CN113293347A - Titanium-silicon hard composite coating and preparation method thereof - Google Patents

Titanium-silicon hard composite coating and preparation method thereof Download PDF

Info

Publication number
CN113293347A
CN113293347A CN202110364449.6A CN202110364449A CN113293347A CN 113293347 A CN113293347 A CN 113293347A CN 202110364449 A CN202110364449 A CN 202110364449A CN 113293347 A CN113293347 A CN 113293347A
Authority
CN
China
Prior art keywords
substrate
bonding layer
coating
titanium
vacuum
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.)
Pending
Application number
CN202110364449.6A
Other languages
Chinese (zh)
Inventor
李军明
韩秀全
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.)
Qingdao denai Nano Technology Co.,Ltd.
Original Assignee
Yingmaidun Nano Materials 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 Yingmaidun Nano Materials Co ltd filed Critical Yingmaidun Nano Materials Co ltd
Priority to CN202110364449.6A priority Critical patent/CN113293347A/en
Publication of CN113293347A publication Critical patent/CN113293347A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/024Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025Metallic sublayers
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641Nitrides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/26Vacuum evaporation by resistance or inductive heating of the source
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3464Sputtering using more than one target

Landscapes

  • 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 relates to the technical field of coating materials, in particular to a titanium-silicon hard composite coating and a preparation method thereof; the titanium-silicon-based composite material comprises a substrate, a bonding layer and a hard coating, wherein the bonding layer is a Ti metal bonding layer covered on the substrate, and the hard coating is a TiSiN coating covered on the Ti metal bonding layer; the titanium silicon hard composite coating prepared by the invention not only has good adhesive force, but also has good corrosion resistance and hardness; the prepared titanium silicon hard composite coating can protect the matrix and prolong the service life of the matrix.

Description

Titanium-silicon hard composite coating and preparation method thereof
Technical Field
The invention relates to the technical field of coating materials, in particular to a titanium-silicon hard composite coating and a preparation method thereof.
Background
Since the end of the twentieth century, with the continuous development of scientific technology, many novel materials with excellent comprehensive properties emerge in the field of material science. The surface coating technology is an important way to improve the performance of materials, and is gaining more and more attention in modern industrial production, and with the continuous development of modern industry, new design concept and manufacturing technology have more and more rigorous requirements on the hardness, high temperature resistance, corrosion resistance and corrosion resistance of materials. The coating technology can be adopted to coat the material with excellent corrosion resistance on the substrate, so that the corrosion resistance of the substrate material can be obviously improved, the service life of the substrate material can be obviously prolonged, the excellent toughness of the substrate and the high hardness of the coating are combined, the substrate material can adapt to severe environment, the application range of the material is greatly expanded, and the composite coating is a widely used coating and widely applied to surgical scissors, medical instruments, high-end door handles and the like which are contacted with human bodies.
However, although the traditional composite coating has certain hardness, the hardness performance is poor, the traditional composite coating does not have corrosion resistance, and the traditional composite coating also does not have good adhesion, so that the performance and the quality of the prepared composite coating are influenced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the titanium-silicon hard composite coating and the preparation method thereof, and the titanium-silicon hard composite coating prepared by the invention not only has good adhesive force, but also has good hardness and corrosion resistance; so that the quality of the prepared titanium silicon hard composite coating is effectively improved.
In order to achieve the purpose, the invention provides the following technical scheme:
a titanium silicon hard composite coating comprises a substrate and also comprises:
the substrate comprises a bonding layer and a hard coating, wherein the bonding layer is a Ti metal bonding layer covering the substrate, and the hard coating is a TiSiN coating covering the Ti metal bonding layer.
By adopting the technical scheme: according to the invention, the Ti metal bonding layer is used as the bonding layer, and the TiSiN coating is used as the hard coating to form the titanium-silicon hard composite coating, so that the prepared titanium-silicon hard composite coating has good corrosion resistance and hardness, can protect the matrix, and prolongs the service life of the matrix.
The invention is further configured to: the bonding layer is a Ti metal bonding layer with the thickness of 200-300nm, and the hard coating is a TiSiN coating with the thickness of 500-800 nm.
By adopting the technical scheme: the Ti metal bonding layer and the TiSiN coating are in a double-layer structure, so that the prepared titanium silicon hard composite coating has good corrosion resistance and hardness.
A preparation method of a titanium silicon hard composite coating comprises the following steps:
and S1, preparing the bonding layer on the substrate by adopting a vacuum evaporation mode.
And S2, further preparing the hard coating on the bonding layer by adopting a vacuum sputtering mode.
By adopting the technical scheme: according to the invention, the Ti metal bonding layer is prepared on the substrate in a vacuum evaporation mode, so that the bonding force between the TiSiN coating and the substrate is improved, and the TiSiN coating is more compact by adding Si element, so that the prepared titanium-silicon hard composite coating has good corrosion resistance and hardness.
The invention is further configured to: before the step S1, cleaning the substrate, where the substrate cleaning method is:
and I, putting a substrate to be cleaned into a water tank of an ultrasonic cleaner, and removing oxides on the surface of the substrate by using a detergent.
And II, removing grease on the surface of the substrate by using a cleaning solution.
And III, adopting a cleaning agent and a cleaning solution with absolute ethyl alcohol residues.
And IV, removing the absolute ethyl alcohol on the surface of the substrate by using deionized water.
And V, drying the cleaned substrate, and quickly putting the substrate into a vacuum chamber.
By adopting the technical scheme: according to the invention, the matrix is cleaned, so that oxides, grease and the like on the surface of the matrix can be removed, and the Ti metal bonding layer can be conveniently prepared on the matrix in the subsequent step.
The invention is further configured to: the cleaning agent is hydrofluoric acid.
By adopting the technical scheme: hydrofluoric acid can be used to remove oxides from the surface of the substrate.
The invention is further configured to: the cleaning solution is acetone.
By adopting the technical scheme: the acetone is used for cleaning various oil stains, dirt, grease and the like on the surface of a substrate.
The invention is further configured to: in step S1, the method for preparing the bonding layer on the substrate by vacuum evaporation includes:
s11, winding the Ti sheet on a heater of a vacuum coating machine.
And S12, pushing the dried substrate into a vacuum coating machine, and keeping the electrodes in close contact.
S13, vacuumizing the pressure in the vacuum coating machine to 5.0 x 10-4Pa。
And S14, starting a vacuum coating machine, melting the Ti sheet by a heater of the vacuum coating machine, evaporating and overflowing Ti, and condensing Ti atoms on the surface of the substrate in a linear motion to finish the preparation of the bonding layer on the substrate.
Wherein, after the substrate enters a vacuum coating machine, the substrate is kept to rotate continuously and uniformly, and the coating time is 20-30 min.
By adopting the technical scheme: according to the invention, the Ti metal bonding layer is prepared on the substrate, so that a transition effect is achieved, the residual stress between the TiSiN coating and the substrate is reduced, and the adhesion strength between the TiSiN coating and the substrate is increased.
The invention is further configured to: in step S2, the method for further preparing the hard coating on the bonding layer by using the vacuum sputtering method includes:
s21, the Ti target with the purity of 99.99% and the Si target with the purity of 99.99% are wiped clean by acetone, dried in the air and mounted on a target platform of a sputtering chamber.
S22, the substrate coated with the bonding layer is placed on a sample stage in the sputtering chamber.
S23, vacuumizing the pressure in the sputtering chamber to 5.0 x 10-4Pa, turning on a heating current to heat the sample table until the temperature of the substrate covered with the bonding layer is 200 ℃.
And S24, introducing argon and nitrogen into the sputtering chamber, sputtering the surface of the Ti target and the surface of the Si target, and depositing a TiSiN coating on the Ti metal bonding layer.
By adopting the technical scheme: the hardness and the corrosion resistance of the coating can be improved by adding the Si element, the matrix is protected, and the comprehensive mechanical property of the prepared coating is better by controlling the sputtering condition.
Advantageous effects
Compared with the known public technology, the technical scheme provided by the invention has the following beneficial effects:
1. according to the invention, the Ti metal bonding layer is used as the bonding layer, and the TiSiN coating is used as the hard coating to form the titanium-silicon hard composite coating, so that the prepared titanium-silicon hard composite coating has good corrosion resistance and hardness, can protect the matrix, and prolongs the service life of the matrix.
2. The Ti metal bonding layer is prepared on the substrate to play a transition role, when the temperature of the base is 200 ℃, the activity of Ti atoms on the substrate is enhanced, the crystal of the Ti metal bonding layer can be preferentially oriented, the residual stress between the TiSiN coating and the substrate is reduced, and the adhesion strength between the TiSiN coating and the substrate is increased.
3. The invention can improve the hardness and corrosion resistance of the coating by adding the Si element, protect the matrix and ensure that the prepared coating has better comprehensive mechanical property by controlling the sputtering condition.
Drawings
FIG. 1 is a schematic structural diagram of a titanium silicon hard composite coating.
Illustration of the drawings:
100. a substrate; 110. a bonding layer; 120. and (3) hard coating.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all 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.
The present invention will be further described with reference to the following examples.
Example 1
A titanium silicon hard composite coating comprising a substrate 100, further comprising:
the substrate 100 comprises a bonding layer 110 and a hard coating 120, wherein the bonding layer 110 is a Ti metal bonding layer covering the substrate 100, and the hard coating 120 is a TiSiN coating covering the Ti metal bonding layer.
The bonding layer 110 is a Ti metal bonding layer with a thickness of 200nm and the hard coating 120 is a TiSiN coating with a thickness of 500 nm.
A preparation method of a titanium silicon hard composite coating comprises the following steps:
s1, preparing the bonding layer 110 on the substrate 100 by vacuum evaporation.
S2, further preparing the hard coating layer 120 on the bonding layer 110 by vacuum sputtering.
Before preparing the bonding layer 110, cleaning the substrate 100, wherein the method for cleaning the substrate 100 comprises the following steps:
i, putting the substrate 100 to be cleaned into a water tank of an ultrasonic cleaner, and removing oxides on the surface of the substrate 100 by using a detergent.
And II, removing grease on the surface of the substrate 100 by using the cleaning solution.
And III, adopting a cleaning agent and a cleaning solution with absolute ethyl alcohol residues.
And IV, removing the absolute ethyl alcohol on the surface of the substrate 100 by using deionized water.
And V, drying the cleaned substrate 100 and quickly putting the substrate into a vacuum chamber.
The cleaning agent is hydrofluoric acid.
The cleaning solution is acetone.
The method for preparing the bonding layer 110 on the substrate 100 by adopting the vacuum evaporation mode comprises the following steps:
s11, winding the Ti sheet on a heater of a vacuum coating machine.
And S12, pushing the dried substrate 100 into a vacuum coating machine to keep the electrodes in close contact.
S13, vacuumizing the pressure in the vacuum coating machine to 5.0 x 10-4Pa。
And S14, starting a vacuum coating machine, melting the Ti sheet by a heater of the vacuum coating machine, evaporating and overflowing Ti, and condensing Ti atoms on the surface of the substrate in a linear motion to finish the preparation of the bonding layer 110 on the substrate 100.
Wherein, after the substrate 100 enters the vacuum coating machine, the substrate 100 keeps rotating uniformly and continuously, and the coating time is 20 min.
The method for further preparing the hard coating on the bonding layer by adopting a vacuum sputtering mode comprises the following steps:
s21, the Ti target with the purity of 99.99% and the Si target with the purity of 99.99% are wiped clean by acetone, dried in the air and mounted on a target platform of a sputtering chamber.
S22, the substrate 100 coated with the bonding layer 110 is placed on a sample stage in a sputtering chamber.
S23, vacuumizing the pressure in the sputtering chamber to 5.0 x 10-4Pa, the sample stage was heated by turning on the heating current to a temperature of 200 ℃ at the substrate 100 covered with the bonding layer 110.
And S24, introducing argon and nitrogen into the sputtering chamber, sputtering the surface of the Ti target and the surface of the Si target, and depositing a TiSiN coating on the Ti metal bonding layer.
Wherein the total pressure of nitrogen and argon entering the sputtering chamber is controlled to be 0.7Pa, the flow of nitrogen is controlled to be 110sccm, the flow of argon is controlled to be 60sccm, the current of the Si target is controlled to be 4A, the current of the Ti target is controlled to be 65A, and the deposition time is controlled to be 150 min.
Example 2
The titanium silicon hard composite coating and the preparation method provided by the embodiment are substantially the same as those of the embodiment 1, and the main differences are as follows: the bonding layer 110 is a Ti metal bonding layer with the thickness of 300nm, and the hard coating 120 is a TiSiN coating with the thickness of 800 nm;
coating a Ti metal bonding layer on the substrate 100 for 30 min;
depositing a TiSiN coating on the Ti metal bonding layer for 180 min;
comparative example 1
The titanium silicon hard composite coating and the preparation method provided by the embodiment are substantially the same as those of the embodiment 1, and the main differences are as follows: no Ti metal bonding layer is coated;
comparative example 2
The titanium silicon hard composite coating and the preparation method provided by the embodiment are substantially the same as those of the embodiment 1, and the main differences are as follows: no TiSiN coating is coated;
performance testing
Taking the titanium silicon hard composite coatings prepared in the examples 1-2 and the comparative examples 1-2, and detecting the relevant performance of the prepared titanium silicon hard composite coatings, wherein the detection method comprises the following steps:
1. the adhesion of each titanium-silicon hard composite coating is detected according to SJ 20130-;
table 1 adhesion detection results of titanium silicon hard composite coatings
Test items Adhesion detection results
Example 1 Is not separated from the matrix
Example 2 Is not separated from the matrix
Comparative example 1 Separated from the substrate
Comparative example 2 Separated from the substrate
2. Respectively detecting the hardness of each titanium-silicon hard composite coating according to the national standard GB/T18449.1-2009, and recording the obtained data in Table 2;
3. respectively detecting the corrosion resistance of the titanium-silicon hard composite coatings according to the national standard GB/T5499-1986, and recording the obtained data in a table 2;
TABLE 2 hardness and Corrosion resistance test results for Ti-Si hard composite coatings
Test items Hardness test results Corrosion rate
Example 1 ≥3800 0.15%
Example 2 ≥3800 0.17%
Comparative example 1 <2500 10%
Comparative example 2 <2500 16%
Through analyzing the relevant data in the tables, the titanium silicon hard composite coating prepared by the method has good adhesive force, and good hardness and corrosion resistance. Therefore, the titanium-silicon hard composite coating and the preparation method thereof have wider market prospect and are more suitable for popularization.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.

Claims (8)

1. The titanium-silicon hard composite coating comprises a substrate and is characterized by further comprising:
the substrate comprises a bonding layer and a hard coating, wherein the bonding layer is a Ti metal bonding layer covering the substrate, and the hard coating is a TiSiN coating covering the Ti metal bonding layer.
2. The titanium silicon hard composite coating according to claim 1, wherein: the bonding layer is a Ti metal bonding layer with the thickness of 200-300nm, and the hard coating is a TiSiN coating with the thickness of 500-800 nm.
3. The preparation method of the titanium-silicon hard composite coating is characterized by comprising the following steps:
s1, preparing a bonding layer on the substrate in a vacuum evaporation mode;
and S2, further preparing the hard coating on the bonding layer by adopting a vacuum sputtering mode.
4. The method for preparing the titanium-silicon hard composite coating according to claim 3, wherein before the step S1, the substrate is cleaned by the following steps:
putting a substrate to be cleaned into a water tank of an ultrasonic cleaner, and removing oxides on the surface of the substrate by using a detergent;
II, removing grease on the surface of the substrate by using cleaning fluid;
III, adopting a cleaning agent and a cleaning solution with absolute ethyl alcohol residues;
IV, removing absolute ethyl alcohol on the surface of the substrate by using deionized water;
and V, drying the cleaned substrate, and quickly putting the substrate into a vacuum chamber.
5. The method for preparing a titanium silicon hard composite coating according to claim 4, wherein the method comprises the following steps: the cleaning agent is hydrofluoric acid.
6. The method for preparing a titanium silicon hard composite coating according to claim 4, wherein the method comprises the following steps: the cleaning solution is acetone.
7. The method for preparing a titanium silicon hard composite coating according to claim 3, wherein the method comprises the following steps: in step S1, the method for preparing the bonding layer on the substrate by vacuum evaporation includes:
s11, winding Ti sheets on a heater of a vacuum coating machine;
s12, pushing the dried substrate into a vacuum coating machine to keep the electrodes in close contact;
s13, vacuumizing the pressure in the vacuum coating machine to 5.0 x 10-4Pa;
S14, starting a vacuum coating machine, melting Ti sheets by a heater of the vacuum coating machine, evaporating and overflowing Ti, condensing Ti atoms on the surface of the substrate in a linear motion manner, and finishing the preparation of the bonding layer on the substrate;
wherein, after the substrate enters a vacuum coating machine, the substrate is kept to rotate continuously and uniformly, and the coating time is 20-30 min.
8. The method for preparing a titanium silicon hard composite coating according to claim 3, wherein the method comprises the following steps: in step S2, the method for further preparing the hard coating on the bonding layer by using the vacuum sputtering method includes:
s21, wiping the Ti target with the purity of 99.99 percent and the Si target with the purity of 99.99 percent clean by acetone, airing and installing on a target platform of a sputtering chamber;
s22, placing the substrate covered with the bonding layer on a sample table in a sputtering chamber;
s23, vacuumizing the pressure in the sputtering chamber to 5.0 x 10-4Pa, opening heating current to heat the sample table until the temperature of the substrate covered with the bonding layer is 200 ℃;
s24, introducing argon and nitrogen into the sputtering chamber, sputtering the Ti target surface and the Si target surface, and depositing a TiSiN coating on the Ti metal bonding layer;
wherein the total pressure of nitrogen and argon entering the sputtering chamber is controlled to be 0.7Pa, the flow rate of nitrogen is controlled to be 110sccm, the flow rate of argon is controlled to be 60sccm, the current of the Si target is controlled to be 4A, the current of the Ti target is controlled to be 65A, and the deposition time is controlled to be 150-180 min.
CN202110364449.6A 2021-04-05 2021-04-05 Titanium-silicon hard composite coating and preparation method thereof Pending CN113293347A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110364449.6A CN113293347A (en) 2021-04-05 2021-04-05 Titanium-silicon hard composite coating and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110364449.6A CN113293347A (en) 2021-04-05 2021-04-05 Titanium-silicon hard composite coating and preparation method thereof

Publications (1)

Publication Number Publication Date
CN113293347A true CN113293347A (en) 2021-08-24

Family

ID=77319394

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110364449.6A Pending CN113293347A (en) 2021-04-05 2021-04-05 Titanium-silicon hard composite coating and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113293347A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114875271A (en) * 2022-05-05 2022-08-09 广东工业大学 Non-stick coating and application and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103510061A (en) * 2013-10-12 2014-01-15 萨姆森涂层纳米科技(上海)有限公司 Method for preparing high-rigidity and high-elasticity modulus TiSiN protection coating
CN204840841U (en) * 2015-03-31 2015-12-09 广州今泰科技股份有限公司 Blue ceramic golf push rod

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103510061A (en) * 2013-10-12 2014-01-15 萨姆森涂层纳米科技(上海)有限公司 Method for preparing high-rigidity and high-elasticity modulus TiSiN protection coating
CN204840841U (en) * 2015-03-31 2015-12-09 广州今泰科技股份有限公司 Blue ceramic golf push rod

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114875271A (en) * 2022-05-05 2022-08-09 广东工业大学 Non-stick coating and application and preparation method thereof
CN114875271B (en) * 2022-05-05 2023-05-12 广东工业大学 Non-stick coating, application and preparation method thereof

Similar Documents

Publication Publication Date Title
CN109735803B (en) TiSiYN multi-component composite gradient cutter coating and preparation method thereof
CN113293347A (en) Titanium-silicon hard composite coating and preparation method thereof
TWI503430B (en) Coated article and method for making the same
CN111321380A (en) Super-hydrophobic diamond-like composite layer structure and preparation method thereof
US8703287B2 (en) Coated article and method for making the same
CN105779943A (en) Method of preparing hydrophobic membrane through physical vapor deposition of fluoroalkyl silane
US20130029174A1 (en) Coated article and method for making the same
US8715822B2 (en) Coated article and method for making the same
CN110438421B (en) Aluminum alloy material and aluminum alloy solution treatment and PVD coating synchronous strengthening method
EP1856004A1 (en) Substrate for hydrophobic coating
US20120141826A1 (en) Coated article and method for making the same
US20200347490A1 (en) Metal surface protective layer and preparation method thereof
US20120213989A1 (en) Coated glass article and method for manufacturing same
CN114369794A (en) Process for plating wear-resistant film on surface of high polymer material and wear-resistant film prepared by process
US20120114967A1 (en) Coated article and method for making the same
US8691380B2 (en) Coated article and method for making the same
US8691379B2 (en) Coated article and method for making the same
US20120077009A1 (en) Coating, article coated with coating, and method for manufacturing article
US20120148869A1 (en) Coated article and method for making the same
US20120141827A1 (en) Coated article and method for making the same
US8709594B2 (en) Coated article and method for making the same
US8722183B2 (en) Coated article and method for making same
CN113278920A (en) DLC (diamond-like carbon) coating and preparation method thereof
CN112359321B (en) Kitchen cutter and forming method of hard film of cutter
CN110484861B (en) Magnesium alloy material and magnesium alloy solution treatment and PVD coating synchronous strengthening method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right

Effective date of registration: 20220112

Address after: 266000 East Room 101, building 3, zone B, Yuanchuang international Blue Bay Creative Park, No. 31 Xinye Road, high tech Zone, Qingdao, Shandong

Applicant after: Qingdao denai Nano Technology Co.,Ltd.

Address before: 266000 room C2-1, Zone C, Qingdao Institute of industrial technology, No. 17, Songyuan Road, high tech Zone, Qingdao, Shandong

Applicant before: Yingmaidun nano materials Co.,Ltd.

TA01 Transfer of patent application right
RJ01 Rejection of invention patent application after publication

Application publication date: 20210824

RJ01 Rejection of invention patent application after publication