CN105839064A - Preparation method of amorphous indium tin oxide thin film - Google Patents
Preparation method of amorphous indium tin oxide thin film Download PDFInfo
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- CN105839064A CN105839064A CN201610242203.0A CN201610242203A CN105839064A CN 105839064 A CN105839064 A CN 105839064A CN 201610242203 A CN201610242203 A CN 201610242203A CN 105839064 A CN105839064 A CN 105839064A
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- indium tin
- thin film
- preparation
- tin oxide
- amorphous oxide
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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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a preparation method of an amorphous indium tin oxide thin film. The preparation method includes the following steps that a substrate is provided; and the substrate is arranged in a cavity of a magnetron sputtering device, and the amorphous indium tin oxide thin film is deposited on the substrate in a magnetron sputtering manner under the vacuum condition by using argon-hydrogen mixed gas with the volume percentage of hydrogen ranging from 1% to 3% as process gas, using indium tin oxide as a target material and controlling the temperature of the substrate to range from 50 DEG C to 100 DEG C. According to the preparation method of the amorphous indium tin oxide thin film, the indium tin oxide target material (the mass ratio of indium oxide ranges from 85% to 93%) used for a conventional crystallization indium tin oxide film is adopted, the argon-hydrogen mixed gas with the volume percentage of hydrogen ranging from 1% to 3% is used as the process gas in the indium tin oxide coating process, hydrogen has good dispersibility and thereby being beneficial to uniform distribution, no expensive checkout equipment needs to be added for monitoring the water partial pressure, and the prepared amorphous indium tin oxide thin film has good stability.
Description
Technical field
The present invention relates to field of vacuum coating, particularly relate to the preparation method of a kind of amorphous oxide indium tin thin film.
Background technology
Tin indium oxide (tin indium oxide) thin film is as the most frequently used transparent conductive film, in Transparence Display field
Have a wide range of applications.Crystallization indium tin oxide films is it is generally required at high temperature prepare (> 200 DEG C), it is follow-up
Pattern processing generally require chloroazotic acid and could etch.But crystallization indium oxide tin film etching needs strong acid, its technique
Controlling difficulty big, etching process easily damages other film layer or product component, environmental pollution simultaneously and to production
The infringement of line is bigger.
Amorphous oxide indium tin thin film has that depositing temperature is low, easily etches, and etching process is low to the damage of product,
Obvious advantage is had at a lot of aspects.But under low temperature, the amorphous oxide indium stannum of preparation is the most unstable, a side
Face square resistance is unstable, the most easily causes follow-up cannot etching from crystallization.
Easily crystallize for tin indium oxide and resistance instability problem, can pass through in tin indium oxide deposition process,
It is passed through the crystallization of a certain proportion of steam inhibited oxidation indium stannum.But by tin indium oxide deposition process
It is passed through that the method for a certain proportion of steam then there is problems in that 1, steam is difficult to uniformly point in vacuum chamber
Dissipate thus cause indium tin oxide films quality of forming film uneven；2, water partial pressure needs accurately to control, and it controls
Need the problems such as expensive monitoring device, additionally its indium tin oxide films prepared in weatherability is tested still
A small amount of crystallisation problems, thus affect following process and use.
Summary of the invention
Based on this, it is necessary to provide a kind of Indium sesquioxide. that can be prepared as the uniform indium tin oxide films of film quality
The preparation method of tin thin film.
The preparation method of a kind of amorphous oxide indium tin thin film, comprises the steps:
Substrate is provided；And
Described substrate is placed in magnetron sputtering apparatus cavity, under vacuum, with the volume basis of hydrogen
Content be the argon hydrogen mixture of 1%～3% be process gas, with tin indium oxide as target, control described substrate
Temperature be-50 DEG C～100 DEG C, magnetron sputtering deposition amorphous oxide indium tin thin film over the substrate.
In one embodiment, the material of described substrate is glass, aluminium oxide, polyethylene terephthalate
Or polyimides.
In one embodiment, the vacuum of described vacuum condition is 1 × 10-6Pa～2 × 10-4Pa。
In one embodiment, the vacuum of described vacuum condition is 9 × 10-5Pa。
In one embodiment, described process gas is the argon hydrogen that volumn concentration is 2.2% mixing of hydrogen
Gas.
In one embodiment, the material of described target is the oxidation that mass content is 85%～93% of Indium sesquioxide.
Indium stannum.
In one embodiment, the material of described target is the tin indium oxide that mass content is 90% of Indium sesquioxide..
In one embodiment, in magnetron sputtering process, described substrate temperature is room temperature.
The preparation method of this amorphous oxide indium tin thin film, uses the oxidation used by conventional crystallization indium oxide tin film
Indium stannum target (Indium sesquioxide. mass ratio is 85%～93%), with the volume of hydrogen during indium oxide coating
Percentage composition be the argon hydrogen mixture of 1%～3% be process gas, hydrogen has good dispersibility thus sharp
In being uniformly distributed, the detection monitoring of tools water partial pressure of costliness, prepared amorphous oxide indium tin thin film need not be increased
Excellent stability.Relative to the preparation method of traditional amorphous oxide indium tin thin film, this amorphous oxide indium
The quality of forming film of the amorphous oxide indium tin thin film that the preparation method of tin thin film prepares is uniform.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of the amorphous oxide indium tin thin film of an embodiment.
Detailed description of the invention
Below mainly in combination with drawings and the specific embodiments amorphous oxide indium tin thin film preparation method, use this non-
Super capacitor electrode slice of preparation method of brilliant indium tin oxide films and preparation method thereof is made further details of
Explanation.
The preparation method of the amorphous oxide indium tin thin film of an embodiment as shown in Figure 1, comprises the steps:
S10, offer substrate.
The material of substrate is glass, aluminium oxide, polyethylene terephthalate (PET) or polyimides (PI).
S20, the substrate obtained by S10 are placed in magnetron sputtering apparatus cavity, under vacuum, with hydrogen
The argon hydrogen mixture that volumn concentration is 1%～3% be process gas, with tin indium oxide as target, control
Substrate temperature processed is-50 DEG C～100 DEG C, magnetron sputtering deposition amorphous oxide indium tin thin film on substrate.
The vacuum of vacuum condition can be 1 × 10-6Pa～2 × 10-4Pa.Preferably, the vacuum of vacuum condition
It is 9 × 10-5Pa。
Preferably, process gas is the argon hydrogen mixture that volumn concentration is 2.2% of hydrogen.
Target can select general tin indium oxide target material.Concrete, the material of target can be the matter of Indium sesquioxide.
Amount content is the tin indium oxide of 85%～93%.
Preferably, the material of target is the tin indium oxide that mass content is 90% of Indium sesquioxide..
Preferably, in magnetron sputtering process, substrate temperature is room temperature.
The preparation method of this amorphous oxide indium tin thin film, uses the oxidation used by conventional crystallization indium oxide tin film
Indium stannum target (Indium sesquioxide. mass ratio is 85%～93%), with the volume of hydrogen during indium oxide coating
Percentage composition be the argon hydrogen mixture of 1%～3% be process gas, hydrogen has good dispersibility thus sharp
In being uniformly distributed, the detection monitoring of tools water partial pressure of costliness, prepared amorphous oxide indium tin thin film need not be increased
Excellent stability.Relative to the preparation method of traditional amorphous oxide indium tin thin film, this amorphous oxide indium
The quality of forming film of the amorphous oxide indium tin thin film that the preparation method of tin thin film prepares is uniform.
It it is below specific embodiment.
Embodiment 1
PET substrate is provided.
PET substrate is placed in magnetron sputtering apparatus cavity, is 9 × 10 in vacuum-5Under the vacuum condition of Pa,
With the argon hydrogen mixture that volumn concentration is 2.2% of hydrogen as process gas, contain with the quality of Indium sesquioxide.
Amount be the tin indium oxide of 90% be target, control PET substrate temperature be room temperature, magnetic control on PET substrate
Sputtering sedimentation amorphous oxide indium tin thin film.
Embodiment 2
Glass substrate is provided.
Glass substrate is placed in magnetron sputtering apparatus cavity, is 1 × 10 in vacuum-6Under the vacuum condition of Pa,
With the argon hydrogen mixture that volumn concentration is 3% of hydrogen as process gas, with the mass content of Indium sesquioxide.
Be 85% tin indium oxide be target, control glass substrate temperature be 100 DEG C, magnetic control spatters on a glass substrate
Penetrate deposited amorphous indium tin oxide films.
Embodiment 3
Alumina substrate is provided.
Alumina substrate is placed in magnetron sputtering apparatus cavity, is 2 × 10 in vacuum-4The vacuum condition of Pa
Under, with the argon hydrogen mixture that volumn concentration is 2% of hydrogen as process gas, with the quality of Indium sesquioxide.
Content be the tin indium oxide of 93% be target, control alumina substrate temperature be-50 DEG C, in alumina substrate
Upper magnetron sputtering deposition amorphous oxide indium tin thin film.
Test case
The amorphous oxide indium tin thin film prepared embodiment 1～3 respectively is at hot and humid (60 DEG C, 90% humidity)
Under conditions of process 240h, then can the test X-ray peak crystallization of amorphous oxide indium tin thin film, oxalic acid lose
Carve and square resistance, obtain table 1.
Table 1: the amorphous oxide indium tin thin film test data that embodiment 1～3 prepares
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| X-ray peak crystallization | Nothing | Nothing | Nothing |
| Can oxalic acid etch | It is | It is | It is |
| Square resistance | 155 Europe | 165 Europe | 163 Europe |
The amorphous oxide indium tin thin film prepared embodiment 1～3 respectively processes 60min at 120 DEG C, then surveys
Can the examination X-ray peak crystallization of amorphous oxide indium tin thin film, oxalic acid etch and square resistance, obtain table 2.
Table 2: the amorphous oxide indium tin thin film test data that embodiment 1～3 prepares
The amorphous oxide indium tin thin film prepared embodiment 1～3 respectively processes 60min at 150 DEG C, then surveys
Can the examination X-ray peak crystallization of amorphous oxide indium tin thin film, oxalic acid etch and square resistance, obtain table 3.
Table 3: the amorphous oxide indium tin thin film test data that embodiment 1～3 prepares
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| X-ray peak crystallization | Nothing | Nothing | Nothing |
| Can oxalic acid etch | It is | It is | It is |
| Square resistance | 151 Europe | 160 Europe | 158 Europe |
In conjunction with table 1～table 3, it can be seen that the amorphous oxide indium tin thin film that embodiment 1～3 prepares all does not contains
There are Indium sesquioxide. tin crystals, workable (can be corroded by oxalic acid), and there is relatively low square resistance.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed,
But therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that, for this area
Those of ordinary skill for, without departing from the inventive concept of the premise, it is also possible to make some deformation and
Improving, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be with appended
Claim is as the criterion.
Claims (8)
1. the preparation method of an amorphous oxide indium tin thin film, it is characterised in that comprise the steps:
Substrate is provided；And
Described substrate is placed in magnetron sputtering apparatus cavity, under vacuum, with the volume basis of hydrogen
Content be the argon hydrogen mixture of 1%～3% be process gas, with tin indium oxide as target, control described substrate
Temperature be-50 DEG C～100 DEG C, magnetron sputtering deposition amorphous oxide indium tin thin film over the substrate.
The preparation method of amorphous oxide indium tin thin film the most according to claim 1, it is characterised in that institute
The material stating substrate is glass, aluminium oxide, polyethylene terephthalate or polyimides.
The preparation method of amorphous oxide indium tin thin film the most according to claim 1, it is characterised in that institute
The vacuum stating vacuum condition is 1 × 10-6Pa～2 × 10-4Pa。
The preparation method of amorphous oxide indium tin thin film the most according to claim 1, it is characterised in that institute
The vacuum stating vacuum condition is 9 × 10-5Pa。
The preparation method of amorphous oxide indium tin thin film the most according to claim 1, it is characterised in that institute
State the argon hydrogen mixture that volumn concentration is 2.2% that process gas is hydrogen.
The preparation method of amorphous oxide indium tin thin film the most according to claim 1, it is characterised in that institute
State the tin indium oxide that the mass content that material is Indium sesquioxide. is 85%～93% of target.
The preparation method of amorphous oxide indium tin thin film the most according to claim 6, it is characterised in that institute
State the tin indium oxide that the mass content that material is Indium sesquioxide. is 90% of target.
The preparation method of amorphous oxide indium tin thin film the most according to claim 1, it is characterised in that magnetic
In control sputter procedure, described substrate temperature is room temperature.
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| CN201610242203.0A CN105839064A (en) | 2016-04-19 | 2016-04-19 | Preparation method of amorphous indium tin oxide thin film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106571174A (en) * | 2016-11-09 | 2017-04-19 | 宜昌南玻显示器件有限公司 | Transparent conductive film preparation method and transparent conductive film |
| CN108183137A (en) * | 2017-12-28 | 2018-06-19 | 中国科学院电工研究所 | Composite conducting antireflective film for silicon/crystalline silicon heterojunction solar cell and preparation method thereof |
| CN108385073A (en) * | 2018-04-24 | 2018-08-10 | 信利（惠州）智能显示有限公司 | The production method of ito thin film |
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| US20060144695A1 (en) * | 2005-01-03 | 2006-07-06 | Yu-Chou Lee | Sputtering process for depositing indium tin oxide and method for forming indium tin oxide layer |
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| TWI242053B (en) * | 2002-03-01 | 2005-10-21 | Ind Tech Res Inst | Low temperature method for producing ultra-planar indium tin oxide (ITO) |
| US20060144695A1 (en) * | 2005-01-03 | 2006-07-06 | Yu-Chou Lee | Sputtering process for depositing indium tin oxide and method for forming indium tin oxide layer |
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Non-Patent Citations (1)
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106571174A (en) * | 2016-11-09 | 2017-04-19 | 宜昌南玻显示器件有限公司 | Transparent conductive film preparation method and transparent conductive film |
| CN106571174B (en) * | 2016-11-09 | 2018-07-10 | 宜昌南玻显示器件有限公司 | The preparation method and transparent conductive film of transparent conductive film |
| CN108183137A (en) * | 2017-12-28 | 2018-06-19 | 中国科学院电工研究所 | Composite conducting antireflective film for silicon/crystalline silicon heterojunction solar cell and preparation method thereof |
| CN108183137B (en) * | 2017-12-28 | 2019-10-15 | 中国科学院电工研究所 | Composite conducting antireflective film and preparation method thereof for silicon/crystalline silicon heterojunction solar cell |
| CN108385073A (en) * | 2018-04-24 | 2018-08-10 | 信利（惠州）智能显示有限公司 | The production method of ito thin film |
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Application publication date: 20160810 |