CN111378926A - Novel H coating - Google Patents

Novel H coating Download PDF

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Publication number
CN111378926A
CN111378926A CN201811630536.6A CN201811630536A CN111378926A CN 111378926 A CN111378926 A CN 111378926A CN 201811630536 A CN201811630536 A CN 201811630536A CN 111378926 A CN111378926 A CN 111378926A
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coating
layer
thickness
alcr
bias voltage
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梁海洋
邓永琪
吴伟亮
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Suzhou Shineland Nano Technology Co ltd
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Suzhou Shineland Nano Technology Co ltd
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    • 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
    • C23C14/0682Silicides
    • 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
    • C23C14/022Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

In order to further improve the performance of the existing coating applied to high-speed steel or hard alloy, the invention provides a novel H coating, which comprises the following components: the substrate comprises a bonding layer 2 attached to the surface of a substrate 1 from inside to outside, and a modulation layer 31 and a functional layer 32 which repeat N cycles in sequence, wherein the bonding layer 2 is an AlCr coating with the thickness of 0.2-0.3um, and the modulation layer 31 is an AlCr coating with the thickness of 0.16-0.20 um; the functional layer 32 is a TiSi coating with a thickness of 0.05um, wherein the ratio of the amount of Ti to the amount of Si in the TiSi coating is 85: 15, in the modulation layer 31 and the functional layer 32 which are sequentially repeated for N periods, N is more than or equal to 4 and less than or equal to 6, N is a natural number, and the total thickness of the combined layer 2+ the modulation layer 31+ the functional layer 32 is 1.04-1.8 um; the method is characterized in that: the ratio of the amount of Al to Cr species in the AlCr coating is 64: 36.

Description

Novel H coating
Technical Field
The invention belongs to the technical field of surface treatment, relates to a surface treatment technology of high-speed steel or hard alloy, and particularly relates to a nano-structured H coating of the high-speed steel or the hard alloy.
Background
In order to prolong the service life of high-speed steel or hard alloy, the surface of the high-speed steel or hard alloy is strengthened by nitriding, metal infiltration, electroplating, chemical plating and other methods at home and abroad at present. But the treatment process has a certain degree of contamination and low hardness.
Physical Vapor Deposition (PVD) is an advanced engineering technology developed on the basis of multiple disciplines such as modern physics, chemistry, materials science, and electronics. The method is a process of depositing a target material (a plated film material) on the surface of a substrate (a workpiece needing to be plated) through a physical process in a vacuum environment. The physical vapor deposition technology is a hot point of research in recent years for manufacturing hard ceramic coatings on the surfaces of cheap metal materials, and the hard ceramic coatings are successfully applied to tools and dies, so that the problems of abrasion and high temperature resistance of cutters are solved. Arc ion plating and magnetron sputtering are the most common techniques for producing hard ceramic coatings in PVD processes.
At present, the structure of a coating with better effect applied to a coating of high-speed steel or hard alloy sequentially comprises the following steps from inside to outside: the substrate comprises a bonding layer attached to the surface of the substrate, and a modulation layer and a functional layer which are sequentially repeated for N periods, wherein the bonding layer is an AlCr coating, the thickness of the AlCr coating is 0.2-0.3um, and the mass ratio of Al to Cr of the AlCr coating is 64: 36; the modulation layer is an AlCr coating with the thickness of 0.16-0.20um, wherein the ratio of the amount of Al to Cr substances of the AlCr coating is 64: 36; the functional layer is a TiSi coating with the thickness of 0.05um, wherein the quantity ratio of Ti to Si in the TiSi coating is 85: 15; in the modulating layer and the functional layer which are sequentially repeated for N periods, N is more than or equal to 4 and less than or equal to 6, N is a natural number, and the total thickness of the combined layer, the modulating layer and the film layer of the functional layer is 1.04-1.8 um.
However, the above coating still has room for improvement, and the stress of the above coating is relatively large and the friction coefficient is large in the burst test, which affects the service life of the coating.
Disclosure of Invention
In view of the above, in order to further improve the performance of the existing coating applied to high-speed steel or hard alloy, the invention provides a novel H coating, which improves the lubricity and corrosion resistance of the AlCr coating and simultaneously ensures the hardness of the AlCr coating by changing the ratio of the amounts of Al and Cr substances of the conventional AlCr coating applied to the bonding layer and the modulation layer of the coating of high-speed steel or hard alloy; in the whole process of coating treatment, the compactness of the AlCr coating is improved by increasing a certain bias voltage, so that the performance of a new AlCr coating is ensured. Meanwhile, the thickness of the AlCr coating is ensured by prolonging the processing time of the AlCr coating. Through the treatment, the finally prepared novel H coating has the advantages of small internal stress and 10% service life improvement.
A novel H-coating, comprising: the substrate comprises a bonding layer 2 attached to the surface of a substrate 1 from inside to outside, and a modulation layer 31 and a functional layer 32 which repeat N cycles in sequence, wherein the bonding layer 2 is an AlCr coating with the thickness of 0.2-0.3um, and the modulation layer 31 is an AlCr coating with the thickness of 0.16-0.20 um; the functional layer 32 is a TiSi coating with a thickness of 0.05um, wherein the ratio of the amount of Ti to the amount of Si in the TiSi coating is 85: 15, in the modulation layer 31 and the functional layer 32 which are sequentially repeated for N periods, N is more than or equal to 4 and less than or equal to 6, N is a natural number, and the total thickness of the combined layer 2+ the modulation layer 31+ the functional layer 32 is 1.04-1.8 um; the method is characterized in that: the ratio of the amount of Al to Cr species in the AlCr coating is 64: 36.
a novel H coating comprises the following treatment processes:
A. vacuumizing and heating: firstly, putting a substrate 1 material into vacuum coating equipment, and adjusting the vacuum degree of the equipment to 6 x 10-5mbar, heating for about 1h, so that the temperature is raised to 460-480 ℃.
B. Cleaning the substrate 1: the ion bombardment is carried out, the bias voltage is 10V, the operating frequency of the molecular pump is reduced to 72 percent from 100 percent during initial vacuumizing, high-purity hydrogen (H) with the purity of 99.999 percent and high-purity argon (Ar) with the purity of 99.999 percent are simultaneously introduced into the equipment, the flow rate of the hydrogen (H) is 50-200sccm, the flow rate of the argon (Ar) is 50sccm, and the ventilation time is 20-30 min. Then, high-purity argon (Ar) was introduced into the apparatus at a bias voltage of 200V at a flow rate of 50sccm for a period of 20 to 30 min.
C. Plating the bonding layer 2: the frequency of the molecular pump was 72%, and the apparatus was filled with nitrogen (N) so that the pressure in the apparatus was 2.5 x 10-2mbar, single opening of AlCr64/36 target, arc current of 150A, bias voltage of 40-150V, and coating time of 13.6-16.8 min. Compared with the traditional coating process, the bias voltage is increased from 120V to 150V, and the coating time is increased from 13-16min to 13.6-16.8min, so that the hardness caused by reducing the Al content in the AlCr coating can be effectively adjustedInsufficient hardness, thickness and energy of the bonding layer 2 are ensured.
D. Plating preparation layer 31: the frequency of the molecular pump was 72%, and the apparatus was filled with nitrogen (N) so that the pressure in the apparatus was 4 x 10-2mbar, single opening of AlCr64/36 target, arc current of 180A, bias voltage of 150V, and coating time of 8.4-12.6 min. Compared with the traditional coating process, the bias voltage is increased from 120V to 150V, and the coating time is increased from 8-12min to 8.4-12.6min, so that the problem of insufficient hardness caused by reduction of Al content in the AlCr coating can be effectively solved, and the hardness, thickness and energy of the prepared layer 31 are ensured.
E. Plating of the functional layer 32: the frequency of the molecular pump was 72%, and nitrogen (N) was flushed into the apparatus, so that the pressure in the apparatus was 4 x 10-2mbar, single-opening TiSi85/15 target, arc current of 200A, bias voltage of 40V, and coating time of 3 min.
F. And D, the step E and the step D are combined, and the cycle work is carried out for 4-6 periods, so that the total thickness of the combined layer 2+ the modulation layer 31+ the functional layer 32 is 1.04-1.8 um.
G. Finally, the temperature is reduced to below 200 ℃ before the furnace is discharged.
The coefficient of friction of the conventional coating with the metal is 0.2 and that of the H coating of the invention is 0.15-0.2, compared to the conventional coating. The indentation method is adopted to test the stress of the coating, the coating bursts when the traditional coating is 100N, and the coating bursts when the H coating is 130N, so that the coating has small stress and large binding force. And under the same working condition, the service life of the prepared H coating is prolonged by 10 percent compared with that of the traditional coating.
The novel H coating prepared by the method has the hardness of 3300V, the binding force can reach the HF1 standard by adopting a Rockwell hardness tester for measurement, the friction coefficient with metal is 0.15-0.2, and the heat-resistant temperature is 900 ℃.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the scope of the claims thereto. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Drawings
FIG. 1 is a schematic cross-sectional structural view of a PVD coated high speed steel or cemented carbide of the present invention.
Description of the main element symbols:
Figure BDA0001928886790000031
Figure BDA0001928886790000041
the following detailed description will further illustrate the invention in conjunction with the above-described figures.
Specific embodiment example 1:
the PVD surface treated high speed steel or hard alloy comprises a substrate 1, a bonding layer 2 attached to the surface of the substrate 1 from inside to outside, a modulation layer 31 and a functional layer 32 which are sequentially repeated for 5 cycles. The bonding layer 2 is an AlCr coating with the thickness of 0.2um, wherein the mass ratio of Al to Cr of the AlCr coating is 64: 36; the modulation layer 31 is an AlCr coating with a thickness of 0.18um, wherein the ratio of the amounts of Al and Cr substances in the AlCr coating is 64: 36; the functional layer 32 is a TiSi coating with a thickness of 0.05um, wherein the ratio of the amount of Ti to the amount of Si in the TiSi coating is 85: 15. the total thickness of the film layers of the bonding layer 2+ the modulation layer 31+ the functional layer 32 was 1.35 um.
The hardness of the high-speed steel and hard alloy coating subjected to PVD surface treatment is 3300V, the binding force can reach the HF1 standard by adopting a Rockwell hardness tester for measurement, the friction coefficient with metal is 0.16, the heat-resistant temperature is 900 ℃, and the coating is cracked at 130N by adopting an indentation method for testing.
The preparation process comprises the following steps:
A. vacuumizing and heating: firstly, the substrate 1 material is placed in a vacuum coating device, and the vacuum of the device is adjustedDegree of 6 x 10-5mbar, heating for about 1h, so that the temperature is raised to 460-480 ℃.
B. Cleaning the substrate 1: the ion bombardment is carried out, the bias voltage is 10V, the operating frequency of the molecular pump is reduced to 72 percent from 100 percent during initial vacuumizing, high-purity hydrogen (H) with the purity of 99.999 percent and high-purity argon (Ar) with the purity of 99.999 percent are simultaneously introduced into the equipment, the flow rate of the hydrogen (H) is 50-200sccm, the flow rate of the argon (Ar) is 50sccm, and the ventilation time is 20-30 min. Then, high-purity argon (Ar) was introduced into the apparatus at a bias voltage of 200V at a flow rate of 50sccm for a period of 20 to 30 min.
C. Plating the bonding layer 2: the frequency of the molecular pump was 72%, and the apparatus was filled with nitrogen (N) so that the pressure in the apparatus was 2.5 x 10-2mbar, single opening of AlCr64/36 target, arc current of 150A, bias voltage of 40-150V, and coating time of 17.8 min.
D. Plating preparation layer 31: the frequency of the molecular pump was 72%, and the apparatus was filled with nitrogen (N) so that the pressure in the apparatus was 4 x 10-2mbar, single opening of AlCr64/36 target, arc current of 180A, bias voltage of 150V, and coating time of 10.5 min.
E. Plating of the functional layer 32: the frequency of the molecular pump was 72%, and nitrogen (N) was flushed into the apparatus, so that the pressure in the apparatus was 4 x 10-2mbar, single-opening TiSi85/15 target, arc current of 200A, bias voltage of 40V, and coating time of 3 min.
F. And D, the step E and the step D are combined, and the work is circulated for 5 periods, so that the total thickness of the combined layer 2+ the modulation layer 31+ the functional layer 32 is 1.35 um.
G. Finally, the temperature is reduced to below 200 ℃ before the furnace is discharged.
Specific embodiment example 2:
the PVD surface treated high speed steel or hard alloy comprises a substrate 1, a bonding layer 2 attached to the surface of the substrate 1 from inside to outside, a modulation layer 31 and a functional layer 32 which are repeated for 4 cycles in sequence. The bonding layer 2 is an AlCr coating with the thickness of 0.3um, wherein the mass ratio of Al to Cr of the AlCr coating is 64: 36; the modulation layer 31 is an AlCr coating with a thickness of 0.16um, wherein the ratio of the amounts of Al and Cr substances in the AlCr coating is 64: 36; the functional layer 32 is a TiSi coating with a thickness of 0.05um, wherein the ratio of the amount of Ti to the amount of Si in the TiSi coating is 85: 15. the total thickness of the film layers of the bonding layer 2+ the modulation layer 31+ the functional layer 32 was 1.14 um.
The hardness of the high-speed steel and the hard alloy coating subjected to PVD surface treatment is 3300V, the binding force can reach the HF1 standard by adopting Rockwell hardness tester measurement, the friction coefficient with metal is 0.18, and the heat-resistant temperature is 900 ℃.
The specific preparation process is not described in detail herein, referring to example 1.
Specific embodiment example 3:
the PVD surface treated high speed steel or hard alloy comprises a substrate 1, a bonding layer 2 attached to the surface of the substrate 1 from inside to outside, a modulation layer 31 and a functional layer 32 which are sequentially repeated for 6 cycles. The bonding layer 2 is an AlCr coating with the thickness of 0.25um, wherein the mass ratio of Al to Cr of the AlCr coating is 64: 36; the modulation layer 31 is an AlCr coating with a thickness of 0.19um, wherein the ratio of the amounts of Al and Cr substances in the AlCr coating is 64: 36; the functional layer 32 is a TiSi coating with a thickness of 0.05um, wherein the ratio of the amount of Ti to the amount of Si in the TiSi coating is 85: 15. the total thickness of the film layers of the bonding layer 2+ the modulation layer 31+ the functional layer 32 was 1.69 um.
The hardness of the high-speed steel and the hard alloy coating subjected to PVD surface treatment is 3200V, the binding force can reach the HF1 standard by adopting a Rockwell hardness tester for measurement, the friction coefficient with metal is 0.18, and the heat-resistant temperature is 1000 ℃.
The specific preparation process is not described in detail herein, referring to example 1.
The above embodiments are described in more detail and specifically, but the invention is not limited thereto. 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 (2)

1. A novel H-coating, comprising: the substrate comprises a bonding layer (2) attached to the surface of a substrate (1) from inside to outside, and a modulation layer (31) and a functional layer (32) which repeat N cycles in sequence, wherein the bonding layer (2) is an AlCr coating with the thickness of 0.2-0.3um, and the modulation layer (31) is an AlCr coating with the thickness of 0.16-0.20 um; the functional layer (32) is a TiSi coating, the thickness of the TiSi coating is 0.05um, and the quantity ratio of Ti to Si in the TiSi coating is 85: 15, in the modulating layer (31) and the functional layer (32) which are sequentially repeated for N periods, N is more than or equal to 4 and less than or equal to 6, N is a natural number, and the total thickness of the bonding layer (2), the modulating layer (31) and the film layer of the functional layer (32) is 1.04-1.8 um; the method is characterized in that: the ratio of the amount of Al to Cr species in the AlCr coating is 64: 36.
2. the novel H-coating of claim 1, which is treated by a process comprising the steps of:
A. vacuumizing and heating: firstly, putting a substrate 1 material into vacuum coating equipment, and adjusting the vacuum degree of the equipment to 6 x 10- 5Heating for about 1h at mbar to raise the temperature to 460-;
B. cleaning the substrate 1: the ion bombardment is carried out, the bias voltage is 10V, the operating frequency of the molecular pump is reduced to 72 percent from 100 percent during initial vacuumizing, high-purity hydrogen (H) with the purity of 99.999 percent and high-purity argon (Ar) with the purity of 99.999 percent are simultaneously introduced into the equipment, the flow rate of the hydrogen (H) is 50-200sccm, the flow rate of the argon (Ar) is 50sccm, and the ventilation time is 20-30 min. Then, setting the bias voltage as 200V, and introducing high-purity argon (Ar) into the equipment, wherein the flow rate of the argon (Ar) is 50sccm, and the introducing time is 20-30 min;
C. plating the bonding layer 2: the frequency of the molecular pump was 72%, and the apparatus was filled with nitrogen (N) so that the pressure in the apparatus was 2.5 x 10-2mbar, single opening of AlCr64/36 target, arc current of 150A, bias voltage of 40-150V, and coating time of 13.6-16.8 min. Compared with the traditional coating process, the bias voltage is increased from 120V to 150V, and the coating time is increased from 13-16min to 13.6-16.8min, so that the content of Al in the AlCr coating is reduced to effectively adjustInsufficient hardness to ensure the hardness, thickness and energy of the bonding layer 2;
D. plating preparation layer 31: the frequency of the molecular pump was 72%, and the apparatus was filled with nitrogen (N) so that the pressure in the apparatus was 4 x 10- 2mbar, single opening of AlCr64/36 target, arc current of 180A, bias voltage of 150V, and coating time of 8.4-12.6 min. Compared with the traditional coating process, the bias voltage is increased from 120V to 150V, and the coating time is increased from 8-12min to 8.4-12.6min, so that the problem of insufficient hardness caused by reduction of Al content in the AlCr coating can be effectively solved, and the hardness, thickness and energy of the prepared layer 31 are ensured;
E. plating of the functional layer 32: the frequency of the molecular pump was 72%, and nitrogen (N) was flushed into the apparatus, so that the pressure in the apparatus was 4 x 10- 2mbar, single-opening TiSi85/15 target, arc current of 200A, bias voltage of 40V, and coating time of 3 min.
The step D and the step E are a group, and the cycle work is carried out for 4 to 6 periods, so that the total thickness of the combined layer (2), the modulation layer (31) and the functional layer (32) is 1.04 to 1.8 um;
F. finally, the temperature is reduced to below 200 ℃ before the furnace is discharged.
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CN114196919A (en) * 2021-12-14 2022-03-18 昆山汇创杰纳米科技有限公司 High-bonding-force hard coating for die and preparation process thereof
CN114369799A (en) * 2021-12-17 2022-04-19 中国船舶重工集团公司第七一一研究所 Composite coating for surface of engine connecting rod, preparation method of composite coating and engine connecting rod

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CN114196919A (en) * 2021-12-14 2022-03-18 昆山汇创杰纳米科技有限公司 High-bonding-force hard coating for die and preparation process thereof
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CN114369799A (en) * 2021-12-17 2022-04-19 中国船舶重工集团公司第七一一研究所 Composite coating for surface of engine connecting rod, preparation method of composite coating and engine connecting rod

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