CN108950501A - A kind of preparation method of high light transmission ZAO conductive film - Google Patents
A kind of preparation method of high light transmission ZAO conductive film Download PDFInfo
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- CN108950501A CN108950501A CN201810773755.3A CN201810773755A CN108950501A CN 108950501 A CN108950501 A CN 108950501A CN 201810773755 A CN201810773755 A CN 201810773755A CN 108950501 A CN108950501 A CN 108950501A
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- zao
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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
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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
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacturing Of Electric Cables (AREA)
- Non-Insulated Conductors (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of preparation methods of ZAO transparent conductive film, using homemade additional Al2O3The ZAO target that mass percentage content is 2%.It reuses rf magnetron sputtering and prepares ZAO film on a glass substrate, using argon gas as sputter gas, ontology vacuum degree is 2~4 × 10‑4Pa, 0.4~0.9pa of sputtering pressure, sputtering power are 80~120W, and sputtering time is 45~60min, and substrate temperature is 80~120 DEG C, and after ZAO film deposition, anneal 2~3h at 200~400 DEG C.The present invention solves the problems, such as that ZAO film photoelectric performance is not easy to meet simultaneously, the ZAO film for preparing the smooth well-crystallized in surface, in visible-range (400~760nm), average transmittance is 80% or more, and ZAO film conductivity is high, has a good application prospect.
Description
Technical field
The present invention relates to transparent conductive film, in particular to photoelectric properties are good mixes for a kind of magnetron sputtering method preparation
The method of aluminum zinc oxide (ZAO) film.
Background technique
Conductive transparent oxide film is widely used in various photoelectric devices.Compared with the transparent ITO being widely used at present
Conductive film, ZnO film it is resourceful, it is cheap, have more extensive application prospect.Studies have shown that ZnO film can
For various photoelectric devices, such as LED, laser diode, photodetector, Field Emission Display, sensor and integrate non-linear
Optical device etc..One important application of ZnO film is exactly to be used for flat panel display device, it is desirable that its smooth surface has good
Translucency and high conductivity, but the photoelectric properties of usually prepared ZnO film are not easy to meet simultaneously.
The present invention uses homemade aluminium (Al) doping zinc-oxide (ZnO) target, using rf magnetron sputtering in glass substrate
Upper preparation ZAO film.Herein, by carrying out mixing Al to ZnO transparent photoelectric material, while keeping its high light transmittance, with
Improve its electric conductivity.
Summary of the invention
The purpose of the present invention is that the photoelectric properties of the prior art is overcome to be not easy the shortcomings that meeting simultaneously, using homemade ZAO
The method that target uses rf magnetron sputtering on a glass substrate prepares ZAO film, makes it while keeping high light transmittance, also mentions
Its high electric conductivity.
The present invention is achieved by following technical solution.
ZAO target and its transparent conductive film the preparation method is as follows:
(1) prepared by ZAO target
Using ZnO and Al2O3For raw material, on the basis of ZnO, Al that additional mass percent content is 2%2O3, according to
Prepared by conventional fabrication process: proportion weighing → ball mill mixing → plus adhesive granulation → dry-pressing formed → isostatic cool pressing → base
Body sintering → mechanical grinding；
(2) ZAO transparent conductive film is prepared using radio-frequency magnetron sputter method
In rf magnetron sputtering equipment, using the ZAO target of step (1) preparation as cathodic sputtering target, it is put into magnetic
Control sputter chamber；Using glass as substrate base, using dehydrated alcohol, using ultrasonic cleaning substrate 25 minutes, and using infrared
Drying equipment is put into magnetron sputtering cavity after being dried, target is 40mm at a distance from substrate；Ontology vacuum degree is taken out
To 2~4 × 10-4Pa is slowly filled with argon gas as sputter gas.Design parameter are as follows: in sputtering process the pressure of argon gas be 0.4~
0.9pa, sputtering power are 80~120W, and sputtering time is 45~60min, heat substrate to 80~120 DEG C；
After ZAO film deposition, anneal 2~3h at 200~400 DEG C.
The purity of step (1) raw material is all larger than 99%.
The purity of argon of the step (2) is 99% or more.
The present invention prepares ZAO film using the method that homemade ZAO target uses rf magnetron sputtering on a glass substrate.This
The film surface that method is prepared is smooth, advantages of good crystallization, ZAO film (400~760nm), average transmittance in visible-range
Rate is 80% or more, and ZAO film conductivity is high.It can satisfy the requirement of most of electronic device, be applied to flat-panel screens
There is biggish advantage when part, has a good application prospect.
Detailed description of the invention
Fig. 1 is the surface topography map for the ZAO Films Example 1 that in the present invention prepared by radio-frequency magnetron sputter method；
Fig. 2 is the XRD and light transmission spectrogram for the ZAO Films Example 1 that in the present invention prepared by radio-frequency magnetron sputter method.
Specific embodiment
The preparation of ZAO target:
Selecting purity is 99% ZnO and Al2O3Powder is 49:1 as raw material, the two mass ratio, uses planetary ball mill
Ball mill mixing 10h is carried out, 7wt% paraffin is added and makees binder granulation, it is dry-pressing formed under the pressure of 35Mpa, in the pressure of 1500N
Isostatic cool pressing in power, obtained green body are heated up between 500 DEG C using the low speed of 50 DEG C/h in room temperature, and in 500 DEG C of heat preservation 3h,
Abundant de-waxing is warming up to 1200 DEG C later with the speed of 100 DEG C/h, and keeps the temperature 4h, and Temperature fall is to room temperature after sintering, most
After carry out mechanical grinding, prepare Al2O3The ZAO target that doping is 2%.
ZAO film preparation:
In rf magnetron sputtering equipment, using the ZAO target of step (1) preparation as cathodic sputtering target, it is put into magnetic
Control sputter chamber.Using glass as substrate base, using dehydrated alcohol, using ultrasonic cleaning substrate 25 minutes, and using infrared
Drying equipment is put into magnetron sputtering cavity after being dried, target is 40mm at a distance from substrate.Ontology vacuum degree is taken out
To 2~4 × 10-4Pa is slowly filled with argon gas as sputter gas.Design parameter are as follows: in sputtering process the pressure of argon gas be 0.4~
0.9pa, sputtering power are 80~120W, and sputtering time is 45~60min, heat substrate to 80~120 DEG C.
After ZAO film deposition, anneal 2~3h at 200~400 DEG C.
See Table 1 for details for the main preparation parameter of ZAO film and electrically conducting transparent performance.
Table 1
Table 1 the experimental results showed that, prepared ZAO film (400~760nm), average transmittance in visible-range
80% or more；And the sheet resistance of prepared ZAO film is low, and this shows its electric conductivity height.
Selection example 1 is used as representative sample, further analyze prepared film surface appearance, crystallization situation and
Film light transmission situation in visible-range, as illustrated in fig. 1 and 2.Fig. 1 SEM shows that prepared ZAO film surface is smooth, flat
It is whole, reach the requirement of manufacture flat-panel screens.ZAO film XRD main diffraction peak is stronger in Fig. 2 illustration, shows prepared film
Crystallization is good, this is advantageous to film heat stability；Compared with pure ZnO XRD standard card (JCPDSNo.65-2880), diffraction maximum
Significant change does not occur for position, this shows that a small amount of Al doping will not make the crystal structure of ZnO that big variation occur, thus will not be right
Its translucency causes big influence, and the transparent test of Fig. 2 and 1 average transmittance of table demonstrate this point.If film preparation
Technological parameter changes, and the electric conductivity and light transmission of prepared film can be slightly changed relative to embodiment, can basis
To the requirement of electric conductivity and light transmission in, suitable preparation technology parameter is selected.
To sum up, ZAO film prepared in the present invention is smooth, advantages of good crystallization, light transmittance are high and good conductivity, can satisfy big
The requirement of some electronic devices has biggish advantage when applied to flat panel display device, have good prospect.
Claims (3)
1. a kind of preparation method of high light transmission ZAO conductive film has following steps:
(1) prepared by ZAO target
Using ZnO and Al2O3For raw material, on the basis of ZnO, Al that additional mass percent content is 2%2O3, according to routine
Prepared by preparation process: proportion weighing → ball mill mixing → plus adhesive granulation → dry-pressing formed → isostatic cool pressing → green body are burnt
Knot → mechanical grinding.
(2) ZAO transparent conductive film is prepared using radio-frequency magnetron sputter method
In rf magnetron sputtering equipment, using the ZAO target of step (1) preparation as cathodic sputtering target, it is put into magnetic control and splashes
Penetrate cavity；Using glass as substrate base, using dehydrated alcohol, using ultrasonic cleaning substrate 25 minutes, and infra-red drying is used
Equipment is put into magnetron sputtering cavity after being dried, target is 40mm at a distance from substrate；Ontology vacuum degree is evacuated to 2~
4×10-4Pa is slowly filled with argon gas as sputter gas；Design parameter are as follows: in sputtering process the pressure of argon gas be 0.4~
0.9pa, sputtering power are 80~120W, and sputtering time is 45~60min, heat substrate to 80~120 DEG C；
After ZAO film deposition, anneal 2~3h at 200~400 DEG C.
2. a kind of preparation method of high light transmission ZAO conductive film according to claim 1, which is characterized in that the step
(1) purity of raw material is all larger than 99%.
3. a kind of preparation method of high light transmission ZAO conductive film according to claim 1, which is characterized in that the step
(2) purity of argon is 99% or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810773755.3A CN108950501A (en) | 2018-07-15 | 2018-07-15 | A kind of preparation method of high light transmission ZAO conductive film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810773755.3A CN108950501A (en) | 2018-07-15 | 2018-07-15 | A kind of preparation method of high light transmission ZAO conductive film |
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| CN108950501A true CN108950501A (en) | 2018-12-07 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050029088A1 (en) * | 2003-08-06 | 2005-02-10 | Energy Photovoltaics, Inc. | Hollow cathode sputtering apparatus and related method |
| CN101221935A (en) * | 2007-01-10 | 2008-07-16 | 日东电工株式会社 | Transparent conductive film and method for producing the same |
| DE102009060547A1 (en) * | 2009-12-23 | 2011-06-30 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V., 80686 | Process for coating a substrate with aluminum-doped zinc oxide |
| CN102260852A (en) * | 2011-06-14 | 2011-11-30 | 中国科学院电工研究所 | Preparation method of AZO membrane with weaving structure |
| CN103643211A (en) * | 2013-11-21 | 2014-03-19 | 山东希格斯新能源有限责任公司 | Novel AZO thin film preparation deposition process |
-
2018
- 2018-07-15 CN CN201810773755.3A patent/CN108950501A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050029088A1 (en) * | 2003-08-06 | 2005-02-10 | Energy Photovoltaics, Inc. | Hollow cathode sputtering apparatus and related method |
| CN101221935A (en) * | 2007-01-10 | 2008-07-16 | 日东电工株式会社 | Transparent conductive film and method for producing the same |
| DE102009060547A1 (en) * | 2009-12-23 | 2011-06-30 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V., 80686 | Process for coating a substrate with aluminum-doped zinc oxide |
| CN102260852A (en) * | 2011-06-14 | 2011-11-30 | 中国科学院电工研究所 | Preparation method of AZO membrane with weaving structure |
| CN103643211A (en) * | 2013-11-21 | 2014-03-19 | 山东希格斯新能源有限责任公司 | Novel AZO thin film preparation deposition process |
Non-Patent Citations (1)
| Title |
|---|
| WEI SHAO: "Fabrication and properties of ZAO powder, sputtering target materials and the related films", 《JOURNAL OF UNIVERSITY OF SCIENCE AND TECHNOLOGY BEIJING》 * |
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Application publication date: 20181207 |