CN101798183A - Preparation method of Al-Doped ZnO film - Google Patents
Preparation method of Al-Doped ZnO film Download PDFInfo
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- CN101798183A CN101798183A CN 201010142138 CN201010142138A CN101798183A CN 101798183 A CN101798183 A CN 101798183A CN 201010142138 CN201010142138 CN 201010142138 CN 201010142138 A CN201010142138 A CN 201010142138A CN 101798183 A CN101798183 A CN 101798183A
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Abstract
The invention discloses a preparation method of an Al-Doped ZnO film, which comprises the following steps of: adding AZO nano particles in a medium; ultrasonically processing a solution for 10-30 minutes to obtain uniform and dispersive nano particle seriflux; adding a coupling agent and a photoinitiator in the seriflux; after adding the coupling agent, carrying out ultrasonic treatment for 0.5-8 hours; spreading AZO nano particle seriflux on glass by using a pulling method or a spinning method and irradiating by ultraviolet light; and then carrying out heat treatment to obtain the ZAO film. The invention does not need vacuum equipment or high temperature, has simple structure, and is suitable for large-scale production.
Description
Technical field
That the present invention relates to is a kind of preparation method of photoelectric material technical field, is specifically related to the preparation method of a kind of Al-Doped ZnO (AZO) film.
Background technology
Al-Doped ZnO film premium properties transparent because of it, conduction is widely used, and is the solar battery window layer material that a kind of development in recent years is rapid, have a extensive future.Element zinc in the AZO film, aluminium element earth reserves are all very abundant, also do not contain poisonous composition, and be environmentally friendly.Main Application Areas has dull and stereotyped liquid-crystal display (LCD), electroluminescent (ELD), solar cell transparency electrode, low emissivity glass, electromagnetic shielding material or the like at present.
Literature search through prior art is found, C.G.Granqvist etc. deliver Optical properties ofsputter-deposited ZnO:Al thin films (utilizing the optical property of the Al-Doped ZnO film of magnetron sputtering method preparation) at " Journal of AppliedPhysics " 1988 64 volumes the 10th phase 5117-5131 page or leaf, the professional has developed multiple preparation method since 1988, as magnetron sputtering method, chemical Vapor deposition process etc., but all exist equipment complexity, cost height, be not suitable for shortcomings such as large-area preparation.Therefore, proposed a kind of can the preparation in a large number, with low cost, the preparation method of eco-friendly AZO film, significant for this area.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of Al-Doped ZnO film is provided.Method green non-pollution of the present invention, the reaction conditions gentleness is simple, with low cost, is suitable for scale operation.
The present invention is achieved by the following technical solutions, may further comprise the steps:
Step 1 adds the AZO nanoparticle in medium, with solution supersound process 10-30 minute, obtain homodisperse AZO nanoparticle slurries;
Step 2 adds coupling agent and light trigger in slurries; After adding coupling agent, need with using supersound process 0.5-8 hour;
In the step 1, described medium is dehydrated alcohol, ethylene glycol, tetrahydrofuran (THF) or N-Methyl pyrrolidone.
In the step 1, it is 5%-30% that described AZO nanoparticle accounts for medium proportion.
In the step 1, the yardstick of described AZO nanoparticle is at 10-50nm, and aluminium content is 1-10% (mass ratio);
In the step 2, described coupling agent is silane coupling agent, titanate coupling agent and aluminate coupling agent.
Described silane coupling agent is: alkyls silane coupling agent, vinyl-based silane coupling agent, chloropropyl silane coupling agent, sulfur-bearing one type of silane coupling agent, amine silane coupling agent, epoxy group(ing) one type of silane coupling agent, acryloxy silane coupling agent or alkoxyl group one type of silane coupling agent; Described titanate coupling agent is: sec.-propyl alkyl benzene sulphonate (ABS) titanic acid ester, isopropoxy two hard ester acyl group polyoxyethylene titanic acid ester, isopropoxy three hard ester acyl titanates, isopropoxy three titanic acid ester, the two titanic acid ester of fluoroacetic acid ester, the two titanic acid ester of tetra isopropyl.
In the step 2, described light trigger is a 1-hydroxy-cyclohexyl phenyl ketone, 2-hydroxyl-aminomethyl phenyl propane-1-ketone, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, 2,4,6-trimethylbenzoyl diphenyl phosphine oxide.
In the step 3, the UV-irradiation time is 0.5-4min.
In the step 3, described thermal treatment is that temperature is 50-300 ℃ at inert atmospheres such as nitrogen, argon gas, helium, and the time is 0.5-4 hour.
Advantage of the present invention: compare with traditional AZO method for manufacturing thin film, this method needing no vacuum equipment, need not high temperature, technology is simple, is applicable to large-area preparation.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the Al-Doped ZnO film of embodiment 1 preparation;
Fig. 2 is the X ray diffracting spectrum of the Al-Doped ZnO film of embodiment 2 preparations;
Fig. 3 is the X ray diffracting spectrum of the Al-Doped ZnO film of embodiment 3 preparations;
Fig. 4 is the X ray diffracting spectrum of the Al-Doped ZnO film of embodiment 4 preparations;
Fig. 5 is the X ray diffracting spectrum of the Al-Doped ZnO film of embodiment 5 preparations;
Fig. 6 is the X ray diffracting spectrum of the Al-Doped ZnO film of embodiment 6 preparations;
Fig. 7 is the X ray diffracting spectrum of the Al-Doped ZnO film of embodiment 7 preparations;
Embodiment
Following example will the invention will be further described in conjunction with the accompanying drawings.Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment 1:
(20nm, wherein aluminium content is 5%) is distributed in the flask that the 10ml dehydrated alcohol is housed with 500mg AZO nanoparticle, with solution supersound process 15 minutes, obtains AZO homodisperse solution; The alkyls silane coupling agent and the 10mg 1-hydroxy-cyclohexyl phenyl ketone that then add 10mg continued supersound process 2 hours; Be coated on the substrate of glass with the AZO nanoparticle of spin-coating method, and utilize the UV-irradiation 2min of wavelength for 254nm with finishing; 200 ℃ of following thermal treatment 4 hours in nitrogen atmosphere at last promptly obtains the AZO film.
Embodiment 2:
(40nm, wherein aluminium content is 20%) is distributed in the flask that the 10ml dehydrated alcohol is housed with 1.5g AZO nanoparticle, with solution supersound process 10 minutes, obtains AZO homodisperse solution; The vinyl-based silane coupling agent and the 5mg 1-hydroxy-cyclohexyl phenyl ketone that then add 15mg.Continued supersound process 0.5 hour; Be coated on the substrate of glass with the AZO nanoparticle of spin-coating method, and utilize the UV-irradiation 0.5min of wavelength for 254nm with finishing; 200 ℃ of following thermal treatment 0.5 hour in nitrogen atmosphere at last promptly obtains the AZO film.
Embodiment 3:
(30nm, wherein aluminium content is 15%) is distributed in the flask that the 10ml dehydrated alcohol is housed with 3g AZO nanoparticle, with solution supersound process 20 minutes, obtains AZO homodisperse solution; Then add the epoxy group(ing) one type of silane coupling agent of 60mg and the 2-hydroxyl of 40mg-aminomethyl phenyl propane-1-ketone, continued supersound process 4 hours; Be coated on the substrate of glass with the AZO nanoparticle of spin-coating method at last, and utilize the UV-irradiation 1min of wavelength for 254nm with finishing; 200 ℃ of following thermal treatment 4 hours in hydrogen atmosphere at last promptly obtains the AZO film.
Embodiment 4:
(50nm, wherein aluminium content is 10%) is distributed in the flask that the 10ml dehydrated alcohol is housed with 1.5g AZO nanoparticle, with solution supersound process 30 minutes, obtains AZO homodisperse solution; Then add 2,4 of isopropoxy three (dioctylphosphoric acid ester) titanate coupling agent of 75mg and 100mg, 6-trimethylbenzoyl diphenyl phosphine oxide continued supersound process 6 hours; And with spin-coating method the AZO nanoparticle of finishing is coated on glassly, utilize the UV-irradiation 1.5min of wavelength for 254nm.300 ℃ of following thermal treatment 4 hours in nitrogen and hydrogen mixed gas atmosphere at last promptly obtains the AZO film.
Embodiment 5:
(30nm, wherein aluminium content is 5%) is distributed in the flask that the 10ml dehydrated alcohol is housed with the 1.5gAZO nanoparticle, with solution supersound process 25 minutes, obtains AZO homodisperse solution; Then add the two titanic acid ester of fluoroacetic acid ester of 75mg and 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone of 150mg, continued supersound process 6 hours; And with crystal pulling method the AZO nanoparticle of finishing is coated on glassly, utilize the UV-irradiation 2min of wavelength for 365nm.300 ℃ of following thermal treatment 1 hour in nitrogen and hydrogen mixed gas atmosphere at last promptly obtains the AZO film.
Embodiment 6:
(10nm, wherein aluminium content is 15%) is distributed in the flask that the 10ml tetrahydrofuran (THF) is housed with 3g AZO nanoparticle, with solution supersound process 10 minutes, obtains AZO homodisperse solution; Then add 60mg amine silane coupling agent and 150mg 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, continued supersound process 7 hours; With crystal pulling method the AZO nanoparticle of finishing is coated on glassly, utilizes the UV-irradiation 0.5min of wavelength for 365nm.100 ℃ of following thermal treatment 4 hours in hydrogen atmosphere at last promptly obtains the AZO film.
Embodiment 7:
(20nm, wherein aluminium content is 5%) is distributed in the flask that the 10ml N-Methyl pyrrolidone is housed with the 1.5gAZO nanoparticle, with solution supersound process 20 minutes, obtains AZO homodisperse solution; Then add 75mg chloropropyl silane coupling agent and 150mg 2-hydroxyl-aminomethyl phenyl propane-1-ketone, continued supersound process 8 hours; With crystal pulling method the AZO nanoparticle of finishing is coated on glassly, utilizes the UV-irradiation 1min of wavelength for 365nm.300 ℃ of following thermal treatment 1 hour in nitrogen and hydrogen mixed gas atmosphere at last promptly obtains the AZO film.
AZO thin-film technique by routine 1-example 7 preparations is simple, cost is low, be easy to scale operation, and has the good optical performance, can be widely used in numerous association areas such as energy-conservation form for building, solar cell, car windshield glass.
Claims (10)
1. the preparation method of an Al-Doped ZnO film is characterized in that: may further comprise the steps:
Step 1 adds the AZO nanoparticle in medium, with solution supersound process 10-30 minute, obtain homodisperse AZO nanoparticle slurries;
Step 2 adds coupling agent and light trigger in slurries; After adding coupling agent, need with using supersound process 0.5-8 hour;
Step 3 is coated in AZO nanoparticle slurries on glass and utilizes UV-irradiation with crystal pulling method or spin-coating method, and thermal treatment obtains the AZO film then.
2. the preparation method of Al-Doped ZnO film as claimed in claim 1 is characterized in that, in the step 1, described medium is dehydrated alcohol, ethylene glycol, tetrahydrofuran (THF) or N-Methyl pyrrolidone.
3. the preparation method of Al-Doped ZnO film as claimed in claim 1 is characterized in that, in the step 1, it is 5%-30% that described AZO nanoparticle accounts for medium proportion.
4. the preparation method of Al-Doped ZnO film as claimed in claim 1 is characterized in that, in the step 1, the yardstick of described AZO nanoparticle is at 10-50nm, and the aluminium quality is 1-10% than content.
5. the preparation method of Al-Doped ZnO film as claimed in claim 1 is characterized in that, in the step 2, described coupling agent is silane coupling agent, titanate coupling agent and aluminate coupling agent.
6. the preparation method of Al-Doped ZnO film as claimed in claim 5, it is characterized in that described silane coupling agent is: alkyls silane coupling agent, vinyl-based silane coupling agent, chloropropyl silane coupling agent, sulfur-bearing one type of silane coupling agent, amine silane coupling agent, epoxy group(ing) one type of silane coupling agent, acryloxy silane coupling agent or alkoxyl group one type of silane coupling agent.
7. the preparation method of Al-Doped ZnO film as claimed in claim 5; it is characterized in that described titanate coupling agent is: sec.-propyl alkyl benzene sulphonate (ABS) titanic acid ester, isopropoxy two hard ester acyl group polyoxyethylene titanic acid ester, isopropoxy three hard ester acyl titanates, isopropoxy three titanic acid ester, the two titanic acid ester of fluoroacetic acid ester, the two titanic acid ester of tetra isopropyl.
8. the preparation method of Al-Doped ZnO film as claimed in claim 1; it is characterized in that; in the step 2; described light trigger is a 1-hydroxy-cyclohexyl phenyl ketone; 2-hydroxyl-aminomethyl phenyl propane-1-ketone, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, 2; 4,6-trimethylbenzoyl diphenyl phosphine oxide.
9. the preparation method of Al-Doped ZnO film as claimed in claim 1 is characterized in that, in the step 3, the UV-irradiation time is 0.5-4min.
10. the preparation method of Al-Doped ZnO film as claimed in claim 1 is characterized in that, in the step 3, described thermal treatment is that temperature is 50-300 ℃ at inert atmospheres such as nitrogen, argon gas, helium, and the time is 0.5-4 hour.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102559143A (en) * | 2012-03-13 | 2012-07-11 | 王昊平 | Waterproof tablet for filming |
| CN102672951A (en) * | 2012-04-27 | 2012-09-19 | 南通天丰电子新材料有限公司 | Preparation method of unilateral drawing uniform adjustable micro-pore structure high temperature resistant diaphragm |
| WO2013159256A1 (en) * | 2012-04-27 | 2013-10-31 | 南通天丰电子新材料有限公司 | Unidirectional stretching method for inducing and producing safety diaphragm with microporous composite structure |
| WO2013159257A1 (en) * | 2012-04-27 | 2013-10-31 | 南通天丰电子新材料有限公司 | Bidirectional synchronous stretching method for manufacturing high temperature resistant diaphragm with uniform and adjustable microporous composite structure |
| CN108083322A (en) * | 2018-01-29 | 2018-05-29 | 首凯汽车零部件（江苏）有限公司 | The preparation method of ZnO nano crystalline substance solution and its film forming coherent condition regulation and control method |
| CN108493299A (en) * | 2018-04-11 | 2018-09-04 | 深圳市太赫兹科技创新研究院 | Azo transparent conductive film and its preparation method and application |
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| CN101054267A (en) * | 2007-02-02 | 2007-10-17 | 广州菲迪材料科技研究有限公司 | Preparation method for ITO thin film |
| CN101349825A (en) * | 2008-09-04 | 2009-01-21 | 友达光电股份有限公司 | Method for manufacturing transflective liquid crystal display panel |
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2010
- 2010-04-09 CN CN 201010142138 patent/CN101798183A/en active Pending
Patent Citations (2)
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| CN101054267A (en) * | 2007-02-02 | 2007-10-17 | 广州菲迪材料科技研究有限公司 | Preparation method for ITO thin film |
| CN101349825A (en) * | 2008-09-04 | 2009-01-21 | 友达光电股份有限公司 | Method for manufacturing transflective liquid crystal display panel |
Non-Patent Citations (1)
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| 《Advanced Engineering Materials》 20041231 Joerg Puetz et.al. Processing of Transparent Conducting Coatings Made With Redispersible Crystalline Nanoparticles 第733页右栏第1-2段、第734页左栏第2段-右栏最后1段 1-10 第6卷, 第9期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102559143A (en) * | 2012-03-13 | 2012-07-11 | 王昊平 | Waterproof tablet for filming |
| CN102672951A (en) * | 2012-04-27 | 2012-09-19 | 南通天丰电子新材料有限公司 | Preparation method of unilateral drawing uniform adjustable micro-pore structure high temperature resistant diaphragm |
| WO2013159256A1 (en) * | 2012-04-27 | 2013-10-31 | 南通天丰电子新材料有限公司 | Unidirectional stretching method for inducing and producing safety diaphragm with microporous composite structure |
| WO2013159257A1 (en) * | 2012-04-27 | 2013-10-31 | 南通天丰电子新材料有限公司 | Bidirectional synchronous stretching method for manufacturing high temperature resistant diaphragm with uniform and adjustable microporous composite structure |
| CN102672951B (en) * | 2012-04-27 | 2015-05-20 | 范建国 | Preparation method of unilateral drawing uniform adjustable micro-pore structure high temperature resistant diaphragm |
| CN108083322A (en) * | 2018-01-29 | 2018-05-29 | 首凯汽车零部件（江苏）有限公司 | The preparation method of ZnO nano crystalline substance solution and its film forming coherent condition regulation and control method |
| CN108083322B (en) * | 2018-01-29 | 2020-03-27 | 首凯汽车零部件（江苏）有限公司 | Preparation method of ZnO nanocrystalline solution and film-forming aggregation state regulation method thereof |
| CN108493299A (en) * | 2018-04-11 | 2018-09-04 | 深圳市太赫兹科技创新研究院 | Azo transparent conductive film and its preparation method and application |
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Open date: 20100811 |