CN104134543B - Metal organic gel electrolyte and manufacturing method and application thereof - Google Patents
Metal organic gel electrolyte and manufacturing method and application thereof Download PDFInfo
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- CN104134543B CN104134543B CN201410321418.2A CN201410321418A CN104134543B CN 104134543 B CN104134543 B CN 104134543B CN 201410321418 A CN201410321418 A CN 201410321418A CN 104134543 B CN104134543 B CN 104134543B
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention discloses a quasi-solid metal organic gel electrolyte used for dye-sensitized solar cells and a manufacturing method thereof. The metal organic gel electrolyte is characterized in that metal ions and organic ligands are used as gelators to form a gel skeleton structure, and the gel skeleton structure absorbs liquid electrolyte components so that the quasi-solid electrolyte is obtained. The manufacturing method is a swelling absorption method, which consists of the steps as below: 1. under normal temperature, metal salt and carboxylic acids ligands are dissolved in organic solvents, and ultrasound is used to realize full dissolution; 2. gel is formed by heating; 3. the formed gel is soaked in the electrolyte solution containing I-/I3- redox couples to absorb the components of the electrolyte solution, and then the metal organic gel electrolyte can be obtained. The manufacturing method is easy, convenient, fast and low-cost, and the synthesized gel electrolyte can be used for solar cells and other battery fields.
Description
Technical field
The present invention relates to the preparation field of quasi-solid electrolyte, and in particular to a kind of metal organogel electrolyte and its system
Preparation Method, especially applies on DSSC.
Background technology
Metal organogel is the important quasi- solid-state soft material of a class, is that metal or metallic compound are incorporated into gelinite
The special supermolecular gel of the class that formed in system, it by the gelator assembling of metal ion or metal ion with it is organic
Part is formed by being coordinated bridge linking effect.This kind of quasi- solid-state material is in catalysis, gas absorption, sensor, pharmaceutical chemistry, quasi- solid-state
The fields such as electrolyte have potential using value.
Electrolyte is the important component part of DSSC, carries the work that light is excited reducing dyes
With, thus its property directly influences the photoelectric conversion performance of battery.Higher battery can generally be obtained using liquid electrolyte
Electricity conversion, but while the shortcoming of existence and stability difference.By contrast, quasi-solid electrolyte can overcome liquid electrolyte
Volatilization leakage, the defects such as sealing are difficult, contact problems, the ionic conductivity of all solid state electrolyte and battery light anode can be solved again
Low problem, thus by the extensive concern of domestic and international researcher.At present the quasi- solid gel electrolyte of research mostly be from
The several types such as sub- liquid, gel-form solid polymer electrolyte, small molecule gel electrolyte.Metal organogel is due to its special net
Network structure, the advantages of prepare simple, with low cost, become the carrier for potentially preparing gel electrolyte.At present, also do not have in the world
There is metal organogel to prepare the report of DSSC quasi-solid electrolyte.
The content of the invention
An object of the present invention is to provide a kind of quasi- solid gel electrolysis formed for carrier by metal organogel
Matter, and it is applied to DSSC.
The second object of the present invention is the method that offer prepares metal organogel electrolyte, the method have it is simple,
Easily and fast and high repeatability and other advantages.
The object of the invention is achieved through the following technical solutions：
The metal organogel electrolyte of the present invention, is to adopt metal ion to be coordinated to be formed with organic ligand for gelator
Gel skeleton structure, absorbs the quasi-solid electrolyte that liquid electrolyte ingredient is formed.
Further, described metal ion is Al3+、Fe3+、In3+Or Ga3+.Preferably, the metal ion is Al3+、Fe3 +、In3+Or Ga3+The nitrate containing water of crystallization or hydrochlorate.
Further, the organic ligand is that carboxylic acidss containing two or three hydroxy-acid groups of the molecular weight less than 1000 are matched somebody with somebody
Body.Preferably, the organic ligand is p-phthalic acid, trimesic acid or naphthalene diacid.
Further, the liquid electrolyte is containing I-/I3 -The DSSC electrolyte of oxidation-reduction pair.
The metal organogel electrolyte of the present invention is prepared by swellable absorbent method, and its step is as follows successively：
(1) under room temperature, slaine and carboxylic acidss part are dissolved in organic solvent, ultrasound makes which fully dissolve；(2) add
Heat forms it into gel；(3) with the soak for preparing in containing I-/I3 -The electrolyte of oxidation-reduction pair, absorbs the electrolysis
Liquid composition is so as to obtaining metal organogel electrolyte.
As a kind of preferred version, in above-mentioned preparation method, the slaine is the nitrate containing water of crystallization or hydrochlorate,
Preferably aluminum nitrate, iron chloride, ferric nitrate, indium nitrate or Ganite (Fujisawa)..
Further, the carboxylic acidss part is carboxylic acidss containing two or three hydroxy-acid groups of the molecular weight less than 1000
Part.Preferably, the carboxylic acidss part is p-phthalic acid, trimesic acid or naphthalene diacid.
Further, molar concentration of the slaine in the organic solvent is 0.005～1.0mol/L；The carboxylic acid
Molar concentration of the class part in the organic solvent is 0.005～1.0mol/L；The organic solvent be ethanol or ethanol with
Acetonitrile mixed solvent；Wherein, the volume of acetonitrile accounts for the 0～50% of mixed solvent volume.
It is as a kind of preferred version, in above-mentioned preparation method, described containing I-/I3 -The liquid electrolyte of oxidation-reduction pair,
Including iodine, lithium iodide, ionic liquid, additive and solvent.The ionic liquid is preferably 1- propyl group, 3- methylpyridinium iodide imidazoles
(PMII), 1- methyl, 3- propyl group iodate imidazoles (MPII), 1,2- dimethyl -3- propyl group iodate imidazoles (DMPII), or 1- ethyls -
One or more of 3- Methylimidazole. sulfocyanic ester (EMINCS).The additive includes guanidine thiocyanate, tert .-butylpyridine, or N-
One or more of tolimidazole.The solvent is preferably acetonitrile, methoxypropionitrile, or the mixed solvent of acetonitrile and valeronitrile
Deng.It is described containing I-/I3 -In the liquid electrolyte of oxidation-reduction pair, the molar concentration of iodine is 0.001～0.5mol/L, lithium iodide
Molar concentration be 0.001～0.5mol/L, the molar concentration of ionic liquid is 0.001～6.0mol/L, and guanidine thiocyanate rubs
Your concentration is 0.001～1.0mol/L, and the molar concentration of tert .-butylpyridine is 0.001～5.0mol/L, N- tolimidazoles
Molar concentration be 0.001～5.0mol/L, the volume of acetonitrile accounts for the 0～100% of mixed solvent volume.
As a kind of preferred version, in above-mentioned preparation method, it is described ultrasound time be 5～45min, reacting by heating temperature
For room temperature～90 DEG C, the time of reacting by heating is 10min～24h, and the time of metal organogel absorption liquid electrolyte is 5h
～72h, metal organogel are 0.1～10 with electrolyte volume ratio.
Obtained in the inventive method, quasi- solid metallic organogel electrolyte has used scanning electron microscope, electrochemical workstation etc.
Instrument has carried out detailed sign.
Obtained in the inventive method, metal organogel electrolyte has widened the range of application of metal organogel, particularly
Dye-sensitized solar cells field is applied to, excellent photoelectric transformation efficiency is achieved.
Compared with prior art, the invention has the advantages that：
(1) metal organogel gel electrolyte proposed by the present invention, has on the one hand widened the application of metal organogel
Scope, on the other hand obtains quasi-solid electrolyte of good performance.
(2) present invention is prepared for quasi-solid electrolyte using swellable absorbent method, and this preparation method has simple, convenient, fast
Speed and high repeatability and other advantages.
(3) gel electrolyte obtained by preparation method of the present invention can be used as the electrolyte component of DSSC
Point, this kind of battery mainly imitates photosynthesis principle, a kind of novel solar battery developed, to new forms of energy with can be again
The exploitation of the raw energy and protection human environment have great importance.Exceeded using prepared gel electrolyte
8% photoelectric transformation efficiency.
Description of the drawings
Fig. 1 is aluminum-prepared by aluminum-trimesic acid metal organogel (left side) prepared by the present invention and swellable absorbent method
The digital photograph (right side) of benzenetricarboxylic acid metal organogel electrolyte.
Fig. 2 is that metal organogel electrolyte prepared by the embodiment of the present invention 1 is applied to quasi-solid-state dye sensitized solar energy
Photoelectric current-the voltage curve of battery.
Specific embodiment
The present invention is explained further below in conjunction with specific embodiment, but embodiment does not do any type of to the present invention
Limit.
Embodiment 1
The preparation of metal organogel electrolyte：0.02mmol trimesic acids, nine nitric hydrates of 0.05mmol are weighed respectively
Aluminum adds 0.5ml ethanol and 0.5ml acetonitriles, ultrasonic 15min dissolvings to be placed in 30min in 80 DEG C of baking ovens and formed in sample bottle
Metal organogel.Take 0.5ml liquid electrolytes to be placed in sample bottle, after absorbing 24h, completely liquid electrolyte will not absorbed
Reclaim, in sample bottle, be metal organogel electrolyte.The liquid electrolyte includes：1.74mol/L 1- propyl group, 3- first
Base iodate imidazoles (PMII), 0.087mol/L elemental iodines, 0.145mol/L lithium iodides, 0.29mol/L guanidine thiocyanates, 1.45mol/
L tert .-butylpyridines, it is 85 that solvent is volume ratio：15 acetonitrile and valeronitrile mixed solvent.
It is prepared by battery：Using the method for silk screen printing by anatase TiO2Nano-particle slurry is printed on FTO electro-conductive glass
On, it is 16 μm or so to control its thickness, 500 DEG C of heat treatment 1h in temperature programmed control Muffle furnace, after being cooled to room temperature, in 70 DEG C of bars
40mmol/L TiCl are soaked under part4Aqueous solution in 30min, then 520 DEG C sintering 30min, when being cooled to 80 DEG C or so,
It is soaked in about 16 hours in N719 dyestuffs, taking-up can obtain the working electrode for adsorbing N719 dyestuffs.With containing chloroplatinic acid
Aqueous isopropanol is dropped on another piece of FTO electro-conductive glass, is calcined 15 minutes at 400 DEG C, is obtained containing Pt to electrode；Finally in work
Make metal organogel electrolyte described in extrusion on electrode, with the method encapsulation battery of sandwich style.It is quasi-solid-state dye sensitized too
The photoelectric transformation efficiency of positive energy battery is 8.60%, as shown in Figure 2.
Embodiment 2
The preparation of metal organogel electrolyte：0.3mmol p-phthalic acids, nine nitric hydrates of 0.2mmol are weighed respectively
Aluminum adds 1ml ethanol, ultrasonic 15min dissolvings to be placed in 30min in 80 DEG C of baking ovens and form metal organogel in sample bottle.Take
1.0ml liquid electrolytes are placed in sample bottle, after absorbing 24h, will not absorbed completely liquid electrolyte and are reclaimed, in sample bottle i.e.
For metal organogel electrolyte.Liquid electrolyte includes：0.6mol/L 1- propyl group, 3- methylpyridinium iodide imidazoles (PMII),
0.03mol/L elemental iodines, 0.05mol/L lithium iodides, 0.1mol/L guanidine thiocyanates, 0.5mol/L tert .-butylpyridines, solvent are body
Product is than being 85：15 acetonitrile and valeronitrile mixed solvent.
The working electrode of N719 dye sensitizations, Pt are prepared to electrode using method as described in example 1 above, assembled battery is too
Positive energy battery.
Embodiment 3
The preparation of metal organogel electrolyte：Weigh 0.1mmol naphthalene diacid respectively, 0.1mmol ANN aluminium nitrate nonahydrates in
In sample bottle, 1ml ethanol, ultrasonic 15min dissolvings is added to be placed in 1h in 80 DEG C of baking ovens and form metal organogel.Take 0.1ml liquid
Body electrolyte is placed in sample bottle, after absorbing 12h, will not absorbed completely liquid electrolyte and is reclaimed, metal is in sample bottle
Organogel electrolyte.Liquid electrolyte includes：0.6mol/L 1- propyl group, 3- methylpyridinium iodide imidazoles (PMII), 0.03mol/L
Elemental iodine, 0.05mol/L lithium iodides, 0.1mol/L guanidine thiocyanates, 0.5mol/L tert .-butylpyridines, it is 85 that solvent is volume ratio：
15 acetonitrile and valeronitrile mixed solvent.
The working electrode of N719 dye sensitizations, Pt are prepared to electrode using method as described in example 1 above, assembled battery is too
Positive energy battery.
Embodiment 3
The preparation of metal organogel electrolyte：0.2mmol trimesic acids, seven nitric hydrate ferrum of 0.2mmol are weighed respectively
In sample bottle, 1ml ethanol, ultrasonic 5min dissolvings is added to be placed in 1h in 40 DEG C of baking ovens and form metal organogel.Take 0.5ml
Liquid electrolyte in sample bottle, after absorbing 24h, will not absorb completely liquid electrolyte and reclaim, metal will be in sample bottle
Organogel electrolyte.Liquid electrolyte includes：0.6mol/L 1,2- dimethyl -3- propyl group iodate imidazoles (DMPII),
0.1mol/L elemental iodines, 0.1mol/L lithium iodides, 0.45mol/L N- tolimidazoles, solvent are 3- methoxypropionitriles.
The working electrode of N719 dye sensitizations, Pt are prepared to electrode using method as described in example 1 above, assembled battery is too
Positive energy battery.
Embodiment 4
The preparation of metal organogel electrolyte：0.1mmol trimesic acids are weighed respectively, and 0.1mmol indium nitrates are in sample
In bottle, 1ml ethanol, ultrasonic 10min dissolvings is added to be placed in 1h in 40 DEG C of baking ovens and form metal organogel.Take 5.0ml liquid electrics
Solution matter is placed in sample bottle, after absorbing 12h, will not absorbed completely liquid electrolyte and is reclaimed, and be metal organic in sample bottle
Gel electrolyte.Liquid electrolyte includes：0.3mol/L 1- propyl group, 3- methylpyridinium iodide imidazoles (PMII), 0.015mol/L iodine lists
Matter, 0.025mol/L lithium iodides, 0.05mol/L guanidine thiocyanates, 0.25mol/L tert .-butylpyridines, it is 85 that solvent is volume ratio：15
Acetonitrile and valeronitrile mixed solvent.
The working electrode of N719 dye sensitizations, Pt are prepared to electrode using method as described in example 1 above, assembled battery is too
Positive energy battery.
Above-mentioned embodiment is the invention is not limited in, if to various changes of the invention or modification without departing from the present invention
Spirit and scope, if these change and modification belong to the present invention claim and equivalent technologies within the scope of, then this
It is bright to be also intended to comprising these changes and modification.
Claims (7)
1. a kind of metal organogel electrolyte, it is characterised in that：It is to adopt metal ion to match somebody with somebody for gelator with organic ligand
Position forms gel skeleton structure, absorbs the quasi-solid electrolyte that liquid electrolyte ingredient is formed；The metal ion is Al3+、Fe3 +、In3+Or Ga3+；The organic ligand is carboxylic acidss part containing two or three hydroxy-acid groups of the molecular weight less than 1000；
The liquid electrolyte is containing I-/I3 -The DSSC electrolyte of oxidation-reduction pair.
2. the metal organogel electrolyte preparation method described in claim 1, it is characterised in that：Its step is as follows successively：
(1) under room temperature, slaine and carboxylic acidss part are dissolved in organic solvent, ultrasound makes which fully dissolve；(2) heating makes its shape
Into gel；(3) with the soak for preparing in containing I-/I3 -The electrolyte of oxidation-reduction pair, Electolyte-absorptive composition so as to
To the metal organogel electrolyte.
3. metal organogel electrolyte preparation method according to claim 2, it is characterised in that：The slaine exists
Molar concentration in the organic solvent is 0.005～1.0mol/L；Carboxylic acidss part the rubbing in the organic solvent
Your concentration is 0.005～1.0mol/L.
4. metal organogel electrolyte preparation method according to claim 2, it is characterised in that：It is described containing I-/I3 -
The liquid electrolyte of oxidation-reduction pair, including iodine, lithium iodide, ionic liquid, additive and solvent.
5. metal organogel electrolyte preparation method according to claim 2, it is characterised in that：It is described ultrasound when
Between be 5～45min, reacting by heating temperature is room temperature～90 DEG C, and time of reacting by heating is 10min～24h, metal organogel
The time for absorbing liquid electrolyte is 5h～72h, and metal organogel is 0.1～10 with electrolyte volume ratio.
6. a kind of preparation method of DSSC, it is characterised in that：Using the method for silk screen printing by anatase
TiO2Nano-particle slurry is printed on FTO electro-conductive glass, heat treated, after being cooled to room temperature, is soaked in 40mmol/L TiCl4
In aqueous solution, then sintering, cooling, are soaked in N719 dyestuffs, and taking-up obtains the working electrode for adsorbing N719 dyestuffs；
Dropped on another piece of FTO electro-conductive glass with the aqueous isopropanol containing chloroplatinic acid, obtained containing Pt to electrode after calcining；In the work
Make the metal organogel electrolyte as claimed in claim 1 of extrusion on electrode, with the method encapsulation battery of sandwich style.
7. application of the metal organogel electrolyte described in claim 1 as DSSC electrolyte.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104465099B (en) * | 2014-12-18 | 2017-12-15 | 中山大学 | A kind of metal organogel electrolyte preparation method |
| CN105244169B (en) * | 2015-10-21 | 2016-08-17 | 景德镇陶瓷大学 | A kind of quasi-solid electrolyte for DSSC and preparation method thereof |
| CN108538605B (en) * | 2018-04-03 | 2020-11-17 | 湖北大学 | Metal gel electrolyte and preparation method thereof |
| CN114657601B (en) * | 2022-05-10 | 2024-01-30 | 琼台师范学院 | Preparation method and application of nickel oxide-iridium nanocluster heterogeneous material |
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| CN1555589A (en) * | 2000-10-18 | 2004-12-15 | �Ű�-�����ۺϻ�ѧƷ��ʽ���� | Gel-type polymer electrolyte and use thereof |
| CN102020748A (en) * | 2009-09-17 | 2011-04-20 | 中国科学院化学研究所 | Polymer-metal ion complex gel electrolyte and preparation method and application thereof |
| CN102161671A (en) * | 2011-02-23 | 2011-08-24 | 中山大学 | Coordination polymer material with multistage pore passage structure and preparation method thereof |
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| CN1555589A (en) * | 2000-10-18 | 2004-12-15 | �Ű�-�����ۺϻ�ѧƷ��ʽ���� | Gel-type polymer electrolyte and use thereof |
| CN102020748A (en) * | 2009-09-17 | 2011-04-20 | 中国科学院化学研究所 | Polymer-metal ion complex gel electrolyte and preparation method and application thereof |
| CN102161671A (en) * | 2011-02-23 | 2011-08-24 | 中山大学 | Coordination polymer material with multistage pore passage structure and preparation method thereof |
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