CN113445000A - Preparation method of ITO film - Google Patents

Preparation method of ITO film Download PDF

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Publication number
CN113445000A
CN113445000A CN202010211521.7A CN202010211521A CN113445000A CN 113445000 A CN113445000 A CN 113445000A CN 202010211521 A CN202010211521 A CN 202010211521A CN 113445000 A CN113445000 A CN 113445000A
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Prior art keywords
substrate
ito film
target
cleaning
sputtering
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Pending
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CN202010211521.7A
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Chinese (zh)
Inventor
杨圣合
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SAE Technologies Development Dongguan Co Ltd
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SAE Technologies Development Dongguan Co Ltd
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Priority to CN202010211521.7A priority Critical patent/CN113445000A/en
Publication of CN113445000A publication Critical patent/CN113445000A/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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • 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
    • 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
    • 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
    • C23C14/50—Substrate holders
    • C23C14/505—Substrate holders for rotation of the substrates
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention relates to the technical field of film processing, and discloses a preparation method of an ITO film, which comprises the steps of firstly pre-cleaning a substrate to remove dirt and dust on the surface of the substrate, then pre-sputtering by taking an indium tin oxide ceramic target as a target material to clean the surface of the target, then ensuring that the temperature of a processing chamber is heated to 100-150 ℃, and ensuring that the vacuum degree of the processing chamber is 2.5 multiplied by 10‑1Pa～3.5×10‑1Pa, and the volume ratio of 16:0.5 introducing argon and oxygen, sputtering the substrate by taking an indium tin oxide ceramic target as a target material to form an ITO film on the substrate, thereby obtaining the ITO film with uniform thicknessThe film has good uniformity, so that charges are easy to conduct away, and the antistatic effect is improved.

Description

Preparation method of ITO film
Technical Field
The invention relates to the technical field of thin film processing, in particular to a preparation method of an ITO thin film.
Background
The fabrication process of the ITO thin film (indium tin oxide thin film) is a process of transferring one material (thin film material) to the surface of another material (substrate) to form a thin film firmly bonded to the substrate. Common ITO film preparation processes include chemical vapor deposition, vacuum reactive evaporation, sol-gel methods, spray pyrolysis, microwave ECR plasma reactive evaporation deposition, pulsed laser deposition, and the like. At present, in order to prevent static electricity from a TFT (Thin-Film Transistor) substrate, methods such as evaporation coating and the like are mostly adopted to prepare an ITO Thin Film on the TFT substrate, but the thickness uniformity of the ITO Thin Film prepared by the conventional evaporation coating is poor, so the static electricity prevention effect is poor.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of an ITO film, which can solve the problem of poor antistatic effect caused by poor thickness uniformity of the ITO film prepared by traditional evaporation coating.
In order to solve the above technical problem, an embodiment of the present invention provides a method for preparing an ITO thin film, including:
pre-cleaning a substrate;
placing the substrate after pre-cleaning in a processing cavity;
carrying out pre-sputtering by taking an indium tin oxide ceramic target as a target material;
the temperature of the processing cavity is heated to 100-150 ℃, and the vacuum degree of the processing cavity is 2.5 multiplied by 10-1Pa～3.5×10-1Pa, and the volume ratio of 16:0.5 introducing argon and oxygen, controlling the substrate to rotate at a preset rotating speed, and sputtering the substrate by taking the indium tin oxide ceramic target as a target material to form an ITO film on the substrate.
As a preferred scheme, the pre-cleaning of the substrate specifically includes:
soaking the substrate in deionized water for 30 min;
putting the substrate into alkali liquor for ultrasonic cleaning, wherein the cleaning time is 20 min;
putting the substrate into acetone for ultrasonic cleaning for 30 min;
putting the substrate into ethanol for ultrasonic cleaning, wherein the cleaning time is 20 min;
putting the substrate into deionized water for ultrasonic cleaning, wherein the cleaning time is 15-25 min;
and drying the substrate by cold air and hot air in sequence, and drying and storing to obtain the substrate after pre-cleaning.
As a preferred scheme, the pre-sputtering with the indium tin oxide ceramic target as the target specifically comprises:
controlling the vacuum degree of the processing chamber to be 1 multiplied by 10-6And torr, controlling the rotating speed of the substrate to be 20r/min, and carrying out pre-sputtering by using an indium tin oxide ceramic target as a target for 100 sec.
Preferably, the preset rotating speed is 20 r/min.
Preferably, the total pressure of oxygen and argon is 0.5 Pa.
Preferably, the substrate is controlled to rotate at a preset rotation speed, and in the step of sputtering the substrate by using the indium tin oxide ceramic target as the target material, the sputtering voltage is 250-300V, and the power is 300-1000 w.
Preferably, after the forming of the ITO thin film on the substrate, the method further comprises:
annealing the substrate with the ITO film formed thereon at 300 deg.C for 40min, and cooling to form an ITO film with a thickness of 0.1-0.25 nm.
Preferably, the substrate is soda-lime-based glass.
The embodiment of the invention has the following beneficial effects:
the preparation method of the ITO film provided by the embodiment of the invention comprises the steps of firstly pre-cleaning a substrate to remove dirt and dust on the surface of the substrate, then pre-sputtering by taking an indium tin oxide ceramic target as a target material to clean the target surface, then ensuring that the temperature of a processing cavity is heated to 100-150 ℃, and ensuring that the vacuum degree of the processing cavity is 2.5 multiplied by 10-1Pa～3.5×10-1Pa, and the volume ratio of 16:0.5 introducing argon and oxygen, sputtering the substrate by taking an indium tin oxide ceramic target as a target material to form an ITO film on the substrate, thereby obtaining the ITO film with more uniform thickness.
Drawings
FIG. 1 is a flowchart of a method for producing an ITO thin film in an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
FIG. 1 is a flow chart of a method for preparing an ITO film according to an embodiment of the present invention.
The preparation method of the ITO film comprises the following steps:
step S101, pre-cleaning a substrate;
step S102, placing the substrate after pre-cleaning in a processing cavity;
step S103, carrying out pre-sputtering by taking an indium tin oxide ceramic target as a target material;
step S104, heating the processing chamber to 100-150 ℃, wherein the vacuum degree of the processing chamber is 2.5 multiplied by 10- 1Pa～3.5×10-1Pa, and the volume ratio of 16:0.5 introducing argon and oxygen, controlling the substrate to rotate at a preset rotating speed, and sputtering the substrate by taking the indium tin oxide ceramic target as a target material to form an ITO film on the substrate.
In the embodiment of the invention, firstly, the substrate is pre-cleaned to remove the surface dirt and dust of the substrate (TFT substrate), then the indium tin oxide ceramic target is used as the target material to carry out pre-sputtering to clean the target surface, then the temperature of the processing chamber is ensured to be heated to 100-150 ℃, and the vacuum degree of the processing chamber is 2.5 multiplied by 10-1Pa～3.5×10-1Pa, and the volume ratio of 16:0.5 introducing argon and oxygen, sputtering the substrate by taking an indium tin oxide ceramic target as a target material to form an ITO film on the substrate, thereby obtaining the ITO film with more uniform thickness.
Specifically, the step S101 "pre-cleaning the substrate" specifically includes:
soaking the substrate in deionized water for 30 min;
putting the substrate into alkali liquor for ultrasonic cleaning, wherein the cleaning time is 20 min;
putting the substrate into acetone for ultrasonic cleaning for 30 min;
putting the substrate into ethanol for ultrasonic cleaning, wherein the cleaning time is 20 min;
putting the substrate into deionized water for ultrasonic cleaning, wherein the cleaning time is 15-25 min;
and drying the substrate by cold air and hot air in sequence, and drying and storing to obtain the substrate after pre-cleaning.
In the embodiment of the invention, the substrate is sequentially cleaned by deionized water, alkali liquor, acetone, ethanol and deionized water to remove dirt and dust on the surface of the substrate, and then is sequentially dried by cold air and hot air, dried and stored so as to be convenient for the subsequent formation of the ITO film with uniform thickness. Illustratively, the alkaline solution is an NAOH solution, and the substrate is soda-lime-based glass.
Specifically, the step S103 of pre-sputtering with an indium tin oxide ceramic target as a target specifically includes:
controlling the vacuum degree of the processing chamber to be 1 multiplied by 10-6And torr, controlling the rotating speed of the substrate to be 20r/min, and carrying out pre-sputtering by using an indium tin oxide ceramic target as a target for 100 sec.
Specifically, in the step S104 ″, the temperature of the processing chamber is heated to 100 to 150 ℃, and the vacuum degree of the processing chamber is 2.5 × 10-1Pa～3.5×10-1Pa, and the volume ratio of 16: and 0.5 introducing argon and oxygen, controlling the substrate to rotate at a preset rotating speed, and sputtering the substrate by using an indium tin oxide ceramic target as a target material to form an ITO film on the substrate, wherein the preset rotating speed is 20r/min, the total pressure of the oxygen and the argon is 0.5Pa, the sputtering voltage is 250-300V, and the power is 300-1000 w.
In the embodiment of the invention, argon and oxygen are introduced according to the argon-oxygen volume ratio of 16:0.5, oxygen is used as reaction gas, and argon is used as process gas. In addition, the sputtering voltage and power are lower than those of the traditional direct-current magnetron sputtering coating and evaporation coating, the energy consumption is low, the energy is saved, the environment is protected, and the preparation cost is reduced. Moreover, the thickness uniformity of the prepared ITO film is good, and the anti-static effect of the TFT substrate is favorably improved.
Specifically, after the step S104, the method further includes:
annealing the substrate with the ITO film formed thereon at 300 deg.C for 40min, and cooling to form an ITO film with a thickness of 0.1-0.25 nm.
The embodiment can eliminate hardness through cooling annealing to avoid the ITO film from falling off, thereby improving the connection stability of the ITO film and the substrate.
To sum up, the embodiment of the present invention provides a method for preparing an ITO thin film, which comprises pre-cleaning a substrate to remove surface contamination and dust of the substrate, pre-sputtering an indium tin oxide ceramic target as a target to clean a target surface, heating a processing chamber to 100-150 ℃ under a vacuum degree of 2.5 × 10-1Pa～3.5×10-1Pa, and the volume ratio of 16:0.5 introducing argon and oxygen, sputtering the substrate by taking an indium tin oxide ceramic target as a target material to form an ITO film on the substrate, thereby obtaining the ITO film with more uniform thickness.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.

Claims (8)

1. A method for preparing an ITO film is characterized by comprising the following steps:
pre-cleaning a substrate;
placing the substrate after pre-cleaning in a processing cavity;
carrying out pre-sputtering by taking an indium tin oxide ceramic target as a target material;
heating the processing chamber to a temperature of 100-150 deg.C and placing in the processing chamberThe degree of vacuum was 2.5X 10-1Pa～3.5×10-1Pa, and the volume ratio of 16:0.5 introducing argon and oxygen, controlling the substrate to rotate at a preset rotating speed, and sputtering the substrate by taking the indium tin oxide ceramic target as a target material to form an ITO film on the substrate.
2. The method for preparing the ITO film according to claim 1, wherein the pre-cleaning of the substrate specifically comprises:
soaking the substrate in deionized water for 30 min;
putting the substrate into alkali liquor for ultrasonic cleaning, wherein the cleaning time is 20 min;
putting the substrate into acetone for ultrasonic cleaning for 30 min;
putting the substrate into ethanol for ultrasonic cleaning, wherein the cleaning time is 20 min;
putting the substrate into deionized water for ultrasonic cleaning, wherein the cleaning time is 15-25 min;
and drying the substrate by cold air and hot air in sequence, and drying and storing to obtain the substrate after pre-cleaning.
3. The method for preparing the ITO film according to claim 1, wherein the pre-sputtering using an indium tin oxide ceramic target as a target specifically comprises:
controlling the vacuum degree of the processing chamber to be 1 multiplied by 10-6And torr, controlling the rotating speed of the substrate to be 20r/min, and carrying out pre-sputtering by using an indium tin oxide ceramic target as a target for 100 sec.
4. The method for preparing the ITO film according to claim 1, wherein the predetermined rotation speed is 20 r/min.
5. The method of preparing an ITO film according to claim 4, wherein the total pressure of oxygen and argon is 0.5 Pa.
6. The method for preparing the ITO film according to claim 1, wherein the step of controlling the substrate to rotate at a predetermined rotation speed and sputtering the substrate with the ITO ceramic target as a target material has a sputtering voltage of 250 to 300V and a power of 300 to 1000 w.
7. The method for preparing an ITO thin film according to any of claims 1 to 6, further comprising, after the forming of the ITO thin film on the substrate:
annealing the substrate with the ITO film formed thereon at 300 deg.C for 40min, and cooling to form an ITO film with a thickness of 0.1-0.25 nm.
8. The method for producing an ITO thin film according to any one of claims 1 to 6, wherein the substrate is soda-lime-based glass.
CN202010211521.7A 2020-03-24 2020-03-24 Preparation method of ITO film Pending CN113445000A (en)

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CN202010211521.7A CN113445000A (en) 2020-03-24 2020-03-24 Preparation method of ITO film

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Application Number Priority Date Filing Date Title
CN202010211521.7A CN113445000A (en) 2020-03-24 2020-03-24 Preparation method of ITO film

Publications (1)

Publication Number Publication Date
CN113445000A true CN113445000A (en) 2021-09-28

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Application publication date: 20210928