CN109023280A - A kind of method that magnetron sputter prepares graduated colors film - Google Patents
A kind of method that magnetron sputter prepares graduated colors film Download PDFInfo
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- CN109023280A CN109023280A CN201811082012.8A CN201811082012A CN109023280A CN 109023280 A CN109023280 A CN 109023280A CN 201811082012 A CN201811082012 A CN 201811082012A CN 109023280 A CN109023280 A CN 109023280A
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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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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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
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
- C23C14/044—Coating on selected surface areas, e.g. using masks using masks using masks to redistribute rather than totally prevent coating, e.g. producing thickness gradient
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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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
- C23C14/35—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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- 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
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
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Abstract
The invention discloses a kind of methods that magnetron sputter prepares graduated colors film, include following steps: S1, optical coating design；S2, the design of shutter design the shape of shutter according to the thickness change of the optical thin-film structure of software simulation；S3, vacuum coating；S4, color and optical property are examined, and carry out color LAB value and visible reflectance curve, visible light transmittance curve detection to the product after vacuum coating, test result is qualified, then can carry out volume production preparation；Test result is unqualified, then in return step S1.The graduated colors film transition region color gradient prepared using this method can prepare the graduated colors film of different color and visual effect naturally, product colour is easily adjusted according to user's requirement.Compared to electron beam evaporation deposition, the film layer structure that magnetron sputter is coated with is fine and close, and stable refractive index, film layer optical property is more stable, thus colour stability is more preferable.
Description
Technical field
The invention belongs to technical field of vacuum plating, in particular to a kind of to be applied to mobile phone, tablet computer, smartwatch etc.
The method that the cover board of electronic product and the magnetron sputter of back-cover prepare graduated colors film.
Background technique
With the arriving of the 5th generation mobile communication technology (5G), more and more cell phone manufacturers are made using glass substituted metal
For the rear cover of mobile phone.Glass is generally colorless and transparent, needs ink for screen printing often as hand-set lid to colour for it.But only silk-screen oil
Ink, color glossiness is poor, also the not no metal-like of metal back cover.With the diversification of the market demand, glass cover-plate is not only
It plays a protective role, the function of beautifying and decorating is also increasingly prominent.For the aesthetic feeling for increasing mobile phone glass cover board, glass cover-plate production
Producer is coated with various high and low refractive index medium stacking film layers or part by optical film technique on transparent glass or diaphragm
Metallic diaphragm is to show different colours, such as blue, silver color, gold etc..In glass cover-plate back side silk-screen black ink, human eye institute
The color seen mainly is determined by the reflected colour of plating made membrane；In other color inks of glass cover-plate back side silk-screen, human eye institute
The color seen mainly is determined by the color that penetrates of the reflected colour of plating made membrane and its ink.
When light vertical incidence and when equivalent index of thin film is less than substrate of glass refractive index, film surface reflected light with it is thin
The reflected light of film and glass interface interferes effect, when 1/4 odd-multiple that the optical thickness of plating made membrane is a certain wavelength
When, two beams reflection light amplitude is identical, and it is contrary, thus there is interference cancellation phenomenon, the wave band color is not presented for reflected light；When
When the optical thickness of film is 1/4 even-multiple of a certain wavelength, occurs interfering and mutually increase phenomenon, the reflected light wave band color is most
By force.When light vertical incidence and when equivalent index of thin film is greater than substrate of glass refractive index, it may appear that opposite phenomenon, i.e., when thin
When the optical thickness of film is 1/4 odd-multiple of a certain wavelength, occurs interfering and mutually increase phenomenon, the reflected light wave band color is most strong；
When the optical thickness of film is 1/4 even-multiple of a certain wavelength, there is interference cancellation phenomenon, the wave band is not presented for reflected light
Color.When high extinction coefficient film layer is added in optical coating design, corresponding change can occur for optical absorption and reflecting properties,
The thickness of metallic film is adjusted, corresponding change will be generated to color saturation, brightness.
For magnetron sputtering, as shown in fig. 6, the distribution obedience gram of atom or atomic group that target as sputter comes out exerts increasing
At most, more toward both sides, distribution is fewer, i.e., off-target material center is closer, film thickness for the distribution of cosine law, i.e. target center position
Bigger, off-target material center is remoter, and film thickness is smaller.Target-substrate distance is bigger, and this influence is smaller, and target-substrate distance is smaller, this influence
It is bigger.
As mobile phone increasingly develops toward personalized, fashion-orientation direction, major mobile phone vendor commercial city is want in glass cover-plate color
On seek to break through, to lead industry trend.Realize that the gradual change of color is exactly a break-through point on glass cover-plate after mobile phone, i.e.,
The different saturation degree effect of different color or same color is presented along the position of the position to the other end of one end of hand-set lid,
Can gradual change along its length, can also in the width direction or other direction gradual changes.Realize the gradual change of color or saturation degree, just
It needs to deposit the deielectric-coating or metal film of different-thickness in workpiece different location.And the evaporation coating techniques of mainstream are due to certainly at present
The defect of body, can not be accurate and stablizes film layer in workpiece different location deposition different-thickness, thus can not stablize and be coated with gradual change
Color film, so electron beam evaporation deposition technology also just can not convert actual production by this innovative point for gradient color.Therefore, originally
Field, which needs one kind, can prepare graduated colors film transition region color gradient naturally, product colour is easily adjusted, can be according to user
It is required that preparing the preparation method of the graduated colors film of different color and visual effect.
In the patent application that number of patent application is CN201711211768.3, a kind of color gradient glass is disclosed, is wrapped
Glass body is included, the upper surface of the glass body is furnished with the film of at least two display different colours from center to outer peripheral portion
System, also discloses the production method of color gradient glass, the first area including the upper surface to glass body is blocked simultaneously
Deposit the membrane system with first kind color；The second area of the upper surface of the glass body is blocked and is deposited with
The membrane system of two class colors, the second area and central symmetry of the first area relative to the glass body.
But the preparation of gradient color disclosed above respectively will separately block first area and second area, it is also necessary to
Central symmetry, graduated colors form is fewer, and production is inconvenient.
Summary of the invention
To solve the above problems, the primary purpose of the present invention is that providing a kind of magnetron sputter prepares graduated colors film
Method, the graduated colors film transition region color gradient prepared using this method can be wanted according to user naturally, product colour is easily adjusted
Seek the graduated colors film for preparing different color and visual effect.Compared to electron beam evaporation deposition, film that magnetron sputter is coated with
Layer compact structure, stable refractive index, film layer optical property is more stable, thus colour stability is more preferable.
To achieve the above object, technical scheme is as follows.
A kind of method that magnetron sputter prepares graduated colors film, includes following steps:
S1, optical coating design establish the optical thin-film structure of simulation by optical coating design software；
S2, the design of shutter, the shutter are arranged between target and workpiece, the optical thin film simulated according to software
The thickness change of structure designs the shape of shutter；
S3, vacuum coating form optical thin-film structure by magnetron sputter sputtering target material on workpiece；
S4, color and optical property are examined, and carry out color LAB value to the product after vacuum coating and visible reflectance is bent
Line, visible light transmittance curve detection, test result is qualified, then can carry out volume production preparation；Test result is unqualified, then returns
In step S1；
Step S1 includes following steps:
S11, basic Film Design carry out workpiece end point position according to the graduated colors of workpiece and the demand of saturation degree
The basic Film Design set, and the thickness value of each film layer of optical thin-film structure needed for obtaining the position；
S12, gradation zone different location Film Design calculate not according to the graduated colors of workpiece and the demand of saturation degree
With the thickness value of each film layer of the optical thin-film structure of gradation zone, it is provided with spacing between different gradation zones, passes through reckoning
Method obtains the gradual change Film Design reflectivity or optical transmission spectra figure of entire workpiece；Wherein, projectional technique is the prior art.
Step S2 includes following steps:
S21 blocks the confirmation of target, according to the optical coating design in step S1 as a result, confirming the thickness of which film layer
Degree is variation in gradation zone, then between the target of this film layer and workpiece, is arranged one along the vertical direction of sputtering target material
Group shutter, if which film layer is remained unchanged in entire gradation zone thicknesses of layers, it is corresponding which does not need setting
Shutter；Shutter is arranged between a kind or a kind or more of target and workpiece；
S22 blocks the confirmation and adjustment of plate shape, long by the included thicknesses of layers of magnetron sputter and shutter first
The relation curve of degree fixes the shutter length of the maximum film layer position of thickness in each film layer, then passes through the light in step S1
Learn Film Design as a result, the thickness of the smallest film layer position of wherein thickness is calculated, with the maximum film layer position of wherein thickness
Thickness compare, calculate the film thickness difference of two positions, pass through the included thicknesses of layers of magnetron sputtering apparatus and shutter length
Relation curve, find out and block length at thicknesses of layers minimum, done along shutter longest and shortest line and be incremented by or pass
Subtract variation, or remains unchanged.
In the present invention, the workpiece can be the cover board and back of the electronic products such as mobile phone, tablet computer, smartwatch
Lid；The optical coating design software includes that TFCalc system design of optical film software, Macleod MacLeod are optically thin
Film design analysis software.The graduated colors film different color and visual effect needed according to user, can be set by optical film
Meter software establishes the optical thin-film structure of different simulations, calculates gradation zone from workpiece one end by optical coating design software
Position to another end position optical thin-film structure each film layer thickness change, according to the optical thin-film structure of software simulation
Thickness designs the shape of shutter, the optical thin-film structure of graduated colors film needed for user then finally can be made.
Graduated colors are realized by changing the optical property of gradation zone different location (as penetrated, absorbing or reflect)
, the thickness for the optical thin-film structure that the shape by changing shutter changes manufactured gradation zone different location becomes
Change, to change the optical property of gradation zone different location, to realize the graduated colors film of different color and visual effect.
By changing shape and the position of shutter, different fade effects may be implemented, matched by optical thin-film structure
The ink or diaphragm for closing various colors, can provide the fade effect of various colors for 3C Products such as mobile phones, it is more to meet market
The demand of sample, and the graduated colors film transition region color gradient prepared by above-mentioned this method is naturally, product colour is easily adjusted
Section, can prepare the graduated colors film of different color and visual effect according to user's requirement.Compared to electron beam evaporation deposition, magnetic control
The film layer structure that sputter is coated with is fine and close, and stable refractive index, film layer optical property is more stable, thus colour stability is more preferable.
Further, it in step S2, is determined between shutter and target and workpiece while designing the shape of shutter
Distance, according to the design result of each thicknesses of layers of the optical coating design in step S1, determine shutter and target and
The distance between workpiece.In the present invention, mainly realize that preparing different color and vision imitates by changing the shape of shutter
The graduated colors film of fruit can also form each film layer by changing shutter and the distance between target and workpiece to assist
Different-thickness, to influence fade effect.
Further, optical thin-film structure made of magnetron sputter establishes the optical thin-film structure packet on workpiece
Prime coat, high refractive index film layer, low refractive index film layer, high extinction coefficient film layer, protective layer are included, the prime coat is set
It sets on workpiece, the high refractive index film layer, low refractive index film layer are successively set on the prime coat, the high delustring
Coefficient film layer is arranged on the low refractive index film layer or high refractive index layer, and the protective layer is arranged in high extinction coefficient
In film layer；In step S3, bottom, high refractive index film is made by sputtering target material in the magnetron sputter on workpiece respectively
Layer, low refractive index film layer, high extinction coefficient film layer, protective layer.In the present invention, shutter can be set close to target
Position, also can be set close to workpiece position, by change shutter shape and position, thus it is possible to vary magnetron sputtering
Machine high refractive index film layer made of sputtering target material, low refractive index film layer, high extinction coefficient film layer thickness, can be with
It is incremented by corresponding film layer in different position thickness, corresponding film layer can also be made in different position thickness-tapereds, it can also
So that the thickness of corresponding film layer remains unchanged, the thickness of the different location by controlling above-mentioned different film layers, so that it may realize
The fade effect of different colors, meets the needs of market diversification；The setting of the prime coat improve workpiece with it is optically thin
Binding force between membrane structure, prevents optical thin-film structure from falling off from workpiece；The setting of protective layer is to protect high delustring system
Several layers are not easy to be destroyed.
Further, the prime coat is one of chromium, nickel, silicon, silica, aluminium oxide or a variety of；The prime coat
With a thickness of 0.1-50nm；
The high refractive index layer be one of titanium oxide, niobium oxide, zirconium oxide, chromium oxide, silicon nitride, tantalum oxide or
It is a variety of, between the shape and shutter and target and workpiece that the thickness change of the high refractive index layer passes through shutter away from
From control；
The low-index film is one of silica, aluminium oxide, and the thickness change of the low-index film is logical
The shape and shutter for crossing shutter are controlled with the distance between target and workpiece；
The high extinction coefficient film layer is one of indium, chromium, silicon, chromium carbide or a variety of, high extinction coefficient thicknesses of layers
For 0.01-100nm；The shape and shutter and magnetron sputtering that the thickness change of the high extinction coefficient film layer passes through shutter
The control of the distance between target and workpiece；
The protective layer is one of silica, aluminium oxide, niobium oxide, titanium oxide or a variety of, protective layer thickness 10-
100nm；
The high refractive index layer and low-index film are repeatable to be stacked as plural layer, constitute (HL) ^n film structure or
(HL) ^nH film structure, H represent high refractive index layer, and L represents low-index film, and n is number of repetition, and the value range of n is
1-10；
The material of the workpiece is one of glass, sapphire, plastics, stainless steel.
In the present invention, keep the stability of the optical thin-film structure more preferable by the setting of above-mentioned material, the gradual change of formation
Color film is more durable persistently, thus it is possible to vary magnetron sputter high refractive index film layer made of sputtering target material, low refraction
The thickness of rate film layer, high extinction coefficient film layer can be such that corresponding film layer is incremented by different position thickness, can also make
Corresponding film layer can also be such that the thickness of corresponding film layer remains unchanged in different position thickness-tapereds, above-mentioned by controlling
The thickness of the different location of different film layers, so that it may which the fade effect for realizing different colors meets the needs of market diversification.
Further, include following steps in step S3:
S31 is fixed on work rest after workpiece cleaning；
S32 is vacuumized, and will be evacuated to 9.0 × 10 in the machine cavity of magnetron sputter-3-1.0×10-3Pa；
S33, ion source cleaning, carries out ion source cleaning to workpiece under the vacuum condition, and used ion source is
Anode layer ion source；
S34 is coated with prime coat, and being passed through magnetron sputter cavity sputter gas flow is 100-800sccm, and prime coat is oxygen
When SiClx or aluminium oxide, also need to be passed through reaction gas flow to be 200-1000sccm, sputtering target material power is 5-30KW；It is coated with
After reaching the prime coat thickness designed in step 1, stop plated film；
S35, alternating are coated with n high refractive index layer and n low-index layer；It is coated with high refractive index layer first, is passed through magnetic control
Sputter cavity sputter gas flow is 100-800sccm, reaction gas flow 200-1000sccm, and sputtering target material power is
5-30KW；After being coated with the high refractive index layer thickness for reaching and designing in step 1, stops plated film, be then coated with low-index layer, be passed through
Magnetron sputter cavity sputter gas flow is 100-800sccm, reaction gas flow 200-1000sccm, sputtering target material function
Rate is 5-30KW；After being coated with the low-index layer thickness for reaching and designing in step 1, stop plated film；Continue to be coated with next high folding
Rate layer is penetrated, it is identical as a upper high refractive index layer to be coated with mode；After the completion of being coated with, continue to be coated with next low-index layer,
It is identical as a upper low-index layer to be coated with mode；And so on, until being coated with n high refractive index layer of completion and n low foldings
Rate layer is penetrated, plated film is stopped；
S36 is coated with high extinction coefficient layer；Being passed through magnetron sputter cavity sputter gas flow is 100-800sccm, reaction
Gas flow is 200-1000sccm, and sputtering target material power is 5-30KW；It is coated with the high extinction coefficient layer for reaching and designing in step 1
After thickness, stop plated film；
S37 is coated with protective layer；Being passed through magnetron sputter cavity sputter gas flow is 100-800sccm, reacting gas stream
Amount is 200-1000sccm, and sputtering target material power is 5-30KW；After being coated with the protective layer thickness for reaching and designing in step 1, stop
Plated film；
S38 after the completion of all film layers are coated with, makes deflation vacuum breaker in the machine cavity of magnetron sputter, and takes out plated film completion
Workpiece.
In the present invention, the model SWOS-2000H of the magnetron sputter of use, cardinal principle are that intermediate frequency reacts magnetic control
Sputtering, is arranged by above-mentioned plated film, keeps the film layer structure after being coated with fine and close, and stable refractive index, film layer optical property is more stable, because
And colour stability is more preferable.
Further, in step S4, the color LAB value and visible reflectance curve, visible light transmittance curve are adopted
It is detected with spectrophotometer, takes a point to be detected from one end of workpiece to the other end every 1-2cm.In the present invention, face
L* in color LAB value is lightness, and so-called lightness is exactly the light and shade of color, depth degree, it is specified that range is 0~100,0 to be most dark,
100 be most bright.A* is by green to red color change, range -128~128, it is pure it is green be -128, it is pure red to be positive 128.B* be by
Indigo plant is to yellow color change, and range -128~128, ethereal blue is -128, and true yellow is positive 128；By above-mentioned setting, make the knot of test
Fruit is more accurate.
Further, the target includes high refractive index target, low-refraction target, and high extinction coefficient target is described
Shutter can be placed in high refractive index target, low-refraction target, one of high extinction coefficient target, two or three of target with
Between workpiece.In the present invention, by shutter different location and setting of different shapes, different color gradients may be implemented
Effect, can satisfy the diversified demand of user.
Further, in step S12, the spacing being arranged between different gradation zones is 1-2cm.
Further, the sputter gas of the magnetron sputter cavity is high-purity argon gas；The magnetron sputter cavity
Reaction gas is high purity oxygen gas, high pure nitrogen, one of high purity acetylene.It in the present invention, can be more preferable by above-mentioned setting
User is made needed for graduated colors film.
The beneficial effects of the present invention are: compared with the prior art, in the present invention, by change shutter shape with
Different fade effects may be implemented in position, and the ink or diaphragm of various colors, Ke Yiwei are cooperated by optical thin-film structure
The 3C Products such as mobile phone provide the fade effect of various colors, meet the needs of market diversification, and pass through above-mentioned party's legal system
Standby graduated colors film transition region color gradient naturally, product colour is easily adjusted, can be prepared according to user's requirement different color and
The graduated colors film of visual effect.
Detailed description of the invention
Fig. 1 is the preparation flow figure for the method that magnetron sputter of the present invention prepares graduated colors film.
Fig. 2 is the structural schematic diagram of the optical thin-film structure for the method that magnetron sputter of the present invention prepares graduated colors film.
Fig. 3 is between the target, workpiece and shutter for the method that magnetron sputter of the present invention prepares graduated colors film
Location arrangements front view.
Fig. 4 is between the target, workpiece and shutter for the method that magnetron sputter of the present invention prepares graduated colors film
Location arrangements side view.
Fig. 5 is between the target, workpiece and shutter for the method that magnetron sputter of the present invention prepares graduated colors film
Location arrangements top view.
Fig. 6 is thicknesses of layers under different target-substrate distances on workpiece with the distribution map apart from target center position.
Fig. 7 is 1 schematic diagram of embodiment of one group of shutter of the method that magnetron sputter of the present invention prepares graduated colors film.
Fig. 8 is 2 schematic diagram of embodiment of one group of shutter of the method that magnetron sputter of the present invention prepares graduated colors film.
Fig. 9 is 3 schematic diagram of embodiment of one group of shutter of the method that magnetron sputter of the present invention prepares graduated colors film.
Figure 10 is the bluish-green to royal purple of the workpiece of the embodiment 1 for the method that magnetron sputter of the present invention prepares graduated colors film
The position gradual change 1-1 to 1-9 visible reflectance curve graph.
Figure 11 is that the workpiece different saturation of the embodiment 2 for the method that magnetron sputter of the present invention prepares graduated colors film is blue
The position color gradual change 1-1 to 1-9 visible light transmittance curve graph.
Figure 12 is that the workpiece different saturation of the embodiment 2 for the method that magnetron sputter of the present invention prepares graduated colors film is blue
The position color gradual change 1-1 to 1-9 visible reflectance curve graph.
Figure 13 is that the workpiece different saturation of the embodiment 3 for the method that magnetron sputter of the present invention prepares graduated colors film is blue
Green arrives the position yellow green gradual change 1-1 to 1-9 visible reflectance curve graph.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Referring to shown in Fig. 1-13, a kind of method that magnetron sputter prepares graduated colors film, includes following steps:
S1, optical coating design establish the optical thin-film structure of simulation by optical coating design software；
S2, the design of shutter 1, shutter 1 are arranged between target 2 and workpiece 3, the optical thin film simulated according to software
The thickness change of structure designs the shape of shutter 1；
S3, vacuum coating form optical thin-film structure on workpiece 3 by magnetron sputter sputtering target material 2；；
S4, color and optical property are examined, and carry out color LAB value to the product after vacuum coating and visible reflectance is bent
Line, visible light transmittance curve detection, test result is qualified, then can carry out volume production preparation；Test result is unqualified, then returns
In step S1；
Step S1 includes following steps:
S11, basic Film Design, the demand according to user to 3 graduated colors of workpiece and saturation degree carry out workpiece one end
Position 1-1 or 1-9 in the basic Film Design of point position, specific endpoint such as Fig. 3-4, and obtain optically thin needed for the position
The thickness value of each film layer of membrane structure；
S12, gradation zone different location Film Design, the demand according to user to 3 graduated colors of workpiece and saturation degree push away
The thickness value of each film layer of the optical thin-film structure of different gradation zones is calculated, spacing is provided between different gradation zones, passes through
Projectional technique obtains the gradual change Film Design reflectivity or optical transmission spectra figure of entire workpiece 3.In the present invention, according to user couple
The demand of 3 graduated colors of workpiece and saturation degree calculates gradation zone position 1- from such as Fig. 3-4 by optical coating design software
The thickness value of each film layer of 1 to position 1-9 optical thin-film structure, so that the adjustment of shape and position is carried out to shutter 1, from
And realize the fade effect of color different needed for user.
Step S2 includes following steps:
S21 blocks the confirmation of target 2, according to the optical coating design in step S1 as a result, confirming the thickness of which film layer
Degree is variation in gradation zone, then between the target of this film layer 2 and workpiece 3, is arranged along the vertical direction of sputtering target material 2
One group of shutter 1, if which film layer is remained unchanged in entire gradation zone thicknesses of layers, it is corresponding which does not need setting
Shutter 1；Shutter 1 is arranged between a kind or a kind or more of target 2 and workpiece 3；
S22, the confirmation and adjustment of 1 shape of shutter, the thicknesses of layers and shutter 1 carried first by magnetron sputter
The relation curve of length fixes 1 length of shutter of the maximum film layer position of thickness in each film layer, then by step S1
Optical coating design as a result, the thickness of the smallest film layer position of wherein thickness is calculated, with the maximum film layer position of wherein thickness
The thickness set compares, and calculates the film thickness difference of two positions, and the thicknesses of layers and shutter 1 carried by magnetron sputtering apparatus is long
The relation curve of degree is found out and blocks length at thicknesses of layers minimum, done along 1 longest of shutter and shortest line be incremented by or
Successively decrease variation, or remains unchanged.Fig. 7-9 is the shutter 1 of three groups of different size shapes, and the adjusting substrate thus amplified out is not
With position thicknesses of layers baffle within the protection scope of the present patent.
In the present invention, the optical coating design software include TFCalc system design of optical film software,
Macleod MacLeod's optical thin film design analyzes software.
The graduated colors film different color and visual effect needed according to user, can be built by optical coating design software
The optical thin-film structure for standing different simulations, by optical coating design software calculate gradation zone from 3 one end position of workpiece to
The thickness value of each film layer of the optical thin-film structure of another end position.It is set according to the thickness of the optical thin-film structure of software simulation
The shape and shutter 1 and the distance between target 2 and workpiece 3 of meter shutter 1, finally can then be made needed for user gradually
Become the optical thin-film structure of color film.
Graduated colors are realized by changing the optical property of gradation zone different location (as penetrated, absorbing or reflect)
, the shape by changing shutter 1 changes the thickness of the optical thin-film structure of manufactured gradation zone different location, from
And change the optical property of gradation zone different location, to realize the graduated colors film of different color and visual effect.
By changing shape and the position of shutter 1, different fade effects may be implemented, matched by optical thin-film structure
The ink or diaphragm for closing various colors, can provide the fade effect of various colors for 3C Products such as mobile phones, it is more to meet market
The demand of sample, and the graduated colors film transition region color gradient prepared by above-mentioned this method is naturally, product colour is easily adjusted
Section, can prepare the graduated colors film of different color and visual effect according to user's requirement.Compared to electron beam evaporation deposition, magnetic control
The film layer structure that sputter is coated with is fine and close, and stable refractive index, film layer optical property is more stable, thus colour stability is more preferable.
In the present embodiment, in step S2, shutter 1 and target 2 and work are determined while designing the shape of shutter 1
The distance between part 3, according to the design result of each thicknesses of layers of the optical coating design in step S1, determine shutter 1 with
The distance between target 2 and workpiece 3.In the present invention, mainly realize that preparation is not homochromy by changing the shape of shutter 1
Color and visual effect graduated colors film, can also be by changing shutter 1 with the distance between target 2 and workpiece 3 come auxiliary
It helps to form the thickness of different each film layers, to influence fade effect.
In the present embodiment, optical thin-film structure made of magnetron sputter establishes the optical thin-film structure packet on workpiece 3
Prime coat, high refractive index film layer, low refractive index film layer, high extinction coefficient film layer, protective layer are included, prime coat setting exists
On workpiece 3, high refractive index film layer, low refractive index film layer are successively set on prime coat, the setting of high extinction coefficient film layer
On low refractive index film layer or high refractive index layer, protective layer is arranged in high extinction coefficient film layer；In step S3, magnetic control
Bottom, high refractive index film layer, low refractive index film layer, high delustring is made by sputtering target material 2 in sputter on workpiece 3 respectively
Coefficient film layer, protective layer.
In the present invention, when high extinction coefficient film layer is added in optical coating design, optical absorption and reflecting properties
Corresponding change can occur, adjust the thickness of metallic film, corresponding change will be generated to color saturation, brightness；Realize color
Or the gradual change of saturation degree, it is necessary in the deielectric-coating or metal film of 3 different location of workpiece deposition different-thickness；The shutter 1
Shape and position can be adjusted according to required graduated colors film, film thickness can be made from the position of one end to another
The position at end is incremented by, and successively decreases, remains unchanged or other variation tendencies.Shutter 1 can be set in the position close to target 2,
It can be set in the position close to workpiece 3
By the shape and the position that change shutter 1, thus it is possible to vary magnetron sputter height made of sputtering target material 2 folding
The thickness for penetrating rate film layer, low refractive index film layer, high extinction coefficient film layer, can make corresponding film layer in different positions
Thickness is incremented by, and corresponding film layer can also be made in different position thickness-tapereds, the thickness of corresponding film layer can also be made to keep
It is constant, the thickness of the different location by controlling above-mentioned different film layers, so that it may realize the fade effect of different colors, meet
The demand of market diversification；The setting of prime coat improves the binding force between workpiece 3 and optical thin-film structure；Prevent optical thin film
Structure falls off from workpiece 3；The setting of protective layer is to protect high extinction coefficient layer to be not easy to be destroyed.
In the present embodiment, prime coat is one of chromium, nickel, silicon, silica, aluminium oxide or a variety of；Prime coat thickness
For 0.1-50nm；
High refractive index layer is one of titanium oxide, niobium oxide, zirconium oxide, chromium oxide, silicon nitride, tantalum oxide or more
Kind, the shape and shutter 1 and the distance between target 2 and workpiece 3 that the thickness change of high refractive index layer passes through shutter 1
Control；
Low-index film is one of silica, aluminium oxide, and the thickness change of low-index film passes through shutter 1
Shape and shutter 1 and the distance between target 2 and workpiece 3 control；
High extinction coefficient film layer is one of indium, chromium, silicon, chromium carbide or a variety of, and high extinction coefficient thicknesses of layers is
0.01-100nm；The shape and shutter and magnetic controlled sputtering target that the thickness change of the high extinction coefficient film layer passes through shutter
The control of the distance between material and workpiece 3；
Protective layer is one of silica, aluminium oxide, niobium oxide, titanium oxide or a variety of, protective layer thickness 10-
100nm；
High refractive index layer and low-index film, which repeat, is stacked as plural layer, constitutes (HL) ^n film structure or (HL)
^nH film structure, H represents high refractive index layer, and L represents low-index film, and n is number of repetition, and the value range of n is 1-
10；
The material of workpiece 3 is one of glass, sapphire, plastics, stainless steel.
In the present invention, keep the stability of the optical thin-film structure more preferable by the setting of above-mentioned material, the gradual change of formation
Color film is more durable persistently, thus it is possible to vary magnetron sputter high refractive index film layer made of sputtering target material 2, low refraction
The thickness of rate film layer, high extinction coefficient film layer can be such that corresponding film layer is incremented by different position thickness, can also make
Corresponding film layer can also be such that the thickness of corresponding film layer remains unchanged in different position thickness-tapereds, above-mentioned by controlling
The thickness of the different location of different film layers, so that it may which the fade effect for realizing different colors meets the needs of market diversification.
For magnetron sputtering, the distribution obedience gram of atom or atomic group that target 2 sputters out exerts increasing cosine law,
I.e. at most, more toward both sides, distribution is fewer, as shown in Figure 6 for the distribution of 2 center position of target.2 center of off-target material is closer, film
Thick bigger, 2 center of off-target material is remoter, and film thickness is smaller.Target-substrate distance is bigger, and this influence is smaller, and target-substrate distance is smaller, this shadow
Sound is bigger.If between sputtering target material 2 and workpiece 3, along the vertical direction of magnetic controlled sputtering target, i.e. axis direction, setting one
Group shutter 1 (as in Figure 3-5), adjusting shutter 1 length, by adjustable workpiece 3 from 1-1 to 1-9 different location
Film thickness, thus realize from 1-1 to 1-9 different location color adaptation.
In the present embodiment, include following steps in step S3:
S31, workpiece 3 are fixed on work rest 4 after cleaning；
S32 is vacuumized, and will be evacuated to 9.0 × 10 in the machine cavity of magnetron sputter-3-1.0×10-3Pa；
S33, ion source cleaning carry out ion source cleaning to workpiece 3 under vacuum conditions, and used ion source is anode
Leafing component；
S34 is coated with prime coat, and being passed through magnetron sputter cavity sputter gas flow is 100-800sccm, and prime coat is oxygen
When SiClx or aluminium oxide, also need to be passed through reaction gas flow to be 200-1000sccm, 2 power of sputtering target material is 5-30KW；Plating
After system reaches the prime coat thickness designed in step 1, stop plated film；
S35, alternating are coated with n high refractive index layer and n low-index layer；It is coated with high refractive index layer first, is passed through magnetic control
Sputter cavity sputter gas flow is 100-800sccm, reaction gas flow 200-1000sccm, 2 power of sputtering target material
For 5-30KW；After being coated with the high refractive index layer thickness for reaching and designing in step 1, stop plated film, be then coated with low-index layer, leads to
Entering magnetron sputter cavity sputter gas flow is 100-800sccm, reaction gas flow 200-1000sccm, sputtering target material
2 power are 5-30KW；After being coated with the low-index layer thickness for reaching and designing in step 1, stop plated film；Continue to be coated with next high
It is identical as a upper high refractive index layer to be coated with mode for index layer；After the completion of being coated with, continue to be coated with next low-refraction
Layer, it is identical as a upper low-index layer to be coated with mode；And so on, until it is low with n to be coated with n high refractive index layer of completion
Index layer stops plated film；
S36 is coated with high extinction coefficient layer；Being passed through magnetron sputter cavity sputter gas flow is 100-800sccm, reaction
Gas flow is 200-1000sccm, and 2 power of sputtering target material is 5-30KW；It is coated with the high extinction coefficient for reaching and designing in step 1
After thickness degree, stop plated film；
S37 is coated with protective layer；Being passed through magnetron sputter cavity sputter gas flow is 100-800sccm, reacting gas stream
Amount is 200-1000sccm, and 2 power of sputtering target material is 5-30KW；After being coated with the protective layer thickness for reaching and designing in step 1, stop
Plated film；
S38 after the completion of all film layers are coated with, makes deflation vacuum breaker in the machine cavity of magnetron sputter, and takes out plated film completion
Workpiece 3.
In the present invention, the model SWOS-2000H of the magnetron sputter of use, cardinal principle are that intermediate frequency reacts magnetic control
Sputtering, is arranged by above-mentioned plated film, keeps the film layer structure after being coated with fine and close, and stable refractive index, film layer optical property is more stable, because
And colour stability is more preferable.
In the present embodiment, in step S4, color LAB value and visible reflectance curve, visible light transmittance curve are adopted
It is detected with spectrophotometer, takes a point to be detected from one end of workpiece 3 to the other end every 1-2cm.In the present invention, face
L* in color LAB value is lightness, and so-called lightness is exactly the light and shade of color, depth degree, it is specified that range is 0~100,0 to be most dark,
100 be most bright.A* is by green to red color change, range -128~128, it is pure it is green be -128, it is pure red to be positive 128.B* be by
Indigo plant is to yellow color change, and range -128~128, ethereal blue is -128, and true yellow is positive 128；By above-mentioned setting, make the knot of test
Fruit is more accurate.
In the present embodiment, target 2 includes high refractive index target, low-refraction target, and high extinction coefficient target blocks
Plate 1 can be placed in high refractive index target, low-refraction target, one of high extinction coefficient target, two or three of target and work
Between part 3.In the present invention, by 1 different location of shutter and setting of different shapes, different color gradients may be implemented
Effect, can satisfy the diversified demand of user.
In the present embodiment, in step S12, the spacing being arranged between different gradation zones is 1-2cm.
In the present embodiment, the sputter gas of magnetron sputter cavity is high-purity argon gas；The reaction of magnetron sputter cavity
Gas is high purity oxygen gas, and high pure nitrogen, one of high purity acetylene, the material of workpiece 3 is glass, in plastics, diaphragm, stainless steel
One kind.In the present invention, by above-mentioned setting, graduated colors film needed for user capable of being preferably made.
The beneficial effects of the present invention are: compared with the prior art, in the present invention, by the shape for changing shutter 1
With position, different fade effects may be implemented, the ink or diaphragm of various colors are cooperated by optical thin-film structure, it can be with
The fade effect of various colors is provided for 3C Products such as mobile phones, meets the needs of market diversification, and pass through above-mentioned this method
The graduated colors film transition region color gradient of preparation can prepare different color according to user's requirement naturally, product colour is easily adjusted
With the graduated colors film of visual effect.Compared to electron beam evaporation deposition, the film layer structure that magnetron sputter is coated with is fine and close, refraction
Rate is stablized, and film layer optical property is more stable, thus colour stability is more preferable.
The method for preparing graduated colors film to magnetron sputter below in conjunction with specific embodiment is specifically described.
Embodiment 1
Sputter used in the present embodiment is SWOS-2000H large size magnetron sputter.
Firstly, the glass cover-plate that will be cleaned up, i.e. workpiece 3, are placed on sputter work rest 4, wherein high refractive index target
Material, low-refraction target and the placement schematic diagram of workpiece 3 and shutter 1 are as in Figure 3-5, shutter 1 and high refractive index target
The distance between material and low-refraction target are 2cm, and the distance between shutter 1 and workpiece 3 are 13cm.2 groups of 1 shapes of shutter
Shape is all made of shape shown in Fig. 7, is respectively placed between high refractive index target and low-refraction target and workpiece 3.It closes the door and is evacuated
To 5.0 × 10-3Pa carries out Ion Cleaning 10 minutes to workpiece 3 with anode layer ion source before plated film.
After anode layer Ion Cleaning, starts plated film, be coated with prime coat on workpiece 3 first, it is high that next is coated with first
Refractivity film layer, is then coated with the first low-index film, is then coated with the second high refractive index layer, is finally coated with the second low folding
Penetrate rate film layer.Wherein, prime coat is silica coating, and the first high refractive index layer and the second high refractive index layer are niobium oxide
Film layer, the first low-index film and the second low-index film are silica coating, prime coat with a thickness of 10nm, first
High refractive index layer with a thickness of 52nm, the second high refractive index layer with a thickness of 49nm, the thickness of the first low-index film
For 34nm, the second low-index film with a thickness of 5nm.
Wherein, the argon flow that plating niobium oxide film layer is passed through sputter cavity is 500sccm, is passed through reaction gas oxygen stream
Amount is 700sccm；The argon flow that applying silicon oxide is passed through is 300sccm, and being passed through reaction gas oxygen flow is 500sccm.
After plated film, vacuum chamber is deflated, and the workpiece 3 plated is taken out, with spectrophotometer measurement 1-9 as shown in Figure 3-4
To the 9 position visible reflectance curves and L*, a*, b* value of 1-9.Figure 10 is reflectance curve measured by embodiment 1.
Table 1 is the L* of 9 positions of 1-9 to 1-9, a*, b* value
| Position | L* | A* | B* |
| 1-1 | 64.4 | -11.3 | -18.8 |
| 1-2 | 62.5 | -10.9 | -21.5 |
| 1-3 | 60.4 | -10.3 | -24.2 |
| 1-4 | 58.2 | -9.3 | -26.9 |
| 1-5 | 55.8 | -7.9 | -29.7 |
| 1-6 | 53.3 | -6.1 | -32.5 |
| 1-7 | 50.6 | -3.6 | -35.3 |
| 1-8 | 47.7 | -0.45 | -38 |
| 1-9 | 44.9 | 3.32 | -40.4 |
From Figure 10 and table 1 as can be seen that from position 1-1 to position 1-9, reflectivity curve is gradually to short wave mobile, L* value
It gradually becomes smaller, a* value is gradually increased, and b* value is gradually reduced, and illustrates that, from position 1-1 to position 1-9, color gradually turns from blue-green
Become bluish violet.Therefore, graduated colors film prepared by the method for graduated colors film is prepared using magnetron sputter of the invention,
It can be realized the effect that bluish violet is gradually converted into from blue-green.
Embodiment 2
Firstly, the glass cover-plate that will be cleaned up, i.e. workpiece 3, are placed on sputter work rest 4, wherein high extinction coefficient
Shutter 1 as shown in Figure 7 is placed between target and substrate of glass, the distance between shutter 1 and high extinction coefficient target are
4cm, the distance between shutter 1 and workpiece 3 are 11cm, unobstructed plate 1 between other targets 2 and workpiece 3.1 shape of shutter
Shape is all made of shape shown in Fig. 7, and shutdown is pumped to 5.0 × 10-3Pa, before plated film with anode layer ion source to workpiece 3 carry out from
Son cleaning 10 minutes.
After anode layer Ion Cleaning, starts plated film, be coated with prime coat on workpiece 3 first, it is high that next is coated with first
Refractivity film layer, is then coated with the first low-index film, is then coated with the second high refractive index layer, is coated with the second low folding later
Rate film layer is penetrated, high extinction coefficient film layer is then coated with, is finally coated with protective layer.Wherein, prime coat is aluminum oxide film layer, the
One high refractive index layer and the second high refractive index layer are columbium oxide film layer, the first low-index film and the second low-refraction
Film layer is silica membrane layer, and high extinction coefficient film layer is indium film layer, and protective layer is silicon oxide film layer, prime coat
With a thickness of 5nm, the first high refractive index layer with a thickness of 44nm, the second high refractive index layer with a thickness of 46nm, the first low folding
Penetrate rate film layer with a thickness of 84nm, the second low-index film with a thickness of 5nm, high extinction coefficient film layer with a thickness of
54nm, protective layer with a thickness of 40nm.
Wherein, the argon flow that plating niobium oxide film layer is passed through sputter cavity is 300sccm, is passed through reaction gas oxygen stream
Amount is 400sccm；The argon flow that applying silicon oxide is passed through is 400sccm, and being passed through reaction gas oxygen flow is 600sccm.
After plated film, vacuum chamber is deflated, and the workpiece 3 plated is taken out, with spectrophotometer measurement 1-9 as in Figure 3-5
To the 9 position visible reflectance curves and visible light transmittance curve of 1-9.Figure 11 is the visible reflectance curve of measurement,
Figure 12 is the visible light transmittance curve of measurement.From Figure 11 and Figure 12 as can be seen that from position 1-1 to position 1-9, reflectivity
Curve gradually decreases, and transmittance curve gradually rises.Illustrate that, from position 1-1 to position 1-9, never transparent blue is transitioned into color
Semi-transparent blue eventually becomes transparent blue.Prepared by embodiment 2 is a kind of blue of transmitance gradual change.Therefore, this hair is used
Bright magnetron sputter prepares graduated colors film prepared by the method for graduated colors film, can be realized never transparent blue transition
To the effect of the transmitance gradual change of semi-transparent blue.
Embodiment 3
Firstly, the glass cover-plate that will be cleaned up, i.e. workpiece 3, are placed on sputter work rest 4, wherein in low-refraction
Shutter 1 as shown in Figure 8 is placed between target and workpiece 3, the distance between shutter 1 and low-refraction target are 5cm, are blocked
The distance between plate 1 and workpiece 3 are 10cm, are not provided with shutter 1 between other targets 2 and workpiece 3.1 shape of shutter is equal
Using shape shown in Fig. 8, shutdown is pumped to 5.0 × 10-3It is clear with anode layer ion source to carry out ion to workpiece 3 before plated film by Pa
It washes 10 minutes.
After anode layer Ion Cleaning, starts plated film, be coated with prime coat on workpiece 3 first, it is high that next is coated with first
Refractivity film layer, is then coated with the first low-index film, is then coated with the second high refractive index layer, is finally coated with the second low folding
Penetrate rate film layer.Wherein, prime coat is aluminum oxide film layer, and the first high refractive index layer and the second high refractive index layer are titanium oxide
Film layer, the first low-index film and the second low-index film are silica membrane layer, prime coat with a thickness of 8nm,
First high refractive index layer with a thickness of 118.9nm, the second high refractive index layer with a thickness of 32nm, the first low-index film
With a thickness of 20.3nm, the second low-index film with a thickness of 10nm.
Wherein, the argon flow that plating thin film of titanium oxide layer is passed through sputter cavity is 400sccm, is passed through reaction gas oxygen
Flow is 500sccm；The argon flow that applying silicon oxide is passed through is 400sccm, and being passed through reaction gas oxygen flow is
600sccm。
After plated film, vacuum chamber is deflated, and takes out the workpiece 3 plated, extremely with spectrophotometer measurement 1-9 as shown in Figure 3
9 position visible reflectance curves of 1-9.Figure 13 is the visible reflectance curve of measurement.As can be seen from Figure 13, from position
1-1 to position 1-9, reflectivity curve is gradually mobile to long wave direction, illustrates from position 1-1 to position 1-9, color from blue-green by
Gradually it is changed into yellow green.Therefore, gradual change face prepared by the method for graduated colors film is prepared using magnetron sputter of the invention
Color film can be realized the effect that yellow green is gradually converted into from blue-green.
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within principle.
Claims (8)
1. a kind of method that magnetron sputter prepares graduated colors film, it is characterised in that include following steps:
S1, optical coating design establish the optical thin-film structure of simulation by optical coating design software；
S2, the design of shutter, the shutter are arranged between target and workpiece, the optical thin-film structure simulated according to software
Thickness change design the shape of shutter；
S3, vacuum coating form optical thin-film structure by magnetron sputter sputtering target material on workpiece；
S4, color and optical property are examined, to the product after vacuum coating carry out color LAB value and visible reflectance curve,
Visible light transmittance curve detection, test result is qualified, then can carry out volume production preparation；Test result is unqualified, then returns to step
In rapid S1；
Step S1 includes following steps:
S11, basic Film Design carry out a certain endpoint location of workpiece according to the graduated colors of workpiece and the demand of saturation degree
Basic Film Design, and the thickness value of each film layer of optical thin-film structure needed for obtaining the position；
S12, gradation zone different location Film Design calculate difference gradually according to the graduated colors of workpiece and the demand of saturation degree
Become the thickness value of each film layer of the optical thin-film structure in region, is provided with spacing between different gradation zones, passes through projectional technique
Obtain the gradual change Film Design reflectivity or optical transmission spectra figure of entire workpiece；
Step S2 includes following steps:
S21 blocks the confirmation of target, according to the optical coating design in step S1 as a result, confirming that the thickness of which film layer exists
Gradation zone is variation, then between the target of this film layer and workpiece, one group of screening is arranged along the vertical direction of sputtering target material
Baffle, if which film layer is remained unchanged in entire gradation zone thicknesses of layers, which does not need setting and blocks accordingly
Plate；Shutter is arranged between a kind or a kind or more of target and workpiece；
S22 blocks the confirmation and adjustment of plate shape, passes through the included thicknesses of layers of magnetron sputter and shutter length first
Relation curve fixes the shutter length of the maximum film layer position of thickness in each film layer, then passes through the optical film in step S1
It is designing as a result, calculating the thickness of the smallest film layer position of wherein thickness, the thickness with the maximum film layer position of wherein thickness
Degree compares, and calculates the film thickness difference of two positions, the pass of the thicknesses of layers and shutter length that are carried by magnetron sputtering apparatus
It is curve, finds out and block length at thicknesses of layers minimum, does increasing or decreasing change along shutter longest and shortest line
Change, or remains unchanged.
2. the method that magnetron sputter according to claim 1 prepares graduated colors film, it is characterised in that in step S2, if
Shutter and the distance between target and workpiece are determined while counting the shape of shutter, according to the optical film in step S1
The design result of each thicknesses of layers of design, determines shutter and the distance between target and workpiece.
3. the method that magnetron sputter according to claim 2 prepares graduated colors film, it is characterised in that magnetron sputter
Manufactured optical thin-film structure is established on workpiece, and the optical thin-film structure includes prime coat, high refractive index film layer, low
Index film layer, high extinction coefficient film layer, protective layer, the prime coat are arranged on workpiece, the high refractive index film
Layer, low refractive index film layer are successively set on the prime coat, and the high extinction coefficient film layer is arranged in the low refraction
In rate film layer or high refractive index layer, the protective layer is arranged in high extinction coefficient film layer；In step S3, the magnetic control
Bottom, high refractive index film layer, low refractive index film layer, high delustring system is made by sputtering target material in sputter on workpiece respectively
Number film layer, protective layer.
4. the method that magnetron sputter according to claim 3 prepares graduated colors film, it is characterised in that the prime coat
For one of chromium, nickel, silicon, silica, aluminium oxide or a variety of；The prime coat is with a thickness of 0.1-50nm；
The high refractive index layer is one of titanium oxide, niobium oxide, zirconium oxide, chromium oxide, silicon nitride, tantalum oxide or more
Kind, the shape and shutter and the distance between target and workpiece that the thickness change of the high refractive index layer passes through shutter
Control；
The low-index film is one of silica, aluminium oxide, and the thickness change of the low-index film passes through screening
The shape and shutter and the distance between target and workpiece of baffle control；
The high extinction coefficient film layer is one of indium, chromium, silicon, chromium carbide or a variety of, and high extinction coefficient thicknesses of layers is
0.01-100nm；The shape and shutter and magnetic controlled sputtering target that the thickness change of the high extinction coefficient film layer passes through shutter
The control of the distance between material and workpiece；
The protective layer is one of silica, aluminium oxide, niobium oxide, titanium oxide or a variety of, protective layer thickness 10-
100nm；
The high refractive index layer and low-index film, which repeat, is stacked as plural layer, constitutes (HL) ^n film structure or (HL)
^nH film structure, H represent high refractive index layer, and L represents low-index film, and n is number of repetition, and the value range of n is 1-
10；
The material of the workpiece is one of glass, sapphire, plastics, stainless steel.
5. the method that magnetron sputter according to claim 4 prepares graduated colors film, it is characterised in that in step S3, packet
Include following steps:
S31 is fixed on work rest after workpiece cleaning；
S32 is vacuumized, and will be evacuated to 9.0 × 10 in the machine cavity of magnetron sputter-3-1.0×10-3Pa；
S33, ion source cleaning carry out ion source cleaning to workpiece under the vacuum condition, and used ion source is anode
Leafing component；
S34 is coated with prime coat, and being passed through magnetron sputter cavity sputter gas flow is 100-800sccm, and prime coat is silica
Or when aluminium oxide, also need to be passed through reaction gas flow to be 200-1000sccm, sputtering target material power is 5-30KW；It is coated with and reaches
After the prime coat thickness designed in step 1, stop plated film；
S35, alternating are coated with n high refractive index layer and n low-index layer；It is coated with high refractive index layer first, is passed through magnetron sputtering
Machine cavity body sputter gas flow is 100-800sccm, and reaction gas flow 200-1000sccm, sputtering target material power is 5-
30KW；After being coated with the high refractive index layer thickness for reaching and designing in step 1, stops plated film, be then coated with low-index layer, be passed through magnetic
Control sputter cavity sputter gas flow is 100-800sccm, reaction gas flow 200-1000sccm, sputtering target material power
For 5-30KW；After being coated with the low-index layer thickness for reaching and designing in step 1, stop plated film；Continue to be coated with next high refraction
It is identical as a upper high refractive index layer to be coated with mode for rate layer；After the completion of being coated with, continue to be coated with next low-index layer, plate
Mode processed is identical as a upper low-index layer；And so on, until being coated with n high refractive index layer of completion and n low refractions
Rate layer stops plated film；
S36 is coated with high extinction coefficient layer；Being passed through magnetron sputter cavity sputter gas flow is 100-800sccm, reaction gas
Flow is 200-1000sccm, and sputtering target material power is 5-30KW；It is coated with the high extinction coefficient thickness degree for reaching and designing in step 1
Afterwards, stop plated film；
S37 is coated with protective layer；Being passed through magnetron sputter cavity sputter gas flow is 100-800sccm, and reaction gas flow is
200-1000sccm, sputtering target material power are 5-30KW；After being coated with the protective layer thickness for reaching and designing in step 1, stop plated film；
S38 after the completion of all film layers are coated with, makes deflation vacuum breaker in the machine cavity of magnetron sputter, and takes out the work of plated film completion
Part.
6. the method that magnetron sputter according to claim 1 prepares graduated colors film, it is characterised in that in step S4, institute
It states color LAB value and visible reflectance curve, visible light transmittance curve is detected using spectrophotometer, from one end of workpiece
A point is taken to be detected every 1-2cm to the other end.
7. the method that magnetron sputter according to claim 1 prepares graduated colors film, it is characterised in that the target packet
High refractive index target, low-refraction target, high extinction coefficient target are included, the shutter can be placed in high refractive index target, low
Refractive index target, between one of high extinction coefficient target, two or three of target and workpiece.
8. the method that magnetron sputter according to claim 5 prepares graduated colors film, it is characterised in that the magnetic control splashes
The sputter gas for penetrating machine cavity body is high-purity argon gas；The reaction gas of the magnetron sputter cavity be high purity oxygen gas, high pure nitrogen,
One of high purity acetylene.
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