CN108559950A - A kind of wear-resisting plated film of superhard water proof anti-soil, process for plating and its detection method - Google Patents

A kind of wear-resisting plated film of superhard water proof anti-soil, process for plating and its detection method Download PDF

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CN108559950A
CN108559950A CN201810523964.2A CN201810523964A CN108559950A CN 108559950 A CN108559950 A CN 108559950A CN 201810523964 A CN201810523964 A CN 201810523964A CN 108559950 A CN108559950 A CN 108559950A
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layer
test
film
color
wear
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李智超
毕文江
朱金波
郭富强
付勇
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Henan Dubang Photoelectric Co Ltd
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Henan Dubang Photoelectric Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021Reactive sputtering or evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641Nitrides
    • C23C14/0652Silicon nitride
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10Glass or silica
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/56Investigating resistance to wear or abrasion

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Abstract

The invention discloses a kind of superhard wear-resisting plated film of water proof anti-soil, including basal layer and the film layer, stain-proofing layer and the air dielectric layer that are sequentially arranged in above the basal layer, the base layer thickness is 0.05 ~ 0.8mm;The film layer is that silicon nitride and Si oxide are alternately arranged, and thickness is 300 ~ 650 nm;The antifouling layer thickness is 10 ~ 20mm;The air dielectric layer is the air dielectric of refractive index NA=1, wavelength X c=550nm;Color film layer is equipped between the film layer and the stain-proofing layer, the color film layer is champagne gold or silver color or sapphirine.Compared with prior art, present invention effect outstanding is that film layer itself provides not only gorgeous color, also has very high mechanical strength and corrosion resistance, is significantly improved to the use feel and durability of plating piece after stain-proofing layer is added.

Description

A kind of wear-resisting plated film of superhard water proof anti-soil, process for plating and its detection method
Technical field
The present invention relates to technical field of optical coating, and in particular to a kind of wear-resisting plated film of superhard water proof anti-soil, process for plating And its detection method.
Background technology
Recently, traditional glass material hand-set lid and fingerprint recognition material are gradually by the better ceramic base material of dielectric properties Substitution, however since the surface nature of ceramic material itself is relative complex, cannot using modes such as traditional plating or silk-screens Meet the appearance of plating piece day excelsior and resistance to usability.Vacuum coating technology involved by this patent can on a ceramic substrate by Layer deposition forms the superhard film for showing particular color, and institute's film plating layer changes film layer material and object with substrate surface firm connection Reason thickness can realize the specific color and luster and sense of touch of film surface;Color plates water proof anti-soil coating materials after realizing in film layer, to increase Strong durability and usage comfort.By optical vacuum coating technique realize it is a kind of suitable in ceramic bases volume production it is wear-resisting It wipes, non-fading antifouling color film is the more urgent and practical problem in the field.
Invention content
To solve drawbacks described above, the object of the present invention is to provide a kind of wear-resisting plated film of superhard water proof anti-soil, process for plating and Its detection method, make mobile fingerprint identification cover board color be multiple color, have superhard wear wiping, resistance to soda boiling, waterproof, it is antifouling and The performances such as resistance to sweat erosion.
It is a further object of the present invention to provide a kind of process for plating of the superhard wear-resisting plated film of water proof anti-soil.
Third object of the present invention is to provide a kind of detection methods of the superhard wear-resisting plated film of water proof anti-soil.
In order to achieve the above objectives, the technical solution adopted by the present invention is:A kind of wear-resisting plated film of superhard water proof anti-soil, including base The bottom and film layer being sequentially arranged in above the basal layer, stain-proofing layer and air dielectric layer, the base layer thickness be 0.05 ~ 0.8mm;The film layer is that silicon nitride and Si oxide are alternately arranged, and thickness is 300 ~ 650 nm;The antifouling thickness Degree is 10 ~ 20mm;The air dielectric layer is the air dielectric of refractive index NA=1, wavelength X c=550nm;The film layer with it is described Color film layer is equipped between stain-proofing layer, the color film layer is champagne gold or silver color or sapphirine.
Further, the basal layer is used as base material using ceramics.
The stain-proofing layer is prepared using fluoropolymer.
When the color film layer is champagne gold, the thicknesses of layers is 300-600nm.
When the color film layer is sapphirine, the thicknesses of layers is 300-500nm.
When the color film layer is silver color, the thicknesses of layers is 300-650nm.
A kind of plating method of the wear-resisting plated film of superhard water proof anti-soil, it is characterised in that include the following steps:
1)It chooses ceramics and is used as basal layer, and basal layer is wiped and cleaned up;
2)On membrane material to be plated after disk installation, ion cleaning is carried out, uses argon gas and oxygen when ion cleaning, flow is 10 ~ 40sccm, processing time are 60 ~ 180 seconds;
3)Under 4-10KW power, choose vacuum degree is Coating Materials after cleaning
3.0~4.5x10-3The condition of Pa, it is argon gas to select working gas, and flow is 200 ~ 400sccm, and reaction gas is oxygen, Oxygen flow is 200 ~ 350sccm, silicon atom and silicon compound molecule is formed in the atmosphere of argon gas and oxygen, in magnetic field and electricity A large amount of Ar+ ions are ionized out under the action of, by the bombardment of Ar+ ion pair Si target material surfaces, make Si ions and O ions or N Ions binding is combined into SiO in vacuum chamber2And Si3Nx(x=3~5);
4)According to the thickness of the membrane system formula and each layer that have set, pass through the establishment of sputter coating machine, Si oxide SiO2And silicon Nitride Si3Nx(x=3 ~ 5) are alternately arranged multilayer and splash down in substrate surface, are formed after orderly depositing in substrate surface Target layer on target layer plus plates color film layer, deposits fluorine in color film surface by resistance hot evaporation mode later Polymer stain-proofing layer, the stain-proofing layer can significantly improve the waterproof anti-fingerprint performance of plated film thin slice to Color influences very little.
Further, when sputter coating machine works, basal layer is hung on roller, the spatter film forming when roller rotates.
Finished product of present invention after the completion of plated film will pass through a series of stringent performance tests, and waterproof angle is greater than 110 degree, Waterproof angle is still higher than 90 degree after steel wool friction, rubber friction 2500cycles at loading 1Kg, salt spray test and artificial perspiration Liquid experiment proves that coated product has preferable corrosion resistance.
The beneficial effects of the invention are as follows:Base material is ceramics, and film layer is coated on the surface of material, the gloss of coated surface Degree and abrasion and corrosion resistance are functional, and coated surface is directly contacted with user after mobile phone module further assembles, stringent A problem that being not in still scratch, colour fading under the conditions of experiment test.Compared with prior art, present invention effect outstanding That film layer itself provides not only gorgeous color, also have very high mechanical strength and corrosion resistance, be added stain-proofing layer after it is right The use feel and durability of plating piece further increase.
Description of the drawings
Below according to accompanying drawings and embodiments, the structure and features of the present invention is further described.
Fig. 1 is the structural schematic diagram for the embodiment of the present invention 1.
Fig. 2 is the corresponding light splitting curve of film layer structure in Fig. 1.
Fig. 3 is the structural schematic diagram for the embodiment of the present invention 2.
Fig. 4 is the corresponding light splitting curve of film layer structure in Fig. 3.
Fig. 5 is the structural schematic diagram for the embodiment of the present invention 3.
Fig. 6 is the corresponding light splitting curve of film layer structure in Fig. 5.
In attached drawing 1,1. basal layers, 2. first film layers, 3. second film layers, 4. third membrane layer, 5. the 4th film layers, 6. the 5th films Layer, 7. the 6th film layers, 8. the 7th film layers, 9. the 8th film layers, 10. the 9th film layers, 11. the tenth film layers, 12. the 11st film layers, 13. Stain-proofing layer.
Specific implementation mode
Embodiment 1:The plated film has 11 tunics, and color film layer is that champagne is golden, by SiO2And Si3Nx(x=3 ~ 5) film layer is handed over Mistake arrangement obtains, with optimization Film Design formula
A/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/ SiO2/Si3Nx(x=3~5)/SiO2/ B/C, wherein A is ceramics, and as basal layer 1,2 to the 11st film layer 12 of the first film layer is divided It is not
SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/ Si3Nx(x=3~5)/SiO2, B is fluoropolymer(10~20nm), as stain-proofing layer 13, C is the air dielectric of refractive index NA=1, ginseng Examine wavelength X c=550nm, and list in order, the physical thickness of each film layer be followed successively by nm/20 A/150 ~ 200 ~ 70nm/20 ~ 60 nm /10~40 nm /20~60 nm /10~50 nm /10~40nm /10~30nm /30~70 nm /20~70nm /10~ Membrane system is worked out, then using ceramics as substrate in 30 nm/10 ~ 20nm/C with sputter coating machine by listing formulas sequence and thickness Layer, ionizes out a large amount of Ar+ ions under the action of magnetic field and electric field, by the bombardment of Ar+ ion pair Si target material surfaces, make Si from Son and O ions or N ions bindings, are combined into SiO in vacuum chamber2And Si3Nx(x=3~5);According to the membrane system formula that has set and The thickness of each layer passes through the establishment of sputter coating machine, Si oxide SiO2With silicon nitride Si3Nx(x=3 ~ 5) are alternately arranged multilayer It splashes down in substrate surface, target layer is formed after orderly depositing in substrate surface, plating champagne is added on target layer Golden color film layer deposits fluoropolymer stain-proofing layer, the stain-proofing layer pair by resistance hot evaporation mode in color film surface later Color influences very little can significantly improve the waterproof anti-fingerprint performance of plated film thin slice, and 11 film structures in the embodiment can be with It is condensed to 9 layers.
Embodiment 2:The plated film has 11 tunics, and color film layer is silver color, by SiO2And Si3Nx(x=3 ~ 5) film layer staggered row Row obtain, with optimization Film Design formula
A/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/ SiO2/Si3Nx(x=3~5)/SiO2/ B/C, A are ceramics, and as basal layer 1,2 to the 11st film layer 12 of the first film layer is respectively
SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/ Si3Nx(x=3~5)/SiO2, B is fluoropolymer(10~20nm), as stain-proofing layer 13, C is the air dielectric of refractive index NA=1, ginseng Examine wavelength X c=550nm, and list in order, the physical thickness of each film layer is followed successively by nm/10 of nm/20 A/10~20~50 Nm/30~60 of nm/50 of nm/100 of nm/50 of nm/10 of~30 nm/10~40~40~150~200~150 Film is worked out in nm/10 of nm/10 nm/40~80~30~20 nm/C with sputter coating machine by listing formulas sequence and thickness System, then using ceramics as basal layer, ionizes out a large amount of Ar+ ions under the action of magnetic field and electric field, passes through Ar+ ion pair Si targets The bombardment on material surface makes Si ions and O ions or N ions bindings, SiO is combined into vacuum chamber2And Si3Nx(x=3~5);Root According to the thickness of the membrane system formula and each layer that have set, pass through the establishment of sputter coating machine, Si oxide SiO2And silicon nitride Si3Nx(x=3 ~ 5) are alternately arranged multilayer and splash down in substrate surface, and target film is formed after orderly depositing in substrate surface Layer on target layer plus plates color film layer silver color, and it is poly- to deposit fluorine in color film surface by resistance hot evaporation mode later Object stain-proofing layer is closed, which can significantly improve the waterproof anti-fingerprint performance of plated film thin slice, the implementation to Color influences very little 11 film structures in example can be condensed to 7 layers.
Embodiment 3:The plated film has 7 tunics, and color film layer is sapphirine, by SiO2And Si3Nx(x=3 ~ 5) film layer is interlocked Arrangement obtains, with optimization Film Design formula A/SiO2/ Si3Nx(x=3~5) /SiO2/ Si3Nx(x=3~5)/SiO2/ Si3Nx (x=3~5) /SiO2/ B/C, A are ceramics, and as basal layer 1,2 to the 7th film layer 8 of the first film layer is respectively
SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2/Si3Nx(x=3~5)/SiO2, B is fluoropolymer(10~ 20nm), as stain-proofing layer 13, C is the air dielectric of refractive index NA=1, reference wavelength λ c=550nm, and list in order, each film The physical thickness of layer is followed successively by
A/10 ~ 40nm/50 ~ 100nm/120 ~ 200nm/10 ~ 50nm/10 ~ 40nm/10 ~ 30nm/100 ~ 200nm/10 ~ 20nm/C, With sputter coating machine membrane system, then using ceramics as basal layer, the work in magnetic field and electric field are worked out by listing formulas sequence and thickness A large amount of Ar+ ions are ionized out under, by the bombardment of Ar+ ion pair Si target material surfaces, make Si ions and O ions or N ion knots It closes, SiO is combined into vacuum chamber2And Si3Nx(x=3~5);According to the thickness of the membrane system formula and each layer that have set, by splashing Penetrate the establishment of coating machine, Si oxide SiO2With silicon nitride Si3Nx(x=3 ~ 5) are alternately arranged multilayer and splash down in substrate surface, Target layer is formed after orderly depositing in substrate surface, and plating color film layer sapphirine, Zhi Houtong are added on target layer It crosses resistance hot evaporation mode and deposits fluoropolymer stain-proofing layer in color film surface, which, can to Color influences very little The waterproof anti-fingerprint performance of plated film thin slice is significantly improved, 7 tunics of the embodiment can be extended to 9 tunics.
It needs to detect by some by plated film made from above-described embodiment 1 and embodiment 2, detection method includes following step Suddenly:
a)Vibrate friction testing:Sample is put into model R180/530 TE-30 vibration friction test equipment, survey within 2 hours Examination within 30 hours abrasive material time, does not allow mm2 or more the point abrasions of S=1 occur;
b)Rubber friction is tested:Using the erasing rubber of Minoan, apply the load of 1kg, friction velocity 40cycle/min, test Stroke 40mm back and forth tests 2500 back and forth, it is desirable that appearance coating is without falling off, and appearance coating color is without change in the coated surface of sample Change, water droplet angle >=90 degree after the test of AF plated films;
c)Pencil hardness test:Pencil-lead is tested using Mitsubishi(Ceramics:≥7H), with 750gf pressure, pencil-lead and surface to be measured Angle be 45 °, draw 5,10mm every long in position to be measured, each position of coated surface does not allow surface visible wiping occur Hinder or scratches;
d)Salt spray resistance is tested:In 35 DEG C ± 2 DEG C of closed environment, humidity>85%, the sodium chloride with mass concentration about 5% is molten Liquid(PH value is within the scope of 6.5-7.2)Brine spray continuously is carried out to sample;48 hours time;Have the needs of surface-treated layer into Row adhesive force is tested;Testing time is subject to the condition of each test object in qualification determination;Painting layer appearance is without exception, appearance It is peeled off without significant change, such as corrosion, discoloration and surface-treated layer;Adhesive force test is carried out after test, the faces AF adhesive force reaches 3B or more;
e)Simulate hand perspiration test:Non-dust cloth after manually sweat impregnates dabs sample surfaces 2min, and 2h is placed under normal temperature environment, Synthetic perspiration's configuration method:By 1.00 ± 0.01g urea, 5.00 ± 0.01g sodium chloride and 1.14 ± 0.02g or 940 ± 20 μ L DL-LACTIC ACID(>88%, analysis is pure)It pours into the water container of a 1000ml.900ml water recently distilleds are added and stir until adding Until all reagents entered are all completely dissolved.It is gently mixed and is carefully added into dilute ammonia solution(1%)Until reaching a stabilization PH value 6.50 ± 0.10.Solution is poured into the volumetric flask of 1000ml and distilled water is added until bottle is expired, appearance is no different after test Often, no deformation, without falling off, flawless, abnormal no discoloration etc. is qualified;
f)Boiling is tested, 80 DEG C ± 2 DEG C of pure water, by sample boiling 30min;Room temperature carries out adhesive force survey after 2 hours Examination.Appearance is without exception, and without falling off, flawless carries out adhesive force test after the abnormality tests such as no discoloration, and the faces AF adhesive force reaches 3B More than.
It needs to detect by some by plated film made from above-described embodiment 3, detection method includes the following steps:
1)AF wear-resisting tests:Before experiment, film-coated plate sample surface water droplet angle, the water droplet angle tested out are first tested>110 degree;It uses 0000# steel wool(BONSTAR), load-bearing 1000g, steel wool area 20mmx20mm are carried out with the speed of 60 cycles per minutes, are rubbed Stroke is wiped in 35-40mm, continuously friction 5000 recycles in film-coated plate sample surface;Water droplet angle before experiment>110 degree, water after experiment Drip angle>90 degree;
2)Steel wool+sweat test:Use 0000# steel wool (steel wool brand:BONSTAR), load-bearing 300g, steel wool area 20mmx20mm is added dropwise sweat 2ml or so in steel wool rubbing surface in test process, steel wool is kept fully to soak;Frictional direction It is parallel with steel wool direction;It is carried out with the speed of 60 cycles per minutes, friction stroke is in 25-30mm, in the cover board plated film table of sample Continuously friction 1000 recycles in face, water droplet angle before testing>110 degree, rear water droplet angle after experiment>70 degree;
3)Rubber friction is tested after sweat 48 hours:Product takes out after finishing artificial sweat 48 hours, and surface layer is wiped clean;Using special Use rubber(PINK PEARL R-33 pink, without sand), heavy burden 1000g;It is carried out with the speed of 60 cycles per minutes, friction row Journey 20mm or so, at continuous 1000 cycles that rub of the cover board coated surface of sample, water droplet angle before testing>110 degree, rear water after experiment Drip angle>80 degree;
4)Pencil hardness test:Mitsubishi's 6H pencils and 1000# sand paper are selected, it is in 90 degree of right angles to make the nib of pencil and sand paper plane, Pencil stub is worn into cylinder;Pencil is mounted on pencil hardness test machine, adjustment adds heavy burden 1Kgf, with 45 ± 1 ° The lines of 3 5-10mm long are marked in angle in the different location of sensor fingerprint sensitive surface, then wipe pencil with erasing rubber and draw Trace, not management and control trace are subject to superficial film corrugationless or breakage, water droplet angle >=105 degree after test;
5)Alkaline boiling test:With good mask, it gets out drug instrument;0.5g sodium chloride is weighed slowly to be put into beaker;It weighs 4.2g sodium bicarbonates are slowly added into beaker;0.1g sodium carbonate is weighed to be slowly added into beaker;Pure water is added into solution, uses Glass bar stirs 5min, instrument test pH value 8.8 ± 0.1;It is 100 DEG C of constant water bath box boilings to be put into temperature, is tested within 2 hours, For sample surface without changing colour, whitening, the point of appearance, bubble diameter are less than 0.5mm, and silk-screen layer is abnormal without corrugation and stripping;
6)Synthetic perspiration tests:It presses《Artificial sweat configuration guide book》The acid artificial sweat solution of configuration, PH=4.6 ± 0.1;With The non-dust cloth for impregnating artificial sweat solution, test specimen is wrapped up close, and sealing poly-bag is used in combination to seal, be placed on 55 ± 3 DEG C, 96H is stored in the climatic chamber of 90-95%RH;The solution of sample surface is dried, observed in 15min and is tested, test structure It is qualification to meet the following conditions:No film plating layer and printing layer fall off, and ceramic member is non-discolouring, does not crack;Product surface is without stain, oil Dirt generates or other abnormal appearances;Adhesive force reaches 3B(Fall off area 5%-15%), use 3M610 gummed papers;For plated film, surface Contact angle >=110 °.
Fingerprint instrument cover board of the color film provided by the invention for a series of smart terminal products such as mobile phones, the color of plating Not only film layer is secured for film, and color is gorgeous, while also having horizontal view angle and vertical angle of view solid colour, the non-discolouring spy of wide-angle Property, and the steel wool friction of requirements at the higher level can be met, the performance tests standard such as rubber friction also has waterproof, antifouling, wear-resisting The performances such as damage, resistance to sweat and alkali resistance boiling.
Corresponding technique and product are reliable and stable in the present invention, which can produce in enormous quantities, have filled up market sky In vain, the high demand of client is met.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair Change, replace, improve on an equal basis etc., it should be included within the scope of the present invention.

Claims (10)

1. a kind of wear-resisting plated film of superhard water proof anti-soil, it is characterised in that:Including basal layer and it is sequentially arranged in above the basal layer Film layer, stain-proofing layer and air dielectric layer, the base layer thickness be 0.05 ~ 0.8mm;The film layer is silicon nitride and silica Compound is alternately arranged, and thickness is 300 ~ 650 nm;The antifouling layer thickness is 10 ~ 20mm;The air dielectric layer is folding Penetrate the air dielectric of rate NA=1, wavelength X c=550nm;Color film layer, the color are equipped between the film layer and the stain-proofing layer Film layer is champagne gold or silver color or sapphirine.
2. the wear-resisting plated film of superhard water proof anti-soil according to claim 1, it is characterised in that:The basal layer is made using ceramics For base material.
3. the wear-resisting plated film of superhard water proof anti-soil according to claim 1, it is characterised in that:The stain-proofing layer is polymerize using fluorine It is prepared by object.
4. the wear-resisting plated film of superhard water proof anti-soil according to claim 1, it is characterised in that:The color film layer is champagne gold When, the thicknesses of layers is 300-600nm.
5. the wear-resisting plated film of superhard water proof anti-soil according to claim 1, it is characterised in that:The color film layer is sapphirine When, the thicknesses of layers is 300-500nm.
6. the wear-resisting plated film of superhard water proof anti-soil according to claim 1, it is characterised in that:The color film layer is silver color When, the thicknesses of layers is 300-650nm.
7. a kind of plating method of the wear-resisting plated film of superhard water proof anti-soil, it is characterised in that include the following steps:1)Ceramics are chosen to make For basal layer, and basal layer is wiped and cleaned up;2)On membrane material to be plated after disk installation, ion cleaning is carried out, from It is 10 ~ 40sccm that argon gas and oxygen, flow are used when son cleans, and processing time is 60 ~ 180 seconds;3)Plating membrane material after cleaning For material under 4-10KW power, selection vacuum degree is 3.0 ~ 4.5x10-3The condition of Pa, it is argon gas, flow 200 to select working gas ~ 400sccm, reaction gas are oxygen, and oxygen flow is 200 ~ 350sccm, and silicon atom is formed in the atmosphere of argon gas and oxygen With silicon compound molecule, a large amount of Ar+ ions are ionized out under the action of magnetic field and electric field, pass through Ar+ ion pair Si target material surfaces Bombardment, make Si ions and O ions or N ions bindings, SiO be combined into vacuum chamber2And Si3Nx(x=3~5);4)According to The thickness of the membrane system formula and each layer of setting passes through the establishment of sputter coating machine, Si oxide SiO2With silicon nitride Si3Nx(x= 3 ~ 5) it is alternately arranged multilayer to splash down in substrate surface, target layer is formed after orderly depositing in substrate surface, in mesh It marks in film layer plus plates color film layer, fluoropolymer stain-proofing layer is deposited in color film surface by resistance hot evaporation mode later, The stain-proofing layer can significantly improve the waterproof anti-fingerprint performance of plated film thin slice to Color influences very little.
8. the plating method of the wear-resisting plated film of superhard water proof anti-soil according to claim 4, it is characterised in that:Sputter coating machine When work, basal layer is hung on roller, the spatter film forming when roller rotates.
9. a kind of detection method of the wear-resisting plated film of superhard water proof anti-soil, it is characterised in that include the following steps:a)Vibration friction is surveyed Examination:Sample is put into model R180/530 TE-30 vibration friction test equipment, test within 2 hours, 30 hours abrasive material time Within, do not allow mm2 or more the point abrasions of S=1 occur;b)Rubber friction is tested:Using the erasing rubber of Minoan, apply 1kg's Load, friction velocity 40cycle/min test stroke 40mm, back and forth test 2500 back and forth in the coated surface of sample, it is desirable that appearance For coating without falling off, appearance coating color is unchanged, water droplet angle >=90 degree after the test of AF plated films;c)Pencil hardness test:Use three Water chestnut tests pencil-lead(Ceramics:≥7H), with 750gf pressure, pencil-lead and the angle on surface to be measured are 45 °, and 5 are drawn in position to be measured Pen, 10mm every long, each position of coated surface do not allow surface visible scratch occur or scratch;d)Salt spray resistance is tested: In 35 DEG C ± 2 DEG C of closed environment, humidity>85%, with the sodium chloride solution of mass concentration about 5%(PH value is in 6.5-7.2 ranges It is interior)Brine spray continuously is carried out to sample;48 hours time;Have surface-treated layer needs progress adhesive force test;When test Between be subject to the condition of each test object in qualification determination;Painting layer appearance is without exception, appearance without significant change, as corrosion, Discoloration and surface-treated layer peeling etc.;Adhesive force test is carried out after test, the faces AF adhesive force reaches 3B or more;e)Simulate hand perspiration Test:Non-dust cloth after manually sweat impregnates dabs sample surfaces 2min, and 2h, synthetic perspiration configuration side are placed under normal temperature environment Method:By 1.00 ± 0.01g urea, 5.00 ± 0.01g sodium chloride and 1.14 ± 0.02g or 940 ± 20 μ L DL-LACTIC ACIDs(> 88%, analysis is pure)It pours into the water container of a 1000ml, 900ml water recently distilleds are added and stir until what is be added is all Until reagent is all completely dissolved,
It is gently mixed and is carefully added into dilute ammonia solution(1%)Until reach a stable pH value 6.50 ± 0.10,
Solution is poured into the volumetric flask of 1000ml and distilled water is added until bottle is expired, appearance is without exception after test, no deformation, without de- It falls, flawless, no discoloration etc. is abnormal for qualification;f)Boiling is tested, 80 DEG C ± 2 DEG C of pure water, by sample boiling 30min;Often Temperature carries out adhesive force test after placing 2 hours,
Appearance is without exception, and without falling off, flawless carries out adhesive force test after the abnormality tests such as no discoloration, and the faces AF adhesive force reaches 3B or more.
10. the detection method of the wear-resisting plated film of superhard water proof anti-soil according to claim 8, when color film layer is sapphirine, The technical characteristic of its detection method, which also resides in, to be included the following steps:1)AF wear-resisting tests:Before experiment, film-coated plate sample table is first tested Face water droplet angle, the water droplet angle tested out>110 degree;Use 0000# steel wool(BONSTAR), load-bearing 1000g, steel wool area 20mmx20mm is carried out with the speed of 60 cycles per minutes, and friction stroke continuously rubs in 35-40mm in film-coated plate sample surface 5000 cycles;Water droplet angle before experiment>110 degree, water droplet angle after experiment>90 degree;2)Steel wool+sweat test:Use 0000# steel wires Suede (steel wool brand:BONSTAR), load-bearing 300g, steel wool area 20mmx20mm, in steel wool rubbing surface in test process Sweat 2ml or so is added dropwise, steel wool is kept fully to soak;Frictional direction is parallel with steel wool direction;With the speed of 60 cycles per minutes Degree carries out, and friction stroke is in 25-30mm, at continuous 1000 cycles that rub of the cover board coated surface of sample, water droplet angle before testing> 110 degree, rear water droplet angle after experiment>70 degree;3)Rubber friction is tested after sweat 48 hours:After product finishes artificial sweat 48 hours It takes out, surface layer is wiped clean;Use special eraser(PINK PEARL R-33 pink, without sand), heavy burden 1000g;It is followed with 60 The speed of ring/minute carries out, friction stroke 20mm or so, in continuous 1000 cycles that rub of the cover board coated surface of sample, experiment Preceding water droplet angle>110 degree, rear water droplet angle after experiment>80 degree;4)Pencil hardness test:Mitsubishi's 6H pencils and 1000# sand paper are selected, is made The nib of pencil and sand paper plane are in 90 degree of right angles, and pencil stub is worn into cylinder;Pencil is mounted on pencil hardness test machine On, adjustment adds heavy burden 1Kgf, and 3 5-10mm are marked in the different location of sensor fingerprint sensitive surface with 45 ± 1 ° of angles Then long lines wipe Pencil scratch with erasing rubber, not management and control trace, are subject to superficial film corrugationless or breakage, test Water droplet angle >=105 degree afterwards;5)Alkaline boiling test:With good mask, it gets out drug instrument;0.5g sodium chloride is weighed slowly to be put into In beaker;4.2g sodium bicarbonates are weighed to be slowly added into beaker;0.1g sodium carbonate is weighed to be slowly added into beaker;Add into solution Enter pure water, 5min, instrument test pH value 8.8 ± 0.1 are stirred with glass bar;It is 100 DEG C of constant water bath box boilings to be put into temperature, It tests within 2 hours, sample surface is without changing colour, whitening, and the point of appearance, bubble diameter are less than 0.5mm, and silk-screen layer is without corrugation and stripping Divorced is normal;6)Synthetic perspiration tests:It presses《Artificial sweat configuration guide book》The acid artificial sweat solution of configuration, PH=4.6 ± 0.1; With the non-dust cloth for impregnating artificial sweat solution, test specimen is wrapped up close, sealing poly-bag is used in combination to seal, be placed on 55 ± 3 DEG C, 96H is stored in the climatic chamber of 90-95%RH;The solution of sample surface is dried, observed in 15min and is tested, test structure It is qualification to meet the following conditions:No film plating layer and printing layer fall off, and ceramic member is non-discolouring, does not crack;Product surface is without stain, oil Dirt generates or other abnormal appearances;Adhesive force reaches 3B(Fall off area 5%-15%), use 3M610 gummed papers;For plated film, surface Contact angle >=110 °.
CN201810523964.2A 2018-05-28 2018-05-28 A kind of wear-resisting plated film of superhard water proof anti-soil, process for plating and its detection method Pending CN108559950A (en)

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CN110272215A (en) * 2019-05-23 2019-09-24 河南镀邦光电股份有限公司 A kind of superhard anti-reflection film process for plating of glass surface
CN111536909A (en) * 2020-04-20 2020-08-14 中物院成都科学技术发展中心 Method for detecting quality of film coating and quality of ultrasonic fastener
CN112267093A (en) * 2020-10-26 2021-01-26 蓝思科技(东莞)有限公司 Film coating method

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CN112267093A (en) * 2020-10-26 2021-01-26 蓝思科技(东莞)有限公司 Film coating method

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