CN106521443B - Preparation method of silicon carbide hard film and glass - Google Patents

Preparation method of silicon carbide hard film and glass Download PDF

Info

Publication number
CN106521443B
CN106521443B CN201611104056.7A CN201611104056A CN106521443B CN 106521443 B CN106521443 B CN 106521443B CN 201611104056 A CN201611104056 A CN 201611104056A CN 106521443 B CN106521443 B CN 106521443B
Authority
CN
China
Prior art keywords
silicon carbide
gas
hard film
substrate
glass
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201611104056.7A
Other languages
Chinese (zh)
Other versions
CN106521443A (en
Inventor
何建军
魏宇新
方凤军
江涛
陈多
洪蒙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yichang Nanbo Display Co ltd
Original Assignee
Yichang Nanbo Display Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yichang Nanbo Display Co ltd filed Critical Yichang Nanbo Display Co ltd
Priority to CN201611104056.7A priority Critical patent/CN106521443B/en
Publication of CN106521443A publication Critical patent/CN106521443A/en
Application granted granted Critical
Publication of CN106521443B publication Critical patent/CN106521443B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
    • 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
    • C23C14/0635—Carbides

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention relates to a preparation method of a silicon carbide hard film and glass, wherein the method takes organic gas with 1-4 carbon atoms as reaction gas, takes gas containing argon as process gas, takes a silicon target as a sputtering target material, controls the reaction temperature to be 100-300 ℃, and deposits the silicon carbide hard film on a substrate through magnetron sputtering. This method can produce a film having a thickness of
Figure DDA0001171060910000011
The thickness of the film layer of the thinner silicon carbide hard film is far less than the nanometer level, so that the hardness of the glass surface can be obviously improved, the scratch resistance of the glass surface is improved, and the glass substrate is effectively protected.

Description

Preparation method of silicon carbide hard film and glass
Technical Field
The invention relates to the field of vacuum coating, in particular to a preparation method of a silicon carbide hard film and glass.
Background
The glass has wide application in the fields of LED chips, cameras, fingerprint identification cover plates and the like. However, the hardness of the surface of the common glass is lower and far lower than that of the sapphire material, when an optical film layer is plated on the glass, the hardness of the surface of the film layer is not high, and the surface of the glass is easily scratched to leave scratches during processing and use. Therefore, researches on improving scratch resistance by adding a hard film layer on the surface of glass or the surface of the film layer are very concerned. At present, most methods for increasing the surface hardness of glass are to prepare an alumina film by a spraying or evaporation coating process or to sputter a silicon nitride film in vacuum, but the silicon nitride film is not wear-resistant and has limited capability of increasing the surface hardness. The spraying coating process generally uses alumina powder as a raw material to carry out processing, the thickness of the obtained coating is thicker, generally more than 50nm, the adhesive force is not good enough, and the appearance quality hardly meets the requirements of optical glass. In the evaporation coating process, an alumina block or powder material is bombarded by a high-energy electron gun and then deposited on the surface of a substrate, generally, only a small-size substrate can be processed, the coating processing of a large-size glass substrate is difficult, and the abrasion resistance of a film layer is poor. The hard film layers prepared by the methods can only achieve the effect of protecting the glass substrate after the thickness of the hard film layers reaches the nanometer level. However, the thickness of the additional hard film is too thick, and the absorption of the hard film material affects the optical performance of the whole glass substrate, thereby limiting the application.
In summary, the hard film layer prepared by the conventional method is thick, and generally needs to reach a thickness of hundreds of nanometers or even microns to achieve the effect of protecting the glass substrate.
Disclosure of Invention
Accordingly, there is a need for a method of manufacturing a thin hard silicon carbide film and glass.
A preparation method of a silicon carbide hard film comprises the following steps:
providing a substrate; and
placing the substrate in a cavity of magnetron sputtering equipment, under the vacuum condition, taking organic gas containing 1-4 carbon atoms as reaction gas, taking gas containing argon as process gas, taking a silicon target as a sputtering target material, controlling the reaction temperature to be 100-300 ℃, and depositing a silicon carbide hard film on the substrate by magnetron sputtering.
In one embodiment, the volume ratio of the reaction gas to the process gas is 0.4 to 4: 1.
In one embodiment, the organic gas having 1 to 4 carbon atoms is at least one selected from methane and acetylene.
In one embodiment, the reaction gas is methane or acetylene, the process gas is argon, and the methane or acetylene accounts for 30% -80% of the total volume of the process gas and the reaction gas.
In one embodiment, the percentage of silicon in the silicon target is 99% or more.
In one embodiment, in the operation of depositing the hard silicon carbide film on the substrate by magnetron sputtering, the sputtering power is 2kW to 5 kW.
In one embodiment, the vacuum degree of the vacuum condition is 1 × 10-3mbar～5×10-3mbar。
In one embodiment, the hard silicon carbide film has a thickness of
Figure BDA0001171060890000021
The following.
In one embodiment, the substrate is a glass substrate.
The glass comprises a glass substrate and a silicon carbide hard film laminated on the glass substrate, wherein the silicon carbide hard film is prepared by the preparation method of the silicon carbide hard film.
The preparation method of the silicon carbide hard film takes organic gas with 1-4 carbon atoms as reaction gas, gas containing argon as process gas, silicon target as sputtering target material, reaction temperature is controlled to be 100-300 ℃, and the silicon carbide hard film is deposited on the substrate through magnetron sputtering. Under the action of an electric field, argon atoms in argon gas are ionized to generate Ar + ions and electrons, the Ar + ions are accelerated to fly to a silicon target under the action of the electric field and bombard the surface of the silicon target at high energy to enable the silicon target to be sputtered to generate sputtering particles, organic gas with 1-4 carbon atoms can react with the sputtering particles chemically, and therefore a silicon carbide hard film is deposited on the substrate. This method can produce a film having a thickness of
Figure BDA0001171060890000022
The thickness of the film layer is in nanometer level, and when the thickness of the silicon carbide hard film is only the same as that of the silicon carbide hard film
Figure BDA0001171060890000023
The Mohs hardness can reach 6 grades at about (angstroms), the hardness of the glass surface is obviously improved, the scratch resistance of the glass surface is improved, and the glass substrate is effectively protected.
Drawings
Fig. 1 is a flowchart of a method for producing a silicon carbide hard film according to an embodiment;
fig. 2 is a schematic structural view of a glass according to an embodiment.
Detailed Description
The following description will mainly refer to the drawings and the specific examples to further describe the preparation method of the silicon carbide hard film and the glass in detail.
The method for preparing a hard silicon carbide film according to one embodiment shown in fig. 1 includes the steps of:
and S10, providing a substrate.
The substrate may be any member requiring a hard coating film, such as glass, a metal plate, an alloy plate, a flexible substrate, and the like.
In one embodiment, the substrate is a glass substrate.
S20, placing the substrate in a cavity of a magnetron sputtering device, under the vacuum condition, taking organic gas containing 1-4 carbon atoms as reaction gas, taking gas containing argon as process gas, taking a silicon target as a sputtering target material, controlling the reaction temperature to be 100-300 ℃, and depositing a silicon carbide hard film on the substrate by magnetron sputtering.
Specifically, the reaction gas and the process gas can be introduced into the cavity of the magnetron sputtering device through the same pipeline, or can be introduced into the cavity of the magnetron sputtering device separately. In the embodiment, two pipelines are adopted for introducing, so that the flow of gas is conveniently regulated and controlled.
Specifically, the volume ratio of the reaction gas to the process gas is 0.4-4: 1. Furthermore, the volume ratio of the reaction gas to the process gas is 0.5-2: 1. Furthermore, the volume ratio of the reaction gas to the process gas is 0.8-1.2: 1.
The reaction gas contains organic gas with 1-4 carbon atoms, an organic gas atmosphere is formed in a cavity of the magnetron sputtering equipment, the organic gas contains carbon (C) atoms, and the carbon (C) atoms and sputtering particle silicon (Si) are subjected to chemical reaction under specific conditions, so that a silicon carbide (SiC)) hard film is deposited on the substrate. It is understood that other gases may be contained in the reaction gas, and other gases may be used as the carrier gas, such as argon (Ar) gas, neon (Ne) gas, and the like.
The process gas contains argon (Ar), argon atoms in the argon (Ar) are ionized to generate Ar + ions and electrons, and the Ar + ions are accelerated to fly to the silicon target under the action of an electric field to bombard the surface of the silicon target. Of course, the process gas may also contain other gases, such as neon (Ne) and the like.
Wherein the organic gas having 1 to 4 carbon atoms may be, for example, methane (CH)4) Ethane (C)2H6) Ethylene (C)2H4) Acetylene (C)2H2) Propane (C)3H8) Butene (C)4H8) N-butane (n-C)4H10) Isobutane (i-C)4H10) Propylene (C)3H6) Or cyclopropane (C)3H6) And so on. The reaction gas introduced into the cavity of the magnetron sputtering device can contain one organic gas or a mixed gas of two or more organic gases. The organic gas contains carbon (C) atoms and chemically reacts with sputtered particulate silicon (Si) under specific conditions to deposit a hard film of silicon carbide (SiC) on the substrate.
Specifically, the organic gas with 1-4 carbon atoms is selected from methane (CH)4) And acetylene (C)2H2) At least one of (1). For example, it may be methane (CH) alone4) Or acetylene (C) alone2H2) As a reaction gas, or with methane (CH)4) With acetylene (C)2H2) The mixed gas of (2) is used as a reaction gas.
Specifically, the organic gas with 1-4 carbon atoms accounts for 30-80% of the total volume of the process gas and the reaction gas. Namely, the mixed gas in the cavity of the magnetron sputtering equipment can be separated according to different gases, and the volume of the organic gas with 1-4 carbon atoms divided by the total volume of the process gas and the reaction gas is 30-80%. The percentage of the organic gas can be adjusted by the gas flow of the gas introduced into the cavity of the magnetron sputtering equipment.
In one embodiment, the gas flow of the organic gas with 1-4 carbon atoms accounts for 40% -60% of the total volume of the process gas and the reaction gas. In another embodiment, the gas flow of the organic gas with 1-4 carbon atoms accounts for 30% -50% of the total volume of the process gas and the reaction gas.
In one embodiment, the reactant gas is methane (CH)4) The process gas is argon (Ar) and methane (CH)4) Accounting for 40 to 60 percent of the total volume of the process gas and the reaction gas. Methane (CH)4) Accounting for 45-50 percent of the total volume of the process gas and the reaction gas.
In another embodiment, the reactant gas is acetylene (C)2H2) The process gas is argon (Ar) or acetylene (C)2H2) Accounting for 40 to 60 percent of the total volume of the process gas and the reaction gas. Further, acetylene (C)2H2) Accounting for 45-50 percent of the total volume of the process gas and the reaction gas.
In particular, methane (CH)4) Or acetylene (C)2H2) The percentage content of the carbon dioxide can be adjusted by the gas flow of gas introduced into the cavity of the magnetron sputtering equipment. For example, methane (CH)4) The flow rate of (3) was 100sccm, and the flow rate of argon (Ar) was 100sccm, to obtain methane (CH)4) Is 50% of gas atmosphere. Corresponding to acetylene (C)2H2) The flow rate of (3) was 100sccm, the flow rate of argon (Ar) was 100sccm, and acetylene (C) was obtained2H2) Is 50% of gas atmosphere.
Specifically, the percentage content of silicon in the silicon target is more than 99%. According to the preparation method of the silicon carbide hard film, a silicon target (Si) can be directly used as a target material, and organic gas with 1-4 carbon atoms is used as reaction gas, so that the thin silicon carbide hard film can be prepared. Compared with a silicon nitride film layer prepared by taking silicon nitride as a target material, the silicon nitride film layer has small thickness and high hardness.
Specifically, in the operation of depositing the silicon carbide hard film on the substrate by magnetron sputtering, the sputtering power is 2kW to 5 kW. The sputtering power of 2 kW-5 kW can better enable the silicon target to sputter, so that the prepared silicon carbide hard film layer is uniform and thin.
Specifically, the degree of vacuum under vacuum was 1X 10-3mbar～5×10-3mbar. Further, the degree of vacuum under vacuum was 2X 10-3mbar～4×10-3mbar。
Specifically, the thickness of the prepared silicon carbide hard film is
Figure BDA0001171060890000051
The following. By the process of the invention, it is possible to prepare a coating having a thickness of
Figure BDA0001171060890000052
Compared with a hard film layer prepared by a spraying or evaporation coating process, the thickness of the ultrathin silicon carbide hard film is obviously reduced, the development of light and thin glass is facilitated, and the integral optical performance is improved.
In one embodiment, by the method of the present invention, a thickness of
Figure BDA0001171060890000053
The following hard silicon carbide film.
In another embodiment, by the process of the present invention, a thickness of
Figure BDA0001171060890000054
The following hard silicon carbide film.
Specifically, the reaction temperature is 100 ℃ to 300 ℃, and further, the reaction temperature is 230 ℃ to 280 ℃. At the temperature of 100-300 ℃, organic gas with 1-4 carbon atoms can react with the sputtered particles, so that a silicon carbide hard film is deposited on the substrate, and the hard film is uniform and thin.
The preparation method of the silicon carbide hard film takes organic gas with 1-4 carbon atoms as reaction gas, gas containing argon as process gas, silicon target as sputtering target material, reaction temperature is controlled to be 100-300 ℃,and depositing a silicon carbide hard film on the substrate by magnetron sputtering. Under the action of an electric field, argon atoms in argon gas are ionized to generate Ar + ions and electrons, the Ar + ions are accelerated to fly to a silicon target under the action of the electric field and bombard the surface of the silicon target at high energy to enable the silicon target to be sputtered to generate sputtering particles, organic gas with 1-4 carbon atoms can react with the sputtering particles chemically, and therefore a silicon carbide hard film is deposited on the substrate. This method can produce a film having a thickness of
Figure BDA0001171060890000055
The thickness of the film layer of the ultra-thin silicon carbide hard film is far less than the nanometer level, and when the thickness of the silicon carbide hard film is only within the range of
Figure BDA0001171060890000056
The Mohs hardness can reach 6 grades at about (angstroms), the scratch resistance of the glass surface can be obviously improved, and the glass substrate can be effectively protected.
In addition, referring to fig. 2, the present invention further provides a glass 10 according to an embodiment. The glass 10 includes a glass substrate 110 and a silicon carbide hard film 120 laminated on the glass substrate 110. Wherein, the silicon carbide hard film 120 is prepared by the preparation method of the silicon carbide hard film. Namely, the glass substrate 110 is used as a substrate, and the silicon carbide hard film 120 is deposited on the glass substrate 110 by magnetron sputtering.
Specifically, the thickness of the hard silicon carbide film 120 is
Figure BDA0001171060890000061
Hereinafter, further, the thickness of the silicon carbide hard film 120 is
Figure BDA0001171060890000062
Hereinafter, further, the thickness of the silicon carbide hard film 120 is
Figure BDA0001171060890000063
The following.
The glass 10 has the advantages that the silicon carbide hard film 120 is thin, the optical performance is good, and the surface of the glass is not easy to scratch. The LED fingerprint identification device can be widely applied to the fields of LED chips, cameras, fingerprint identification cover plates and the like.
The following are specific examples.
Example 1
Using soda-lime glass as substrate, placing soda-lime glass in cavity of magnetron sputtering equipment, 2.5X 10-3Under the mbar vacuum condition, acetylene is used as a reaction gas, argon is used as a process gas, wherein the flow rate of acetylene is 100sccm, and the flow rate of argon is 150 sccm. Adopting a silicon target as a sputtering target material, wherein the sputtering power is as follows: 3.5kW, the reaction temperature is controlled to be 200 ℃, and the thickness of the magnetron sputtering deposition on the substrate is about
Figure BDA0001171060890000064
The hard film of silicon carbide.
And (3) carrying out scribing test on the thickness of the prepared silicon carbide hard film by adopting Mohs hardness pens with different grades. If the silicon carbide hard film is scratched, the hardness of the silicon carbide hard film is lower than the hardness grade of the Mohs hardness pen for testing, and if the silicon carbide hard film is not scratched, the hardness of the silicon carbide hard film is higher than the hardness grade of the Mohs hardness pen for testing. The following examples, which are not specifically illustrated, all employ this method for testing hardness. The hard film of silicon carbide measured in this example had a mohs hardness of 6, while soda lime glass had an original mohs hardness of 3. The silicon carbide hard film prepared by the embodiment is thinner, and the hardness of the surface of the glass can be obviously improved.
Example 2
High alumina glass is taken as a substrate, and the high alumina glass is placed in a cavity of a magnetron sputtering device, wherein the volume of the cavity is 3.2 multiplied by 10-3Under the mbar vacuum condition, acetylene is used as a reaction gas, argon is used as a process gas, wherein the flow rate of acetylene is 100sccm, and the flow rate of argon is 250 sccm. Adopting a silicon target as a sputtering target material, wherein the sputtering power is as follows: 3.5kW, the reaction temperature is controlled to be 250 ℃, and the thickness of the magnetron sputtering deposition on the substrate is about
Figure BDA0001171060890000071
The hard film of silicon carbide.
The hard film of silicon carbide measured in this example had a Mohs hardness of 6, while the original Mohs hardness of high alumina glass was 3. The silicon carbide hard film prepared by the embodiment is thinner, and the hardness of the surface of the glass can be obviously improved.
Example 3
Using soda-lime glass as substrate, placing soda-lime glass in cavity of magnetron sputtering equipment, 2.1 × 10-3Under the mbar vacuum condition, methane is used as a reaction gas, argon is used as a process gas, wherein the flow rate of methane is 100sccm, and the flow rate of argon is 150 sccm. Adopting a silicon target as a sputtering target material, wherein the sputtering power is as follows: 5kW, the reaction temperature is controlled to be 300 ℃, and the thickness of the magnetron sputtering deposition on the substrate is about
Figure BDA0001171060890000072
The hard film of silicon carbide.
The hard film of silicon carbide measured in this example had a mohs hardness of 6, while soda lime glass had an original mohs hardness of 3. The silicon carbide hard film prepared by the embodiment is thinner, and the hardness of the surface of the glass can be obviously improved.
Example 4
The soda-lime glass is taken as a substrate and is placed in a cavity of the magnetron sputtering equipment, and the size of the cavity is 5 multiplied by 10-3Under the mbar vacuum condition, the mixed gas of methane and acetylene is used as reaction gas, argon is used as process gas, wherein the gas flow of methane is 100sccm, the gas flow of acetylene is 300sccm, and the gas flow of argon is 100 sccm. Adopting a silicon target as a sputtering target material, wherein the sputtering power is as follows: 4kw, controlling the reaction temperature at 220 ℃, and depositing the thickness of the magnetron sputtering on the substrate
Figure BDA0001171060890000073
The hard film of silicon carbide.
The hard film of silicon carbide measured in this example had a mohs hardness of 6, while soda lime glass had an original mohs hardness of 3. The silicon carbide hard film prepared by the embodiment is thinner, and the hardness of the surface of the glass can be obviously improved.
Example 5
Using soda-lime glass as substrate, placing soda-lime glass in cavity of magnetron sputtering equipment, 1.8X 10-3Under the mbar vacuum condition, methane is used as a reaction gas, argon is used as a process gas, wherein the flow rate of methane is 100sccm, and the flow rate of argon is 100 sccm. Adopting a silicon target as a sputtering target material, wherein the sputtering power is as follows: 5kw, reaction temperature is controlled at 280 ℃, and the thickness of the magnetron sputtering deposition on the substrate is about
Figure BDA0001171060890000081
The hard film of silicon carbide.
The hard film of silicon carbide measured in this example had a mohs hardness of 5, while soda lime glass had an original mohs hardness of 3. The silicon carbide hard film prepared by the embodiment is thinner, and the hardness of the surface of the glass can be obviously improved.
Example 6
Using soda-lime glass as substrate, placing soda-lime glass in cavity of magnetron sputtering equipment, 1 × 10-3Under the mbar vacuum condition, ethylene is used as a reaction gas, argon is used as a process gas, wherein the flow rate of ethylene is 100sccm, and the flow rate of argon is 350 sccm. Adopting a silicon target as a sputtering target material, wherein the sputtering power is as follows: 2kw, controlling the reaction temperature at 100 ℃, and the thickness of the magnetron sputtering deposition on the substrate is about
Figure BDA0001171060890000082
The hard film of silicon carbide.
The hard film of silicon carbide measured in this example had a mohs hardness of 6, while soda lime glass had an original mohs hardness of 3. The silicon carbide hard film prepared by the embodiment is thinner, and the hardness of the surface of the glass can be obviously improved.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (5)

1. A preparation method of a silicon carbide hard film is characterized by comprising the following steps:
providing a substrate; and
placing the substrate in a cavity of magnetron sputtering equipment, under the vacuum condition, taking organic gas containing 1-4 carbon atoms as reaction gas, taking gas containing argon as process gas, taking a silicon target as a sputtering target material, controlling the reaction temperature to be 100-300 ℃, and depositing a silicon carbide hard film on the substrate by magnetron sputtering;
the volume ratio of the reaction gas to the process gas is 0.4-4: 1;
the thickness of the hard silicon carbide film is
Figure FDA0002318787550000011
The following;
the percentage content of silicon in the silicon target is more than 99 percent;
in the operation of depositing the silicon carbide hard film on the substrate by magnetron sputtering, the sputtering power is 2 kW-5 kW;
the degree of vacuum under the vacuum condition is 1X 10-3mbar～5×10-3mbar。
2. The method for producing a silicon carbide hard film according to claim 1, wherein the organic gas having 1 to 4 carbon atoms is at least one selected from methane and acetylene.
3. The method of preparing a silicon carbide hard film according to claim 1 or 2, wherein the reaction gas is methane or acetylene, the process gas is argon, and the methane or acetylene accounts for 30 to 80% of the total volume of the process gas and the reaction gas.
4. The method for producing a silicon carbide hard film according to claim 1, wherein the substrate is a glass substrate.
5. A glass comprising a glass substrate and a hard silicon carbide film laminated on the glass substrate, wherein the hard silicon carbide film is produced by the method for producing a hard silicon carbide film according to any one of claims 1 to 4.
CN201611104056.7A 2016-12-05 2016-12-05 Preparation method of silicon carbide hard film and glass Active CN106521443B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611104056.7A CN106521443B (en) 2016-12-05 2016-12-05 Preparation method of silicon carbide hard film and glass

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611104056.7A CN106521443B (en) 2016-12-05 2016-12-05 Preparation method of silicon carbide hard film and glass

Publications (2)

Publication Number Publication Date
CN106521443A CN106521443A (en) 2017-03-22
CN106521443B true CN106521443B (en) 2020-04-21

Family

ID=58354867

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611104056.7A Active CN106521443B (en) 2016-12-05 2016-12-05 Preparation method of silicon carbide hard film and glass

Country Status (1)

Country Link
CN (1) CN106521443B (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105543795A (en) * 2015-12-18 2016-05-04 厦门大学 Growing method for polycrystalline silicon carbide thin film
CN105861986A (en) * 2016-03-31 2016-08-17 程海涛 Production process of metal matrix with IP black film layer and metal matrix thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103243304B (en) * 2013-05-14 2015-05-20 西南交通大学 Method for improving mechanical property on surface of metal workpiece

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105543795A (en) * 2015-12-18 2016-05-04 厦门大学 Growing method for polycrystalline silicon carbide thin film
CN105861986A (en) * 2016-03-31 2016-08-17 程海涛 Production process of metal matrix with IP black film layer and metal matrix thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"非晶碳化硅薄膜的光电性能";朱尧江等;《中国电子学会电子材料学专业学会编. 全国固体薄膜学术会论文集》;19900930;第47页第2-9行 *

Also Published As

Publication number Publication date
CN106521443A (en) 2017-03-22

Similar Documents

Publication Publication Date Title
Wu et al. Effects of magnetic field strength and deposition pressure on the properties of TiN films produced by high power pulsed magnetron sputtering (HPPMS)
Imai et al. Hydrogen-free fluorinated DLC films with high hardness prepared by using T-shape filtered arc deposition system
US9249499B2 (en) Coated article and method for making same
CN111364017B (en) Aluminum nitride film and preparation method and application thereof
TW201035350A (en) Sputtering target and process for producing same
Chen et al. Characterization of Ta–Si–N coatings prepared using direct current magnetron co-sputtering
CN111334794B (en) Modified film containing Ti transition layer and titanium-doped diamond-like carbon deposited on surface of substrate and method
US20090236217A1 (en) Capillaritron ion beam sputtering system and thin film production method
US20130157044A1 (en) Coated article and method for making same
US20120263941A1 (en) Coated article and method for making the same
CN106521443B (en) Preparation method of silicon carbide hard film and glass
KR100991770B1 (en) Method for depositing cbn thin film
Sasaki et al. Influence of hydrogen gas flow ratio on the properties of silicon-and nitrogen-doped diamond-like carbon films by plasma-enhanced chemical vapor deposition
KR20090020292A (en) Multi-layer thin film structure for providing metallic sense of polymer material and manufacturing method thereof
Ma et al. High-rate, room-temperature synthesis of amorphous silicon carbide films from organo-silicon in high-density helicon wave plasma
CN108315700A (en) The method that coating material and ion beam source deposition prepare coating material
CN110629174A (en) Method for preparing Ti-Al-N hard film by using pull-type nitrogen plasma enhanced reaction atmosphere environment
Khanna et al. Effects of deposition parameters on the structure of AlN coatings grown by reactive magnetron sputtering
Kang et al. Surface treatment of polycarbonate and polyethersulphone for SiNx thin film deposition
JP3931229B2 (en) Carbon oxide thin film and carbon oxynitride thin film and methods for producing these carbon oxide thin films
Tian et al. Deposition of cubic boron nitride films by anode layer linear ion source assisted radio frequency magnetron sputtering
TW201947053A (en) Method for enhancing adhesion of anti-fouling film
Ha et al. Control of stress and delamination in single and multi-layer carbon thin films prepared by cathodic arc and RF plasma deposition and implantation
Zhou et al. Catalytic effect of Al and AlN interlayer on the growth and properties of containing carbon films
Vassallo et al. Effects of nitrogen concentration on microstructure of tungsten coatings synthesized by plasma sputtering method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant