CN102509618A - Preparation method of gel electrolyte of dye-sensitized nanocrystalline solar cell - Google Patents
Preparation method of gel electrolyte of dye-sensitized nanocrystalline solar cell Download PDFInfo
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- CN102509618A CN102509618A CN2011103090190A CN201110309019A CN102509618A CN 102509618 A CN102509618 A CN 102509618A CN 2011103090190 A CN2011103090190 A CN 2011103090190A CN 201110309019 A CN201110309019 A CN 201110309019A CN 102509618 A CN102509618 A CN 102509618A
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Abstract
The invention discloses a preparation method of the gel electrolyte of a dye-sensitized nanocrystalline solar cell, and relates to a preparation method of gel electrolyte applied to a dye-sensitized nanocrystalline solar cell. The method adopts a mode of doping organic fused salt and nano tin oxide gel, and comprises the following steps of: reacting the low-molecular weight polyethylene oxide with difluoro sulfoxide to generate fluoro polyethylene oxide; reacting the fluoro polyethylene oxide with 1-methylimidazole in N,N-dimethyl formamide to obtain fused salt of which the anion is fluorine ion; preparing nano tin oxide gel; and mixing the fused salt and the nano tin oxide gel, and performing aging and purification to obtain stable gel electrolyte. The gel electrolyte prepared by the preparation method has the same performance as liquid electrolyte and high stability, high electric conductivity and long service life. The method disclosed by the invention plays an important role in the field of preparation of the dye-sensitized solar cell, and has a broad application prospect.
Description
Technical field
The present invention relates to a kind of preparation method who is used for the dye sensitized nano crystal salar battery gel electrolyte, belong to the electrolyte preparing technical field.
Background technology
The petrochemical industry resource that can exploit at present only can be maintained to before and after the year two thousand twenty, and the crisis of the energy is the problem that presses for solution at present.Solar energy is inexhaustible green resource, is the optimal path that solves China's energy resource structure and environmental problem.The exploitation and the production of solar cell have broad application prospects.At present the based semiconductor photovoltaic effect is monocrystalline silicon and non-crystal silicon solar cell, though its conversion efficiency is high, complex process, cost an arm and a leg, material requirements is harsh, thereby be difficult to popularize.Nineteen nineties; The dye sensitized nano crystal salar battery that the Michael of Lausanne, SUI university
professor works out; This dye sensitized nano crystal salar battery can overcome the shortcoming of silicon solar cell; Have advantages such as manufacture craft is simple, material purity is less demanding, cheap, become this hot research fields.
It is work electrode that dye sensitized nano crystal salar battery adopts the nanometer crystal film of the wide bandgap semiconductor of surface adsorption sensitising agent, because nanometer crystal film has very large specific area, can adsorb a large amount of sensitising agents, thereby can effectively absorb sunlight.The operation principle of dye sensitized nano crystal salar battery: when dyestuff absorbed sunlight, electronics was from the ground state transition to excitation state, and the electronics of excitation state is transferred to rapidly in the semi-conductive conduction band; And the hole is stayed in the dyestuff; Electronics is transferred to electrode through external circuit with after the Nano semiconductor network diffuses to conductive substrates, and the dyestuff of oxidation state is reduced the electrolyte reduction of attitude; The electrolyte of oxidation state is reduced in that electrode is accepted electronics, thereby accomplishes the transportation of electronics.
In dye-sensitized solar cells, be mostly to adopt in the liquid electrolyte as hole mobile material.The use of liquid electrolyte can bring and much be difficult to the shortcoming that overcomes, mainly shows as:
(1) complicated because of sealing technology, be prone to cause electrolyte leakage;
(2) in liquid electrolyte, sealant might react with electrolyte, and sensitizing dyestuff is prone to desorption;
(3) have deoxygenationization-other outer side reaction of reduction circulation in the electrolyte, making owing to the reverse migration of ion causes the compound chance of photogenerated charge increases, and reduces photoelectric conversion efficiency;
(4) solvent is volatile under the high temperature, possibly cause the dyestuff degraded with the sensitizing dyestuff effect;
In order to overcome the above problems; A kind of effective method adopts ion liquid based gel electrolyte to substitute liquid electrolyte exactly; The existing characteristics with liquid electrolyte low viscosity, macroion diffusion coefficient of ion liquid based gel electrolyte can not improve the long-time stability of DSSC because of it can not volatilize again.Yet ionic liquid still has certain fluidity, and this still can influence the long-time stability and encapsulation characteristic of DSSC.
Summary of the invention
The object of the present invention is to provide the preparation method of the dye sensitized nano crystal salar battery of a kind of good stability, high conductivity with organic fuse salt-nano tin dioxide gel electrolyte.
Specific embodiments is: a kind of dye sensitized nano crystal salar battery is with the preparation method of gel electrolyte:
The first step, the preparation of organic fuse salt: under the situation that pyridine exists,, generate the PEO of fluoro with low-molecular-weight PEO and the reaction of difluoro sulfoxide; The PEO of fluoro is purified back and 1-methylimidazole at N, and reaction is 48 hours in the N-dimethylformamide, and reaction temperature 85-95 ℃, product is purified with absolute ether again; Dry in vacuum drying oven then, baking temperature is 120 ℃, obtains the fuse salt that anion is a fluorine ion.The cation of this fuse salt is the substituted glyoxaline cation of low-molecular-weight PEO, and the structure of this glyoxaline cation is following:
Wherein, n is 9-14; The R base is H, OH, OCH
3Not polymerizable groups or CH
2=CHCOO-, CH
2=CCH
3The COO-polymerizable groups; The anion of this fuse salt is a fluorine ion; The molecular weight for preparing the low-molecular-weight PEO of this fuse salt is 450-550;
In second step, the preparation of nano tin dioxide gel: take by weighing nano oxidized glass putty and polyvinyl alcohol at 1: 1 by mass ratio, the nitric acid of 1.5-8mol/L is added drop-wise in the said mixture under vigorous stirring, be mixed with the acidic mixed salting liquid, mixing time is 30min; The ammonia spirit of 5-10.8mol/L is added drop-wise under vigorous stirring in the above-mentioned acidic mixed salting liquid, regulates the pH value to 5-7, control reaction temperature is 0-10 ℃, and mixing time is 30min; Place baking oven to carry out polymerization reaction in 80-280 ℃ the solution that regulates the pH value, form stable solid shape gel up to solution;
The 3rd step; The doping of organic fuse salt and nano tin dioxide gel: an amount of nano tin dioxide gel with the preparation of second step under 80-90 ℃ joins in organic fuse salt of first step preparation; The volume ratio of organic fuse salt and nano tin dioxide gel is 50: (7～15), constantly stirring is dissolved the nano tin dioxide gel fully, and insulation is 6-8 hour under this temperature; Nano tin dioxide gel and organic fuse salt are fully reacted, up to the gel electrolyte that forms homogeneous;
In the 4th step, the ageing of gel electrolyte and purifying: the gel electrolyte of above-mentioned the 3rd step preparation, is constantly stirred more than 24 hours 90-100 ℃ of insulation therebetween, so that the gel electrolyte homogeneous, the conductivity that records this gel electrolyte is 15.3-18.7mScm
-1, the gel electrolyte behind ageing and the purifying is cooled off the airtight preservation in back with for use.
Polyvinyl alcohol in second step can replace with: citric acid, tartaric acid, amino acid, ethylene glycol, polyethylene glycol, disodium salt or malic acid.
In the 3rd step, in the nano tin dioxide gel being joined organic fuse salt of first step preparation in, can add the nano particle gel, this nano particle gel is selected from Al
2O
3, SiO
2, TiO
2, ZrO
2Or ZnO nano particle.
Embodiment
Embodiment 1
Under the situation that pyridine exists, with molecular weight 450 PEO and the reaction of difluoro sulfoxide, the PEO of generation fluoro; The PEO of fluoro is purified back and 1-methylimidazole at N, and reaction is 48 hours in the N-dimethylformamide, 95 ℃ of reaction temperatures, and product is purified with absolute ether again; Dry in vacuum drying oven then, baking temperature is 120 ℃, obtains the fuse salt that anion is a fluorine ion.The cation of this fuse salt is the substituted glyoxaline cation of low-molecular-weight PEO, and the structure of this glyoxaline cation is following:
Wherein, n is 9-14; The R base is H, OH, OCH
3Not polymerizable groups or CH
2=CHCOO-, CH
2=CCH
3The COO-polymerizable groups; The anion of this fuse salt is a fluorine ion; Take by weighing putty powder and polyethylene glycol at 1: 1 by mass ratio, the nitric acid of 1.5mol/L is added drop-wise in the said mixture under vigorous stirring, be mixed with the acidic mixed salting liquid, mixing time is 30min; The ammonia spirit of 5mol/L is added drop-wise under vigorous stirring in the above-mentioned acidic mixed salting liquid, regulates pH value to 7, control reaction temperature is 10 ℃, and mixing time is 30min; Place baking oven to carry out polymerization reaction in 280 ℃ the solution that regulates the pH value, form stable solid shape gel up to solution; In 90 ℃ of organic fuse salts that down an amount of nano tin dioxide gel joined; The volume ratio of organic fuse salt and nano tin dioxide gel is 50: 7; Constantly stirring dissolves the nano tin dioxide gel fully; Insulation is 6 hours under this temperature, and nano tin dioxide gel and organic fuse salt are fully reacted, up to the gel electrolyte that forms homogeneous; Be incubated 24 hour or more at 100 ℃ the gel electrolyte of above-mentioned the 3rd step preparation; Constantly stir therebetween, so that the gel electrolyte homogeneous, the complete betwixt solvation of above-mentioned nano tin dioxide gel combines with above-mentioned organic fuse salt; So that acquisition has the performance identical with liquid electrolyte; And have the gel electrolyte in high stability, high conductivity and long useful life, through measuring, conductivity is 15.3mScm
-1, the gel electrolyte behind ageing and the purifying is cooled off the airtight preservation in back with for use.
Embodiment 2
Under the situation that pyridine exists, with molecular weight 450 PEO and the reaction of difluoro sulfoxide, the PEO of generation fluoro; The PEO of fluoro is purified back and 1-methylimidazole at N, and reaction is 48 hours in the N-dimethylformamide, 95 ℃ of reaction temperatures, and product is purified with absolute ether again; Dry in vacuum drying oven then, baking temperature is 120 ℃, obtains the fuse salt that anion is a fluorine ion.The cation of this fuse salt is the substituted glyoxaline cation of low-molecular-weight PEO, and the structure of this glyoxaline cation is following:
Wherein, n is 9-14; The R base is H, OH, OCH
3Not polymerizable groups or CH
2=CHCOO-, CH
2=CCH
3The COO-polymerizable groups; The anion of this fuse salt is a fluorine ion; Take by weighing putty powder and polyethylene glycol at 1: 1 by mass ratio, the nitric acid of 2mol/L is added drop-wise in the said mixture under vigorous stirring, be mixed with the acidic mixed salting liquid, mixing time is 30min; The ammonia spirit of 6mol/L is added drop-wise under vigorous stirring in the above-mentioned acidic mixed salting liquid, regulates pH value to 7, control reaction temperature is 5 ℃, and mixing time is 30min; Place baking oven to carry out polymerization reaction in 200 ℃ the solution that regulates the pH value, form stable solid shape gel up to solution; In 90 ℃ of organic fuse salts that down an amount of nano tin dioxide gel joined; The volume ratio of organic fuse salt and nano tin dioxide gel is 5: 1; Constantly stirring dissolves the nano tin dioxide gel fully; Insulation is 6 hours under this temperature, and nano tin dioxide gel and organic fuse salt are fully reacted, up to the gel electrolyte that forms homogeneous; Be incubated 24 hour or more at 100 ℃ the gel electrolyte of above-mentioned the 3rd step preparation; Constantly stir therebetween, so that the gel electrolyte homogeneous, the complete betwixt solvation of above-mentioned nano tin dioxide gel combines with above-mentioned organic fuse salt; So that acquisition has the performance identical with liquid electrolyte; And have the gel electrolyte in high stability, high conductivity and long useful life, through measuring, conductivity is 16.5mScm
-1, the gel electrolyte behind ageing and the purifying is cooled off the airtight preservation in back with for use.
Embodiment 3
Under the situation that pyridine exists, with molecular weight 550 PEO and the reaction of difluoro sulfoxide, the PEO of generation fluoro; The PEO of fluoro is purified back and 1-methylimidazole at N, and reaction is 48 hours in the N-dimethylformamide, 85 ℃ of reaction temperatures, and product is purified with absolute ether again; Dry in vacuum drying oven then, baking temperature is 120 ℃, obtains the fuse salt that anion is a fluorine ion.The cation of this fuse salt is the substituted glyoxaline cation of low-molecular-weight PEO, and the structure of this glyoxaline cation is following:
Wherein, n is 9-14; The R base is H, OH, OCH
3Not polymerizable groups or CH
2=CHCOO-, CH
2=CCH
3The COO-polymerizable groups; The anion of this fuse salt is a fluorine ion; Take by weighing putty powder and tartaric acid at 1: 1 by mass ratio, the nitric acid of 8mol/L is added drop-wise in the said mixture under vigorous stirring, be mixed with the acidic mixed salting liquid, mixing time is 30min; The ammonia spirit of 10.8mol/L is added drop-wise under vigorous stirring in the above-mentioned acidic mixed salting liquid, regulates pH value to 5, control reaction temperature is 0 ℃, and mixing time is 30min; Place baking oven to carry out polymerization reaction in 80 ℃ the solution that regulates the pH value, form stable solid shape gel up to solution; In 80 ℃ of organic fuse salts that down an amount of nano tin dioxide gel joined, add Al simultaneously
2O
3Nano particle, organic fuse salt, nano tin dioxide gel, Al
2O
3The volume ratio of nano particle is 50: 15: 1, constantly stirs the nano tin dioxide gel is dissolved fully, and insulation is 8 hours under this temperature, and nano tin dioxide gel and organic fuse salt are fully reacted, up to the gel electrolyte that forms homogeneous; Be incubated 24 hour or more at 90 ℃ the gel electrolyte of above-mentioned the 3rd step preparation; Constantly stir therebetween, so that the gel electrolyte homogeneous, the complete betwixt solvation of above-mentioned nano tin dioxide gel combines with above-mentioned organic fuse salt; So that acquisition has the performance identical with liquid electrolyte; And have the gel electrolyte in high stability, high conductivity and long useful life, through measuring, conductivity is 18.7mScm
-1, the gel electrolyte behind ageing and the purifying is cooled off the airtight preservation in back with for use.
Claims (3)
1. the preparation method of a dye sensitized nano crystal salar battery gel electrolyte is characterized in that:
The first step, the preparation of organic fuse salt: under the situation that pyridine exists,, generate the PEO of fluoro with low-molecular-weight PEO and the reaction of difluoro sulfoxide; The PEO of fluoro is purified back and 1-methylimidazole at N, and reaction is 48 hours in the N-dimethylformamide, and reaction temperature 85-95 ℃, product is purified with absolute ether again; Dry in vacuum drying oven then, baking temperature is 120 ℃, obtains the fuse salt that anion is a fluorine ion; The cation of this fuse salt is the substituted glyoxaline cation of low-molecular-weight PEO, and the structure of this glyoxaline cation is following:
Wherein, n is 9-14; The R base is H, OH, OCH
3Not polymerizable groups or CH
2=CHCOO-, CH
2=CCH
3The COO-polymerizable groups; The anion of this fuse salt is a fluorine ion; The molecular weight for preparing the low-molecular-weight PEO of this fuse salt is 450-550;
In second step, the preparation of nano tin dioxide gel: take by weighing nano oxidized glass putty and polyvinyl alcohol at 1: 1 by mass ratio, the nitric acid of 1.5-8mol/L is added drop-wise in the said mixture under vigorous stirring, be mixed with the acidic mixed salting liquid, mixing time is 30min; The ammonia spirit of 5-10.8mol/L is added drop-wise under vigorous stirring in the above-mentioned acidic mixed salting liquid, regulates the pH value to 5-7, control reaction temperature is 0-10 ℃, and mixing time is 30min; Place baking oven to carry out polymerization reaction in 80-280 ℃ the solution that regulates the pH value, form stable solid shape gel up to solution;
The 3rd step; The doping of organic fuse salt and nano tin dioxide gel: an amount of nano tin dioxide gel with the preparation of second step under 80-90 ℃ joins in organic fuse salt of first step preparation; The volume ratio of organic fuse salt and nano tin dioxide gel is 50: (7～15), constantly stirring is dissolved the nano tin dioxide gel fully, and insulation is 6-8 hour under this temperature; Nano tin dioxide gel and organic fuse salt are fully reacted, up to the gel electrolyte that forms homogeneous;
In the 4th step, the ageing of gel electrolyte and purifying: the gel electrolyte of above-mentioned the 3rd step preparation, is constantly stirred more than 24 hours 90-100 ℃ of insulation therebetween, so that the gel electrolyte homogeneous, the conductivity that records this gel electrolyte is 15.3-18.7mScm
-1, the gel electrolyte behind ageing and the purifying is cooled off the airtight preservation in back with for use.
2. the preparation method of dye sensitized nano crystal salar battery gel electrolyte according to claim 1 is characterized in that: the polyvinyl alcohol in second step replaces with: citric acid, tartaric acid, amino acid, ethylene glycol, polyethylene glycol, disodium salt or malic acid.
3. the preparation method of dye sensitized nano crystal salar battery gel electrolyte according to claim 1 is characterized in that: in the 3rd step, add the nano particle gel, this nano particle gel is selected from Al
2O
3, SiO
2, TiO
2, ZrO
2Or ZnO nano particle.
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|---|---|---|---|
| CN 201110309019 CN102509618B (en) | 2011-10-13 | 2011-10-13 | Preparation method of gel electrolyte of dye-sensitized nanocrystalline solar cell |
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| CN 201110309019 CN102509618B (en) | 2011-10-13 | 2011-10-13 | Preparation method of gel electrolyte of dye-sensitized nanocrystalline solar cell |
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| CN102509618B CN102509618B (en) | 2013-06-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103489644A (en) * | 2013-09-13 | 2014-01-01 | 北京航空航天大学 | Polymer iodide gel electrolyte and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1456861A1 (en) * | 2001-12-21 | 2004-09-15 | Sony International (Europe) GmbH | A polymer gel hybrid solar cell |
| US20080006322A1 (en) * | 2003-04-30 | 2008-01-10 | Peng Wang | Dye sensitized solar cell |
| CN102130364A (en) * | 2011-02-12 | 2011-07-20 | 中南大学 | Gel-type polymer electrolyte used for lithium-sulfur secondary battery system and preparation method |
-
2011
- 2011-10-13 CN CN 201110309019 patent/CN102509618B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1456861A1 (en) * | 2001-12-21 | 2004-09-15 | Sony International (Europe) GmbH | A polymer gel hybrid solar cell |
| US20080006322A1 (en) * | 2003-04-30 | 2008-01-10 | Peng Wang | Dye sensitized solar cell |
| CN102130364A (en) * | 2011-02-12 | 2011-07-20 | 中南大学 | Gel-type polymer electrolyte used for lithium-sulfur secondary battery system and preparation method |
Non-Patent Citations (2)
| Title |
|---|
| MIAO WANG等: "Investigation of PEO-imidazole ionic liquid oligomer electrolytes for dye-sensitized solar cells", 《SOLAR ENERGY MATERIALS & SOLAR CELLS》, 20 February 2007 (2007-02-20) * |
| 王 淼等: "一种新型的准固态电解质在染料敏化太阳能电池中的应用", 《科学通报》, vol. 51, no. 9, 31 May 2006 (2006-05-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103489644A (en) * | 2013-09-13 | 2014-01-01 | 北京航空航天大学 | Polymer iodide gel electrolyte and preparation method thereof |
| CN103489644B (en) * | 2013-09-13 | 2017-02-01 | 北京航空航天大学 | Polymer iodide gel electrolyte and preparation method thereof |
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