CN112626457A - High-hardness PVD (physical vapor deposition) film and preparation method thereof - Google Patents

High-hardness PVD (physical vapor deposition) film and preparation method thereof Download PDF

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Publication number
CN112626457A
CN112626457A CN202110056037.6A CN202110056037A CN112626457A CN 112626457 A CN112626457 A CN 112626457A CN 202110056037 A CN202110056037 A CN 202110056037A CN 112626457 A CN112626457 A CN 112626457A
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layer
target
tungsten carbide
hardness
pvd
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冯伟
吴海平
杜晓颖
杜国才
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Huizhou Changxingrong Technology Co ltd
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Huizhou Changxingrong 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
    • C23C14/0635Carbides
    • 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

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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)
  • Physical Vapour Deposition (AREA)

Abstract

The invention provides a high-hardness PVD (physical vapor deposition) film and a preparation method thereof, wherein the method is deposited on a base material by adopting a vacuum coating method and specifically comprises the following steps: cleaning the base material; the method comprises the following steps of sequentially plating a bottom layer, a thick film layer, a transition layer and a color layer on the surface of a base material, wherein the bottom layer is a tungsten carbide composite plating layer, the thick film layer is a tungsten carbide composite plating layer, the transition layer is a tungsten carbide composite plating layer, and the color layer is a tungsten carbide composite plating layer. The high-hardness PVD film layer disclosed by the invention has no white dew in a vibration wear test of 2H, a salt spray test of 72H, an artificial sweat test of 96H and a poaching Baige test. The high-hardness PVD film layer prepared by the method provided by the invention can improve the product quality, prolong the service life and expand the product use conditions.

Description

High-hardness PVD (physical vapor deposition) film and preparation method thereof
Technical Field
The invention relates to the technical field of vacuum coating, in particular to a high-hardness PVD (physical vapor deposition) film and a preparation method thereof.
Background
At present, a coating process is applied to appearance decoration of a plurality of electronic product parts and workpieces so as to improve corrosion resistance and further prolong the service life of the electronic product parts and the workpieces. However, the film formed by the existing coating technology has insufficient hardness, and is easy to crack and fall off in the use process, or is easy to scratch when contacting with an external object, so that the film gradually falls off from the damaged part.
Disclosure of Invention
In view of the above, in order to overcome the defects of the prior art, the invention provides a high-hardness PVD film with good product quality and long service life.
Specifically, the high-hardness PVD film layer is deposited on a base material by adopting a vacuum coating method, and the preparation method of the high-hardness PVD film layer comprises the following steps:
cleaning the substrate;
sequentially plating a bottom layer, a film thick layer, a transition layer and a color layer on the surface of the base material,
the bottom layer is a tungsten carbide composite coating, the thick film layer is a tungsten carbide composite coating, the transition layer is a tungsten carbide composite coating, and the color layer is a tungsten carbide composite coating.
Further, the bottom layer is plated by adopting a vacuum coating method, and the preparation parameters are as follows: current is 10-100A, bias voltage is 50-350V, time is 60-1200 seconds, vacuum degree is 1.0-1-5.0-1 Pa; the target material is chromium target or titanium target.
The preparation of the bottom layer is divided into two steps, and the specific operation is as follows:
firstly, starting an arc target, and adjusting the current to be 50-100A, the bias voltage to be 150-350V, the time to be 60-300 seconds and the vacuum degree to be 1.0-1 Pa; adopting a chromium target or a titanium target as a target material;
then starting the column target, adjusting the current to 10-30A, the bias voltage to 50-200V, the time to 600-1200 seconds and the vacuum degree to 3.0-1-5.0-1 Pa; the target material is chromium target or titanium target.
The thick film is plated by adopting a vacuum coating method, and the preparation parameters are as follows: current 10-30A, bias voltage 30-200V, time 3600-; the target material is titanium target, zirconium target, chromium target, tungsten carbide target or silicon target.
The transition layer is plated by adopting a vacuum coating method, and the preparation parameters are as follows: current 10-30A, bias voltage 30-200V, time 600-; the target material is titanium target, zirconium target, chromium target, tungsten carbide target or silicon target.
The color layer is plated by adopting a vacuum coating method, and the preparation parameters are as follows: current 10-30A, bias voltage 30-200V, time 7200-; the target material is titanium target, zirconium target, chromium target, tungsten carbide target or silicon target.
The "cleaning the substrate" includes: glow cleaning, ion source cleaning and metal ion cleaning.
The high-hardness PVD film plated by the preparation method of the high-hardness PVD film is deposited on the surface of a base material, and the PVD film sequentially comprises the following components from bottom to top from the surface of the base material:
the bottom layer is a tungsten carbide composite coating;
the film thick layer is a tungsten carbide composite coating;
the transition layer is a tungsten carbide composite coating;
the color layer is a tungsten carbide composite coating.
The thickness of the bottom layer is 0.1-0.25 μm, the thickness of the film thick layer is 1.4-1.65 μm, the thickness of the transition layer is 0.1-0.25 μm, and the thickness of the color layer is 0.1-0.25 μm.
The thickness ratio of the film thick layer to the whole PVD film layer is 1: 3.
the high-hardness PVD film layer disclosed by the invention has no white dew in a vibration wear test of 2H, a salt spray test of 72H, an artificial sweat test of 96H and a poaching Baige test. The high-hardness PVD film layer prepared by the method provided by the invention can improve the product quality, prolong the service life and expand the product use conditions.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a high hardness PVD film of the invention.
Reference numerals:
1-a substrate; 2-a bottom layer; 3-a film thick layer; 4-a transition layer; 5-color layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to FIG. 1, this example provides a high hardness PVD film deposited on the surface of a substrate 1. Alternatively, the material of the substrate 1 may be metal, stainless steel, glass, ceramic or plastic. The PVD rete by 1 surface of substrate from up including in proper order down:
bottom layer 2: the adhesive force of the film layer is improved; the material is a tungsten carbide composite coating with the thickness of 0.1-0.25 mu m. In some embodiments, the bottom layer 2 is a composite of tungsten carbide (WC) and other elements, which may be Ti/Cr.
Film thickness layer 3: the hardness of the film layer is enhanced; the material is a tungsten carbide composite coating with the thickness of 1.4-1.65 mu m. In some embodiments, the bottom layer 2 is a composite of tungsten carbide and other elements, which may be Ti/Cr/W/Zr/Si.
Transition layer 4: used for improving the adhesive force of the color layer 5 and the film thickness layer 3; the material is a tungsten carbide composite coating with the thickness of 0.1-0.25 mu m. In some embodiments, the transition layer 4 is a composite of tungsten carbide and other elements, which may be Ti/Cr/W/Zr/Si.
Color layer 5: the color adjusting device is used for adjusting the color to be within a target range on the basis of ensuring the basic performance of the film layer; the material is a tungsten carbide composite coating with the thickness of 2.5-2.85 μm. In some embodiments, the color layer is a composite of 5-bit tungsten carbide and other elements, which may be Ti/Cr/W/Zr/Si.
The thickness of the high-hardness PVD film provided in this embodiment is 4.1-5 μm, and the thickness ratio of the film thickness layer 3 to the entire film is 1: 3, the thickness ratio of the film thickness layer 3 to the bottom layer 2 is 8: 1.
example 2
The embodiment provides a preparation method of a high-hardness PVD (physical vapor deposition) film layer, which is used for preparing the high-hardness PVD film layer described in the embodiment 1.
S1: after being hung on a substrate 1, the substrate enters an autonomous cleaning line to be cleaned with oil removal, wax removal, oxide layer removal and the like, the cleaning time is 120 minutes, the substrate is baked for 80 minutes at the temperature of 120 +/-5 ℃, and then the substrate is placed in a furnace.
S2: heating after vacuumizing for 20 minutes, setting the temperature at 100-250 ℃, continuing to vacuumize for 60-90 minutes, and finally enabling the vacuum degree to be less than or equal to 0.006 Pa.
S3: starting glow cleaning: ar: 300SLM, bias voltage 300V-1000V, duty ratio 50%, vacuum degree: 1.0Pa, time 600-.
S4: and (3) carrying out ion source cleaning: ar was adjusted to 50SLM, vacuum: 8.0-2Pa, duty ratio of 30% -80%, bias voltage of 500V-1600V, ion source voltage of 1200V-1800V, and total cleaning time of 1800 seconds.
S5: and (3) cleaning metal ions: the current is 60A-120A, Ar is adjusted to be 20SLM, and the vacuum degree is 8.5-2Pa, bias voltage of 100V-500V, duty ratio of 50%, starting arc targets 1, 2, 3 and 4 in sequence, each time 180 seconds.
S6: preparation of bottom layer 2:
s61: simultaneously starting all arc targets, wherein the bias voltage is 150-350V, the current is 50-100A, the duty ratio is 50%, the time is 60-300 seconds, and closing all arc targets after finishing; the target material is Ti/Cr.
S62: starting the column target, and keeping the vacuum degree: 3.0-1-5.0-1Pa, column target current 10A-30A, bias voltage 50V-200V, duty ratio 50%600 seconds and 1200 seconds; the target material is Ti/Cr.
S7: preparation of a thick film 3: starting the column target, with current of 10A-30A and bias voltage of 30V-200V, C2H2: 10-150SLM, time 3600-; the target material is Ti/Cr/W/Zr/Si/tungsten carbide.
S8: preparing a transition layer 4: current 10A-30A, bias voltage 30V-200V, duty ratio 50%, and vacuum degree 3.0-1-5.0- 1Pa,C2H2: 10-100SLM, time 600-; the target material is Ti/Cr/W/Zr/Si/tungsten carbide.
S9: preparation of color layer 5: current 10A-30A, bias voltage 30V-200V, duty ratio 50%, and vacuum degree 3.0-1-5.0- 1Pa,C2H2: 20-200SLM, time 7200 and 14400 seconds; the target material is Ti/Cr/W/Zr/Si/tungsten carbide.
And (5) taking out of the furnace after the film coating and cooling are finished for 20 minutes.
Example 3
A high hardness PVD film layer is deposited on the surface of SUS316L stainless steel substrate 1. The PVD rete by 1 surface of substrate from up including in proper order down:
bottom layer 2: the material is Cr tungsten carbide, and the thickness is 0.2 mu m;
film thickness layer 3: the material is Cr tungsten carbide with the thickness of 1.6 mu m;
transition layer 4: the material is Cr tungsten carbide, and the thickness is 0.2 mu m;
color layer 5: the material is Cr tungsten carbide, and the thickness is 2.8 mu m.
The high-hardness PVD film layer is plated by a vacuum coating method, and the method comprises the following specific operations:
s01: the substrate 1 made of SUS316L was hung on a rack and then entered into an autonomous cleaning line to be cleaned for oil removal, wax removal, oxide layer removal, etc., for a cleaning time of 120 minutes, baked at a temperature of 120 ℃ ± 5 ℃ for 80 minutes, and then put into a furnace.
S02: heating after vacuumizing for 20 minutes, setting the temperature at 220 ℃, and continuously vacuumizing for 60 minutes until the vacuum degree reaches 0.0003 Pa.
S03: starting glow cleaning: ar: 300SLM, bias voltage is increased from 300V to 500V, 50V is increased per minute, duty ratio is 50%, vacuum degree: 1.0Pa, time 1200 seconds.
S04: and (3) carrying out ion source cleaning: ar is adjusted to be 50SLM, the duty ratio is 50%, the bias voltage is 1000V, and the ion source voltage is 1200V; then the bias voltage plus 100V and the ion source voltage plus 100V are adjusted to be 1200V and 1600V for 1800 seconds.
S05: and (3) turning off an ion power supply to clean metal ions: ar is adjusted to be 20SLM, and the vacuum degree is 8.5-2The bias voltage is adjusted to be 500V, the duty ratio is 50%, and arc targets 1, 2, 3 and 4 are started in sequence, wherein the time is 180 seconds each time.
S06: preparing a bottom layer 2 with Cr tungsten carbide:
s061: and simultaneously starting all arc targets, adjusting the bias voltage to 300V, adjusting the duty ratio to 50%, and closing all arc targets after the operation is finished for 300 seconds. The arc target is made of Cr;
s062: ar was adjusted to 150SLM, vacuum: 5.0-1Pa, Cr column target current 20A, bias voltage 100V, duty ratio 50%, time 1200 seconds.
S07: film thickness layer 3 made of Cr tungsten carbide: starting WC target, current 20A, C2H2: 20-100SLM, C2H2 set step size 1SLM/60 seconds, add to 100SLM stop adding, time 9000 seconds.
S08: preparing a transition layer 4 with Cr tungsten carbide as a component: cr current 20A, WC current 20A, bias voltage 100V, duty cycle 50%, C2H2: 100SLM, time 3600 seconds.
S09: preparing a color layer 5 with Cr tungsten carbide as a component: cr current 10A, WC current 10A, bias voltage 150V, duty ratio 50%, C2H2: 100SLM, time 7200 seconds.
And (5) taking out of the furnace after the film coating and cooling are finished for 20 minutes.
The Vickers hardness 1180HV load of the high-hardness PVD film layer is 50 g, and the Vickers hardness 1090HV load is 25 g; the test result shows that 2H has no whitening through a vibration abrasion resistance test, 72H through a salt spray test, 96H through an artificial sweat test and a poaching hundred-grid test. The high-hardness PVD film layer prepared by the method provided by the invention can improve the product quality, prolong the service life and expand the product use conditions.
The above-mentioned embodiments are only preferred embodiments of the present invention, and not intended to limit the present invention, and various modifications other than the above-mentioned embodiments may be made, and the technical features of the above-mentioned embodiments may be combined with each other, and any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A preparation method of a high-hardness PVD (physical vapor deposition) film layer is characterized by comprising the following steps of:
cleaning the substrate;
sequentially plating a bottom layer, a film thick layer, a transition layer and a color layer on the surface of the base material,
the bottom layer is a tungsten carbide composite coating, the thick film layer is a tungsten carbide composite coating, the transition layer is a tungsten carbide composite coating, and the color layer is a tungsten carbide composite coating.
2. The method for preparing a high-hardness PVD film according to claim 1, wherein the bottom layer is coated by a vacuum coating method, and the preparation parameters are as follows: current of 10-100A, bias voltage of 50-350V, time of 60-1200 s, and vacuum degree of 1.0-1-5.0-1Pa; the target material is chromium target or titanium target.
3. The preparation method of the high-hardness PVD film layer as recited in claim 2, wherein the preparation of the bottom layer is divided into two steps, and the specific operation is as follows:
firstly, starting the arc target, adjusting the current to 50-100A, the bias voltage to 150-350V, the time to 60-300 seconds and the vacuum degree to 1.0-1Pa; adopting a chromium target or a titanium target as a target material;
then, starting the column target, adjusting the current to 10-30A, the bias voltage to 50-200V, the time to 600-1200 seconds and the vacuum degree to 3.0-1-5.0-1Pa; the target material is chromium target or titanium target.
4. The method for preparing a high-hardness PVD film layer as recited in claim 1, wherein the thick film layer is coated by a vacuum coating method, and the preparation parameters are as follows: current 10-30A, bias voltage 30-200V, time 3600--1-5.0-1Pa、C2H210-150 SLM; the target material is titanium target, zirconium target, chromium target, tungsten carbide target or silicon target.
5. The preparation method of the high-hardness PVD film layer as recited in claim 1, wherein the transition layer is coated by a vacuum coating method, and the preparation parameters are as follows: current 10-30A, bias voltage 30-200V, time 600--1-5.0-1Pa、C2H210-100 SLM; the target material is titanium target, zirconium target, chromium target, tungsten carbide target or silicon target.
6. The preparation method of the high-hardness PVD film layer as recited in claim 1, wherein the color layer is coated by a vacuum coating method, and the preparation parameters are as follows: current 10-30A, bias voltage 30-200V, time 7200--1-5.0-1Pa、C2H220-200 SLM; the target material is titanium target, zirconium target, chromium target, tungsten carbide target or silicon target.
7. The method for preparing the high-hardness PVD film layer as recited in claim 1, wherein the step of "cleaning the substrate" comprises: glow cleaning, ion source cleaning and metal ion cleaning.
8. A high-hardness PVD (physical vapor deposition) film layer deposited on the surface of a substrate according to the preparation method of any one of claims 1 to 7, wherein the PVD film layer sequentially comprises from bottom to top of the substrate surface:
the bottom layer is a tungsten carbide composite coating;
the film thick layer is a tungsten carbide composite coating;
the transition layer is a tungsten carbide composite coating;
the color layer is a tungsten carbide composite coating.
9. The high-hardness PVD film layer as recited in claim 8, wherein the thickness of the bottom layer is 0.1-0.25 μm, the thickness of the thick film layer is 1.4-1.65 μm, the thickness of the transition layer is 0.1-0.25 μm, and the thickness of the color layer is 0.1-0.25 μm.
10. The high-hardness PVD film layer as recited in claim 8, wherein a thickness ratio of the thick film layer to the overall PVD film layer is 1: 3.
CN202110056037.6A 2021-01-15 2021-01-15 High-hardness PVD (physical vapor deposition) film and preparation method thereof Pending CN112626457A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113136557A (en) * 2021-04-24 2021-07-20 东莞市立恒镀膜科技有限公司 Corrosion-resistant and wear-resistant PVD (physical vapor deposition) film and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN208121182U (en) * 2018-04-11 2018-11-20 深圳市正和忠信股份有限公司 A kind of black conductive PVD film

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN208121182U (en) * 2018-04-11 2018-11-20 深圳市正和忠信股份有限公司 A kind of black conductive PVD film

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113136557A (en) * 2021-04-24 2021-07-20 东莞市立恒镀膜科技有限公司 Corrosion-resistant and wear-resistant PVD (physical vapor deposition) film and preparation method thereof

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Application publication date: 20210409