CN110504369B - Preparation method of high-conductivity carbon electrode - Google Patents
Preparation method of high-conductivity carbon electrode Download PDFInfo
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- CN110504369B CN110504369B CN201910610580.9A CN201910610580A CN110504369B CN 110504369 B CN110504369 B CN 110504369B CN 201910610580 A CN201910610580 A CN 201910610580A CN 110504369 B CN110504369 B CN 110504369B
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- H—ELECTRICITY
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- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
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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
- Y02E10/549—Organic PV cells
Abstract
The invention relates to a preparation method of screen-printable carbon slurry and a high-conductivity carbon electrode, which comprises the following steps: 1) Preparation of carbon slurry: mixing conductive carbon materials in proportion, wherein the conductive carbon materials comprise graphite flakes, carbon black and carbon fibers; adding ethyl cellulose and zirconia as binders, putting into a baking oven for baking, cooling to room temperature, adding turpentine permeant as a solvent, fully stirring, and uniformly mixing to obtain carbon slurry; 2) Preparation of a carbon electrode: and (3) performing screen printing on the carbon slurry in the step 1) to form the high-conductivity carbon electrode after high-temperature sintering. The beneficial effects of the invention are as follows: according to the invention, the conductivity and the conductivity of the carbon electrode are improved by adding the carbon fibers into the carbon slurry, more perovskite precursor solution is led to be uniformly filled between mesoporous bracket layers, and an independent perovskite film layer is formed between the carbon electrode layer and the zirconia mesoporous layer, so that a battery structure is formed, the cost is low, and the preparation process is simple.
Description
Technical Field
The invention relates to a preparation method of carbon slurry and a carbon electrode for a sintered carbon-based perovskite solar cell, in particular to a preparation method of a high-conductivity carbon electrode.
Background
Novel thin film solar cells have been rapidly developed in recent years, and the development speed of perovskite solar cells is particularly high. The efficiency of the material rises linearly within a few years, and at present, 24% of the material breaks through. The standard metal electrode perovskite solar cell uses organic-inorganic hybridization perovskite as a light absorption layer and uses organic micromolecular material Spiro-OMeTAD as a hole transport layer, so that the preparation environment is severely required, the raw materials are expensive, and the large-scale commercial production is not facilitated. The adoption of low-cost carbon materials to replace expensive metal electrodes and hole transport layers, and simultaneously, the reduction of the requirements on the process environment, will be a trend of large-area development of perovskite solar cells in the future.
At present, the carbon electrode used in the perovskite solar cell mainly comprises low-temperature carbon and sintered carbon, and the preparation modes of screen printing or knife coating are adopted. For low-temperature carbon slurry, the requirement on the solvent is high, even the perovskite film is influenced, the solvent in the carbon slurry cannot be completely volatilized at a lower temperature, and the residual solvent can damage the stability of the perovskite film, so that the long-term stability of the battery efficiency is influenced. In sintered carbon, this problem can be solved by high-temperature sintering, and the resistance of the sintered carbon electrode is further reduced. The main problem is that when the perovskite precursor solution permeates into the mesoporous layer through the sintered carbon, the perovskite precursor solution remains in the carbon electrode due to the obstruction of the graphite sheet, and the final efficiency of the device is affected.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a high-conductivity carbon electrode, wherein carbon fibers with a specific proportion are added into carbon slurry, so that the conductivity and the conductivity of the carbon electrode are improved, and the conversion efficiency of a perovskite solar cell is improved.
The preparation method of the screen-printable carbon paste and the high-conductivity carbon electrode comprises the following steps:
1) Preparation of carbon slurry: mixing conductive carbon materials in proportion, wherein the conductive carbon materials comprise graphite flakes, carbon black and carbon fibers; adding ethyl cellulose and zirconia as binders, putting into a baking oven for baking, cooling to room temperature, adding turpentine permeant as a solvent, fully stirring, and uniformly mixing to obtain carbon slurry;
2) Preparation of a carbon electrode: and (3) performing screen printing on the carbon slurry in the step 1) to form the high-conductivity carbon electrode after high-temperature sintering.
As preferable: in the step 1), the mass ratio of the carbon fiber, the carbon black and the graphite flake is 1-2:2:6.
As preferable: in the step 1), the drying temperature of the oven is 50-250 ℃ and the drying time is 30-90 min.
As preferable: in the step 1), the specification of the carbon fiber is as follows: the diameter is 100 nm-300 nm, the specific surface area is 1-50 g/cm 3 The length is 5-100 μm. The carbon fiber is vapor grown chopped carbon fiber, and has good mechanical property and high conductivity. In addition, the wettability of the carbon fiber and the perovskite precursor liquid is better than that of graphite flake and carbon black. The scaly graphite layers overlap, which hinders the infiltration process of perovskite precursor liquid. When carbon fibers are inserted into the graphite sheets, a bridge for connection is erected between the graphite sheets, and the carbon electrode is dredged by the perovskite precursor liquid. Therefore, the addition of the carbon fiber reduces the residue of the perovskite precursor liquid in the carbon electrode, so that the perovskite precursor liquid is more fully filled in the mesoporous bracket layer, and more effective light absorption is generated.
As preferable: in the step 1), the solid content of the conductive carbon material of the carbon slurry is 10-50%.
As preferable: in the step 1), the mixing and stirring time in the preparation process of the carbon slurry is 30-120 min.
As preferable: in the step 2), the thickness of the prepared carbon electrode is 10-30 μm.
As preferable: in the step 2), the high-temperature sintering temperature is 300-450 ℃.
As preferable: in the step 2), after the sintering is completed, the temperature is not reduced to room temperature, but the carbon electrode is taken out at 50-150 ℃.
As preferable: step 2) is followed by step 3) of preparing the perovskite solar cell: sequentially depositing a compact layer, a titanium oxide mesoporous layer, a zirconium oxide mesoporous layer and a carbon electrode layer on FTO glass, uniformly distributing perovskite precursor solution in the titanium oxide mesoporous layer and the zirconium oxide mesoporous layer through the flow guide of the carbon electrode layer, heating to form a perovskite light absorption layer, and forming an independent perovskite film layer between the carbon electrode layer and the zirconium oxide mesoporous layer to prepare a perovskite solar cell, wherein the perovskite solar cell structure sequentially comprises the compact layer, the titanium oxide mesoporous layer, the perovskite light absorption layer, the zirconium oxide mesoporous layer, the perovskite film layer and the carbon electrode layer from bottom to top; the thickness of the perovskite film layer is 100 nm-300 nm; the compact layer is a metal oxide film, the material is at least one of titanium oxide and its adulterants, zinc oxide and its adulterants, cobalt oxide and its adulterants or nickel oxide and its adulterants, and the thickness of the compact layer is 30-50 nm.
The beneficial effects of the invention are as follows: according to the invention, the carbon fiber is added into the carbon slurry, so that on one hand, the conductivity of the carbon electrode is improved, on the other hand, the conductivity of the carbon electrode is improved, more perovskite precursor solution is guided to be uniformly filled between mesoporous bracket layers, and an independent perovskite film layer is formed between the carbon electrode layer and the zirconia mesoporous layer, so that a battery structure is formed, the cost is low, the preparation process is simple, and the conversion efficiency of the perovskite solar cell is improved.
Drawings
Fig. 1 is an I-V characteristic curve of the assembled battery of examples 1 to 4 (wherein, four curves represent I-V characteristic curves of assembled batteries to which different amounts of carbon fibers were added, respectively).
Fig. 2 is an I-V characteristic curve of the assembled battery of example 3 and comparative example 1.
Fig. 3 is a schematic SEM cross-sectional view of assembled batteries of example 3 and comparative example 1.
Detailed Description
The invention is further described below with reference to examples. The following examples are presented only to aid in the understanding of the invention. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
The carbon electrode is applied to a sintered carbon-based perovskite solar cell, the cell structure comprises a compact layer, a perovskite light absorption layer, a mesoporous support layer, a perovskite film layer and a carbon electrode layer from bottom to top, the perovskite precursor solution is uniformly distributed in the mesoporous support layer through the flow guide of the carbon electrode layer, the perovskite light absorption layer is formed by heating, and an independent perovskite film layer is formed between the carbon electrode layer and a zirconia mesoporous layer, wherein the thickness of the perovskite film layer is about 100 nm-300 nm. The dense layer of the perovskite solar cell is a metal oxide film, preferably at least one of titanium oxide and its dopant, zinc oxide and its dopant, cobalt oxide and its dopant, nickel oxide and its dopant, and the thickness of the dense layer is 30-50 nm. The mesoporous support layer of the perovskite solar cell is a double-layer metal oxide mesoporous film, the lower layer is preferably titanium oxide and doping thereof, the thickness is 300-800 nm, the upper layer is preferably at least one of zirconium oxide, aluminum oxide and nickel oxide, and the thickness is 1-2 mu m.
Example 1:
(1) And (3) preparing a carbon slurry. Carbon fiber, carbon black and graphite flake powder are mixed according to the following ratio of 1:2:6, adding ethyl cellulose and zirconia as binding agents after mixing according to the mass ratio, putting into a baking oven for drying at 100 ℃, taking out, and cooling to room temperature. 28g of turpentine permeant is added, mixed and stirred for 10min, and defoamed for 20min. This was repeated 3 times.
(2) Preparation of a carbon electrode. The carbon paste was printed on the zirconia mesoporous layer to a thickness of about 15 μm, dried at 100 c, and then calcined in a muffle furnace at 430 c for 30min.
(3) Preparation of perovskite solar cell. And depositing a compact layer, a titanium oxide mesoporous layer, a zirconium oxide mesoporous layer and a carbon electrode layer on the FTO glass in sequence. Uniformly distributing perovskite precursor solution in a titanium oxide mesoporous layer and a zirconium oxide mesoporous layer through a carbon electrode, heating for 1h at 50 ℃ to form a perovskite light absorption layer, and forming an independent perovskite film layer between the zirconium oxide mesoporous layer and the carbon electrode.
Example 2:
(1) And (3) preparing a carbon slurry. Carbon fiber, carbon black and graphite flake powder are mixed according to the following ratio of 1.2:2:6, adding ethyl cellulose and zirconia as binding agents after mixing according to the mass ratio, putting into a baking oven for drying at 100 ℃, taking out, and cooling to room temperature. 28g of turpentine permeant is added, mixed and stirred for 10min, and defoamed for 20min. This was repeated 3 times.
(2) Preparation of a carbon electrode. The carbon paste was printed on the zirconia mesoporous layer to a thickness of about 15 μm, dried at 100 c, and then calcined in a muffle furnace at 430 c for 30min.
(3) Preparation of perovskite solar cell. And depositing a compact layer, a titanium oxide mesoporous layer, a zirconium oxide mesoporous layer and a carbon electrode layer on the FTO glass in sequence. Uniformly distributing perovskite precursor solution in a titanium oxide mesoporous layer and a zirconium oxide mesoporous layer through a carbon electrode, heating for 1h at 50 ℃ to form a perovskite light absorption layer, and forming an independent perovskite film layer between the zirconium oxide mesoporous layer and the carbon electrode.
Example 3:
(1) And (3) preparing a carbon slurry. Carbon fiber, carbon black and graphite flake powder according to the weight ratio of 1.5:2:6, adding ethyl cellulose and zirconia as binding agents after mixing according to the mass ratio, putting into a baking oven for drying at 100 ℃, taking out, and cooling to room temperature. 28g of turpentine permeant is added, mixed and stirred for 10min, and defoamed for 20min. This was repeated 3 times.
(2) Preparation of a carbon electrode. The carbon paste was printed on the zirconia mesoporous layer to a thickness of about 15 μm, dried at 100 c, and then calcined in a muffle furnace at 430 c for 30min.
(3) Preparation of perovskite solar cell. And depositing a compact layer, a titanium oxide mesoporous layer, a zirconium oxide mesoporous layer and a carbon electrode layer on the FTO glass in sequence. Uniformly distributing perovskite precursor solution in a titanium oxide mesoporous layer and a zirconium oxide mesoporous layer through a carbon electrode, heating for 1h at 50 ℃ to form a perovskite light absorption layer, and forming an independent perovskite film layer between the zirconium oxide mesoporous layer and the carbon electrode.
Example 4:
(1) And (3) preparing a carbon slurry. Carbon fiber, carbon black and graphite flake powder are mixed according to the following ratio of 2:2:6, adding ethyl cellulose and zirconia as binding agents after mixing according to the mass ratio, putting into a baking oven for drying at 100 ℃, taking out, and cooling to room temperature. 28g of turpentine permeant is added, mixed and stirred for 10min, and defoamed for 20min. This was repeated 3 times.
(2) Preparation of a carbon electrode. The carbon paste was printed on the zirconia mesoporous layer to a thickness of about 15 μm, dried at 100 c, and then calcined in a muffle furnace at 430 c for 30min.
(3) Preparation of perovskite solar cell. And depositing a compact layer, a titanium oxide mesoporous layer, a zirconium oxide mesoporous layer and a carbon electrode layer on the FTO glass in sequence. Uniformly distributing perovskite precursor solution in a titanium oxide mesoporous layer and a zirconium oxide mesoporous layer through a carbon electrode, heating for 1h at 50 ℃ to form a perovskite light absorption layer, and forming an independent perovskite film layer between the zirconium oxide mesoporous layer and the carbon electrode.
Comparative example 1:
(1) And (3) preparing a carbon slurry. Carbon fiber, carbon black and graphite flake powder are mixed according to the following ratio of 0:2:6, adding ethyl cellulose and zirconia as binding agents after mixing according to the mass ratio, putting into a baking oven for drying at 100 ℃, taking out, and cooling to room temperature. 28g of turpentine permeant is added, mixed and stirred for 10min, and defoamed for 20min. This was repeated 3 times.
(2) Preparation of a carbon electrode. The carbon paste was printed on the zirconia mesoporous layer to a thickness of about 15 μm, dried at 100 c, and then calcined in a muffle furnace at 430 c for 30min.
(3) Preparation of perovskite solar cell. And depositing a compact layer, a titanium oxide mesoporous layer, a zirconium oxide mesoporous layer and a carbon electrode layer on the FTO glass in sequence. Uniformly distributing the perovskite precursor solution in the titanium oxide mesoporous layer and the zirconium oxide mesoporous layer through the carbon electrode, and heating at 50 ℃ for 1h to form the perovskite light absorption layer.
The following table shows the parameters of the photoelectric performance of perovskite solar cells assembled with carbon electrodes to which different amounts of carbon fibers were added:
TABLE 1 comparison of the photovoltaic Performance parameters of perovskite solar cells assembled with carbon electrodes added with different amounts of carbon fibers
Claims (9)
1. The preparation method of the high-conductivity carbon electrode is characterized by comprising the following steps of:
1) Preparation of carbon slurry: mixing conductive carbon materials in proportion, wherein the conductive carbon materials comprise graphite flakes, carbon black and carbon fibers; adding ethyl cellulose and zirconia as binders, putting into a baking oven for baking, cooling to room temperature, adding turpentine permeant as a solvent, fully stirring, and uniformly mixing to obtain carbon slurry; the carbon fibers are added into the carbon slurry, so that the conductivity of the carbon electrode is improved, and more perovskite precursor solutions are led to be uniformly filled between mesoporous bracket layers;
in the step 1), the specification of the carbon fiber is as follows: the diameter is 100nm to 300nm, and the specific surface area is 1 g/cm to 50g/cm 3 The length is 5-100 mu m;
2) Preparation of a carbon electrode: and (3) performing screen printing on the carbon slurry in the step 1), and performing high-temperature sintering to form the carbon electrode.
2. The method for preparing a high-conductivity carbon electrode according to claim 1, wherein in the step 1), the ratio of carbon fiber, carbon black to graphite flake is 1-2:2:6.
3. The method for preparing the high-conductivity carbon electrode according to claim 1, wherein in the step 1), the drying temperature of the oven is 50-250 ℃ and the drying time is 30-90 min.
4. The method for preparing a high-conductivity carbon electrode according to claim 1, wherein in the step 1), the solid content of the conductive carbon material of the carbon paste is 10% -50%.
5. The method for preparing a high-conductivity carbon electrode according to claim 1, wherein in the step 1), the mixing and stirring time is 30-120 min in the preparation process of the carbon slurry.
6. The method for preparing a high conductivity carbon electrode according to claim 1, wherein in the step 2), the thickness of the prepared carbon electrode is 10 μm to 30 μm.
7. The method for preparing a high-conductivity carbon electrode according to claim 1, wherein in the step 2), the high-temperature sintering temperature is 300 ℃ to 450 ℃.
8. The method for preparing a high conductivity carbon electrode according to claim 1, wherein in the step 2), the carbon electrode is taken out when the temperature is reduced to 50 ℃ to 150 ℃ after the sintering is completed.
9. The method for preparing a high conductivity carbon electrode according to claim 1, wherein the step 2) is followed by the step 3), and the perovskite solar cell is prepared: sequentially depositing a compact layer, a titanium oxide mesoporous layer, a zirconium oxide mesoporous layer and a carbon electrode layer on FTO glass, uniformly distributing perovskite precursor solution in the titanium oxide mesoporous layer and the zirconium oxide mesoporous layer through the flow guide of the carbon electrode layer, heating to form a perovskite light absorption layer, and forming an independent perovskite film layer between the carbon electrode layer and the zirconium oxide mesoporous layer to prepare a perovskite solar cell, wherein the perovskite solar cell structure sequentially comprises the compact layer, the titanium oxide mesoporous layer, the perovskite light absorption layer, the zirconium oxide mesoporous layer, the perovskite film layer and the carbon electrode layer from bottom to top; the thickness of the perovskite film layer is 100 nm-300 nm; the compact layer is a metal oxide film, the material is at least one of titanium oxide and its adulterants, zinc oxide and its adulterants, cobalt oxide and its adulterants or nickel oxide and its adulterants, and the thickness of the compact layer is 30-50 nm.
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