CN1600896A - Preparation method of zinc oxide film with enhanced ultraviolet emission - Google Patents
Preparation method of zinc oxide film with enhanced ultraviolet emission Download PDFInfo
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- CN1600896A CN1600896A CN 200410067128 CN200410067128A CN1600896A CN 1600896 A CN1600896 A CN 1600896A CN 200410067128 CN200410067128 CN 200410067128 CN 200410067128 A CN200410067128 A CN 200410067128A CN 1600896 A CN1600896 A CN 1600896A
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- Prior art keywords
- zinc
- oxide film
- ultraviolet emission
- zinc oxide
- target
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 32
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052742 iron Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000011701 zinc Substances 0.000 claims abstract description 16
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims description 22
- 229960001296 zinc oxide Drugs 0.000 claims description 22
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 11
- 238000005516 engineering process Methods 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 238000003466 welding Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000010408 film Substances 0.000 claims 2
- 239000010409 thin film Substances 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 8
- 238000011161 development Methods 0.000 abstract description 3
- 239000002019 doping agent Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract 2
- 229910052751 metal Inorganic materials 0.000 abstract 2
- 238000005546 reactive sputtering Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000002950 deficient Effects 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000002294 plasma sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
A method for preparing zinc oxide film with enhanced ultraviolet emission adopts a magnetron reactive sputtering method, and is characterized in that: 99.999 percent of metal zinc is adopted as a cathode target, and 0.1 to 5 weight percent of spectrally pure metal iron is doped in the cathode target. The zinc oxide film plated by the method of the invention after iron doping has obviously enhanced ultraviolet band edge emission and low cost. Pure iron is used as a doping agent, argon is used as a working gas, oxygen is used as a reaction raw material, the material source is rich, the price is low, and the material has development and application values.
Description
Technical field
The present invention relates to zinc-oxide film, specifically a kind of ultraviolet emission strengthens the preparation method of zinc-oxide film.
Background technology
Zinc oxide is a kind of self activation semiconductor material with wide forbidden band with hexagonal structure, energy gap under the room temperature is 3.36eV, particularly its exciton binding energy is up to 60 milli ev, leading in semiconductor material commonly used at present, this characteristic makes it possess the favourable condition of short-wave long light-emitting under the room temperature.In addition, zinc oxide has very high electroconductibility, and it is also the same with other oxide compounds to have very high chemical stability and high temperature resistant character, and its source enriches, and is cheap.These advantages make it become the excellent material of preparation opto-electronic device, have the value of development and application.
As a kind of semiconductor material with wide forbidden band, be that the various luminescent materials of matrix have been furtherd investigate and widespread use with zinc oxide.The method for preparing zinc-oxide film has a variety of, as magnetron sputtering, chemical vapour deposition, plasma sputtering, pulsed laser deposition and molecular beam epitaxy etc.Though pulsed laser deposition and molecular beam epitaxy technique can be prepared high-quality zinc-oxide film, these two kinds of methods are because equipment price costliness and maintenance cost height consider to be difficult to realize industrialization from economic benefit.The easiest the most frequently used most economical method is a magnetron sputtering at present.Because the restriction of technology of preparing itself, generally the atomic ratio with zinc and oxygen in the zinc-oxide film of magnetron sputtering preparation is a non-stoichiometric, and this is because the existence of defectives such as a large amount of zinc gaps or oxygen room.This not only causes the ultraviolet emission intensity of zinc oxide low, and the emission that caused by defective also occurred at visible light wave range.
Summary of the invention
The object of the present invention is to provide a kind of economical and practical, the at room temperature deposition and the preparation method of ultraviolet emission enhanced zinc-oxide film.
To achieve these goals, technical scheme of the present invention is:
A kind of preparation method of ultraviolet emission enhanced zinc-oxide film adopts the reactive magnetron sputtering method, it is characterized in that: the metallic zinc of employing 99.999% is mixed the specpure metallic iron of 0.1-5wt% and is made sputter cathode target.
The concrete steps of the inventive method are as follows:
The specpure metallic iron that mixes 0.1-5wt% (weight percent) in the metallic zinc powder of experiment employing 99.999% is made into block sputter cathode target, and this sputter zinc target welding is received on the red copper base plate, to guarantee the water-cooling effect and the conductivity of target.Anode links to each other with vacuum chamber; Substrate after the ultrasonic cleaning is contained on the substrate chuck, and shifting board places between substrate chuck and the target; Vacuumize after shutting each air valve, reach 3 * 10 until vacuum tightness
-3More than the Pa; Feed an amount of argon gas and oxygen, argon oxygen ratio is 1: 1-1: 10; Regulate high valve to required operating air pressure (～10
-1Pa); Open the pre-sputter of direct supply build-up of luminance 5～10 minutes; Regulating electric current is the 0.25-0.50 ampere, and the rotation substrate chuck is removed shifting board, the beginning deposit film; Keep default sputtering technology condition, voltage is 2Kv, and air pressure is 0.5Pa.
Described substrate is quartz plate or crystal wafer or silicon chip.
Test prepared zinc-oxide film and show through room temperature fluorescence spectrum test result, compare with unadulterated zinc-oxide film, the ultraviolet band edge emission of mixing the zinc-oxide film behind the iron obviously strengthens, referring to Fig. 1.
The present invention compares with technology formerly, and the advantage that has is that cost is low.Adopt pure iron to make doping agent, as reaction raw materials, material source is abundant, and is cheap as working gas, oxygen for argon gas, has the value of development and application.
Description of drawings
Fig. 1 is a fluorescent emission spectrogram of mixing iron front and back zinc-oxide film
Embodiment
The invention will be further described below by embodiment, but should not limit protection scope of the present invention with this.
Embodiment 1
Under the room temperature, adopt the reactive magnetron sputtering method, equipment is DMD-450 type magnetron sputtering plane coating equipment, and experiment adopts 99.999% metallic zinc as the negative electrode target, anode links to each other with vacuum chamber, mixes the specpure metallic iron of 0.1wt% (weight percent) in cathode targets.In experimental installation, sputter zinc target welding is received on the red copper base plate, to guarantee the water-cooling effect and the conductivity of target.Substrate after the ultrasonic cleaning is contained on the substrate chuck, and shifting board places between substrate chuck and the target; Vacuumize after shutting each air valve, reach 3 * 10 until vacuum tightness
-3More than the Pa; Feed an amount of argon gas and oxygen, argon oxygen ratio is 1: 1; Regulate high valve to required operating air pressure-0.5Pa; Open the pre-sputter of direct supply build-up of luminance 5 minutes; Regulating electric current is 0.25 ampere, and the rotation substrate chuck is removed shifting board, the beginning deposit film; Keep default sputtering technology condition, voltage is 2Kv, and air pressure is 0.5Pa.
, obviously strengthen by the prepared zinc-oxide film ultraviolet emission of reaction magnetocontrol sputtering after mixing iron 0.1wt%, as the negative electrode target with pure zinc referring to Fig. 1.
Embodiment 2
Under the room temperature, adopt the reactive magnetron sputtering method, equipment is DMD-450 type magnetron sputtering plane coating equipment, and experiment adopts 99.999% metallic zinc as the negative electrode target, and anode links to each other with vacuum chamber, mixes the specpure metallic iron of 2wt% in cathode targets.In experimental installation, sputter zinc target welding is received on the red copper base plate, to guarantee the water-cooling effect and the conductivity of target.Substrate after the ultrasonic cleaning is contained on the substrate chuck, and shifting board places between substrate chuck and the target; Vacuumize after shutting each air valve, reach 3 * 10 until vacuum tightness
-3More than the Pa; Feed an amount of argon gas and oxygen, argon oxygen ratio is 1: 5; Regulate high valve to required operating air pressure (0.5Pa); Open the pre-sputter of direct supply build-up of luminance 8 minutes; Regulating electric current is 0.35 ampere, and the rotation substrate chuck is removed shifting board, the beginning deposit film; Keep default sputtering technology condition, voltage is 2Kv, and air pressure is 0.5Pa.
, obviously strengthen by the prepared zinc-oxide film ultraviolet emission of reaction magnetocontrol sputtering after mixing iron 2wt%, as the negative electrode target with pure zinc referring to Fig. 1.
Embodiment 3
Under the room temperature, adopt the reactive magnetron sputtering method, equipment is DMD-450 type magnetron sputtering plane coating equipment, and experiment adopts 99.999% metallic zinc as the negative electrode target, and anode links to each other with vacuum chamber, mixes the specpure metallic iron of 5wt% in cathode targets.In experimental installation, sputter zinc target welding is received on the red copper base plate, to guarantee the water-cooling effect and the conductivity of target.Substrate after the ultrasonic cleaning is contained on the substrate chuck, and shifting board places between substrate chuck and the target; Vacuumize after shutting each air valve, reach 3 * 10 until vacuum tightness
-3More than the Pa; Feed an amount of argon gas and oxygen, argon oxygen ratio is 1: 10; Regulate high valve to required operating air pressure-0.5Pa; Open the pre-sputter of direct supply build-up of luminance 10 minutes; Regulating electric current is 0.50 ampere, and the rotation substrate chuck is removed shifting board, the beginning deposit film; Keep default sputtering technology condition, voltage is 2Kv, and air pressure is 0.5Pa.
, obviously strengthen by the prepared zinc-oxide film ultraviolet emission of reaction magnetocontrol sputtering after mixing iron 5wt%, as the negative electrode target with pure zinc referring to Fig. 1.
Claims (3)
1, a kind of preparation method of ultraviolet emission enhanced zinc-oxide film adopts the reactive magnetron sputtering method, it is characterized in that: the metallic zinc of employing 99.999% is mixed the specpure metallic iron of 0.1-5wt% as the negative electrode target in cathode targets.
2, ultraviolet emission enhanced method for preparing zinc oxide thin film according to claim 1, the concrete steps that it is characterized in that this method are: adopt 99.999% metallic zinc, the specpure metallic iron that mixes 0.1-5wt% again is made into block negative electrode target, and this negative electrode target welding is received on the red copper base plate; Anode links to each other with vacuum chamber; Substrate after the ultrasonic cleaning is contained on the substrate chuck, and shifting board places between substrate chuck and the target; Vacuumize after shutting each air valve, reach 3 * 10 until vacuum tightness
-3More than the Pa; Feed an amount of argon gas and oxygen, argon oxygen ratio is 1: 1-1: 10; Turn down high valve to required operating air pressure-10
-1Pa; Opened the pre-sputter 5-10 of direct supply build-up of luminance minute; Regulating electric current is the 0.25-0.50 ampere, and the rotation substrate chuck is removed shifting board, the beginning deposit film; Keep default sputtering technology condition, voltage is 2Kv, and air pressure is 0.5Pa.
3, ultraviolet emission enhanced method for preparing zinc oxide thin film according to claim 1 and 2 is characterized in that described substrate is quartz plate or crystal wafer or silicon chip.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410067128 CN1600896A (en) | 2004-10-13 | 2004-10-13 | Preparation method of zinc oxide film with enhanced ultraviolet emission |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410067128 CN1600896A (en) | 2004-10-13 | 2004-10-13 | Preparation method of zinc oxide film with enhanced ultraviolet emission |
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| Publication Number | Publication Date |
|---|---|
| CN1600896A true CN1600896A (en) | 2005-03-30 |
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| CN 200410067128 Pending CN1600896A (en) | 2004-10-13 | 2004-10-13 | Preparation method of zinc oxide film with enhanced ultraviolet emission |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100509998C (en) * | 2005-11-26 | 2009-07-08 | 中国科学院合肥物质科学研究院 | Zinc oxide nano-sheet film material with ultraviolet light-emitting property and preparation method thereof |
-
2004
- 2004-10-13 CN CN 200410067128 patent/CN1600896A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100509998C (en) * | 2005-11-26 | 2009-07-08 | 中国科学院合肥物质科学研究院 | Zinc oxide nano-sheet film material with ultraviolet light-emitting property and preparation method thereof |
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| PB01 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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