CN102503162A - Preparation method for Ag-Al co-doped p type ZnO film - Google Patents

Preparation method for Ag-Al co-doped p type ZnO film Download PDF

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CN102503162A
CN102503162A CN2011103383666A CN201110338366A CN102503162A CN 102503162 A CN102503162 A CN 102503162A CN 2011103383666 A CN2011103383666 A CN 2011103383666A CN 201110338366 A CN201110338366 A CN 201110338366A CN 102503162 A CN102503162 A CN 102503162A
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谭红琳
马正洪
艾国齐
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Abstract

The invention relates to a preparation method for an Ag-Al co-doped p type ZnO film, which comprises the following steps: weighting a right amount of precursor zinc salt; taking an organic solvent with corresponding volume; dissolving the zinc salt into the organic solvent; adding diethanolameine as a stabilizing agent, wherein the mole weight of the diethanolameine is equal to the mole weight of zinc ions; adopting water-bath heating and continuously stirring; adding doped source aluminum nitrate and silver nitrate, and continuously stirring; taking out a solution, ageing into sol, coating a film on a substrate, and then pre-processing; and performing annealing treatment, thereby obtaining the required film. The preparation method is simple in process; the cost of equipment is low; the required raw materials are easily obtained; the uniformity of the film is excellent; the preparation method can be applied to industrialized production; and the application prospect is wide.

Description

A kind of preparation method of Ag-Al codoped p type ZnO film
Technical field
The present invention relates to a kind of preparation method of Ag-Al codoped p type ZnO film, belong to technical field of chemistry and chemical engineering.
Background technology
The research of modern sol-gel technique starts from the middle of the 19th century, utilizes colloidal sol and preparing gel single-component compound.Because it is more much lower than traditional height method of fusion to be equipped with the required temperature of glass with this legal system, so be called the low temperature synthesis method of glass again.Nineteen thirty-nine W.Geffcken and E.Berger adopt sol-gel pickling process coated glass pane first, have prepared to change the coating of glass optical reflectance property, and have obtained patent, in patent documentation, propose sol-gel Dipping technology first.Nineteen fifty-nine, Germany special glass stock company adopted collosol and gel Dipping technology to begin to produce in batches automobile rearview mirror.H.Sehroeder in 1962 has developed the thin film physics of oxide compound on the basis of broad research optical coating.Dislich and Leven etc. have set forth the principles of chemistry of using many components of so1-gel technology preparation oxide compound respectively subsequently.Schott glass company in 1969 is raw material with the metal alkoxide, adopts the immersion coating explained hereafter to go out sunshade TiO 2Coating is applied to the buildings decoration and uses solar energy reflection glass.
The characteristics of sol-gel method are that to utilize liquid chemical reagent (or be dissolved in solvent powdered reagent) or colloidal sol be raw material; Rather than with traditional powdery object, reactant uniform mixing and reacting under liquid phase, resultant of reaction is the stable sols system; Change gel into through placing certain hour; Wherein contain a large amount of liquid phases, need to remove liquid medium by evaporation, rather than mechanical dehydration.Under colloidal sol or gel state, promptly may be molded to required goods, and be lower than sintering under traditional firing temperature.
Along with science and technology development, high resolving power, the large size flat-panel screens, solar cell, energy-conservation infrared reflection film, widespread uses such as electrochromic are more and more big to the demand of ZnO transparent conductive film.Transparent conductive film is mainly used in fields such as transparency electrode, video display, hot mirror, transparent surface calorifier, flexible luminescent device, plastic liquid crystal indicating meter.This just requires transparent conductive film that good electroconductibility not only will be arranged, and good visible light light transmission also will be arranged.At present, oneself has developed the growing technology of many ZnO films after deliberation, except sol-gel method, magnetron sputtering method plated film (Magnetron Sputtering is arranged ], pulsed laser deposition (PLD), chemical Vapor deposition process (CVD), molecular beam epitaxy (MEB), spray pyrolysis (Spray Pyrolysis) etc.
Over nearest more than 20 years, the doping of p type ZnO film research becomes the research topic of a hot topic.How preparing fine p type ZnO semiconductor film is the core that realizes the zno-based photoelectric device.As a kind of n type proper semiconductor, ZnO will realize that the transformation from the n type to the p type must pass through the acceptor doping ion.Can know from knowwhy; Because there are many native defects among the ZnO; Ion for acceptor doping has produced the height auto-compensation, and the acceptor impurity solid solubility is very low, is difficult to realize that the p type changes; Thereby make the p-n junction structure of one of semiconducter device core parts ZnO to make, so the development and application of zno-based sealed cell receives great restriction.According to report, people such as Michio Kadota adopt dc reactive magnetron sputtering technique, have realized that the p type of ZnO film changes; The method of human PLD such as Y.R.Ryu is mixed As and is made p-ZnO on the GaAs substrate, (400～500 ℃ of underlayer temperatures) obtains acceptor concentration 10 through test 17～10 21Cm -3, hall mobility is 0.1～50cm 2/ vs mainly is through heating, realizes that in ZnO film, As plays the effect of acceptor doping, has compensated oxygen vacancy concentration and the zinc gap in the crystal simultaneously to As from the substrate thermodiffusion to film; Li Xiaomin etc. adopt the N-In codoped, and normal pressure ullrasonic spraying hot saw method has also successfully been prepared the p type ZnO film of excellent performance; The technology that T.Aoki injects with laser is mixed p and is also obtained p type ZnO film.People such as Zhou Liping have realized also that through the Al-F codoped p type changes, and the film lowest resistivity is 6.5 * 10 -2Europe centimetre.Nearly for some time, people such as the Ji Zhenguo of Zhejiang University, Lv Jianguo have also carried out number of research projects to the P type doping of ZnO film, find that the Al-N codoped can make ZnO film p typeization, and utilize the preparation method of common film just can realize.
The ZnO material has tempting application prospect, develop photoelectric device, needs to solve the problem that how to prepare low-resistance P-type ZnO.ZnO has 6 kinds of intrinsic point defects, and these defectives make the ZnO of intrinsic be n type conductivity type.
Summary of the invention
For solving the problem that the ZnO that exists in the prior art is difficult to be p type conductivity type, the present invention provides a kind of preparation method of Ag-Al codoped p type ZnO film, realizes through following technical proposal.
A kind of preparation method of Ag-Al codoped p type ZnO film, following each step of process:
(1) with the precursor zinc salt be dissolved in the organic solvent to concentration be 0.5～2mol/L, the mol ratio by diethylolamine and zine ion is 1 ︰ 1 again, adds diethylolamine as stablizer, obtains mixing solutions;
(2) place 70～75 ℃ to stir 30～45 minutes down step (1) gained mixing solutions, and then press Ag +And A1 3+Account for Zn 2+Mass percent be 1～5% to add aluminum nitrate and Silver Nitrate, and continue down to stir 30～45 minutes at 70～75 ℃;
(3) step (2) gained solution was carried out ageing 12～24 hours, make solution form colloidal sol;
(4) substrate material being carried out substrate cleans;
(5) adopt spin-coating method or dip-coating method, with plated film on the substrate material of step (3) gained colloidal sol after step (4) is cleaned;
(6) substrate material behind step (5) the gained plated film was heated under 150～200 ℃ 10～15 minutes; So repeating step (5) and (6) 5～40 times;
(7) again the substrate material after the heating of step (6) gained is annealed sintering after 30～60 minutes under 450～550 ℃, promptly obtaining Ag-Al codoped p type ZnO film.
The precursor zinc salt of said step (1) is an organic or inorganic, like zinc salt zinc acetate or zinc nitrate.
The organic solvent of said step (1) is alcohol or ether, like ethanol or methyl ether.
Ag in the aluminum nitrate of the adding of said step (2) and the Silver Nitrate +︰ A1 3+Mass ratio is 4 ︰ 1.
The substrate material of said step (4) is silica glass or glass.
It is to carry out substrate with 30% ydrogen peroxide 50,10% Hydrogen chloride, 10% dilute sulphuric acid, acetone, deionized water or ethanol to clean that the substrate of said step (4) cleans.
The spin speed of the spin-coating method of said step (5) is 1000～1600 rev/mins.
The pull rate of the dip-coating method of said step (5) is 3～6cm/ branch.
The p type of ZnO mixes and can mix the alternative position of zinc through the metals ion Ag of IB family in present method; Form deep acceptor; Again through mixing a small amount of III Al metals ion, regulate it and can be with and make it become the shallow acceptor energy level, the present invention is the p type ZnO film that utilizes Prepared by Sol Gel Method Ag-Al codoped.
Advantage of the present invention and effect:
The p type ZnO film of the present invention's preparation is with low cost, and pattern is preferable, good in optical property, and film is even compact very, has no crack performance; This method process step is simple, need not main equipment, and sintering temperature is lower than ordinary method, mixes at molecular level, is easy to the controlled doping amount, and prepared sample surfaces pattern is good, can be used for scale operation.
Description of drawings
Fig. 1 is Ag +And Al 3+Different total doping (Ag +And A1 3+Quality account for Zn 2+Mass percent) uv-visible absorption spectroscopy figure.
Embodiment
To combine embodiment further to illustrate content of the present invention below, but these instances do not limit protection scope of the present invention.
Embodiment 1
(1) with two hydration zinc acetates be dissolved in the absolute ethyl alcohol to concentration be 0.5mol/L, the mol ratio by diethylolamine and zine ion is 1 ︰ 1 again, adds diethylolamine as stablizer, obtains mixing solutions;
(2) place 70 ℃ to stir 30 minutes down step (1) gained mixing solutions, and then press Ag +And A1 3+Account for Zn 2+Mass percent be 1% to add nine water aluminum nitrate and Silver Nitrates, wherein Ag in nine water aluminum nitrates and the Silver Nitrate +︰ A1 3+Mass ratio is 4 ︰ 1, and continues down to stir 45 minutes at 72 ℃;
(3) step (2) gained solution was carried out ageing 24 hours, make solution form colloidal sol;
(4) the substrate material silica glass being carried out substrate with 30% ydrogen peroxide 50 cleans;
(5) the employing spin speed is 1000 rev/mins a spin-coating method, with plated film on the substrate material of step (3) gained colloidal sol after step (4) is cleaned;
(6) substrate material behind step (5) the gained plated film was heated under 150 ℃ 15 minutes; So repeating step (5) and (6) 20 times;
(7) again the substrate material after the heating of step (6) gained is annealed sintering after 60 minutes under 500 ℃, promptly obtaining Ag-Al codoped p type ZnO film.
Embodiment 2
(1) with two hydration zinc acetates be dissolved in the absolute ethyl alcohol to concentration be 2mol/L, the mol ratio by diethylolamine and zine ion is 1 ︰ 1 again, adds diethylolamine as stablizer, obtains mixing solutions;
(2) place 72 ℃ to stir 40 minutes down step (1) gained mixing solutions, and then press Ag +And A1 3+Account for Zn 2+Mass percent be 3% to add nine water aluminum nitrate and Silver Nitrates, wherein Ag in nine water aluminum nitrates and the Silver Nitrate +︰ A1 3+Mass ratio is 4 ︰ 1, and continues down to stir 30 minutes at 75 ℃;
(3) step (2) gained solution was carried out ageing 12 hours, make solution form colloidal sol;
(4) substrate material glass being carried out substrate with 10% Hydrogen chloride cleans;
(5) adopting pull rate is the dip-coating method that 3cm/ divides, with plated film on the substrate material of step (3) gained colloidal sol after step (4) is cleaned;
(6) substrate material behind step (5) the gained plated film was heated under 180 ℃ 12 minutes; So repeating step (5) and (6) 5 times;
(7) again the substrate material after the heating of step (6) gained is annealed sintering after 45 minutes under 450 ℃, promptly obtaining Ag-Al codoped p type ZnO film.
Embodiment 3
(1) with two hydration zinc acetates be dissolved in the absolute ethyl alcohol to concentration be 1.5mol/L, the mol ratio by diethylolamine and zine ion is 1 ︰ 1 again, adds diethylolamine as stablizer, obtains mixing solutions;
(2) place 75 ℃ to stir 45 minutes down step (1) gained mixing solutions, and then press Ag +And A1 3+Account for Zn 2+Mass percent be 5% to add nine water aluminum nitrate and Silver Nitrates, wherein Ag in nine water aluminum nitrates and the Silver Nitrate +︰ A1 3+Mass ratio is 4 ︰ 1, and continues down to stir 40 minutes at 70 ℃;
(3) step (2) gained solution was carried out ageing 20 hours, make solution form colloidal sol;
(4) the substrate material silica glass being carried out substrate with 10% dilute sulphuric acid cleans;
(5) the employing spin speed is 1600 rev/mins a spin-coating method, with plated film on the substrate material of step (3) gained colloidal sol after step (4) is cleaned;
(6) substrate material behind step (5) the gained plated film was heated under 200 ℃ 10 minutes; So repeating step (5) and (6) 40 times;
(7) again the substrate material after the heating of step (6) gained is annealed sintering after 30 minutes under 550 ℃, promptly obtaining Ag-Al codoped p type ZnO film.
Embodiment 4
(1) with zinc nitrate hexahydrate be dissolved in the methyl ether to concentration be 1mol/L, the mol ratio by diethylolamine and zine ion is 1 ︰ 1 again, adds diethylolamine as stablizer, obtains mixing solutions;
(2) place 75 ℃ to stir 30 minutes down step (1) gained mixing solutions, and then press Ag +And A1 3+Account for Zn 2+Mass percent be 2% to add ANN aluminium nitrate nonahydrate and Silver Nitrate, wherein Ag in aluminum nitrate and the Silver Nitrate +︰ A1 3+Mass ratio is 4 ︰ 1, and continues down to stir 45 minutes at 70 ℃;
(3) step (2) gained solution was carried out ageing 24 hours, make solution form colloidal sol;
(4) substrate material glass being carried out substrate with acetone cleans;
(5) adopting pull rate is the dip-coating method that 6cm/ divides, with plated film on the substrate material of step (3) gained colloidal sol after step (4) is cleaned;
(6) substrate material behind step (5) the gained plated film was heated under 200 ℃ 15 minutes; So repeating step (5) and (6) 30 times;
(7) again the substrate material after the heating of step (6) gained is annealed sintering after 60 minutes under 450 ℃, promptly obtaining Ag-Al codoped p type ZnO film.
Embodiment 5
(1) with zinc nitrate hexahydrate be dissolved in the methyl ether to concentration be 0.5mol/L, the mol ratio by diethylolamine and zine ion is 1 ︰ 1 again, adds diethylolamine as stablizer, obtains mixing solutions;
(2) place 73 ℃ to stir 40 minutes down step (1) gained mixing solutions, and then press Ag +And A1 3+Account for Zn 2+Mass percent be 4% to add ANN aluminium nitrate nonahydrate and Silver Nitrate, wherein Ag in aluminum nitrate and the Silver Nitrate +︰ A1 3+Mass ratio is 4 ︰ 1, and continues down to stir 35 minutes at 75 ℃;
(3) step (2) gained solution was carried out ageing 24 hours, make solution form colloidal sol;
(4) substrate material glass being carried out substrate with deionized water cleans;
(5) the employing spin speed is 1200 rev/mins a spin-coating method, with plated film on the substrate material of step (3) gained colloidal sol after step (4) is cleaned;
(6) substrate material behind step (5) the gained plated film was heated under 150 ℃ 10 minutes; So repeating step (5) and (6) 25 times;
(7) again the substrate material after the heating of step (6) gained is annealed sintering after 60 minutes under 480 ℃, promptly obtaining Ag-Al codoped p type ZnO film.
Embodiment 6
(1) with zinc nitrate hexahydrate be dissolved in the methyl ether to concentration be 1mol/L, the mol ratio by diethylolamine and zine ion is 1 ︰ 1 again, adds diethylolamine as stablizer, obtains mixing solutions;
(2) place 75 ℃ to stir 30 minutes down step (1) gained mixing solutions, and then press Ag +And A1 3+Account for Zn 2+Mass percent be 1% to add ANN aluminium nitrate nonahydrate and Silver Nitrate, wherein Ag in aluminum nitrate and the Silver Nitrate +︰ A1 3+Mass ratio is 4 ︰ 1, and continues down to stir 30 minutes at 75 ℃;
(3) step (2) gained solution was carried out ageing 18 hours, make solution form colloidal sol;
(4) the substrate material silica glass being carried out substrate with ethanol cleans;
(5) adopting pull rate is the dip-coating method that 4cm/ divides, with plated film on the substrate material of step (3) gained colloidal sol after step (4) is cleaned;
(6) substrate material behind step (5) the gained plated film was heated under 200 ℃ 15 minutes; So repeating step (5) and (6) 35 times;
(7) again the substrate material after the heating of step (6) gained is annealed sintering after 60 minutes under 550 ℃, promptly obtaining Ag-Al codoped p type ZnO film.

Claims (8)

1. the preparation method of an Ag-Al codoped p type ZnO film is characterized in that through following each step:
(1) with the precursor zinc salt be dissolved in the organic solvent to concentration be 0.5～2mol/L, the mol ratio by diethylolamine and zine ion is 1 ︰ 1 again, adds diethylolamine as stablizer, obtains mixing solutions;
(2) place 70～75 ℃ to stir 30～45 minutes down step (1) gained mixing solutions, and then press Ag +And A1 3+Account for Zn 2+Mass percent be 1～5% to add aluminum nitrate and Silver Nitrate, and continue down to stir 30～45 minutes at 70～75 ℃;
(3) step (2) gained solution was carried out ageing 12～24 hours, make solution form colloidal sol;
(4) substrate material being carried out substrate cleans;
(5) adopt spin-coating method or dip-coating method, with plated film on the substrate material of step (3) gained colloidal sol after step (4) is cleaned;
(6) substrate material behind step (5) the gained plated film was heated under 150～200 ℃ 10～15 minutes; So repeating step (5) and (6) 5～40 times;
(7) again the substrate material after the heating of step (6) gained is annealed sintering after 30～60 minutes under 450～550 ℃, promptly obtaining Ag-Al codoped p type ZnO film.
2. preparation method according to claim 1 is characterized in that: the precursor zinc salt of said step (1) is an organic or inorganic, like zinc salt zinc acetate or zinc nitrate.
3. preparation method according to claim 1 is characterized in that: the organic solvent of said step (1) is alcohol or ether, like ethanol or methyl ether.
4. preparation method according to claim 1 is characterized in that: Ag in the aluminum nitrate of the adding of said step (2) and the Silver Nitrate +︰ A1 3+Mass ratio is 4 ︰ 1.
5. preparation method according to claim 1 is characterized in that: the substrate material of said step (4) is silica glass or glass.
6. preparation method according to claim 1 is characterized in that: it is to carry out substrate with 30% ydrogen peroxide 50,10% Hydrogen chloride, 10% dilute sulphuric acid, acetone, deionized water or ethanol to clean that the substrate of said step (4) cleans.
7. preparation method according to claim 1 is characterized in that: the spin speed of the spin-coating method of said step (5) is 1000～1600 rev/mins.
8. preparation method according to claim 1 is characterized in that: the pull rate of the dip-coating method of said step (5) is 3～6cm/ branch.
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CN103881123A (en) * 2012-12-21 2014-06-25 中国科学院大连化学物理研究所 Preparation method of PBI/H3PO4 doped film for high temperature fuel cells
CN104409337A (en) * 2014-11-05 2015-03-11 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of sulphur and silver co-doped p type zinc oxide optoelectronic thin film
CN105603400A (en) * 2016-01-21 2016-05-25 深圳市国华光电科技有限公司 Preparation method of ZnO transparent conductive film
CN107034452A (en) * 2017-04-26 2017-08-11 长春理工大学 The chemical preparation method of flexible doping type ZnO-based transparent conductive film
CN109935733A (en) * 2017-12-15 2019-06-25 深圳Tcl工业研究院有限公司 A kind of N-shaped ZnO film and preparation method thereof and QLED device
CN110699640A (en) * 2019-09-25 2020-01-17 安徽省含山县锦华氧化锌厂 Preparation method of nano zinc oxide film with enhanced conductivity

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CN103881123A (en) * 2012-12-21 2014-06-25 中国科学院大连化学物理研究所 Preparation method of PBI/H3PO4 doped film for high temperature fuel cells
CN104409337A (en) * 2014-11-05 2015-03-11 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of sulphur and silver co-doped p type zinc oxide optoelectronic thin film
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CN105603400A (en) * 2016-01-21 2016-05-25 深圳市国华光电科技有限公司 Preparation method of ZnO transparent conductive film
CN107034452A (en) * 2017-04-26 2017-08-11 长春理工大学 The chemical preparation method of flexible doping type ZnO-based transparent conductive film
CN109935733A (en) * 2017-12-15 2019-06-25 深圳Tcl工业研究院有限公司 A kind of N-shaped ZnO film and preparation method thereof and QLED device
CN110699640A (en) * 2019-09-25 2020-01-17 安徽省含山县锦华氧化锌厂 Preparation method of nano zinc oxide film with enhanced conductivity

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