CN107479116A - A kind of two-sided low reflective chrome membrane system and preparation method thereof - Google Patents

A kind of two-sided low reflective chrome membrane system and preparation method thereof Download PDF

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Publication number
CN107479116A
CN107479116A CN201710800208.5A CN201710800208A CN107479116A CN 107479116 A CN107479116 A CN 107479116A CN 201710800208 A CN201710800208 A CN 201710800208A CN 107479116 A CN107479116 A CN 107479116A
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film
films
substrate
membrane system
magnetron sputtering
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CN107479116B (en
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陈翻
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WUHAN GENUINE GAOLI OPTICS CO Ltd
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WUHAN GENUINE GAOLI OPTICS CO Ltd
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/113—Anti-reflection coatings using inorganic layer materials only
    • G02B1/115—Multilayers
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

The invention provides a kind of two-sided low reflective chrome membrane system and preparation method thereof, belong to optical field.Two-sided low reflective chrome membrane system provided by the invention is arranged at substrate single side surface, includes the first Cr directly contacted with substrate successively2O3Film, it is arranged on the first Cr2O3The CrN films of film upper surface, the Cr films for being arranged on CrN films upper surface and the 2nd Cr for being arranged on Cr films upper surface2O3Film.The present invention obtains a kind of two-sided low reflective chrome membrane system by the setting to membranous layer ingredient and thickness, embodiment result shows, two-sided low reflective chrome membrane system provided by the invention can make plated film side and substrate side all reach less than 4% using the reflectivity of wave band in conventional terminal product, and the reflectivity of substrate side minimum point can reach 0.035%.

Description

A kind of two-sided low reflective chrome membrane system and preparation method thereof
Technical field
The present invention relates to the technical field of optical film, more particularly to a kind of two-sided low reflective chrome membrane system and its preparation side Method.
Background technology
Low reflection chromium plate develops on the basis of bright chromium plate, using relatively broad in optical field.It is low anti- The structural principle for penetrating chromium plate is to be initially formed a layer thickness on the glass substrate to beThe chromium film of left and right, this layer of chromium are commonly referred to as Bright chromium；Then forming thickness on the basis of bright layers of chrome again isThe chromium oxide layer of left and right, that is, the dark chromium being generally called, that is, Low reflective chrome.Because oxide layer is to the antiradar reflectivity of light, the light beats coefficient of substrate surface greatly declines, so that light is passing through During substrate, the light in clear zone, which can pass through, to be gone, and the light of black area can be oxidized film absorption, and then greatly reduces reflected light and signal is done Disturb.
But low reflection chromium plate can only produce low reflection (minimum point reflectivity is 2~3%) in plated film side, in substrate side simultaneously The effect of low reflection can not be reached, so as to larger in interference of the substrate side reflected light to signal.
At present, prior art is obtained double by being coated with the method for chromium oxide film-chromium film-chromium oxide film successively in substrate Face low-reflection film system, the membrane system can reduce the reflectivity of substrate side to a certain degree, but the minimum point of this kind of method substrate side Reflectivity is also only capable of reaching 2~3%, still can not meet higher optical design requirements.
The content of the invention
In view of this, present invention aims at a kind of two-sided low reflective chrome membrane system and preparation method thereof is provided, the present invention carries The two-sided low reflective chrome membrane system supplied can make plated film side and substrate side while obtain the effect of low reflection, and substrate side minimum point Reflectivity can reach 0.035%.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The invention provides a kind of two-sided low reflective chrome membrane system, substrate single side surface is arranged at, is included successively straight with substrate First Cr of contact2O3Film, it is arranged on the first Cr2O3The CrN films of film upper surface, the Cr films for being arranged on CrN films upper surface and set Put the 2nd Cr in Cr films upper surface2O3Film；
First Cr2O3The thickness of film is
The thickness of the CrN films is
The thickness of the Cr films is
2nd Cr2O3The thickness of film is
Preferably, the first Cr2O3The thickness of film is
The thickness of the CrN films is
The thickness of the Cr films is
2nd Cr2O3The thickness of film is
Preferably, the first Cr2O3The thickness of film is
The thickness of the CrN films is
The thickness of the Cr films is
2nd Cr2O3The thickness of film is
The invention provides the preparation method of membrane system described in such scheme, comprise the following steps：
First Cr is coated with substrate surface using magnetron sputtering method successively2O3Film, CrN films, Cr films and the 2nd Cr2O3Film, obtain To two-sided low reflective chrome membrane system.
Preferably, the magnetron sputtering is coated with the first Cr2O3During film, cathode targets are Cr targets；Magnetron sputtering power is 4500~5500W；The speed of service of substrate is 150~180mm/min；
The magnetron sputtering is coated with the first Cr2O3Film is in Ar-N2-CO2Carried out in mixed-gas atmosphere；Described Ar, N2And CO2 Gas flow ratio be 1:1:3~4.
Preferably, when the magnetron sputtering is coated with CrN films, cathode targets are Cr targets；Magnetron sputtering power be 4500~ 5500W；The speed of service of substrate is 500~600mm/min；
The magnetron sputtering is coated with CrN films in Ar-N2Carried out in mixed-gas atmosphere；The Ar and N2Gas flow ratio For 1:0.9~1.1.
Preferably, when the magnetron sputtering is coated with Cr films, cathode targets are Cr targets；Magnetron sputtering power be 1500~ 2500W；The speed of service of substrate is 450~550mm/min；
The magnetron sputtering is coated with CrN films and carried out in an ar atmosphere.
Preferably, the magnetron sputtering is coated with the 2nd Cr2O3During film, cathode targets are Cr targets；Magnetron sputtering power is 5000~6000W；The speed of service of substrate is 140~150mm/min；
The magnetron sputtering is coated with the 2nd Cr2O3Film is in Ar-N2-CO2Carried out in mixed-gas atmosphere；Described Ar, N2And CO2 Gas flow ratio be 1:1:3~4.
A kind of optical element, including substrate and the two-sided low reflective chrome membrane system for being arranged on substrate single side surface；It is described two-sided Preparation method described in two-sided low reflective chrome membrane system or such scheme described in low reflective chrome membrane system such scheme is prepared two-sided low Reflective chrome membrane system.
The invention provides a kind of two-sided low reflective chrome membrane system, include the first Cr successively from bottom to top2O3Film, CrN films, Cr Film and the 2nd Cr2O3Film；First Cr2O3The thickness of film isThe thickness of the CrN films is The thickness of the Cr films is2nd Cr2O3The thickness of film isThe present invention is by film The setting of composition of layer and thickness, a kind of two-sided low reflective chrome membrane system is obtained, embodiment result shows, provided by the invention two-sided Low reflective chrome membrane system can make plated film side and substrate side use the reflectivity of wave band (low reflected waveband) all in conventional terminal product Reach less than 4%, and the reflectivity of substrate side minimum point can reach 0.035%.
Present invention also offers the preparation method of membrane system described in such scheme, comprise the following steps：Using magnetron sputtering method Successively the first Cr is coated with substrate surface2O3Film, CrN films, Cr films and the 2nd Cr2O3Film.Preparation method letter provided by the invention Single, easily operation, is easy to industrialized production.
Present invention also offers a kind of optical element, including substrate and the two-sided low reflective chrome for being arranged on substrate single side surface Membrane system.Optical element provided by the invention can obtain low reflectivity in plated film side and substrate side, disclosure satisfy that optical field Design requirement.
Brief description of the drawings
Fig. 1 is the schematic diagram of two-sided low reflective chrome membrane system prepared by the embodiment of the present invention；
Fig. 2 is the reflectance map of chromium membrane system plated film side prepared by the embodiment of the present invention 1；
Fig. 3 is the reflectance map of chromium membrane system substrate side prepared by the embodiment of the present invention 1；
Fig. 4 is the reflectance map of chromium membrane system substrate side prepared by the embodiment of the present invention 2；
Fig. 5 is the reflectance map of chromium membrane system substrate side prepared by the embodiment of the present invention 3；
Fig. 6 is the reflectance map of chromium membrane system substrate side prepared by comparative example 1 of the present invention.
Embodiment
The invention provides a kind of two-sided low reflective chrome membrane system, structure is as shown in figure 1, two-sided low reflection provided by the invention Chromium membrane system is arranged at substrate single side surface, includes the first Cr directly contacted with substrate successively2O3Film, it is arranged on the first Cr2O3Film The CrN films of upper surface, the Cr films for being arranged on CrN films upper surface and the 2nd Cr for being arranged on Cr films upper surface2O3Film.
In the present invention, the first Cr2O3The thickness of film isPreferablyMore preferably For
The thickness of the CrN films isPreferablyMore preferably
The thickness of the Cr films isPreferablyMore preferably
2nd Cr2O3The thickness of film isPreferablyMore preferably
The present invention adds chromium nitride layer in traditional membrane system, is arranged on the first Cr2O3Between film and Cr films, nitrogen is utilized Change the characteristics of chromium refractive index is higher, by adjusting the thicknesses of layers of CrN films, plated film side and substrate side is obtained low reflection Effect.
Present invention also offers the preparation method of membrane system described in above-mentioned technical proposal, comprise the following steps：
First Cr is coated with substrate surface using magnetron sputtering method successively2O3Film, CrN films, Cr films and the 2nd Cr2O3Film, obtain To two-sided low reflective chrome membrane system.
In the present invention, the step of preferably also including cleaning substrate before the magnetron sputtering plating；The present invention is right The specific method of the cleaning does not have particular/special requirement, can be by substrate table using cleaning method well known to those skilled in the art Face impurity cleans up, and in a particular embodiment of the present invention, is preferably cleaned using supersonic cleaning machine.The present invention is to described Substrate does not have particular/special requirement, specific such as simple glass, optics using plated film substrate well known to those skilled in the art Glass, crystal and sapphire etc..
In the present invention, before the plated film, preferred pair substrate is preheated；The temperature of the preheating is preferably 170~ 190 DEG C, more preferably 180 DEG C；The time of the preheating is preferably 2~4min, more preferably 5min；In the specific reality of the present invention Apply in example, substrate is preferably loaded into magnetron sputtering Special tooling clamp, substrate is loaded in vacuum chamber, is then turned on extract system Start to vacuumize, vacuum reaches 1 × 10-3During Pa, heated baking equipment is opened, substrate is preheated.
After the completion of substrate preheating, the present invention is coated with the first Cr in substrate surface successively using magnetron sputtering method2O3Film, CrN Film, Cr films and the 2nd Cr2O3Film.In the present invention, the magnetron sputtering is coated with the first Cr2O3During film, cathode targets are preferably Cr Target；The magnetron sputtering power is preferably 4500~5500W, more preferably 5000W；The speed of service of the substrate is preferably 150~180mm/min, more preferably 155~175mm/min, most preferably 155mm/min or 175mm/min.
In the present invention, the magnetron sputtering is coated with the first Cr2O3Film is preferably in Ar-N2-CO2Enter in mixed-gas atmosphere OK；Described Ar, N2And CO2Gas flow ratio be preferably 1:1:3~4, more preferably 1:1:3；In the specific embodiment of the present invention In, the gas flow of the Ar is preferably 25~35sccm, more preferably 30sccm；The N2Gas flow be preferably 25~ 35sccm, more preferably 30sccm；The CO2Gas flow be preferably 85~95sccm, more preferably 90sccm.
The first Cr is coated with magnetic sputtering2O3During film, Cr targets are under plasma environment by Ar+Ions Bombardment, from After target as sputter comes out, and and CO2The O ionized out2-React generation Cr2O3, Cr2O3Constantly accumulated in substrate surface, so as to Obtain Cr2O3Film layer.
In the present invention, when the magnetron sputtering is coated with CrN films, cathode targets are preferably Cr targets；The magnetron sputtering Sputtering power when being coated with CrN films is preferably 4500~5500W, more preferably 5000W；When the magnetron sputtering is coated with CrN films The speed of service of substrate is preferably 550~650mm/min, more preferably 600mm/min；It is excellent that the magnetron sputtering is coated with CrN films It is selected in Ar-N2Carried out in mixed-gas atmosphere；The Ar and N2Gas flow ratio be preferably 1:0.9~1.1, more preferably 1: 1；In a particular embodiment of the present invention, the gas flow of the Ar is preferably 50~60sccm, more preferably 50sccm；It is described N2Gas flow be preferably 45~55sccm, more preferably 50sccm.
During magnetic sputtering is coated with CrN films, Cr targets are under plasma environment by Ar+Ions Bombardment, from target After sputtering out, and and N2The N ionized out-React generation CrN, and CrN constantly accumulates in substrate surface, so as to obtain CrN films Layer.The present invention is in the first Cr2O3Between film and Cr films set CrN film layers, by control magnetron sputtering process gas flow ratio, The translational speed of sputtering power and substrate makes CrN film layers obtain suitable thickness, and in sputter procedure gas flow proportional The atomic ratio of Cr and N in CrN film layers can be influenceed, the present invention is by controlling suitable gas flow ratio, to adjust in CrN film layers The ratio of Cr atoms and N atoms, so as to the chromium nitride film layer that can reduce film surface reflectivity being more suitable for.
In the present invention, when the magnetron sputtering is coated with Cr films, cathode targets are preferably Cr targets；The magnetic control is coated with Cr Sputtering power during film is preferably 1500~2500W, more preferably 2000W；The fortune of substrate when the magnetron sputtering is coated with Cr films Scanning frequency degree is preferably 200~500mm/min, more preferably 500mm/min；The magnetron sputtering is coated with CrN films preferably in Ar gas Carried out in atmosphere；The gas flow of the Ar is preferably 50~60sccm, more preferably 55sccm.
During magnetic sputtering is coated with Cr films, Cr targets are under plasma environment by Ar+Ions Bombardment, splashed from target After shooting out, constantly accumulated in substrate surface, so as to obtain Cr film layers.
In the present invention, the magnetron sputtering is coated with the 2nd Cr2O3During film, cathode targets are preferably Cr targets；The magnetic control Sputtering is coated with the 2nd Cr2O3Sputtering power during film is preferably 5000~6000W, more preferably 5500W；The magnetron sputtering Make the 2nd Cr2O3The speed of service of substrate is preferably 145~202mm/min during film, more preferably 145mm/min；The magnetic control splashes Penetrate and be coated with the 2nd Cr2O3Film is preferably in Ar-N2-CO2Carried out in mixed-gas atmosphere；Described Ar, N2And CO2Gas flow ratio it is excellent Elect 1 as:1:3~4, more preferably 1:1:4；In a particular embodiment of the present invention, the gas flow of the Ar be preferably 25~ 35sccm, more preferably 30sccm；The N2Gas flow be preferably 25~35sccm, more preferably 30sccm；The CO2 Gas flow be preferably 115~125sccm, more preferably 120sccm.
In the present invention, the first Cr2O3Film and the 2nd Cr2O3The thickness of film can influence the low anti-of two-sided low reflective chrome membrane system Ejected wave section, the low reflected waveband of membrane system can be with Cr2O3The thickness of film changes, such as the first Cr2O3Film and the 2nd Cr2O3Film Thickness isWhen, the low reflected waveband of two-sided low reflective chrome membrane system is 400~600nm, the first Cr2O3Film and second Cr2O3The thickness of film isWhen, the low reflected waveband of two-sided low reflective chrome membrane system is 600~800nm.In this hair In bright specific embodiment, the first Cr can be determined according to the demand to low reflected waveband2O3Film and the 2nd Cr2O3The tool of film Body thickness.
In a particular embodiment of the present invention, preferably above-mentioned plating run is imported in magnetron sputtering coating system, then Start plated film.In the present invention, whole coating process is all carried out under vacuum；The vacuum of the coating process is preferably 1.0×10-3~2.0 × 10-3Pa, more preferably 1.0 × 10-3Pa。
Present invention also offers a kind of optical element, including substrate and it is arranged on described in the such scheme of substrate single side surface Two-sided low reflective chrome membrane system.In the present invention, the species of the substrate is identical with such scheme, will not be repeated here；At this In the specific embodiment of invention, the substrate surface is preferably provided with pattern；The present invention is not special to the shape of the pattern It is required that it is configured according to the real needs to optical element；The present invention is not special to the specific method for setting pattern It is required that using method well known to those skilled in the art, the addition technique of plated film after the specific drawing such as first photoetching.
Optical element provided by the invention can obtain low reflectivity in plated film side and substrate side, disclosure satisfy that optics is led The design requirement in domain.
Two-sided low reflective chrome membrane system provided by the invention and preparation method thereof is carried out specifically with reference to embodiment It is bright, but they can not be interpreted as limiting the scope of the present invention.
The structural representation of two-sided low reflective chrome membrane system prepared by the embodiment of the present invention is as shown in Figure 1.
Embodiment 1
B270 non-optical glass substrates after cleaning are loaded into Special tooling clamp, reruned to vacuum chamber, are imported advance Designed plating run, starts plated film, and step is as follows：
Start extract system, vacuum reaches 1*10 in vacuum chamber-3During Pa, heated baking equipment is opened；Heating substrate arrives 180 DEG C, 3 minutes are incubated, then starts plated film, coating process comprises the following steps：
It is coated with the first Cr2O3Film：Cathode targets are Cr targets, magnetron sputtering power 5500W, the speed of service of substrate 155mm/min, gas flow：Ar 30sccm、N230sccm、CO290sccm；Gained Cr2O3Film ulking thickness is
It is coated with CrN films：Cathode targets are Cr targets, magnetron sputtering power 5000W, the speed of service 600mm/ of substrate Min, gas flow：Ar55sccm, N250sccm；Gained CrN film thicknesses are
It is coated with Cr films：Cathode targets are Cr targets, magnetron sputtering power 2000W, the speed of service 500mm/ of substrate Min, gas flow：Ar55sccm；Gained Cr films ulking thickness is about
It is coated with the 2nd Cr2O3Film：Cathode targets are Cr targets, magnetron sputtering power 5500W, the speed of service of substrate 145mm/min, gas flow：Ar 30sccm, N230sccm, CO2120sccm；The Cr of gained the 2nd2O3Film thickness is about
0 ° of incidence of light, is detected to the coating side reflection rate of the chromium membrane system, acquired results as shown in Fig. 2 according to Fig. 2 can be seen that reflectivity of the plated film side in 600~700nm wave bands section below 2.5%, and minimum point reflectivity is 0.210%；
The reflectivity of gained chromium membrane system substrate side is detected, acquired results are as shown in Figure 3；According to Fig. 3 as can be seen that Reflectivity of the substrate side in 600~780nm wave bands section is all less than 4%, and minimum point reflectivity is 0.537%.
Method in international standard ISO9211-3-2008 detects to the adhesive force of gained membrane system, as a result shows Gained chromium membrane system disclosure satisfy that the requirement of adhesive force in international standard.
Method in international standard ISO9022-12 detects to the environmental suitability of gained film layer, as a result shows Gained chromium membrane system disclosure satisfy that the requirement of environmental suitability in international standard.
Embodiment 2
B270 non-optical glass substrates after cleaning are loaded into Special tooling clamp, loaded in vacuum chamber, importing is pre-designed Good plating run, starts plated film, and step is as follows：
Start extract system, vacuum reaches 1*10 in vacuum chamber-3During Pa, heated baking equipment is opened；Heating substrate arrives 180 DEG C, 3 minutes are incubated, then starts plated film, coating process comprises the following steps：
It is coated with the first Cr2O3Film：Cathode targets are Cr targets, magnetron sputtering power 5500W, the speed of service of substrate 175mm/min, gas flow：Ar 30sccm、N230sccm、CO290sccm；Gained Cr2O3Film ulking thickness is
It is coated with CrN films：Cathode targets are Cr targets, magnetron sputtering power 5000W, the speed of service 600mm/ of substrate Min, gas flow：Ar 55sccm, N250sccm；Gained CrN film thicknesses are
It is coated with Cr films：Cathode targets are Cr targets, magnetron sputtering power 2000W, the speed of service 500mm/ of substrate Min, gas flow：Ar 55sccm；Gained Cr films ulking thickness is about
It is coated with the 2nd Cr2O3Film：Cathode targets are Cr targets, magnetron sputtering power 5500W, the speed of service of substrate 145mm/min, gas flow：Ar 30sccm, N230sccm, CO2120sccm；The Cr of gained the 2nd2O3Film thickness is about
The coating side reflection rate of the chromium membrane system is detected, as a result shows plated film side in 600~700nm wave bands section Reflectivity all be less than 4%, and minimum point reflectivity be 0.233%；
The reflectivity of gained chromium membrane system substrate side is detected, acquired results are as shown in Figure 4；According to Fig. 4 as can be seen that Reflectivity of the substrate side in 520~780nm wave bands section is all less than 4%, and minimum point reflectivity is 0.335%.
Method in international standard ISO9211-3-2008 detects to the adhesive force of gained membrane system, as a result shows Gained chromium membrane system disclosure satisfy that the requirement of adhesive force in international standard.
Method in international standard ISO9022-12 detects to the environmental suitability of gained film layer, as a result shows Gained chromium membrane system disclosure satisfy that the requirement of environmental suitability in international standard.
Embodiment 3
By the B270 non-optical glass substrates after cleaning on film coating jig, and run to vacuum chamber, be then introduced into pre- First designed plating run, starts plated film, and step is as follows：
Start extract system, vacuum reaches 1*10 in vacuum chamber-3During Pa, heated baking equipment is opened；Heating substrate arrives 180 DEG C, 3 minutes are incubated, then starts plated film, coating process comprises the following steps：
It is coated with the first Cr2O3Film：Cathode targets are Cr targets, magnetron sputtering power 5000W, the speed of service of substrate 178mm/min, gas flow：Ar 30sccm、N230sccm、CO290sccm；Gained Cr2O3Film ulking thickness is
It is coated with CrN films：Cathode targets are Cr targets, magnetron sputtering power 5000W, the speed of service 500mm/ of substrate Min, gas flow：Ar55sccm, N250sccm；Gained CrN film thicknesses are
It is coated with Cr films：Cathode targets are Cr targets, magnetron sputtering power 5000W, the speed of service 200mm/ of substrate Min, gas flow：Ar55sccm；Gained Cr films ulking thickness is about
It is coated with the 2nd Cr2O3Film：Cathode targets are Cr targets, magnetron sputtering power 5000W, the speed of service of substrate 202mm/min, gas flow：Ar 30sccm, N230sccm, CO2120sccm；The Cr of gained the 2nd2O3Film thickness is about
The coating side reflection rate of the chromium membrane system is detected, as a result shows plated film side in 600~700nm wave bands section Reflectivity all be less than 4%, and minimum point reflectivity be 0.198%；
The reflectivity of gained chromium membrane system substrate side is detected, acquired results are as shown in Figure 5；According to Fig. 5 as can be seen that Reflectivity of the substrate side in 600~700nm wave bands section is all less than 1.5%, and minimum point reflectivity is 0.035%.
Method in international standard ISO9211-3-2008 detects to the adhesive force of gained membrane system, as a result shows Gained chromium membrane system disclosure satisfy that the requirement of adhesive force in international standard.
Method in international standard ISO9022-12 detects to the environmental suitability of gained film layer, as a result shows Gained chromium membrane system disclosure satisfy that the requirement of environmental suitability in international standard.
Comparative example 1
B270 non-optical glass substrates after cleaning are loaded into Special tooling clamp, it is pre-designed to load importing in vacuum chamber Plating run, start plated film, step is as follows：
Start extract system, vacuum reaches 1*10 in vacuum chamber-3During Pa, heated baking equipment is opened；Heating substrate arrives 180 DEG C, 3 minutes are incubated, then starts plated film, coating process comprises the following steps：
It is coated with Cr2O3Film：Cathode targets are Cr targets, magnetron sputtering power 5500W, the speed of service 155mm/ of substrate Min, gas flow：Ar 30sccm、N230sccm、CO290sccm；Gained Cr2O3Film ulking thickness is
It is coated with Cr films：Cathode targets are Cr targets, magnetron sputtering power 2000W, the speed of service 500mm/ of substrate Min, gas flow：Ar 55sccm；Gained Cr films ulking thickness is about
It is coated with Cr2O3Film：Cathode targets are Cr targets, magnetron sputtering power 5500W, the speed of service 145mm/ of substrate Min, gas flow：Ar 30sccm, N230sccm, CO2120sccm；The Cr of gained the 2nd2O3Film thickness is about
The reflectivity of gained chromium membrane system substrate side is detected, acquired results are as shown in Figure 6；According to Fig. 6 as can be seen that The reflectivity of substrate side is all more than 4%.
As seen from the above embodiment, it is only the preferred embodiment of the present invention that the present invention is described above, it is noted that for For those skilled in the art, under the premise without departing from the principles of the invention, can also make it is some improvement and Retouching, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (9)

1. a kind of two-sided low reflective chrome membrane system, is arranged at substrate single side surface, it is characterised in that includes directly connecing with substrate successively The first tactile Cr2O3Film, it is arranged on the first Cr2O3The CrN films of film upper surface, the Cr films for being arranged on CrN films upper surface and it is arranged on 2nd Cr of Cr films upper surface2O3Film；
First Cr2O3The thickness of film is
The thickness of the CrN films is
The thickness of the Cr films is
2nd Cr2O3The thickness of film is
2. two-sided low reflective chrome membrane system according to claim 1, it is characterised in that the first Cr2O3The thickness of film is
The thickness of the CrN films is
The thickness of the Cr films is
2nd Cr2O3The thickness of film is
3. two-sided low reflective chrome membrane system according to claim 1 or 2, it is characterised in that the first Cr2O3The thickness of film For
The thickness of the CrN films is
The thickness of the Cr films is
2nd Cr2O3The thickness of film is
4. the preparation method of two-sided low reflective chrome membrane system, comprises the following steps described in claims 1 to 3 any one：
First Cr is coated with substrate surface using magnetron sputtering method successively2O3Film, CrN films, Cr films and the 2nd Cr2O3Film, obtain double The low reflective chrome membrane system in face.
5. preparation method according to claim 4, it is characterised in that the magnetron sputtering is coated with the first Cr2O3It is cloudy during film Pole target is Cr targets；Magnetron sputtering power is 4500~5500W；The speed of service of substrate is 150~180mm/min；
The magnetron sputtering is coated with the first Cr2O3Film is in Ar-N2-CO2Carried out in mixed-gas atmosphere；Described Ar, N2And CO2Gas Body flow-rate ratio is 1:1:3~4.
6. preparation method according to claim 4, it is characterised in that when the magnetron sputtering is coated with CrN films, cathode targets For Cr targets；Magnetron sputtering power is 4500~5500W；The speed of service of substrate is 500~600mm/min；
The magnetron sputtering is coated with CrN films in Ar-N2Carried out in mixed-gas atmosphere；The Ar and N2Gas flow ratio be 1: 0.9~1.1.
7. preparation method according to claim 4, it is characterised in that when the magnetron sputtering is coated with Cr films, cathode targets For Cr targets；Magnetron sputtering power is 1500~2500W；The speed of service of substrate is 200~500mm/min；
The magnetron sputtering is coated with CrN films and carried out in an ar atmosphere.
8. preparation method according to claim 4, it is characterised in that the magnetron sputtering is coated with the 2nd Cr2O3It is cloudy during film Pole target is Cr targets；Magnetron sputtering power is 5000~6000W；The speed of service of substrate is 145~202mm/min；
The magnetron sputtering is coated with the 2nd Cr2O3Film is in Ar-N2-CO2Carried out in mixed-gas atmosphere；Described Ar, N2And CO2Gas Body flow-rate ratio is 1:1:3~4.
9. a kind of optical element, including substrate and the two-sided low reflective chrome membrane system for being arranged on substrate single side surface；It is described two-sided low Reflective chrome membrane system is the two-sided low reflective chrome membrane system or claim 4~8 any one described in claims 1 to 3 any one Two-sided low reflective chrome membrane system prepared by the preparation method.
CN201710800208.5A 2017-09-07 2017-09-07 Two-sided low reflective chrome membrane system of one kind and preparation method thereof Active CN107479116B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114674233A (en) * 2020-03-31 2022-06-28 大日本印刷株式会社 Reflective optical scale for encoder and reflective optical encoder

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1532606A (en) * 2003-03-26 2004-09-29 鸿富锦精密工业（深圳）有限公司 Black matrix, color optical filter and liquid crystal display device
CN102691043A (en) * 2011-03-21 2012-09-26 鸿富锦精密工业（深圳）有限公司 Film coating member and its preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1532606A (en) * 2003-03-26 2004-09-29 鸿富锦精密工业（深圳）有限公司 Black matrix, color optical filter and liquid crystal display device
CN102691043A (en) * 2011-03-21 2012-09-26 鸿富锦精密工业（深圳）有限公司 Film coating member and its preparation method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114674233A (en) * 2020-03-31 2022-06-28 大日本印刷株式会社 Reflective optical scale for encoder and reflective optical encoder

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