CN104459835A - Infrared glass GASIR1 antireflection film and preparation method thereof - Google Patents

Infrared glass GASIR1 antireflection film and preparation method thereof Download PDF

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CN104459835A
CN104459835A CN201410816909.4A CN201410816909A CN104459835A CN 104459835 A CN104459835 A CN 104459835A CN 201410816909 A CN201410816909 A CN 201410816909A CN 104459835 A CN104459835 A CN 104459835A
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layer
gasir1
zns
reflection film
infrared glass
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CN104459835B (en
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朱敏
李全民
王国力
谢玉春
梁思远
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Nanjing Wavelength Optoelectronics Technology Co Ltd
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Nanjing Wavelength Optoelectronics Technology 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623—Sulfides, selenides or tellurides
    • C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Toxicology (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Physical Vapour Deposition (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention discloses an infrared glass GASIR1 antireflection film and a preparation method of the infrared glass GASIR1 antireflection film. The infrared glass GASIR1 antireflection film comprises a substrate layer, a ZnSe layer, Ge layers, ZnS layers and YF3 layers in sequence, wherein the Ge layers and ZnS layers are arranged alternately, the YF3 layers and the ZnS layers are arranged alternately, the Ge layers are not adjacent to the YF3 layers, the outermost layer of the infrared glass GASIR1 antireflection film is one ZnS layer, and the thickness of the infrared glass GASIR1 antireflection film except the substrate layer is 4000+/-200 nm. The infrared glass GASIR1 antireflection film is low in single-side reflectivity and easy to prepare, and all the layers are high in density, matched in stress and high in adhesive force.

Description

A kind of infrared glass GASIR1 anti-reflection film and preparation method thereof
Technical field
The present invention relates to a kind of infrared glass GASIR1 anti-reflection film and preparation method thereof.
Background technology
Anti-reflection film, also known as antireflecting film, is deposited on optical element surface, and to reduce surface reflection, increase the optical thin film of transmissivity of optical system, it can improve contrast by the scattered light in minimizing system.There is the defects such as reflectivity is high, film inter-laminar stress does not mate, film adhesion difference in existing infrared glass GASIR1 anti-reflection film.
Summary of the invention
There is the defects such as reflectivity is high, film inter-laminar stress does not mate, film adhesion difference to overcome infrared glass GASIR1 anti-reflection film in prior art, the invention provides a kind of infrared glass GASIR1 anti-reflection film and preparation method thereof.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is as follows:
A kind of infrared glass GASIR1 anti-reflection film, the YF comprising basalis, ZnSe layer, the Ge layer mutually replaced and ZnS layer successively and mutually replace 3layer and layer ZnS, wherein, Ge layer and YF 3layer is non-conterminous, and the outermost layer of infrared glass GASIR1 anti-reflection film is ZnS layer, and the thickness of infrared glass GASIR1 anti-reflection film except basalis is 4000 ± 200nm.
Above-mentioned basalis is infrared glass GASIR1.
Ge layer and YF 3layer is non-conterminous, refers to Ge layer and YF 3layer between with ZnS interlayer every.The outermost layer of infrared glass GASIR1 anti-reflection film refers to the layer contacted with air, also namely from basalis layer farthest.
Above-mentioned infrared glass GASIR1 anti-reflection film is particularly suited for the surperficial evaporation at infrared glass GASIR1, and the application's infrared glass GASIR1 anti-reflection film solves Stress match and the adhesion difficult problem of rete while possessing antireflective effect.
The thickness in monolayer of ZnSe layer thickness to be the thickness in monolayer of 60-400nm, ZnS layer be 60-700nm, Ge layer is 100-350nm, YF 3the thickness in monolayer of layer is 200-500nm.The Stress match degree between rete and adhesion can be strengthened so further.
Infrared glass GASIR1 anti-reflection film has 13 ± 2 layers except basalis.Reduce further the reflectivity of anti-reflection film like this.
Preferably, Ge layer has 2-5 layer, YF 3layer has 2-5 layer.Further ensure the reflectivity that anti-reflection film is low like this.
Further preferably, infrared glass GASIR1 anti-reflection film has 13 layers except basalis, is followed successively by ZnSe layer, Ge layer, ZnS layer, Ge layer, ZnS layer, Ge layer, ZnS layer, YF 3layer, ZnS layer, YF 3layer, ZnS layer, YF 3layer and ZnS layer.Reduce further the reflectivity of anti-reflection film like this, the unrelieved stress reducing rete improves the adhesion of rete simultaneously.
More preferably, be that ground floor is counted with ZnSe layer, ZnS layer is from third layer, and first three time appears as thick-layer, and latter three layers appear as thin layer, and wherein, thick-layer ZnS thickness is 500-700nm, and thin layer ZnS thickness is 60-200nm.Reduce further the reflectivity of anti-reflection film like this, enhance Stress match between each layer and adhesion.
The one side reflectivity of above-mentioned infrared glass GASIR1 anti-reflection film in the wave band of 8 to 14 microns is less than 1%.
The film-forming apparatus of above-mentioned anti-reflection film: preferably adopt southern light 900 type coating machine, it mainly comprises film-thickness monitoring, ion gun, vacuum chamber and vapo(u)rization system composition.Film thickness monitoring system is divided into light-operated and brilliant control two parts, and wherein brilliant control have employed the MDC360 controller of import, utilizes quartz crystal oscillation frequency to change and measures film quality thickness.Ion gun adopts the Kaufman ion source of Chinese Academy of Sciences's Beijing Institute For Space Studies development, controls ion energy by adjustment plate voltage and ion beam current, improves the density of deposit film, improves optics and mechanical property.Vacuum chamber cooperatively interacts by mechanical pump and diffusion pump system the vacuum tightness obtaining requirement of experiment, measures vacuum tightness with thermocouple needle.Not mentioned above all with reference to prior art.
The preparation method of above-mentioned infrared glass GASIR1 anti-reflection film, adopt and carry out plated film under vacuum conditions containing ionogenic coating machine, initial vacuum tightness is 2 × 10 -3± 2 × 10 -4pa, temperature is 150 ± 20 DEG C; Ionogenic accelerating potential is 200 ± 20V, and plate voltage is 400 ± 20V, and line is 40 ± 5mA.
Above-mentioned initial vacuum tightness refers to the vacuum tightness before starting material evaporation.
Before each layer raw materials evaporate, first with ion gun, substrate is carried out to the bombardment of 10 ± 2min.The preferred Kaufman ion source of ion gun, above-mentioned bombardment object is cleaning substrate, improves coefficient of concentration, strengthens the adhesion of rete.In the process of rete deposition, use Kaufman ion source to change based on the momentum of ion pair deposited particles, improve the kinetic energy of deposited particles and the mobility of deposited particles, increase gather density, improve structural intergrity and Stress match, thus improve performance and the service time of rete.
Preferably, the raw-material evaporation rate of ZnSe layer is the raw-material evaporation rate of 0.4 ± 0.05nm/s, Ge layer be the raw-material evaporation rate of 0.2 ± 0.05nm/s, ZnS layer is 0.4 ± 0.05nm/s, YF 3the raw-material evaporation rate of layer is 0.5 ± 0.05nm/s.Further ensure density and the adhesion of each layer like this, thus further increase the optical property of anti-reflection film.
The application adopts light-operated method control both optical thickness, adopts brilliant control method to control evaporation rate simultaneously, requires that the variations in refractive index of adjacent two layers material is little, and raw-material character is little by preparation effects of process parameters.
Because Ge material can cause splash when line is excessive, therefore be coated with in process want abundant fritting, the implication of unit nm/s is increased nano thickness per second.
The NM technology of the present invention is all with reference to prior art.
Infrared glass GASIR1 anti-reflection film one side reflectivity of the present invention is low, and each rete density is high, and the stress between each rete matches, strong adhesion, and the preparation of infrared glass GASIR1 anti-reflection film is simple.
Accompanying drawing explanation
Fig. 1 is embodiment 3 gained infrared glass GASIR1 anti-reflection film structural representation.
In figure, 1 be basalis, 2 for ZnSe layer, 3 is Ge layer, and 4 is ZnS layer, and 5 is YF 3layer.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
The film-forming apparatus of anti-reflection film in each example: adopt southern light 900 type coating machine, it mainly comprises film-thickness monitoring, ion gun, vacuum chamber and vapo(u)rization system composition.Film thickness monitoring system is divided into light-operated and brilliant control two parts, and wherein brilliant control have employed the MDC360 controller of import, utilizes quartz crystal oscillation frequency to change and measures film quality thickness.Ion gun adopts the Kaufman ion source of Chinese Academy of Sciences's Beijing Institute For Space Studies development, controls ion energy by adjustment plate voltage and ion beam current, improves the density of deposit film, improves optics and mechanical property.Vacuum chamber cooperatively interacts by mechanical pump and diffusion pump system the vacuum tightness obtaining requirement of experiment, measures vacuum tightness with thermocouple needle.
Embodiment 1
Infrared glass GASIR1 anti-reflection film, comprises basalis, ZnSe layer, Ge layer, ZnS layer, Ge layer, ZnS layer, Ge layer, ZnS layer, YF successively 3layer, ZnS layer, YF 3layer and ZnS layer.The thickness of infrared glass GASIR1 anti-reflection film except basalis is 3800nm.
The thick of ZnSe layer is 60nm, is that ground floor is counted with ZnSe layer, and ZnS layer is from third layer, and first three time appears as thick-layer, two-layerly appears as thin layer afterwards, and wherein, thick-layer ZnS thickness is 500nm, and thin layer ZnS thickness is 60nm; Ge layer thickness in monolayer is 200nm.
The preparation method of above-mentioned infrared glass GASIR1 anti-reflection film, initial vacuum tightness is 2 × 10 -3-10 -4pa, temperature is 130 DEG C; Ionogenic accelerating potential is 180V, and plate voltage is 380V, and line is 35mA.
Before each layer raw materials evaporate, first with ion gun, substrate is carried out to the bombardment of 8min.
The raw-material evaporation rate of ZnSe layer is the raw-material evaporation rate of 0.4-0.05nm/s, Ge layer be the raw-material evaporation rate of 0.2-0.05nm/s, ZnS layer be the raw-material evaporation rate of 0.4-0.05nm/s, YF3 layer is 0.5-0.05nm/s.
In embodiment, other technology NM is with reference to prior art.
Embodiment 2
Infrared glass GASIR1 anti-reflection film, comprises basalis, ZnSe layer, Ge layer, ZnS layer, Ge layer, ZnS layer, Ge layer, ZnS layer, YF successively 3layer, ZnS layer, YF 3layer, ZnS layer, YF 3layer, ZnS layer, YF 3layer and ZnS layer.The thickness of infrared glass GASIR1 anti-reflection film except basalis is 4200nm.
The thick of ZnSe layer is 400nm, is that ground floor is counted with ZnSe layer, and ZnS layer is from third layer, and first three time appears as thick-layer, and latter four layers appear as thin layer, and wherein, thick-layer ZnS thickness is 700nm, and thin layer ZnS thickness is 200nm; Ge thickness is 100nm.
The preparation method of above-mentioned infrared glass GASIR1 anti-reflection film, initial vacuum tightness is 2 × 10 -3+ 10 -4pa, temperature is 170 DEG C; Ionogenic accelerating potential is 220V, and plate voltage is 420V, and line is 45mA.
Before each layer raw materials evaporate, first with ion gun, substrate is carried out to the bombardment of 12min.
The raw-material evaporation rate of ZnSe layer is the raw-material evaporation rate of 0.4+0.05nm/s, Ge layer be the raw-material evaporation rate of 0.2+0.05nm/s, ZnS layer be the raw-material evaporation rate of 0.4+0.05nm/s, YF3 layer is 0.5+0.05nm/s.
Embodiment 3
Infrared glass GASIR1 anti-reflection film as shown in the figure, comprises basalis, ZnSe layer, Ge layer, ZnS layer, Ge layer, ZnS layer, Ge layer, ZnS layer, YF successively 3layer, ZnS layer, YF 3layer, ZnS layer, YF 3layer and ZnS layer.The thickness of infrared glass GASIR1 anti-reflection film except basalis is 4000nm.
The thick of ZnSe layer is 200nm, is that ground floor is counted with ZnSe layer, and ZnS layer is from third layer, and first three time appears as thick-layer, and latter three layers appear as thin layer, and wherein, thick-layer ZnS thickness is 650nm, and thin layer ZnS thickness is 100nm; Ge thickness is 250nm.
The preparation method of above-mentioned infrared glass GASIR1 anti-reflection film, initial vacuum tightness is 2 × 10 -3pa, temperature is 150 DEG C; Ionogenic accelerating potential is 200V, and plate voltage is 400V, and line is 40mA.
Before each layer raw materials evaporate, first with ion gun, substrate is carried out to the bombardment of 10min.
The raw-material evaporation rate of ZnSe layer is the raw-material evaporation rate of 0.4nm/s, Ge layer is 0.2nm/s, and the raw-material evaporation rate of ZnSe layer is the raw-material evaporation rate of 0.4nm/s, YF3 layer is 0.5nm/s.
In above-mentioned each example, the performance test of gained anti-reflection film is as follows:
Film layer spectrum is tested:
Adopt the one side reflectivity of SPECTRUM100 spectrophotometer to film of PE company of the U.S. to test, the anti-reflection film in each example is at the equal < 1% of the reflectivity R of 8 to 14 micron wavebands.
Film performance is tested:
According to the requirement of GJB2485-95 optical film general specification, the following environmental test to each routine gained anti-reflection film sample has carried out:
(1) high/low temperature test: under Packing Condition, plated film print is put into high/low temperature experimental box (intensification of this high/low temperature experimental box and cooling rate are all less than 2 DEG C/min), 2h is kept respectively in the low temperature of (one 62 ± 2) DEG C, in the high temperature of (70 ± 2) DEG C, keep 2h, the rete of each routine gained anti-reflection film is all without phenomenons such as peeling, foaming, crackle, demouldings.
(2) physical strength experiment: wrap up in 2 layers of drying defatted gauze outside rubber friction head, rubs to rete along same track under keeping 4.9N pressure, and come and go 25 times, the rete of each routine gained anti-reflection film is all without scratch equivalent damage.
(3) poly-adhesion experiment: with wide be 2cm, the adhesive tape of peel strength I>2.94N/cm is cemented in the film surface of each routine gained anti-reflection film, by adhesive tape from the edge of part after the rapid pull-up of vertical direction on surface, the rete of each routine gained anti-reflection film all without coming off, not damaged.

Claims (10)

1. an infrared glass GASIR1 anti-reflection film, is characterized in that: the YF comprising basalis, ZnSe layer, the Ge layer mutually replaced and ZnS layer successively and mutually replace 3layer and layer ZnS, wherein, Ge layer and YF 3layer is non-conterminous, and the outermost layer of infrared glass GASIR1 anti-reflection film is ZnS layer, and the thickness of infrared glass GASIR1 anti-reflection film except basalis is 4000 ± 200nm.
2. infrared glass GASIR1 anti-reflection film as claimed in claim 1, is characterized in that: the thickness in monolayer of ZnSe layer thickness to be the thickness in monolayer of 60-400nm, ZnS layer be 60-700nm, Ge layer is 100-350nm, YF 3the thickness in monolayer of layer is 200-500nm.
3. infrared glass GASIR1 anti-reflection film as claimed in claim 1 or 2, is characterized in that: infrared glass GASIR1 anti-reflection film has 13 ± 2 layers except basalis.
4. infrared glass GASIR1 anti-reflection film as claimed in claim 3, is characterized in that: Ge layer has 2-5 layer, YF 3layer has 2-5 layer.
5. infrared glass GASIR1 anti-reflection film as claimed in claim 4, is characterized in that: infrared glass GASIR1 anti-reflection film has 13 layers except basalis, is followed successively by ZnSe layer, Ge layer, ZnS layer, Ge layer, ZnS layer, Ge layer, ZnS layer, YF 3layer, ZnS layer, YF 3layer, ZnS layer, YF 3layer and ZnS layer.
6. infrared glass GASIR1 anti-reflection film as claimed in claim 5, is characterized in that: be that ground floor is counted with ZnSe layer, ZnS layer is from third layer, first three time appears as thick-layer, and latter three layers appear as thin layer, wherein, thick-layer ZnS thickness is 500-700nm, and thin layer ZnS thickness is 60-200nm.
7. infrared glass GASIR1 anti-reflection film as claimed in claim 1 or 2, is characterized in that: the one side reflectivity of infrared glass GASIR1 anti-reflection film in the wave band of 8 to 14 microns is less than 1%.
8. the preparation method of the infrared glass GASIR1 anti-reflection film described in claim 1-7 any one, is characterized in that: adopt and carry out plated film under vacuum conditions containing ionogenic coating machine, initial vacuum tightness is 2 × 10 -3± 2 × 10 -4pa, temperature is 150 ± 20 DEG C; Ionogenic accelerating potential is 200 ± 20V, and plate voltage is 400 ± 20V, and line is 40 ± 5mA.
9. preparation method as claimed in claim 8, is characterized in that: before each layer raw materials evaporate, first with ion gun, substrate is carried out to the bombardment of 10 ± 2min.
10. preparation method as claimed in claim 8, it is characterized in that: the raw-material evaporation rate of ZnSe layer is 0.4 ± 0.05nm/s, the raw-material evaporation rate of Ge layer is 0.2 ± 0.05nm/s, the raw-material evaporation rate of ZnS layer is the raw-material evaporation rate of 0.4 ± 0.05nm/s, YF3 layer is 0.5 ± 0.05nm/s.
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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN105388542A (en) * 2015-12-02 2016-03-09 中国建筑材料科学研究总院 Ge-As-Se infrared glass with anti-reflection film and preparation method thereof
CN105911616A (en) * 2016-06-23 2016-08-31 南京波长光电科技股份有限公司 Antireflection coating plated on infrared glass and preparation method thereof
CN107227460A (en) * 2017-07-13 2017-10-03 南京波长光电科技股份有限公司 A kind of anti-reflection DLC film by substrate of chalcogenide infrared glass and preparation method thereof
CN108318944A (en) * 2018-02-07 2018-07-24 无锡奥芬光电科技有限公司 A kind of resin anti-reflection film and preparation method thereof
CN108330440A (en) * 2018-01-05 2018-07-27 昆明凯航光电科技有限公司 A kind of 3-12 μm of ZnS substrates optical infrared anti-reflection film and preparation method thereof

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JP2012501073A (en) * 2008-08-28 2012-01-12 エーエスエムエル ネザーランズ ビー．ブイ． Spectral purity filter and lithographic apparatus
CN102812386A (en) * 2010-10-12 2012-12-05 住友电工硬质合金株式会社 Optical component
CN204331075U (en) * 2014-12-24 2015-05-13 南京波长光电科技股份有限公司 A kind of infrared glass GASIR1 anti-reflection film

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CN101960338A (en) * 2008-02-27 2011-01-26 Asml荷兰有限公司 The device of optical element, the lithographic equipment that comprises this optical element, device making method and manufacturing
JP2012501073A (en) * 2008-08-28 2012-01-12 エーエスエムエル ネザーランズ ビー．ブイ． Spectral purity filter and lithographic apparatus
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105388542A (en) * 2015-12-02 2016-03-09 中国建筑材料科学研究总院 Ge-As-Se infrared glass with anti-reflection film and preparation method thereof
CN105911616A (en) * 2016-06-23 2016-08-31 南京波长光电科技股份有限公司 Antireflection coating plated on infrared glass and preparation method thereof
CN107227460A (en) * 2017-07-13 2017-10-03 南京波长光电科技股份有限公司 A kind of anti-reflection DLC film by substrate of chalcogenide infrared glass and preparation method thereof
CN107227460B (en) * 2017-07-13 2019-09-06 南京波长光电科技股份有限公司 It is a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof
CN108330440A (en) * 2018-01-05 2018-07-27 昆明凯航光电科技有限公司 A kind of 3-12 μm of ZnS substrates optical infrared anti-reflection film and preparation method thereof
CN108318944A (en) * 2018-02-07 2018-07-24 无锡奥芬光电科技有限公司 A kind of resin anti-reflection film and preparation method thereof

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