CN107227460B - It is a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof - Google Patents
It is a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof Download PDFInfo
- Publication number
- CN107227460B CN107227460B CN201710570521.4A CN201710570521A CN107227460B CN 107227460 B CN107227460 B CN 107227460B CN 201710570521 A CN201710570521 A CN 201710570521A CN 107227460 B CN107227460 B CN 107227460B
- Authority
- CN
- China
- Prior art keywords
- layer
- dlc film
- infrared glass
- znse
- reflection
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
- C23C28/046—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material with at least one amorphous inorganic material layer, e.g. DLC, a-C:H, a-C:Me, the layer being doped or not
-
- 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
-
- 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
- C23C14/0605—Carbon
- C23C14/0611—Diamond
-
- 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
- C23C14/34—Sputtering
- C23C14/46—Sputtering by ion beam produced by an external ion source
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof.Using chalcogenide infrared glass as the anti-reflection DLC film of substrate, including chalcogenide infrared glass basal layer, DLC film layer and the adhesive layer being located between chalcogenide infrared glass basal layer and DLC film layer, adhesive layer includes the ZnSe layer alternateed and Ge layers, and ZnSe layer has 2-5 layers.The present invention has excellent antireflective effect, heat resistance, mechanical strength and adhesive force using chalcogenide infrared glass as the anti-reflection DLC film of substrate, and prepares simple, easy to operate.
Description
Technical field
The present invention relates to a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof, belongs to film manufacture
Field field.
Background technique
Chalcogenide infrared glass is that emerging infrared lens materials are compared with general infra-red material, the softening of this kind of material
Temperature is lower, and thermal expansion coefficient is larger, and plated film is easy to fall off on chalcogenide glass, especially plating DLC film, at present country's industry
There are no the reports that DLC film is plated on chalcogenide infrared glass.
Summary of the invention
In order to solve the defect of plated film hardly possible on chalcogenide infrared glass in the prior art, the present invention provides a kind of infrared with sulphur system
Glass is the anti-reflection DLC film and preparation method thereof of substrate.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
It is a kind of using chalcogenide infrared glass as the anti-reflection DLC film of substrate, including chalcogenide infrared glass basal layer, DLC film layer, with
And it is located at the adhesive layer between chalcogenide infrared glass basal layer and DLC film layer, adhesive layer includes the ZnSe layer and Ge alternateed
Layer, ZnSe layer have 2-5 layers.
Above-mentioned DLC film can reach single side reflectivity of the average reflectance less than 1.2%.
Chalcogenide glass refers to based on chalcogen Se etc. in the periodic table of elements and introduces a certain amount of other metalloid members
Element is formed by chalcogenide infrared glass, glass used in the preferred chalcogenide infrared glass basal layer of the application be Hubei Xinhua light letter
The chalcogenide glass of Materials Co., Ltd's production is ceased, the glass trade mark includes IRG202, IRG204, IRG205, IRG206 etc..
In order to guarantee that the antireflective effect and bond effect of products obtained therefrom, the anti-reflection wave band of anti-reflection DLC film are 8-12 microns.
In order to guarantee that the antireflective effect and bond effect of products obtained therefrom, chalcogenide infrared glass basal layer are adjacent with ZnSe layer；
Ge layers adjacent with DLC film layer.
Be in contact, fit for two layers mentioned by the adjacent finger of the application, between there is no other substances.
It is above-mentioned using chalcogenide infrared glass as the anti-reflection DLC film of substrate, including be connected in order chalcogenide infrared glass basal layer,
First ZnSe layer, the first Ge layers, the second ZnSe layer, the 2nd Ge layers, third ZnSe layer, the 3rd Ge layers and DLC film layer.
The above-mentioned total number of plies of method for using three kinds of materials to be alternately deposited can reach average reflectance less than 1.2% for 7 layers
The single side reflectivity of (external index is 1.5%), wherein the material selection of adhesive layer (that is: 6 layers preceding) and Film Design be very
Key directly affects adhesive force and antireflective effect between film layer.
In order to further ensure using chalcogenide infrared glass as the mechanical property and antireflective effect of the anti-reflection DLC film of substrate,
The thickness of one ZnSe layer, the second ZnSe layer and third ZnSe layer successively successively decreases, it is preferable that from the first ZnSe layer to DLC film layer, each layer
Physical thickness be followed successively by 400 ± 5nm, 242 ± 5nm, 246 ± 5nm, 177 ± 5nm, 180 ± 5nm, 400 ± 5nm and 1285 ±
5nm；Chalcogenide infrared glass basal layer with a thickness of 2-10mm.
In order to improve the antireflective effect of gained film layer, using chalcogenide infrared glass as the anti-reflection DLC film of substrate, including ZnS layers,
First YF3 layers, the first ZnSe layer, the 2nd YF3 layers, the second ZnSe layer, chalcogenide infrared glass basal layer, the first ZnSe layer, first
Ge layers, the second ZnSe layer, the 2nd Ge layers, third ZnSe layer, the 3rd Ge layers and DLC film layer, wherein ZnS layers with a thickness of 200 ±
5nm, the first YF3 layers with a thickness of 1046 ± 5nm, the first ZnSe layer with a thickness of 296 ± 5nm, the 2nd YF3 layers with a thickness of
105 ± 5nm, the second ZnSe layer with a thickness of 865 ± 5nm.
It is above-mentioned using chalcogenide infrared glass as the preparation method of the anti-reflection DLC film of substrate, successively in chalcogenide infrared glass substrate
Adhesive layer and DLC film layer are made on layer, the preparation of adhesive layer is plated under vacuum conditions using the coating machine containing ion source
Film, starting vacuum degree are (1 ± 0.1) × 10-3Pa, temperature are 100 ± 5 DEG C；The acceleration voltage of ion source is 200 ± 10V, anode
Voltage is 400 ± 10V, and line is 40 ± 5mA.
The application preferably uses southern 1100 type coating machine of light (for existing commercial equipment), mainly by film-thickness monitoring, from
Component, vacuum chamber and vapo(u)rization system composition.Film thickness monitoring system is divided into light-operated and brilliant control two parts, wherein brilliant control uses import
MDC360 controller, be to change to measure film quality thickness using quartz crystal frequency of oscillation, controlled using light-operated method
Optical thickness, while evaporation rate is controlled using brilliant control method.Ion source is using the Institute For Space Studies development of Chinese Academy of Sciences Beijing
Kaufman ion source can be improved the consistency of deposition film, improve optically and mechanically property by rationally controlling ion energy
Energy.Vacuum chamber cooperates to obtain the vacuum degree of requirement of experiment by mechanical pump and diffusion pumping system, with thermocouple needle to vacuum
Degree measures.
Before evaporation, the bombardment of 2min is carried out to substrate, it is therefore an objective to which cleaning substrate improves coefficient of concentration, reinforces the attached of film layer
Put forth effort.During film deposition, is converted using Kaufman ion source based on the momentum of ion pair deposited particles, improve deposition
The kinetic energy of particle and the mobility of deposited particles increase gather density, improve structural intergrity and Stress match, to improve
The performance of film layer and use the time.
In order to improve the accuracy of control and the anti-reflection performance and mechanics new capability of gained film, the evaporation rate of Ge is 0.2
The evaporation rate of ± 0.01nm/s, ZnSe are 0.4 ± 0.01nm/s (evaporation rate of two-sided ZnSe is consistent), YF3Evaporation speed
Rate is 0.6 ± 0.01nm/s.
DLC film layer is prepared in FJL600 type high vacuum hard carbon films filming equipment, and the sulphur system for having plated adhesive layer is red
After outer glass substrate layers ethanol ether (volume ratio 2:8) mixed liquor wiped clean, it is placed in FJL600 type high vacuum hard carbon films
FJL600 type high vacuum hard carbon films filming equipment is evacuated to less than 1.5 × 10 by the bottom crown of filming equipment-2Pa is passed through Ar
Gas, keeps gas pressure 3.3Pa~4Pa, power 200W, cleaning plated the chalcogenide infrared glass basal layer 5 of adhesive layer ±
1min；Then pass to methane, methane flow is 40sccm~50sccm, operating pressure is 7Pa~20Pa, power be 700 ±
DLC is deposited under conditions of 10W, and (diamond-like hard carbon films is sunk by the carbon atom that methane after radio frequency source ionization mixed gas decomposites
Product is at the DLC film based on diamond SP3 key) 30 ± 5min, power supply is then shut off, to get with sulphur after cooling 30 ± 5min clock
Series infrared glass is the anti-reflection DLC film layer of substrate.
DLC film-forming apparatus preferably uses FJL600 type high vacuum hard carbon films filming equipment (for existing commercial equipment), mainly
By coating chamber, target electrode, radio-frequency power supply and control power supply, sample rotary table；Pumping system, vacuum measurement system, air-channel system；Electricity
Control system；The composition such as water cooling system.Vacuum chamber cooperates to obtain desired vacuum degree by mechanical pump and molecular pump system,
Vacuum degree is measured with a Pirani gauge and an ionization gauge.Device is by the way of the coupling of upper and lower plates capacitance, up and down
Pole plate diameter ratio is 9/4, pole plate spacing 65mm, and excitation power supply is the radio frequency source of frequency 13.56MHz, power 2kW.
It is infrared using chalcogenide infrared glass as base in the surface of germanium selenium pozzuolite series infrared glass vapor deposition that The present invention gives a kind of
The preparation method of the anti-reflection DLC film at bottom has film layer while having DLC (diamond-film-like) scraping and wiping resistance performance anti-reflection
The effect of film can also solve the adhesive force problem that DLC film film layer is plated directly on such glass.
The unmentioned technology of the present invention is referring to the prior art.
The present invention has excellent antireflective effect, heat resistance, machine using chalcogenide infrared glass as the anti-reflection DLC film of substrate
Tool intensity and adhesive force, and prepare simple, easy to operate.
Detailed description of the invention
Fig. 1 is able to the single side reflectivity for the anti-reflection DLC film that chalcogenide infrared glass is substrate by embodiment 1；
Fig. 2 is able to the structural schematic diagram for the anti-reflection DLC film that chalcogenide infrared glass is substrate by embodiment 1；
Fig. 3 is the spectral detection curve graph of 3 gained film of embodiment；
In figure, 1 chalcogenide infrared glass basal layer, 2 first ZnSe layers, 3 the oneth Ge layers, 4 second ZnSe layers, 5 the 2nd Ge layers,
6 third ZnSe layers, 7 the 3rd Ge layers, 8DLC film layers.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
In each example, the preparation of adhesive layer uses southern 1100 type coating machine of light (for existing commercial equipment), mainly by film thickness
Controller, ion source, vacuum chamber and vapo(u)rization system composition.Film thickness monitoring system is divided into light-operated and brilliant control two parts, wherein brilliant control
Using the MDC360 controller of import, it is to be changed using quartz crystal frequency of oscillation to measure film quality thickness, uses
Light-operated method controls optical thickness, while controlling evaporation rate using brilliant control method.Ion source is ground using the Chinese Academy of Sciences, space, Beijing
Study carefully developed Kaufman ion source, by rationally controlling ion energy, the consistency of deposition film can be improved, improve optics
And mechanical performance.Vacuum chamber cooperates to obtain the vacuum degree of requirement of experiment by mechanical pump and diffusion pumping system, uses thermocouple
Meter measures vacuum degree.Before evaporation, the bombardment of 2min is carried out to substrate, it is therefore an objective to which cleaning substrate improves coefficient of concentration, adds
The adhesive force of strong film layer.During film deposition, turned using Kaufman ion source based on the momentum of ion pair deposited particles
It changes, improves the kinetic energy of deposited particles and the mobility of deposited particles, increase gather density, improve structural intergrity and stress
Match, to improve the performance of film layer and use the time.
The preparation of DLC film uses FJL600 type high vacuum hard carbon films filming equipment (for existing commercial equipment), mainly by plating
Film room, target electrode, radio-frequency power supply and control power supply, sample rotary table；Pumping system, vacuum measurement system, air-channel system；Automatically controlled system
System；The composition such as water cooling system.Vacuum chamber cooperates to obtain desired vacuum degree by mechanical pump and molecular pump system, with one
Branch Pirani gauge and an ionization gauge measure vacuum degree.Device is by the way of the coupling of upper and lower plates capacitance, upper bottom crown
Diameter ratio is 9/4, pole plate spacing 65mm, and excitation power supply is the radio frequency source of frequency 13.56MHz, power 2kW.
The glass trade mark used in chalcogenide infrared glass basal layer is IRG202, chalcogenide infrared glass in embodiment 2 in embodiment 1
The glass trade mark used in basal layer is IRG206.
Embodiment 1
It is a kind of using chalcogenide infrared glass as the anti-reflection DLC film of substrate, including be connected in order chalcogenide infrared glass basal layer,
First ZnSe layer, the first Ge layers, the second ZnSe layer, the 2nd Ge layers, third ZnSe layer, the 3rd Ge layers and DLC film layer.From first
ZnSe layer to DLC film layer, the physical thickness of each layer be followed successively by 400nm, 242nm, 246nm, 177nm, 180nm, 400nm,
1285nm, chalcogenide infrared glass basal layer with a thickness of 8mm.The anti-reflection wave band of anti-reflection DLC film is 8-12 microns.
It is above-mentioned using chalcogenide infrared glass as the preparation method of the anti-reflection DLC film of substrate, successively in chalcogenide infrared glass substrate
Adhesive layer and DLC film layer are made on layer, the preparation of adhesive layer is plated under vacuum conditions using the coating machine containing ion source
Film, starting vacuum degree are 1 × 10-3Pa, temperature are 100 DEG C；The acceleration voltage of ion source is 200V, plate voltage 400V, beam
Stream is 40A.The evaporation rate of Ge is that the evaporation rate of 0.2nm/s, ZnSe are 0.4nm/s.
DLC film layer is prepared in FJL600 type high vacuum hard carbon films filming equipment, and the sulphur system for having plated adhesive layer is red
After outer glass substrate layers ethanol ether (V ethyl alcohol: V ether 2:8) mixed liquor wiped clean, it is placed in FJL600 type high vacuum hard carbon
FJL600 type high vacuum hard carbon films filming equipment is evacuated to less than 1.5 × 10 by the bottom crown of film filming equipment-2Pa is passed through
Ar gas, keeps gas pressure 3.8Pa, power 200W, and the chalcogenide infrared glass basal layer 5min of adhesive layer has been plated in cleaning；So
After be passed through methane, under conditions of methane flow is 45sccm, operating pressure 14Pa, power are 700W deposit DLC (diamond-like
Stone hard carbon films) 30min, power supply is then shut off, to get using chalcogenide infrared glass as the anti-reflection DLC film of substrate after cooling 30min clock
Layer, namely obtain the anti-reflection DLC film using chalcogenide infrared glass as substrate.
As shown in Figure 1, use the SPECTRUM100 spectrophotometer of PE company, the U.S. to be able to chalcogenide infrared glass for
The single side reflectivity of the anti-reflection DLC film of substrate is tested, and the obtained curve of spectrum has reached design requirement (Ravg <
1.2%).
Embodiment 2
It is a kind of using chalcogenide infrared glass as the anti-reflection DLC film of substrate, including be connected in order chalcogenide infrared glass basal layer,
First ZnSe layer, the first Ge layers, the second ZnSe layer, the 2nd Ge layers, third ZnSe layer, the 3rd Ge layers, the 4th ZnSe layer, the 4th Ge
Layer and DLC film layer.From the first ZnSe layer to DLC film layer, the physical thickness of each layer be followed successively by 400nm, 242nm, 246nm,
177nm, 180nm, 400nm, 150nm, 365nm, 1285nm, chalcogenide infrared glass basal layer with a thickness of 5mm.Anti-reflection DLC film
Anti-reflection wave band be 8-12 microns.
The preparation method is the same as that of Example 1.
Embodiment 3
Above-mentioned anti-reflection plus DLC film layer is to be plated in the convex surface of chalcogenide glass lens, primarily serves the work of scratch resistance desertification dirt
With, and anti-reflection film is also plated in the another side of chalcogenide glass lens, to improve the whole transmitance of lens.It plates and increases on chalcogenide glass
On the one hand permeable membrane will play the role of antireflective, while being also required to solve the problems, such as the firmness of film layer, resulting anti-reflection in embodiment 1
The another side of DLC film increases antireflection layer, wherein G represents glass, and H represents ZnSe, L generation according to the sequence of G/H/L/H/L/M/A
Table YF3, M represent ZnS, and A represents air, the physical thickness of each film layer H/L/H/L/M (from chalcogenide infrared glass layer to air layer)
It respectively is: 865nm, 105nm, 296nm, 1046nm, 200nm, wherein the evaporation rate of ZnSe is 0.4nm/s, YF3's
Evaporation rate is 0.6 ± 0.01nm/s.
It can achieve in the average reflectance that the single side of 8-12 micron waveband reflects less than 1%, it is another to plate anti-reflection coating on one side
The mean transmissivity after anti-reflection plus DLC film is plated on one side is more than or equal to 92%.Spectral detection curve is as shown in Figure 3.
Film obtained by above-mentioned each example (embodiment 1-3) is performed the following performance tests, test reference standard is GJB2485-95
Optical film layer general specification, concrete outcome are as follows:
(1) under Packing Condition, plated film print the high and low temperature test: is put into high/low temperature experimental box (this high/low temperature experimental box
Heating and cooling rate be respectively less than 2 DEG C/min), 2h is kept in the low temperature of (one 62 ± 2) DEG C respectively, in (70 ± 2) DEG C
Keep 2h in high temperature, film layer without peeling, blistering, crackle, demoulding phenomena such as.
(2) wear-resistant strength is tested: being wrapped up in 2 layers of drying defatted gauze outside rubber friction head, is kept under 9.8N pressure along same
One track rubs to film layer, and round-trip 40 times, film layer is without scratch equivalent damage.
(3) adhesive force is tested: being 2cm with width, the adhesive tape of peel strength I > 2.94N/cm is cemented in film surface, by glue
After the rapid pull-up of vertical direction 10 times with paper from the edge of part towards surface, film layer nothing falls off, is not damaged.
(4) soak test: sample is completely immersed in distilled water or deionized water, and film layer does not occur new after 96 hours
The defects of peeling, removing, crackle, blistering.
Claims (5)
1. a kind of using chalcogenide infrared glass as the anti-reflection DLC film of substrate, it is characterised in that: double-sided coating, wherein back side coating film packet
Include the ZnS layer successively to connect, the first YF3 layers, the first ZnSe ' layer, the 2nd YF3 layers, the 2nd ZnSe ' layer and chalcogenide infrared glass base
Bottom, wherein ZnS layers with a thickness of 200 ± 5nm, the first YF3 layers with a thickness of 1046 ± 5nm, the thickness of the first ZnSe ' layer
For 296 ± 5nm, the 2nd YF3 layers with a thickness of 105 ± 5nm, the 2nd ZnSe ' layer with a thickness of 865 ± 5nm；Front plated film includes
It the DLC film layer that is sequentially arranged on chalcogenide infrared glass basal layer and is located between chalcogenide infrared glass basal layer and DLC film layer
Adhesive layer, adhesive layer includes the ZnSe layer alternateed and Ge layers, and ZnSe layer haves three layers；Each layer is successively are as follows: the sulphur being connected in order
Series infrared glass basal layer, the first ZnSe layer, the first Ge layers, the second ZnSe layer, the 2nd Ge layers, third ZnSe layer, the 3rd Ge layers
With DLC film layer；The thickness of first ZnSe layer, the second ZnSe layer and third ZnSe layer successively successively decreases；From the first ZnSe layer to DLC film
Layer, the physical thickness of each layer are followed successively by 400 ± 5nm, 242 ± 5nm, 246 ± 5nm, 177 ± 5nm, 180 ± 5nm, 400 ± 5nm
With 1285 ± 5nm；Chalcogenide infrared glass basal layer with a thickness of 2-10mm；
Using chalcogenide infrared glass as the preparation method of the anti-reflection DLC film of substrate: successively being made on chalcogenide infrared glass basal layer
The preparation of adhesive layer and DLC film layer, adhesive layer carries out plated film using the coating machine containing ion source under vacuum conditions, and starting is true
Reciprocal of duty cycle is (1 ± 0.1) × 10-3Pa；The acceleration voltage of ion source is 200 ± 10V, and plate voltage is 400 ± 10V, line 40
±5mA。
2. as described in claim 1 using chalcogenide infrared glass as the anti-reflection DLC film of substrate, it is characterised in that: with sulphur, system is infrared
Glass is that the anti-reflection wave band of the anti-reflection DLC film of substrate is 8-12 microns.
3. as claimed in claim 1 or 2 using chalcogenide infrared glass as the anti-reflection DLC film of substrate, it is characterised in that: when preparation
Temperature is 100 ± 5 DEG C.
4. as claimed in claim 1 or 2 using chalcogenide infrared glass as the anti-reflection DLC film of substrate, it is characterised in that: the evaporation of Ge
Rate is 0.2 ± 0.01nm/s, the evaporation rate of ZnSe is 0.4 ± 0.01nm/s, YF3Evaporation rate be 0.6 ± 0.01nm/
s。
5. as claimed in claim 1 or 2 using chalcogenide infrared glass as the anti-reflection DLC film of substrate, it is characterised in that: DLC film layer
It is prepared in FJL600 type high vacuum hard carbon films filming equipment, the chalcogenide infrared glass basal layer second of adhesive layer will have been plated
After alcohol ether mixed liquor wiped clean, it is placed in the bottom crown of FJL600 type high vacuum hard carbon films filming equipment, FJL600 type is high
Vacuum hard carbon films filming equipment is evacuated to less than 1.5 × 10-2Pa is passed through Ar gas, keeps gas pressure 3.3Pa~4Pa, power
5 ± 1min of chalcogenide infrared glass basal layer of adhesive layer has been plated in 200W, cleaning；Methane is then passed to, is in methane flow
DLC30 ± 5min is deposited under conditions of 40sccm~50sccm, operating pressure are 7Pa~20Pa, power is 700 ± 10W, then
Power supply is closed, to get using chalcogenide infrared glass as the anti-reflection DLC film layer of substrate after cooling 30 ± 5min clock.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710570521.4A CN107227460B (en) | 2017-07-13 | 2017-07-13 | It is a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710570521.4A CN107227460B (en) | 2017-07-13 | 2017-07-13 | It is a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107227460A CN107227460A (en) | 2017-10-03 |
| CN107227460B true CN107227460B (en) | 2019-09-06 |
Family
ID=59956433
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710570521.4A Active CN107227460B (en) | 2017-07-13 | 2017-07-13 | It is a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107227460B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108802864A (en) * | 2018-06-07 | 2018-11-13 | 云南北方驰宏光电有限公司 | A kind of silicon base high-efficiency anti-reflection film being applicable in 3.7-4.8 mu m wavebands |
| CN109576706A (en) * | 2018-12-21 | 2019-04-05 | 云南北方驰宏光电有限公司 | A kind of silicon base diamond-like protective film and preparation method thereof |
| CN111485237A (en) * | 2020-04-09 | 2020-08-04 | 有研国晶辉新材料有限公司 | Substrate infrared anti-reflection protective film and preparation method thereof |
| CN113584481A (en) * | 2021-08-11 | 2021-11-02 | 南京波长光电科技股份有限公司 | Carbon dioxide laser superhard film and preparation method thereof |
| CN114019591B (en) * | 2021-09-23 | 2023-08-01 | 有研国晶辉新材料有限公司 | Optical element comprising anti-reflection protective film and preparation method thereof |
| CN115161596B (en) * | 2022-08-26 | 2022-11-29 | 有研国晶辉新材料有限公司 | Glass substrate film structure and preparation method thereof |
| CN116540332B (en) * | 2023-04-26 | 2024-05-31 | 云南驰宏国际锗业有限公司 | AR/DLC composite coated infrared chalcogenide glass lens and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104090312A (en) * | 2014-07-30 | 2014-10-08 | 中国船舶重工集团公司第七一七研究所 | Infrared metal reflecting film with high adhesive force and manufacturing method thereof |
| CN104459835A (en) * | 2014-12-24 | 2015-03-25 | 南京波长光电科技股份有限公司 | Infrared glass GASIR1 antireflection 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 |
| CN106517818A (en) * | 2016-10-27 | 2017-03-22 | 宁波舜宇红外技术有限公司 | Chalcogenide lens and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN206916217U (en) * | 2017-07-13 | 2018-01-23 | 南京波长光电科技股份有限公司 | A kind of anti-reflection DLC film using chalcogenide infrared glass as substrate |
-
2017
- 2017-07-13 CN CN201710570521.4A patent/CN107227460B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104090312A (en) * | 2014-07-30 | 2014-10-08 | 中国船舶重工集团公司第七一七研究所 | Infrared metal reflecting film with high adhesive force and manufacturing method thereof |
| CN104459835A (en) * | 2014-12-24 | 2015-03-25 | 南京波长光电科技股份有限公司 | Infrared glass GASIR1 antireflection 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 |
| CN106517818A (en) * | 2016-10-27 | 2017-03-22 | 宁波舜宇红外技术有限公司 | Chalcogenide lens and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107227460A (en) | 2017-10-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107227460B (en) | It is a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof | |
| CN206916217U (en) | A kind of anti-reflection DLC film using chalcogenide infrared glass as substrate | |
| Alvisi et al. | HfO2 films with high laser damage threshold | |
| Logothetidis | Hydrogen‐free amorphous carbon films approaching diamond prepared by magnetron sputtering | |
| CN106783173B (en) | A kind of all-transparent BZT film varactor and preparation method thereof | |
| Zhang | Stainless-steel–AlN cermet selective surfaces deposited by direct current magnetron sputtering technology | |
| CN1304857C (en) | ZnS infrared window transparent increasing protective film and its preparing method | |
| CN101464528A (en) | DLC infrared anti-refiection protective film and method for producing the same | |
| CN109292732B (en) | Broken line type nanometer gap with plasma focusing performance and preparation method thereof | |
| CN111960693B (en) | Preparation method of silicon oxide/titanium oxide-based indoor decoration multi-reflection-color coated glass | |
| CN105568227B (en) | A kind of homogeneity bilayer hafnium oxide antireflective film and preparation method thereof | |
| CN107746187A (en) | A kind of infrared chalcogenide glass lenses for plating DLC film and preparation method thereof | |
| CN104480436A (en) | Method for preparing high-hardness germanium carbide film with variable refractive index | |
| CN107179569A (en) | A kind of near-infrared is to middle ultra-wideband anti-reflection film and preparation method thereof | |
| CN112501557B (en) | Sapphire substrate 1-5 mu m ultra-wideband antireflection film and preparation method thereof | |
| CN109837517A (en) | A kind of external reflectance silverskin preparation method based on magnetron sputtering | |
| CN101231352A (en) | HfON/BP antireflecting protective film for infrared optical window and manufacture method thereof | |
| Ming-Dong et al. | Determination of thickness and optical constants of ZnO thin films prepared by filtered cathode vacuum arc deposition | |
| CN206920633U (en) | A kind of near-infrared is to middle ultra-wideband anti-reflection film | |
| CN205720741U (en) | A kind of anti-reflection film being plated on infrared glass | |
| CN105911616A (en) | Antireflection coating plated on infrared glass and preparation method thereof | |
| Rademacher et al. | Sputtering of dielectric single layers by metallic mode reactive sputtering and conventional reactive sputtering from cylindrical cathodes in a sputter-up configuration | |
| CN108842186A (en) | Preparation method for the antireflective zinc telluridse plane of crystal micro-structure of terahertz wave band | |
| CN112553585B (en) | Polymethyl methacrylate substrate medium antireflection film and preparation method thereof | |
| CN102368097B (en) | Dim light and laser transmission and medium-infrared reflection film and prism, preparation method of prism |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 211123 No.18, boguang Road, Hushu industrial concentration area, Jiangning District, Nanjing City, Jiangsu Province Patentee after: NANJING WAVELENGTH OPTOELECTRONICS TECHNOLOGY Co.,Ltd. Patentee after: WAVELAB SCIENTIFIC NANJING Co.,Ltd. Address before: 211123 No.18, boguang Road, Hushu industrial concentration area, Jiangning District, Nanjing City, Jiangsu Province Patentee before: NANJING WAVELENGTH OPTOELECTRONICS TECHNOLOGY Co.,Ltd. Patentee before: NANJING GUANGYAN SOFTWARE SYSTEM Co.,Ltd. |