversion efficiency of battery significantly.
And for example the patent No. is that the disclosed quasi-solid electrolyte of Chinese invention patent " dye sensitized nano crystal salar battery quasi-solid electrolyte and its preparation method and application " (Authorization Notice No. is CN102543447B) of ZL201210058165.5 comprises: polyoxyethylene and the inclined hexafluoropropylene mixture of polytetrafluoroethylene, Nano particles of silicon dioxide, oxidation-reduction pair, two (trifluoromethanesulp-onyl-onyl imide) lithium and organic solvent.Wherein two (trifluoromethanesulp-onyl-onyl imide) lithium plays a part plasticizer, is conducive to the ionic conductivity improving quasi-solid electrolyte, the final raising promoting dye sensitized nano crystal salar battery efficiency.But the limitation that this plasticizer improves short circuit current, can not improve the photoelectric conversion efficiency of battery equally significantly.
Summary of the invention
Simultaneously technical problem to be solved by this invention provides a kind of for the above-mentioned state of the art to improve the short circuit current of dye sensitized nano crystal salar 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 present invention solves the problems of the technologies described above adopted technical scheme: a kind of polymer dielectric, comprises mixture A, organic solvent B, mol ratio be the I of 1:5 ~ 1:10
2/ KI oxidation-reduction pair, plasticizer and crosslinking agent;
Described mixture A comprises the polyoxyethylene and vinylidene fluoride-hexafluoropropylene copolymer that weight ratio is 1:4 ~ 4:1, and the total weight of described mixture A is 2% ~ 10% of organic solvent B weight;
Described organic solvent B comprises the propene carbonate and glycol dimethyl ether that volume ratio is 1:8 ~ 8:1;
Described I
2k in/KI oxidation-reduction pair and the O in polyoxyethylene meets, and K/O mol ratio is 0.6 ~ 0.8;
The weight of described plasticizer is 10% ~ 30% of mixture A total weight;
The weight of described crosslinking agent is 25% ~ 125% of mixture A total weight, the aprotic solvent of described crosslinking agent to be concentration the be thiocarbamide of 0.05g/ml ~ 0.10g/ml.
Preferably, described aprotic solvent is one or more in 4-tert .-butylpyridine, dimethyl sulfoxide (DMSO), dimethyl formamide, dioxanes, hexamethyl phosphoramide and oxolane.
As improvement, the polymer dielectric of technique scheme also comprises absolute ethyl alcohol, and the proportioning of described plasticizer and absolute ethyl alcohol is 0.02g/ml ~ 0.1g/ml.
Preferably, described plasticizer is Nano particles of silicon dioxide.In polymer dielectric, Nano particles of silicon dioxide plays a part solid plasticizer, effectively can improve the ionic conductivity of polymer dielectric.
A kind of method for preparing polymer electrolytes, comprises the steps:
1. polyoxyethylene and vinylidene fluoride-hexafluoropropylene copolymer is taken by weight 1:4 ~ 4:1, mixing composition mixture A, 1:8 ~ 8:1 measures propene carbonate and glycol dimethyl ether by volume, mixing composition organic solvent B, mixture A is added in organic solvent B, the total weight of mixture A is 2% ~ 10% of organic solvent B weight, water-bath at 60 DEG C ~ 100 DEG C, until dissolve completely, add plasticizer, the weight of described plasticizer is 10% ~ 30% of mixture A total weight, obtains high molecular nanometer mixed liquor;
2. in the high molecular nanometer mixed liquor of step 1. gained, the I that mol ratio is 1:5 ~ 1:10 is added
2/ KI oxidation-reduction pair, obtains polymer electrolyte matrix, described I
2k in/KI oxidation-reduction pair and the O in polyoxyethylene meets, and K/O mol ratio is 0.6 ~ 0.8;
3. while constantly stirring, crosslinking agent is added in the polymer electrolyte matrix that 2. step obtains, continue stirring until and mix, obtain the polymer dielectric based on crosslinking agent, the weight of described crosslinking agent is 25% ~ 125% of mixture A total weight, the aprotic solvent of described crosslinking agent to be concentration the be thiocarbamide of 0.05g/ml ~ 0.10g/ml.
Described step 1. in, described plasticizer is first dissolved in absolute ethyl alcohol, then is added in the mixed liquor of mixture A and organic solvent B, and the proportioning of described plasticizer and absolute ethyl alcohol is 0.02g/ml ~ 0.1g/ml.
Described aprotic solvent is one or more in 4-tert .-butylpyridine, dimethyl sulfoxide (DMSO), dimethyl formamide, dioxanes, hexamethyl phosphoramide and oxolane.
Preferably, described plasticizer is Nano particles of silicon dioxide.
The polymer dielectric of technique scheme can be particularly applicable in dye sensitized nano crystal salar battery.
Compared with prior art, the invention has the advantages that: after with the addition of crosslinking agent in polymer dielectric, oxidation-reduction pair I
2/ I
3 -can form heavy ion group with crosslinking agent by complexation reaction, this heavy ion group is more conducive to ion transportation.In addition; the synergy of plasticizer and crosslinking agent can effectively improve electrolyte ion conductivity; thus improve the short circuit current of dye sensitized nano crystal salar battery; and form protective layer with the coordination of light anode titanium dioxide; reduce dark reaction reaction ratio; improve open circuit voltage, the final photoelectric conversion efficiency improving battery.
In addition, crosslinking agent in the present invention is the aprotic solvent of thiocarbamide, because thiocarbamide can form coordination to improve ion transportation ability with iodide ion, and the titanium ion in the aprotic solvent of such as 4-tert .-butylpyridine and titanium dioxide forms coordination, thus reduce dark reaction ratio, improve open circuit voltage, and then improve the conversion efficiency of battery.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
By weight polyoxyethylene (the PEO)/vinylidene fluoride-hexafluoropropylene copolymer (P (VDF-HFP)) taking 0.2g for 2:3 in 80 DEG C of organic solvents being mixed in propene carbonate (PC) that 6g volume ratio is 7:3 and glycol dimethyl ether (DME), continue stirring until and dissolve completely, then add 0.02g SiO
2nano particle and absolute ethyl alcohol, SiO
2nano particle and ethanol solution, according to following proportions: 0.02g/ml ~ 0.1g/ml, continue to add thermal agitation and make it mix, obtain high molecular nanometer mixed liquor.Nano particles of silicon dioxide is as high molecular solid plasticizer, and Nano particles of silicon dioxide anhydrous alcohol solution also joins in mixture.
0.057g I is added in high molecular nanometer mixed liquor
2form oxidation-reduction pair with 0.25g KI, obtain polymer electrolyte matrix, I
2be I with the mol ratio of KI
2: the O in KI=1:7, K and PEO meets: K/O mol ratio is 0.8, and under normal temperature, stirring 4 ~ 8 is little of evenly blended.
In polymer electrolyte matrix, the 4-tert .-butylpyridine solution that 0.05g concentration is 0.05g/ml thiocarbamide is added, Keep agitation 12 ~ 24 hours while stirring.Quasi-solid electrolyte system through crosslinking agent modification is added drop-wise on dye sensitized nano crystal film, under the environment of 70 DEG C, continues baking 1 ~ 3 hour in horizontal positioned to baking oven, cover platinum to electrode.
At room temperature environment, use xenon lamp simulated solar irradiation, light intensity is 95.53mW.cm
-2under (light intensity: use silicon photoelectric diode to demarcate) condition, (effective illuminating area is 0.16cm to record dye sensitized nano crystal salar battery
2) short circuit current be 12.83mA.cm
-2, than the quasi-solid electrolyte solar cell short circuit current (12.46mA.cm not adding crosslinking agent of comparative example 1
-2) improve 0.37mA.cm
-2; Its open circuit voltage is 638.2mV, improves 36.6mV than the quasi-solid electrolyte solar energy open circuit voltage (601.6mV) without interpolation crosslinking agent of comparative example 1; Its photoelectric conversion efficiency is 4.63%, improves about 0.50% than the quasi-solid electrolyte solar battery efficiency (4.13%) without interpolation crosslinking agent of comparative example 1.
Embodiment 2
The present embodiment difference from Example 1 is: in oxidation-reduction pair, I
2be I with the mol ratio of KI
2: the O in KI=1:10, K and ethylene oxide meets: K/O mol ratio is 0.8.
(effective illuminating area is 0.16cm to the dye sensitized nano crystal salar battery assembled by this polymer dielectric
2) short circuit current be 12.6mA.cm
-2, than the quasi-solid electrolyte solar cell short circuit current (12.46mA.cm not adding crosslinking agent of comparative example 1
-2) improve 0.14mA.cm
-2; Its open circuit voltage is 620.8mV, improves 19.2mV than the quasi-solid electrolyte solar energy open circuit voltage (601.6mV) without interpolation crosslinking agent of comparative example 1; Its photoelectric conversion efficiency is 4.59%, improves about 0.46% than the quasi-solid electrolyte solar battery efficiency (4.13%) not adding crosslinking agent of comparative example 1.
Embodiment 3
The present embodiment difference from Example 1 is: in polymer electrolyte matrix, add 0.10g crosslinking agent---the 4-tert .-butylpyridine solution of thiocarbamide, concentration is 0.05g/ml.
(effective illuminating area is 0.16cm to the dye sensitized nano crystal salar battery assembled by this polymer dielectric
2) short circuit current be 14.20mA.cm
-2, than the quasi-solid electrolyte solar cell short circuit current (12.46mA.cm not adding crosslinking agent of comparative example 1
-2) improve 1.74mA.cm
-2; Its open circuit voltage is 650.8mV, improves 49.2mV than the quasi-solid electrolyte solar energy open circuit voltage (601.6mV) without interpolation crosslinking agent of comparative example 1; Its photoelectric conversion efficiency is 5.02%, improves about 0.89% than the quasi-solid electrolyte solar battery efficiency (4.13%) without interpolation crosslinking agent of comparative example 1.
Embodiment 4
The present embodiment difference from Example 1 is: in polymer electrolyte matrix, add 0.25g crosslinking agent---the 4-tert .-butylpyridine solution of thiocarbamide, concentration is 0.1g/ml.
(effective illuminating area is 0.16cm to the dye sensitized nano crystal salar battery assembled by this polymer dielectric
2) short circuit current be 13.21mA.cm
-2, than the quasi-solid electrolyte solar cell short circuit current (12.46mA.cm not adding crosslinking agent of comparative example 1
-2) improve 0.75mA.cm
-2; Its open circuit voltage is 630.5mV, improves 28.9mV than the quasi-solid electrolyte solar energy open circuit voltage (601.6mV) without interpolation crosslinking agent of comparative example 1; Its photoelectric conversion efficiency is 4.81%, improves about 0.68% than the quasi-solid electrolyte solar battery efficiency (4.13%) without interpolation crosslinking agent of comparative example 1.
Comparative example 1:
Being mixed in 6g volume ratio by weight the PEO/P (VDF-HFP) taking 0.2g for 2:3 at 80 DEG C is in the organic solvent of PC and DME of 7:3, continues stirring until and dissolves completely, then add 0.02g SiO
2nano particle and absolute ethyl alcohol, continue to add thermal agitation and make it mix.
0.057g I is added in mixed solution
2with 0.25g KI, form oxidation-reduction pair, I
2be I with the mol ratio of KI
2: the O in KI=1:7, K and ethylene oxide meets: K/O mol ratio is 0.8.Under normal temperature, stirring 4 ~ 8 is little of evenly blended.
The quasi-solid electrolyte system of not adding crosslinking agent is added drop-wise on dye sensitized nano crystal film, under the environment of 70 DEG C, continues baking 1 ~ 3 hour in horizontal positioned to baking oven, cover platinum to electrode.
At room temperature environment, use xenon lamp simulated solar irradiation, light intensity is 95.53mW.cm
-2under (light intensity: use silicon photoelectric diode to demarcate) condition, (effective illuminating area is 0.16cm to record dye sensitized nano crystal salar battery
2) short circuit current be 12.46mA.cm
-2, open circuit voltage is 601.6Mv, and photoelectric conversion efficiency is 4.13%.
Comparative example 2
Be with comparative example 1 difference: crosslinking agent is 0.05g thiocarbamide.
(effective illuminating area is 0.16cm to the dye sensitized nano crystal salar battery assembled by this polymer dielectric
2) short circuit current be 13.58mA.cm
-2, open circuit voltage is 605.8mV, and its photoelectric conversion efficiency is 4.27%.
Comparative example 3
Be with comparative example 1 difference: crosslinking agent is 0.05g 4-tert .-butylpyridine.
(effective illuminating area is 0.16cm to the dye sensitized nano crystal salar battery assembled by this polymer dielectric
2) short circuit current be 10.43mA.cm
-2, open circuit voltage is 653.3mV, and its photoelectric conversion efficiency is 4.45%.
Shown in the battery performance parameter table specific as follows of above-described embodiment:
| n(I 2/KI) | SiO 2/g | Crosslinking agent/g | Jsc/mA.cm -2 | V OC/mV | Photoelectric conversion efficiency/% | |
| Embodiment 1 | 1:7 | 0.02 | 0.05 | 12.83 | 638.2 | 4.63 |
| Embodiment 2 | 1:10 | 0.02 | 0.05 | 12.6 | 620.8 | 4.59 |
| Embodiment 3 | 1:7 | 0.02 | 0.10 | 14.2 | 650.8 | 5.02 |
| Embodiment 4 | 1:7 | 0.02 | 0.15 | 13.21 | 630.5 | 4.81 |
| Comparative example 1 | 1:7 | 0.02 | 0 | 12.46 | 601.6 | 4.13 |
| Comparative example 2 | 1:7 | 0.02 | 0.05 | 13.58 | 605.8 | 4.27 |
| Comparative example 3 | 1:7 | 0.02 | 0 | 10.43 | 653.3 | 4.45 |
Can obviously be found out by above table: the battery efficiency of embodiment 3 is the highest, now I
2be I with the mol ratio of KI
2: KI=1:7, the weight of plasticizer Nano particles of silicon dioxide is 0.02g, crosslinking agent is 0.1g, only have and meet this three conditions simultaneously, just can reach the dye sensitized nano crystal salar battery of performance the best, its photoelectric conversion efficiency is also the highest, as can be seen here, proportioning between above-mentioned three kinds of components and component is an indivisible entirety, and this is also crosslinking agent and the synergistic result of plasticizer.
4-tert .-butylpyridine in above-described embodiment also can substitute with dimethyl sulfoxide (DMSO), dimethyl formamide, dioxanes, hexamethyl phosphoramide and oxolane, and the trend presented is as the same table.
Claims (9)
1. a polymer dielectric, is characterized in that: comprise mixture A, organic solvent B, mol ratio be the I of 1:5 ~ 1:10
2/ KI oxidation-reduction pair, plasticizer and crosslinking agent;
Described mixture A comprises the polyoxyethylene and vinylidene fluoride-hexafluoropropylene copolymer that weight ratio is 1:4 ~ 4:1, and the total weight of described mixture A is 2% ~ 10% of organic solvent B weight;
Described organic solvent B comprises the propene carbonate and glycol dimethyl ether that volume ratio is 1:8 ~ 8:1;
Described I
2k in/KI oxidation-reduction pair and the O in polyoxyethylene meets, and K/O mol ratio is 0.6 ~ 0.8;
The weight of described plasticizer is 10% ~ 30% of mixture A total weight;
The weight of described crosslinking agent is 25% ~ 125% of mixture A total weight, the aprotic solvent of described crosslinking agent to be concentration the be thiocarbamide of 0.05g/ml ~ 0.10g/ml.
2. polymer dielectric according to claim 1, is characterized in that: described aprotic solvent is one or more in 4-tert .-butylpyridine, dimethyl sulfoxide (DMSO), dimethyl formamide, dioxanes, hexamethyl phosphoramide and oxolane.
3. polymer dielectric according to claim 1, is characterized in that: also comprise absolute ethyl alcohol, and the proportioning of described plasticizer and absolute ethyl alcohol is 0.02g/ml ~ 0.1g/ml.
4. the polymer dielectric according to claim 1 or 2 or 3, is characterized in that: described plasticizer is Nano particles of silicon dioxide.
5. a method for preparing polymer electrolytes, is characterized in that comprising the steps:
1. polyoxyethylene and vinylidene fluoride-hexafluoropropylene copolymer is taken by weight 1:4 ~ 4:1, mixing composition mixture A, 1:8 ~ 8:1 measures propene carbonate and glycol dimethyl ether by volume, mixing composition organic solvent B, mixture A is added in organic solvent B, the total weight of mixture A is 2% ~ 10% of organic solvent B weight, water-bath at 60 DEG C ~ 100 DEG C, until dissolve completely, add plasticizer, the weight of described plasticizer is 10% ~ 30% of mixture A total weight, obtains high molecular nanometer mixed liquor;
2. in the high molecular nanometer mixed liquor of step 1. gained, the I that mol ratio is 1:5 ~ 1:10 is added
2/ KI oxidation-reduction pair, obtains polymer electrolyte matrix, described I
2k in/KI oxidation-reduction pair and the O in polyoxyethylene meets, and K/O mol ratio is 0.6 ~ 0.8;
3. while constantly stirring, crosslinking agent is added in the polymer electrolyte matrix that 2. step obtains, continue stirring until and mix, obtain the polymer dielectric based on crosslinking agent, the weight of described crosslinking agent is 25% ~ 125% of mixture A total weight, the aprotic solvent of described crosslinking agent to be concentration the be thiocarbamide of 0.05g/ml ~ 0.10g/ml.
6. preparation method according to claim 5, it is characterized in that: described step 1. in, described plasticizer is first dissolved in absolute ethyl alcohol, then is added in the mixed liquor of mixture A and organic solvent B, and the proportioning of described plasticizer and absolute ethyl alcohol is 0.02g/ml ~ 0.1g/ml.
7. the preparation method according to claim 5 or 6, is characterized in that: described aprotic solvent is one or more in 4-tert .-butylpyridine, dimethyl sulfoxide (DMSO), dimethyl formamide, dioxanes, hexamethyl phosphoramide and oxolane.
8. the preparation method according to claim 5 or 6, is characterized in that: described plasticizer is Nano particles of silicon dioxide.
9. a claim 1 or 2 or the application of polymer dielectric on dye sensitized nano crystal salar battery described in 3 or 4.
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| CN201510033112.1A CN104681295B (en) | 2015-01-23 | 2015-01-23 | Method for preparing polymer electrolytes |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111384261A (en) * | 2018-12-28 | 2020-07-07 | Tcl集团股份有限公司 | Thin film and preparation method thereof and quantum dot light-emitting diode |
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 |
|---|
| G.D.SHARMA等: "Effect of thiourea incorporation in the electrolyte on the photovoltaic performance of the DSSC sensitized with pyridyl functionalized porphyrin", 《ELECTROCHIMICA ACTA》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111384261A (en) * | 2018-12-28 | 2020-07-07 | Tcl集团股份有限公司 | Thin film and preparation method thereof and quantum dot light-emitting diode |
| CN111384261B (en) * | 2018-12-28 | 2021-08-10 | Tcl科技集团股份有限公司 | Thin film and preparation method thereof and quantum dot light-emitting diode |
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