CN106702340A - Preparation method for stannic oxide transparent conductive thin film - Google Patents

Preparation method for stannic oxide transparent conductive thin film Download PDF

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Publication number
CN106702340A
CN106702340A CN201611226744.0A CN201611226744A CN106702340A CN 106702340 A CN106702340 A CN 106702340A CN 201611226744 A CN201611226744 A CN 201611226744A CN 106702340 A CN106702340 A CN 106702340A
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substrate
sputtering
preparation
target
argon gas
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不公告发明人
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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Priority to CN201611226744.0A priority Critical patent/CN106702340A/en
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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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a preparation method for a stannic oxide transparent conductive thin film. The preparation method is good in universality, low in facility request, simple in preparation and good in repeatability. According to the preparation method, the crystal structure and surface appearance are optimized, the photoelectric characteristics of the conductive thin film are enhanced, and the stability of the thin film is improved, so that the properties of the thin film are perfected, the reaction temperature is reduced, the control precision is increased, the preparation cost is lowered, and the preparation method is suitable for scaled production.

Description

A kind of preparation method of transparent conductive tin oxide thin films
Technical field
The present invention relates to conductive film field, and in particular to a kind of preparation method of transparent conductive tin oxide thin films.
Background technology
Transparent conductive oxide film was always the focus of photoelectric field in recent years, wherein ito thin film be at present research and Most widely used transparent conductive oxide (TCO) film, various photoelectricity are widely used in because of its good photoelectric characteristic Device, but because the prices of raw materials are expensive, indium resource is rare and environment is polluted, so as to limit its development and application.
SnO2It is a kind of broad-band gap oxide semiconductor to visible transparent, energy gap 3.7-4.0eV, with positive four Face body rutile structure.After fluorine has been mixed, SnO2 films have that, UV absorption coefficient good to visible light transmission be big, resistance Rate is low, stable chemical performance and the advantages of antiacid alkali ability is strong at room temperature.SnO is prepared at present2Prepared by transparent conducting glass Main method is to mix the SnO of F2Film, abbreviation FTO.FTO electro-conductive glass is the SnO of doping fluorine2Transparent conducting glass (SnO2：F), Referred to as FTO.FTO glass is exploited by the replacement articles for use as ITO electro-conductive glass, can be widely used in liquid crystal display The fields such as screen, photocatalysis, thin-film solar cells substrate, DSSC, electrochomeric glass.
The current FTO coated glasss mode of production mainly has two kinds：Chemical vapour deposition technique (APCVD) and magnetron sputtering method (PVD).Due to needing F atom of adulterating, therefore common magnetron sputtering to prepare FTO and mixed to meet, it is necessary to carry out certain transformation The problems such as potential safety hazard, equipment corrosion that miscellaneous F atom is brought.
The content of the invention
The present invention provides a kind of preparation method of transparent conductive tin oxide thin films, and the preparation method universality is good, equipment It is required that it is low, prepare simple, reproducible, the Optimization of preparation crystal structure and surface topography, strengthen the light of conductive film Electrical characteristics, improve thin film stability, so as to improve film performance, reduce reaction temperature, raising control accuracy, reduction preparation cost Mass produced with adaptation.
To achieve these goals, the invention provides a kind of preparation method of transparent conductive tin oxide thin films, the party Method comprises the following steps：
（1）Prepare target
Raw material powder chromium oxide powder is mixed with glass putty, the mass content of the chromium oxide of doping is 0.5%, and then material powder is entered Row ball-milling treatment, obtains fine size and uniform spherical particle；
Treated powder 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, semi-finished product is machined after standing cooling, it is ensured that interior positive camber is smooth, obtains Target.
（2）Treatment substrate
Grinding and polishing simultaneously cleans glass substrate, standby；
（3）Above-mentioned target is placed in magnetic control equipment with above-mentioned substrate, sputtering baffle plate is rotated between target and substrate, closed Opening of device vacuum.Gas in extracting device, makes vacuum indoor pressure reach 10-3Below Pa, heats substrate, makes underlayer temperature At 200 DEG C, to argon gas and oxygen is passed through in magnetic control equipment, oxygen is 1 with the ratio of argon gas to stabilization:3, the vacuum valve of adjusting device Door, pressure reaches 2Pa in making equipment.Shielding power supply is opened afterwards, and adjustment sputtering power is 100-150W, pre-sputtering 20-30 points Zhong Hou, removes sputtering baffle plate, starts sputtering, after sputtering time 50-70 minutes, sputtering baffle plate is rotated between target and substrate, Shielding power supply is closed, oxygen and argon gas valve are closed afterwards, the pressure in equipment is reduced to 10 again-3Pa.By the temperature of substrate Degree is promoted to 350-370 DEG C, anneals 50-70 minutes, after annealing terminates, takes out substrate.
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 use 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, bias It is -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 glass putty, the mass content of the chromium oxide of doping is 0.5%, and then material powder is entered Row ball-milling treatment, obtains fine size and uniform spherical particle；Treated powder is carried out die-filling；Carried out after die-filling cold Isostatic pressed, pressure limit 100MPa, is then fired, and baking temperature range is 1200 DEG C DEG C；Semi-finished product are obtained after firing, Semi-finished product are machined after standing cooling, it is ensured that interior positive camber is smooth, obtains target.
Grinding and polishing simultaneously cleans glass substrate, 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 used 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, It is -100V to bias, and 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.
Above-mentioned target is placed in magnetic control equipment with above-mentioned substrate, sputtering baffle plate is rotated between target and substrate, sealed Hull closure opens vacuum.Gas in extracting device, makes vacuum indoor pressure reach 10-3Below Pa, heats substrate, makes substrate temperature At 200 DEG C, to argon gas and oxygen is passed through in magnetic control equipment, oxygen is 1 with the ratio of argon gas to degree stabilization:3, the vacuum of adjusting device Valve, pressure reaches 2Pa in making equipment.Open shielding power supply afterwards, adjustment sputtering power is 100W, pre-sputtering is after 20 minutes, Sputtering baffle plate is removed, starts sputtering, sputtering time was rotated between target and substrate sputtering baffle plate after 50 minutes, closed sputtering Power supply, closes oxygen and argon gas valve afterwards, and the pressure in equipment is reduced into 10 again-3Pa.Substrate temperature is promoted to 350 DEG C, anneal 50 minutes, after annealing terminates, take out substrate.
Embodiment two
Raw material powder chromium oxide powder is mixed with glass putty, the mass content of the chromium oxide of doping is 0.5%, and then material powder is entered Row ball-milling treatment, obtains fine size and uniform spherical particle；Treated powder is carried out die-filling；Carried out after die-filling cold Isostatic pressed, pressure limit 200MPa, is then fired, and baking temperature range is 1500 DEG C；Semi-finished product are obtained after firing, it is quiet Semi-finished product are machined after putting cooling, it is ensured that interior positive camber is smooth, obtains target.
Grinding and polishing simultaneously cleans glass substrate, 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 used 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, It is -100V to bias, and 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.
Above-mentioned target is placed in magnetic control equipment with above-mentioned substrate, sputtering baffle plate is rotated between target and substrate, sealed Hull closure opens vacuum.Gas in extracting device, makes vacuum indoor pressure reach 10-3Below Pa, heats substrate, makes substrate temperature At 200 DEG C, to argon gas and oxygen is passed through in magnetic control equipment, oxygen is 1 with the ratio of argon gas to degree stabilization:3, the vacuum of adjusting device Valve, pressure reaches 2Pa in making equipment.Open shielding power supply afterwards, adjustment sputtering power is 150W, pre-sputtering is after 30 minutes, Sputtering baffle plate is removed, starts sputtering, sputtering time was rotated between target and substrate sputtering baffle plate after 70 minutes, closed sputtering Power supply, closes oxygen and argon gas valve afterwards, and the pressure in equipment is reduced into 10 again-3Pa.Substrate temperature is promoted to 370 DEG C, anneal 70 minutes, after annealing terminates, take out substrate.

Claims (2)

1. a kind of preparation method of transparent conductive tin oxide thin films, the method comprises the following steps：
（1）Prepare target
Raw material powder chromium oxide powder is mixed with glass putty, the mass content of the chromium oxide of doping is 0.5%, and then material powder is entered Row ball-milling treatment, obtains fine size and uniform spherical particle；
Treated powder 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, semi-finished product is machined after standing cooling, it is ensured that interior positive camber is smooth, obtains Target；
（2）Treatment substrate
Grinding and polishing simultaneously cleans glass substrate, standby；
（3）Above-mentioned target is placed in magnetic control equipment with above-mentioned substrate, sputtering baffle plate is rotated between target and substrate, closed Opening of device vacuum,
Gas in extracting device, makes vacuum indoor pressure reach 10-3Below Pa, heats substrate, makes underlayer temperature stabilization 200 DEG C, to argon gas and oxygen is passed through in magnetic control equipment, the ratio of oxygen and argon gas is 1:3, the vacuum valve of adjusting device makes equipment Middle pressure reaches 2Pa, and shielding power supply is opened afterwards, and adjustment sputtering power is 100-150W, after pre-sputtering 20-30 minutes, is removed Sputtering baffle plate, starts sputtering, after sputtering time 50-70 minutes, sputtering baffle plate is rotated between target and substrate, closes sputtering electricity Source, closes oxygen and argon gas valve afterwards, and the pressure in equipment is reduced into 10 again-3Pa, substrate temperature is promoted to 350-370 DEG C, anneal 50-70 minutes, after annealing terminates, take out substrate.
2. the method for claim 1, it is characterised in that in the step（2）In, the grinding and polishing can be by substrate Corase grind 10min first is carried out on the boart boart wheel disc of 600 mesh, then fine grinding is carried out 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, and it is -100V to bias, 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.
CN201611226744.0A 2016-12-27 2016-12-27 Preparation method for stannic oxide transparent conductive thin film Pending CN106702340A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114525427A (en) * 2020-11-06 2022-05-24 湖南七点钟文化科技有限公司 Tin-based alloy material, preparation method thereof, high-resistance film and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
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
CN102978578A (en) * 2012-08-28 2013-03-20 河北工业大学 Copper oxide doped tin dioxide base ammonia gas sensitive sensor manufacturing method
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
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
CN102978578A (en) * 2012-08-28 2013-03-20 河北工业大学 Copper oxide doped tin dioxide base ammonia gas sensitive sensor manufacturing method
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)

* Cited by examiner, † Cited by third party
Title
SHIU-JEN LIU,ET AL.: "Physical properties of polycrystalline Cr-doped SnO2 films grown on glasses using reactive dc magnetron co-sputtering technique", 《APPLIED SURFACE SCIENCE》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114525427A (en) * 2020-11-06 2022-05-24 湖南七点钟文化科技有限公司 Tin-based alloy material, preparation method thereof, high-resistance film and preparation method thereof

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