CN108018541A - A kind of low temperature fast performance liquid method for preparing nickel oxide film - Google Patents
A kind of low temperature fast performance liquid method for preparing nickel oxide film Download PDFInfo
- Publication number
- CN108018541A CN108018541A CN201711233102.8A CN201711233102A CN108018541A CN 108018541 A CN108018541 A CN 108018541A CN 201711233102 A CN201711233102 A CN 201711233102A CN 108018541 A CN108018541 A CN 108018541A
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- CN
- China
- Prior art keywords
- nickel oxide
- oxide film
- nickel
- low temperature
- precursor solution
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
Abstract
The invention belongs to material, chemistry and chemical field, more particularly to a kind of quick cryogenic fluid method for preparing nickel oxide film.Include the following steps：Nickel acetate is weighed, measures solvent, configuration concentration is the nickel oxide precursor solution of 0.01 0.5 mol/Ls, and the nickel oxide precursor solution of clear is formed by 0.1 3 magnetic agitations when small and ultrasonic disperse；Nickel oxide precursor solution is coated to formation nickel oxide precursor film on cleaned substrate, is annealed by the light waves of 1 4.9 minutes, the temperature in light wave annealing process is 100 300 DEG C；Coating and annealing can be repeated several times to obtain the nickel oxide film of different-thickness requirement.Gained nickel oxide film performance of the invention is high, is expected to be applied in the devices such as transistor, solar cell, sensor.Can be to avoid common process cycle length or expensive device etc. by the technique of the present invention, cost is low, is adapted to industrialization large-scale production.
Description
Technical field
The invention belongs to material, chemistry and chemical field, more particularly to it is a kind of it is quick prepare nickel oxide film low temperature it is molten
Liquid method, nickel oxide film have important application prospect in fields such as transistor, solar cell, sensors.
Background technology
Nickel oxide is a kind of broad stopband metal oxide with 3d electronic structures, the energy gap under room temperature for 3.5~
3.7eV.Nickel oxide has the performances such as electrochromism, anti-ferromagnetism, vapor sensitivity, p-type conductivity, is widely used in electrode
Material, electrochromic material, resistive material and catalyst etc..For technology of preparing, the preparation method of nickel oxide film
It is varied, mainly include two major class of vapor phase method and liquid phase method.For example, sputtering method, chemical vapour deposition technique, thermal oxidation method, spray
The methods of mist pyrolysismethod, sol-gel process, is all used to prepare nickel oxide film.However, these gas phase process usually require very
Altitude, adds the raising of the complexity and cost of equipment.In recent years, liquid phase process increasingly causes extensive concern and rapid
Development, such as sol-gel process, spray pyrolysis etc..For example, the Chinese invention patent of Publication No. CN106927692A is public
A kind of preparation method of mesoporous nickel oxide film is opened：First nickel hydroxide colloidal sol is prepared by definite component ratio；Secondly make
It is standby to contain the mixed sols of ethyl cellulose, terpinol and nickel hydroxide as spin coating precursor liquid；Then rotary coating is passed through
Film after spin coating is placed on the hot plate of certain temperature and toasts in clean FTO electro-conductive glass spin-coated thin films by method；Finally
Film is annealed the regular hour at 500 DEG C, obtains the uniform mesoporous nickel oxide film of covering.Publication No.
The Chinese invention patent of CN103904216A discloses a kind of preparation method of titanium doped nickel oxide Memister film：By vinegar
Sour nickel and second phthalein acetone are dissolved in ethylene glycol monomethyl ether adds acrylic acid after stirring 5-6h, continues to stir 1-2h, old after stirring
Change 20-24h, obtain oxidation nickel sol, the nickel oxide film for lifting obtained doping is heat-treated at 500 DEG C.
Although liquid phase method can prepare the nickel oxide film of superior performance, liquid phase it can be seen from foregoing invention patent
Method usually requires high temperature（Higher than 400 DEG C）Annealing, just can promote precursor thin-film to decompose and be densified, form uniform nickel oxide
Film.Therefore, a kind of new cryogenic fluid technology of preparing is found, is for large-scale application of the nickel oxide film in various fields
Particularly important and urgent.
The content of the invention
It is an object of the invention to provide a kind of quick cryogenic fluid method for preparing nickel oxide film, nickel oxide is realized
Rapidly and efficiently prepare, it is easier to large-scale production and commercial applications.The innovative point of the present invention essentially consists in：Newly fast is developed
Fast low temperature sol-gel method efficiently synthesizes nickel oxide film.
Technical scheme, specifically includes following steps：
(1) nickel oxide precursor solution is configured：The nickel salt of solubility is weighed, measures solvent, configuration concentration rubs for 0.01-0.5
You/liter nickel oxide precursor solution, the nickel oxide of clear is formed by magnetic agitations of 0.1-3 when small and ultrasonic disperse
Precursor solution；
(2) deposited oxide nickel film：Nickel oxide precursor solution is coated on cleaned substrate and forms nickel oxide precursor
Film, annealed by the light waves of 1-4.9 minutes, and the temperature in light wave annealing process is 100-300 DEG C；
(3) step 1 and 2 can be repeated several times to obtain the nickel oxide film of different-thickness requirement.
In the step of preparation method of the present invention (1), the soluble nickel salt is nickel acetate, nickel formate, nitric acid
The one or more of nickel.
In the step of preparation method of the present invention (1), the solvent is ethylene glycol monomethyl ether, in ethanol, ethylene glycol, water
One or more.
In the step of preparation method of the present invention (2), the painting method for spin coating method, drop-coating, dip coating,
Spray-on process or ink-jet printing process.
In the step of preparation method of the present invention (2), the generation instrument of the light wave is the light-wave cooker as kitchen tools
Or the heating instrument with halogen lamp tube.
In the step of preparation method of the present invention (2), the substrate is rigid substrate, such as silicon chip, sheet glass；It is or soft
Property substrate, such as plastic sheet, sheet metal.
The beneficial effects of the invention are as follows：Present invention process is simple and quick easy to operate, and raw material is cheap and easy to get, prepared oxygen
It is high to change nickel film performance, is expected to be applied in the devices such as transistor, solar cell, sensor.Pass through the work of the present invention
Skill can be to avoid common process cycle length or expensive device etc., and cost is low, is adapted to industrialization large-scale production.
Brief description of the drawings
The present invention is further illustrated below in conjunction with the accompanying drawings.
Attached drawing 1 is the atomic force microscope images of the nickel oxide film of one of embodiment, and picture scanning scope is 2 micron * 2
Micron.
Embodiment
The present invention is further illustrated with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1：
0.185 g nickel formates are weighed, measure 10 milliliters of ethanol solutions, configuration concentration is molten for the nickel oxide precursor of 0.1 mol/L
Liquid, forms the nickel oxide precursor solution of clear by 3 magnetic agitations when small and ultrasonic disperse.By nickel oxide precursor
Solution is coated to formation nickel oxide precursor film on cleaned substrate, anneals by the light waves of 3 minutes, light wave annealing process
In temperature be 100 DEG C, that is, obtain nickel oxide film.
Embodiment 2：
0.062 g nickel acetates are weighed, 5 milliliters of ethylene glycol monomethyl ether solution are measured, before configuration concentration is the nickel oxide of 0.05 mol/L
Liquid solution is driven, the nickel oxide precursor solution of clear is formed by 0.1 magnetic agitation when small and ultrasonic disperse.Will oxidation
Nickel precursor solution is coated to formation nickel oxide precursor film on cleaned substrate, anneals by the light wave of 0.5 minute, light
Temperature in ripple annealing process is 200 DEG C, that is, obtains nickel oxide film.
Embodiment 3：
0.044 g nickel nitrates are weighed, measure 15 milliliters of ethylene glycol solutions, configuration concentration is the nickel oxide forerunner of 0.01 mol/L
Liquid solution, forms the nickel oxide precursor solution of clear by 1 magnetic agitation when small and ultrasonic disperse.Before nickel oxide
Drive liquid solution and be coated to formation nickel oxide precursor film on cleaned substrate, anneal by the light waves of 3 minutes, light wave annealing
During temperature be 150 DEG C, that is, obtain nickel oxide film.
Embodiment 4：
2.49 g nickel acetates are weighed, measure 20 milliliters of ethanol solutions, configuration concentration is molten for the nickel oxide precursor of 0.5 mol/L
Liquid, forms the nickel oxide precursor solution of clear by 2 magnetic agitations when small and ultrasonic disperse.By nickel oxide precursor
Solution is coated to formation nickel oxide precursor film on cleaned substrate, anneals by the light waves of 4.9 minutes, and light wave is annealed
Temperature in journey is 200 DEG C, that is, obtains nickel oxide film.
Embodiment 5：
0.218 g nickel nitrates are weighed, measure 15 milliliters of aqueous solutions, configuration concentration is molten for the nickel oxide precursor of 0.05 mol/L
Liquid, forms the nickel oxide precursor solution of clear by 3 magnetic agitations when small and ultrasonic disperse.By nickel oxide precursor
Solution is coated to formation nickel oxide precursor film on cleaned substrate, anneals by the light waves of 2 minutes, light wave annealing process
In temperature be 250 DEG C, that is, obtain nickel oxide film.
The embodiment of the present invention is described in above-described embodiment combination attached drawing, but not the present invention is protected
The limitation of scope.Those skilled in the art should understand that on the basis of technical scheme, those skilled in the art
Need not make the creative labor can make to the present invention various modifications or deformation, still protection scope of the present invention with
It is interior.
Claims (6)
- A kind of 1. low temperature fast performance liquid method for preparing nickel oxide film, it is characterised in that include the following steps：(1) nickel oxide precursor solution is configured：The nickel salt of solubility is weighed, measures solvent, configuration concentration rubs for 0.01-0.5 You/liter nickel oxide precursor solution, the nickel oxide of clear is formed by magnetic agitations of 0.1-3 when small and ultrasonic disperse Precursor solution；(2) deposited oxide nickel film：Nickel oxide precursor solution is coated on cleaned substrate and forms nickel oxide precursor Film, annealed by the light waves of 0.5-4.9 minutes, and the temperature in light wave annealing process is 100-300 DEG C；(3) step 1 and 2 can be repeated several times to obtain the nickel oxide film of different-thickness requirement.
- A kind of 2. low temperature fast performance liquid method for preparing nickel oxide film according to claim 1, it is characterised in that：It is described Soluble nickel salt for nickel acetate, nickel formate, the one or more of nickel nitrate.
- A kind of 3. low temperature fast performance liquid method for preparing nickel oxide film according to claim 1, it is characterised in that：It is described Solvent be ethylene glycol monomethyl ether, more than ethanol, ethylene glycol, one or both of water.
- A kind of 4. low temperature fast performance liquid method for preparing nickel oxide film according to claim 1, it is characterised in that：It is described Painting method is spin coating method, drop-coating, dip coating, spray-on process or ink-jet printing process.
- A kind of 5. low temperature fast performance liquid method for preparing nickel oxide film according to claim 2, it is characterised in that：It is described The generation instrument of light wave be the light-wave cooker as kitchen tools, there is the heating instrument of halogen or similar fluorescent tube.
- A kind of 6. low temperature fast performance liquid method for preparing nickel oxide film according to claim 2, it is characterised in that：It is described Substrate be rigid substrate, such as silicon chip, sheet glass；Or flexible substrate, such as plastic sheet, sheet metal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711233102.8A CN108018541A (en) | 2017-11-30 | 2017-11-30 | A kind of low temperature fast performance liquid method for preparing nickel oxide film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711233102.8A CN108018541A (en) | 2017-11-30 | 2017-11-30 | A kind of low temperature fast performance liquid method for preparing nickel oxide film |
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| CN108018541A true CN108018541A (en) | 2018-05-11 |
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| CN201711233102.8A Pending CN108018541A (en) | 2017-11-30 | 2017-11-30 | A kind of low temperature fast performance liquid method for preparing nickel oxide film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715958A (en) * | 2022-03-08 | 2022-07-08 | 华能新能源股份有限公司 | Spray pyrolysis method of nickel oxide and perovskite solar cell |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699273A (en) * | 2005-04-29 | 2005-11-23 | 北京科技大学 | Lithium titanium co-doped nickel oxide base ceramic film and preparation method thereof |
| CN106409668A (en) * | 2016-09-14 | 2017-02-15 | 齐鲁工业大学 | Low-temperature solution preparation method for aluminium oxide dielectric film |
-
2017
- 2017-11-30 CN CN201711233102.8A patent/CN108018541A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699273A (en) * | 2005-04-29 | 2005-11-23 | 北京科技大学 | Lithium titanium co-doped nickel oxide base ceramic film and preparation method thereof |
| CN106409668A (en) * | 2016-09-14 | 2017-02-15 | 齐鲁工业大学 | Low-temperature solution preparation method for aluminium oxide dielectric film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715958A (en) * | 2022-03-08 | 2022-07-08 | 华能新能源股份有限公司 | Spray pyrolysis method of nickel oxide and perovskite solar cell |
| CN114715958B (en) * | 2022-03-08 | 2024-04-02 | 华能新能源股份有限公司 | Spray pyrolysis method of nickel oxide and perovskite solar cell |
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Application publication date: 20180511 |