CN1696356A - Self-assembly method for developing film of zinc oxide through induction of seed crystal and liquid phase epitaxy in low temperature - Google Patents
Self-assembly method for developing film of zinc oxide through induction of seed crystal and liquid phase epitaxy in low temperature Download PDFInfo
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- CN1696356A CN1696356A CN 200410010860 CN200410010860A CN1696356A CN 1696356 A CN1696356 A CN 1696356A CN 200410010860 CN200410010860 CN 200410010860 CN 200410010860 A CN200410010860 A CN 200410010860A CN 1696356 A CN1696356 A CN 1696356A
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- zno
- seed crystal
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- low temperature
- zinc acetate
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Abstract
A process for growing zinc oxide film by seed crystal inducing and low-temp liquid-phase epitaxial self-assembly includes mixing zinc acetate with sodium bicarbonate, grinding, reacting at 160 deg.C for 2-4 hrs, washing with deionized water, baking at 100 deg.C to obtain substrate, spinning-coating the alcohol solution of non-crystal ZnO on the substrate, reaction at 180-200 deg.C for 2-4 hrs to generate crystal seeds with same orientation, immersing it in organics solution of zinc acetate, and growing at 80-100 deg.C for 15-20 hrs.
Description
Technical field
The invention belongs to technical field of semiconductor, relate to the preparation of oxide semiconductor thin-film, specifically a kind of seed crystal is induced, the method for low temperature liquid phase extension self-assembled growth zinc-oxide film.
Background technology
ZnO is a direct broad-band gap II-VI family semiconductor material, and its bandwidth is 3.37eV, and the room-temperature exciton bound energy is up to 60meV, and it is luminous to obtain efficient ultraviolet (UV) with it in theory.ZnO has similar crystalline network and energy gap to GaN, but the ZnO cost of material is cheap, acquisition easily, and has higher fusing point than GaN, and fusing point is at 1975 ℃.ZnO room-temperature exciton bound energy is 60meV.Because tiing up, the room-temperature exciton card can also far above the exciton bind energy 28meV of GaN, make ZnO at room temperature can produce laser far above the hot ionization energy 25meV of room temperature with lower energy.ZnO exciton stimulated emission at room temperature is observed.Because to growing demands of UV photoelectric device such as UV-laser apparatus, ultraviolet light-emitting diode (UV-LED), UV-sensitive detection parts, to the research of ZnO, so ZnO becomes the recent studies on focus in this field, the current world rapidly to people diversion.
Research work development about the ZnO material both at home and abroad is rapid, and its method for manufacturing thin film is mainly the deriving technology of metal organic chemical vapor deposition (MOCVD), molecular beam epitaxy (MBE) and these methods.Adopt aforesaid method all to need expensive equipment and high operating cost, and all must under the high temperature more than 500 ℃, finish the material growth.At high temperature carry out the ZnO crystal film growth and be easy to generate thermal defect, in addition, ZnO crystal film and Al
2O
3Substrate also very easily produces thermal defect in the difference of aspects such as lattice parameter and thermal expansivity, thereby is difficult to the high-quality ZnO film of preparation.Though scientists both domestic and external research has in this respect obtained than much progress, also has very big distance from the ZnO film material that satisfies the device quality requirement.
Summary of the invention
The method that the purpose of this invention is to provide a kind of good reproducibility, reliability height, low temperature liquid phase extension self-assembled growth zinc-oxide film that cost is low.
For achieving the above object, the present invention utilizes amorphous-seed crystal induction method growing zinc oxide film.At first, prepare amorphous ZnO by chemical reaction; Utilize the metastable characteristic of amorphous ZnO then, on substrate, generate the ZnO seed crystal of high same orientation; At last at low temperatures, as 200 ℃, with the ZnO film of rheotaxy self-assembling technique growing high-quality.
Preparation amorphous ZnO.With etc. the zinc acetate of quality and sodium bicarbonate at room temperature fully grind, zinc acetate is mixed fully with sodium bicarbonate, help both complete reactions.Reacted 2～4 hours down at 160 ℃, product is obtained the amorphous ZnO powder of white with washed with de-ionized water and after 100 ℃ of oven dry.
On substrate, generate the ZnO seed crystal of high same orientation.Utilize spin coating technique that 1～3% amorphous ZnO ethanolic soln is spin-coated on the cleaned substrate equably, wherein substrate can adopt crystal SiO
2, Al
2O
3, GaAs or Si.Reacted 2～4 hours down at 180～200 ℃.Because the metastable characteristic of amorphous ZnO, amorphous ZnO molecule is activated when 180 ℃～200 ℃ of temperature, generates the ZnO seed crystal of same orientation under the inducing of substrate along substrate direction crystallization.
Grow ZnO film with the rheotaxy self-assembling method.Crystallization on the substrate is generated the ZnO seed crystal of same orientation, place 1～5 * 10
-5In the zinc acetate organic solution of M/mL, under 80 ℃～100 ℃ low temperature, grew 15～20 hours, just obtain high-quality ZnO crystal film.Used organic solvent is ethanol or a condensed ethandiol or tirethylene glycol or propyl carbinol or urotropine or Polyacrylamide.
Owing to utilize amorphous-seed crystal revulsion and low temperature liquid phase extension self-assembling technique, therefore, with the ZnO crystal film of the present invention preparation have quality height, good reproducibility, reliability height, cost low, easily form advantage such as industrialization, for the application and the industrialized development of ZnO ultraviolet light photo device provides effective material preparation method.
Embodiment
At room temperature, etc. zinc acetate, the sodium bicarbonate of quality fully be ground to and make zinc acetate and sodium bicarbonate that chemical reaction can take place fully.Zinc acetate and sodium bicarbonate are the chemical analysis pure reagent.After zinc acetate and sodium bicarbonate fully grind, zinc acetate is mixed fully with sodium bicarbonate, help both complete reactions.Reacted 2 hours down at 160 ℃, product obtains the amorphous ZnO powder of white with washed with de-ionized water and 100 ℃ of oven dry.
Utilize spin coating technique that 1% amorphous ZnO ethanolic soln is spin-coated on the cleaned substrate equably.Employed ethanol is the chemical analysis pure reagent, and used substrate is crystal Al
2O
3, the lattice direction of substrate is (0001).Reacted 3 hours down at 200 ℃.After the amorphous ZnO reaction, at substrate Al
2O
3(0001) the direction crystallization generates the ZnO seed crystal of same orientation.
With Al
2O
3Crystallization generates the ZnO seed crystal of same orientation on the substrate, places 1 * 10
-5In the zinc acetate organic solution of M/mL, under 80 ℃ of low temperature, grew 20 hours, prepare the ZnO crystal film.Used organic solvent is a tirethylene glycol.Tirethylene glycol is the chemical analysis pure reagent.
Measure the ZnO crystal film with the X ray method of spreading out.The X-ray diffraction result only demonstrates the diffraction peak of ZnO (002), and its half-width only is 7 ' (0.12 °).From the room temperature photoluminescence spectra, learn and have only ultraviolet emission.
Claims (5)
1, seed crystal induce, the method for low temperature liquid phase extension self-assembled growth zinc-oxide film, it is characterized in that: at first, prepare amorphous ZnO by chemical reaction; Utilize the metastable characteristic of amorphous ZnO then, on substrate, generate the ZnO seed crystal of high same orientation; At last at low temperatures, use the ZnO film of rheotaxy self-assembling technique growing high-quality.
2, seed crystal according to claim 1 induce, the method for low temperature liquid phase extension self-assembled growth zinc-oxide film, it is characterized in that with etc. the zinc acetate of quality and sodium bicarbonate at room temperature fully grind, zinc acetate is mixed fully with sodium bicarbonate, reacted 2～4 hours down at 160 ℃, product is obtained the amorphous ZnO powder of white with washed with de-ionized water and after 100 ℃ of oven dry; With spin coating technique 1～3% amorphous ZnO ethanolic soln is spin-coated on the cleaned substrate equably, 160～200 ℃ of reactions 2～4 hours down, amorphous ZnO generates the ZnO seed crystal of same orientation along substrate direction crystallization; Crystallization on the substrate is generated the ZnO seed crystal of same orientation, place 1～5 * 10
-5In the zinc acetate organic solution of M/mL, under 80 ℃～100 ℃ low temperature, grew 15～20 hours, obtain high-quality ZnO crystal film.
3, seed crystal according to claim 2 induce, the method for low temperature liquid phase extension self-assembled growth zinc-oxide film, it is characterized in that substrate adopts crystal SiO
2Or Al
2O
3Or GaAs or Si.
4, seed crystal according to claim 3 induce, the method for low temperature liquid phase extension self-assembled growth zinc-oxide film, the organic solvent that it is characterized in that described zinc acetate organic solution is ethanol or a condensed ethandiol or tirethylene glycol or propyl carbinol or urotropine or Polyacrylamide.
5, seed crystal according to claim 4 induce, the method for low temperature liquid phase extension self-assembled growth zinc-oxide film, it is characterized in that zinc acetate and sodium bicarbonate fully grind after, zinc acetate is mixed fully, 160 ℃ of reactions 2 hours down with sodium bicarbonate; With spin coating technique 1% amorphous ZnO ethanolic soln is spin-coated on the cleaned substrate equably, used substrate is crystal Al
2O
3, the lattice direction of substrate is (0001), reacts 3 hours down at 200 ℃; With Al
2O
3Crystallization generates the ZnO seed crystal of same orientation on the substrate, places 1 * 10
-5In the zinc acetate organic solution of M/mL, under 80 ℃ of low temperature, grew 20 hours, used organic solvent is a tirethylene glycol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410010860 CN1696356A (en) | 2004-05-12 | 2004-05-12 | Self-assembly method for developing film of zinc oxide through induction of seed crystal and liquid phase epitaxy in low temperature |
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| CN 200410010860 CN1696356A (en) | 2004-05-12 | 2004-05-12 | Self-assembly method for developing film of zinc oxide through induction of seed crystal and liquid phase epitaxy in low temperature |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012037729A1 (en) * | 2010-09-25 | 2012-03-29 | Ye Zhizhen | METHOD FOR MANUFACTURING P-TYPE ZnO-BASED MATERIAL |
| CN104818526A (en) * | 2015-01-27 | 2015-08-05 | 夏洋 | Preparation method for vapor grown two-dimensional material |
-
2004
- 2004-05-12 CN CN 200410010860 patent/CN1696356A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012037729A1 (en) * | 2010-09-25 | 2012-03-29 | Ye Zhizhen | METHOD FOR MANUFACTURING P-TYPE ZnO-BASED MATERIAL |
| CN103180491A (en) * | 2010-09-25 | 2013-06-26 | 叶志镇 | Method for preparing p-type zno-based material |
| CN103180491B (en) * | 2010-09-25 | 2016-02-17 | 叶志镇 | A kind of preparation method of p-type zno-based material |
| CN104818526A (en) * | 2015-01-27 | 2015-08-05 | 夏洋 | Preparation method for vapor grown two-dimensional material |
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