CN107275493A - Preparation method of all print perovskite high osmosis porous carbon used for solar batteries to electrode - Google Patents
Preparation method of all print perovskite high osmosis porous carbon used for solar batteries to electrode Download PDFInfo
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- CN107275493A CN107275493A CN201710396871.3A CN201710396871A CN107275493A CN 107275493 A CN107275493 A CN 107275493A CN 201710396871 A CN201710396871 A CN 201710396871A CN 107275493 A CN107275493 A CN 107275493A
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/60—Forming conductive regions or layers, e.g. electrodes
- H10K71/611—Forming conductive regions or layers, e.g. electrodes using printing deposition, e.g. ink jet printing
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Abstract
The present invention relates to a kind of preparation method of all print perovskite high osmosis porous carbon used for solar batteries to electrode.This method adds polystyrene spheres in carbon pastes, prepares carbon-coating by silk-screen printing, after high temperature sintering, porous carbon is obtained to electrode by the decomposition of polystyrene spheres in carbon-coating.Simultaneously the carbon of different performance can be prepared to electrode by changing the size and addition of polystyrene spheres.The inventive method is simple, workable, with low cost.Compared with prior art, the porous carbon prepared by the present invention, to electrode, can be CH3NH3PbI3The passage permeated downwards is provided, increases its filling rate in mesoporous layer, the discreteness that battery efficiency is reduced while can print the battery efficiency of perovskite solar cell without hole transmission layer is lifted.
Description
Technical field
The present invention relates to a kind of porous carbon to electrode, and in particular to a kind of all print perovskite Thief zone used for solar batteries
Preparation method of the property porous carbon to electrode.
Background technology
Solar cell development is maked rapid progress.Miyasaka seminars in 2009 are first by perovskite material
(CH3NH3PbI3) it is elected to be sensitizer and applied to solar cell, and obtain 3.8% photoelectric transformation efficiency.With research people
Member continually develops new material and optimization preparation technology, and battery efficiency constantly refreshes and stability is further lifted, by the end of
Current PSCs highest photoelectric transformation efficiencies have broken through 22%.That the battery device is selected is still conventional structure (c-TiO2/m-
TiO2/CH3NH3PbI3/ spiro-OMeTAD/Au), although the PSCs based on this structure has higher photoelectric transformation efficiency, but simultaneously
It is not suitable for commercial applications.One of principal element be use in such battery structure to electrode by noble metal system
Standby, cost is higher.Carbon material exists extensively in the Nature, and has been widely used in social life.With metal material phase
Compare, carbon material (CNT, activated carbon, carbon black, fullerene, graphite, graphene etc.) has many special excellent properties.
Carbon is applied in DSSC to electrode and obtains preferable performance.2013, Han seminars were in exploitation
Carbon is firstly introduced in printable PSCs to electrode, and obtains 6.64% photoelectric transformation efficiency.
In prepared by current printable PSCs, carbon is fine by graphite, carbon black, zirconium oxide, ethyl by printing to electrode
The slurry of dimension element composition is obtained, and the electrode of gained is loose structure, and comparatively dense.In subsequent device preparatory phase,
CH3NH3PbI3Precursor solution is added in the way of drop coating, to obtain higher device performance, CH3NH3PbI3Precursor liquid should be complete
Carbon electrode is penetrated entirely, and is sufficient filling with following TiO2Layer.But carbon prepared by current conventional method is to electrode, right
CH3NH3PbI3Process of osmosis still have larger obstruction.To solve the above problems, there is scholar to propose to use ordered mesopore carbon as carbon
To electrode, so as to improve CH3NH3PbI3Permeability.However, the method has that preparation process is complicated, pore size is smaller etc. and lacked
Fall into.This patent adds the transformable PS balls of diameter, porous and hole is prepared to reach on the premise of traditional carbon pastes are not changed
Size manageable carbon in road is to electrode.
The content of the invention
It is an object of the invention to provide one kind is simple and effective, method of the porous carbon to electrode is prepared, is specially one kind
Preparation method of all print perovskite high osmosis porous carbon used for solar batteries to electrode.
The present invention is achieved by the following technical solutions:
A kind of preparation method of all print perovskite high osmosis porous carbon used for solar batteries to electrode, it is characterised in that bag
Include following steps:
(1) preparation of carbon pastes
After graphite, zirconium oxide, carbon black and polystyrene spheres are mixed, absolute ethyl alcohol is added, passes through magnetic agitation, ultrasound point
Dissipating makes slurry fully dispersed uniform, and above-mentioned steps are in triplicate;Then above-mentioned solution is subjected to centrifugation and obtains sediment, then will
Sediment is redissolved in absolute ethyl alcohol, is separately added into terpinol, ethyl cellulose/ethanol solution and repeats magnetic agitation and ultrasound
Dispersion steps;Finally ethanol will be evaporated off after above-mentioned slurry ball milling 10h, so as to obtain carbon pastes needed for experiment;
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print;
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after high annealing, obtains porous carbon to electrode.
The average diameter of polystyrene spheres is 0.1~8 μm in step (1).
It is 5.6g, graphite, zirconium oxide, carbon black that graphite, zirconium oxide, carbon black and polystyrene gross mass are kept in step (1)
Mass ratio be 4:0.6:1, the mass fraction of polystyrene spheres is 0.1%~30%.It is preferred that the mass fraction of polystyrene spheres
For 10%.
Centrifugation rate is 4500rpm, time 5min in step (1).
The terpinol quality of addition is 8.21g in step (1).
The mass fraction of ethyl cellulose is 10% in ethyl cellulose/ethanol solution in step (1).
Rotary evaporation is 45 DEG C, 3 hours in step (1).
The annealing temperature of carbon-coating is 400~500 DEG C in step (3), is incubated 1 hour.
In order to ensure CH3NH3PbI3Precursor solution can smoothly enter TiO2Layer, the present invention is made from polystyrene spheres
It is added to for pore creating material in carbon pastes and prepares porous carbon to electrode.At normal temperatures, the property of polystyrene is relatively stable, and density is about
For 0.02~0.04g/cm3, its fusing point is 70~115 DEG C, and decomposition temperature is 70~350 DEG C, and at high temperature, polystyrene spheres
After decomposition, substantially without residue.Compared to the complexity of mesoporous carbon preparation process, polystyrene spheres preparation method letter in this method
It is single and easily operated.
Compared with prior art, the invention has the advantages that and beneficial effect:
The inventive method is simple to operate, cost-effective, using polystyrene spheres as pore creating material, is added in carbon pastes,
High annealing after film forming is printed, polystyrene spheres pyrolytic forms pore space structure in carbon is to electrode.Prepared by this method many
Hole carbon can be as the carbon without the printable perovskite solar cell of hole transmission layer to electrode, and it is CH3NH3PbI3There is provided downward
The passage of infiltration, increases CH3NH3PbI3Filling rate in mesoporous layer, lifting battery efficiency while reduce battery efficiency from
Dissipate property.
Brief description of the drawings
Fig. 1 is used for preparation flow schematic diagram during battery device for porous carbon in embodiment 1 to electrode.
Fig. 2 calcines front and rear surface scan electron microscope for porous carbon in embodiment 1 to electrode.
Fig. 3 calcines front and rear cross-sectional scans electron microscope for porous carbon in embodiment 1 to electrode.
Fig. 4 is J-V curve of the porous carbon in embodiment 1 to battery after electrode assembling device.
Fig. 5 is discreteness figure of the porous carbon in embodiment 1 to battery efficiency after electrode assembling device.
Fig. 6 is that different polystyrene spheres dopings prepare porous carbon to J-V curve maps after electrode assembling device.
Embodiment
With reference to embodiment, the invention will be further described, and these embodiments are only intended to the explanation present invention, but this
The protection domain of invention is not limited to following embodiments.
Embodiment 1
(1) preparation of carbon pastes
A certain amount of 3.6g graphite, 0.54g zirconium oxides, 0.90g carbon blacks and 0.56g polystyrene spheres are weighed respectively first to put
Enter into beaker, adding 60ml absolute ethyl alcohols, magnetic agitation 5min, ultrasonic disperse 5min, then magnetic agitation 5min, (step is repeated
Three times);Secondly above-mentioned solution is subjected to centrifugation and obtains sediment.Sediment is then redissolved in absolute ethyl alcohol, is separately added into
Terpinol, ethyl cellulose/ethanol solution simultaneously repeat magnetic agitation and ultrasonic disperse step;Finally by above-mentioned slurry ball milling 10h
Ethanol is removed using Rotary Evaporators afterwards, so as to obtain carbon pastes needed for experiment.
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print.
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after 400 DEG C of high annealings, obtains porous carbon to electrode.
Embodiment 2
(1) preparation of carbon pastes
Weigh a certain amount of 4g graphite, 0.6g zirconium oxides, 1g carbon blacks and 0g polystyrene spheres respectively first and be put into beaker
In, add absolute ethyl alcohol, magnetic agitation 5min, ultrasonic disperse 5min, then magnetic agitation 5min (step is in triplicate);Secondly will
Above-mentioned solution carries out centrifugation and obtains sediment.Sediment is then redissolved in absolute ethyl alcohol, terpinol, ethyl is separately added into fine
Tie up element/ethanol solution and repeat magnetic agitation and ultrasonic disperse step;Finally rotary evaporation will be used after above-mentioned slurry ball milling 10h
Instrument removes ethanol, so as to obtain carbon pastes needed for experiment.
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print.
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after 400 DEG C of high annealings, obtains porous carbon to electrode.
Embodiment 3
(1) preparation of carbon pastes
A certain amount of 3.8g graphite, 0.57g zirconium oxides, 0.95g carbon blacks and 0.28g polystyrene spheres are weighed respectively first to put
Enter into beaker, adding absolute ethyl alcohol, magnetic agitation 5min, ultrasonic disperse 5min, then magnetic agitation 5min, (step repeats three
It is secondary);Secondly above-mentioned solution is subjected to centrifugation and obtains sediment.Sediment is then redissolved in absolute ethyl alcohol, pine is separately added into
Oleyl alcohol, ethyl cellulose/ethanol solution simultaneously repeat magnetic agitation and ultrasonic disperse step;Finally by after above-mentioned slurry ball milling 10h
Ethanol is removed using Rotary Evaporators, so as to obtain carbon pastes needed for experiment.
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print.
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after 400 DEG C of high annealings, obtains porous carbon to electrode.
Embodiment 4
(1) preparation of carbon pastes
A certain amount of 2.8g graphite, 0.42g zirconium oxides, 0.7g carbon blacks and 1.68g polystyrene spheres are weighed respectively first to put
Enter into beaker, adding absolute ethyl alcohol, magnetic agitation 5min, ultrasonic disperse 5min, then magnetic agitation 5min, (step repeats three
It is secondary);Secondly above-mentioned solution is subjected to centrifugation and obtains sediment.Sediment is then redissolved in absolute ethyl alcohol, pine is separately added into
Oleyl alcohol, ethyl cellulose/ethanol solution simultaneously repeat magnetic agitation and ultrasonic disperse step;Finally by after above-mentioned slurry ball milling 10h
Ethanol is removed using Rotary Evaporators, so as to obtain carbon pastes needed for experiment.
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print.
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after 400 DEG C of high annealings, obtains porous carbon to electrode.
Addition is we illustrated below distinguishes 0%, 5%, 10% and 30% i.e. embodiment 2,3,1 and 4 (by appearance in text
Performance comparison figure sequentially), such as Fig. 6 (J-V curve maps);This other data can also be shown with the form of form, such as table 1
It is shown.)
The different polystyrene spheres dopings of table 1. prepare average behavior parameter of the porous carbon to electrode assembling device
Fig. 6 and table 1 are reflected after addition 10%PS balls, and battery performance lifting effect is best.
Embodiment 5
(1) preparation of carbon pastes
Measure 10ml original carbon pastes (the wherein graphite prepared respectively first:Zirconium oxide:Carbon black=1:0.15:
0.25) it is put into 0ml polystyrene spheres in beaker, adds absolute ethyl alcohol, magnetic agitation 5min, ultrasonic disperse 5min, then magnetic
Power stirring 5min (step is in triplicate);Finally ethanol will be removed using Rotary Evaporators after above-mentioned slurry ball milling 10h, so as to obtain
Required carbon pastes must be tested.
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print.
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after 350 DEG C of high annealings, obtains porous carbon to electrode.
Embodiment 6
(1) preparation of carbon pastes
Measure 5ml original carbon pastes (the wherein graphite prepared respectively first:Zirconium oxide:Carbon black=1:0.15:
0.25) it is put into 5ml polystyrene spheres in beaker, adds absolute ethyl alcohol, magnetic agitation 5min, ultrasonic disperse 5min, then magnetic
Power stirring 5min (step is in triplicate);Finally ethanol will be removed using Rotary Evaporators after above-mentioned slurry ball milling 10h, so as to obtain
Required carbon pastes must be tested.
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print.
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after 350 DEG C of high annealings, obtains porous carbon to electrode.
Embodiment 7
(1) preparation of carbon pastes
Measure 5ml original carbon pastes (the wherein graphite prepared respectively first:Zirconium oxide:Carbon black=1:0.15:
0.25) it is put into 5ml polystyrene spheres in beaker, adds absolute ethyl alcohol, magnetic agitation 5min, ultrasonic disperse 5min, then magnetic
Power stirring 5min (step is in triplicate);Finally ethanol will be removed using Rotary Evaporators after above-mentioned slurry ball milling 10h, so as to obtain
Required carbon pastes must be tested.
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print.
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after 500 DEG C of high annealings, obtains porous carbon to electrode.
Embodiment 8
(1) preparation of carbon pastes
Measure 5ml original carbon pastes (the wherein graphite prepared respectively first:Zirconium oxide:Carbon black=1:0.15:
0.25) it is put into 5ml polystyrene spheres (0.1 μm) in beaker, adds absolute ethyl alcohol, magnetic agitation 5min, ultrasonic disperse
5min, then magnetic agitation 5min (step is in triplicate);Second finally will be removed using Rotary Evaporators after above-mentioned slurry ball milling 10h
Alcohol, so as to obtain carbon pastes needed for experiment.
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print.
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after 400 DEG C of high annealings, obtains porous carbon to electrode.
Embodiment 9
(1) preparation of carbon pastes
Measure 5ml original carbon pastes (the wherein graphite prepared respectively first:Zirconium oxide:Carbon black=1:0.15:
0.25) it is put into 5ml polystyrene spheres (8 μm) in beaker, addition absolute ethyl alcohol, magnetic agitation 5min, ultrasonic disperse 5min,
Magnetic agitation 5min again (step is in triplicate);Finally ethanol will be removed using Rotary Evaporators after above-mentioned slurry ball milling 10h, from
And obtain carbon pastes needed for experiment.
(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print.
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after 400 DEG C of high annealings, obtains porous carbon to electrode.
Claims (9)
1. a kind of all print perovskite high osmosis porous carbon used for solar batteries is to the preparation method of electrode, it is characterised in that including
Following steps:
(1) preparation of carbon pastes
After graphite, zirconium oxide, carbon black and polystyrene spheres are mixed, absolute ethyl alcohol is added, is made by magnetic agitation, ultrasonic disperse
Slurry is fully dispersed uniform, and above-mentioned steps are in triplicate;Then above-mentioned solution is subjected to centrifugation and obtains sediment, then will precipitation
Thing is redissolved in absolute ethyl alcohol, is separately added into terpinol, ethyl cellulose/ethanol solution and repeats magnetic agitation and ultrasonic disperse
Step;Finally ethanol will be evaporated off after above-mentioned slurry ball milling 10h, so as to obtain carbon pastes needed for experiment;(2) prepared by the printing of carbon-coating
The carbon pastes prepared are prepared into carbon-coating by screen printer print;
(3) preparation of the carbon to electrode
The carbon-coating that above-mentioned steps are prepared is put into stove and carried out after high annealing, obtains porous carbon to electrode.
2. the preparation method of described all print perovskite high osmosis porous carbon used for solar batteries to electrode is required according to right 1,
It is characterized in that:The average diameter of polystyrene spheres is 0.1~8 μm in step (1).
3. the preparation method of described all print perovskite high osmosis porous carbon used for solar batteries to electrode is required according to right 1,
It is characterized in that:It is 5.6g, graphite, zirconium oxide, charcoal that graphite, zirconium oxide, carbon black and polystyrene gross mass are kept in step (1)
Black mass ratio is 4:0.6:1, the mass fraction of polystyrene spheres is 0.1%~30%.
4. require that described addition polystyrene spheres prepare method of the porous carbon to electrode according to right 3, it is characterised in that:Step
(1) it is 5.6g that graphite, zirconium oxide, carbon black and polystyrene gross mass are kept in, and graphite, zirconium oxide, the mass ratio of carbon black are 4:
0.6:1, the mass fraction of polystyrene spheres is 10%.
5. the preparation method of described all print perovskite high osmosis porous carbon used for solar batteries to electrode is required according to right 1,
It is characterized in that:Centrifugation rate is 4500rpm, time 5min in step (1).
6. the preparation method of described all print perovskite high osmosis porous carbon used for solar batteries to electrode is required according to right 1,
It is characterized in that:The terpinol quality of addition is 8.21g in step (1).
7. the preparation method of described all print perovskite high osmosis porous carbon used for solar batteries to electrode is required according to right 1,
It is characterized in that:The mass fraction of ethyl cellulose is 10% in ethyl cellulose/ethanol solution in step (1).
8. the preparation method of described all print perovskite high osmosis porous carbon used for solar batteries to electrode is required according to right 1,
It is characterized in that:Rotary evaporation is 45 DEG C, 3 hours in step (1).
9. the preparation method of described all print perovskite high osmosis porous carbon used for solar batteries to electrode is required according to right 1,
It is characterized in that:The annealing temperature of carbon-coating is 400~500 DEG C in step (3), is incubated 1 hour.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108922654A (en) * | 2018-06-30 | 2018-11-30 | 中国科学院上海硅酸盐研究所 | A kind of low temperature can silk-screen printing carbon pastes and high conductivity carbon electrode |
CN109585054A (en) * | 2018-12-12 | 2019-04-05 | 新疆大学 | The dry conductive carbon paste of green solvent Shift Method is applied to perovskite solar battery |
CN109671849A (en) * | 2018-12-18 | 2019-04-23 | 中国科学院半导体研究所 | Mesoporous carbon electrode and preparation method thereof for carbon-based perovskite solar battery |
CN110797463A (en) * | 2019-10-30 | 2020-02-14 | 华中科技大学 | Carbon counter electrode perovskite solar cell and preparation method thereof |
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CN101388294A (en) * | 2008-08-07 | 2009-03-18 | 中国科学院物理研究所 | Full carbon counter electrode dye-sensitized solar cell and preparing method |
KR20120105823A (en) * | 2011-03-16 | 2012-09-26 | 고려대학교 산학협력단 | Ordered hierarchical nano-structured carbon for li storage and lithium secondary battery comprising the same |
CN103848413A (en) * | 2012-12-05 | 2014-06-11 | 中国科学院上海硅酸盐研究所 | Preparation method of mesoporous carbon sphere material |
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CN101388294A (en) * | 2008-08-07 | 2009-03-18 | 中国科学院物理研究所 | Full carbon counter electrode dye-sensitized solar cell and preparing method |
KR20120105823A (en) * | 2011-03-16 | 2012-09-26 | 고려대학교 산학협력단 | Ordered hierarchical nano-structured carbon for li storage and lithium secondary battery comprising the same |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108922654A (en) * | 2018-06-30 | 2018-11-30 | 中国科学院上海硅酸盐研究所 | A kind of low temperature can silk-screen printing carbon pastes and high conductivity carbon electrode |
CN109585054A (en) * | 2018-12-12 | 2019-04-05 | 新疆大学 | The dry conductive carbon paste of green solvent Shift Method is applied to perovskite solar battery |
CN109671849A (en) * | 2018-12-18 | 2019-04-23 | 中国科学院半导体研究所 | Mesoporous carbon electrode and preparation method thereof for carbon-based perovskite solar battery |
CN110797463A (en) * | 2019-10-30 | 2020-02-14 | 华中科技大学 | Carbon counter electrode perovskite solar cell and preparation method thereof |
CN110797463B (en) * | 2019-10-30 | 2021-08-20 | 华中科技大学 | Carbon counter electrode perovskite solar cell and preparation method thereof |
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