CN103031556A - Deposition preparation method of ZnO/Al/ZnO photoelectric transparent conducting thin film - Google Patents
Deposition preparation method of ZnO/Al/ZnO photoelectric transparent conducting thin film Download PDFInfo
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- CN103031556A CN103031556A CN2012105760261A CN201210576026A CN103031556A CN 103031556 A CN103031556 A CN 103031556A CN 2012105760261 A CN2012105760261 A CN 2012105760261A CN 201210576026 A CN201210576026 A CN 201210576026A CN 103031556 A CN103031556 A CN 103031556A
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Abstract
The invention belongs to the field of transparent conducting materials, and particularly relates to a deposition preparation method of a ZnO/Al/ZnO photoelectric transparent conducting thin film. The method comprises the steps that a glass substrate is cleaned and sent to a vapor deposition reaction chamber; argon and oxygen both containing Zn(CH2CH3)2 are supplied into the reaction chamber; deposition preparation is performed to form a 20-50nm thick ZnO thin film; then the substrate is placed in a magnetron sputtering chamber for magnetron sputtering by taking pure Al as a target material to form a 5-30nm thick Al film; the substrate is transferred into the vapor deposition reaction chamber again; the deposition preparation is performed again to form a 20-50nm ZnO thin film; the substrate is subjected to high-temperature annealing at 100-400 DEG C; and the ZnO/Al/ZnO photoelectric transparent conducting thin film is obtained. The method is simple in preparation technology, and a deposition process is easy to control. The prepared transparent conducting thin film is good in uniformity, and excellent in photoelectric property, and can be used for fabricating transparent electrodes of photoelectric devices such as solar cells, light emitting diodes, LCDs (liquid crystal displays) and mobile phones.
Description
Technical field
The invention belongs to the transparent conductive material field, be specifically related to a kind of deposition preparation of ZnO/Al/ZnO photoelectricity transparent conductive film.
Background technology
Along with advancing by leaps and bounds of social development and science and technology, human demand to functional materials increases day by day, and new function material has become the key of new technology and infant industry's development.Along with the development of the industries such as sun power, flat pannel display and semiconductor lighting, a kind of new functional materials---transparent conductive material thereupon Emergence and Development gets up.General electro-conductive material such as metal and alloy-based semiconductor equalizing are opaque material, but in actual applications, as as the electrode of electrode of solar battery, thin-film solar cells, the electrode of liquid-crystal display etc., all require in conduction, can see through visible light, in general, satisfy following two requirements and can become transparent conductive material: (1) is to visible light (the average transmittances T of wavelength X=380～780nm)
Avg80%; (2) possess excellent conductivity, resistivity is lower than 10
-3Ω cm.
The electrically conducting transparent semiconductor equalizing of development is the broad stopband oxide semiconductor material at present, be transparent conductive film (transparent conductive oxide, referred to as the TCO film), the common light electrical characteristic such as this class film has that the forbidden band is wide, visible range optical transmittance height and resistivity are low, can further improve its conductivity through after the suitable doping, have broad application prospects.
The TCO material of at present widespread use is mainly three classes, ITO-In
2O
3Base film (Sn doping), FTO-SnO
2Base film (F doping) and AZO-ZnO base film (Al doping) etc. are described below respectively: (1) ITO-In
2O
3Crystalline structure be body-centered cubic Ferromanganese Ore structure, the about 3.5eV of energy gap, thereby transparent at visible-range, T
Avg90%, lowest resistivity can reach 10
-5Ω
.The cm magnitude.ITO is present the most ripe, most widely used TCO, but because ITO must use rare metal indium (1.3 ten thousand tons of Chinese indium retained reserves, account for the whole world 2/3), thereby cause production cost very high, along with TFT-LCD panel market continues further developing of amplification and solar cell, 83% of global indium consumption is used for ITO, thereby has also caused the problem that the indium ore deposit will exhaust gradually in future, and phosphide material is poisonous, and is harmful in preparation and application process.The nucleidic mass of indium and tin is larger in addition, penetrate into easily substrate interior in the film process, poison substrate material, especially contamination phenomenon is serious in liquid crystal display device, and for the sun power industry, TCO glass must possess the ability that improves scattering of light, and the ITO plated film is difficult to accomplish this point, and laser ablation poor-performing, ITO are also stable not in plasma body, and in a word, it is imperative to seek suitable substitute products; (2) FTO-SnO
2Rutile structure with positive tetrahedron, energy gap is 3.6eV, obtain the FTO film by doped with fluorine, can further strengthen conductivity, FTO compares with ITO has the thermostability height, corrosion-resistant, the advantages such as hardness height, and in plasma body, also has good stability, thereby become the photovoltaic TCO material of present commercial applications, but, high crystalline quality FTO film preparation is difficulty relatively, preparation technology is required height, owing to the existence of film subsurface defect makes its transmittance and specific conductivity be lower than ito thin film, simultaneously owing to need fluorine element (severe toxicity) to mix thereby there is certain pollution in technological process, in addition, because the FTO film hardness is high thereby relatively be difficult to etching; (3) AZO-ZnO belongs to N-type II-VI family semiconductor material, its crystalline structure is the about 3.4eV of hexagonal wurtzite structure energy gap, transmittance can reach more than 90%, simultaneously ZnO existence owing to intrinsic oxygen vacancy defect in plain situation also has higher specific conductivity, by the element (Al of III family, Ga, B) doping can further improve electroconductibility, ZnO is used for the TCO film and has abundant raw material, with low cost, preparation technology is simple, nontoxic, the significant advantage of grade free from environmental pollution, and, ZnO can stability be better than ito thin film in hydrogen plasma, have and be easy to again etching can be with the comparable photoelectric characteristic of ito thin film the time, but ZnO high efficiency transmission ITO is difficult to the short wavelength light of transmission in addition, thereby no matter be on solar cell or flat pannel display, ZnO is the strong rival who substitutes ITO and FTO.
At present the relevant report about the film of ZnO and ZnO doping Al element has a lot, but adopt general doping way, the osmotic effect of Al element in the vacancy defect of ZnO is bad, carrier concentration is not high, contribution for the specific conductivity that improves film is very limited, therefore, how to make the Al element be doped to better in the ZnO film, further improving the conductivity of conductive transparent material, is present problem demanding prompt solution.
Summary of the invention
The present invention is directed to the problem that prior art exists, the invention provides a kind of deposition preparation of ZnO/Al/ZnO photoelectricity transparent conductive film, purpose is to deposit preparation quality excellence, ZnO/Al/ZnO transparent conductive film that conductivity is good by adopting plasma to strengthen mode that electron cyclotron resonace organic chemical vapor deposition system combines with magnetic control sputtering system, and its resistivity can be low to moderate 9.2 * 10
-5Ω cm, and its transmittance can reach more than 80%.
The technical scheme of realization the object of the invention is carried out according to following steps:
(1) glass substrate is used acetone, ethanol and deionized water ultrasonic cleaning successively after, dry up with nitrogen and to send into phase depositing reaction chamber, reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:(100-150), the control microwave power is 650W, the thick ZnO film of deposition preparation 20-50nm, deposition is cleaned phase depositing reaction chamber with high pure nitrogen after finishing, and takes out substrate;
The substrate that (2) will deposit ZnO film places magnetron sputtering chamber, and the magnetron sputtering chamber vacuum is evacuated to 10
-4Behind the Pa, heated substrate to 100 ℃, passing into argon gas control air pressure is 8Pa, carries out magnetron sputtering take pure Al as target, and sputtering power is 100W, and sputtering time is 1-5min, is depositing the Al film that sputter 5-30nm is thick on the glass substrate of ZnO film;
(3) substrate after the above-mentioned sputter is transferred in the phase depositing reaction chamber, reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:(100-150), the control microwave power is 650W, the thick ZnO film of deposition preparation 20-50nm again, deposition is cleaned vapor deposition reaction with high pure nitrogen after finishing, and takes out substrate;
(4) to above-mentioned substrate in 100-400 ℃ of high temperature annealing 30min, obtaining structure is the photoelectricity transparent conductive film of ZnO/Al/ZnO.
Described glass substrate is common corning glass substrate.
Compared with prior art, characteristics of the present invention and beneficial effect are:
The inventive method is to adopt plasma to strengthen the mode that electron cyclotron resonace organic chemical vapor deposition technology combines with magnetron sputtering technique, utilize the low-resistivity of the good photoelectric properties of ZnO and Al, form the laminated film of ZnO/Al/ZnO structure, passed through again the high temperature anneal;
The sandwich structure of ZnO/Al/ZnO, be very beneficial for diffusion and the infiltration of Al between film, because Al mixes, carrier concentration increases in the hole of ZnO, the conductivity of film is greatly improved, simultaneously can keep transmittance to reach more than 80%, owing to be organic chemical vapor deposition, its film quality is fabulous;
Preparation technology of the present invention is simple, and deposition process is easy to control.The transparent conductive film good uniformity of the present invention's preparation, photoelectric properties are excellent, can be used for making the transparency electrode of the photoelectric devices such as solar cell, photodiode, LCD and mobile phone.
Description of drawings
Fig. 1 is the ZnO/Al/ZnO transparent conductive film synoptic diagram that the inventive method obtains;
Wherein: 1: glass substrate; The 2:ZnO film; The 3:Al intermediate layer film;
Fig. 2 is the transmittance figure of ZnO/Al/ZnO transparent conductive film under visible wavelength of the embodiment of the invention 1 preparation;
Fig. 3 is the SEM figure of the ZnO/Al/ZnO transparent conductive film of the embodiment of the invention 1 preparation.
Embodiment
It is the ECR-PEMOCVP system that plasma described in the present invention strengthens electron cyclotron resonace organic chemical vapor deposition system, has been open in 201210247144.8 the patent application at application number; Described magnetron sputtering Controlling System is JPGD-450 magnetic control platform.
The invention will be further described below in conjunction with embodiment.
After glass substrate used acetone, ethanol and deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into phase depositing reaction chamber;
Reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:150, the control microwave power is 650W, the thick ZnO film of deposition preparation 20nm, deposition is cleaned phase depositing reaction chamber with high pure nitrogen after finishing, and takes out substrate;
The substrate that deposits ZnO film is placed magnetron sputtering chamber, the magnetron sputtering chamber vacuum is evacuated to 10
-4Behind the Pa, heated substrate to 100 ℃, passing into argon gas control air pressure is 8Pa, carries out magnetron sputtering take pure Al as target, and sputtering power is 100W, and sputtering time is 1min, is depositing the Al film that sputter 5nm is thick on the glass substrate of ZnO film;
Substrate after the above-mentioned sputter is transferred in the phase depositing reaction chamber, reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:100, the control microwave power is 650W, the thick ZnO film of deposition preparation 20nm again, deposition is cleaned vapor deposition reaction with high pure nitrogen after finishing, and takes out substrate;
In 100 ℃ of high temperature annealings, obtaining structure is the photoelectricity transparent conductive film of ZnO/Al/ZnO to above-mentioned substrate.
To its in visible-range transmittance and test, as shown in Figure 2, can find out its transmittance more than 80%, its SEM figure as shown in Figure 3, Al particle and ZnO particle uniform doping are conducive to strengthen its electric property as can be seen from Figure 3.
After glass substrate used acetone, ethanol and deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into phase depositing reaction chamber;
Reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:100, the control microwave power is 650W, the thick ZnO film of deposition preparation 30nm, deposition is cleaned phase depositing reaction chamber with high pure nitrogen after finishing, and takes out substrate;
The substrate that deposits ZnO film is placed magnetron sputtering chamber, the magnetron sputtering chamber vacuum is evacuated to 10
-4Behind the Pa, heated substrate to 100 ℃, passing into argon gas control air pressure is 8Pa, carries out magnetron sputtering take pure Al as target, and sputtering power is 100W, and sputtering time is 2min, is depositing the Al film that sputter 10nm is thick on the glass substrate of ZnO film;
Substrate after the above-mentioned sputter is transferred in the phase depositing reaction chamber, reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:110, the control microwave power is 650W, the thick ZnO film of deposition preparation 30nm again, deposition is cleaned vapor deposition reaction with high pure nitrogen after finishing, and takes out substrate;
In 200 ℃ of high temperature annealings, obtaining structure is the photoelectricity transparent conductive film of ZnO/Al/ZnO to above-mentioned substrate.
After glass substrate used acetone, ethanol and deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into phase depositing reaction chamber;
Reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:120, the control microwave power is 60W, the thick ZnO film of deposition preparation 40nm, deposition is cleaned phase depositing reaction chamber with high pure nitrogen after finishing, and takes out substrate;
The substrate that deposits ZnO film is placed magnetron sputtering chamber, the magnetron sputtering chamber vacuum is evacuated to 10
-4Behind the Pa, heated substrate to 100 ℃, passing into argon gas control air pressure is 8Pa, carries out magnetron sputtering take pure Al as target, and sputtering power is 100W, and sputtering time is 3min, is depositing the Al film that sputter 20nm is thick on the glass substrate of ZnO film;
Substrate after the above-mentioned sputter is transferred in the phase depositing reaction chamber, reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:140, the control microwave power is 650W, the thick ZnO film of deposition preparation 40nm again, deposition is cleaned vapor deposition reaction with high pure nitrogen after finishing, and takes out substrate;
In 300 ℃ of high temperature annealing 30min, obtaining structure is the photoelectricity transparent conductive film of ZnO/Al/ZnO to above-mentioned substrate.
Embodiment 4
After glass substrate used acetone, ethanol and deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into phase depositing reaction chamber;
Reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:120, the control microwave power is 650W, the thick ZnO film of deposition preparation 50nm, deposition is cleaned phase depositing reaction chamber with high pure nitrogen after finishing, and takes out substrate;
The substrate that deposits ZnO film is placed magnetron sputtering chamber, the magnetron sputtering chamber vacuum is evacuated to 10
-4Behind the Pa, heated substrate to 100 ℃, passing into argon gas control air pressure is 8Pa, carries out magnetron sputtering take pure Al as target, and sputtering power is 100W, and sputtering time is 4min, is depositing the Al film that sputter 30nm is thick on the glass substrate of ZnO film;
Substrate after the above-mentioned sputter is transferred in the phase depositing reaction chamber, reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:150, the control microwave power is 650W, the thick ZnO film of deposition preparation 50nm again, deposition is cleaned vapor deposition reaction with high pure nitrogen after finishing, and takes out substrate;
In 400 ℃ of high temperature annealing 30min, obtaining structure is the photoelectricity transparent conductive film of ZnO/Al/ZnO to above-mentioned substrate.
Embodiment 5
After glass substrate used acetone, ethanol and deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into phase depositing reaction chamber;
Reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:150, the control microwave power is 650W, the thick ZnO film of deposition preparation 20nm, deposition is cleaned phase depositing reaction chamber with high pure nitrogen after finishing, and takes out substrate;
The substrate that deposits ZnO film is placed magnetron sputtering chamber, the magnetron sputtering chamber vacuum is evacuated to 10
-4Behind the Pa, heated substrate to 100 ℃, passing into argon gas control air pressure is 8Pa, carries out magnetron sputtering take pure Al as target, and sputtering power is 100W, and sputtering time is 5min, is depositing the Al film that sputter 20nm is thick on the glass substrate of ZnO film;
Substrate after the above-mentioned sputter is transferred in the phase depositing reaction chamber, reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:120, the control microwave power is 650W, the thick ZnO film of deposition preparation 30nm again, deposition is cleaned vapor deposition reaction with high pure nitrogen after finishing, and takes out substrate;
In 250 ℃ of high temperature annealing 30min, obtaining structure is the photoelectricity transparent conductive film of ZnO/Al/ZnO to above-mentioned substrate.
Claims (1)
1. the deposition preparation of a ZnO/Al/ZnO photoelectricity transparent conductive film is characterized in that carrying out according to following steps:
(1) glass substrate is used acetone, ethanol and deionized water ultrasonic cleaning successively after, dry up with nitrogen and to send into phase depositing reaction chamber, reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:(100-150), the control microwave power is 650W, the thick ZnO film of deposition preparation 20-50nm, deposition is cleaned phase depositing reaction chamber with high pure nitrogen after finishing, and takes out substrate;
The substrate that (2) will deposit ZnO film places magnetron sputtering chamber, and the magnetron sputtering chamber vacuum is evacuated to 10
-4Behind the Pa, heated substrate to 100 ℃, passing into argon gas control air pressure is 8Pa, carries out magnetron sputtering take pure Al as target, and sputtering power is 100W, and sputtering time is 1-5min, is depositing the Al film that sputter 5-30nm is thick on the glass substrate of ZnO film;
(3) substrate after the above-mentioned sputter is transferred in the phase depositing reaction chamber, reaction chamber is evacuated to 7.0 * 10
-4Behind the Pa, with substrate heating to 400 ℃, pass into simultaneously in the reaction chamber and carry Zn (CH
2CH
3)
2Argon gas and oxygen, wherein the throughput ratio of argon gas and oxygen is 1:(100-150), the control microwave power is 650W, the thick ZnO film of deposition preparation 20-50nm again, deposition is cleaned vapor deposition reaction with high pure nitrogen after finishing, and takes out substrate;
(4) to above-mentioned substrate in 100-400 ℃ of high temperature annealing 30min, obtaining structure is the photoelectricity transparent conductive film of ZnO/Al/ZnO.
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|---|---|---|---|
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|---|---|---|---|
| CN201210576026.1A CN103031556B (en) | 2012-12-27 | 2012-12-27 | A kind of deposition preparation of ZnO/Al/ZnO photoelectricity transparent conductive film |
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| CN103031556B CN103031556B (en) | 2015-07-29 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103337562A (en) * | 2013-07-12 | 2013-10-02 | 南开大学 | Wide-spectrum, high-transparency, high-down-degree and low-resistance transparent conductive film and preparation method of conductive film |
| CN104894520A (en) * | 2015-05-06 | 2015-09-09 | 大连理工大学 | Metal Mg-based UVC wave band transparent conducting structure and preparation method thereof |
| CN105734512A (en) * | 2016-03-16 | 2016-07-06 | 上海理工大学 | Preparation method of ZnO/Mo/ZnO transparent electric conducting film |
| CN106637204A (en) * | 2016-12-01 | 2017-05-10 | 梁结平 | Depositing method for Ag/ZnO/Mg photoelectric transparent conducting thin film |
| CN108165948A (en) * | 2018-02-09 | 2018-06-15 | 旭科新能源股份有限公司 | A kind of online real-time monitoring device and method for magnetron sputtering method production transparent conductive film |
-
2012
- 2012-12-27 CN CN201210576026.1A patent/CN103031556B/en active Active
Non-Patent Citations (3)
| Title |
|---|
| HUANG. CW.,ET AL.: "Characteristics of ZnO/Al/ZnO multilayers on glass with different ZnO film thickness prepared by cathodic vacuum arc deposition", 《2012 19TH INTERNATIONAL WORKSHOP ON ACTIVE-MATRIX FLATPANEL DISPLAYS AND DEVICES(AM-FPD)-TFT TECHNOLOGIES AND FPD MATERIALS》 * |
| M.A. AL-MAGHRABI,ET AL.: "influence of vacuum annealing on the physical properties of ZnO/Al/ZnO multilayer coatings", 《JOURNAL OF VACUUM SCIENCE & TECHNOLOGY A》 * |
| S.Y. CHOI,ET AL.: "Electrical and optical properties of ZnO films deposited by ECR-PECVD", 《PHYS. STAT. SOL. (A)》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103337562A (en) * | 2013-07-12 | 2013-10-02 | 南开大学 | Wide-spectrum, high-transparency, high-down-degree and low-resistance transparent conductive film and preparation method of conductive film |
| CN104894520A (en) * | 2015-05-06 | 2015-09-09 | 大连理工大学 | Metal Mg-based UVC wave band transparent conducting structure and preparation method thereof |
| CN105734512A (en) * | 2016-03-16 | 2016-07-06 | 上海理工大学 | Preparation method of ZnO/Mo/ZnO transparent electric conducting film |
| CN106637204A (en) * | 2016-12-01 | 2017-05-10 | 梁结平 | Depositing method for Ag/ZnO/Mg photoelectric transparent conducting thin film |
| CN108165948A (en) * | 2018-02-09 | 2018-06-15 | 旭科新能源股份有限公司 | A kind of online real-time monitoring device and method for magnetron sputtering method production transparent conductive film |
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|---|---|
| CN103031556B (en) | 2015-07-29 |
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