CN117888062B - Black and blue PVD decorative film and preparation method thereof - Google Patents
Black and blue PVD decorative film and preparation method thereof Download PDFInfo
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- CN117888062B CN117888062B CN202311694401.7A CN202311694401A CN117888062B CN 117888062 B CN117888062 B CN 117888062B CN 202311694401 A CN202311694401 A CN 202311694401A CN 117888062 B CN117888062 B CN 117888062B
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- 238000002360 preparation method Methods 0.000 title abstract description 12
- 230000007704 transition Effects 0.000 claims abstract description 59
- 125000004429 atom Chemical group 0.000 claims abstract description 46
- 230000037452 priming Effects 0.000 claims abstract description 41
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 37
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 26
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 18
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims description 51
- 238000000151 deposition Methods 0.000 claims description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 33
- 229910052799 carbon Inorganic materials 0.000 claims description 33
- 230000008021 deposition Effects 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 19
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 30
- 239000011248 coating agent Substances 0.000 abstract description 28
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000001771 vacuum deposition Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 141
- 239000011651 chromium Substances 0.000 description 51
- 239000007789 gas Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 16
- 238000012360 testing method Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000003086 colorant Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910010037 TiAlN Inorganic materials 0.000 description 1
- 102100029469 WD repeat and HMG-box DNA-binding protein 1 Human genes 0.000 description 1
- 101710097421 WD repeat and HMG-box DNA-binding protein 1 Proteins 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Classifications
-
- 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
- C23C14/0084—Producing gradient compositions
-
- 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
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- 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
- C23C14/0635—Carbides
-
- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates 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
-
- 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
-
- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering 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)
- Inorganic Chemistry (AREA)
- Laminated Bodies (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a black and blue PVD decorative film and a preparation method thereof, and relates to the technical field of vacuum coating. The black and blue PVD decorative film comprises a priming layer, a transition layer and a color layer which are sequentially arranged, wherein the priming layer is a Cr layer, the transition layer is a CrSiC layer, the color layer is a CrSiC layer, the sum of Cr and Si atom contents in the transition layer is larger than C atom content, cr atom content is larger than Si atom content, the sum of Cr and Si atom content in the color layer is smaller than C atom content, and Cr atom content is smaller than Si atom content. The invention adopts the magnetron sputtering process to prepare and obtain the black-blue composite coating, the color of the coating is regarded as bluish black, and continuous black-blue gradient samples can be prepared by adjusting the coating process according to the requirement, so that the color values of the series are controllable and adjustable.
Description
Technical Field
The invention relates to the technical field of vacuum coating, in particular to a black and blue PVD decorative film and a preparation method thereof.
Background
The PVD decorative coating film adopts physical vapor deposition technology to form a layer of uniform, smooth and metal-like surface on the surface of the substrate. The film has high wear resistance and corrosion resistance, and can improve the appearance effect of the product, so that the film is attractive.
The PVD decorative film has various colors including silver, gold, black, gray, blue, purple, coffee, multiple colors and the like. With the increasing diversity of color demands of consumers, more diversified decorative film plating products are also introduced in the market, so that higher requirements are put on the development of the decorative film plating process with rich colors.
Among the many decorative films, black and blue gives a mystery and profound feel, is an attractive color and is highly appreciated by consumers. Under the general condition, people often adopt a metal aluminum target and a titanium target to co-sputter, and simultaneously, the blue film is prepared and obtained by introducing nitrogen, but the L value in the Lab value of the color is larger, the brightness requirement cannot be met, and meanwhile, the corrosion resistance of the TiAlN film component is lower, and the corrosion resistance requirement of high-end electronic products cannot be met. Meanwhile, currently proposed black and blue films are prepared by adopting metal targets (chromium, titanium and the like) and carbon source gases (methane, acetylene and the like) through a PVD method, and the preparation method has certain defects in color debugging, and mainly comprises that the prepared product is not blue enough, cannot meet the demands of consumers, and is insufficient in wear resistance of a color film layer and the like.
Disclosure of Invention
The invention aims to overcome the technical defects and provide a black and blue PVD decorative film and a preparation method thereof, so as to solve the technical problems of insufficient color and poor wear resistance of the PVD decorative film in the prior art.
In order to achieve the technical purpose, the technical scheme of the invention provides a black and blue PVD decorative film and a preparation method thereof.
The black and blue PVD decorative film is deposited on the surface of a substrate, and comprises a priming layer, a transition layer and a color layer which are sequentially arranged, wherein the priming layer is a Cr layer and is arranged between the substrate and the transition layer for improving the adhesive force of a coating; the transition layer is CrSiC layers, the sum of Cr and Si atom contents in the transition layer is larger than C atom content, cr atom content is larger than Si atom content, and the transition layer is arranged between the priming layer and the color layer and is used for improving the binding force of the coating; the color layer is CrSiC layers, the sum of Cr and Si atom contents in the color layer is smaller than C atom content, cr atom content is smaller than Si atom content, and the black and blue tone can be controlled.
First, the sum of Cr and Si atom contents in the transition layer is larger than the C atom content, and the Cr atom content is larger than the Si atom content. This composition arrangement allows the transition layer to have a relatively high refractive index and to absorb a portion of light of a specific wavelength, especially red and green light. This results in the absence of red and green components in the light spectrum passing through the transition layer.
Next, the sum of the Cr and Si atom contents in the color layer is smaller than the C atom content, and the Cr atom content is smaller than the Si atom content. This allows the color layer to have a lower refractive index and to scatter the remaining light. Since the transition layer absorbs a portion of the red and green light, the blue component of the spectrum is relatively high after passing through the color layer. At the same time, the path of light reflected in the color layer increases due to the presence of scattering, resulting in the surface of the color layer appearing darker.
Thus, the blue-black color of the film surface is caused by the absorption of red and green light by the materials in the color layer and the scattering of blue light. This combination gives a relatively high blue component of the spectrum through the film, and a low red and green component, thus giving the appearance of black and blue.
Preferably, the thickness of the priming layer is 100-500 nm, the thickness of the transition layer is 300-1500 nm, and the thickness of the color layer is 300-1000 nm.
Preferably, the color value of the film is measured by a spectrophotometer, wherein the value of L is 35.08-40, the value of a is-0.71-0.45, the value of b is-5.45 to-1.08, L represents the brightness range of colors, a represents the color component from green to red, b represents the color component from blue to yellow, a is positive value for red, negative value for green, b is positive value for yellow, and negative value for blue.
Preferably, the substrate is made of one of stainless steel, glass and aluminum alloy.
The preparation method of the black and blue PVD decorative film based on the above comprises the following steps:
S1, cleaning a substrate: respectively ultrasonically cleaning in absolute ethyl alcohol and deionized water solution for 15 minutes, and then drying by a blower;
S2, loading the base material on a workpiece frame of a coating machine: starting a rotating frame system of the coating machine, setting the rotating speed to be 2-10 rpm, starting an air extraction system, pumping to the vacuum degree of 3-8 multiplied by 10 -3 Pa of a vacuum cavity, starting a heating system of the coating machine, and setting the temperature to be 100-300 ℃;
S3, performing ion cleaning on the base material in the vacuum cavity; the bias voltage applied to the workpiece is 400-1500V, the bias duty ratio is 20-80%, the Ar flow is 500-1200 sccm, the vacuum degree is 0.8-1.2 Pa, and the ion cleaning time is 10-60 min;
S4, adopting intermediate frequency magnetron sputtering to deposit the priming layer: introducing Ar flow of 300-600 sccm, vacuum degree of 0.3-0.6 Pa, workpiece bias voltage of 50-300V, bias duty ratio of 30-80%, medium frequency Cr target power of 5-15 kw, and performing first deposition on the cleaned substrate, wherein the time of the first deposition is 10-60 min, thus obtaining the substrate with a priming layer;
s5, depositing the transition layer by adopting medium-frequency magnetron sputtering; ar and carbon source gas 1 are introduced, the flow of Ar is 300-600sccm, the flow of the carbon source gas 1 gradually increases from 10sccm to 150-200 sccm, the vacuum degree is 0.3-0.6 Pa, the bias voltage of a workpiece is 50-300V, the bias duty ratio is 30-80%, a Cr target and a Si target are simultaneously started, the power of an intermediate frequency Cr target is 10-15 kw, the power of an intermediate frequency Si target is 5-10 kw, the second deposition is carried out on a substrate carrying a base layer, and the time of the second deposition is 30-120 min, so that the substrate carrying the base layer and a transition layer is obtained;
The sum of the Cr and Si atom contents in the transition layer is larger than the C atom content, the Cr atom content is larger than the Si atom content, the sum of the Cr and Si atom contents in the color layer is smaller than the C atom content, and the Cr atom content is smaller than the Si atom content. In order to achieve the above object, the C atom content is controlled by a carbon source gas, and the Cr to Si atom content is controlled by power. The initial flow rate of the carbon source gas 2 is the final flow rate of the carbon source gas 1. Wherein, the carbon source gas 1 and the carbon source gas 2 are one of C 2H2、CH4.
S6, adopting intermediate frequency magnetron sputtering to deposit the color layer: introducing Ar and carbon source gas 2, wherein the flow of Ar is 300-600sccm, the initial flow of the carbon source gas 2 is 150-200 sccm, the initial flow is gradually increased to 200-400 sccm, the vacuum degree is 0.3-0.6 Pa, the bias voltage of a workpiece is 50-300V, the bias duty ratio is 30-80%, meanwhile, a Cr target and a Si target are started, the power of an intermediate frequency Cr target is 3-10 kw, the power of an intermediate frequency Si target is 10-15 kw, and third deposition is carried out on the substrate carrying the underlayer and the transition layer, and the time of the third deposition is 20-90 min, so that the substrate carrying the underlayer, the transition layer and the color layer is obtained;
And S7, preserving the heat of the base material with the priming layer, the transition layer and the color layer in the vacuum cavity for 5-30 min to obtain the base material with the black and blue PVD decorative film.
Compared with the prior art, the invention has the beneficial effects that:
1. The invention adopts the magnetron sputtering technology to prepare and obtain the black-blue composite coating, the color of the coating is regarded as bluish black, the b value of the Lab value of the color is between-6 and-1, and the requirements of consumers on the special color of the black-blue can be met;
2. The process adopted by the invention is flexible and adjustable, a continuous black and blue gradient sample can be prepared and obtained by adjusting coating process parameters according to the need, the L value and the b value can be reduced by increasing the content of carbon source gas, the L value and the b value can be increased by increasing Cr power in a film layer, the Si power in the film layer can be increased, and the L value and the b value can be increased, so that the color values of the series are controllable and adjustable, and the stability is good, and the method is suitable for mass production;
3. the coating prepared by the invention is provided with the priming layer and the transition layer, so that the whole coating has good film-base binding force; the coating has good compactness through process control and bias voltage setting; the CrSiC coating has excellent wear resistance due to the amorphous structure and the high sp 3C-C bond content, thereby greatly prolonging the service life of the matrix and the film.
Drawings
FIG. 1 is a block diagram of a substrate carrying a black-and-blue PVD decorative film provided in an embodiment of the invention;
FIG. 2 is a further block diagram of a substrate carrying a black-blue PVD decorative film provided in accordance with an embodiment of the invention.
FIG. 3 is a block diagram of a substrate carrying a PVD decorative film provided in comparative example 4.
Wherein: 01-substrate, 02-primer, 03-transition, 04-color layer.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
As shown in FIG. 1, the black and blue PVD decorative film is deposited on the surface of stainless steel, and comprises a priming layer, a transition layer and a color layer which are sequentially arranged, wherein the priming layer is a Cr layer and is arranged between a base material and the transition layer for improving the adhesive force of the coating; the transition layer is CrSiC layers, the sum of Cr and Si atom contents in the transition layer is larger than C atom content, cr atom content is larger than Si atom content, and the transition layer is arranged between the priming layer and the color layer and is used for improving the binding force of the coating; the color layer is CrSiC layers, the sum of Cr and Si atom contents in the color layer is smaller than C atom content, cr atom content is smaller than Si atom content, and the black and blue tone can be controlled.
The control parameter of the film thickness is mainly time, the longer the time is, the thicker the film thickness is, the thickness of the base layer is 300nm, the thickness of the transition layer is 1000nm, and the thickness of the color layer is 700nm. The color value of the film is measured by a spectrophotometer.
The preparation method of the black and blue PVD decorative film based on the above comprises the following steps:
S1, cleaning a substrate: respectively ultrasonically cleaning in absolute ethyl alcohol and deionized water solution for 15 minutes, and then drying by a blower;
S2, loading the base material on a workpiece frame of a coating machine: starting a rotating frame system of the coating machine, setting the rotating speed to be 8rpm, starting an air extraction system, vacuumizing until the vacuum degree of a vacuum cavity is 5 multiplied by 10 -3 Pa, starting a heating system of the coating machine, and setting the temperature to be 160 ℃;
S3, performing ion cleaning on the base material in the vacuum cavity; the bias voltage applied to the workpiece is 1000V, the bias duty ratio is 60%, the Ar flow is 1000sccm, the vacuum degree is 1.0Pa, and the ion cleaning time is 30min;
S4, adopting intermediate frequency magnetron sputtering to deposit the priming layer: introducing Ar flow of 400sccm and vacuum degree of 0.5Pa, wherein the bias voltage of a workpiece is 200V, the bias duty ratio is 50%, the power of an intermediate frequency Cr target is 10kw, and performing first deposition on the cleaned substrate, wherein the time of the first deposition is 30min, so as to obtain the substrate carrying the priming layer;
S5, depositing the transition layer by adopting medium-frequency magnetron sputtering; introducing Ar and carbon source gas 1CH 4, wherein the flow rate of Ar is 500sccm, the flow rate of the carbon source gas 1 is increased from 10sccm to 200sccm, the vacuum degree is 0.5Pa, the bias voltage of a workpiece is 200V, the bias duty ratio is 50%, simultaneously starting a Cr target and a Si target, the power of the intermediate frequency Cr target is 15kw, the power of the intermediate frequency Si target is 10kw, performing second deposition on a substrate carrying a priming layer, and the time of the second deposition is 70min, thereby obtaining the substrate carrying the priming layer and a transition layer;
S6, adopting intermediate frequency magnetron sputtering to deposit the color layer: introducing Ar and carbon source gas 2CH 4, wherein the flow rate of Ar is 300-600 sccm, the flow rate of the carbon source gas 2 is increased from 200sccm to 300sccm, the vacuum degree is 0.5Pa, the bias voltage of a workpiece is 200V, the bias duty ratio is 50%, simultaneously starting a Cr target and a Si target, the power of the intermediate frequency Cr target is 3kw, the power of the intermediate frequency Si target is 10kw, and performing third deposition on the substrate carrying the primer layer and the transition layer, wherein the time of the third deposition is 55min, so as to obtain the substrate carrying the primer layer, the transition layer and the color layer;
And S7, preserving the heat of the base material with the priming layer, the transition layer and the color layer in the vacuum cavity for 20min to obtain the base material with the black and blue PVD decorative film.
Example 2
The black and blue PVD decorative film is deposited on the surface of a glass substrate and comprises a priming layer, a transition layer and a color layer which are sequentially arranged; the transition layer is CrSiC layers, the sum of Cr and Si atom contents in the transition layer is larger than the C atom content, and the Cr atom content is larger than the Si atom content; the sum of Cr and Si atom contents in the color layer is smaller than C atom content, and Cr atom content is smaller than Si atom content.
The thickness of the priming layer is 100nm, the thickness of the transition layer is 300nm, and the thickness of the color layer is 300nm.
The preparation method of the black and blue PVD decorative film based on the above comprises the following steps:
S1, cleaning a substrate: respectively ultrasonically cleaning in absolute ethyl alcohol and deionized water solution for 15 minutes, and then drying by a blower;
S2, loading the base material on a workpiece frame of a coating machine: starting a rotating frame system of the coating machine, setting the rotating speed to be 6rpm, starting an air extraction system, vacuumizing to a vacuum degree of 5X 10 -3 Pa of a vacuum cavity, starting a heating system of the coating machine, and setting the temperature to be 200 ℃;
S3, performing ion cleaning on the base material in the vacuum cavity; the bias voltage applied to the workpiece is 400V, the bias duty ratio is 20%, the Ar flow is 500sccm, the vacuum degree is 0.8Pa, and the ion cleaning time is 10min;
S4, adopting intermediate frequency magnetron sputtering to deposit the priming layer: introducing Ar flow of 300sccm, vacuum degree of 0.3Pa, workpiece bias voltage of 50V, bias duty ratio of 30%, intermediate frequency Cr target power of 5kw, and performing first deposition on the cleaned substrate for 10min to obtain a substrate carrying a priming layer;
S5, depositing the transition layer by adopting medium-frequency magnetron sputtering; introducing Ar and carbon source gas 1C 2H2 gas, wherein the flow rate of Ar is 300sccm, the flow rate of the carbon source gas 1 is increased from 10sccm to 150sccm, the vacuum degree is 0.3-0.6 Pa, the bias voltage of a workpiece is 50-300V, the bias duty ratio is 30-80%, simultaneously starting a Cr target and a Si target, the power of an intermediate frequency Cr target is 10-15 kw, the power of an intermediate frequency Si target is 5-10 kw, and performing second deposition on a substrate carrying a base layer, wherein the time of the second deposition is 30-120 min, so as to obtain the substrate carrying the base layer and a transition layer;
S6, adopting intermediate frequency magnetron sputtering to deposit the color layer: introducing Ar and carbon source gas 2C 2H2 gas, wherein the flow rate of Ar is 300sccm, the flow rate of the carbon source gas 2 is increased from 150sccm to 200sccm, the vacuum degree is 0.3Pa, the bias voltage of a workpiece is 50V, the bias duty ratio is 30%, meanwhile, a Cr target and a Si target are started, the power of the intermediate frequency Cr target is 3kw, the power of the intermediate frequency Si target is 10kw, third deposition is carried out on the substrate carrying the base layer and the transition layer, and the time of the third deposition is 20min, so that the substrate carrying the base layer, the transition layer and the color layer is obtained;
And S7, preserving the heat of the base material with the priming layer, the transition layer and the color layer in the vacuum cavity for 5-30 min to obtain the base material with the black and blue PVD decorative film.
Example 3
The black and blue PVD decorative film is deposited on the surface of an aluminum alloy substrate and comprises a priming layer, a transition layer and a color layer which are sequentially arranged; the sum of the atomic contents of Cr and Si in the transition layer is larger than the atomic content of C, and the atomic content of Cr is larger than the atomic content of Si; the sum of Cr and Si atom contents in the color layer is smaller than C atom content, and Cr atom content is smaller than Si atom content.
The thickness of the priming layer is 500nm, the thickness of the transition layer is 1500nm, and the thickness of the color layer is 1000nm.
The preparation method of the black and blue PVD decorative film based on the above comprises the following steps:
S1, cleaning a substrate: respectively ultrasonically cleaning in absolute ethyl alcohol and deionized water solution for 15 minutes, and then drying by a blower;
S2, loading the base material on a workpiece frame of a coating machine: starting a rotating frame system of the coating machine, setting the rotating speed to be 5rpm, starting an air extraction system, vacuumizing to a vacuum degree of 5X 10 -3 Pa of a vacuum cavity, starting a heating system of the coating machine, and setting the temperature to be 200 ℃;
S3, performing ion cleaning on the base material in the vacuum cavity; the bias voltage applied to the workpiece is 1500V, the bias duty ratio is 80%, the Ar flow is 1200sccm, the vacuum degree is 1.2Pa, and the ion cleaning time is 60min;
s4, adopting intermediate frequency magnetron sputtering to deposit the priming layer: introducing Ar flow of 600sccm, vacuum degree of 0.6Pa, workpiece bias voltage of 300V, bias duty ratio of 80%, intermediate frequency Cr target power of 15kw, and performing first deposition on the cleaned substrate, wherein the first deposition time is 60min, so as to obtain the substrate carrying the priming layer;
S5, depositing the transition layer by adopting medium-frequency magnetron sputtering; introducing Ar and carbon source gas 1C 2H2, wherein the flow rate of Ar is 600sccm, the flow rate of the carbon source gas 1 is increased from 10sccm to 190sccm, the vacuum degree is 0.6Pa, the bias voltage of a workpiece is 300V, the bias duty ratio is 80%, simultaneously starting a Cr target and a Si target, the power of the intermediate frequency Cr target is 15kw, the power of the intermediate frequency Si target is 10kw, performing second deposition on a substrate carrying a priming layer, and the time of the second deposition is 120min, thereby obtaining the substrate carrying the priming layer and a transition layer;
s6, adopting intermediate frequency magnetron sputtering to deposit the color layer: introducing Ar and carbon source gas 2C 2H2, wherein the flow rate of Ar is 300-600sccm, the flow rate of the carbon source gas 2 is increased from 190sccm to 400sccm, the vacuum degree is 0.6Pa, the bias voltage of a workpiece is 300V, the bias duty ratio is 80%, meanwhile, a Cr target and a Si target are started, the power of the intermediate frequency Cr target is 10kw, the power of the intermediate frequency Si target is 15kw, third deposition is carried out on the substrate carrying the priming layer and the transition layer, and the time of the third deposition is 90min, so that the substrate carrying the priming layer, the transition layer and the color layer is obtained;
and S7, insulating the base material with the priming layer, the transition layer and the color layer in a vacuum cavity for 30min to obtain the base material with the black and blue PVD decorative film.
Example 4
This embodiment is identical to embodiment 1, except that:
and S5, in the transition layer, the power of the intermediate frequency Cr target is 10kw, and the power of the intermediate frequency Si target is 5kw.
Example 5
This embodiment is identical to embodiment 1, except that:
In the step S6, in the color layer, the power of the intermediate frequency Cr target is 10kw, and the power of the intermediate frequency Si target is 15kw.
Comparative example 1
This comparative example is identical to example 1, except that in this comparative example, step S5 is not performed, i.e., deposition of the transition layer is not performed, and the structure of the resulting substrate carrying the black-and-blue PVD decorative film is shown in fig. 2.
Comparative example 2
This comparative example is the same as example 1 except that the flow rate of the carbon source gas 1 in S5 in this comparative example is 300sccm, the intermediate frequency Cr target power is 20kw, and the intermediate frequency Si target power is 20kw.
Comparative example 3
This comparative example is the same as example 1 except that the carbon source gas 2 in S6 of this comparative example was 500sccm, the intermediate frequency Cr target power was 15kw, and the intermediate frequency Si target power was 20kw.
Comparative example 4
The comparative example is the same as example 1, except that the coating layer in the comparative example is a primer layer and a color layer sequentially from bottom to top of the substrate, the primer layer is a Cr primer layer, the color layer is a CrC layer, and the preparation method in the comparative example does not have the step S5, S6, in the process of depositing the color layer by using intermediate frequency magnetron sputtering, the intermediate frequency target is only a Cr target, and there is no Si target. The structure of the substrate carrying the PVD decorative film in this comparative example is shown in FIG. 3.
The films on the substrates of the PVD decorative films prepared in examples 1 to 5 and comparative examples 1 to 4 described above were subjected to color and performance tests as follows;
Color test: measuring L, a and b of the sample by using a spectrophotometer, wherein L represents the brightness range of the color, a represents red by positive value, green by negative value, yellow by positive value and blue by negative value;
Hundred grid test: vertically cutting the test surface of the sample with a hundred-grid blade at uniform intervals of 1mm, and after cutting, carrying out drawing test by using a 3M adhesive tape, wherein the cutting-out and falling-off area of the coating is less than 5% for judging to be qualified;
Vibration abrasion resistance test: the samples were placed in a vibratory abrader and special wear particles were used to simulate the wear of the samples under normal use conditions. After testing 2H, judging that the surface coating of the sample is qualified if no falling exists;
72H salt spray test: and (3) spraying sodium chloride solution on the surface of the sample by using a salt water spray testing machine, wherein the concentration of sodium chloride is 5%, the testing temperature is 35 ℃, the PH value is 6.5-7.3, and the sample testing surface is judged to be qualified when the sample is tested for 72 hours without abnormal color and coating falling off.
The color and performance test results are shown in table 1;
TABLE 1 color and Performance test
The above-described embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (9)
1. The black and blue PVD decorative film is deposited on the surface of a substrate and is characterized by comprising a priming layer, a transition layer and a color layer which are sequentially arranged, wherein the priming layer is a Cr layer, the transition layer is CrSiC layers, the color layer is CrSiC layers, the sum of Cr and Si atom contents in the transition layer is larger than C atom content, cr atom content is larger than Si atom content, the sum of Cr and Si atom contents in the color layer is smaller than C atom content, and Cr atom content is smaller than Si atom content.
2. The black and blue PVD decorative film according to claim 1, wherein the thickness of the primer layer is 100-500 nm, the thickness of the transition layer is 300-1500 nm, and the thickness of the color layer is 300-1000 nm.
3. The black and blue PVD decorative film according to claim 1, wherein the film has a color value measured using a spectrophotometer having an L value of 35.08 to 40, an a value of-0.71 to 0.45, and a b value of-5.45 to-1.08, wherein L represents a lightness range of a color, a represents a color component from green to red, and b represents a color component from blue to yellow.
4. The black and blue PVD decorative film according to claim 1, wherein the substrate is one of stainless steel, glass, aluminum alloy.
5. A method for preparing a black and blue PVD decorative film according to claims 1-4, comprising the steps of:
s1, cleaning a substrate in a vacuum cavity by plasma;
S2, adopting intermediate frequency magnetron sputtering to deposit the priming layer: introducing Ar flow of 300-600 sccm, vacuum degree of 0.3-0.6 Pa, workpiece bias voltage of 50-300V, bias duty ratio of 30-80%, medium frequency Cr target power of 5-15 kw, and performing first deposition on the cleaned substrate, wherein the time of the first deposition is 10-60 min, thus obtaining the substrate with a priming layer;
S3, depositing the transition layer by adopting medium-frequency magnetron sputtering; introducing Ar and carbon source gas 1, wherein the flow rate of the carbon source gas 1 gradually increases from 10sccm to 150-200 sccm, simultaneously starting a Cr target and a Si target, wherein the power of the intermediate frequency Cr target is 10-15 kw, the power of the intermediate frequency Si target is 5-10 kw, and performing secondary deposition on a substrate carrying a priming layer, wherein the time of the secondary deposition is 30-120 min, so as to obtain the substrate carrying the priming layer and a transition layer;
S4, adopting intermediate frequency magnetron sputtering to deposit the color layer: introducing Ar and carbon source gas 2, wherein the initial flow of the carbon source gas 2 is 150-200 sccm, gradually increases to 200-400 sccm, simultaneously starts a Cr target and a Si target, the power of the intermediate frequency Cr target is 3-10 kw, the power of the intermediate frequency Si target is 10-15 kw, and carries out third deposition on the substrate carrying the priming layer and the transition layer, and the time of the third deposition is 20-90 min, thus obtaining the substrate carrying the priming layer, the transition layer and the color layer;
And S5, preserving the heat of the base material with the priming layer, the transition layer and the color layer in the vacuum cavity for 5-30 min to obtain the base material with the black and blue PVD decorative film.
6. The method of manufacturing a black and blue PVD decorative film according to claim 5, wherein the ion cleaning process in S1 is as follows, the workpiece is applied with a bias voltage of 400-1500V, a bias duty ratio of 20-80%, ar flow of 500-1200 sccm, vacuum degree of 0.8-1.2 Pa, and ion cleaning time of 10-60 min.
7. The method for preparing a black and blue PVD decorative film according to claim 5, wherein in the second deposition and the third deposition in S3, ar is introduced at a flow rate of 300-600 sccm, a vacuum degree of 0.3-0.6 Pa, a workpiece bias voltage of 50-300V, and a bias duty ratio of 30-80%.
8. The method of claim 5, wherein the initial amount of the carbon source gas 2 in S4 is the final amount of the carbon source gas 1 in S3.
9. The method of claim 5, wherein the carbon source gas 1 in S3 and the carbon source gas 2 in S4 are each one of C 2H2、CH4.
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| CN103305802B (en) * | 2013-07-05 | 2015-09-30 | 东明兴业科技股份有限公司 | Electronic product metallic surface PVD film and preparation method thereof |
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| CN110863173B (en) * | 2019-10-29 | 2022-08-12 | 富联科技(山西)有限公司 | PVD film layer, preparation method thereof and metal product with PVD film layer |
| US11719865B2 (en) * | 2020-03-11 | 2023-08-08 | Apple Inc. | Visible-light-reflecting coatings for electronic devices |
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| CN113046696A (en) * | 2020-06-23 | 2021-06-29 | 比亚迪股份有限公司 | Decorative material, preparation method thereof and electronic equipment |
| WO2022025033A1 (en) * | 2020-07-31 | 2022-02-03 | 東ソー株式会社 | Cr-Si-C-BASED SINTERED BODY |
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