CN105388542A - Ge-As-Se infrared glass with anti-reflection film and preparation method thereof - Google Patents
Ge-As-Se infrared glass with anti-reflection film and preparation method thereof Download PDFInfo
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- CN105388542A CN105388542A CN201510874951.6A CN201510874951A CN105388542A CN 105388542 A CN105388542 A CN 105388542A CN 201510874951 A CN201510874951 A CN 201510874951A CN 105388542 A CN105388542 A CN 105388542A
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- germanium antimony
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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
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Abstract
The invention discloses Ge-As-Se infrared glass with an anti-reflection film and a preparation method thereof. The Ge-As-Se infrared glass with the anti-reflection film comprises a Ge-As-Se infrared glass base layer, the Ge-As-Se infrared glass base layer is composed of 12% of Ge, 28% of As and 60% of Se by weight, and a first ytterbium fluoride layer, a first zinc sulfide layer, a second ytterbium fluoride layer and a second zinc sulfide layer are deposited on the Ge-As-Se infrared glass base layer successively. The Ge-As-Se infrared glass of the invention can effectively prevent the anti-reflection film from falloff, and the reflectivity of the infrared glass is reduced.
Description
Technical field
The present invention relates to glass processing field, be specifically related to a kind of germanium antimony selenium infrared glass with antireflective film and preparation method thereof.
Background technology
Germanium antimony selenium infrared glass is the infrared optical material of a class function admirable, but its fragility is large, and surface residual reflectivity is high, cannot directly use.
The conventional means of the reflectivity of current reduction glass material is at glass material plated surface antireflective film, patent CN104459835A describes a kind of infrared glass GASIRl anti-reflection film, it adopts 4 kinds of coating materials, rete number is 13 scholar 2 layers, gross thickness reaches 4000 scholar 200nm, through design, surface residual reflectivity can be down to less than 1%.
But this film system exists and adopts coating materials too much, the number of plies and the shortcoming such as thickness is large; In addition, GASIRl infrared glass is Ge-As-Se system, and different from germanium antimony selenium infrared glass physicochemical characteristic, this film structure and preparation method are not suitable for germanium antimony selenium infrared glass.Compared with the infrared crystal material such as germanium, the outer glass transformation temperature of germanium antimony selenium ruby is low, fragility is large, physicochemical characteristic is poor, and the rete adopting conventional film preparation technology to prepare, very easily occurs the problems such as rete comes off.The physico-chemical property difference of germanium antimony selenium infrared glass and Ge-As-Se system and elemental Germanium thereof is very large, and the antireflective film that the two can not be adopted directly is used on germanium antimony selenium infrared glass, and has not yet to see the report about the anti-reflection of germanium antimony selenium infrared glass.
Summary of the invention
Fundamental purpose of the present invention is, provides a kind of germanium antimony selenium infrared glass with antireflective film, reduces the reflectivity of germanium antimony selenium infrared glass, and its antireflective film system stress coupling is good, prevents the outer coating film on glass of germanium antimony selenium ruby to come off.
Present invention also offers a kind of preparation method with the germanium antimony selenium infrared glass of antireflective film.
Object of the present invention and technical solution problem thereof are achieved by the following technical solution:
Have a germanium antimony selenium infrared glass for antireflective film, it comprises the outer glass-base of germanium antimony selenium ruby; The outer glass-base of described germanium antimony selenium ruby is made up of following component by mass percentage: germanium: 12%, antimony: 28%, selenium: 60%; The outer glass-base of described germanium antimony selenium ruby deposits successively first fluoridizes ytterbium layer, the first zinc sulfide layer, second fluoridizes ytterbium layer and the second zinc sulfide layer.
Further, described first to fluoridize ytterbium layer optical thickness be 173 ± 20nm.
Further, the first described zinc sulfide layer optical thickness is 1817 ± 120nm.
Further, described second to fluoridize ytterbium layer optical thickness be 1566 ± 80nm.
Further, the second described zinc sulfide layer optical thickness is 333 ± 25nm.
On the other hand, a kind of preparation method with the germanium antimony selenium infrared glass of antireflective film, comprises the steps:
(1) the outer glass substrate of germanium antimony selenium ruby is cleaned and preheating;
(2) ion gun is adopted to carry out cleaning before copper plating to the outer glass substrate of described germanium antimony selenium ruby;
(3) evaporation first fluoridizes ytterbium layer successively, the first zinc sulfide layer, second fluoridizes ytterbium layer and the second zinc sulfide layer;
(4) be cooled to room temperature obtain described in there is the germanium antimony selenium infrared glass of antireflective film.
Further, described step (1) specifically comprises the steps:
Acetone and alcohol ether is adopted to carry out ultrasonic cleaning, in vacuum tightness>=5.0 × 10 to the outer glass substrate of described germanium antimony selenium ruby
-3heat under pa condition, design temperature is 100-120 DEG C, and heating rate is: from room temperature to 60 DEG C, 1.5-3 DEG C/min, from 60 DEG C to described design temperature, and 1-2 DEG C/min; Insulation.
Further, described step (2) specifically comprises the steps: to open ion gun, and described ion gun is hall ion source, and being filled with argon gas amount is 30-40sccm, and arranging pressure is 7.0 × 10
-3-1.0 × 10
-2pa, anode voltage is 100-150V, and anode current is 1-2A, and scavenging period is 15-20min.
Further, described first to fluoridize the evaporation plating parameter of ytterbium layer as follows: pressure is 8.0 × 10-3-2.0 × 10-2pa, rate of sedimentation is 0.1-0.3nm/s, deposit optical thickness is 150-180nm, argon gas amount is 30-40sccm, and anode voltage is 100-150V, and anode current is 1-2A, in deposition process, workpiece plate rotating speed is 10-20rpm;
The evaporation plating parameter of the first described zinc sulfide layer is as follows: pressure is 5.0 × 10
-3-2.0 × 10
-2pa, rate of sedimentation is 1-3nm/s, and deposit optical thickness is 1600-1950nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, and anode current is 1-2A, and in deposition process, workpiece plate rotating speed is 10-20rpm;
The evaporation plating parameter of the second described zinc sulfide layer is as follows: pressure is 8.0 × 10
-3-2.0 × 10
-2pa, rate of sedimentation is 0.1-0.3nm/s, and deposit optical thickness is 1300-1700nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, and anode current is 1-2A, and in deposition process, workpiece plate rotating speed is 10-20rpm;
Described second to fluoridize the evaporation plating parameter of ytterbium layer as follows: pressure is 5.0 × 10
-3-2.0 × 10
-2pa, rate of sedimentation is 1-3nm/s, and deposit optical thickness is 200-400nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, and anode current is 1-2A, and in deposition process, workpiece plate rotating speed is 10-20rpm.
Further, described to be cooled to room temperature concrete steps as follows: being down to 60 DEG C of rate of temperature fall from described design temperature is 2-4 DEG C/min, and being down to room temperature rate of temperature fall from 60 DEG C is 3-5 DEG C/min.
Compared with prior art, the present invention's germanium antimony selenium infrared glass with antireflective film and preparation method thereof at least has following beneficial effect:
The present patent application is provided with antireflective film by germanium antimony selenium infrared glass, reduces surface residual reflectivity, improves the through performance of germanium antimony selenium infrared glass.
Film system gross thickness is low, film system Stress match is good: infrared film system gross thickness is larger, stress generally increases with the increase of thickness, the firmness of stress to rete increased is huge threat, therefore, during Film Design, just must consider collocation and the gross thickness of each thicknesses of layers in film system, the present patent application utilizes zinc sulphide contrary with fluoridizing ytterbium stress types, and controls individual layer and gross thickness size, achieves good Stress match.
Rete and substrate, rete and film ply adhesion good; Residual reflectance is low, meet optical system to infrared glass through requiring; The outer glass expansion coefficient of germanium antimony selenium ruby is comparatively large, belongs to hard brittle material, adopts gradient increased temperature and cooling during plated film, effectively prevent infrared glass because of problems such as easily breaking of causing greatly of temperature variation; Adopt low energy high density ion assisted deposition mode, avoid the temperature rise in coating process, improve the performance of rete.
Accompanying drawing explanation
Fig. 1 the present invention has the film structure schematic diagram of the germanium antimony selenium infrared glass of antireflective film;
Fig. 2 is the film structure residual reflectance Theoretical Design curve that the present invention has the germanium antimony selenium infrared glass of antireflective film;
Fig. 3 is the film structure residual reflectance measured curve that the present invention has the germanium antimony selenium infrared glass of antireflective film.
Embodiment
Embodiments provide a kind of germanium antimony selenium infrared glass with antireflective film, its antireflective film difficult drop-off, anti-reflection is effective.
Germanium antimony selenium glass selected in following examples is Ge
12sb
28se
60glass, is namely made up of the component of following massfraction: germanium: 12%, antimony: 28%, selenium: 60%.
Fig. 1 is the germanium antimony selenium ruby outer glass structure schematic diagram in the embodiment of the present invention with antireflective film.
Embodiment 1
There is the preparation method of the germanium antimony selenium infrared glass of antireflective film, comprise the steps:
(1) cleaning and preheating thereof: adopt acetone and alcohol ether to mix liquid respectively and carry out Ultrasonic Cleaning to infrared glass substrate, scavenging period is each 15min, finally, oven for drying is put in substrate; After oven dry completes, vacuum chamber is put in quick-clamping substrate, extracting vacuum.Vacuum reaches 5.0 × 10
-3pa, adjustment drying lamp output voltage, heating rate is: room temperature-60 DEG C, 30min, 60 DEG C-100 DEG C, 30min, after temperature, insulation 1.2h.
Here it should be noted that: germanium antimony selenium infrared glass is hard brittle material, the glass breakage that gradient increased temperature can prevent temperature variation from acutely causing.
(2) the auxiliary cleaning of ion, open ion gun, being filled with argon gas amount is 35sccm, and pressure in vacuum tank is 9 × 10
-3pa, anode voltage is 130V, and anode current is 1.5A, and workpiece plate rotating speed is 10rpm, and scavenging period is 18min.
(3) plated film:
Be coated with a YbF
3film, during evaporation, pressure in vacuum tank is 9.0 × 10
-3pa, rate of sedimentation is 0.2nm/s, and adopt crystal oscillator instrument control rate of sedimentation, deposit optical thickness is 173nm, adopts optical film thickness meter to control rete optical thickness.
Be coated with ground floor ZnS film, during evaporation, pressure in vacuum tank is 8.0 × 10
-3pa, rate of sedimentation is 1nm/s, and deposit optical thickness is 1817nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
Be coated with the 2nd YbF
3film, during evaporation, pressure in vacuum tank is 9.0 × 10
-3pa, rate of sedimentation is 0.2nm/s, and deposit optical thickness is 1566nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
Be coated with the 2nd ZnS film, during evaporation, pressure in vacuum tank is 8.0 × 10
-3pa, rate of sedimentation is 1nm/s, and deposit optical thickness is 333nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
Here it should be noted that: in coating process, along with the increase of thicknesses of layers, the refractive index of whole infrared glass system will change, more scientific and reasonable by the rate of sedimentation of control both optical thickness and plated film thereof; Rete is too thick easily causes coming off of film, too thinly cannot reach again desirable anti-reflection effect; Under vacuum condition, plated film can strengthen adhesion and the compactness of rete, improves its anti-reflection effect.
After being coated with, lower the temperature by following rate of temperature fall: 100 DEG C-60 DEG C, 30min, 60 DEG C-room temperature, 30min.Take out plated film infrared glass; Gradient cooling is adopted to prevent the rete acutely caused for temperature variation from easily coming off.
As shown in Figure 1, the film structure that the germanium antimony selenium infrared glass that prepared by the present embodiment has is 4 Rotating fields of 2 kinds of coating materials compositions;
Ground floor is YbF
3, optical thickness is 173nm, and the 2nd layer is ZnS, and optical thickness is 1817nm, and the 3rd layer is YbF
3, optical thickness is 1566nm, and the 4th layer of ZnS, optical thickness is 333nm.
Here it should be noted that: zinc sulphide is contrary with fluoridizing ytterbium stress types, the film adhesion that can prevent stress from causing is not strong; Four film structure make the thickness of every tunic moderate, and anti-reflection is satisfactory for result, if be duplicature, anti-reflection effect is undesirable; And if rete is more than four layers, although anti-reflection is satisfactory for result, gross thickness increases, and coating cost can increase a lot, and four film structure can reach good anti-reflection effect completely and adhesion is good; Result is as follows after tested:
Fig. 2 and Fig. 3 is respectively film structure residual reflectance Theoretical Design curve and the measured curve that the present embodiment has the germanium antimony selenium infrared glass of antireflective film.As can be seen from Figure 2, the theoretical anti-reflection effect of these four layers of antireflective films is fine, and in 8-12nm, its reflectivity is below 0.7%, and as can be seen from Figure 3, within the scope of wavelength 8-12um, this antireflective film system can by Ge
12sb
28se
60infrared glass surface residual reflectivity, by 18.3% during non-plated film, is reduced to less than 1%, and its luminance factor theoretical value is slightly high, and this is due in deposition process, and thicknesses of layers departure causes; Meanwhile, antireflective film prepared by the present invention, can by the environmental testing of GJB150-90, excellent performance.
Embodiment 2
Adopt acetone and alcohol ether to mix liquid respectively and carry out Ultrasonic Cleaning to infrared glass substrate, scavenging period is respectively each 13min and 16min, finally, oven for drying is put in substrate.
After oven dry completes, vacuum chamber is put in quick-clamping substrate, extracting vacuum; Vacuum reaches 8.0 × 10
-3pa, adjustment drying lamp output voltage, heating rate is: room temperature-60 DEG C, 30min, 60 DEG C-120 DEG C, 40min; After temperature, be incubated 1.5 hours.
Be filled with argon gas 40sccm, pressure in vacuum tank is 8.0 × 10
-3pa, opens ion gun, and adjustment source parameters is: anode voltage 100V, anode current is 2A, and workpiece plate rotating speed is 10rpm.
Be coated with a YbF
3film, during evaporation, pressure in vacuum tank is 1.0 × 10
-2pa, rate of sedimentation is 0.15nm/s, and adopt crystal oscillator instrument control rate of sedimentation, deposit optical thickness is 153nm, adopts optical film thickness meter to control rete optical thickness.
Be coated with a ZnS film, during evaporation, pressure in vacuum tank is 9.0 × 10
-3pa, rate of sedimentation is 1.5nm/s, and deposit optical thickness is 1697nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
Be coated with the 2nd YbF
3film, during evaporation pressure in vacuum tank be 1.0 ×
-2pa, rate of sedimentation is 0.15nm/s, and deposit optical thickness is 1646nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
Be coated with the 2nd ZnS film, during evaporation, pressure in vacuum tank is 9.0 × 10
-3pa, rate of sedimentation is 1.5nm/s, and deposit optical thickness is 358nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
After being coated with, lower the temperature by following rate of temperature fall: 120 DEG C-60 DEG C, 55min, 60 DEG C-room temperature, 25min, takes out plated film infrared glass.
Here it should be noted that: the present embodiment utilizes zinc sulphide contrary with fluoridizing ytterbium stress types, and controls individual layer and gross thickness size, achieves good Stress match.
Rete and substrate, rete and film ply adhesion good; Residual reflectance is low, meet optical system to infrared glass through requiring; Adopt gradient increased temperature and cooling during plated film, effectively prevent infrared glass because of problems such as easily breaking of causing greatly of temperature variation; Adopt low energy high density ion assisted deposition mode, avoid the temperature rise in coating process, improve the performance of rete.
The film structure had of this enforcement preparation is 4 Rotating fields of 2 kinds of coating materials compositions; 1st layer is YbF
3, optical thickness is 153nm, and the 2nd layer is ZnS, and optical thickness is 1697nm, and the 3rd layer is YbF
3, optical thickness is 1646nm, and the 4th layer of ZnS, optical thickness is 358nm.
Embodiment 3
Adopt acetone and alcohol ether to mix liquid respectively and carry out Ultrasonic Cleaning to infrared glass substrate, scavenging period is respectively each 18min and 12min, finally, oven for drying is put in substrate.
After oven dry completes, vacuum chamber is put in quick-clamping substrate, extracting vacuum; Vacuum reaches 1.0 × 10
-2pa, adjustment drying lamp output voltage, heating rate is: room temperature-60 DEG C, 30min, 60 DEG C-120 DEG C, 40min; After temperature, be incubated 1.5 hours.
Be filled with argon gas 40sccm, pressure in vacuum tank is 2.0 × 10
-2pa, opens ion gun, and adjustment source parameters is: anode voltage 150V, anode current is 1A, and workpiece plate rotating speed is 20rpm.
Be coated with a YbF
3film, during evaporation, pressure in vacuum tank is 2.0 × 10
-2pa, rate of sedimentation is 0.15nm/s, and adopt crystal oscillator instrument control rate of sedimentation, deposit optical thickness is 193nm, adopts optical film thickness meter to control rete optical thickness.
Be coated with a ZnS film, during evaporation, pressure in vacuum tank is 2.0 × 10
-2pa, rate of sedimentation is 3nm/s, and deposit optical thickness is 1937nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
Be coated with the 2nd YbF
3film, during evaporation pressure in vacuum tank be 2.0 ×
-2pa, rate of sedimentation is 0.3nm/s, and deposit optical thickness is 1486nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
Be coated with the 2nd ZnS film, during evaporation, pressure in vacuum tank is 2.0 × 10
-2pa, rate of sedimentation is 3nm/s, and deposit optical thickness is 308nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
After being coated with, lower the temperature by following rate of temperature fall: 120 DEG C-60 DEG C, 55min, 60 DEG C-room temperature, 25min, takes out plated film infrared glass.
Rete and substrate, rete and film ply adhesion good; Residual reflectance is low, meet optical system to infrared glass through requiring; Adopt gradient increased temperature and cooling during plated film, effectively prevent infrared glass because of problems such as easily breaking of causing greatly of temperature variation; Adopt low energy high density ion assisted deposition mode, avoid the temperature rise in coating process, improve the performance of rete.
Embodiment 4
Adopt acetone and alcohol ether to mix liquid respectively and carry out Ultrasonic Cleaning to infrared glass substrate, scavenging period is respectively each 15min and 17min, finally, oven for drying is put in substrate.
After oven dry completes, vacuum chamber is put in quick-clamping substrate, extracting vacuum; Vacuum reaches 7.0 × 10
-3pa, adjustment drying lamp output voltage, heating rate is: room temperature-60 DEG C, 30min, 60 DEG C-100 DEG C, 55min; After temperature, be incubated 1.5 hours.
Be filled with argon gas 40sccm, pressure in vacuum tank is 2.0 × 10
-2pa, opens ion gun, and adjustment source parameters is: anode voltage 125V, anode current is 1.5A, and workpiece plate rotating speed is 15rpm, and scavenging period is 20min.
Be coated with a YbF
3film, during evaporation, pressure in vacuum tank is 8.0 × 10
-3pa, rate of sedimentation is 0.1nm/s, and adopt crystal oscillator instrument control rate of sedimentation, deposit optical thickness is 183nm, adopts optical film thickness meter to control rete optical thickness.
Be coated with a ZnS film, during evaporation, pressure in vacuum tank is 5.0 × 10
-3pa, rate of sedimentation is 1nm/s, and deposit optical thickness is 1937nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
Be coated with the 2nd YbF
3film, during evaporation pressure in vacuum tank be 8.0 ×
-3pa, rate of sedimentation is 0.1nm/s, and deposit optical thickness is 1486nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
Be coated with the 2nd ZnS film, during evaporation, pressure in vacuum tank is 5.0 × 10
-3pa, rate of sedimentation is 1nm/s, and deposit optical thickness is 308nm, adopts crystal oscillator instrument control rate of sedimentation, adopts optical film thickness meter to control rete optical thickness.
After being coated with, lower the temperature by following rate of temperature fall: 120 DEG C-60 DEG C, 35min, 60 DEG C-room temperature, 35min, takes out plated film infrared glass.
Rete and substrate, rete and film ply adhesion good; Residual reflectance is low, meet optical system to infrared glass through requiring; Adopt gradient increased temperature and cooling during plated film, effectively prevent infrared glass because of problems such as easily breaking of causing greatly of temperature variation; Adopt low energy high density ion assisted deposition mode, avoid the temperature rise in coating process, improve the performance of rete.
The present invention program does not use up part, is those skilled in the art and adopts routine techniques to complete as required, be not described in detail in this.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (10)
1. have a germanium antimony selenium infrared glass for antireflective film, it comprises the outer glass-base of germanium antimony selenium ruby; The outer glass-base of described germanium antimony selenium ruby is made up of following component by mass percentage: germanium: 12%, antimony: 28%, selenium: 60%; It is characterized in that, the outer glass-base of described germanium antimony selenium ruby deposits successively first fluoridizes ytterbium layer, the first zinc sulfide layer, second fluoridizes ytterbium layer and the second zinc sulfide layer.
2. the germanium antimony selenium infrared glass with antireflective film according to claim 1, is characterized in that, described first to fluoridize ytterbium layer optical thickness be 173 ± 20nm.
3. the germanium antimony selenium infrared glass with antireflective film according to claim 1, it is characterized in that, the first described zinc sulfide layer optical thickness is 1817 ± 120nm.
4. the germanium antimony selenium infrared glass with antireflective film according to claim 1, is characterized in that, described second to fluoridize ytterbium layer optical thickness be 1566 ± 80nm.
5. the germanium antimony selenium infrared glass with antireflective film according to claim 1, it is characterized in that, the second described zinc sulfide layer optical thickness is 333 ± 25nm.
6. there is a preparation method for the germanium antimony selenium infrared glass of antireflective film, it is characterized in that, comprise the steps:
(1) the outer glass substrate of germanium antimony selenium ruby is cleaned and preheating;
(2) ion gun is adopted to carry out cleaning before copper plating to the outer glass substrate of described germanium antimony selenium ruby;
(3) evaporation first fluoridizes ytterbium layer successively, the first zinc sulfide layer, second fluoridizes ytterbium layer and the second zinc sulfide layer;
(4) be cooled to room temperature obtain described in there is the germanium antimony selenium infrared glass of antireflective film.
7. the preparation method with the germanium antimony selenium infrared glass of antireflective film according to claim 6, it is characterized in that, described step (1) specifically comprises the steps:
Acetone and alcohol ether is adopted to carry out ultrasonic cleaning, in vacuum tightness>=5.0 × 10 to the outer glass substrate of described germanium antimony selenium ruby
-3heat under pa condition, design temperature is 100-120 DEG C, and heating rate is: from room temperature to 60 DEG C, 1.5-3 DEG C/min, from 60 DEG C to described design temperature, and 1-2 DEG C/min; Insulation.
8. the preparation method with the germanium antimony selenium infrared glass of antireflective film according to claim 6, it is characterized in that, described step (2) specifically comprises the steps: to open ion gun, described ion gun is hall ion source, being filled with argon gas amount is 30-40sccm, and arranging pressure is 7.0 × 10
-3-1.0 × 10
-2pa, anode voltage is 100-150V, and anode current is 1-2A, and scavenging period is 15-20min.
9. the preparation method with the germanium antimony selenium infrared glass of antireflective film according to claim 6, it is characterized in that, described first to fluoridize the evaporation plating parameter of ytterbium layer as follows: pressure is 8.0 × 10-3-2.0 × 10-2pa, rate of sedimentation is 0.1-0.3nm/s, and deposit optical thickness is 150-180nm, and argon gas amount is 30-40sccm, anode voltage is 100-150V, anode current is 1-2A, and in deposition process, workpiece plate rotating speed is 10-20rpm;
The evaporation plating parameter of the first described zinc sulfide layer is as follows: pressure is 5.0 × 10
-3-2.0 × 10
-2pa, rate of sedimentation is 1-3nm/s, and deposit optical thickness is 1600-1950nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, and anode current is 1-2A, and in deposition process, workpiece plate rotating speed is 10-20rpm;
Described second to fluoridize the evaporation plating parameter of ytterbium layer as follows: pressure is 8.0 × 10
-3-2.0 × 10
-2pa, rate of sedimentation is 0.1-0.3nm/s, and deposit optical thickness is 1300-1700nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, and anode current is 1-2A, and in deposition process, workpiece plate rotating speed is 10-20rpm;
The evaporation plating parameter of the second described zinc sulfide layer is as follows: pressure is 5.0 × 10
-3-2.0 × 10
-2pa, rate of sedimentation is 1-3nm/s, and deposit optical thickness is 200-400nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, and anode current is 1-2A, and in deposition process, workpiece plate rotating speed is 10-20rpm.
10. the preparation method with the germanium antimony selenium infrared glass of antireflective film according to claim 6, it is characterized in that, described to be cooled to room temperature concrete steps as follows: being down to 60 DEG C of rate of temperature fall from described design temperature is 2-4 DEG C/min, and being down to room temperature rate of temperature fall from 60 DEG C is 3-5 DEG C/min.
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| CN109502970A (en) * | 2018-12-25 | 2019-03-22 | 南通瑞森光学股份有限公司 | A kind of infrared long wave leads to glass and its preparation process |
| CN111206214A (en) * | 2020-03-04 | 2020-05-29 | 成都国泰真空设备有限公司 | Coating process for effectively improving firmness problem of sulfur-series glass coating film |
| CN113031123A (en) * | 2021-03-02 | 2021-06-25 | 长春理工大学 | Antireflection sheet preparation method and antireflection sheet |
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| CN115494565A (en) * | 2022-09-15 | 2022-12-20 | 安徽光智科技有限公司 | Infrared antireflection film for protecting laser, preparation method and application |
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