CN106782898A - A kind of preparation method of silicon base neodymium strontium cobalt thin film - Google Patents
A kind of preparation method of silicon base neodymium strontium cobalt thin film Download PDFInfo
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- CN106782898A CN106782898A CN201710143752.7A CN201710143752A CN106782898A CN 106782898 A CN106782898 A CN 106782898A CN 201710143752 A CN201710143752 A CN 201710143752A CN 106782898 A CN106782898 A CN 106782898A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
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Abstract
The invention discloses a kind of preparation method of silicon base neodymium strontium cobalt thin film, the present invention can well improve its affine performance to conductive colloidal sol by carrying out pretreatment to silicon substrate surface, so that conductive colloidal sol is more evenly distributed in silicon substrate surface in spraying process, the present invention is used with acetic acid neodymium, strontium acetate and this kind of simple organic salt of cobalt acetate as raw material, greatly reduce the cost of raw material, it is and whole technical process can be operated in atmospheric environment and non-toxic.
Description
Technical field
The present invention relates to conductive material field, and in particular to a kind of preparation method of silicon base neodymium strontium cobalt thin film.
Background technology
Transparent conductive film is a kind of basic photoelectric material for having both high connductivity and visible light wave range high transparency characteristic, extensively
The photoelectric display such as display, luminescent device, solar cell, sensor, flexible touch screen field is applied to, with extensive business
Industry application prospect.
Transparent conductive oxide (TCO) film because its in visible-range high transmittance, to infrared light there is high reflection
Rate and relatively low resistivity, in field of photoelectric devices such as solar cell, plate of flat liquid crystal display, light emitting diodes (LED)
Show its wide application prospect.TCO thin film commercial at present, using it is most be tin-doped indium oxide film (ITO), but
It is that the phosphide element in ito thin film is expensive and poisonous.Neodymium strontium-cobalt-oxygen conductive film material has excellent at room temperature because of it
Electric conductivity, can be widely used for the electrode of fuel cell, oxygen permeable membrane and ferroelectric memory and receive much concern.
Retrieved through to prior art, most of technologies are that the ink prepared using all kinds of conductive materials is coated with or is sprayed on
Flexible transparent conductive film, transparent conductive film prepared by such technology are prepared into flexible substrates, although with preferably thin
Film adhesive force, but optical transmittance and electric conductivity still have to be hoisted.
The content of the invention
The present invention provides a kind of preparation method of silicon base neodymium strontium cobalt thin film, and the present invention is pre- by carrying out to silicon substrate surface
Treatment can well improve its affine performance to conductive colloidal sol so that conductive colloidal sol is more evenly distributed in spraying process
Silicon substrate surface, the present invention is used with acetic acid neodymium, strontium acetate and this kind of simple organic salt of cobalt acetate as raw material, is substantially reduced
The cost of raw material, and whole technical process can operate in atmospheric environment, and nontoxicity.
To achieve these goals, the invention provides a kind of preparation method of silicon base neodymium strontium cobalt thin film, the method bag
Include following steps：
（1）Base treatment
Make substrate with Si (100), substrate surface is gently cleaned repeatedly with cotton ball soaked in alcohol, to remove the organic matter on surface；
The substrate that will be cleaned is put into the beaker equipped with acetone, is cleaned 10-15 minutes in ultrasonic cleaning tank；
Then substrate is put into and 2-4h is standing and soak in nitric acid；
Taking-up substrate is put into and 2-3h is stood in deionized water, removes the nitric acid on surface；
Standing dries 5-10h in being placed on fume hood；
（2）Prepare conductive colloidal sol
Solvent is acetic acid, deionized water, and stabilizer is acetylacetone,2,4-pentanedione, and their volume ratio is 25-30: 6-8: 3-5, and solute is vinegar
Sour neodymium, strontium acetate, cobalt acetate, their mol ratio are 1: 1: 2, are dissolved in solution with 0.3-0.5M concentration；
By above-mentioned preparation ratio, first by solvent acetic acid, water, solute acetic acid neodymium, strontium acetate, cobalt acetate mixing are heated to 75-85 DEG C
It is completely dissolved solute；
Mix during acetylacetone,2,4-pentanedione is added into above-mentioned mixed solution again, be heated to 110-115 DEG C, time 115-125min makes molten
Liquid is fully flowed back, and the concentration of solution then is adjusted into 0.3-0.5M, that is, be made the conductive colloidal sol of stabilization；
（3）By conductive colloidal sol, zinc oxide gel film is prepared in above-mentioned substrate using spin-coating method, oxidation gel of zinc will be obtained thin
Film in atmosphere, dries 10-20min under the conditions of 100-105 DEG C；Then in atmosphere, 10- is heat-treated under the conditions of 450-500 DEG C
20min, obtains zinc-oxide film.
Specific embodiment
Embodiment one
Make substrate with Si (100), substrate surface is gently cleaned repeatedly with cotton ball soaked in alcohol, to remove the organic matter on surface；To clean
The substrate crossed is put into the beaker equipped with acetone, is cleaned 10 minutes in ultrasonic cleaning tank；Substrate is put into afterwards quiet in nitric acid
Put immersion 2h；Taking-up substrate is put into and 2h is stood in deionized water, removes the nitric acid on surface；It is placed in fume hood to stand and dries
5h。
Solvent is acetic acid, deionized water, and stabilizer is acetylacetone,2,4-pentanedione, and their volume ratio is 25: 6: 3, and solute is acetic acid
Neodymium, strontium acetate, cobalt acetate, their mol ratio are 1: 1: 2, are dissolved in solution with 0.3M concentration；By above-mentioned preparation ratio, first will
Solvent acetic acid, water, solute acetic acid neodymium, strontium acetate, cobalt acetate mixing, being heated to 75 DEG C is completely dissolved solute；Again by levulinic
Ketone mixes in adding above-mentioned mixed solution, is heated to 110 DEG C, and time 115min makes solution fully flow back, then by solution
Concentration is adjusted to 0.4M, that is, be made the conductive colloidal sol of stabilization.
By conductive colloidal sol, zinc oxide gel film is prepared in above-mentioned substrate using spin-coating method, will obtain aoxidizing gel of zinc
Film in atmosphere, 1min is dried under the conditions of 100 DEG C；Then in atmosphere, 10min is heat-treated under the conditions of 450 DEG C, aoxidized
Zinc film.
Embodiment two
Make substrate with Si (100), substrate surface is gently cleaned repeatedly with cotton ball soaked in alcohol, to remove the organic matter on surface；To clean
The substrate crossed is put into the beaker equipped with acetone, is cleaned 15 minutes in ultrasonic cleaning tank；Substrate is put into afterwards quiet in nitric acid
Put immersion 4h；Taking-up substrate is put into and 3h is stood in deionized water, removes the nitric acid on surface；It is placed in fume hood to stand and dries
10h。
Solvent is acetic acid, deionized water, and stabilizer is acetylacetone,2,4-pentanedione, and their volume ratio is 30: 8: 5, and solute is acetic acid
Neodymium, strontium acetate, cobalt acetate, their mol ratio are 1: 1: 2, are dissolved in solution with 0.5M concentration；By above-mentioned preparation ratio, first will
Solvent acetic acid, water, solute acetic acid neodymium, strontium acetate, cobalt acetate mixing, being heated to 85 DEG C is completely dissolved solute；Again by levulinic
Ketone mixes in adding above-mentioned mixed solution, is heated to 115 DEG C, and time 125min makes solution fully flow back, then by solution
Concentration is adjusted to 0.5M, that is, be made the conductive colloidal sol of stabilization.
By conductive colloidal sol, zinc oxide gel film is prepared in above-mentioned substrate using spin-coating method, will obtain aoxidizing gel of zinc
Film in atmosphere, 20min is dried under the conditions of 105 DEG C；Then in atmosphere, 20min is heat-treated under the conditions of 500 DEG C, obtain oxygen
Change zinc film.
The above, is only presently preferred embodiments of the present invention, and any limitation is not done to the present invention, every according to invention skill
Any simple modification, change and equivalent structure change that art is substantially made to above example, still fall within the technology of the present invention
In the protection domain of scheme.
Claims (1)
1. a kind of preparation method of silicon base neodymium strontium cobalt thin film, the method comprises the following steps：
（1）Base treatment
Make substrate with Si (100), substrate surface is gently cleaned repeatedly with cotton ball soaked in alcohol, to remove the organic matter on surface；
The substrate that will be cleaned is put into the beaker equipped with acetone, is cleaned 10-15 minutes in ultrasonic cleaning tank；
Then substrate is put into and 2-4h is standing and soak in nitric acid；
Taking-up substrate is put into and 2-3h is stood in deionized water, removes the nitric acid on surface；
Standing dries 5-10h in being placed on fume hood；
（2）Prepare conductive colloidal sol
Solvent is acetic acid, deionized water, and stabilizer is acetylacetone,2,4-pentanedione, and their volume ratio is 25-30: 6-8: 3-5, and solute is vinegar
Sour neodymium, strontium acetate, cobalt acetate, their mol ratio are 1: 1: 2, are dissolved in solution with 0.3-0.5M concentration；
By above-mentioned preparation ratio, first by solvent acetic acid, water, solute acetic acid neodymium, strontium acetate, cobalt acetate mixing are heated to 75-85 DEG C
It is completely dissolved solute；
Mix during acetylacetone,2,4-pentanedione is added into above-mentioned mixed solution again, be heated to 110-115 DEG C, time 115-125min makes molten
Liquid is fully flowed back, and the concentration of solution then is adjusted into 0.3-0.5M, that is, be made the conductive colloidal sol of stabilization；
（3）By conductive colloidal sol, zinc oxide gel film is prepared in above-mentioned substrate using spin-coating method, oxidation gel of zinc will be obtained thin
Film in atmosphere, dries 10-20min under the conditions of 100-105 DEG C；Then in atmosphere, 10- is heat-treated under the conditions of 450-500 DEG C
20min, obtains zinc-oxide film.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107299328A (en) * | 2017-08-11 | 2017-10-27 | 苏州南尔材料科技有限公司 | A kind of preparation method of neodymium strontium cobalt thin film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732879A (en) * | 2012-07-10 | 2012-10-17 | 浙江大学 | Preparation method of titanium-dioxide-base conducting film |
| CN105575551A (en) * | 2015-12-23 | 2016-05-11 | 西北工业大学 | Method of directly preparing flexible and transparent conductive film through sol-gel process |
| CN106191821A (en) * | 2016-08-26 | 2016-12-07 | 天津梦龙新能源技术有限公司 | The preparation method of lanthanum-strontium-cobalt-oxygen conductive film material |
-
2017
- 2017-03-12 CN CN201710143752.7A patent/CN106782898A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732879A (en) * | 2012-07-10 | 2012-10-17 | 浙江大学 | Preparation method of titanium-dioxide-base conducting film |
| CN105575551A (en) * | 2015-12-23 | 2016-05-11 | 西北工业大学 | Method of directly preparing flexible and transparent conductive film through sol-gel process |
| CN106191821A (en) * | 2016-08-26 | 2016-12-07 | 天津梦龙新能源技术有限公司 | The preparation method of lanthanum-strontium-cobalt-oxygen conductive film material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107299328A (en) * | 2017-08-11 | 2017-10-27 | 苏州南尔材料科技有限公司 | A kind of preparation method of neodymium strontium cobalt thin film |
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Application publication date: 20170531 |