CN114105223A - Method for improving characteristics of nickel oxide film - Google Patents
Method for improving characteristics of nickel oxide film Download PDFInfo
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- CN114105223A CN114105223A CN202111356523.6A CN202111356523A CN114105223A CN 114105223 A CN114105223 A CN 114105223A CN 202111356523 A CN202111356523 A CN 202111356523A CN 114105223 A CN114105223 A CN 114105223A
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- nickel oxide
- oxide film
- diethanolamine
- precursor solution
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- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 117
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 238000000034 method Methods 0.000 title claims abstract description 33
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000006227 byproduct Substances 0.000 claims abstract description 41
- 229940043237 diethanolamine Drugs 0.000 claims abstract description 39
- 239000002243 precursor Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 12
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 5
- 239000010408 film Substances 0.000 claims description 54
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 claims description 2
- 230000006872 improvement Effects 0.000 abstract description 3
- 230000007246 mechanism Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000005525 hole transport Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for improving the characteristics of a nickel oxide film, wherein the nickel oxide film is prepared by a solution method, the improvement is realized by improving the purity of nickel oxide, the method for improving the purity of nickel oxide is to reduce the generation of nickel oxide by-products, the reduced by-products are realized by synthesizing a complex which is easy to decompose by heating, and the synthesis of the complex which is easy to decompose by heating is realized by adding diethanol amine into a nickel oxide precursor solution; specifically, the method comprises the following steps: starting from a precursor solution prepared from the nickel oxide film, diethanolamine is added into the nickel oxide precursor solution, so that byproducts generated in the nickel oxide film are changed, and the characteristics of the nickel oxide film are improved. According to the invention, from a precursor solution prepared from a nickel oxide film, diethanolamine is added into the precursor solution, so that the synthesis mechanism of the nickel oxide film is changed; thereby changing the by-product formed in the nickel oxide film, optimizing the characteristics of the nickel oxide film and improving the performance of the device.
Description
Technical Field
The invention belongs to the field of film preparation, and particularly relates to a method for improving the characteristics of a nickel oxide film.
Background
The hole transport layer in the photovoltaic device plays a crucial role in the performance of the device, and organic semiconductor materials are widely applied to the hole transport layer, and the preparation process of the materials is complex and unstable, so that the commercial application of the materials is limited. The inorganic material nickel oxide is widely used in semiconductor devices due to its advantages of low preparation temperature, easy processing, etc.
At present, the nickel oxide film can be prepared by a plurality of methods, such as pulsed laser deposition, atomic layer deposition, spray pyrolysis and the like, and the methods are expensive to prepare and are not suitable for large-area deposition. Therefore, the solution method for preparing a nickel oxide thin film has been widely studied.
The solution process of preparing nickel oxide films is accompanied by the production of nickel oxide by-products, which affect the properties of the nickel oxide film and thus the performance of the entire device. The influence of the byproducts on the nickel oxide is negative, so that the problems of reducing the generation of the byproducts in the nickel oxide film and improving the performance of the byproducts in the nickel oxide film are needed to be solved.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects of the prior art, the invention provides a method for improving the characteristics of a nickel oxide film.
The technical scheme is as follows: a method for improving the characteristics of a nickel oxide film, wherein the nickel oxide film is prepared by a solution method, the improvement is to improve the purity of nickel oxide by reducing the generation of nickel oxide by-products, the reduced by-products are realized by synthesizing a complex which is easily decomposed by heating, and the synthesis of the complex which is easily decomposed by heating is realized by adding diethanol amine into a nickel oxide precursor solution; specifically, the method comprises the following steps:
starting from a precursor solution prepared from a nickel oxide film, adding diethanolamine into the nickel oxide precursor solution to change a byproduct generated in the nickel oxide film and improve the characteristics of the nickel oxide film;
the formation process of the nickel oxide film is shown by the following equation:
(1) and (2) the equation shows that 6-hydrated sodium nitrate is directly dissolved in 2-methoxy ethanol solution, the solution is coated on a substrate in a spin mode and simultaneously heated to obtain a nickel oxide film, and a by-product generated in the process is nickel hydroxide;
after diethanolamine is added into the nickel oxide precursor solution, the reaction equations become (1), (3) and (5), and no by-product is generated in the nickel oxide after spin coating and heating;
and the diethanolamine is added, so that the purity of the nickel oxide is improved to a great extent, the generation of byproducts is reduced, and the property of the nickel oxide film is optimized.
As an optimization: after the diethanolamine is added into the nickel oxide precursor solution, a small part of the solution inevitably reacts (1), so that the purity of the nickel oxide is improved after the diethanolamine is added, but a small amount of by-products are generated.
As an optimization: the invention adopts X-ray photoelectron spectroscopyThe nickel oxide film after film formation is tested to carry out peak separation treatment on the nickel oxide film, the amount of the nickel oxide in the nickel oxide film is greatly improved after diethanolamine is added, and the by-product Ni (OH) is reduced compared with the film without diethanolamine2。
As an optimization: according to the invention, triethanolamine is added into the precursor solution, the reaction equations are (1), (3) and (4), and the by-product Ni (OH) is reduced similarly to the addition of diethanolamine2。
Has the advantages that: according to the invention, from a precursor solution prepared from a nickel oxide film, diethanolamine is added into the precursor solution, so that the synthesis mechanism of the nickel oxide film is changed; thereby changing the by-product formed in the nickel oxide film, optimizing the characteristics of the nickel oxide film and improving the performance of the device.
According to the invention, diethanolamine is added into the nickel oxide precursor solution, so that the by-product generated in the nickel oxide film is changed, and the characteristics of the nickel oxide film are improved. The invention improves the characteristics of the nickel oxide film by changing the chemical reaction formed by the nickel oxide; meanwhile, diethanolamine is added to reduce the generation of byproducts and change the characteristics of the byproducts in the nickel oxide film; after the diethanolamine is added, a complex which is easy to decompose by heating is generated in the reaction process, so that the purity of the generated nickel oxide is improved; not only diethanolamine, but compounds like diethanolamine can also improve the purity of nickel oxide.
Drawings
FIG. 1 is a schematic diagram showing the characteristic peak energy spectrum of nickel in nickel oxide formed without adding diethanolamine and after adding the nickel oxide according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below so that those skilled in the art can better understand the advantages and features of the present invention, and thus the scope of the present invention will be more clearly defined. The embodiments described herein are only a few embodiments of the present invention, rather than all embodiments, and all other embodiments that can be derived by one of ordinary skill in the art without inventive faculty based on the embodiments described herein are intended to fall within the scope of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
A method for improving the characteristics of a nickel oxide film, wherein the nickel oxide film is prepared by a solution method, the improvement is to improve the purity of nickel oxide by reducing the generation of nickel oxide by-products, the reduced by-products are realized by synthesizing a complex which is easily decomposed by heating, and the synthesis of the complex which is easily decomposed by heating is realized by adding diethanol amine into a nickel oxide precursor solution; specifically, the method comprises the following steps: starting from a precursor solution prepared from the nickel oxide film, diethanolamine is added into the nickel oxide precursor solution, so that byproducts generated in the nickel oxide film are changed, and the characteristics of the nickel oxide film are improved.
The formation process of the nickel oxide film is shown by the following equation:
(1) and (2) the equation shows that sodium nitrate 6-hydrate is directly dissolved in a 2-methoxyethanol solution, the solution is spin-coated on a substrate while heating to obtain a nickel oxide thin film, and nickel hydroxide is produced as a by-product in the process. After diethanolamine is added into the nickel oxide precursor solution, the reaction equations become (1), (3) and (5), and no by-product is generated in the nickel oxide after the final spin coating and heating, which is ideal. And the diethanolamine is added, so that the purity of the nickel oxide is improved to a great extent, the generation of byproducts is reduced, and the property of the nickel oxide film is optimized. After the diethanolamine is added into the nickel oxide precursor solution, a small part of the solution inevitably reacts (1), so that the purity of the nickel oxide is improved after the diethanolamine is added, but a small amount of by-products are generated.
In order to further research the influence of diethanolamine on the nickel oxide precursor solution, the invention adopts X-ray photoelectron spectroscopy to test the components of the nickel oxide after film formation, and as shown in figure 1, the nickel oxide film is subjected to peak separation treatment as shown in the characteristic peak energy spectrum of nickel in the nickel oxide formed after diethanolamine is not added or added. After diethanolamine is added, the amount of nickel oxide in the nickel oxide film is greatly increased, and the by-product Ni (OH) is reduced compared with the film without diethanolamine2。
To further investigate the effect of diethanolamine on nickel oxide precursors, triethanolamine was added to the precursor solution in accordance with equations (1), (3) and (4), and the by-product Ni (OH) was reduced similarly to the diethanolamine addition2。
Obviously, the method for synthesizing nickel oxide by using diethanolamine to change the complex in the reaction process has the following advantages:
1) the method is simple, diethanolamine is added into the precursor solution, the complex formed in the middle is changed, and the components of the finally synthesized nickel oxide are changed;
2) the amount of the original by-product is reduced without increasing other by-products.
3) The purity of the nickel oxide formed is improved, and the characteristics of the nickel oxide film are improved.
4) And a substance similar to diethanolamine is added into the nickel oxide precursor solution, so that the effect of improving the purity of the nickel oxide can be achieved.
Claims (4)
1. A method for improving the characteristics of a nickel oxide film is characterized by comprising the following steps: the nickel oxide film is prepared by a solution method, the improved way is to improve the purity of nickel oxide, the method for improving the purity of nickel oxide is to reduce the generation of nickel oxide by-products, the reduced by-products are realized by synthesizing a complex which is easy to decompose by heating, and the synthesis of the complex which is easy to decompose by heating is realized by adding diethanol amine into a nickel oxide precursor solution; specifically, the method comprises the following steps:
starting from a precursor solution prepared from a nickel oxide film, adding diethanolamine into the nickel oxide precursor solution to change a byproduct generated in the nickel oxide film and improve the characteristics of the nickel oxide film;
the formation process of the nickel oxide film is shown by the following equation:
(1)
(2)
(3)
(4)
(5)
(1) and (2) the equation shows that 6-hydrated sodium nitrate is directly dissolved in 2-methoxy ethanol solution, the solution is coated on a substrate in a spin mode and simultaneously heated to obtain a nickel oxide film, and a by-product generated in the process is nickel hydroxide;
after diethanolamine is added into the nickel oxide precursor solution, the reaction equations become (1), (3) and (5), and no by-product is generated in the nickel oxide after spin coating and heating;
and the diethanolamine is added, so that the purity of the nickel oxide is improved to a great extent, the generation of byproducts is reduced, and the property of the nickel oxide film is optimized.
2. The method for improving the characteristics of a nickel oxide thin film according to claim 1, wherein: after the diethanolamine is added into the nickel oxide precursor solution, a small part of the solution inevitably reacts (1), so that the purity of the nickel oxide is improved after the diethanolamine is added, but a small amount of by-products are generated.
3. The method for improving the characteristics of a nickel oxide thin film according to claim 1, wherein: the invention adopts X-ray photoelectron spectroscopy to test the components of nickel oxide after film formation, carries out peak separation treatment on the nickel oxide film, and after diethanolamine is added, the amount of nickel oxide in the nickel oxide film is greatly improved, and compared with the film without diethanolamine, the invention reduces the byproduct Ni (OH)2。
4. The method for improving the characteristics of a nickel oxide thin film according to claim 1, wherein: according to the invention, triethanolamine is added into the precursor solution, the reaction equations are (1), (3) and (4), and the by-product Ni (OH) is reduced similarly to the addition of diethanolamine2。
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| CN202111356523.6A CN114105223B (en) | 2021-11-16 | 2021-11-16 | Method for improving nickel oxide film characteristics |
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| CN202111356523.6A CN114105223B (en) | 2021-11-16 | 2021-11-16 | Method for improving nickel oxide film characteristics |
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| CN114105223A true CN114105223A (en) | 2022-03-01 |
| CN114105223B CN114105223B (en) | 2023-11-28 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130023744A (en) * | 2011-08-29 | 2013-03-08 | 부산대학교 산학협력단 | Transparent composite conductive oxide thin films and method for preparing the oxide thin films |
| CN106966441A (en) * | 2016-07-14 | 2017-07-21 | 浙江大学 | A kind of preparation method of copper ion doped nickel oxide colloid nanocrystalline and products thereof and its application |
| CN108529690A (en) * | 2018-04-17 | 2018-09-14 | 广东普加福光电科技有限公司 | A kind of preparation method and applications of nickel oxide nano crystal |
| CN110880554A (en) * | 2018-09-05 | 2020-03-13 | 杭州纤纳光电科技有限公司 | Equipment and method for coating precursor solution and surfactant step by step |
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2021
- 2021-11-16 CN CN202111356523.6A patent/CN114105223B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130023744A (en) * | 2011-08-29 | 2013-03-08 | 부산대학교 산학협력단 | Transparent composite conductive oxide thin films and method for preparing the oxide thin films |
| CN106966441A (en) * | 2016-07-14 | 2017-07-21 | 浙江大学 | A kind of preparation method of copper ion doped nickel oxide colloid nanocrystalline and products thereof and its application |
| CN108529690A (en) * | 2018-04-17 | 2018-09-14 | 广东普加福光电科技有限公司 | A kind of preparation method and applications of nickel oxide nano crystal |
| CN110880554A (en) * | 2018-09-05 | 2020-03-13 | 杭州纤纳光电科技有限公司 | Equipment and method for coating precursor solution and surfactant step by step |
Non-Patent Citations (1)
| Title |
|---|
| 施建珍;王玮;金永龙;宋德江;徐宜泽;方靖淮: "Fe3O4/Ag复合纳米材料的制备及SERS研究", 中国材料科技与设备, vol. 8, no. 006, pages 33 - 35 * |
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