CN111575666B - Method for preparing (222) strong texture ITO film - Google Patents
Method for preparing (222) strong texture ITO film Download PDFInfo
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- CN111575666B CN111575666B CN202010523344.6A CN202010523344A CN111575666B CN 111575666 B CN111575666 B CN 111575666B CN 202010523344 A CN202010523344 A CN 202010523344A CN 111575666 B CN111575666 B CN 111575666B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/541—Heating or cooling of the substrates
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Abstract
The invention discloses a method for preparing (222) a strong texture ITO film, which comprises the following steps: (1) cleaning a silicon substrate and installing the silicon substrate in a cavity of magnetron sputtering equipment; (2) placing a target material in a cavity of a magnetron sputtering device, and adjusting the distance between the target material and a silicon substrate; (3) carrying out vacuum pumping treatment on the chamber; (4) heating the silicon substrate; (5) introducing argon and oxygen into the chamber; (6) starting magnetron sputtering equipment to sputter the silicon substrate; (7) after the sputtering is finished, the ITO film with the crystal face (222) in the preferred orientation is obtained. The invention realizes the preparation of the ITO film with the crystal face of (222) in the highly preferred orientation on the common monocrystal Si (100) substrate, does not need to introduce a seed layer, is beneficial to the integration of the high-quality electronic ceramic film on Si, and has the characteristics of good crystallinity, simple and convenient process and easy industrialization.
Description
Technical Field
The invention belongs to the technical field of semiconductor conductive film preparation, and particularly relates to a method for preparing (222) a strong-texture ITO film.
Background
An ITO (indium tin oxide) thin film is a semiconductor material of great interest because of its excellent photoelectric properties, and can be used as a Transparent Conductive Oxide (TCO) material to obtain a material for a specific application by adjusting process parameters during deposition. Because of these characteristics, ITO films are useful for developing high performance photovoltaic and photovoltaic devices, and in order to use ITO thin films for photovoltaic applications, samples having reproducible characteristics are required.
The method for preparing the ITO film comprises the methods of chemical solution deposition, magnetron sputtering, pulse laser deposition and the like, among the preparation methods of the ITO film, the radio frequency magnetron sputtering is most widely applied, and has the characteristics of high efficiency, large-area uniform film formation and the like, but most of the ITO films prepared by the radio frequency magnetron sputtering at present are deposited on amorphous substrates such as glass and the like, and the ITO film with polycrystalline orientation or (400) preferred orientation is easily prepared on common monocrystalline silicon (100).
Disclosure of Invention
The invention aims to provide a method for preparing (222) a strong texture ITO film so as to realize the integration of a high-quality electronic ceramic film on Si.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method of making (222) a strongly textured ITO film, comprising the steps of:
(1) cleaning a silicon substrate and installing the silicon substrate in a cavity of magnetron sputtering equipment;
(2) placing a target material in a cavity of a magnetron sputtering device, and adjusting the distance between the target material and a silicon substrate;
(3) carrying out vacuum pumping treatment on the chamber;
(4) heating the silicon substrate;
(5) introducing argon and oxygen into the chamber;
(6) starting magnetron sputtering equipment to sputter the silicon substrate;
(7) after the sputtering is finished, the ITO film with the crystal face (222) in the preferred orientation is obtained.
Preferably, in the step (1), the silicon substrate cleaning specifically comprises the following steps: sequentially ultrasonically cleaning the glass substrate by acetone, absolute ethyl alcohol and deionized water for 15min, and blow-drying the glass substrate by high-purity nitrogen after cleaning treatment is finished.
Preferably, in the step (2), the distance between the target and the silicon substrate is adjusted to be 60 mm.
Preferably, in the step (3), the chamber is vacuumized to a vacuum degree lower than 2 × 10-4Pa。
Preferably, in the step (4), the heating temperature is 500 ℃.
Preferably, in the step (5), the flow ratio of argon to oxygen is 38: 2-30: 10.
preferably, in the step (5), after introducing argon and oxygen, the vacuum degree of the chamber is adjusted to 0.2Pa-0.9 Pa.
Preferably, in the step (6), the sputtering power is 80W, and the sputtering time is 10-20 min.
Has the advantages that: the invention realizes the preparation of the ITO film with the (222) high preferred orientation on the single crystal Si (100) by adjusting the proper magnetron sputtering process parameters, does not need to introduce an induction layer or subsequent annealing treatment, has the characteristics of simple process and easy realization of industrialization, and the prepared ITO film has the characteristics of high preferred orientation of the (222) crystal face and high crystallization quality, and is beneficial to the integration of the high-quality electronic ceramic film on Si.
Drawings
FIG. 1 is an XRD pattern of a highly preferentially oriented (222) ITO film deposited in example 1;
FIG. 2 is an XRD pattern of ITO thin films deposited under different argon-oxygen ratios in example 2;
FIG. 3 is an XRD pattern of ITO thin films deposited under different pressures in example 3;
FIG. 4 is an XRD pattern of ITO thin films deposited at different sputtering times in example 3.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
1) Cleaning a 10X 10mm Si substrate, wherein the specific process of the cleaning treatment is as follows: sequentially ultrasonically cleaning the glass substrate for 15min by acetone, absolute ethyl alcohol and deionized water, and blow-drying the glass substrate by high-purity nitrogen after cleaning treatment is finished;
2) placing the Si substrate in a cavity of magnetron sputtering equipment, and setting the distance between the target and the Si substrate to be 60 mm;
3) vacuumizing the chamber to make the vacuum degree of the chamber lower than 2 x 10-4Pa；
4) Heating the Si substrate at 500 ℃;
5) introducing argon and oxygen into the chamber, and adjusting the flow ratio to be 34: 6, regulating the vacuum degree of the chamber to be 0.5 Pa;
6) the sputtering power was set at 80W, and then the shutter plate was opened to sputter the substrate for 18 min.
Example 2
1) Cleaning a 10X 10mm Si substrate, wherein the specific process of the cleaning treatment is as follows: sequentially ultrasonically cleaning the glass substrate for 15min by using acetone, absolute ethyl alcohol and deionized water, and blow-drying the glass substrate by using high-purity nitrogen after cleaning treatment is finished;
2) placing the Si substrate in a cavity of magnetron sputtering equipment, and setting the distance between the target and the Si substrate to be 60 mm;
3) vacuumizing the chamber to make the vacuum degree of the chamber lower than 2 x 10-4Pa；
4) Heating the Si substrate at 500 ℃;
5) introducing argon and oxygen into the chamber, and adjusting the flow ratio to be 36: 4. 34: 6. 32: 8. 30: 10, and adjusting the vacuum degree of the chamber to be 0.5 Pa;
6) the sputtering power was set at 80W, and then the shutter plate was opened to sputter the substrate for 18 min.
Example 3
1) Cleaning a 10X 10mm Si substrate, wherein the specific process of the cleaning treatment is as follows: sequentially ultrasonically cleaning the glass substrate for 15min by using acetone, absolute ethyl alcohol and deionized water, and blow-drying the glass substrate by using high-purity nitrogen after cleaning treatment is finished;
2) placing the Si substrate in a cavity of magnetron sputtering equipment, and setting the distance between the target and the Si substrate to be 60 mm;
3) carrying out vacuum pumping treatment on the chamber to ensure that the vacuum degree of the chamber is lower than 2 x 10 < -4 > Pa;
4) heating the Si substrate at 500 ℃;
5) introducing argon and oxygen into the chamber, and adjusting the flow ratio to be 34: 6, regulating the vacuum degree of the chamber to be 0.3Pa, 0.5Pa and 0.8 Pa;
6) the sputtering power was set at 80W, and then the shutter plate was opened to sputter the substrate for 18 min.
Example 4
1) Cleaning a 10X 10mm Si substrate, wherein the specific process of the cleaning treatment is as follows: sequentially ultrasonically cleaning the glass substrate for 15min by using acetone, absolute ethyl alcohol and deionized water, and blow-drying the glass substrate by using high-purity nitrogen after cleaning treatment is finished;
2) placing the Si substrate in a cavity of magnetron sputtering equipment, and setting the distance between the target and the Si substrate to be 60 mm;
3) vacuumizing the chamber to make the vacuum degree of the chamber lower than 2 x 10-4Pa；
4) Heating the Si substrate at 500 ℃;
5) introducing argon and oxygen into the chamber, and adjusting the flow ratio to be 34: 6, regulating the vacuum degree of the chamber to be 0.5 Pa;
6) the sputtering power is set to be 80W, then the baffle is opened, and the substrate is sputtered for 12min, 15min and 18 min.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A method of making (222) a strongly textured ITO film, comprising: the method comprises the following steps:
(1) cleaning a silicon substrate and installing the silicon substrate in a cavity of magnetron sputtering equipment;
(2) placing a target material in a cavity of a magnetron sputtering device, and adjusting the distance between the target material and a silicon substrate;
(3) carrying out vacuum pumping treatment on the chamber;
(4) heating the silicon substrate;
(5) introducing argon and oxygen into the chamber;
(6) starting magnetron sputtering equipment, and sputtering the silicon substrate, wherein the sputtering power is 80W, and the sputtering time is 10-20 min;
(7) after the sputtering is finished, the ITO film with the crystal face (222) in the preferred orientation is obtained.
2. The method of making (222) a strongly textured ITO film of claim 1, wherein: in the step (1), the silicon substrate cleaning specifically comprises the following steps: sequentially ultrasonically cleaning the glass substrate by acetone, absolute ethyl alcohol and deionized water for 15min, and blow-drying the glass substrate by high-purity nitrogen after cleaning treatment is finished.
3. The method of making (222) a strongly textured ITO film of claim 1, wherein: in the step (2), the distance between the target and the silicon substrate is adjusted to be 60 mm.
4. The method of making (222) a strongly textured ITO film of claim 1, wherein: in the step (3), the chamber is vacuumized until the vacuum degree is lower than 2 x 10-4Pa。
5. The method of making (222) a strongly textured ITO film of claim 1, wherein: in the step (4), the heating temperature is 500 ℃.
6. The method of making (222) a strongly textured ITO film of claim 1, wherein: in the step (5), the flow ratio of argon to oxygen is 38: 2-30: 10.
7. the method of making (222) a strongly textured ITO film of claim 1, wherein: in the step (5), after argon and oxygen are introduced, the vacuum degree of the chamber is adjusted to be 0.2Pa-0.9 Pa.
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| CN202010523344.6A CN111575666B (en) | 2020-06-10 | 2020-06-10 | Method for preparing (222) strong texture ITO film |
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| CN202010523344.6A CN111575666B (en) | 2020-06-10 | 2020-06-10 | Method for preparing (222) strong texture ITO film |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000238178A (en) * | 1999-02-24 | 2000-09-05 | Teijin Ltd | Transparent conductive laminate |
| JPWO2004065656A1 (en) * | 2003-01-24 | 2006-05-18 | 株式会社ブリヂストン | ITO thin film, film forming method thereof, transparent conductive film, and touch panel |
| JP6261987B2 (en) * | 2013-01-16 | 2018-01-17 | 日東電工株式会社 | Transparent conductive film and method for producing the same |
| CN105714262A (en) * | 2016-05-05 | 2016-06-29 | 常州工学院 | Preparation method of preferred growing ITO transparent conductive film |
| CN108588657B (en) * | 2018-04-17 | 2020-03-17 | 西安交通大学 | Method for preparing ITO nanowire and gas sensor thereof by high radio frequency power sputtering |
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2020
- 2020-06-10 CN CN202010523344.6A patent/CN111575666B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| HIT太阳电池中ITO薄膜的结构和光电性能;任丙彦等;《太阳能学报》;20070528(第05期);第52-55页 * |
| 退火温度对室温沉积的ITO薄膜与p-Si接触性能的影响;吴斯泰等;《半导体光电》;20161028(第05期);第69-73、78页 * |
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