CN115125480A - Coating film and method for producing coating film - Google Patents
Coating film and method for producing coating film Download PDFInfo
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- CN115125480A CN115125480A CN202210604876.1A CN202210604876A CN115125480A CN 115125480 A CN115125480 A CN 115125480A CN 202210604876 A CN202210604876 A CN 202210604876A CN 115125480 A CN115125480 A CN 115125480A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 82
- 238000000576 coating method Methods 0.000 title claims abstract description 82
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000000758 substrate Substances 0.000 claims abstract description 104
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 83
- 238000000151 deposition Methods 0.000 claims abstract description 60
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 46
- 239000002131 composite material Substances 0.000 claims abstract description 45
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 43
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 43
- 238000004544 sputter deposition Methods 0.000 claims abstract description 42
- 229910019974 CrSi Inorganic materials 0.000 claims abstract description 35
- 230000002829 reductive effect Effects 0.000 claims abstract description 15
- 239000013077 target material Substances 0.000 claims abstract description 15
- 239000010410 layer Substances 0.000 claims description 236
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- 238000004140 cleaning Methods 0.000 claims description 22
- 230000008859 change Effects 0.000 claims description 8
- 239000002356 single layer Substances 0.000 claims description 7
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 229910052804 chromium Inorganic materials 0.000 abstract description 35
- 238000002360 preparation method Methods 0.000 abstract description 17
- 229910052710 silicon Inorganic materials 0.000 abstract description 14
- 239000011651 chromium Substances 0.000 description 153
- 239000010408 film Substances 0.000 description 124
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- 230000008569 process Effects 0.000 description 16
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- 238000005260 corrosion Methods 0.000 description 13
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Images
Classifications
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0084—Producing gradient compositions
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
-
- 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
- C23C14/0664—Carbonitrides
-
- 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
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/345—Applying energy to the substrate during sputtering using substrate bias
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3464—Sputtering using more than one target
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3492—Variation of parameters during sputtering
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- G—PHYSICS
- G04—HOROLOGY
- G04B—MECHANICALLY-DRIVEN CLOCKS OR WATCHES; MECHANICAL PARTS OF CLOCKS OR WATCHES IN GENERAL; TIME PIECES USING THE POSITION OF THE SUN, MOON OR STARS
- G04B37/00—Cases
- G04B37/22—Materials or processes of manufacturing pocket watch or wrist watch cases
- G04B37/223—Materials or processes of manufacturing pocket watch or wrist watch cases metallic cases coated with a nonmetallic layer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The embodiment of the application provides a coating film and a preparation method of the coating film; the preparation method comprises the following steps: starting an arc target to sputter, wherein the arc target is made of Cr, applying a first negative bias to the substrate, and depositing the Cr on the surface of the substrate to form a bottom layer; introducing nitrogen and acetylene, co-sputtering on the bottom layer by taking a Cr target and a Si target as target materials to deposit and form a CrSi composite film layer on the bottom layer, wherein the CrSi composite film layer is an intermediate layer; continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as targets, co-sputtering on the CrSi composite film layer, adjusting the proportion of Cr and Si by controlling the current of the Cr target and the Si target to be gradually reduced, and depositing on the CrSi composite film layer to form a gradient layer; and continuously introducing nitrogen and acetylene, taking the Cr target and the Si target as targets, adjusting the current of the Cr target and the Si target to be less than 10A, depositing on the gradient layer to form a color layer, wherein the color layer comprises a CrSiCN component, and finally forming a coating film on the substrate.
Description
Technical Field
The embodiment of the application relates to the technical field of preparation of coating materials, in particular to a coating and a preparation method of the coating.
Background
Currently, the black color process is widely used in Physical Vapor Deposition (PVD) industry. Especially in the current situation that intelligent wearing is rapidly developed, taking a common intelligent watch as an example, the surface of the shell of the intelligent watch mostly needs to be subjected to PVD (physical vapor deposition) coating treatment, and a black process has a very large proportion.
In the conventional PVD coating technology, when a black coating is prepared by using a single Cr target, a single W target and a single Ti target, debugging is difficult, and pure black cannot be realized, for example, the L value for evaluating black purity is usually less than 32. Moreover, the black film layer prepared had only a warm tone (b value is positive, the film layer showed a yellow phase). Meanwhile, the black prepared by the traditional process has poor color stability, and is easy to cause local color, so that the appearance effect of the product is influenced.
Disclosure of Invention
The application aims to provide a novel technical scheme of a coating film and a preparation method of the coating film.
In a first aspect, the present application provides a method for preparing a coating film, which is characterized by comprising:
preparing a bottom layer: starting an arc target to sputter, wherein the arc target is made of Cr, applying a first negative bias to a substrate, and depositing the Cr on the surface of the substrate to form a bottom layer;
preparing an intermediate layer: introducing nitrogen and acetylene, co-sputtering on the bottom layer by taking a Cr target and a Si target as target materials to deposit and form a CrSi composite film layer on the bottom layer, wherein the CrSi composite film layer is an intermediate layer;
preparing a gradient layer: continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as targets, co-sputtering on the CrSi composite film layer, gradually reducing and adjusting the ratio of Cr to Si by controlling the current of the Cr target and the Si target, and depositing on the CrSi composite film layer to form a gradient layer; and
preparing a color layer: and continuously introducing nitrogen and acetylene, taking the Cr target and the Si target as target materials, adjusting the current of the Cr target and the Si target to be less than 10A, depositing a color layer on the gradient layer, wherein the color layer comprises a CrSiCN composite component, and finally forming a coating film on the substrate.
Optionally, the preparing the bottom layer further comprises: and starting a Cr target for sputtering, applying a second negative bias voltage to the substrate, depositing Cr on the surface of the substrate, and depositing a pure Cr film layer on the surface of the substrate, wherein the bottom layer also comprises the formed pure Cr film layer.
Optionally, in the step of preparing the bottom layer: the first negative bias is-200V to-300V, the pulse duty ratio is 60-70%, and the time is 90-300 s.
Optionally, the second negative bias voltage is-150V to-300V, the pulse duty ratio is 60% to 70%, and the time is 300s to 600 s.
Optionally, in the step of preparing the intermediate layer: the current for the Cr target is 15A to 20A, and the current for the Si target is 5A to 13A.
Optionally, the number of the intermediate layers is 4-10, and the deposition forming time of a single layer is 600-900 s.
Optionally, in the step of preparing the graded layer: the deposition forming time of the gradient layer is 3000 s-3600 s.
Optionally, in the step of preparing the graded layer, the current control manner for the Cr target and the Si target is: the current of the Cr target and the Si target is controlled to be reduced by 1A to 2A every 600 s.
Optionally, in the step of preparing the color layer: the deposition forming time of the color layer is 600 s-900 s.
Optionally, the content of Cr in the intermediate layer is 60% to 70%, and the content of Si in the intermediate layer is 30% to 40%.
Alternatively, the amount ratio of the nitrogen to the acetylene is 1: 1.5 to 2.
Optionally, the preparation method further comprises glow cleaning: glow cleaning the surface of the substrate;
the glow cleaning comprises the following steps: and applying a set negative bias to the substrate, wherein the set negative bias is-400V-600V, the pulse duty ratio is 50-70%, and the time is 300-900 s.
In a second aspect, the present application provides a coating film prepared by the preparation method as described above.
According to the embodiment of the application, a coating preparation scheme is provided, an intermediate layer is formed by co-sputtering a Cr target and a Si target, the corrosion resistance of a coating can be improved, two reaction gases of acetylene and nitrogen are also utilized, C can be introduced by participation of acetylene, the coating can display black, the formed black can have diversity, namely, deep black, blue black (cool tone), traditional black (warm tone) and the like can be prepared, the nitrogen can play a role in protecting the formed black, and a black coating deeper than the traditional black can be prepared.
Other features of the present description and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof, which proceeds with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the specification and together with the description, serve to explain the principles of the specification.
Fig. 1 is a flowchart of a method for producing a plating film according to an embodiment of the present application;
fig. 2 is a schematic structural diagram of a plating film provided in an embodiment of the present application.
Detailed Description
Various exemplary embodiments of the present application will now be described in detail with reference to the accompanying drawings. It should be noted that: the relative arrangement of the components and steps, the numerical expressions, and numerical values set forth in these embodiments do not limit the scope of the present application unless specifically stated otherwise.
The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the application, its application, or uses.
Techniques and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be considered a part of the specification where appropriate.
In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be discussed further in subsequent figures.
The plating film and the method for producing the plating film provided in the embodiments of the present application are described in detail below with reference to fig. 1 to 2, respectively.
According to an embodiment of the present application, there is provided a method for preparing a plated film, which may include steps S110 to S140, and may finally form a plated film on a substrate, as shown in fig. 1.
The substrate may be, for example, a workpiece to be coated.
The workpiece to be coated may be, for example, the case of a smart watch. Can form corrosion-resistant and black higher black coating film of black purity on the shell of intelligence wrist-watch.
Step S110, preparing a bottom layer, comprising the following steps:
starting an arc target to sputter, wherein the arc target is made of Cr, and applying a first negative bias to a substrate (a workpiece to be coated) to deposit the Cr on the surface of the substrate to form a bottom layer.
In step S110 of this embodiment, when the arc target is sputtered, the high-energy ions initially reaching the substrate (workpiece to be coated) sputter atoms of the substrate, and this process of sputtering the substrate atoms is reverse sputtering. The substrate atoms sputtered off will also be ionized in the plasma space into ions which will be accelerated back to the substrate by the negative bias on the substrate. Thus, the Cr film layer formed by arc target sputtering can be formed firmly on the surface of the substrate.
In the step S110, a Cr target may be turned on to perform sputtering, and a second negative bias voltage may be applied to the substrate to deposit Cr on the substrate surface to form a pure Cr film layer on the substrate surface, where the underlayer further includes the formed pure Cr film layer.
In this way, a very high purity Cr film layer can be formed on the surface of the substrate.
It should be noted that, a Cr film layer may also be formed on the surface of the substrate by arc target sputtering only, and a person skilled in the art may flexibly adjust the specific steps included in the preparation of the underlayer according to specific needs, which is not specifically limited in the embodiments of the present application.
In the embodiment of the present application, not only the Cr film layer may be formed by the arc target, but also the Cr film layer may be formed by the Cr target, so that the Cr film layer having a very high purity may be formed on the surface of the substrate and used as the underlayer. The use of this primer layer for connecting the substrate to other layers in the coating film has a very critical effect on whether the coating film can be stably fixed to the substrate.
In the embodiment of the present application, the substrate may be made of stainless steel, for example, and the bottom layer of pure Cr material may be formed to be firmly bonded to the stainless steel. The arc source sputtering is adopted, the energy of the arc source sputtering is very large, when the chromium Cr material is sputtered onto the substrate, the substrate can synchronously have reverse sputtering, therefore, the reverse sputtering material is combined with the arc source material, namely, the chromium Cr material returns to the substrate, the arc source material is obtained in the step, in addition, the material of the substrate per se is deposited on the surface of the substrate, a pseudo diffusion layer can be formed in the process, the transition is performed to other film layers of the coating film, the bonding force between the coating film and the substrate is better in the process, and the coating film can be effectively prevented from falling off from the substrate.
And, wherein can also carry on the sputtering through the pure chromium Cr target, so can further promote the purity of chromium Cr membranous layer formed.
In the embodiment of the application, the chromium Cr film layer is used as the bottom layer of the whole coating film, so that other film layers formed by compounding the chromium Cr material and other materials in the process of transition from the pure chromium Cr layer to the coating film can be realized, the smooth transition can be realized, and the effect of improving the binding force can be realized.
After the step of forming the bottom layer on the surface of the substrate is completed, the following steps can be entered:
step S120, preparing an intermediate layer:
and introducing nitrogen and acetylene, taking a Cr target and a Si target as target materials, and carrying out co-sputtering on the bottom layer to deposit and form a CrSi composite film layer on the bottom layer, wherein the CrSi composite film layer is an intermediate layer.
That is, in step S120, a composite film layer including Cr and Si may be formed on the underlayer by co-sputtering two targets, i.e., a Cr target and a Si target, on the underlayer formed in step S110 and then depositing for a certain period of time. It can be seen that in this step, silicon Si can be incorporated into chromium Cr.
With the continuous application and development of PVD technology in smart watches, users also put higher demands on the performance of the coating on the smart watch case. In particular, the requirement on the corrosion resistance of the coating film is continuously improved. In the scheme of the application, the Si material is properly introduced into the chromium Cr material, so that the corrosion resistance of the finally formed coating film can be greatly improved, and the requirement on the corrosion resistance of the coating film is well met.
In the above step S120, nitrogen and acetylene are introduced, so that N and C may be introduced, and CrC, CrNC, SiCrNC, and the like may be formed in this layer.
After the intermediate layer is formed, then:
step S130, preparing a gradient layer: and continuously introducing nitrogen and acetylene, taking the Cr target and the Si target as target materials, co-sputtering on the CrSi composite film layer, and gradually reducing and adjusting the ratio of Cr to Si by controlling the current of the Cr target and the Si target to deposit and form a gradient layer on the CrSi composite film layer.
In step S130, a gradient layer of the plating film is formed, in which the ratio of Cr and Si can be adjusted by controlling the current of the Cr target and the Si target to be gradually decreased, and the content of Si, N, and C to be introduced is increased (compared with the intermediate layer), so that the color of the plating film can achieve better blackness while the corrosion resistance of the plating film is optimized.
After the formation of the graded layer, the following steps can be entered:
and S140, continuously introducing nitrogen and acetylene, taking the Cr target and the Si target as targets, adjusting the current of the Cr target and the Si target to be less than 10A, depositing a color layer on the gradient layer, wherein the color layer comprises a CrSiCN composite component, and finally forming a coating film on the substrate.
In the step S140, the currents of the Cr target and the Si target are further adjusted to be as small as possible, and the amount of acetylene introduced in this step can be increased (more than in the steps S120 and S130) to introduce more C, so that the black color formed has higher purity and darker color, and the nitrogen therein can well protect the black color formed. The finally formed coating film has dark black color and good stability, and the condition of local color can not occur.
According to the coating film disclosed by the embodiment of the application, as the Si element is added into part of the film layer, the corrosion resistance of the finally formed coating film is greatly improved, and the color performance is stable and various. It can be made darker and more pure than traditional black. In the process of preparing the middle layer, the gradual change layer and the color layer, nitrogen and acetylene enter into reaction together, the acetylene can provide black, the nitrogen can play a role in protecting the black, the color of the coating film can be displayed under the condition of blacker color, the phenomenon of color is avoided, and the appearance effect can be improved.
According to the embodiment of the application, a coating preparation scheme is provided, an intermediate layer is formed by co-sputtering a Cr target and a Si target, the corrosion resistance of a coating can be improved, two reaction gases of acetylene and nitrogen are also utilized, C can be introduced by participation of acetylene, the coating can display black, the formed black can have diversity, namely, deep black, blue black (cool tone), traditional black (warm tone) and the like can be prepared, the nitrogen can play a protection role on the formed black, and a black coating which is darker than the traditional black can be prepared.
In some examples of the present application, as shown in fig. 1, before preparing the bottom layer, a step S100 may further be included: and (4) glow cleaning. That is, the surface of the substrate is glow-cleaned.
The glow cleaning includes the following parameters: and applying a set negative bias to the substrate, wherein the set negative bias is-400V-600V, the pulse duty ratio is 50-70%, and the time is 300-900 s.
For example, a pulse negative bias can be applied to the surface of the substrate, so that gas desorption of electron bombardment and removal of certain hydrocarbons can be realized, and the surface of the substrate becomes cleaner, thereby facilitating the improvement of the bonding force between the finally formed coating and the substrate and preventing the coating from easily falling off due to poor bonding force between the coating and the substrate.
It should be noted that the negative bias is set to be a pulse negative bias, and the pulse duty ratio is set to be 50% to 70%. It can be interpreted as:
for example, in the time range of 300s to 900s, 10s is used as a pulse period, that is, 10s is used as a pulse period, when sputtering is performed on the surface of the substrate, the pulse duty ratio is set to 70%, and on the basis of this, the time for which the substrate surface receives bombardment is 7s, and the rest 3s are not subjected to bombardment.
By adopting the above parameters to carry out glow cleaning treatment on the surface of the substrate, the cleanliness of the surface can be higher without damaging the surface, which is beneficial to improving the bonding force between the finally formed coating and the surface of the substrate.
In a specific embodiment of the present application, the substrate may be placed in a cavity of a glow cleaning apparatus, and the substrate is subjected to glow cleaning: applying negative bias to the substrate, setting the negative bias to-400V-600V, the pulse duty ratio to 50% -70% and the time to 300-900 s.
After the step of glow cleaning the substrate surface is completed, the process may proceed to step S110.
It should be noted that, in the embodiment of the present application, the substrate is not limited to be subjected to glow cleaning before film coating, and other cleaning manners may also be adopted as long as the surface of the substrate is cleaned to facilitate subsequent film coating, and a person skilled in the art may flexibly select a specific cleaning manner according to needs, which is not specifically limited in the embodiment of the present application.
In some examples of the present application, before the glow cleaning, the method further comprises the step of enabling the vacuum degree of the coating environment to reach 6.0 × 10 -3 Pa or less.
In the embodiments of the present application, a Physical Vapor Deposition (PVD) technique is used, which is a technique of vaporizing a material (solid or liquid) surface into gaseous atoms or molecules or partially ionizing the gaseous atoms or molecules into ions by a Physical method under a vacuum condition, and depositing a thin film on a substrate surface by a low-pressure gas (or plasma) process. Therefore, a vacuum environment is very important.
In some examples of the present application, in the step of preparing the underlayer: the first negative bias is-200V to-300V, the pulse duty ratio is 60-70%, and the time is 90-300 s.
By controlling the above parameter ranges, a firmly adhered Cr film layer can be formed on the surface of the substrate.
In some examples of the present application, in the step of preparing the underlayer: the second negative bias is-150V to-300V, the pulse duty ratio is 60-70%, and the time is 300-600 s.
By controlling the parameter range, a Cr film layer with higher purity can be formed on the surface of the substrate, and the Cr film layer can form a complete bottom layer with the Cr film layer formed by arc target sputtering.
In the embodiment of the application, in the step of preparing the underlayer, one sputtering may be involved to form the Cr film layer, and two sputtering may also be involved to form the Cr film layer with higher purity.
When two times of co-sputtering are involved, namely the arc target sputtering and the Cr target sputtering, the negative bias control on the substrate needs to be slowly reduced, otherwise the internal stress of the film layer formed by sputtering at different stages may be too large, which may cause the formed bottom layer to be fragile, and may crack upon slight extrusion or upon collision, so that the plasticity of the formed bottom layer is not strong, and the bonding force between the coating film and the substrate may also be poor.
In some examples of the present application, in the step of preparing the intermediate layer: the current for the Cr target is 15A to 20A, and the current for the Si target is 5A to 13A.
In the process of preparing the intermediate layer, the amount ratio of Cr and Si in the formed composite film layer can be controlled by controlling the current of the Cr target and the Si target.
For example, the content of Cr in the CrSi composite film layer is 60-70%, and the content of Si is 30-40%. A certain content of Si is introduced in the preparation of the intermediate layer.
By reasonably adjusting the contents of Cr and Si, the corrosion resistance of the finally formed coating film can be improved, and the requirements of users are well met.
At the same time, N and C are also introduced appropriately in this step by means of nitrogen and acetylene. Wherein, the amount of nitrogen and the amount of acetylene can be controlled to be 1: 1.5 to 2. The specific amount can be adjusted according to the actual blackness requirement, but the amount of acetylene is more than that of nitrogen.
In some examples of the present application, the intermediate layer is 4 to 10 layers, and the deposition forming time of the single layer is 600 to 900 seconds.
The number of deposited layers of the CrSi composite film layer can be controlled by one skilled in the art as required, and the embodiment of the present application does not limit this. Different numbers of layers deposited may affect the overall process duration.
In the embodiment of the application, the time of the whole process is not too long by controlling the middle layer to be 4-10 layers, and the thickness of the coating film is not too large.
For example, the thickness of the plating film is usually controlled to 2 μm to 3.5. mu.m. This can meet the requirement of most products for coating thickness at present.
In addition, the production cost can be well controlled.
In some examples of the present application, in the step of preparing the graded layer: the deposition forming time of the gradient layer is 3000 s-3600 s.
The deposition time of the graded layer may affect the thickness of the formed film layer and may also affect the thickness of the finally formed coating film. The embodiment of the application controls the thickness of the coating film to be 2-3.5 μm, which can meet the requirement of most products on the thickness of the coating film at present.
In some examples of the present application, in the step of preparing the graded layer, the current control manner for the Cr target and the Si target is: the current of the Cr target and the Si target is controlled to be reduced by 1A to 2A every 600 s.
In the preparation of the graded layer, the current control for the Cr target and the Si target was performed in a manner of gradually decreasing in a trapezoidal shape. For example, the content of each material in the formed composite film layer can be adjusted by controlling the current value to be reduced by 2A every 10 min.
In the process of forming the gradient layer of the coating, the ratio of Cr and Si is adjusted by controlling the current of the Cr target and the Si target to be gradually reduced, wherein the content of Si, N and C is increased (compared with the intermediate layer), so that the corrosion resistance of the coating is optimal, and the color of the coating can reach better blackness.
In some examples of the present application, in the step of preparing the color layer: the deposition forming time of the color layer is 600 s-900 s.
The deposition time of the color layer will affect the thickness of the formed film layer and will also affect the thickness of the finally formed coating film. The embodiment of the application controls the thickness of the coating film to be 2-3.5 μm, which can meet the requirement of most products on the thickness of the coating film at present.
It should be noted that, in the specific production, a person skilled in the art can flexibly adjust the deposition time of each film layer according to the thickness of the plated film and the condition of each film layer constituting the plated film.
In some examples of the present application, the nitrogen and the acetylene are in a ratio of 1: 1.5 to 2.
In the embodiment of the application, nitrogen and acetylene are required to be introduced in the process of preparing the middle layer, the gradual change layer and the color layer, and N and C can be introduced into the three layers. The intermediate layer, the gradual change layer and the color layer form gradual transition, wherein the contents of Si and C are gradually increased, so that the corrosion resistance of the coating film is improved, and the black purity of the coating film is higher.
In the process of forming the color layer, the introduction amount of acetylene can be increased properly (compared with the middle layer and the gradual change layer, for example, acetylene is twice of that of nitrogen) to introduce more C, so that the formed black has higher purity and darker color, and the nitrogen can well protect the formed black.
According to the preparation method provided by the embodiment of the application, the finally formed coating film is dark in black and good in stability, and the situation of color development cannot occur. The resulting black color L can be made to be < 30, significantly lower than the conventional value (< 32).
The preparation method of the coating film provided by the embodiment of the application can obtain the micron-sized coating film and is a pollution-free environment-friendly surface treatment method. The thickness of the coating film is micron-sized and is thinner, so that various physical properties and chemical properties of the surface of the substrate can be improved under the condition of hardly influencing the original size of the substrate. The coating film has the characteristics of good corrosion resistance, chemical stability and the like, and also has the characteristics of high hardness and high wear resistance (low friction coefficient).
In an embodiment of the present application, a method for preparing a plating film according to the embodiment of the present application includes the following steps:
step S200, making the vacuum degree of the coating environment reach 6.0 multiplied by 10 -3 Pa or less.
Step S210, glow cleaning: glow cleaning the surface of the substrate;
the glow cleaning comprises the following steps: and applying a set negative bias to the substrate, wherein the set negative bias is-400V-600V, the pulse duty ratio is 50-70%, and the time is 300-900 s.
Step S220, preparing a bottom layer, comprising the following steps:
starting an arc target to sputter, wherein the arc target is made of chromium Cr, applying a first negative bias to the substrate, and depositing the chromium Cr on the surface of the substrate;
starting a chromium Cr target for sputtering, applying a second negative bias to the substrate, depositing chromium Cr on the surface of the substrate, and depositing a pure Cr film on the surface of the substrate;
in the step of preparing the bottom layer: the first negative bias is-200V to-300V, the pulse duty ratio is 60-70%, and the time is 90-300 s; the second negative bias is-150V to-300V, the pulse duty ratio is 60-70%, and the time is 300-600 s.
Step S230, preparing an intermediate layer: introducing nitrogen and acetylene, co-sputtering on the bottom layer by taking a Cr target and a Si target as target materials to deposit and form a CrSi composite film layer on the bottom layer, wherein the CrSi composite film layer is an intermediate layer;
wherein the current of the Cr target is 15A-20A, and the current of the Si target is 5A-13A;
wherein the content of Cr in the intermediate layer is 60-70%, and the content of Si is 30-40%;
the number of the middle layers is 4-10, and the deposition forming time of a single layer is 600-900 s.
Step S240, preparing a gradient layer: continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as target materials, co-sputtering on the CrSi composite film layer, adjusting the ratio of Cr to Si by controlling the current of the Cr target and the current of the Si target to be gradually reduced, and depositing on the CrSi composite film layer to form a gradient layer;
the deposition forming time of the gradient layer is 3000 s-3600 s; the current control method for the Cr target and the Si target is as follows: the current is reduced by 1A to 2A every 600 s.
Step S250, color layer preparation: continuously introducing nitrogen and acetylene, taking the Cr target and the Si target as target materials, adjusting the current of the Cr target and the Si target to be less than 10A, depositing on the gradual change layer to form a color layer, wherein the color layer comprises CrSiCN composite components, and finally forming a coating film on the substrate;
the deposition forming time of the color layer is 600 s-900 s.
In steps S230 to S250, the amount ratio of nitrogen to acetylene is 1: 1.5 to 2. In the preparation of the color layer, the content of acetylene can be increased appropriately.
Example 1
The vacuum degree of the coating environment reaches 6.0 multiplied by 10 -3 Pa below;
glow cleaning the surface of the substrate: applying a set negative bias to the substrate, wherein the set negative bias is-400V, the pulse duty ratio is 50%, and the time is 300 s;
starting an arc target to sputter, wherein the arc target is made of chromium Cr, applying a first negative bias to the substrate, and depositing the chromium Cr on the surface of the substrate; starting a chromium Cr target for sputtering, applying a second negative bias voltage to the substrate, and depositing chromium Cr on the surface of the substrate to form a pure Cr film layer on the surface of the substrate by deposition; finally forming a bottom layer; wherein the first negative bias voltage is-200V, the pulse duty ratio is 60%, and the time is 90 s; the second negative bias voltage is-150V, the pulse duty ratio is 60%, and the time is 300 s;
introducing nitrogen and acetylene, co-sputtering on the bottom layer by taking a Cr target and a Si target as target materials, and depositing a CrSi composite film layer on the bottom layer, wherein the CrSi composite film layer is an intermediate layer; the current of the Cr target is 15A, and the current of the Si target is 5A; the content of Cr in the intermediate layer is 60%, and the content of Si is 40%; the number of the middle layers is 4-10, and the deposition forming time of a single layer is 600-900 s.
Continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as targets, co-sputtering on the CrSi composite film layer, adjusting the proportion of Cr and Si by controlling the current of the Cr target and the Si target to be gradually reduced, and depositing on the CrSi composite film layer to form a gradient layer; the deposition forming time of the gradient layer is 3000 s; the current control method for the Cr target and the Si target is as follows: controlling the current to be reduced by 1A every 600 s;
continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as target materials, adjusting the current of the Cr target and the Si target to be less than 10A, depositing on the gradual change layer to form a color layer, wherein the color layer comprises a CrSiCN composite component, and forming a coating film on the substrate; the deposition forming time of the color layer is 600 s.
Example 2
The vacuum degree of the coating environment reaches 6.0 multiplied by 10 -3 Pa below;
glow cleaning the surface of the substrate: applying a set negative bias to the substrate, wherein the set negative bias is-500V, the pulse duty ratio is 65%, and the time is 900 s;
starting an arc target to sputter, wherein the arc target is made of chromium Cr, applying a first negative bias to the substrate, and depositing the chromium Cr on the surface of the substrate; starting a chromium Cr target to sputter, applying a second negative bias to the substrate, and depositing chromium Cr on the surface of the substrate to form a pure Cr film layer on the surface of the substrate; finally forming a bottom layer; wherein the first negative bias voltage is-250V, the pulse duty ratio is 65%, and the time is 150 s; the second negative bias voltage is-200V, the pulse duty ratio is 65%, and the time is 450 s;
introducing nitrogen and acetylene, co-sputtering on the bottom layer by taking a Cr target and a Si target as target materials, and depositing a CrSi composite film layer on the bottom layer, wherein the CrSi composite film layer is an intermediate layer; the current of the Cr target is 18A, and the current of the Si target is 9A; the content of Cr in the intermediate layer is 65%, and the content of Si is 35%; the number of the middle layers is 4-10, and the deposition forming time of a single layer is 600-900 s.
Continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as targets, co-sputtering on the CrSi composite film layer, adjusting the proportion of Cr and Si by controlling the current of the Cr target and the Si target to be gradually reduced, and depositing on the CrSi composite film layer to form a gradient layer; the deposition forming time of the gradient layer is 4500 s; the current control method for the Cr target and the Si target is as follows: the control current is reduced by 1.5A every 600 s;
continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as target materials, adjusting the current of the Cr target and the Si target to be less than 6A, depositing a color layer on the gradient layer, wherein the color layer comprises a CrSiCN composite component, and forming a coating film on the substrate; the deposition forming time of the color layer is 750 s.
Example 3
The vacuum degree of the coating environment reaches 6.0 multiplied by 10 -3 Pa below;
glow cleaning the surface of the substrate: applying a set negative bias voltage to the substrate, wherein the set negative bias voltage is-600V, the pulse duty ratio is 70%, and the time is 900 s;
starting an arc target to sputter, wherein the sputtering material of the arc target is chromium Cr, and applying a first negative bias voltage to the substrate to deposit the chromium Cr on the surface of the substrate; starting a chromium Cr target to sputter, applying a second negative bias to the substrate, and depositing chromium Cr on the surface of the substrate to form a pure Cr film layer on the surface of the substrate; finally forming a bottom layer; wherein the first negative bias voltage is-300V, the pulse duty ratio is 70%, and the time is 300 s; the second negative bias voltage is-300V, the pulse duty ratio is 70%, and the time is 600 s;
introducing nitrogen and acetylene, co-sputtering on the bottom layer by taking a Cr target and a Si target as target materials, and depositing a CrSi composite film layer on the bottom layer, wherein the CrSi composite film layer is an intermediate layer; the current of the Cr target is 20A, and the current of the Si target is 13A; the content of Cr in the intermediate layer is 70%, and the content of Si is 30%; the number of the middle layers is 4-10, and the deposition forming time of a single layer is 600-900 s.
Continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as targets, co-sputtering on the CrSi composite film layer, adjusting the proportion of Cr and Si by controlling the current of the Cr target and the Si target to be gradually reduced, and depositing on the CrSi composite film layer to form a gradient layer; the deposition forming time of the gradient layer is 3600 s; the current control method for the Cr target and the Si target is as follows: controlling the current to be reduced by 2A every 600 s;
continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as target materials, adjusting the current of the Cr target and the Si target to be less than 5A, depositing on the gradual change layer to form a color layer, wherein the color layer comprises a CrSiCN composite component, and forming a coating film on the substrate; the deposition forming time of the color layer is 900 s.
In the embodiment, the coating film is prepared by compounding Cr and Si, so that the PVD black coating film has a blacker color, can be used for making warm-tone black and cold-tone black, and the black film layer prepared by the method has a more stable color.
In a second aspect, the present application provides a coating film prepared by the preparation method as described above.
As shown in fig. 2, the plating film includes: an underlayer 10 formed on a substrate, the underlayer 10 may be a pure Cr film layer, an intermediate layer 20 formed on the underlayer 10, the intermediate layer 20 being a CrSi composite film layer, a graded layer 30 formed on the intermediate layer 20, and a color layer 40 formed on the graded layer 30.
The coating film provided by the embodiment of the application has good corrosion resistance, is stable and diversified in color performance, is darker in black color than the traditional black color, and does not have a color phenomenon.
In the above embodiments, the differences between the embodiments are described in emphasis, and different optimization features between the embodiments can be combined to form a better embodiment as long as the differences are not contradictory, and further description is omitted here in consideration of brevity of the text.
Although some specific embodiments of the present application have been described in detail by way of illustration, it should be understood by those skilled in the art that the above illustration is only for purposes of illustration and is not intended to limit the scope of the present application. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the present application. The scope of the application is defined by the appended claims.
Claims (13)
1. A method for preparing a coating film is characterized by comprising the following steps:
preparing a bottom layer: starting an arc target to sputter, wherein the arc target is made of Cr, applying a first negative bias to a substrate, and depositing the Cr on the surface of the substrate to form a bottom layer;
preparing an intermediate layer: introducing nitrogen and acetylene, co-sputtering on the bottom layer by taking a Cr target and a Si target as target materials to deposit and form a CrSi composite film layer on the bottom layer, wherein the CrSi composite film layer is an intermediate layer;
preparing a gradient layer: continuously introducing nitrogen and acetylene, taking a Cr target and a Si target as targets, co-sputtering on the CrSi composite film layer, gradually reducing and adjusting the ratio of Cr to Si by controlling the current of the Cr target and the Si target, and depositing on the CrSi composite film layer to form a gradient layer; and
preparing a color layer: and continuously introducing nitrogen and acetylene, taking the Cr target and the Si target as targets, adjusting the current of the Cr target and the Si target to be less than 10A, depositing on the gradual change layer to form a color layer, wherein the color layer comprises a CrSiCN composite component, and finally forming a coating film on the substrate.
2. The method of manufacturing according to claim 1, wherein the bottom layer manufacturing further comprises: and starting a Cr target for sputtering, applying a second negative bias voltage to the substrate, depositing Cr on the surface of the substrate, depositing a pure Cr film layer on the surface of the substrate, and forming the bottom layer further comprising the formed pure Cr film layer.
3. The production method according to claim 1, characterized in that, in the step of preparing the underlayer: the first negative bias is-200V to-300V, the pulse duty ratio is 60-70%, and the time is 90-300 s.
4. The method according to claim 2, wherein the second negative bias voltage is-150V to-300V, the pulse duty ratio is 60% to 70%, and the time is 300s to 600 s.
5. The production method according to claim 1, characterized in that, in the step of producing the intermediate layer: the current for the Cr target is 15A to 20A, and the current for the Si target is 5A to 13A.
6. The method according to claim 1, wherein the intermediate layer comprises 4-10 layers, and the deposition time of the monolayer is 600-900 s.
7. The production method according to claim 1, wherein, in the step of producing the gradation layer: the deposition forming time of the gradient layer is 3000 s-3600 s.
8. The method according to claim 7, wherein in the step of preparing the graded layer, current control is performed on the Cr target and the Si target in such a manner that: the current of the Cr target and the Si target is controlled to be reduced by 1A to 2A every 600 s.
9. The method for producing according to claim 1, wherein, in the step of producing the color layer: the deposition forming time of the color layer is 600 s-900 s.
10. The method according to claim 1, wherein the intermediate layer contains 60 to 70% of Cr and 30 to 40% of Si.
11. The method according to claim 1, wherein the nitrogen gas and the acetylene are in a ratio of 1: 1.5 to 2.
12. The method of claim 1, further comprising glow cleaning: glow cleaning the surface of the substrate;
the glow cleaning comprises the following steps: and applying a set negative bias to the substrate, wherein the set negative bias is-400V-600V, the pulse duty ratio is 50-70%, and the time is 300-900 s.
13. A coated film, characterized in that it is produced by the production method according to any one of claims 1 to 12.
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| CN117888062A (en) * | 2023-12-08 | 2024-04-16 | 武汉中科先进材料科技有限公司 | Black and blue PVD decorative film and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110484867A (en) * | 2018-05-15 | 2019-11-22 | 蓝思科技（长沙）有限公司 | Furvous coating Logo and preparation method thereof for nonmetallic cover board |
| CN112281125A (en) * | 2020-09-29 | 2021-01-29 | 维达力实业(深圳)有限公司 | Composite metal film and preparation method and application thereof |
| CN216337918U (en) * | 2021-05-27 | 2022-04-19 | 东莞领益精密制造科技有限公司 | Color-adjustable PVD (physical vapor deposition) film |
-
2022
- 2022-05-30 CN CN202210604876.1A patent/CN115125480A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110484867A (en) * | 2018-05-15 | 2019-11-22 | 蓝思科技（长沙）有限公司 | Furvous coating Logo and preparation method thereof for nonmetallic cover board |
| CN112281125A (en) * | 2020-09-29 | 2021-01-29 | 维达力实业(深圳)有限公司 | Composite metal film and preparation method and application thereof |
| CN216337918U (en) * | 2021-05-27 | 2022-04-19 | 东莞领益精密制造科技有限公司 | Color-adjustable PVD (physical vapor deposition) film |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117888062A (en) * | 2023-12-08 | 2024-04-16 | 武汉中科先进材料科技有限公司 | Black and blue PVD decorative film and preparation method thereof |
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