CN101650990A - Method for preparing c-orientated arrangement ZnO: Al film - Google Patents
Method for preparing c-orientated arrangement ZnO: Al film Download PDFInfo
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- CN101650990A CN101650990A CN200910023727A CN200910023727A CN101650990A CN 101650990 A CN101650990 A CN 101650990A CN 200910023727 A CN200910023727 A CN 200910023727A CN 200910023727 A CN200910023727 A CN 200910023727A CN 101650990 A CN101650990 A CN 101650990A
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Abstract
The invention relates to a method for preparing a c-orientated arrangement ZnO: Al film. The method comprises the following steps: preparing a precursor solution, dissolving zinc nitrate or zinc acetate and aluminum nitrate, aluminium acetate or aluminum chloride into glacial acetic acid according to a Zn0.99 Al0.01 O chemical formula, then adding glycol and triethanolamine and regulating the pH of a solution to be less than 5 by hydrochloric acid after adding the glacial acetic acid into the solution so as to obtain the precursor solution; smearing the precursor solution on a substrate by adopting a dip-coating or spin-coating technique; and after annealing the smeared substrate in a high-temperature furnace of 650-750 DEG C for 60min, cooling naturally to obtain the c-orientated arrangement ZnO: Al film. In the invention, the ZnO: Al film is prepared on the substrate by applying a colloidal sol-gel method, a highly c-orientated long column-shaped particle film is obtained by quicklyheating at a speed greater than 200 DEG C/min and annealing at 650-750 DEG C, and the length direction of the column shape is the c-axis direction of a crystal and is parallel to the surface of the substrate. The transparent test shows that the posterior film has large light transmittance and transparent wavelength range.
Description
Technical field
The invention belongs to field of material preparation, be specifically related to a kind of preparation method of c-orientations ZnO:Al film.
Background technology
ZnO is a kind of semiconductor material with wide forbidden band of hexagonal wurtzite structure, has multiple good physical and chemical performance, stablize as good heat conductivity, chemical property, and material source is very abundant, is a kind of multi-function membrane material.A small amount of Al mixes and can further increase light transmission and conductance.Al doping ZnO transparent conductive film is with a wide range of applications in fields such as photodetector, light-emitting diode, surface acoustic wave device, rheostat, gas sensor, solar cells.
In these are used, require film that high transmitance and low resistivity are arranged.Because the optical anisotropy of ZnO crystal, generally maximum transmitance is arranged on perpendicular to the c-direction of principal axis at incident light.Be orientated at present and preparation that the c-axle is parallel to the film of substrate generally has only the technology of a spot of complexity can realize under specific process conditions for c-.Sol-gel process is that technology is simple, and chemical composition all should, be easy to realize stoichiometric proportion and the low a kind of technology of cost, uses sol-gel process at present and is difficult to preparation this special and ZnO:Al film substrate Rankine-Hugoniot relations and specific orientation.
Summary of the invention
The object of the present invention is to provide the preparation method of the simple c-orientations of a kind of preparation technology ZnO:Al film, obtain the long column shape particle film that height c-is orientated by preparation method of the present invention, the length direction of column is the c-direction of principal axis of crystal and is parallel to substrate surface.Printing opacity test shows film of the present invention has big light transmittance and transparent wavelength range.
For achieving the above object, the technical solution used in the present invention is:
1) preparation of precursor solution: press Zn
0.99Al
0.01The O chemical formula dissolves in zinc nitrate or zinc acetate and aluminum nitrate, aluminium acetate or aluminium chloride in the glacial acetic acid, and then adding ethylene glycol and triethanolamine, solution metal ion mol ratio is: ethylene glycol: triethanolamine=1: 2: 5-10, the concentration of using zinc ion in the glacial acetic acid regulator solution again is to 0.01mol/l, is that pH＜5 of the hydrochloric acid conditioning solution of 35%-37% obtain precursor solution with mass concentration;
2) film: adopt dip-coating or spin coating proceeding that precursor solution is coated on the substrate, after each coating with it 120 ℃ of dryings, above-mentioned repeatedly coating and dry run are until the film that obtains required thickness;
3) annealing: natural cooling obtained c-orientations ZnO:Al film after the substrate of the substrate after will filming from room temperature is warming up to 650-750 ℃ of annealing 60min or directly will films with the heating rate greater than 200 ℃/min after put into 650-750 ℃ high temperature furnace annealing 60min.
The present invention is in order to reduce the viscosity of precursor solution, with precursor solution at 60-80 ℃ of gelation 30-60min; Substrate adopting quartz glass substrate,, air-dry before filming with absolute ethyl alcohol and acetone difference ultrasonic cleaning 15-30min.
The present invention uses preparation ZnO:Al film on the sol-gel process substrate, being rapidly heated with the speed greater than 200 ℃/min then obtains the long column shape particle film of height c-orientation 650-750 ℃ of annealing, the length direction of column is the c-direction of principal axis of crystal and is parallel to substrate surface.A kind of film has big light transmittance and transparent wavelength range after the printing opacity test shows.
Description of drawings
Fig. 1 is the XRD figure of ZnO:Al film of the present invention, and wherein (a) is that 400 ℃ of preannealing 60min are then in the XRD figure of the ZnO:Al film of 700 ℃ of annealing 60min (b) 700 ℃ annealing 60min;
Fig. 2 is the AFM microphoto of ZnO:Al film of the present invention, wherein Fig. 2 (a) be 400 ℃ of preannealing 60min then at 400 ℃ of preannealing 60min then at 700 ℃ of annealing 60min, Fig. 2 (b) 4 is the AFM microphoto of ZnO:Al film behind 700 ℃ of annealing 60min;
Fig. 3 is the printing opacity curve of ZnO:Al film of the present invention, and wherein dotted line is 400 ℃ of preannealing 60min, 700 ℃ of annealing 60min then, and solid line is the printing opacity curve of ZnO:Al film behind 700 ℃ of annealing 60min.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further details.
Embodiment 1:1) preparation of precursor solution: press Zn
0.99Al
0.01The O chemical formula dissolves in zinc nitrate and aluminum nitrate in the glacial acetic acid, and then adding ethylene glycol and triethanolamine, solution metal ion mol ratio is: ethylene glycol: triethanolamine=1: 2: 8, the concentration of using zinc ion in the glacial acetic acid regulator solution again is to 0.01mol/1, for the formation mass concentration that prevents precipitate metal hydroxides in the long-time put procedure of solution is that pH＜5 of the hydrochloric acid conditioning solution of 35%-37% obtain precursor solution, in order to reduce the viscosity of precursor solution, with precursor solution at 60 ℃ of gelation 60min;
2) film: get quartz glass substrate, use absolute ethyl alcohol and acetone ultrasonic cleaning 15-30min respectively before filming, air-dry, adopt dip-coating or spin coating proceeding that precursor solution is coated on the substrate then, after each coating with it 120 ℃ of dryings, above-mentioned repeatedly coating and dry run are until the film that obtains required thickness;
3) annealing: 400 ℃ of preannealing 60min of the substrate after will filming then behind 700 ℃ of annealing 60min natural cooling obtain the ZnO:Al film of arbitrary orientation (Fig. 1 a and Fig. 2 be a); Substrate after filming natural cooling from room temperature is warming up to 700 ℃ of annealing 60min with the heating rate greater than 200 ℃/min after is obtained c-orientations ZnO:Al film (Fig. 1 b and Fig. 2 b).
4) light transmission performance: c-orientations ZnO:Al film has big transmitance and transparent wavelength range (Fig. 3) than arbitrary orientation film.
Embodiment 2:1) preparation of precursor solution: press Zn
0.99Al
0.01The O chemical formula dissolves in zinc acetate and aluminium chloride in the glacial acetic acid, and then adding ethylene glycol and triethanolamine, solution metal ion mol ratio is: ethylene glycol: triethanolamine=1: 2: 5, the concentration of using zinc ion in the glacial acetic acid regulator solution again is to 0.01mol/l, for the formation mass concentration that prevents precipitate metal hydroxides in the long-time put procedure of solution is that pH＜5 of the hydrochloric acid conditioning solution of 35%-37% obtain precursor solution, in order to reduce the viscosity of precursor solution, with precursor solution at 80 ℃ of gelation 30min;
2) film: get quartz glass substrate, use absolute ethyl alcohol and acetone ultrasonic cleaning 15-30min respectively before filming, air-dry, adopt dip-coating or spin coating proceeding that precursor solution is coated on the substrate then, after each coating with it 120 ℃ of dryings, above-mentioned repeatedly coating and dry run are until the film that obtains required thickness;
3) annealing: the natural cooling from room temperature is warming up to 650 ℃ of annealing 60min with the heating rate greater than 200 ℃/min after of the substrate after will filming obtains c-orientations ZnO:Al film.
Embodiment 3:1) preparation of precursor solution: press Zn
0.99Al
0.01The O chemical formula dissolves in zinc nitrate and aluminium acetate in the glacial acetic acid, and then adding ethylene glycol and triethanolamine, solution metal ion mol ratio is: ethylene glycol: the mol ratio of triethanolamine=1: 2: 10, the concentration of using zinc ion in the glacial acetic acid regulator solution again is to 0.01mol/l, for the formation mass concentration that prevents precipitate metal hydroxides in the long-time put procedure of solution is that pH＜5 of the hydrochloric acid conditioning solution of 35%-37% obtain precursor solution, in order to reduce the viscosity of precursor solution, with precursor solution at 70 ℃ of gelation 45min;
2) film: get quartz glass substrate, use absolute ethyl alcohol and acetone ultrasonic cleaning 15-30min respectively before filming, air-dry, adopt dip-coating or spin coating proceeding that precursor solution is coated on the substrate then, after each coating with it 120 ℃ of dryings, above-mentioned repeatedly coating and dry run are until the film that obtains required thickness;
3) annealing: the natural cooling from room temperature is warming up to 750 ℃ of annealing 60min with the heating rate greater than 200 ℃/min after of the substrate after will filming obtains c-orientations ZnO:Al film.
Embodiment 4:1) preparation of precursor solution: press Zn
0.99Al
0.01The O chemical formula dissolves in zinc acetate and aluminum nitrate in the glacial acetic acid, and then adding ethylene glycol and triethanolamine, the mol ratio of solution metal ion is: ethylene glycol: triethanolamine=1: 2: 6, the concentration of using zinc ion in the glacial acetic acid regulator solution again is to 0.01mol/l, for the formation mass concentration that prevents precipitate metal hydroxides in the long-time put procedure of solution is that pH＜5 of the hydrochloric acid conditioning solution of 35%-37% obtain precursor solution;
2) film: get quartz glass substrate, use absolute ethyl alcohol and acetone ultrasonic cleaning 15-30min respectively before filming, air-dry, adopt dip-coating or spin coating proceeding that precursor solution is coated on the substrate then, after each coating with it 120 ℃ of dryings, above-mentioned repeatedly coating and dry run are until the film that obtains required thickness;
3) annealing: natural cooling obtained c-orientations ZnO:Al film after the substrate after will filming was directly put into 650 ℃ high temperature furnace annealing 60min.
Embodiment 5:1) preparation of precursor solution: press Zn
0.99Al
0.01The O chemical formula dissolves in zinc acetate and aluminium chloride in the glacial acetic acid, and then adding ethylene glycol and triethanolamine, the mol ratio of solution metal ion is: ethylene glycol: the mol ratio of triethanolamine=1: 2: 7, the concentration of using zinc ion in the glacial acetic acid regulator solution again is to 0.01mol/l, for the formation mass concentration that prevents precipitate metal hydroxides in the long-time put procedure of solution is that pH＜5 of the hydrochloric acid conditioning solution of 35%-37% obtain precursor solution;
2) film: get quartz glass substrate, use absolute ethyl alcohol and acetone ultrasonic cleaning 15-30min respectively before filming, air-dry, adopt dip-coating or spin coating proceeding that precursor solution is coated on the substrate then, after each coating with it 120 ℃ of dryings, above-mentioned repeatedly coating and dry run are until the film that obtains required thickness;
3) annealing: natural cooling obtained c-orientations ZnO:Al film after the substrate after will filming was directly put into 750 ℃ high temperature furnace annealing 60min.
Claims (3)
1, a kind of preparation method of c-orientations ZnO:Al film is characterized in that, may further comprise the steps:
1) preparation of precursor solution: press Zn
0.99Al
0.01The O chemical formula dissolves in zinc nitrate or zinc acetate and aluminum nitrate, aluminium acetate or aluminium chloride in the glacial acetic acid, and then adding ethylene glycol and triethanolamine, solution metal ion mol ratio is: ethylene glycol: triethanolamine=1: 2: 5-10, the concentration of using zinc ion in the glacial acetic acid regulator solution again is to 0.01mol/l, is that pH＜5 of the hydrochloric acid conditioning solution of 35%-37% obtain precursor solution with mass concentration;
2) film: adopt dip-coating or spin coating proceeding that precursor solution is coated on the substrate, after each coating with it 120 ℃ of dryings, above-mentioned repeatedly coating and dry run are until the film that obtains required thickness;
3) annealing: natural cooling obtained c-orientations ZnO:Al film after the substrate of the substrate after will filming from room temperature is warming up to 650-750 ℃ of annealing 60min or directly will films with the heating rate greater than 200 ℃/min after put into 650-750 ℃ high temperature furnace annealing 60min.
2, the preparation method of c-orientations ZnO:Al film according to claim 1 is characterized in that: in order to reduce the viscosity of precursor solution, with precursor solution at 60-80 ℃ of gelation 30-60min.
3, the preparation method of c-orientations ZnO:Al film according to claim 1 is characterized in that: said substrate adopting quartz glass substrate, and, air-dry before filming with absolute ethyl alcohol and acetone difference ultrasonic cleaning 15-30min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103107291A (en) * | 2011-11-11 | 2013-05-15 | 海洋王照明科技股份有限公司 | Substrate of organic electroluminescence device and production method thereof |
| CN103194741A (en) * | 2013-04-03 | 2013-07-10 | 苏州大学 | Alumina precursor solution, and preparation method and application thereof |
| CN106374052A (en) * | 2016-09-26 | 2017-02-01 | Tcl集团股份有限公司 | QLED and preparation method therefor |
-
2009
- 2009-08-28 CN CN200910023727A patent/CN101650990A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103107291A (en) * | 2011-11-11 | 2013-05-15 | 海洋王照明科技股份有限公司 | Substrate of organic electroluminescence device and production method thereof |
| CN103194741A (en) * | 2013-04-03 | 2013-07-10 | 苏州大学 | Alumina precursor solution, and preparation method and application thereof |
| CN103194741B (en) * | 2013-04-03 | 2015-01-28 | 苏州大学 | Alumina precursor solution, and preparation method and application thereof |
| CN106374052A (en) * | 2016-09-26 | 2017-02-01 | Tcl集团股份有限公司 | QLED and preparation method therefor |
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