CN115233197B - Titanium nitride plating diamond and production process thereof - Google Patents

Titanium nitride plating diamond and production process thereof Download PDF

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CN115233197B
CN115233197B CN202210949108.XA CN202210949108A CN115233197B CN 115233197 B CN115233197 B CN 115233197B CN 202210949108 A CN202210949108 A CN 202210949108A CN 115233197 B CN115233197 B CN 115233197B
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diamond
titanium
titanium nitride
parts
powder
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CN115233197A (en
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张风岭
吴定雨
卢蓓蓓
兰帅锋
赵静
戚燕杰
杨怀建
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Zhongnan Diamond Co Ltd
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Zhongnan Diamond Co Ltd
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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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • 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
    • C23C14/0641—Nitrides
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation

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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)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Polishing Bodies And Polishing Tools (AREA)

Abstract

The invention relates to a production process for plating a titanium nitride film on the surface of diamond, which comprises the following steps: 1) Uniformly mixing absolute ethyl alcohol, butanol and glycerol according to a mass ratio to prepare an adhesive; 2) Mixing titanium trichloride, titanium powder and titanium hydride uniformly according to the mass ratio to prepare powder; 3) Cleaning, impurity removing and drying the titanized diamond; 4) Uniformly mixing the titanized diamond, the adhesive and the powder according to the mass ratio; 5) Heating the mixed raw materials for 3-6h under the nitrogen atmosphere; 6) The titanium nitride plating diamond can be obtained after ball milling and sieving. The invention designs and improves the diamond surface coating, and the titanium nitride coating has certain ceramic brittleness, so that the cutting edge of the diamond can be quickened, and the cutting and grinding efficiency of a diamond tool can be improved. In addition, the titanium nitride coating has good conductivity, basically meets the requirement of electroplating, can replace the process of chemical nickel plating before diamond electroplating, reduces the cost and is environment-friendly.

Description

Titanium nitride plating diamond and production process thereof
Technical Field
The invention belongs to the technical field of film plating, and particularly relates to titanium nitride plating diamond and a production process thereof, namely, a titanium nitride film is plated on the surface of the titanium plating diamond.
Background
The surface of the diamond is coated with a layer of film, so that the interfacial bonding capability of the diamond and a matrix can be enhanced, and the wear resistance and cutting capability of the diamond tool are improved. In the diamond electroplating industry, since diamond is not conductive, it is generally necessary to first form a conductive nickel coating on the surface of diamond (or titanium-plated diamond) by using an electroless plating method, and then electroplating (nickel plating, copper plating, etc.) is performed. The use of electroless plating not only has higher production cost, but also causes environmental pollution.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the titanium nitride-plated diamond, which utilizes the brittleness of titanium nitride ceramics to improve the service efficiency of a diamond grinding tool on one hand and utilizes titanium nitride with better conductivity to replace a conductive nickel plating layer of chemical plating on the other hand. When the diamond electroplating nickel is carried out, the current value of the titanium nitride plating diamond basically reaches 80-90% of that of the electroless plating diamond under the same voltage condition. Therefore, the conductivity of the titanium nitride-plated diamond can completely meet the electroplating requirement.
The invention also provides a production process of the titanium nitride plated diamond.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a titanium nitride-plated diamond, which is plated with a titanium nitride layer on the surface of the titanium nitride-plated diamond; namely, a Ti film is plated on the surface of the diamond, and the surface of the Ti film is a TiN film.
The production process of the titanium nitride plated diamond comprises the steps of uniformly mixing titanium plated diamond, adhesive and powder according to mass ratio to prepare mixed raw materials, and heating the mixed raw materials in nitrogen atmosphere; the method specifically comprises the following steps:
1) Preparation of an adhesive: uniformly mixing absolute ethyl alcohol, butanol and glycerol to obtain an adhesive for later use;
2) Powder preparation: uniformly mixing titanium trichloride, titanium powder and titanium hydride to obtain powder for later use;
3) Washing the titanized diamond to remove impurities and drying:
4) Mixing the raw materials: uniformly mixing the titanized diamond, the powder and the adhesive to obtain a mixed raw material;
5) Negative pressure evaporation: placing the mixed raw materials into a vacuum heating furnace, vacuumizing until the pressure is lower than 0.1 Pa, and heating at 400-600 ℃ for 1-2h; then raising the temperature to 750-900 ℃, intermittently and repeatedly charging nitrogen, and then controlling the pressure of the nitrogen to 10% 3 ～10 4 Maintaining at 750-900 deg.C for 3-6 hr under Pa;
6) Grinding and sieving: and ball milling (generally for 10-20 min) and sieving the reacted diamond to obtain the titanium nitride plated diamond.
Specifically, in the step 1), 80-90 parts of absolute ethyl alcohol, 10-20 parts of butanol and 5-10 parts of glycerol are uniformly mixed according to the mass ratio.
Further, in the step 2), 10-30 parts of titanium trichloride, 20-50 parts of titanium powder and 20-50 parts of titanium hydride are uniformly mixed according to the mass ratio.
Further, the washing and impurity removing steps in the step 3) are specifically as follows: placing the titanized diamond in deionized water, carrying out ultrasonic oscillation treatment for 20-60 min by using an ultrasonic machine, and then drying the titanized diamond.
Specifically, in the step 4), 90 to 120 parts of titanized diamond, 25 to 35 parts of powder and 1 to 5 parts of adhesive are uniformly mixed according to the mass ratio.
Specifically, in the step 5), the nitrogen gas is filled intermittently for a plurality of times, so that the nitrogen gas and the activated titanium powder are prevented from excessively reacting, and diamond is burnt. The negative pressure evaporation in the step 5) is specifically as follows: heating at 400-600deg.C for 1-2 hr after vacuum pressure is lower than 0.1 Pa, heating to 750-900deg.C, and heating under nitrogen pressure of 10 3 ～10 4 Heating under Pa for 3-6h.
Further preferably, the particle size of the titanium powder and titanium hydride is not less than 500 mesh, for example, 500 mesh, 600 mesh, 700 mesh, etc.
The invention provides the titanium nitride plated diamond produced by the process.
The invention is suitable for the field of diamond plating, and the superiority and practicability are mainly shown in the following aspects:
1) The conductivity of the titanium nitride diamond reaches 80-90% of that of the electroless gold diamond, so that the requirement of diamond electroplating is met, and the titanium nitride diamond can replace the diamond electroless plating conductive nickel plating layer;
2) The titanium nitride diamond innovatively uses a vacuum evaporation technology, has simple process and lower cost, and is beneficial to batch production; compared with chemical gold-plated diamond, the method not only reduces the cost, but also is environment-friendly;
3) The titanium nitride coating has ceramic brittleness, which is beneficial to the rapid toughness of diamond;
4) The diamond coating is designed and improved, the diamond/titanium nitride coatings are sequentially arranged, the transition between the coatings is uniform, and the binding force is strong.
Drawings
FIG. 1 is a schematic diagram of a structure of a titanium nitride-plated diamond of the present invention, wherein a Ti film is plated on the surface of the diamond, and a TiN film is formed on the surface of the Ti film;
FIG. 2 is a schematic view of a titanium nitride coated diamond product of the present invention having a particle size of 40/45;
FIG. 3 is a graph showing the composition analysis of the surface coating of the titanium nitride coated diamond of the present invention.
Detailed Description
The following describes the technical scheme of the present invention in further detail with reference to examples, but the scope of the present invention is not limited thereto.
In the following examples, all materials used, unless otherwise specified, were commercially available products which were commercially available as they are.
Example 1
A titanium nitride-plated diamond is provided, wherein a titanium nitride layer is plated on the surface of the titanium-plated diamond, namely, a Ti film is plated on the surface of the diamond, and the surface of the Ti film is a TiN film as shown in figure 1.
The production process of the titanium nitride plated diamond specifically comprises the following steps:
1) Preparation of an adhesive: uniformly mixing 85 parts of absolute ethyl alcohol, 15 parts of butanol and 8 parts of glycerol according to the mass ratio to obtain an adhesive for later use;
2) Powder preparation: uniformly mixing 15 parts of titanium trichloride, 30 parts of titanium powder and 30 parts of titanium hydride to obtain powder for later use;
3) Washing the titanized diamond to remove impurities and drying: placing the titanized diamond in deionized water, carrying out ultrasonic oscillation treatment for 30-40min by using an ultrasonic machine, and then placing the titanized diamond in a drying oven to be dried for 3h at 100 ℃;
4) Mixing the raw materials: uniformly mixing 105 parts of titanized diamond, 30 parts of powder and 3 parts of adhesive according to the mass ratio to obtain a mixed raw material; the granularity of titanium powder and titanium hydride in the powder is 500 meshes;
5) Negative pressure evaporation: will bePlacing the mixed raw materials into a vacuum heating furnace, vacuumizing to below 0.1 Pa, and heating at 500 ℃ for 2 hours; then the temperature of the vacuum furnace is increased to 870 ℃, and nitrogen is intermittently injected for a plurality of times, so that the air pressure in the furnace is maintained at 10 percent 3 -10 4 Holding at 870 ℃ for 4 hours after Pa;
6) Grinding and sieving: ball milling the reacted titanium-plated diamond for 15min, and screening to obtain the titanium-plated diamond.
FIG. 2 is a schematic view showing the titanium nitride coated diamond product of this example, showing a particle size of 40/45.
Fig. 3 shows analysis of the composition of the surface coating of the titanium nitride coated diamond of this example, and shows that: the coating layer has a TiN component.
Example 2
A titanium nitride-plated diamond is provided, wherein a titanium nitride layer is plated on the surface of the titanium nitride-plated diamond.
The production process of the titanium nitride plated diamond specifically comprises the following steps:
1) Preparation of an adhesive: uniformly mixing 80 parts of absolute ethyl alcohol, 20 parts of butanol and 10 parts of glycerol according to the mass ratio to obtain an adhesive for later use;
2) Powder preparation: uniformly mixing 10 parts of titanium trichloride, 25 parts of titanium powder and 40 parts of titanium hydride to obtain powder for later use;
3) Washing the titanized diamond to remove impurities and drying: placing the titanized diamond in deionized water, carrying out ultrasonic oscillation treatment for 30-40min by using an ultrasonic machine, and then placing the titanized diamond in a drying oven to be dried for 3h at 100 ℃;
4) Mixing the raw materials: uniformly mixing 95 parts of titanized diamond, 35 parts of powder and 5 parts of adhesive according to the mass ratio to obtain a mixed raw material; the granularity of titanium powder and titanium hydride in the powder is 500 meshes;
5) Negative pressure evaporation: placing the mixed raw materials into a vacuum heating furnace, vacuumizing to below 0.1 Pa, and heating at 500 ℃ for 2 hours; then the temperature of the vacuum furnace is increased to 800 ℃, and nitrogen is intermittently injected for a plurality of times, so that the air pressure in the furnace is maintained at 10 percent 3 -10 4 Maintaining at 800 ℃ for 5 hours after Pa;
6) Grinding and sieving: ball milling the reacted titanium-plated diamond for 20min, and screening to obtain the titanium-plated diamond.
Example 3
A titanium nitride-plated diamond is provided, wherein a titanium nitride layer is plated on the surface of the titanium nitride-plated diamond.
The production process of the titanium nitride plated diamond specifically comprises the following steps:
1) Preparation of an adhesive: uniformly mixing 90 parts of absolute ethyl alcohol, 10 parts of butanol and 5 parts of glycerol according to the mass ratio to obtain an adhesive for later use;
2) Powder preparation: uniformly mixing 30 parts of titanium trichloride, 20 parts of titanium powder and 25 parts of titanium hydride to obtain powder for later use;
3) Washing the titanized diamond to remove impurities and drying: placing the titanized diamond in deionized water, carrying out ultrasonic oscillation treatment for 30-40min by using an ultrasonic machine, and then placing the titanized diamond in a drying oven to be dried for 3h at 100 ℃;
4) Mixing the raw materials: uniformly mixing 115 parts of titanized diamond, 25 parts of powder and 2 parts of adhesive according to the mass ratio to obtain a mixed raw material; the granularity of titanium powder and titanium hydride in the powder is 500 meshes;
5) Negative pressure evaporation: placing the mixed raw materials into a vacuum heating furnace, vacuumizing to below 0.1 Pa, and heating at 500 ℃ for 2 hours; then the temperature of the vacuum furnace is increased to 900 ℃, and nitrogen is intermittently injected for a plurality of times, so that the air pressure in the furnace is maintained at 10 percent 3 -10 4 Maintaining at 900 ℃ for 3 hours after Pa;
6) Grinding and sieving: ball milling the reacted titanium-plated diamond for 20min, and screening to obtain the titanium-plated diamond.
Application test
The electroless gold diamond plating current is compared with the titanium nitride diamond of example 1 of the present invention at the same plating voltage as shown in the following table. The results are shown according to the table comparison: the conductivity of the titanium nitride diamond reaches 80-90% of that of the electroless plating diamond, meets the requirement of direct electroplating, and can replace electroless plating to carry out electroplating process.
In conclusion, the invention designs and improves the diamond surface coating, and the titanium nitride coating has certain ceramic brittleness, so that the cutting edge of the diamond can be quickened, and the cutting and grinding efficiency of the diamond tool can be improved. In addition, the titanium nitride coating has good conductivity, basically meets the requirement of electroplating, can replace the process of chemical nickel plating before diamond electroplating, reduces the cost and is environment-friendly.

Claims (6)

1. The production process of the titanium nitride plating diamond is characterized by comprising the following steps:
1) Preparation of an adhesive: uniformly mixing absolute ethyl alcohol, butanol and glycerol to obtain an adhesive for later use;
2) Powder preparation: uniformly mixing titanium trichloride, titanium powder and titanium hydride to obtain powder for later use;
3) Washing the titanized diamond to remove impurities and drying;
4) Mixing the raw materials: uniformly mixing the titanized diamond, the powder and the adhesive to obtain a mixed raw material;
5) Negative pressure evaporation: placing the mixed raw materials into a vacuum heating furnace, vacuumizing to a pressure lower than 0.1 Pa, heating at 400-600deg.C for 1-2 hr, increasing the temperature to 750-900deg.C, intermittently introducing nitrogen gas for several times, and maintaining the nitrogen gas pressure at 10 3 ～10 4 Maintaining at 750-900 deg.C for 3-6 hr under Pa;
6) Grinding and sieving: and ball milling and sieving the reacted diamond to obtain the titanium nitride plated diamond.
2. The process for producing titanium nitride-plated diamond according to claim 1, wherein in step 1), 80 to 90 parts of absolute ethyl alcohol, 10 to 20 parts of butanol and 5 to 10 parts of glycerol are uniformly mixed according to a mass ratio.
3. The process for producing titanium nitride-plated diamond according to claim 1, wherein in step 2), 10 to 30 parts of titanium trichloride, 20 to 50 parts of titanium powder and 20 to 50 parts of titanium hydride are uniformly mixed according to the mass ratio.
4. The process for producing titanium nitride-plated diamond according to claim 1, wherein in step 3), the cleaning and impurity removal steps are as follows: and placing the titanized diamond in deionized water for ultrasonic oscillation treatment for 20-60 min.
5. The process for producing titanium nitride coated diamond according to claim 1, wherein in step 4), 90 to 120 parts of titanium coated diamond, 25 to 35 parts of powder and 1 to 5 parts of adhesive are uniformly mixed according to the mass ratio.
6. A process for producing titanium nitride coated diamond according to claim 3 wherein said titanium powder and titanium hydride have a particle size of not less than 500 mesh.
CN202210949108.XA 2022-08-09 2022-08-09 Titanium nitride plating diamond and production process thereof Active CN115233197B (en)

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CN116217270B (en) * 2022-12-26 2024-04-09 何思义 Production process of diamond film coated dielectric ball with surface of zirconia ball

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1109921A (en) * 1995-03-22 1995-10-11 樊联哲 Superhard film coating technique for diamond monocrystal
KR20140074081A (en) * 2012-12-07 2014-06-17 일진다이아몬드(주) Wire tool and method for manufactruing the same
CN107107206A (en) * 2014-10-29 2017-08-29 住友电气工业株式会社 Composite diamond body and composite diamond instrument
CN108315737A (en) * 2018-02-07 2018-07-24 上海三朗纳米技术有限公司 A kind of composite coating preparation process based on cutting tool
CN109023250A (en) * 2018-08-23 2018-12-18 中南钻石有限公司 A kind of nickel plating diamond and its production technology
CN109047775A (en) * 2018-08-23 2018-12-21 中南钻石有限公司 A kind of plating carbonization titanium diamond and its production technology

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1109921A (en) * 1995-03-22 1995-10-11 樊联哲 Superhard film coating technique for diamond monocrystal
KR20140074081A (en) * 2012-12-07 2014-06-17 일진다이아몬드(주) Wire tool and method for manufactruing the same
CN107107206A (en) * 2014-10-29 2017-08-29 住友电气工业株式会社 Composite diamond body and composite diamond instrument
CN108315737A (en) * 2018-02-07 2018-07-24 上海三朗纳米技术有限公司 A kind of composite coating preparation process based on cutting tool
CN109023250A (en) * 2018-08-23 2018-12-18 中南钻石有限公司 A kind of nickel plating diamond and its production technology
CN109047775A (en) * 2018-08-23 2018-12-21 中南钻石有限公司 A kind of plating carbonization titanium diamond and its production technology

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