CN106637118A - Preparation method of aluminum-doped zinc oxide conductive thin film - Google Patents
Preparation method of aluminum-doped zinc oxide conductive thin film Download PDFInfo
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- CN106637118A CN106637118A CN201611226708.4A CN201611226708A CN106637118A CN 106637118 A CN106637118 A CN 106637118A CN 201611226708 A CN201611226708 A CN 201611226708A CN 106637118 A CN106637118 A CN 106637118A
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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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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a preparation method of an aluminum-doped zinc oxide conductive thin film. The preparation method has the advantages of being simple and easy to operate, low in requirements for equipment, simple in preparation and good in repeatability. After the preparation method is adopted, the crystal structure and the surface morphology are optimized, the photoelectric characteristic of the conductive thin film is improved, and the stability of the thin film is improved; therefore, the preparation method perfects the performance of the thin film, reduces the reaction temperature, improves the control accuracy, reduces preparation cost and adapts to mass production.
Description
Technical field
The present invention relates to conductive film field, and in particular to a kind of preparation method of Al-Doped ZnO conductive film.
Background technology
In recent years transparent conductive oxide film was always the focus of photoelectric field, wherein ito thin film be research at present and
Most widely used transparent conductive oxide (TCO) film, because of its good photoelectric characteristic various photoelectricity are widely used in
Device, but because the prices of raw materials are expensive, indium resource is rare and to environment, so as to limit its development and application.
According to initial estimate, the demand of TCO glass substrates will be more than 1,200,000,000 square metres in the year two thousand twenty world wide.It is existing
The wide variety of nesa coating of industrial circle mainly includes tin indium oxide (abbreviation ITO), zinc oxide aluminum (abbreviation AZO) and Fluorin doped
Tin oxide (abbreviation FTO) three major types.Wherein ITO is because a large amount of using expensive phosphide material so as to which application is extremely restricted.FTO
ITO levels close with the photoelectric properties of AZO systems, obtain certain applications in flat-panel monitor, but the preparation of FTO and AZO
During need to introduce high-temperature technology, working condition is required higher, therefore the extensive application to FTO and AZO causes limit
System.
Al-Doped ZnO (AZO) film not only has the photoelectric characteristic compared favourably with ITO, and with aboundresources, material
The advantage such as material is nontoxic, chemical stability is good, with low cost and wear-resistant in hydrogen plasma, therefore AZO films are considered
The optimal candidate material of ito thin film is substituted, research boom has at home and abroad been started then.
AZO transparent conductive film performance is closely related with target performance.Target material composition uniformity directly determines prepared thin
The homogeneity of ingredients of film；Target crystal structure, grain size and its uniformity then with film growth rates in magnetron sputtering process
It is directly related, therefore, it is to ensure that sputtered film has the uniformity of relatively low resistivity, the high transparency and film thickness,
The target for the being used uniformity that either composition or crystal orientation all must have, possesses high density and low bulk resistor
Rate.Highdensity target has relatively low resistivity, higher thermal conductivity, can sputter under relatively low substrate temperature and obtain low electricity
The film of resistance rate, high light transmittance rate, low body resistivity can improve sputter rate.
The content of the invention
The present invention provides a kind of preparation method of Al-Doped ZnO conductive film, and the preparation method is simple to operation, equipment
Require it is low, prepares simple, reproducible advantage, the Optimization of preparation crystal structure and surface topography, enhancing conductive thin
The photoelectric characteristic of film, improves thin film stability, so as to improving film performance, reducing reaction temperature, improve control accuracy, reduce system
Standby cost and adaptation large-scale production.
To achieve these goals, the invention provides a kind of preparation method of Al-Doped ZnO conductive film, the method
Comprise the steps：
（1）Prepare target
Raw material powder chromium oxide powder is mixed with Al-Doped ZnO powder, the mass content of the chromium oxide of doping is 0.5%, then to original
Feed powder body carries out ball-milling treatment, obtains fine size and uniform spherical particle；
The powder for processing is carried out die-filling；
Isostatic cool pressing is carried out after die-filling, pressure limit 100MPa-200MPa is then fired, and baking temperature range is 1200
℃-1500℃；
Semi-finished product are obtained after firing, is stood semi-finished product are machined after cooling, it is ensured that interior positive camber is smooth, obtains
The rotary target material of chromium doping Al-Doped ZnO.
（2）Process substrate
Grinding and polishing simultaneously cleans SiO2Substrate, it is standby；
（3）Using magnetron sputtering method, the rotary target material of chromium doping Al-Doped ZnO is made over the substrate and is led
Conductive film；
Magnetron sputtering makes the actual conditions of conductive film, sputtering chamber pressure 1-5Pa, sputtering chamber atmosphere be argon gas or nitrogen or
Argon hydrogen gaseous mixture, underlayer temperature is 100-300 DEG C, and sputtering power is 5-8W/cm2, sedimentation rate is 10-100nm/min, sputtering
Time is 2-4h.
Preferably, in the step（2）In, the grinding and polishing can be first on the boart boart wheel disc of 600 mesh by substrate
Corase grind 10min is carried out, fine grinding 10min is then carried out on the boart boart wheel disc of 1200 mesh, then with the diamond polishing of W2.5
Powder is polished, the ultrasonic cleaning uniformly bright to specimen surface, can in the following order clean the substrate after grinding and polishing,
Acetone is cleaned by ultrasonic 5min → absolute ethyl alcohol stand-by, the ion gun cleaning that is cleaned by ultrasonic 5min → drying, can adopt Hall from
Component carries out cleaning 5min to substrate, and pressure is 2 × 10-2Pa, underlayer temperature is 300 DEG C, and argon gas flux is 10sccm, is biased
For -100V, cathode current is 29.5A, and cathode voltage is 19V, and anode current is 7A, and anode voltage is 80V, to remove substrate table
The adsorbed gas in face and impurity, improve the bond strength and quality of forming film of sputtering layer and substrate.
Specific embodiment
Embodiment one
Raw material powder chromium oxide powder is mixed with Al-Doped ZnO powder, the mass content of the chromium oxide of doping is 0.5%, then to original
Feed powder body carries out ball-milling treatment, obtains fine size and uniform spherical particle；The powder for processing is carried out die-filling；It is die-filling
After carry out isostatic cool pressing, pressure limit 100MPa is then fired, baking temperature range be 1200 DEG C DEG C；Obtain after firing
Semi-finished product, stand semi-finished product are machined after coolings, it is ensured that interior positive camber is smooth, obtains chromium and mixes aluminium
The rotary target material of zinc oxide.
Grinding and polishing simultaneously cleans SiO2Substrate, it is standby.The grinding and polishing, can be by substrate first in the boart boart of 600 mesh
Corase grind 10min is carried out on wheel disc, fine grinding 10min is then carried out on the boart boart wheel disc of 1200 mesh, then with the Buddha's warrior attendant of W2.5
Stone polishing powder is polished, the ultrasonic cleaning uniformly bright to specimen surface, can be by the substrate after grinding and polishing by following suitable
Sequence is cleaned, and acetone ultrasonic cleaning 5min → absolute ethyl alcohol ultrasonic cleaning 5min → drying is stand-by, and the ion gun cleaning can be adopted
Hall ion source carries out cleaning 5min to substrate, and pressure is 2 × 10-2Pa, underlayer temperature is 300 DEG C, and argon gas flux is 10sccm,
Bias as -100V, cathode current is 29.5A, and cathode voltage is 19V, and anode current is 7A, and anode voltage is 80V, to remove lining
The adsorbed gas of basal surface and impurity, improve the bond strength and quality of forming film of sputtering layer and substrate.
Using magnetron sputtering method, the rotary target material is made into over the substrate the conductive film；Magnetron sputtering system
Actual conditions into the titania-doped film of the chromium tantalum is that sputtering chamber pressure 1Pa, sputtering chamber atmosphere is argon gas or nitrogen or argon
Hydrogen gaseous mixture, underlayer temperature is 100 DEG C, and sputtering power is 5W/cm2, sedimentation rate is 10nm/min, and sputtering time is 2h.
Embodiment two
Raw material powder chromium oxide powder is mixed with Al-Doped ZnO powder, the mass content of the chromium oxide of doping is 0.5%, then to original
Feed powder body carries out ball-milling treatment, obtains fine size and uniform spherical particle；The powder for processing is carried out die-filling；It is die-filling
After carry out isostatic cool pressing, pressure limit 200MPa is then fired, baking temperature range be 1500 DEG C；Half is obtained after firing
Finished product, stands semi-finished product are machined after cooling, it is ensured that interior positive camber is smooth, obtains chromium and mixes alumina
Change the rotary target material of zinc.
Grinding and polishing simultaneously cleans SiO2Substrate, it is standby.The grinding and polishing, can be by substrate first in the boart boart of 600 mesh
Corase grind 10min is carried out on wheel disc, fine grinding 10min is then carried out on the boart boart wheel disc of 1200 mesh, then with the Buddha's warrior attendant of W2.5
Stone polishing powder is polished, the ultrasonic cleaning uniformly bright to specimen surface, can be by the substrate after grinding and polishing by following suitable
Sequence is cleaned, and acetone ultrasonic cleaning 5min → absolute ethyl alcohol ultrasonic cleaning 5min → drying is stand-by, and the ion gun cleaning can be adopted
Hall ion source carries out cleaning 5min to substrate, and pressure is 2 × 10-2Pa, underlayer temperature is 300 DEG C, and argon gas flux is 10sccm,
Bias as -100V, cathode current is 29.5A, and cathode voltage is 19V, and anode current is 7A, and anode voltage is 80V, to remove lining
The adsorbed gas of basal surface and impurity, improve the bond strength and quality of forming film of sputtering layer and substrate.
Using magnetron sputtering method, the rotary target material is made into over the substrate the conductive film；Magnetron sputtering system
Actual conditions into the titania-doped film of the chromium tantalum is that sputtering chamber pressure 5Pa, sputtering chamber atmosphere is argon gas or nitrogen or argon
Hydrogen gaseous mixture, underlayer temperature is 300 DEG C, and sputtering power is 8W/cm2, sedimentation rate is 100nm/min, and sputtering time is 4h.
Claims (2)
1. a kind of preparation method of Al-Doped ZnO conductive film, the method comprises the steps：
（1）Prepare target
Raw material powder chromium oxide powder is mixed with Al-Doped ZnO powder, the mass content of the chromium oxide of doping is 0.5%, then to original
Feed powder body carries out ball-milling treatment, obtains fine size and uniform spherical particle；
The powder for processing is carried out die-filling；
Isostatic cool pressing is carried out after die-filling, pressure limit 100MPa-200MPa is then fired, and baking temperature range is 1200
℃-1500℃；
Semi-finished product are obtained after firing, is stood semi-finished product are machined after cooling, it is ensured that interior positive camber is smooth, obtains
The rotary target material of chromium doping Al-Doped ZnO；
（2）Process substrate
Grinding and polishing simultaneously cleans SiO2Substrate, it is standby；
（3）Using magnetron sputtering method, the rotary target material of chromium doping Al-Doped ZnO is made over the substrate and is led
Conductive film；
Magnetron sputtering makes the actual conditions of conductive film, sputtering chamber pressure 1-5Pa, sputtering chamber atmosphere be argon gas or nitrogen or
Argon hydrogen gaseous mixture, underlayer temperature is 100-300 DEG C, and sputtering power is 5-8W/cm2, sedimentation rate is 10-100nm/min, sputtering
Time is 2-4h.
2. the method for claim 1, it is characterised in that in the step（2）In, the grinding and polishing can be by substrate
First corase grind 10min is carried out on the boart boart wheel disc of 600 mesh, then carry out fine grinding on the boart boart wheel disc of 1200 mesh
10min, then, the ultrasonic cleaning uniformly bright to specimen surface is polished with the diamond polishing powder of W2.5, will can grind
Substrate after polishing is cleaned in the following order, and acetone ultrasonic cleaning 5min → absolute ethyl alcohol ultrasonic cleaning 5min → drying is stand-by,
The ion gun cleaning, can carry out cleaning 5min to substrate using hall ion source, and pressure is 2 × 10-2Pa, underlayer temperature is
300 DEG C, argon gas flux is 10sccm, is biased as -100V, and cathode current is 29.5A, and cathode voltage is 19V, and anode current is
7A, anode voltage is 80V, to remove adsorbed gas and the impurity of substrate surface, improves the bond strength of sputtering layer and substrate
And quality of forming film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611226708.4A CN106637118A (en) | 2016-12-27 | 2016-12-27 | Preparation method of aluminum-doped zinc oxide conductive thin film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611226708.4A CN106637118A (en) | 2016-12-27 | 2016-12-27 | Preparation method of aluminum-doped zinc oxide conductive thin film |
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| CN106637118A true CN106637118A (en) | 2017-05-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611226708.4A Pending CN106637118A (en) | 2016-12-27 | 2016-12-27 | Preparation method of aluminum-doped zinc oxide conductive thin film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111863590A (en) * | 2019-04-24 | 2020-10-30 | 世界先进积体电路股份有限公司 | Substrate structure and manufacturing method of semiconductor structure comprising same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921982A (en) * | 2010-09-06 | 2010-12-22 | 厦门大学 | Method for preparing nano-structured nitrogen silicon zirconium coating on surface of hard alloy substrate |
| CN102747334A (en) * | 2012-07-30 | 2012-10-24 | 中国科学院宁波材料技术与工程研究所 | Zinc-oxide-based transparent conductive film and preparation method thereof |
| CN105063559A (en) * | 2015-08-17 | 2015-11-18 | 基迈克材料科技（苏州）有限公司 | Zr element-doped AZO target material with enhanced photoelectric property |
-
2016
- 2016-12-27 CN CN201611226708.4A patent/CN106637118A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921982A (en) * | 2010-09-06 | 2010-12-22 | 厦门大学 | Method for preparing nano-structured nitrogen silicon zirconium coating on surface of hard alloy substrate |
| CN102747334A (en) * | 2012-07-30 | 2012-10-24 | 中国科学院宁波材料技术与工程研究所 | Zinc-oxide-based transparent conductive film and preparation method thereof |
| CN105063559A (en) * | 2015-08-17 | 2015-11-18 | 基迈克材料科技（苏州）有限公司 | Zr element-doped AZO target material with enhanced photoelectric property |
Non-Patent Citations (1)
| Title |
|---|
| Y.M.HU,ET AL.: "The morphology and optical properties of Cr-doped ZnO films grown using the magnetron co-sputtering method", 《APPLIED SURFACE SCIENCE》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111863590A (en) * | 2019-04-24 | 2020-10-30 | 世界先进积体电路股份有限公司 | Substrate structure and manufacturing method of semiconductor structure comprising same |
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