CN107275486A - Double-deck double yardstick composite construction oxide titanium deoxid films and its preparation technology and purposes - Google Patents
Double-deck double yardstick composite construction oxide titanium deoxid films and its preparation technology and purposes Download PDFInfo
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- CN107275486A CN107275486A CN201710375600.XA CN201710375600A CN107275486A CN 107275486 A CN107275486 A CN 107275486A CN 201710375600 A CN201710375600 A CN 201710375600A CN 107275486 A CN107275486 A CN 107275486A
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Abstract
The present invention discloses a kind of double-deck double yardstick composite construction oxide titanium deoxid films and its preparation technology and purposes, including the second material layer that the primary structure titanium oxide with hole, the little particle secondary structure titanium oxide of filling primary structure titanium oxide hole formation compact texture and the little particle oxide above secondary structure titanium oxide are constituted.Film of the present invention, using TiCl4For titanium source, with the method for low temperature hydrolysis, using relatively small particles filled big hole, form more dense film, and with other modified oxide titanium dioxide, battery efficiency can be greatly improved in perovskite solar cell by applying, stability and reduce back stagnant.The film has preparation technology simple, and raw material sources are wide and cheap, and the matrix that can be deposited on any size is first-class a little, can further promote the commercialization process of perovskite solar cell.
Description
Technical field
The present invention relates to nano-titanium dioxide film technical field, a kind of double-deck double yardstick composite construction oxidations are mainly related to
Thing-titanium deoxid film and its preparation technology.
Background technology
Since the industrial revolution, the mankind increasingly increase the demand of the energy, and which results in energy crisis on the earth is serious, aggravation
The pollution of environment, therefore it is extremely urgent to develop clean reproducible energy.The renewable sources of energy are water energy, the wind that can be regenerated
The general designation of energy, solar energy, geothermal energy, biological energy source and ocean energy etc..Solar energy is both primary energy, is regenerative resource again.It
Aboundresources, both can freely be used, and without transport, to environment without any pollution.And do not limited because it has by geographical conditions,
Efficiently, the advantage such as cleaning, low cost and receive much concern.Wherein, photoelectrical solar conversion is that solar energy is directly changed into electric energy,
It is one of research topic that countries in the world government most payes attention to.One of important way of photoelectrical solar conversion is to prepare solar-electricity
Pond.
Titanium dioxide, in photocatalysis, the field such as solar power generation has a wide range of applications always.Using titanium dioxide as electricity
Sub- transport layer, new organic inorganic hybridization perovskite solar cell, from 2009 to 2017, its electricity conversion
It is fast-developing to 22.1% from 3.8%, it is shown that huge potentiality.Titanium dioxide is generally answered with loose structure and compact texture
In perovskite solar cell.Because the titanium deoxid film of loose structure needs the high temperature sintering more than 450 DEG C, and
Uniform large-area preparation is difficult to, people begin to use the titanium deoxid film of compact texture.The titanium dioxide of compact texture
The preparation method of film mainly has spin coating colloidal solution, magnetron sputtering, ald and spray pyrolysis.However, these sides
Method, otherwise with high costs, low production efficiency, otherwise there is still a need for high-temperature process.Also, the titanium dioxide of simple compact texture
There are many defects and under ultraviolet light in film, cause perovskite solar battery efficiency low, unstable, also
In the presence of it is serious return it is stagnant.In order to solve these problems, people start to be doped titanium deoxid film or surface modification, than
Chlorine is such as mixed in titanium dioxide, can be very good to solve back stagnant problem；With the very thin film modified dioxy of cesium bromide or C60
Change titanium film to can be very good to improve the stability of battery.
But people can only solve the subproblem of titanium dioxide at present.If can simultaneously titanium dioxide large area,
Low temperature preparation and stability problem, perovskite solar cell will be commercialized quickly.
The content of the invention
It is an object of the invention to provide a kind of double-deck double yardstick composite construction oxide-titanium deoxid films and its preparation
Technique and purposes, the film can reduce titanium dioxide surface defect state well, can be greatly improved as electron transfer layer
The efficiency and stability of perovskite solar cell, moreover it is possible to reduce back stagnant.
To achieve these goals, the present invention is adopted the following technical scheme that：
Double-deck double yardstick composite construction oxide-titanium deoxid films, including the primary structure titanium oxide with hole, fill out
Fill the little particle secondary structure titanium oxide of primary structure titanium oxide hole formation compact texture and on secondary structure titanium oxide
The second material layer that the little particle oxide of side is constituted.
Further, the particle size of primary structure titanium oxide is 5-100nm, and pore size is 5-50nm, and thickness is 20-
300nm；The particle size of little particle secondary structure titanium oxide is 3-50nm；Little particle secondary structure titanium oxide is not only once being tied
It is distributed in structure titanium oxide space, while in surface distributed, thickness is 3-100nm.
Further, the particle size for the second material layer that little particle oxide is constituted is 3-70nm, and thickness is 3-
100nm。
Further, the second material layer that little particle oxide is constituted is in the little particle secondary structure titanium oxide of compact texture
The heterogeneous forming core in top, and form firm combination with titanium dioxide.
Further, the material for the second material layer that little particle oxide is constituted is tin oxide.
The preparation technology of double-deck double yardstick composite construction oxide-titanium deoxid films, is comprised the steps of：
Step one, matrix is infiltrated into the TiCl in 100-600mM4In aqueous solution, 70-120 DEG C of sealing thermal insulation 30-
120min；Take out after matrix, rinse well, 10-60min or the high temperature at 400-500 DEG C are then dried at 90-180 DEG C
10-30min is sintered, the primary structure titanium oxide with hole is obtained；
Step 2, after drying, the matrix for having deposited the primary structure titanium oxide with hole infiltrates 10mM- again
80mM TiCl4In the aqueous solution, 70 DEG C of -120 DEG C of sealing thermal insulation 30min-120min；Take out after matrix, rinse well, Ran Hou
The 10-60min or high temperature sintering 10-30min at 400-500 DEG C is dried at 90-180 DEG C, filling primary structure oxidation is obtained
The little particle secondary structure titanium oxide of titanium hole formation compact texture；
Step 3, matrix is infiltrated again the mixed solution of 10mM-400mM oxide precursor, 70 DEG C -120 DEG C
Sealing thermal insulation 30min-120min；Take out after matrix, rinse well, 10-120min is then dried at 90-180 DEG C, table is obtained
The second material layer that layer little particle oxide is constituted.
Further, TiCl in step one and step 24The aqueous solution passes through TiCl4Mixed with water or acid or hydrolysis inhibitor
Configuration is formed.
Further, oxide precursor uses one in oxychlorination things metal salt, the pure salt of aluminium or chlorination metal salt
Plant or several；The mixed solution of oxide precursor, is configured by oxide precursor and water, alcohol or other hydrolysis inhibitors
Form.
Double-deck double yardstick composite construction oxide-titanium deoxid films are applied to the application of perovskite solar cell.
Relative to prior art, the invention has the advantages that：
The present invention discloses a kind of double-deck double yardstick composite construction oxide-titanium deoxid films and its preparation technology, passes through
First time TiCl4Hydrolysis, prepares the hole titanium dioxide with nano-scale dimension (particle size is 5-100nm) on matrix
Film；Pass through second of TiCl4Processing, with the nanometer of the titanium dioxide nanoparticle filling hydrolysis generation for the first time of smaller yardstick
Hole, finer and close, the titanium deoxid film of the double yardsticks of tool of formation；The hydrolysis of other oxide precursors is eventually passed,
One layer of modified oxide layer is prepared on the titanium deoxid film of double yardsticks.The present invention fills macrovoid using little particle, and uses
Double-decker sull, using the method for low temperature hydrolysis, is prepared with double-deck double yardstick composite construction oxides-two
Thin film of titanium oxide.
Compared with prior art, film of the present invention, using TiCl4For titanium source, with the method for low temperature hydrolysis, using relatively small
Particles filled big hole, form more dense film, and with other modified oxide titanium dioxide, apply in calcium titanium
Battery efficiency can be increased substantially in ore deposit solar cell to 22% by 20%, stability of the battery efficiency in one month by
60% originally is increased substantially to 90%, and the stagnant aspect of battery time, is just sweeping efficiency and the anti-difference for sweeping efficiency is big by 15%
Amplitude is reduced to 5%.The film has preparation technology simple, and raw material sources are wide and cheap, can be deposited on any chi
Very little matrix is first-class a little, can further promote the commercialization process of perovskite solar cell.
Brief description of the drawings
Fig. 1 is double-deck double yardstick composite construction oxide-titanium deoxid film structural representations；
Fig. 2 is double-deck double yardstick composite construction oxide-titanium deoxid film preparation process schematic diagrames；
Embodiment
The specific embodiment provided the following is inventor is, it is necessary to which explanation, these embodiments are the present invention preferably examples
Son, for it will be understood by those skilled in the art that the present invention, but the invention is not limited in these embodiments.
A kind of double-deck double yardstick composite construction oxide-titanium deoxid films of the invention, including the once knot with hole
Structure titanium oxide 1, the hole of filling primary structure titanium oxide 1 form the little particle secondary structure titanium oxide 2 of compact texture and positioned at two
The second material layer 3 that the little particle oxide of the secondary top of structure titanium white 2 is constituted.
The particle size of primary structure titanium oxide 1 is 5-100nm, and pore size is 5-50nm, and thickness is 20-300nm；It is small
The particle size of particle secondary structure titanium oxide 2 is 3-50nm；Little particle secondary structure titanium oxide 2 is not only aoxidized in primary structure
It is distributed in the space of titanium 1, while in surface distributed, thickness is 3-100nm.
The particle size for the second material layer 3 that little particle oxide is constituted is 3-70nm, and thickness is 3-100nm.
The second material layer 3 that little particle oxide is constituted is different in the top of little particle secondary structure titanium oxide 2 of compact texture
Matter forming core, and form firm combination with titanium dioxide.
The material for the second material layer 3 that little particle oxide is constituted is tin oxide.
TiCl4The aqueous solution passes through TiCl4Formed with water or acid or hydrolysis inhibitor mixed configuration.
Embodiment 1：
A kind of double-deck double yardstick composite construction oxide-titanium deoxid films, are comprised the steps of：
Step one, by matrix 0 in ultrasonic wave successively use ethanol, acetone and water cleaning, then dried up with nitrogen, and by its
Infiltrate the TiCl in 200mM4In aqueous solution, 70 DEG C of sealing thermal insulation 80min.Treat that solution is cooled to room temperature, take out matrix 0,
Acetone is used successively, ethanol and water are rinsed, dried up with nitrogen respectively, 10min is then dried at 100 DEG C, one is obtained on substrate 0
Layer has the primary structure titanium oxide 1 of hole；
Step 2, after above-mentioned drying, has deposited TiO2The matrix 0 of film, ultrasound washes 5min in water, and infiltration is arrived
40mM TiCl4In the aqueous solution, 90 DEG C of sealing thermal insulation 60min.Treat that solution is cooled to room temperature, take out matrix 0, successively with acetone,
Ethanol and water are rinsed respectively, and 20min is then dried at 90 DEG C, are obtained the hole of filling primary structure titanium oxide 1 and are formed fine and close knot
The little particle secondary structure titanium oxide 2 of structure.
Step 3, the TiO that deposition is had to double mesostructures2The matrix 0 of film, is cleaned up, and infiltration again arrives 40mM's
In the mixed solution of the second alcohol and water of stannous chloride, 90 DEG C of sealing thermal insulation 60min.Treat that solution is cooled to room temperature, take out matrix, according to
Secondary use acetone, ethanol and water are rinsed respectively, and 30min is then dried at 180 DEG C, double chis with tin oxide decorative layer 3 are obtained
Spend the titanium deoxid film of composite construction.This, which is applied in perovskite solar cell, significantly to carry battery efficiency by 20%
It is high that stability of the battery efficiency in one month is increased substantially to 90% by original 60% to 22%, and battery return it is stagnant
Aspect, is just sweeping efficiency and is being greatly reduced with the anti-difference for sweeping efficiency by 15% to 5%.
Embodiment 2：
A kind of double-deck double yardstick composite construction oxide-titanium deoxid films, are comprised the steps of：
Step one, by matrix in ultrasonic wave successively use ethanol, acetone and water cleaning, then dried up with nitrogen, and by its
Infiltrate the TiCl in 300mM4In aqueous solution, 80 DEG C of sealing thermal insulation 50min.Treat that solution is cooled to room temperature, take out matrix, according to
Secondary use acetone, ethanol and water are rinsed, dried up with nitrogen respectively, and 10min is then dried at 150 DEG C, one with hole is obtained
Secondary structure titanium white 1；
Step 2, after above-mentioned drying, has deposited TiO2The matrix of film, ultrasound washes 5min in water, and infiltration is arrived
50mM TiCl4In the aqueous solution, 100 DEG C of sealing thermal insulation 40min.Treat that solution is cooled to room temperature, take out matrix, successively with acetone,
Ethanol and water are rinsed respectively, then the high temperature sintering 10min at 400 DEG C, are obtained the hole formation of filling primary structure titanium oxide 1 and are caused
The little particle secondary structure titanium oxide 2 of close structure.
Step 3, the TiO that deposition is had to double mesostructures2The matrix of film, is cleaned up, and infiltration again arrives 400mM's
In the mixed solution of the second alcohol and water of zirconium oxychloride, 120 DEG C of sealing thermal insulation 60min.Treat that solution is cooled to room temperature, take out matrix,
Acetone is used successively, ethanol and water are rinsed respectively, 60min is then dried at 90 DEG C, double chis with tin oxide decorative layer 3 are obtained
Spend the titanium deoxid film of composite construction.
Embodiment 3：
A kind of double-deck double yardstick composite construction oxide-titanium deoxid films, are comprised the steps of：
Step one, by matrix in ultrasonic wave successively use ethanol, acetone and water cleaning, then dried up with nitrogen, and by its
Infiltrate the TiCl in 400mM4In aqueous solution, 100 DEG C of sealing thermal insulation 40min.Treat that solution is cooled to room temperature, take out matrix,
Acetone is used successively, and propyl alcohol and water are rinsed, dried up with nitrogen respectively, and then the high temperature sintering 30min at 500 DEG C, is obtained with hole
The primary structure titanium oxide 1 of gap；
Step 2, after above-mentioned drying, has deposited TiO2The matrix of film, ultrasound washes 5min in water, and infiltration is arrived
In the 60mM TiCl4 aqueous solution, 120 DEG C of sealing thermal insulation 30min.Treat that solution is cooled to room temperature, take out matrix, successively with acetone,
Ethanol and water are rinsed respectively, and 60min is then dried at 120 DEG C, are obtained the hole of filling primary structure titanium oxide 1 and are formed fine and close knot
The little particle secondary structure titanium oxide 2 of structure.
Step 3, the TiO that deposition is had to double mesostructures2The matrix of film, is cleaned up, and infiltration again arrives 100mM's
In the mixed solution of the second alcohol and water of aluminium isopropoxide, 110 DEG C of sealing thermal insulation 30min.Treat that solution is cooled to room temperature, take out matrix,
Acetone is used successively, ethanol and water are rinsed respectively, 30min is then dried at 180 DEG C, obtain double with tin oxide decorative layer 3
The titanium deoxid film of yardstick composite construction.
Embodiment 4：
A kind of double-deck double yardstick composite construction oxide-titanium deoxid films, are comprised the steps of：
Step one, by matrix in ultrasonic wave successively use ethanol, acetone and water cleaning, then dried up with nitrogen, and by its
Infiltrate the TiCl in 600mM4In aqueous solution, 120 DEG C of sealing thermal insulation 30min.Treat that solution is cooled to room temperature, take out matrix,
Acetone is used successively, and ethanol and water are rinsed, dried up with nitrogen respectively, and then the high temperature sintering 10min at 400 DEG C, is obtained with hole
The primary structure titanium oxide 1 of gap；
Step 2, after above-mentioned drying, has deposited TiO2The matrix of film, ultrasound washes 5min in water, and infiltration is arrived
In the 80mM TiCl4 aqueous solution, 70 DEG C of sealing thermal insulation 70min.Treat that solution is cooled to room temperature, take out matrix, successively with acetone, second
Alcohol and water is rinsed respectively, then the high temperature sintering 30min at 500 DEG C, is obtained the hole of filling primary structure titanium oxide 1 and is formed densification
The little particle secondary structure titanium oxide 2 of structure.
Step 3, the TiO that deposition is had to double mesostructures2The matrix of film, is cleaned up, and infiltration again arrives 200mM's
In the mixed solution of the second alcohol and water of aluminum oxide, 70 DEG C of sealing thermal insulation 120min.Treat that solution is cooled to room temperature, take out matrix, according to
Secondary use acetone, ethanol and water are rinsed respectively, and 120min is then dried at 120 DEG C, double chis with tin oxide decorative layer 3 are obtained
Spend the titanium deoxid film of composite construction.
Embodiment 5：
A kind of double-deck double yardstick composite construction oxide-titanium deoxid films, are comprised the steps of：
Step one, by matrix in ultrasonic wave successively use ethanol, acetone and water cleaning, then dried up with nitrogen, and by its
Infiltrate the TiCl in 200mM4In aqueous solution, 70 DEG C of sealing thermal insulation 80min.Treat that solution is cooled to room temperature, take out matrix, according to
Secondary use acetone, ethanol and water are rinsed, dried up with nitrogen respectively, and 60min is then dried at 90 DEG C, is obtained with hole once
Structure titanium white 1；
Step 2, after above-mentioned drying, has deposited TiO2The matrix of film, ultrasound washes 5min in water, and infiltration is arrived
10mM TiCl4In the aqueous solution, 90 DEG C of sealing thermal insulation 30min.Treat that solution is cooled to room temperature, take out matrix, successively with acetone, second
Alcohol and water is rinsed respectively, and 10min is then dried at 180 DEG C, obtains the hole formation compact texture of filling primary structure titanium oxide 1
Little particle secondary structure titanium oxide 2.
Step 3, will deposit the matrix for the TiO2 films for having double mesostructures, cleans up, again oxygen of the infiltration to 10mM
In the mixed solution of the second alcohol and water of zirconium chloride, 90 DEG C of sealing thermal insulation 60min.Treat that solution is cooled to room temperature, take out matrix, successively
With acetone, ethanol and water are rinsed respectively, and 30min is then dried at 150 DEG C, double yardsticks with zirconium oxide decorative layer 3 are obtained
The titanium deoxid film of composite construction.
Embodiment 6：
A kind of double-deck double yardstick composite construction oxide-titanium deoxid films, are comprised the steps of：
Step one, by matrix in ultrasonic wave successively use ethanol, acetone and water cleaning, then dried up with nitrogen, and by its
Infiltrate the TiCl in 100mM4In aqueous solution, 70 DEG C of sealing thermal insulation 120min.Treat that solution is cooled to room temperature, take out matrix,
Acetone is used successively, ethanol and water are rinsed, dried up with nitrogen respectively, 15min is then dried at 180 DEG C, is obtained with hole
Primary structure titanium oxide 1；
Step 2, after above-mentioned drying, has deposited TiO2The matrix of film, ultrasound washes 5min in water, and infiltration is arrived
40mM TiCl4In the aqueous solution, 90 DEG C of sealing thermal insulation 60min.Treat that solution is cooled to room temperature, take out matrix, successively with acetone, second
Alcohol and water is rinsed respectively, and 20min is then dried at 90 DEG C, obtains the hole formation compact texture of filling primary structure titanium oxide 1
Little particle secondary structure titanium oxide 2.
Step 3, the TiO that deposition is had to double mesostructures2The matrix of film, is cleaned up, and the different of 40mM is arrived in infiltration again
In the mixed solution of the second alcohol and water of aluminium propoxide, 120 DEG C of sealing thermal insulation 60min.Treat that solution is cooled to room temperature, take out matrix, according to
Secondary use acetone, ethanol and water are rinsed respectively, and 10min is then dried at 180 DEG C, double chis with aluminum oxide decorative layer 2 are obtained
Spend the titanium deoxid film of composite construction.
Claims (9)
1. double-deck double yardstick composite construction oxide-titanium deoxid films, it is characterised in that including the primary structure with hole
Titanium oxide (1), the little particle secondary structure titanium oxide (2) of filling primary structure titanium oxide (1) hole formation compact texture and position
The second material layer (3) that little particle oxide above secondary structure titanium oxide (2) is constituted.
2. according to claim 1 pair of yardstick composite construction titanium deoxid film, it is characterised in that primary structure titanium oxide
(1) particle size is 5-100nm, and pore size is 5-50nm, and thickness is 20-300nm；Little particle secondary structure titanium oxide
(2) particle size is 3-50nm；During film forming, the particle size of particle secondary structure titanium oxide (2) is once tied less than corresponding
The particle size of structure titanium oxide (1)；Little particle secondary structure titanium oxide (2) not only divides in primary structure titanium oxide (1) space
Cloth, while in surface distributed, thickness is 3-100nm.
3. double-deck double yardstick composite construction oxide-titanium deoxid films according to claim 1, it is characterised in that small
The particle size for the second material layer (3) that oxide particle is constituted is 3-70nm, and thickness is 3-100nm.
4. double-deck double yardstick composite construction oxide-titanium deoxid films according to claim 1, it is characterised in that small
The second material layer (3) that oxide particle is constituted heterogeneous forming core above the little particle secondary structure titanium oxide (2) of compact texture,
And form firm combination with titanium dioxide.
5. double-deck double yardstick composite construction oxide-titanium deoxid films according to claim 1, it is characterised in that small
The material for the second material layer (3) that oxide particle is constituted is tin oxide.
6. the preparation technology of double-deck double yardstick composite construction oxide-titanium deoxid films, it is characterised in that include following step
Suddenly：
Step one, matrix is infiltrated into the TiCl in 100-600mM4In aqueous solution, 70-120 DEG C of sealing thermal insulation 30-120min；
Take out after matrix, rinse well, the 10-60min or high temperature sintering 10- at 400-500 DEG C is then dried at 90-180 DEG C
30min, obtains the primary structure titanium oxide (1) with hole；
Step 2, after drying, the matrix for having deposited the primary structure titanium oxide (1) with hole infiltrates 10mM- again
80mM TiCl4In the aqueous solution, 70 DEG C of -120 DEG C of sealing thermal insulation 30min-120min；Take out after matrix, rinse well, Ran Hou
The 10-60min or high temperature sintering 10-30min at 400-500 DEG C is dried at 90-180 DEG C, filling primary structure oxidation is obtained
The little particle secondary structure titanium oxide (2) of titanium (1) hole formation compact texture；
Step 3, matrix is infiltrated again the mixed solution of 10mM-400mM oxide precursor, 70 DEG C of -120 DEG C of sealings
It is incubated 30min-120min；Take out after matrix, rinse well, 10-120min is then dried at 90-180 DEG C, top layer is obtained small
The second material layer (3) that oxide particle is constituted.
7. preparation technology according to claim 6, it is characterised in that TiCl in step one and step 24The aqueous solution passes through
TiCl4Formed with water or acid or hydrolysis inhibitor mixed configuration.
8. preparation technology according to claim 6, it is characterised in that oxide precursor using oxychlorination things metal salt,
One or more in the pure salt or chlorination metal salt of aluminium；The mixed solution of oxide precursor, passes through oxide precursor
Formed with the configuration of water, alcohol or other hydrolysis inhibitors.
9. the double yardstick composite construction oxide-titanium deoxid films of bilayer any one of claim 1 to 5 are applied to calcium
The purposes of titanium ore solar cell.
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| CN112786793A (en) * | 2020-12-24 | 2021-05-11 | 隆基绿能科技股份有限公司 | Composite carrier transport layer, preparation method thereof, solar cell and light-emitting device |
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| CN105810832A (en) * | 2016-03-22 | 2016-07-27 | 南京工业大学 | Optimized perovskite solar cell based on excellent-conductivity oxide |
| CN105762283A (en) * | 2016-05-05 | 2016-07-13 | 天津市职业大学 | Perovskite solar cell light-absorbing layer nano sol film-coating solution and preparation method |
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| CN112786793A (en) * | 2020-12-24 | 2021-05-11 | 隆基绿能科技股份有限公司 | Composite carrier transport layer, preparation method thereof, solar cell and light-emitting device |
| WO2022134993A1 (en) * | 2020-12-24 | 2022-06-30 | 隆基绿能科技股份有限公司 | Composite carrier transport layer and preparation method therefor, solar cell, and light emitting device |
| CN112786793B (en) * | 2020-12-24 | 2023-10-10 | 隆基绿能科技股份有限公司 | Composite carrier transport layer, preparation method thereof, solar cell and light-emitting device |
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