CN108987117A - CoSe2The preparation method of electrocatalysis material and its application in two-sided quasi-solid-state dye sensitized solar battery - Google Patents
CoSe2The preparation method of electrocatalysis material and its application in two-sided quasi-solid-state dye sensitized solar battery Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2022—Light-sensitive devices characterized by he counter electrode
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
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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
Abstract
The present invention discloses CoSe2The preparation method of electrocatalysis material and its in the application in two-sided quasi-solid-state dye sensitized solar battery.CoSe2The preparation method of electrocatalysis material, including selenium powder and cobalt salt, are dissolved in primary distilled water, and hydrazine hydrate and ammonium hydroxide is added；Then ultrasound, stir evenly；It is placed in autoclave, carries out hydro-thermal reaction；After hydro-thermal reaction stops, decompression is filtered, is cleaned, is dry.CoSe2Application of the electrocatalysis material in two-sided quasi-solid-state dye sensitized solar battery, comprising: CoSe2The preparation of electrocatalysis material suspension；The preparation of light anode；Preparation to electrode；The encapsulation of battery.The cell light of assembling obtains 733mV open-circuit photovoltage, 16.14mA/cm from front2Circuit photocurrent density, fill factor 0.70, corresponding photoelectric conversion efficiency are 8.28%；Light irradiates from the negative obtains 665mV open-circuit photovoltage, 10.38mA/cm2Circuit photocurrent density, fill factor 0.70, corresponding photoelectric conversion efficiency are 4.83%.
Description
Technical field
The present invention relates to sensitized cells technical fields.Specifically CoSe2The preparation method of electrocatalysis material and its
Application in two-sided quasi-solid-state dye sensitized solar battery.
Background technique
Dye-sensitized solar cells mainly imitates photosynthetic principle, a kind of new type solar energy developed
Battery.As a kind of substitute of most promising traditional silion cell, dye-sensitized solar cells abundant raw materials, cost
Low, technology is simple, is conducive to the industrialized production of large area.And raw material used, production technology are all nontoxic, nothing
Pollution, some materials can also recycle, and have great importance to protection environment.Due to the above feature it cause science and
The extensive concern of industrial two big industries, can effectively solve the energy problem of the mankind.Dye-sensitized solar cells is with low cost
Nano-titanium dioxide and light-sensitive coloring agent be primary raw material, simulating plant in nature using the sun can be carried out photosynthesis, will
Solar energy is converted into electric energy.It has a kind of typical " sandwich " structure, and a usual DSSC is consisted of three parts, and one
TiO is brushed with what N719 dyestuff impregnated2The electro-conductive glass of film contains (I as light anode-/I3 -) oxidation-reduction pair
Electrolyte solution and one conducting surface be coated with electrocatalysis material to electrode.Under light illumination, dye-sensitized molecules obtain
Visible light jumps to excitation state, and then photoelectron jumps to the conduction band of semiconductor, is transported, is collected, and finally enters external circuit and passes to
To electrode, electric current is generated.In general, restoring I to catalysis3 -For Pt be preferred material, it has superior electric conductivity, and electro-catalysis is living
Property and good stability.However, Pt is as a kind of noble metal, abundance is low, and cost price is expensive, is unfavorable for commercialization and answers
With hindering its large-scale use, Pt is not a kind of suitable catalyst.In order to solve this problem, totle drilling cost is reduced,
Keep the performance of battery again simultaneously, scientists are introduced in Devoting Major Efforts To Developing substitute, several catalysis materials at low cost
In solar battery.For example, carbon material, polymer, organic material and composite material etc..
Summary of the invention
For this purpose, technical problem to be solved by the present invention lies in provide a kind of CoSe2The preparation method of electrocatalysis material and
Its application in two-sided quasi-solid-state dye sensitized solar battery
In order to solve the above technical problems, the invention provides the following technical scheme:
CoSe2The preparation method of electrocatalysis material, includes the following steps:
(1) selenium powder and cobalt salt, are dissolved in primary distilled water, and hydrazine hydrate and ammonium hydroxide is added；Then ultrasound, stir evenly
(2) it is placed in autoclave, carries out hydro-thermal reaction；
(3) after hydro-thermal reaction stops, decompression is filtered, is cleaned, is dry.
Above-mentioned CoSe2The preparation method of electrocatalysis material, in step (1), the selenium powder of 0.222g and 0.238g's
CoCl2·6H2O is dissolved in the primary distilled water of 36mL, and the hydrazine hydrate of 24mL is added, then ultrasound 30min, then magnetic force stirs
Mix 20min.
Above-mentioned CoSe2The preparation method of electrocatalysis material, in step (2), will in step (1) be uniformly mixed reaction
Object, that pours into 100mL has in the autoclave of polytetrafluoroethyllining lining, carries out hydro-thermal reaction, and reaction temperature is 180 DEG C, instead
Answering temperature is 5h.
Above-mentioned CoSe2The preparation method of electrocatalysis material after hydro-thermal reaction stops, being cooled to room temperature in step (3),
Decompression filters, and filter cake uses primary distilled water and dehydrated alcohol alternately to rinse 10 times respectively, and obtained solid is done in a vacuum drying oven
Dry 2h, then it is finely ground with agate mortar, obtain CoSe2Electrocatalysis material.
CoSe2Application of the electrocatalysis material in two-sided quasi-solid-state dye sensitized solar battery, includes the following steps:
(2-1)CoSe2The preparation of electrocatalysis material suspension；
The preparation of (2-2) light anode；
The preparation of (2-3) to electrode；
The encapsulation of (2-4) battery.
Above-mentioned CoSe2Application of the electrocatalysis material in two-sided quasi-solid-state dye sensitized solar battery, in step (2-
1) in, the CoSe of 1.8mg is weighed2Electrocatalysis material, is added 5mL ethyl alcohol and 5mL ultrapure water is added in vial, is subsequently placed in
Ultrasound 30min, obtains configured CoSe in ultrasonic cleaner2Electrocatalysis material suspension.
Above-mentioned CoSe2Application of the electrocatalysis material in two-sided quasi-solid-state dye sensitized solar battery, in step (2-
2) in, the TiO with a thickness of 15 μm will be loaded with2The FTO electro-conductive glass of film immerses the TiCl that concentration is 0.05mol/L4Aqueous solution
In, it is placed in 70 DEG C of baking oven, places 0.5h, then take out and be loaded with TiO2The electro-conductive glass of film is rinsed dry with deionized water
Only, after being dried with nitrogen, be put into Muffle furnace and made annealing treatment: 1h to 450 DEG C of heating keeps the temperature 30min, naturally cools to 120
After DEG C；Take out TiO2The FTO electro-conductive glass of film is put into rapidly in prepared N719 dye solution, after standing 16h, is taken out
Light anode, the N719 dyestuff of film surface physical absorption is washed with anhydrous acetonitrile after purification, then is dried with nitrogen, institute
Obtain the TiO that electrode is dye sensitization2Light anode；
The N719 dyestuff the preparation method comprises the following steps: accurately weigh N719 dyestuff 3mg, take the tertiary fourth of 5mL with disposable syringe
Pure and mild 5mL acetonitrile is dissolved in brown sample bottle, ultrasonic 30min, is kept in dark place stand-by.
Above-mentioned CoSe2Application of the electrocatalysis material in two-sided quasi-solid-state dye sensitized solar battery, in step (2-
3) in, its patch on the conducting surface of the FTO electro-conductive glass of 3M sticker after the pre-treatment, will be made at the square of 0.6cm × 0.6cm；
With the CoSe prepared in liquid-transfering gun aspiration step (2-1)2Electrocatalysis material hangs 10 μ L of solution, drips to FTO electro-conductive glass patch 3M glue
In the square of cloth one side, it is placed in infrared oven and dries after drop is good, CoSe2Material can be deposited in FTO box, repeat to grasp
After making drop coating 8 times to electrode, the dry 2h in 100 DEG C of vacuum ovens；The electrode obtained is CoSe2Electrocatalysis material system
It is standby to electrode.
Above-mentioned CoSe2Application of the electrocatalysis material in two-sided quasi-solid-state dye sensitized solar battery, feature exist
In taking the Surlyn film of 30 μ m-thicks, be placed in CoSe in step (2-3)2Electrocatalysis material preparation to electrode and dyestuff
The TiO of sensitization2Between light anode, then it is placed in heat-sealing instrument hot pressing at 120 DEG C, clings, after being cooled to room temperature, to electricity
0.05mL quasi-solid electrolyte is dripped on the hole at the pole back side, so that the electrolyte on hole is fully entered inside battery, cell package is complete
At obtaining CoSe2Electrocatalysis material makes two-sided quasi-solid-state dye sensitized solar battery.
Above-mentioned CoSe2Application of the electrocatalysis material in two-sided quasi-solid-state dye sensitized solar battery, quasi- solid state electrolysis
Matter the preparation method is as follows: liquid iodine electrolyte is prepared under nitrogen atmosphere in glove box, liquid iodine electrolyte includes
The I of the LiI of 0.1mol/L, 0.05mol/L2, the additive 4- of the ionic liquid DMPII and 0.5mol/L of 0.6mol/L
Tert .-butylpyridine, solvent are the anhydrous acetonitrile of redistillation, DMPII 1,2- dimethyl -3- propyl iodate imidazoles；Then to
The vinylidene fluoride hexafluoropropylene copolymer of 5wt%, 80 DEG C of inclined fluorine second for being heated to solid colloidal are added in liquid iodophor electrolyte
Alkene-perfluoropropene copolymer fully dissolved obtains quasi-solid electrolyte after cooling.
Technical solution of the present invention achieves following beneficial technical effect:
The present invention synthesizes CoSe with hydro-thermal method2Metal selenide nano material, and use XRD and scanning electron microscope sem pair
It is characterized.Its catalytic activity is studied by cyclic voltammetric, electrochemical impedance, polarization curve.Finally, having studied CoSe2
Photoelectric property of the nano material in the two-sided dye-sensitized solar cells of quasi- solid-state.The battery of assembling, light are obtained from front
733mV open-circuit photovoltage, 16.14 mA/cm2Circuit photocurrent density, fill factor 0.70, corresponding photoelectric conversion efficiency
It is 8.28%.Light irradiates from the negative obtains 665mV open-circuit photovoltage, 10.38mA cm-2Circuit photocurrent density, filling because
Son is 0.70, and corresponding photoelectric conversion efficiency is 4.83%.It was found that the incident photon-to-electron conversion efficiency of metal selenide is very high, have very big
Application prospect.
Detailed description of the invention
Fig. 1 CoSe of the present invention2The XRD spectra of electrocatalysis material；
Fig. 2 CoSe of the present invention2The SEM of electrocatalysis material schemes；
Fig. 3 CoSe of the present invention2The cyclic voltammetry curve figure of electrocatalysis material and Pt to electrode；
Fig. 4 CoSe of the present invention2Electrocatalysis material is in quasi-solid electrolyte and Pt is to electrode electro Chemical AC impedance figure；
Fig. 5 CoSe of the present invention2The Tafel polarization curve of electrocatalysis material and Pt to electrode pair；
Fig. 6 CoSe of the present invention2Electrocatalysis material and Pt are to electrode, and group trues up the Solid Double face dye sensitization sun respectively
The J-V curve graph of energy battery.
Specific embodiment
One, experimental section
1CoSe2Electrocatalysis material preparation
(1) CoCl of the selenium powder of 0.222g and 0.238g2·6H2O is dissolved in the primary distilled water of 36mL, is added
The hydrazine hydrate of 24mL, then ultrasound 30min, then magnetic agitation 20min；
(2) uniformly mixed reactant, that pours into 100mL has in the autoclave of polytetrafluoroethyllining lining, carries out water
Thermal response, reaction temperature are 180 DEG C, reaction temperature 5h；
(3) it after hydro-thermal reaction stops, being cooled to room temperature, decompression filters, and filter cake uses primary distilled water and dehydrated alcohol respectively
It alternately rinses 10 times, obtained solid dries 2h in a vacuum drying oven, then finely ground with agate mortar, obtains CoSe2Electro-catalysis material
Material.
The encapsulation of 2 sensitization solar batteries
(2-1)CoSe2Electrocatalysis material suspension is prepared
Weigh the CoSe of 1.8mg2Electrocatalysis material, is added 5mL ethyl alcohol and 5mL ultrapure water is added in vial, then sets
Ultrasound 30min, obtains configured CoSe in ultrasonic cleaner2Electrocatalysis material suspension.
The preparation of (2-2) light anode
The TiO with a thickness of 15 μm will be loaded with2The FTO electro-conductive glass of film immerses the TiCl that concentration is 0.05 mol/L4Water
It in solution, is placed in 70 DEG C of baking oven, places 0.5h, then take out and be loaded with TiO2The electro-conductive glass of film, is rushed with deionized water
Wash clean after being dried with nitrogen, is put into Muffle furnace and is made annealing treatment: 1h to 450 DEG C of heating keeps the temperature 30min, natural cooling
To after 120 DEG C；Take out TiO2The FTO electro-conductive glass of film is put into rapidly in prepared N719 dye solution, after standing 16h,
Light anode is taken out, the N719 dyestuff of film surface physical absorption is washed with anhydrous acetonitrile after purification, then nitrogen is blown
Dry, the electrode obtained is the TiO of dye sensitization2Light anode；
The N719 dyestuff the preparation method comprises the following steps: accurately weigh N719 dyestuff 3mg, take the tertiary fourth of 5mL with disposable syringe
Pure and mild 5mL acetonitrile is dissolved in brown sample bottle, ultrasonic 30min, is kept in dark place stand-by.
The preparation of (2-3) to electrode
Its patch on the conducting surface of the FTO electro-conductive glass of 3M sticker after the pre-treatment, will be made at the pros of 0.6cm × 0.6cm
Shape；With the CoSe prepared in liquid-transfering gun aspiration step (2-1)2Electrocatalysis material hangs 10 μ L of solution, drips to FTO electro-conductive glass patch
In the square of 3M adhesive plaster one side, it is placed in infrared oven and dries after drop is good, CoSe2Material can be deposited in FTO box, weight
After operating drop coating 8 times again to electrode, the dry 2h in 100 DEG C of vacuum ovens；The electrode obtained is CoSe2Electro-catalysis material
Material preparation to electrode.
The encapsulation of (2-4) battery
The Surlyn film for taking out 30 μ m-thicks, is placed in CoSe2Electrocatalysis material preparation to electrode and dye sensitization
TiO2Between light anode, then it is placed in heat-sealing instrument hot pressing at 120 DEG C, clings, after being cooled to room temperature, to the electrode back side
Hole on drip 0.05mL quasi-solid electrolyte, so that the electrolyte on hole is fully entered inside battery, cell package is completed, and is obtained
CoSe2Electrocatalysis material makes two-sided quasi-solid-state dye sensitized solar battery.
Quasi-solid electrolyte the preparation method is as follows: in glove box under nitrogen atmosphere prepare liquid iodine electrolyte, liquid
Iodine electrolyte includes the LiI of 0.1mol/L, the I of 0.05mol/L2, the ionic liquid DMPII and 0.5mol/L of 0.6mol/L
Additive 4- tert .-butylpyridine, solvent be redistillation anhydrous acetonitrile, DMPII 1,2- dimethyl -3- propyl iodate miaow
Azoles；Then the vinylidene fluoride hexafluoropropylene copolymer of 5wt% is added into liquid iodophor electrolyte, 80 DEG C are heated to solid gum
The vinylidene of shape-perfluoropropene copolymer fully dissolved obtains quasi-solid electrolyte after cooling.
Two results and discussion
1.CoSe2Structure and morphology characterization
The XRD spectrum of metal selenide is as shown in Figure 1, CoSe as we can see from the figure22 angles θ at 24.2 °, 28.5 °,
32.6 °, 33.6 °, 36.1 °, 48.3 °, 53.2 °, it is CoSe that 63.5 ° corresponding2(011) of crystal, (101), (111),
(120), (211), (002), (031), (120) diffraction crystal face.This with can be preferable with standard spectrum graph card [PDF#52-1008]
Coincide.There is no other impurity peaks to occur in map, shows that synthesized nano material is very pure.
Synthetic product CoSe is observed using SEM2The microscopic appearance of film.As shown in Fig. 2, CoSe in figure2Shape be it is rodlike
Structure, the characterization result of SEM show through hydrothermal synthesis method, CoCl2·6H2O can be reacted with Se powder generates CoSe2It receives
Rice profile material.
2.CoSe2The characterization of electrocatalysis material catalytic activity
2.1 cyclic voltammetry
Cyclic voltammetric is a kind of test method for the electro-chemical activity and comprehensive performance of evaluating electrode class material, this
In secondary test i.e. using three-electrode system: drop coating has to electrode CoSe2The FTO glass of electrocatalysis material is working electrode (drop coating
Range is 1cm × 1cm, and dripping quantity is 220 μ L, is put into two hours in vacuum oven, 80 DEG C), Ag/Ag+For reference electricity
Pole, Pt is to electrode.Required electrolyte is the I of LiI, 1mmol/L of 10mmol/L2, 0.1mol/L LiClO4。
Cyclic voltammogram as shown in Figure 3 is measured, in CoSe2Nano material and Pt are in the CV curve of electrode material, and
One redox peaks are the reaction process of formula (1), and the second redox peaks are the reaction process of formula (2).Because in dyestuff
In the catalytic process to electrode of sensitization solar battery, major function is catalysis reduction I3 -.Therefore, the first redox
As the emphasis studied, (spike potential difference is E at peakpp).It can be seen from the figure that the E of PtppValue (0.41V) compares CoSe2EppValue
(0.33V) is big.EppIt is smaller, show that the catalytic activity of electrode material is better.Pt and CoSe2Cyclic voltammetric in identical scanning
Occur reduction peak in range, illustrates that the catalytic activity of the two is relatively high, and CoSe2Peak current it is relatively high,
Show that its catalytic performance is more preferable.
I3 -+2e-=3I- (1)
3I2+2e-=2I3 - (2)
2.2 ac impedance spectroscopy
The electrochemical alternate impedance spectrum figure of dye-sensitized solar cells can be divided into three parts, including starting point, high frequency
Area, low frequency range.As, there are two semicircle, the semicircle on the left side is that its radius size of high frequency region is R in Fig. 4ct(to electrode and electrolyte
The charge transfer resistance at interface), RctIt is smaller, indicate that the electro catalytic activity of specimen material is better；Half circular diameter of the right low frequency range
For ZN(I inside electrolyte3 -/I-The energy of electricity pair this special diffusion resistance), starting point corresponds to string in the intercept of high frequency region real axis (Z ')
Join resistance Rs.Judge that the catalytic activity of battery mainly sees left side semicircle (i.e. Rct) radius.CoSe it can be seen from Fig. 42
RctValue is 2.82 Ω, the R of Ptct3.01 Ω of value.This shows CoSe2There is higher catalytic activity relative to Pt.
2.3 Tafel polarization curves
In order to preferably measure EIS, we are polarized three times before measuring EIS each time.In general, polarization is bent
Line is made of three regions, corresponds to I in areas of high potential3 -/I-In the electrolyte the limit diffusion, low potential area be by
Caused by polarization, intermediate potential area is then the as polarized area due to caused by electric charge transfer.It is illustrated in figure 5 CoSe2With
The polarization curve of Pt, CoSe2Cathode, anode slope ratio Pt it is big.The intersection point of cathode, anode and ordinate represents battery limit
Current density.Slope is bigger, and limiting current density is bigger, and the electro catalytic activity of material is better.From fig. 5, it can be seen that CoSe2
Electro catalytic activity is better than Pt to electrode material.The consistent of result (Fig. 1) of this and AC impedance
3.CoSe2For the photoelectric property to electrode assembling battery
CoSe2With Pt as two-sided quasi-solid-state dye sensitized solar battery to J-V curve measured by electrode such as figure
Shown in 6.Relevant photoelectric parameter is shown in Table 1.CoSe2Nano material is used as to electrode, and under front illuminated, open-circuit voltage is
733mv, circuit photocurrent density are 16.14mA cm-2, fill factor 0.70, it is 8.28% that incident photon-to-electron conversion efficiency, which reaches,；Reverse side
When irradiation, open-circuit voltage 665mV, short-circuit current density is 10.38mA cm2, fill factor 0.70, incident photon-to-electron conversion efficiency
It is 4.83%.Under the conditions of same test, front illuminated Pt is to obtain 753mV open-circuit photovoltage to the quasi- solid state battery of electrode,
13.92mA cm-2Circuit photocurrent density, corresponding photoelectric conversion efficiency be 7.44%；Reverse side irradiates battery and obtains 725mV
Open-circuit photovoltage, 7.98mA cm-2Circuit photocurrent density, incident photon-to-electron conversion efficiency 4.05%.Circuit photocurrent density and
The size of incident photon-to-electron conversion efficiency is ordered as CoSe2> Pt, it is consistent with the electro catalytic activity sequence surveyed, illustrate surveyed
In material, CoSe2There is better photovoltaic performance.And reverse side irradiates CoSe2The photoelectric conversion efficiency of the quasi- solid state battery of assembling
It is also two kinds to higher in electrode material, illustrates CoSe2It is suitable as pair of two-sided quasi-solid-state dye sensitized solar battery
Electrode material not only ensure that the efficiency of front illuminated, while also have excellent reverse side illumination efficiency.
Table 1CoSe2It is the J_V data that the two-sided quasi- solid state battery of what valence is assembled to electrode material with Pt
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.
For those of ordinary skill in the art, other various forms of changes can also be made on the basis of the above description
Change or changes.There is no necessity and possibility to exhaust all the enbodiments.And obvious change extended from this
Change or changes among still in present patent application scope of protection of the claims.
Claims (10)
1.CoSe2The preparation method of electrocatalysis material, which comprises the steps of:
(1) selenium powder and cobalt salt, are dissolved in primary distilled water, and hydrazine hydrate and ammonium hydroxide is added；Then ultrasound, stir evenly；
(2) it is placed in autoclave, carries out hydro-thermal reaction；
(3) after hydro-thermal reaction stops, decompression is filtered, is cleaned, is dry.
2. CoSe according to claim 12The preparation method of electrocatalysis material, which is characterized in that in step (1),
The selenium powder of 0.222g and the CoCl of 0.238g2·6H2O is dissolved in the primary distilled water of 36mL, the hydrazine hydrate of 24mL is added, so
Ultrasound 30min afterwards, then magnetic agitation 20min.
3. CoSe according to claim 22The preparation method of electrocatalysis material, which is characterized in that in step (2), will walk
Suddenly the reactant being uniformly mixed in (1), that pours into 100mL has in the autoclave of polytetrafluoroethyllining lining, and it is anti-to carry out hydro-thermal
It answers, reaction temperature is 180 DEG C, reaction temperature 5h.
4. CoSe according to claim 12The preparation method of electrocatalysis material, which is characterized in that in step (3), hydro-thermal
It after reaction stops, being cooled to room temperature, decompression filters, and filter cake uses primary distilled water and dehydrated alcohol alternately to rinse 10 times respectively, institute
It obtains solid and dries 2h in a vacuum drying oven, then is finely ground with agate mortar, obtain CoSe2Electrocatalysis material.
5.CoSe2Application of the electrocatalysis material in two-sided quasi-solid-state dye sensitized solar battery, which is characterized in that including such as
Lower step:
(2-1)CoSe2The preparation of electrocatalysis material suspension；
The preparation of (2-2) light anode；
The preparation of (2-3) to electrode；
The encapsulation of (2-4) battery.
6. CoSe according to claim 52Electrocatalysis material answering in two-sided quasi-solid-state dye sensitized solar battery
With, which is characterized in that in step (2-1), weigh the CoSe of 1.8mg25mL ethyl alcohol and 5mL ultrapure water is added in electrocatalysis material
It is added in vial, is subsequently placed in ultrasound 30min in ultrasonic cleaner, obtains configured CoSe2Electrocatalysis material is suspended
Liquid.
7. CoSe according to claim 52Electrocatalysis material answering in two-sided quasi-solid-state dye sensitized solar battery
With, which is characterized in that in step (2-2), the TiO with a thickness of 15 μm will be loaded with2The FTO electro-conductive glass of film immerses concentration
For the TiCl of 0.05mol/L4It in aqueous solution, is placed in 70 DEG C of baking oven, places 0.5h, then take out and be loaded with TiO2Film is led
Electric glass, is rinsed well with deionized water, after being dried with nitrogen, is put into Muffle furnace and is made annealing treatment: 1h to 450 DEG C of heating,
30min is kept the temperature, after naturally cooling to 120 DEG C；Take out TiO2The FTO electro-conductive glass of film is put into rapidly prepared N719 dye
Expect in solution, after standing 16h, takes out light anode, wash film surface physical absorption with anhydrous acetonitrile after purification
N719 dyestuff, then be dried with nitrogen, the electrode obtained is the TiO of dye sensitization2Light anode；
The N719 dyestuff the preparation method comprises the following steps: accurately weigh N719 dyestuff 3mg, with disposable syringe take the 5mL tert-butyl alcohol and
5mL acetonitrile is dissolved in brown sample bottle, ultrasonic 30min, is kept in dark place stand-by.
8. CoSe according to claim 62Electrocatalysis material answering in two-sided quasi-solid-state dye sensitized solar battery
With, which is characterized in that in step (2-3), by the conducting surface of the FTO electro-conductive glass of 3M sticker after the pre-treatment, make its patch
At the square of 0.6cm × 0.6cm；With the CoSe prepared in liquid-transfering gun aspiration step (2-1)2Electrocatalysis material hangs 10 μ of solution
L is dripped in the square of FTO electro-conductive glass patch 3M adhesive plaster one side, is placed in infrared oven and is dried after drop is good, CoSe2Material meeting
Be deposited in FTO box, after repetitive operation drop coating 8 times to electrode, the dry 2h in 100 DEG C of vacuum ovens；The electrode obtained
As CoSe2Electrocatalysis material preparation to electrode.
9. CoSe according to claim 62Electrocatalysis material answering in two-sided quasi-solid-state dye sensitized solar battery
With, which is characterized in that in step (2-3), the Surlyn film of 30 μ m-thicks is taken, CoSe is placed in2Pair of electrocatalysis material preparation
The TiO of electrode and dye sensitization2Between light anode, then it is placed in heat-sealing instrument hot pressing at 120 DEG C, clings, be cooled to room temperature
Afterwards, 0.05mL quasi-solid electrolyte is dripped on the hole to the electrode back side, and the electrolyte on hole is made to fully enter inside battery, battery
Encapsulation is completed, and CoSe is obtained2Electrocatalysis material makes two-sided quasi-solid-state dye sensitized solar battery.
10. CoSe according to claim 92Electrocatalysis material answering in two-sided quasi-solid-state dye sensitized solar battery
With, which is characterized in that quasi-solid electrolyte is electrolysed the preparation method is as follows: preparing liquid iodine under nitrogen atmosphere in glove box
Matter, liquid iodine electrolyte include the LiI of 0.1mol/L, the I of 0.05mol/L2, the ionic liquid DMPII of 0.6mol/L and
The additive 4- tert .-butylpyridine of 0.5mol/L, solvent are the anhydrous acetonitrile of redistillation, DMPII 1,2- dimethyl -3- third
Base iodate imidazoles；Then the vinylidene fluoride hexafluoropropylene copolymer of 5wt%, 80 DEG C of heating are added into liquid iodophor electrolyte
To the vinylidene fluoride hexafluoropropylene copolymer fully dissolved of solid colloidal, quasi-solid electrolyte is obtained after cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810721764.8A CN108987117A (en) | 2018-07-04 | 2018-07-04 | CoSe2The preparation method of electrocatalysis material and its application in two-sided quasi-solid-state dye sensitized solar battery |
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