CN103014655A - Preparation method of Ga/Al-codoped ZnO film by ECR-PEMOCVD (electron cyclotron resonance-plasma-enhanced metal-organic chemical vapor deposition) low-temperature deposition - Google Patents
Preparation method of Ga/Al-codoped ZnO film by ECR-PEMOCVD (electron cyclotron resonance-plasma-enhanced metal-organic chemical vapor deposition) low-temperature deposition Download PDFInfo
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Abstract
The invention relates to a preparation method of a Ga/Al-codoped ZnO film by ECR-PEMOCVD (electron cyclotron resonance-plasma-enhanced metal-organic chemical vapor deposition) low-temperature deposition, belonging to the field of new material deposition preparation. The method comprises the following steps: (1) sequentially carrying out ultrasonic cleaning on a substrate with acetone, ethanol and deionized water, blow-drying with nitrogen gas, and sending the substrate into a reaction chamber; (2) vacuumizing the reaction chamber to 1.0*10<-3>Pa, heating the substrate to 20-600 DEG C, introducing argon-carried diethyl zinc, argon-carried trimethyl gallium, argon-carried trimethyl aluminum and oxygen into the reaction chamber, wherein the oxygen-diethyl zinc-trimethyl gallium-trimethyl aluminum flow ratio is controlled by a mass flowmeter at (100-150):(4-8):(1-2):1, and the total gas pressure is controlled at 0.8-2.0Pa; and reacting for 30 minutes to 3 hours under the ECR frequency of 650W to obtain the Ga/Al-codoped ZnO photoelectric transparent conducting film. The Ga/Al-codoped ZnO transparent photoelectric conducting film product has the advantages of low resistivity, favorable light transmittance and low price, and can easily implement large-area industrialized production.
Description
Technical field
The invention belongs to novel material deposition preparation field, the particularly preparation method of a kind of ECR-PEMOCVD low temperature depositing Ga, Al co-doped ZnO film.
Background technology
In the industry of the conductive electrodes such as current solar cell, LED photodiode, LCD flat panel demonstration and handset touch panel, the ITO(tin-doped indium oxide) because excellent electroconductibility and good visible light transmissivity become the necessary indispensable material of making conductive electrode.But because phosphide material is very rare, price is very expensive, the very large several factors such as hypertoxicity are arranged, studying in the world the substitute of ITO material at present, ZnO is exactly main a kind of replacement material always.
The deposition preparation of transparent conductive film and the performance of its film have very large related.Magnetron sputtering, laser pulse sputter and spraying method etc. have been proposed at present, but because the uniformity of film for preparing under the method exists very large problem and doping composition to be difficult to the series of problems such as control, make its performance always mutually weaker with the application of reality, when alternative ITO transparent conductive film, do not reach expected effect.
Plasma reinforcing and metal organic chemical vapor deposition (ECR-PEMOCVD) is the most frequently used experimental installation of preparation semiconductor film, is the most effective experimental program of the present semiconductor material of preparation.The most widely used semiconductor materials such as ZnO, GaN.It with hydride of the organic compound of III family, II family element and V, VI family element etc. as crystal growth source material, carry out the organic-matter chemical vapour phase epitaxy in the pyrolysis mode at substrate, the thin layer monocrystal material of grow various III-V family, group Ⅱ-Ⅵ compound semiconductor and their multivariate solid solution.The ECR-PEMOCVD technology plays an important role in the research and production practice.Its technology has the following advantages: the thickness of controlled made membrane makes its growth very thin film; Can realize the structure of multilayer film stack; Can carry out the accurate control of polynary mixed crystal composition; Can carry out the scale operation of compound semiconductor materials; Reactant gas source does not adopt halogenide, does not contain the very strong material that is corrosive in the reaction end gas, and in this case, the space segment of substrate and reaction can corrosion.
Current ECR-PEMOCVD technology and relevant device all do not have the transparent conductive film for the production of ZnO, therefore how to utilize the ECR-PEMOCVD technological merit, and the ZnO transparent conductive film of producing excellent performance is the difficult point that we study.
Summary of the invention
In order to solve present technical deficiency, the present invention adopts ECR-PEMOCVD low temperature depositing Ga, Al co-doped ZnO(GAZO) film, the preparation method of a kind of ECR-PEMOCVD low temperature depositing of the present invention Ga, Al co-doped ZnO film, carry out according to following steps:
(1) substrate is cleaned with ultrasonic wave successively with acetone, ethanol and deionized water after, dry up with nitrogen and to send into reaction chamber;
(2) reaction chamber is evacuated to 1.0 * 10
-3Pa, with substrate heating to 20 ~ 600 ℃, pass into the zinc ethyl that argon gas carries, the trimethyl-gallium that argon gas carries, trimethyl aluminium and the oxygen that argon gas carries in the reaction chamber, oxygen, zinc ethyl, trimethyl-gallium and trimethyl aluminium throughput ratio are (100 ~ 150): (4 ~ 8): (1 ~ 2): 1, controlled by mass flowmeter; Control gas total pressure is 0.8 ~ 2.0Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min ~ 3h obtains Ga, Al co-doped ZnO photoelectricity transparent conductive film.
Described substrate is common corning glass, sapphire, quartz, solar battery sheet, silicon chip or organic polymer.
Described solar battery sheet is not introduce the cell piece of negative potential or is the thin film solar cell sheet of introducing negative potential.
Described zinc ethyl Zn (CH
2CH
3)
2, trimethyl-gallium (TMGa) and trimethyl aluminium (TMAl) reaction source purity all be 99.99%, and carried by argon gas and to enter reaction chamber.
The purity in described oxygen reaction source is 99.99%.
The ECR-PEMOCVD technology of the low temperature depositing that utilization of the present invention can accurately be controlled, deposition is prepared high-quality doping ZnO transparent conductive film, and in conjunction with the problem that may occur in the actual production, propose a series of solution strategy, the industrialization of ZnO transparent conductive film is had very large Research Significance.(it is low that the transparent photoelectric conductive film product of GAZO has resistivity to the common doping ZnO of gallium aluminium of the present invention, the advantage of the industrialization that light transmission is good, cheap, be easy to realize that big area is produced.
Description of drawings
Fig. 1 is the analysis collection of illustrative plates of embodiment 1 film projection spectrum.
Embodiment
The below elaborates to embodiments of the invention, but protection scope of the present invention is not limited to following embodiment.
ECR-PEMOCVD of the present invention system is that application number is the equipment that 201210247144.8 invention is protected.
The electrical performance testing of sample of the present invention Hall testing apparatus, the model of Hall system is HL5500PC, range is 0.1 Ohm/square-100 GOhm/square.
The model of projection spectrum analysis equipment used is: finish on the MAYA2000PRO fiber spectrometer of Ocean company, light source is DH-2000-BAL, and spectral range is 190-1100nm.
Embodiment 1
After common corning glass cleaned with ultrasonic wave successively with acetone, ethanol and deionized water, dry up with nitrogen and to send into reaction chamber;
Reaction chamber is evacuated to 1.0 * 10
-3Pa, with substrate heating to 100 ℃, pass into the zinc ethyl that argon gas carries, the trimethyl-gallium that argon gas carries, trimethyl aluminium and the oxygen that argon gas carries in the reaction chamber, oxygen, zinc ethyl, trimethyl-gallium and the flow-ratio control of trimethyl aluminium reaction source are 100:4:2:1, by quality flowmeter flow quantity control, flow parameter is respectively 100 sccm, 4sccm, 2sccm, 1sccm; Control gas total pressure is 1.8Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min obtains Ga, Al co-doped ZnO photoelectricity transparent conductive film.
After finishing, experiment adopt the Hall testing apparatus that resistivity, mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 1, and Ga, Al jointly mix ZnO and compare with common ZnO film as can be seen from Table 1, and its resistivity obviously reduces, and mobility and carrier concentration obviously improve.Sample thin film has been carried out the analysis of projection spectrum, as shown in Figure 1, its result shows ECR-PEMOCVD system hypothermia deposition Ga, Al co-doped ZnO(GAZO) its transmittance of transparent conductive film can reach more than 80%.
The electric property contrast of table 1 ECR-PEMOCVD system hypothermia deposition Ga, Al co-doped ZnO and common magnetron sputtering ZnO
Embodiment 2
After common corning glass cleaned with ultrasonic wave successively with acetone, ethanol and deionized water, dry up with nitrogen and to send into reaction chamber;
Reaction chamber is evacuated to 1.0 * 10
-3Pa, with substrate heating to 100 ℃, pass into the zinc ethyl that argon gas carries, the trimethyl-gallium that argon gas carries, trimethyl aluminium and the oxygen that argon gas carries in the reaction chamber, oxygen, zinc ethyl, trimethyl-gallium and the flow-ratio control of trimethyl aluminium reaction source are 100:5:1:1, by quality flowmeter flow quantity control, flow parameter is respectively 100 sccm, 5sccm, 1sccm, 1sccm; Control gas total pressure is 1.2Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min obtains Ga, Al co-doped ZnO photoelectricity transparent conductive film.
After finishing, experiment adopt the Hall testing apparatus that resistivity, mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 2, and Ga, Al jointly mix ZnO and compare with common ZnO film as can be seen from Table 2, and its resistivity obviously reduces, and mobility and carrier concentration obviously improve.
The electric property contrast of table 2 ECR-PEMOCVD system hypothermia deposition Ga, Al co-doped ZnO and common magnetron sputtering ZnO
Embodiment 3:
After common corning glass cleaned with ultrasonic wave successively with acetone, ethanol and deionized water, dry up with nitrogen and to send into reaction chamber;
Reaction chamber is evacuated to 1.0 * 10
-3Pa, with substrate heating to 100 ℃, pass into the zinc ethyl that argon gas carries, the trimethyl-gallium that argon gas carries, trimethyl aluminium and the oxygen that argon gas carries in the reaction chamber, oxygen, zinc ethyl, trimethyl-gallium and the flow-ratio control of trimethyl aluminium reaction source are 100:6:2:1, by quality flowmeter flow quantity control, flow parameter is respectively 100 sccm, 6sccm, 2sccm, 1sccm; Control gas total pressure is 1.4Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min obtains Ga, Al co-doped ZnO photoelectricity transparent conductive film.
After finishing, experiment adopt the Hall testing apparatus that resistivity, mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 3, and Ga, Al jointly mix ZnO and compare with common ZnO film as can be seen from Table 3, and its resistivity obviously reduces, and mobility and carrier concentration obviously improve.
The electric property contrast of table 3 ECR-PEMOCVD system hypothermia deposition Ga, Al co-doped ZnO and common magnetron sputtering ZnO
Embodiment 4
After common corning glass cleaned with ultrasonic wave successively with acetone, ethanol and deionized water, dry up with nitrogen and to send into reaction chamber;
Reaction chamber is evacuated to 1.0 * 10
-3Pa, with substrate heating to 100 ℃, pass into the zinc ethyl that argon gas carries, the trimethyl-gallium that argon gas carries, trimethyl aluminium and the oxygen that argon gas carries in the reaction chamber, oxygen, zinc ethyl, trimethyl-gallium and trimethyl aluminium reaction source throughput ratio are made as 100:4:2:1, by quality flowmeter flow quantity control, flow parameter is respectively 100 sccm, 4sccm, 2sccm, 1sccm; Control gas total pressure is 1.6Pa; Be 650W in electron cyclotron resonance frequency, reaction 3h obtains Ga, Al co-doped ZnO photoelectricity transparent conductive film.
After finishing, experiment adopt the Hall testing apparatus that resistivity, mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 4, and Ga, Al jointly mix ZnO and compare with common ZnO film as can be seen from Table 4, and its resistivity obviously reduces, and mobility and carrier concentration obviously improve.
The electric property contrast of table 4 ECR-PEMOCVD system hypothermia deposition Ga, Al co-doped ZnO and common magnetron sputtering ZnO
Embodiment 5
After solar battery sheet cleaned with ultrasonic wave successively with acetone, ethanol and deionized water, dry up with nitrogen and to send into reaction chamber;
Reaction chamber is evacuated to 1.0 * 10
-3Pa, with substrate heating to 100 ℃, pass into the zinc ethyl that argon gas carries, the trimethyl-gallium that argon gas carries, trimethyl aluminium and the oxygen that argon gas carries in the reaction chamber, oxygen, zinc ethyl, trimethyl-gallium and the flow-ratio control of trimethyl aluminium reaction source are 100:8:2:1, by quality flowmeter flow quantity control, flow parameter is respectively 100 sccm, 8sccm, 2sccm, 1sccm; Control gas total pressure is 2.0Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min obtains Ga, Al co-doped ZnO photoelectricity transparent conductive film.
After finishing, experiment adopt the Hall testing apparatus that resistivity, mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 5, and Ga, Al jointly mix ZnO and compare with common ZnO film as can be seen from Table 4, and its resistivity obviously reduces, and mobility and carrier concentration obviously improve.
The electric property contrast of table 5 ECR-PEMOCVD system hypothermia deposition Ga, Al co-doped ZnO and common magnetron sputtering ZnO
Embodiment 6
After silicon chip cleaned with ultrasonic wave successively with acetone, ethanol and deionized water, dry up with nitrogen and to send into reaction chamber;
Reaction chamber is evacuated to 1.0 * 10
-3Pa, with substrate heating to 600 ℃, pass into the zinc ethyl that argon gas carries, the trimethyl-gallium that argon gas carries, trimethyl aluminium and the oxygen that argon gas carries in the reaction chamber, oxygen, zinc ethyl, trimethyl-gallium and trimethyl aluminium reaction source throughput ratio are 150:8:2:1, by quality flowmeter flow quantity control, flow parameter is respectively 150 sccm, 8sccm, 2sccm, 1sccm; Control gas total pressure is 0.8Pa; Be 650W in electron cyclotron resonance frequency, reaction 1.5h obtains Ga, Al co-doped ZnO photoelectricity transparent conductive film.
After finishing, experiment adopt the Hall testing apparatus that resistivity, mobility and the carrier concentration of film have been carried out test analysis.Ga, Al jointly mix ZnO and compare with common ZnO film, and its resistivity obviously reduces, and mobility and carrier concentration obviously improve.
Embodiment 7
After quartz cleaned with ultrasonic wave successively with acetone, ethanol and deionized water, dry up with nitrogen and to send into reaction chamber;
Reaction chamber is evacuated to 1.0 * 10
-3Pa, with substrate heating to 20 ℃, pass into the zinc ethyl that argon gas carries, the trimethyl-gallium that argon gas carries, trimethyl aluminium and the oxygen that argon gas carries in the reaction chamber, oxygen, zinc ethyl, trimethyl-gallium and the flow-ratio control of trimethyl aluminium reaction source are 150:8:2:1, by quality flowmeter flow quantity control, flow parameter is respectively 150 sccm, 8sccm, 2sccm, 1sccm; Control gas total pressure is 2.0Pa; Be 650W in electron cyclotron resonance frequency, reaction 1.5h obtains Ga, Al co-doped ZnO photoelectricity transparent conductive film.
After finishing, experiment adopt the Hall testing apparatus that resistivity, mobility and the carrier concentration of film have been carried out test analysis.Ga, Al jointly mix ZnO and compare with common ZnO film, and its resistivity obviously reduces, and mobility and carrier concentration obviously improve.
Claims (5)
1. the preparation method of an ECR-PEMOCVD low temperature depositing Ga, Al co-doped ZnO film is characterized in that carrying out according to following steps:
(1) substrate is cleaned with ultrasonic wave successively with acetone, ethanol and deionized water after, dry up with nitrogen and to send into reaction chamber;
(2) adopt the ECR-PEMOCVD system, reaction chamber is evacuated to 1.0 * 10
-3Pa, with substrate heating to 20 ~ 600 ℃, pass into the zinc ethyl that argon gas carries, the trimethyl-gallium that argon gas carries, trimethyl aluminium and the oxygen that argon gas carries in the reaction chamber, oxygen, zinc ethyl, trimethyl-gallium and trimethyl aluminium throughput ratio are (100 ~ 150): (4 ~ 8): (1 ~ 2): 1, controlled by mass flowmeter; Control gas total pressure is 0.8 ~ 2.0Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min ~ 3h obtains Ga, Al co-doped ZnO photoelectricity transparent conductive film.
2. the preparation method of a kind of ECR-PEMOCVD low temperature depositing Ga according to claim 1, Al co-doped ZnO film is characterized in that described substrate is common corning glass, sapphire, quartz, solar battery sheet, silicon chip or organic polymer.
3. the preparation method of a kind of ECR-PEMOCVD low temperature depositing Ga according to claim 2, Al co-doped ZnO film is characterized in that described solar battery sheet is not introduce the cell piece of negative potential or is the thin film solar cell sheet of introducing negative potential.
4. the preparation method of a kind of ECR-PEMOCVD low temperature depositing Ga according to claim 1, Al co-doped ZnO film, the purity that it is characterized in that described zinc ethyl, trimethyl-gallium and trimethyl aluminium reaction source is 99.99%, and is carried by argon gas and to enter reaction chamber.
5. the preparation method of a kind of ECR-PEMOCVD low temperature depositing Ga according to claim 1, Al co-doped ZnO film, the purity that it is characterized in that described oxygen reaction source is 99.99%.
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| CN2012105764718A CN103014655A (en) | 2012-12-27 | 2012-12-27 | Preparation method of Ga/Al-codoped ZnO film by ECR-PEMOCVD (electron cyclotron resonance-plasma-enhanced metal-organic chemical vapor deposition) low-temperature deposition |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103352208A (en) * | 2013-07-17 | 2013-10-16 | 沈阳工程学院 | Preparation method for InN film low temperature sedimentation on diamond plated film by adopting ECR-PEMOCVD |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020130032A1 (en) * | 2001-03-15 | 2002-09-19 | Ahn Kie Y. | Method and apparatus for the fabrication of ferroelectric films |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020130032A1 (en) * | 2001-03-15 | 2002-09-19 | Ahn Kie Y. | Method and apparatus for the fabrication of ferroelectric films |
Non-Patent Citations (2)
| Title |
|---|
| A. MARTIN, ET AL: "Preparation of transparent and conductive Al-doped ZnO thin films by ECR plasma enhanced CVD", 《SURFACE AND COATINGS TECHNOLOGY》 * |
| WOOJIN LEE，ET AL: "Investigation of electronic and optical properties in Al_Ga codoped ZnO thin films", 《CURRENT APPLIED PHYSICS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103352208A (en) * | 2013-07-17 | 2013-10-16 | 沈阳工程学院 | Preparation method for InN film low temperature sedimentation on diamond plated film by adopting ECR-PEMOCVD |
| CN103352208B (en) * | 2013-07-17 | 2015-08-12 | 沈阳工程学院 | The preparation method of ECR-PEMOCVD low temperature depositing InN film on the Si of gold-plated diamond thin film |
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Application publication date: 20130403 |