CN110504369A - It is a kind of can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method - Google Patents

It is a kind of can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method Download PDF

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Publication number
CN110504369A
CN110504369A CN201910610580.9A CN201910610580A CN110504369A CN 110504369 A CN110504369 A CN 110504369A CN 201910610580 A CN201910610580 A CN 201910610580A CN 110504369 A CN110504369 A CN 110504369A
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carbon
layer
pastes
carbon electrode
preparation
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CN110504369B (en
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寿春晖
杨松旺
沈黎丽
金胜利
沈曲
戴豪波
尹旭军
邱鹤
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Zhejiang Zheneng Technology Environmental Protection Group Co ltd
Shanghai Institute of Ceramics of CAS
Zhejiang Energy Group Research Institute Co Ltd
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Shanghai Institute of Ceramics of CAS
Zhejiang Energy Group Research Institute Co Ltd
Zhejiang Tiandi Environmental Protection Technology Co Ltd
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    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/80Constructional details
    • H10K30/81Electrodes
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10Deposition of organic active material
    • H10K71/12Deposition of organic active material using liquid deposition, e.g. spin coating
    • H10K71/13Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/549Organic PV cells

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  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
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  • Hybrid Cells (AREA)
  • Inert Electrodes (AREA)
  • Photovoltaic Devices (AREA)

Abstract

The present invention relates to can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, comprising steps of the 1) preparation of carbon pastes: conductive carbon material being mixed in proportion, wherein conductive carbon material includes graphite flake, carbon black and carbon fiber;Ethyl cellulose and zirconium oxide are added as binder, baking oven drying is put into, the saturating alcohol of turpentine oil is added after being cooled to room temperature as solvent, is sufficiently stirred, is uniformly mixed, obtains carbon pastes;2) preparation of carbon electrode: pass through screen printing step 1) in carbon pastes form high water conservancy diversion carbon electrode after high temperature sintering.The beneficial effects of the present invention are: the present invention is by being added carbon fiber into carbon pastes, improve the electric conductivity of carbon electrode and flow conductivity, more perovskite precursor solutions are guided uniformly to fill to mesoporous bracket interlayer, and one layer of independent perovskite thin film layer is formed in carbon electrode layer and Zirconia mesoporous interlayer, and then form a kind of battery structure, low in cost, preparation process is simple.

Description

It is a kind of can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method
Technical field
The present invention relates to a kind of carbon-based perovskite of sintering carbon pastes used for solar batteries and carbon electrode preparation, it is more specific and Speech, be related to it is a kind of can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method.
Background technique
Novel thin film solar battery develops rapidly in recent years, and wherein the development speed of perovskite solar battery is fast outstanding For protrusion.Its efficiency linear ramps within the short several years, have broken through 24% at present.The metal electrode perovskite solar energy of standard Battery, using hybrid inorganic-organic perovskite as light absorbing layer, organic small molecule material Spiro-OMeTAD is hole transmission layer, Its preparation environmental requirement is harsh, and expensive raw material price is unfavorable for large-scale commercial production.It is high using cheap carbon material substitution Expensive metal electrode and hole transmission layer, while the requirement to process environments is reduced, it will be the following perovskite solar battery One trend of development larger in area.
The carbon electrode that perovskite solar battery uses at present mainly has two kinds of carbon of cryogenic carbon and sintering, uses screen printing The preparation method of brush or knife coating.For low temperature carbon pastes, the requirement to solvent is high, or even generates shadow to perovskite thin film It rings, and lower temperature cannot be guaranteed that the solvent in carbon pastes volatilizees completely, remaining solvent can be destroyed to perovskite thin film Stablize, and then influences the long-time stability of battery efficiency.In sintering carbon, which can pass through the method solution of high temperature sintering Certainly, by sintered carbon electrode, resistance also be will further decrease.Its existing main problem is, perovskite presoma When solution is infiltrated into mesoporous layer by being sintered carbon, due to the obstruction of graphite flake, perovskite precursor liquid can be remained in carbon electrode, Influence the final efficiency of device.
Summary of the invention
The purpose of the present invention is overcoming deficiency in the prior art, providing one kind can silk-screen printing carbon pastes and high water conservancy diversion carbon The carbon fiber of special ratios is added in carbon pastes, increases the flow conductivity and electric conductivity of carbon electrode for the preparation method of electrode, thus Improve the transfer efficiency of perovskite solar battery.
It is this can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, comprising the following steps:
1) preparation of carbon pastes: conductive carbon material is mixed in proportion, wherein conductive carbon material include graphite flake, carbon black and Carbon fiber;Ethyl cellulose and zirconium oxide are added as binder, baking oven drying is put into, turpentine oil is added after being cooled to room temperature Saturating alcohol is sufficiently stirred as solvent, is uniformly mixed, obtains carbon pastes;
2) preparation of carbon electrode: pass through screen printing step 1) in carbon pastes form high water conservancy diversion after high temperature sintering Carbon electrode.
As preferred: in the step 1), the ratio of carbon fiber, carbon black and graphite flake is 1~2:2:6.
As preferred: in the step 1), baking oven drying temperature be 50 DEG C~250 DEG C, drying time be 30min~ 90min。
As preferred: in the step 1), the specification of carbon fiber are as follows: diameter be 100nm~300nm, specific surface area be 1~ 50g/cm3, length is 5 μm~100 μm.Used carbon fiber is the chopped carbon fiber of vapor phase growth, and good mechanical properties are led It is electrically high.In addition, the wellability of carbon fiber and perovskite precursor liquid is more preferable than graphite flake, carbon black.Flaky graphite overlaps layer by layer, Hinder the process of osmosis of perovskite precursor liquid.And after being inserted into carbon fiber in graphite flake, just erected between graphite flake The bridge of connection plays the elicitation effect to perovskite precursor liquid in carbon electrode.Therefore, the addition of carbon fiber reduces calcium Residual of the titanium ore precursor liquid in carbon electrode, is more satisfactory filling with it into mesoporous shelf layer, and then generates more effective light It absorbs.
As preferred: in the step 1), the conductive carbon material solid content of carbon pastes is 10%~50%.
As preferred: in the step 1), the time being mixed in carbon pastes preparation process is 30min~120min.
As preferred: in the step 2), be made carbon electrode with a thickness of 10 μm~30 μm.
As preferred: in the step 2), high temperature sintering temperature is 300 DEG C~450 DEG C.
As preferred: in the step 2), after the completion of sintering, temperature not etc. is not down to room temperature, but at 50 DEG C~150 DEG C When just take out carbon electrode.
As preferred: carrying out step 3), the preparation of perovskite solar battery: on FTO glass after the step 2) It is sequentially depositing compacted zone, medium pore of titania layer, Zirconia mesoporous layer and carbon electrode layer, perovskite precursor solution passes through carbon electrode The water conservancy diversion of layer is uniformly distributed in medium pore of titania layer and Zirconia mesoporous layer, is thermally formed perovskite light absorbing layer, and in carbon Electrode layer and Zirconia mesoporous interlayer form one layer of independent perovskite thin film layer, and perovskite solar battery, calcium is prepared Titanium ore solar battery structure successively includes compacted zone, medium pore of titania layer, perovskite light absorbing layer, zirconium oxide Jie from the bottom up Aperture layer, perovskite thin film layer and carbon electrode layer;Perovskite thin film layer with a thickness of 100nm~300nm;Compacted zone is metal oxidation Object film, material are titanium oxide and its dopant, zinc oxide and its dopant, cobalt oxide and its dopant or nickel oxide and its mix At least one of sundries, compacted zone with a thickness of 30~50nm.
The beneficial effects of the present invention are: the present invention by being added carbon fiber into carbon pastes, on the one hand improves carbon electricity On the other hand the electric conductivity of pole improves the flow conductivity of carbon electrode, guide more perovskite precursor solutions uniformly fill to Mesoporous bracket interlayer, and one layer of independent perovskite thin film layer is formed in carbon electrode layer and Zirconia mesoporous interlayer, and then formed A kind of battery structure, low in cost, preparation process is simple, and improves the transfer efficiency of perovskite solar battery.
Detailed description of the invention
Fig. 1 is that (wherein, it is different to respectively represent addition for four curves for the I-V characteristic curve graph of Examples 1 to 4 assembled battery Measure the assembled battery I-V characteristic curve of carbon fiber).
Fig. 2 is the I-V characteristic curve graph of embodiment 3 and 1 assembled battery of comparative example.
Fig. 3 is the SEM sectional schematic diagram of embodiment 3 and 1 assembled battery of comparative example.
Specific embodiment
The present invention is described further below with reference to embodiment.The explanation of following embodiments is merely used to help understand this Invention.It should be pointed out that for those skilled in the art, without departing from the principle of the present invention, also Can be with several improvements and modifications are made to the present invention, these improvement and modification also fall into the protection scope of the claims in the present invention It is interior.
Carbon electrode is applied in being sintered carbon-based perovskite solar battery, which successively includes densification from the bottom up Layer, perovskite light absorbing layer, mesoporous shelf layer, perovskite thin film layer, carbon electrode layer, perovskite precursor solution pass through carbon electrode The water conservancy diversion of layer is uniformly distributed in mesoporous shelf layer, is thermally formed perovskite light absorbing layer, and be situated between in carbon electrode layer and zirconium oxide Hole interlayer forms one layer of independent perovskite thin film layer, and thickness is about 100nm~300nm.The densification of perovskite solar battery Layer is metal-oxide film, preferably titanium oxide and its dopant, zinc oxide and its dopant, cobalt oxide and its dopant, At least one of nickel oxide and its dopant, compacted zone with a thickness of 30~50nm.The mesoporous branch of perovskite solar battery Rack-layer is two layer metal oxide mesopore film, and lower layer is preferably titanium oxide and its dopant, with a thickness of 300nm~800nm, on Layer is preferably at least one of zirconium oxide, aluminium oxide, nickel oxide, with a thickness of 1 μm~2 μm.
Embodiment 1:
(1) preparation of carbon pastes.After carbon fiber, carbon black, graphite flake powder are mixed according to 1:2:6 ratio, it is fine that ethyl is added Dimension element and zirconium oxide take out after being then placed in 100 DEG C of baking oven drying, are cooled to room temperature as binder.It is saturating that 28g turpentine oil is added 10min, deaeration 20min is mixed in alcohol.3 times repeatedly.
(2) preparation of carbon electrode.Above-mentioned carbon pastes are printed on Zirconia mesoporous layer, thickness is about 15 μm, 100 DEG C It dries, then 430 DEG C of calcining 30min in Muffle furnace.
(3) preparation of perovskite solar battery.Compacted zone, medium pore of titania layer, oxidation are sequentially depositing on FTO glass The mesoporous layer of zirconium and carbon electrode layer.Perovskite precursor solution is evenly distributed on medium pore of titania layer and zirconium oxide by carbon electrode In mesoporous layer, after 50 DEG C of heating 1h, perovskite light absorbing layer is formed, and form one in Zirconia mesoporous layer and carbon electrode interlayer The independent perovskite thin film layer of layer.
Embodiment 2:
(1) preparation of carbon pastes.After carbon fiber, carbon black, graphite flake powder are mixed according to 1.2:2:6 ratio, ethyl is added Cellulose and zirconium oxide take out after being then placed in 100 DEG C of baking oven drying, are cooled to room temperature as binder.28g turpentine oil is added 10min, deaeration 20min is mixed in saturating alcohol.3 times repeatedly.
(2) preparation of carbon electrode.Above-mentioned carbon pastes are printed on Zirconia mesoporous layer, thickness is about 15 μm, 100 DEG C It dries, then 430 DEG C of calcining 30min in Muffle furnace.
(3) preparation of perovskite solar battery.Compacted zone, medium pore of titania layer, oxidation are sequentially depositing on FTO glass The mesoporous layer of zirconium and carbon electrode layer.Perovskite precursor solution is evenly distributed on medium pore of titania layer and zirconium oxide by carbon electrode In mesoporous layer, after 50 DEG C of heating 1h, perovskite light absorbing layer is formed, and form one in Zirconia mesoporous layer and carbon electrode interlayer The independent perovskite thin film layer of layer.
Embodiment 3:
(1) preparation of carbon pastes.After carbon fiber, carbon black, graphite flake powder are mixed according to 1.5:2:6 ratio, ethyl is added Cellulose and zirconium oxide take out after being then placed in 100 DEG C of baking oven drying, are cooled to room temperature as binder.28g turpentine oil is added 10min, deaeration 20min is mixed in saturating alcohol.3 times repeatedly.
(2) preparation of carbon electrode.Above-mentioned carbon pastes are printed on Zirconia mesoporous layer, thickness is about 15 μm, 100 DEG C It dries, then 430 DEG C of calcining 30min in Muffle furnace.
(3) preparation of perovskite solar battery.Compacted zone, medium pore of titania layer, oxidation are sequentially depositing on FTO glass The mesoporous layer of zirconium and carbon electrode layer.Perovskite precursor solution is evenly distributed on medium pore of titania layer and zirconium oxide by carbon electrode In mesoporous layer, after 50 DEG C of heating 1h, perovskite light absorbing layer is formed, and form one in Zirconia mesoporous layer and carbon electrode interlayer The independent perovskite thin film layer of layer.
Embodiment 4:
(1) preparation of carbon pastes.After carbon fiber, carbon black, graphite flake powder are mixed according to 2:2:6 ratio, it is fine that ethyl is added Dimension element and zirconium oxide take out after being then placed in 100 DEG C of baking oven drying, are cooled to room temperature as binder.It is saturating that 28g turpentine oil is added 10min, deaeration 20min is mixed in alcohol.3 times repeatedly.
(2) preparation of carbon electrode.Above-mentioned carbon pastes are printed on Zirconia mesoporous layer, thickness is about 15 μm, 100 DEG C It dries, then 430 DEG C of calcining 30min in Muffle furnace.
(3) preparation of perovskite solar battery.Compacted zone, medium pore of titania layer, oxidation are sequentially depositing on FTO glass The mesoporous layer of zirconium and carbon electrode layer.Perovskite precursor solution is evenly distributed on medium pore of titania layer and zirconium oxide by carbon electrode In mesoporous layer, after 50 DEG C of heating 1h, perovskite light absorbing layer is formed, and form one in Zirconia mesoporous layer and carbon electrode interlayer The independent perovskite thin film layer of layer.
Comparative example 1:
(1) preparation of carbon pastes.After carbon fiber, carbon black, graphite flake powder are mixed according to 0:2:6 ratio, it is fine that ethyl is added Dimension element and zirconium oxide take out after being then placed in 100 DEG C of baking oven drying, are cooled to room temperature as binder.It is saturating that 28g turpentine oil is added 10min, deaeration 20min is mixed in alcohol.3 times repeatedly.
(2) preparation of carbon electrode.Above-mentioned carbon pastes are printed on Zirconia mesoporous layer, thickness is about 15 μm, 100 DEG C It dries, then 430 DEG C of calcining 30min in Muffle furnace.
(3) preparation of perovskite solar battery.Compacted zone, medium pore of titania layer, oxidation are sequentially depositing on FTO glass The mesoporous layer of zirconium and carbon electrode layer.Perovskite precursor solution is evenly distributed on medium pore of titania layer and zirconium oxide by carbon electrode In mesoporous layer, after 50 DEG C of heating 1h, perovskite light absorbing layer is formed.
Following table is to add the photoelectric properties parameter of the perovskite solar battery of carbon electrode assembling of not same amount carbon fiber:
The photoelectric properties parameter that table 1 adds the perovskite solar battery of the carbon electrode assembling of not same amount carbon fiber compares

Claims (10)

1. one kind can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, which comprises the following steps:
1) preparation of carbon pastes: conductive carbon material is mixed in proportion, and wherein conductive carbon material includes graphite flake, carbon black and carbon fiber Dimension;Ethyl cellulose and zirconium oxide are added as binder, baking oven drying is put into, the saturating alcohol of turpentine oil is added after being cooled to room temperature It as solvent, is sufficiently stirred, is uniformly mixed, obtains carbon pastes;
2) preparation of carbon electrode: pass through screen printing step 1) in carbon pastes, after high temperature sintering, formed carbon electrode.
2. it is according to claim 1 can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, which is characterized in that In the step 1), the ratio of carbon fiber, carbon black and graphite flake is 1~2:2:6.
3. it is according to claim 1 can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, which is characterized in that In the step 1), baking oven drying temperature is 50 DEG C~250 DEG C, and drying time is 30min~90min.
4. it is according to claim 1 can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, which is characterized in that In the step 1), the specification of carbon fiber are as follows: diameter is 100nm~300nm, and specific surface area is 1~50g/cm3, length is 5 μm ~100 μm.
5. it is according to claim 1 can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, which is characterized in that In the step 1), the conductive carbon material solid content of carbon pastes is 10%~50%.
6. it is according to claim 1 can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, which is characterized in that In the step 1), the time being mixed in carbon pastes preparation process is 30min~120min.
7. it is according to claim 1 can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, which is characterized in that In the step 2), be made carbon electrode with a thickness of 10 μm~30 μm.
8. it is according to claim 1 can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, which is characterized in that In the step 2), high temperature sintering temperature is 300 DEG C~450 DEG C.
9. it is according to claim 1 can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, which is characterized in that In the step 2), after the completion of sintering, temperature takes out carbon electrode when being down to 50 DEG C~150 DEG C.
10. it is according to claim 1 can silk-screen printing carbon pastes and high water conservancy diversion carbon electrode preparation method, feature exists Step 3) is carried out after, the step 2), the preparation of perovskite solar battery: be sequentially depositing on FTO glass compacted zone, Medium pore of titania layer, Zirconia mesoporous layer and carbon electrode layer, perovskite precursor solution are uniformly divided by the water conservancy diversion of carbon electrode layer It is distributed in medium pore of titania layer and Zirconia mesoporous layer, is thermally formed perovskite light absorbing layer, and in carbon electrode layer and zirconium oxide Mesoporous interlayer forms one layer of independent perovskite thin film layer, and perovskite solar battery, perovskite solar battery is prepared Structure is successively thin including compacted zone, medium pore of titania layer, perovskite light absorbing layer, Zirconia mesoporous layer, perovskite from the bottom up Film layer and carbon electrode layer;Perovskite thin film layer with a thickness of 100nm~300nm;Compacted zone is metal-oxide film, and material is In titanium oxide and its dopant, zinc oxide and its dopant, cobalt oxide and its dopant or nickel oxide and its dopant at least One kind, compacted zone with a thickness of 30~50nm.
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CN108922653A (en) * 2018-06-30 2018-11-30 中国科学院上海硅酸盐研究所 A kind of perovskite carbon pastes used for solar batteries and electrode
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
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014135270A (en) * 2012-12-10 2014-07-24 Mitsubishi Rayon Co Ltd Porous carbon electrode and method of manufacturing the same
CN108269918A (en) * 2016-12-31 2018-07-10 中国科学院上海硅酸盐研究所 Porous perovskite thin film, carbon pastes and the solar cell based on carbon electrode
CN107146847A (en) * 2017-05-16 2017-09-08 华中科技大学 It is a kind of new based on all solid state printable perovskite solar cell of carbon electrode
US10290432B1 (en) * 2018-02-13 2019-05-14 Nano And Advanced Materials Institute Limited Method for forming perovskite solar cell with printable carbon electrode
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