CN105388542B - Germanium antimony selenium infrared glass with antireflective film and preparation method thereof - Google Patents
Germanium antimony selenium infrared glass with antireflective film and preparation method thereof Download PDFInfo
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- CN105388542B CN105388542B CN201510874951.6A CN201510874951A CN105388542B CN 105388542 B CN105388542 B CN 105388542B CN 201510874951 A CN201510874951 A CN 201510874951A CN 105388542 B CN105388542 B CN 105388542B
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- 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
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Abstract
The invention discloses a kind of germanium antimony selenium infrared glass with antireflective film and preparation method thereof, belong to glass processing field, wherein the germanium antimony selenium infrared glass with antireflective film, it includes the outer glass-base of germanium antimony selenium ruby；The outer glass-base of described germanium antimony selenium ruby is made up of by weight/mass percentage composition following component：Germanium：12%, antimony：28%, selenium：60%；The first fluorination ytterbium layer, the first zinc sulfide layer, the second fluorination ytterbium layer and the second zinc sulfide layer have been sequentially depositing on the outer glass-base of described germanium antimony selenium ruby.The germanium antimony selenium infrared glass with antireflective film in the present invention can effectively prevent coming off for antireflective film, reduce the reflectivity of infrared glass.
Description
Technical field
The present invention relates to glass processing field, and in particular to a kind of germanium antimony selenium infrared glass and its preparation with antireflective film
Method.
Background technology
Germanium antimony selenium infrared glass is the infrared optical material of a class function admirable, but its fragility is big, surface residual reflectivity
It is high, it is impossible to directly to use.
The conventional means for reducing the reflectivity of glass material at present is in glass material plated surface antireflective film, patent
CN104459835A describes a kind of infrared glass GASIRl anti-reflection films, and it uses 4 kinds of coating materials, and film layer number is 2 layers of 13 scholar, total thickness
Degree reaches 4000 scholar 200nm, and through design, surface residual reflectivity can be down to less than 1%.
But the membrane system exist it is excessive using coating materials, the shortcomings of the number of plies and big thickness；In addition, GASIRl infrared glasses are Ge-
As-Se systems, different from germanium antimony selenium infrared glass physicochemical characteristic, the film structure and preparation method are not suitable for outside germanium antimony selenium ruby
Glass.Compared with the infrared crystal material such as germanium, germanium antimony selenium ruby is outer, and glass transformation temperature is low, fragility is big, physicochemical characteristic is poor, using normal
The rule film layer for preparing of film layer preparation technology, the problems such as easily film layer occur and come off.Germanium antimony selenium infrared glass and Ge-As-Se
The physico-chemical property difference of system and its elemental Germanium is very big, it is impossible to which the two antireflective film for being used directly is used into the outer glass of germanium antimony selenium ruby
On glass, and have not yet to see the report about germanium antimony selenium infrared glass anti-reflection.
The content of the invention
Present invention is primarily aimed at, there is provided a kind of germanium antimony selenium infrared glass with antireflective film, reduce germanium antimony selenium ruby
The reflectivity of outer glass, its antireflective film system stress matching is good, it is therefore prevented that the outer coating film on glass of germanium antimony selenium ruby comes off.
Present invention also offers a kind of preparation method of the germanium antimony selenium infrared glass with antireflective film.
The purpose of the present invention and its solution technical problem are achieved by the following technical solution：
A kind of germanium antimony selenium infrared glass with antireflective film, it includes the outer glass-base of germanium antimony selenium ruby；Described germanium antimony selenium
Infrared glass basic unit is made up of by weight/mass percentage composition following component：Germanium：12%, antimony：28%, selenium：60%；The germanium antimony selenium ruby
The first fluorination ytterbium layer, the first zinc sulfide layer, the second fluorination ytterbium layer and the second zinc sulfide layer have been sequentially depositing on outer glass-base.
Further, the first described fluorination ytterbium layer optical thickness is 173 ± 20nm.
Further, the first described zinc sulfide layer optical thickness is 1817 ± 120nm.
Further, the second described fluorination ytterbium layer optical thickness is 1566 ± 80nm.
Further, the second described zinc sulfide layer optical thickness is 333 ± 25nm.
On the other hand, a kind of preparation method of the germanium antimony selenium infrared glass with antireflective film, comprises the following steps：
(1) the outer glass substrate of germanium antimony selenium ruby is cleaned and is preheated；
(2) cleaning before copper plating is carried out to the outer glass substrate of described germanium antimony selenium ruby using ion gun；
(3) evaporation first is fluorinated ytterbium layer, the first zinc sulfide layer, the second fluorination ytterbium layer and the second zinc sulfide layer successively；
(4) it is cooled to room temperature and obtains the germanium antimony selenium infrared glass with antireflective film.
Further, described step (1) specifically includes following steps：
The outer glass substrate of described germanium antimony selenium ruby is cleaned by ultrasonic using acetone and alcohol ether, vacuum >=
5.0×10-3Heated under the conditions of pa, design temperature is 100-120 DEG C, heating rate is：From room temperature to 60 DEG C, 1.5-3 DEG C/min,
From 60 DEG C to described design temperature, 1-2 DEG C/min；Insulation.
Further, described step (2) specifically includes following steps：Ion gun is opened, described ion gun is Hall
Ion gun, is filled with argon gas amount for 30-40sccm, and it is 7.0 × 10 to set pressure-3-1.0×10-2Pa, anode voltage is 100-
150V, anode current is 1-2A, and scavenging period is 15-20min.
Further, the evaporation plating parameter of the first described fluorination ytterbium layer is as follows：Pressure is 8.0 × 10-3-2.0 × 10-
2pa, sedimentation rate is 0.1-0.3nm/s, and deposit optical thickness is 150-180nm, and argon gas amount is 30-40sccm, anode voltage
It is 100-150V, 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, sedimentation rate
It is 1-3nm/s, deposit optical thickness is 1600-1950nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, anode
Electric 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, sedimentation rate
It is 0.1-0.3nm/s, deposit optical thickness is 1300-1700nm, and argon gas amount is 30-40sccm, and 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 second described fluorination ytterbium layer is as follows：Pressure is 5.0 × 10-3-2.0×10-2Pa, sedimentation rate
It is 1-3nm/s, deposit optical thickness is 200-400nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, anode electricity
It is 1-2A to flow, and in deposition process, workpiece plate rotating speed is 10-20rpm.
Further, the described room temperature that is cooled to is comprised the following steps that：60 DEG C of cooling speed are down to from described design temperature
Rate is 2-4 DEG C/min, and room temperature rate of temperature fall is down to from 60 DEG C for 3-5 DEG C/min.
Compared with prior art, the germanium antimony selenium infrared glass of the present invention with antireflective film and preparation method thereof at least has such as
Lower beneficial effect：
The present patent application will be provided with antireflective film on germanium antimony selenium infrared glass, reduce surface residual reflectivity, improve
The through performance of germanium antimony selenium infrared glass.
Membrane system gross thickness is low, and membrane system Stress match is good：Infrared film system gross thickness is larger, and stress is typically with the increase of thickness
Increase, the stress of increase is huge threat to the firmness of film layer, therefore, during Film Design, just must take into consideration each in membrane system
The collocation of thicknesses of layers and gross thickness, the present patent application using zinc sulphide with fluorination ytterbium stress types conversely, simultaneously control individual layer and
Gross thickness size, realizes good Stress match.
Film layer and substrate, film layer are good with film ply adhesion；Residual reflectance is low, meets optical system to infrared glass
Transmission require；The outer glass expansion coefficient of germanium antimony selenium ruby is larger, belongs to fragile material, and gradient increased temperature and cooling are used during plated film, has
Effect avoid infrared glass because temperature change it is big caused by it is easily rupturable the problems such as；Using low energy high density ion assisted deposition side
Formula, it is to avoid the temperature rise in coating process, improves the performance of film layer.
Brief description of the drawings
The film structure schematic diagram of Fig. 1 germanium antimony selenium infrared glasses of the present invention with antireflective film；
Fig. 2 is that the film structure residual reflectance Theoretical Design of germanium antimony selenium infrared glass of the present invention with antireflective film is bent
Line；
Fig. 3 is the film structure residual reflectance measured curve of germanium antimony selenium infrared glass of the present invention with antireflective film.
Specific embodiment
A kind of germanium antimony selenium infrared glass with antireflective film is the embodiment of the invention provides, its antireflective film is difficult for drop-off, subtracts
Minus effect is good.
Germanium antimony selenium glass selected in following examples is Ge12Sb28Se60Glass, i.e., by the group of following mass fraction
It is grouped into：Germanium：12%, antimony：28%, selenium：60%.
Fig. 1 is the outer glass structure schematic diagram of the germanium antimony selenium ruby with antireflective film in the embodiment of the present invention.
Embodiment 1
The preparation method of the germanium antimony selenium infrared glass with antireflective film, comprises the following steps：
(1) clean and its preheat：Acetone and alcohol ether mixed liquor is respectively adopted carries out ultrasonic wave to infrared glass substrate
Cleaning, scavenging period is each 15min, finally, substrate is put into oven for drying；After the completion of drying, quick-clamping substrate is put into very
Empty room, extracts vacuum.Vacuum reaches 5.0 × 10-3Pa, adjusts drying lamp output voltage, and heating rate is：- 60 DEG C of room temperature,
30min, 60 DEG C -100 DEG C, 30min to after temperature, is incubated 1.2h.
Need exist for explanation be：Germanium antimony selenium infrared glass is fragile material, and gradient increased temperature can prevent temperature change acute
The strong glass for causing ruptures.
(2) cleaning of ion auxiliary, opens ion gun, is filled with argon gas amount for 35sccm, and pressure in vacuum tank is 9 × 10-3Pa, sun
Pole tension is 130V, and anode current is 1.5A, and workpiece plate rotating speed is 10rpm, and scavenging period is 18min.
(3) plated film：
It is coated with a YbF3Film, pressure in vacuum tank is 9.0 × 10 during evaporation-3Pa, sedimentation rate is 0.2nm/s, using crystalline substance
Vibration Meter controls sedimentation rate, and deposit optical thickness is 173nm, and film layer optical thickness is controlled using optical film thickness meter.
Ground floor ZnS films are coated with, pressure in vacuum tank is 8.0 × 10 during evaporation-3Pa, sedimentation rate is 1nm/s, deposit optical
Thickness is 1817nm, using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
It is coated with the 2nd YbF3Film, pressure in vacuum tank is 9.0 × 10 during evaporation-3Pa, sedimentation rate is 0.2nm/s, deposits light
Thickness is 1566nm, using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
The 2nd ZnS films are coated with, pressure in vacuum tank is 8.0 × 10 during evaporation-3Pa, sedimentation rate is 1nm/s, and deposit optical is thick
It is 333nm to spend, and using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
Need exist for explanation be：In coating process, with the increase of thicknesses of layers, the refraction of whole infrared glass system
Rate will change, by controlling the sedimentation rate of optical thickness and its plated film more scientific and reasonable；Film layer is too thick easily to be made
Film forming comes off, too thin and be unable to reach preferable anti-reflection effect；Under vacuum condition plated film can strengthen film layer adhesive force and
Compactness, improves its anti-reflection effect.
After the completion of 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 plating
Film infrared glass；Using gradient cooling prevents the film layer acutely caused for temperature change easy to fall off.
As shown in figure 1, the film structure that germanium antimony selenium infrared glass manufactured in the present embodiment has is 2 kinds the 4 of coating materials composition
Rotating fields；
Ground floor is YbF3, optical thickness is 173nm, and the 2nd layer is ZnS, and optical thickness is 1817nm, and the 3rd layer is YbF3,
Optical thickness is 1566nm, the 4th layer of ZnS, and optical thickness is 333nm.
Need exist for explanation be：Zinc sulphide is with fluorination ytterbium stress types conversely, film layer is attached caused by can preventing stress
Put forth effort not strong；Four film structures cause that the thickness of every tunic is moderate, and anti-reflection effect is preferable, and if duplicature, anti-reflection effect is not
It is preferable；And if film layer is more than four layers, although anti-reflection effect is preferable, but gross thickness increases, and coating cost can increase a lot, four layers
Membrane structure has fully achieved preferable anti-reflection effect and adhesive force is good；Result is as follows after tested：
Fig. 2 and Fig. 3 are respectively the film structure residual reflectance that the present embodiment has the germanium antimony selenium infrared glass of antireflective film
Theoretical Design curve and measured curve.Figure it is seen that the theoretical anti-reflection effect of four layers of antireflective film is very well, in 8-12nm
Below 0.7%, from figure 3, it can be seen that in the range of wavelength 8-12um, the anti-reflection membranous system can be by for interior its reflectivity
Ge12Sb28Se60When infrared glass surface residual reflectivity is by non-plated film 18.3%, less than 1% is reduced to, its luminance factor reason
Slightly higher by being worth, this is because in deposition process, thicknesses of layers control error is caused；Meanwhile, antireflective film prepared by the present invention, energy
Enough environmental testings by GJB150-90, excellent performance.
Embodiment 2
Acetone and alcohol ether mixed liquor is respectively adopted carries out ultrasonic wave cleaning, scavenging period difference to infrared glass substrate
It is each 13min and 16min, finally, substrate is put into oven for drying.
After the completion of drying, quick-clamping substrate is put into vacuum chamber, extracts vacuum；Vacuum reaches 8.0 × 10-3Pa, adjustment is dried
Heat lamp output voltage, heating rate is：- 60 DEG C of room temperature, 30min, 60 DEG C -120 DEG C, 40min；To after temperature, 1.5 hours are incubated.
Argon gas 40sccm is filled with, pressure in vacuum tank is 8.0 × 10-3Pa, opens ion gun, and adjustment source parameters is：Sun
Pole tension 100V, anode current is 2A, and workpiece plate rotating speed is 10rpm.
It is coated with a YbF3Film, pressure in vacuum tank is 1.0 × 10 during evaporation-2Pa, sedimentation rate is 0.15nm/s, using crystalline substance
Vibration Meter controls sedimentation rate, and deposit optical thickness is 153nm, and film layer optical thickness is controlled using optical film thickness meter.
A ZnS films are coated with, pressure in vacuum tank is 9.0 × 10 during evaporation-3Pa, sedimentation rate is 1.5nm/s, deposit optical
Thickness is 1697nm, using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
It is coated with the 2nd YbF3Film, during evaporation pressure in vacuum tank be 1.0 ×-2Pa, sedimentation rate is 0.15nm/s, deposit optical
Thickness is 1646nm, using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
The 2nd ZnS films are coated with, pressure in vacuum tank is 9.0 × 10 during evaporation-3Pa, sedimentation rate is 1.5nm/s, deposit optical
Thickness is 358nm, using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
After the completion of 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.
Need exist for explanation be：The present embodiment using zinc sulphide with fluorination ytterbium stress types conversely, simultaneously control individual layer and
Gross thickness size, realizes good Stress match.
Film layer and substrate, film layer are good with film ply adhesion；Residual reflectance is low, meets optical system to infrared glass
Transmission require；Gradient increased temperature and cooling are used during plated film, infrared glass is effectively prevent because temperature change is big caused fragile
The problems such as splitting；Using low energy high density ion assisted deposition mode, it is to avoid the temperature rise in coating process, the property of film layer is improve
Energy.
The film structure having prepared by this implementation is 2 kinds of 4 Rotating fields of coating materials composition；1st layer is YbF3, optical thickness
It is 153nm, the 2nd layer is ZnS, and optical thickness is 1697nm, the 3rd layer is YbF3, optical thickness is 1646nm, the 4th layer of ZnS, light
Thickness is 358nm.
Embodiment 3
Acetone and alcohol ether mixed liquor is respectively adopted carries out ultrasonic wave cleaning, scavenging period difference to infrared glass substrate
It is each 18min and 12min, finally, substrate is put into oven for drying.
After the completion of drying, quick-clamping substrate is put into vacuum chamber, extracts vacuum；Vacuum reaches 1.0 × 10-2Pa, adjustment is dried
Heat lamp output voltage, heating rate is：- 60 DEG C of room temperature, 30min, 60 DEG C -120 DEG C, 40min；To after temperature, 1.5 hours are incubated.
Argon gas 40sccm is filled with, pressure in vacuum tank is 2.0 × 10-2Pa, opens ion gun, and adjustment source parameters is：Sun
Pole tension 150V, anode current is 1A, and workpiece plate rotating speed is 20rpm.
It is coated with a YbF3Film, pressure in vacuum tank is 2.0 × 10 during evaporation-2Pa, sedimentation rate is 0.15nm/s, using crystalline substance
Vibration Meter controls sedimentation rate, and deposit optical thickness is 193nm, and film layer optical thickness is controlled using optical film thickness meter.
A ZnS films are coated with, pressure in vacuum tank is 2.0 × 10 during evaporation-2Pa, sedimentation rate is 3nm/s, and deposit optical is thick
It is 1937nm to spend, and using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
It is coated with the 2nd YbF3Film, during evaporation pressure in vacuum tank be 2.0 ×-2Pa, sedimentation rate is 0.3nm/s, deposit optical
Thickness is 1486nm, using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
The 2nd ZnS films are coated with, pressure in vacuum tank is 2.0 × 10 during evaporation-2Pa, sedimentation rate is 3nm/s, and deposit optical is thick
It is 308nm to spend, and using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
After the completion of 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.
Film layer and substrate, film layer are good with film ply adhesion；Residual reflectance is low, meets optical system to infrared glass
Transmission require；Gradient increased temperature and cooling are used during plated film, infrared glass is effectively prevent because temperature change is big caused fragile
The problems such as splitting；Using low energy high density ion assisted deposition mode, it is to avoid the temperature rise in coating process, the property of film layer is improve
Energy.
Embodiment 4
Acetone and alcohol ether mixed liquor is respectively adopted carries out ultrasonic wave cleaning, scavenging period difference to infrared glass substrate
It is each 15min and 17min, finally, substrate is put into oven for drying.
After the completion of drying, quick-clamping substrate is put into vacuum chamber, extracts vacuum；Vacuum reaches 7.0 × 10-3Pa, adjustment is dried
Heat lamp output voltage, heating rate is：- 60 DEG C of room temperature, 30min, 60 DEG C -100 DEG C, 55min；To after temperature, 1.5 hours are incubated.
Argon gas 40sccm is filled with, pressure in vacuum tank is 2.0 × 10-2Pa, opens ion gun, and adjustment source parameters is：Sun
Pole tension 125V, anode current is 1.5A, and workpiece plate rotating speed is 15rpm, and scavenging period is 20min.
It is coated with a YbF3Film, pressure in vacuum tank is 8.0 × 10 during evaporation-3Pa, sedimentation rate is 0.1nm/s, using crystalline substance
Vibration Meter controls sedimentation rate, and deposit optical thickness is 183nm, and film layer optical thickness is controlled using optical film thickness meter.
A ZnS films are coated with, pressure in vacuum tank is 5.0 × 10 during evaporation-3Pa, sedimentation rate is 1nm/s, and deposit optical is thick
It is 1937nm to spend, and using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
It is coated with the 2nd YbF3Film, during evaporation pressure in vacuum tank be 8.0 ×-3Pa, sedimentation rate is 0.1nm/s, deposit optical
Thickness is 1486nm, using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
The 2nd ZnS films are coated with, pressure in vacuum tank is 5.0 × 10 during evaporation-3Pa, sedimentation rate is 1nm/s, and deposit optical is thick
It is 308nm to spend, and using crystal oscillator instrument control sedimentation rate, film layer optical thickness is controlled using optical film thickness meter.
After the completion of 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.
Film layer and substrate, film layer are good with film ply adhesion；Residual reflectance is low, meets optical system to infrared glass
Transmission require；Gradient increased temperature and cooling are used during plated film, infrared glass is effectively prevent because temperature change is big caused fragile
The problems such as splitting；Using low energy high density ion assisted deposition mode, it is to avoid the temperature rise in coating process, the property of film layer is improve
Energy.
The not most part of the present invention program, is what those skilled in the art can complete using routine techniques as needed,
Will not be described in detail herein.
The above, specific embodiment only of the invention, but protection scope of the present invention is not limited thereto, and it is any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all contain
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (5)
1. a kind of germanium antimony selenium infrared glass with antireflective film, it includes the outer glass-base of germanium antimony selenium ruby；Described germanium antimony selenium ruby
Outer glass-base is made up of by weight/mass percentage composition following component：Germanium：12%, antimony：28%, selenium：60%；Characterized in that, institute
The first fluorination ytterbium layer, the first zinc sulfide layer, the second fluorination ytterbium layer and the have been sequentially depositing on the outer glass-base of the germanium antimony selenium ruby stated
Curing zinc layers；
The first described fluorination ytterbium layer optical thickness is 173 ± 20nm；
The first described zinc sulfide layer optical thickness is 1817 ± 120nm；
The second described fluorination ytterbium layer optical thickness is 1566 ± 80nm；
The second described zinc sulfide layer optical thickness is 333 ± 25nm.
2. a kind of preparation method of the germanium antimony selenium infrared glass with antireflective film, it is characterised in that comprise the following steps：
(1) the outer glass substrate of germanium antimony selenium ruby is cleaned and is preheated；
(2) cleaning before copper plating is carried out to the outer glass substrate of described germanium antimony selenium ruby using ion gun；
(3) evaporation first is fluorinated ytterbium layer, the first zinc sulfide layer, the second fluorination ytterbium layer and the second zinc sulfide layer successively；
(4) it is cooled to room temperature and obtains the germanium antimony selenium infrared glass with antireflective film；
The evaporation plating parameter of the first described fluorination ytterbium layer is as follows：Pressure is 8.0 × 10-3-2.0 × 10-2pa, and sedimentation rate is
0.1-0.3nm/s, deposit optical thickness is 150-180nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, anode
Electric 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, sedimentation rate is 1-
3nm/s, deposit optical thickness is 1600-1950nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, anode current
It is 1-2A, in deposition process, workpiece plate rotating speed is 10-20rpm；
The evaporation plating parameter of the second described fluorination ytterbium layer is as follows：Pressure is 8.0 × 10-3-2.0×10-2Pa, sedimentation rate is 0.1-
0.3nm/s, deposit optical thickness is 1300-1700nm, and argon gas amount is 30-40sccm, and anode voltage is 100-150V, anode electricity
It is 1-2A to flow, 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, sedimentation rate is 1-
3nm/s, 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, in deposition process, workpiece plate rotating speed is 10-20rpm.
3. the preparation method of the germanium antimony selenium infrared glass with antireflective film according to claim 2, it is characterised in that described
The step of (1) specifically include following steps：
The outer glass substrate of described germanium antimony selenium ruby is cleaned by ultrasonic using acetone and alcohol ether, vacuum >=5.0 ×
10-3Heated under the conditions of pa, design temperature is 100-120 DEG C, heating rate is：From room temperature to 60 DEG C, 1.5-3 DEG C/min, from 60
DEG C to described design temperature, 1-2 DEG C/min；Insulation.
4. the preparation method of the germanium antimony selenium infrared glass with antireflective film according to claim 2, it is characterised in that described
The step of (2) specifically include following steps：Ion gun is opened, described ion gun is hall ion source, be filled with argon gas amount for 30-
40sccm, it is 7.0 × 10 to set pressure-3-1.0×10-2Pa, anode voltage is 100-150V, and anode current is 1-2A, cleaning
Time is 15-20min.
5. the preparation method of the germanium antimony selenium infrared glass with antireflective film according to claim 3, it is characterised in that described
The room temperature that is cooled to comprise the following steps that：60 DEG C of rate of temperature fall are down to for 2-4 DEG C/min from described design temperature, from 60 DEG C of drops
It is 3-5 DEG C/min to room temperature rate of temperature fall.
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| CN107356992A (en) * | 2017-07-31 | 2017-11-17 | 江苏淘镜有限公司 | A kind of antifatigue hardening lens and its production method |
| 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 |
| CN115201941B (en) * | 2021-04-13 | 2023-09-12 | 中国科学院上海技术物理研究所 | Efficient infrared wide-spectrum antireflection film suitable for space environment |
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| CN115494565B (en) * | 2022-09-15 | 2023-05-05 | 安徽光智科技有限公司 | Laser-protected infrared antireflection film, preparation method and application |
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| US7262412B2 (en) * | 2004-12-10 | 2007-08-28 | L-3 Communications Corporation | Optically blocked reference pixels for focal plane arrays |
| CN101445323B (en) * | 2008-12-31 | 2011-01-26 | 西安工业大学 | Chalcogenide infrared glass and preparation process thereof |
| CN103232161B (en) * | 2013-05-03 | 2015-11-04 | 中国建筑材料科学研究总院 | A kind of preparation method of Ge-Sb-Se system IR glass and equipment |
| CN104459835B (en) * | 2014-12-24 | 2016-06-29 | 南京波长光电科技股份有限公司 | A kind of infrared glass GASIR1 anti-reflection film and preparation method thereof |
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