CN109576706A - A kind of silicon base diamond-like protective film and preparation method thereof - Google Patents
A kind of silicon base diamond-like protective film and preparation method thereof Download PDFInfo
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- CN109576706A CN109576706A CN201811574807.0A CN201811574807A CN109576706A CN 109576706 A CN109576706 A CN 109576706A CN 201811574807 A CN201811574807 A CN 201811574807A CN 109576706 A CN109576706 A CN 109576706A
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- protective film
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- 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
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- 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
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- 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
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/343—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one DLC or an amorphous carbon based layer, the layer being doped or not
Abstract
The invention discloses a kind of silicon base diamond-like protective films, including silicon base, diamond-like protective film and germanium articulamentum；The germanium articulamentum is set between silicon base and diamond-like protective film.One of present invention silicon base diamond-like protective film; germanium articulamentum is provided between silicon base and diamond-like protective film; enhance the adhesive force of diamond-like protective film on a silicon substrate; in particular improve the adhesive force of silicon substrate feather edge diamond-like protective film; it avoids edge and stripping phenomenon occurs; it realizes the unified stable covering on a silicon substrate of diamond-like protective film, reduces rejection rate, save production cost.
Description
Technical field
The present invention relates to infrared coating technique field more particularly to a kind of silicon base diamond-like protective film and its preparation sides
Method.
Background technique
In military and space technology, silicon base optical element majority all works in severe natural environment, element warp
Be subjected to wind erosion, husky erosion, drench with rain and the test of chemical attack, many optical elements all because its mechanical strength and corrosivity difference and
Vulnerable to damage, and then reduce its proper property.Therefore it needs to mention by being coated with the DLC film with defencive function
The environmental suitability of high silicon base element.Existing technology is that single layer DLC film is coated in Si substrate, film layer knot
Structure and process for plating are relatively easy, but since in the presence of matching, binding ability is not good enough to ask silicon base with diamond-like protective film itself
, easily there is stripping phenomenon in topic.The especially biggish silicon substrate feather edge stripping phenomenon of bore frequently occurs, and seriously reduces product conjunction
Lattice rate.
Summary of the invention
It is existing between diamond-like protective film and silicon base to match the not good enough skill of binding ability to solve in the prior art
Art problem, technical scheme is as follows:
One of present invention silicon base diamond-like protective film, including silicon base, diamond-like protective film and germanium connection
Layer；The germanium articulamentum is set between silicon base and diamond-like protective film.
In a preferred embodiment, mean transmissivity >=66% of the diamond-like protective film, average reflection
Rate≤3%.
In a preferred embodiment, material used by the silicon base is infrared optical material silicon.
The invention also discloses the preparation methods of above-mentioned silicon base diamond-like protective film, include the following steps:
Step S1: silicon base is fixed on workpiece plate using double-sided elevated temperature adhesive tape；
Step S2: germanium articulamentum is coated with silicon substrate surface is unified using electron beam evaporation deposition equipment；
Step S3: using plasma chemical vapor depsotition equipment is coated with class in the silicon substrate surface for being coated with germanium articulamentum
Diamond protective film.
In a preferred embodiment, the coating temperature in step S2 be 170 ± 5 DEG C, be coated with during using from
Component carries out ion auxiliary.
In a preferred embodiment, the carbon-source gas deposited in step S3 is butane, and diluent gas is argon gas.
In a preferred embodiment, butane concentration is 60~150%.
In a preferred embodiment, the deposition power of step S3 plasma chemical vapor depsotition equipment is
600~1500W, sedimentation time are 7~13min.
One of present invention silicon base diamond-like protective film and preparation method thereof is compared with prior art, beneficial
Effect are as follows:
One of present invention silicon base diamond-like protective film, is provided between silicon base and diamond-like protective film
Germanium articulamentum enhances the adhesive force of diamond-like protective film on a silicon substrate, in particular improves silicon substrate feather edge diamond-like
The adhesive force of stone protective film avoids edge and stripping phenomenon occurs, realizes that diamond-like protective film is unified steady on a silicon substrate
Fixed covering, reduces rejection rate, saves production cost.
Detailed description of the invention
Fig. 1 is a kind of film layer structure schematic diagram of silicon base diamond-like protective film in the present invention；
Fig. 2 is the light transmittance spectral curve of the preparation of embodiment 1 gained diamond-like protective film in the present invention；
Fig. 3 is the reflectance spectrum curve graph of the preparation of embodiment 1 gained diamond-like protective film in the present invention.
Specific embodiment
Below in conjunction with attached drawing of the invention, technical solution of the present invention is clearly and completely described.Based on this hair
Embodiment in bright, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
As shown in Figure 1, a kind of silicon base diamond-like protective film of the invention, including silicon base 1, diamond-like protective film
2 and germanium articulamentum 3；The germanium articulamentum 3 is set between silicon base 1 and diamond-like protective film 2.Wherein diamond-like is protected
Mean transmissivity >=66%, average reflectance≤3% of film.Material used by silicon base is infrared optical material silicon.
The invention also discloses the preparation methods of above-mentioned silicon base diamond-like protective film, include the following steps:
Step S1: silicon base is fixed on workpiece plate using double-sided elevated temperature adhesive tape；
Step S2: germanium articulamentum, coating temperature are coated with silicon substrate surface is unified using electron beam evaporation deposition equipment
It is 170 ± 5 DEG C, ion auxiliary is carried out using ion source during being coated with；
Step S3: using plasma chemical vapor depsotition equipment is coated with class in the silicon substrate surface for being coated with germanium articulamentum
The carbon-source gas of diamond protective film, deposition is butane, and diluent gas is argon gas, butane (C4H10/ Ar) concentration be 60~150%
(percent by volume).The deposition power of apparatus for plasma chemical vapor deposition be 600~1500W, sedimentation time be 7~
13min。
Embodiment 1
It selects the silicon window of Φ 25.4mm × 3mm as substrate material layer, is fixed silicon base using double-sided elevated temperature adhesive tape
On workpiece plate, germanium articulamentum is coated with silicon substrate surface is unified using electron beam evaporation deposition equipment later, is coated with temperature
Control carries out ion auxiliary using ion source during being coated at 170 DEG C.Using plasma chemical vapor deposition is set later
Standby, the carbon-source gas in the silicon substrate surface plating diamond protective film for being coated with germanium articulamentum, deposition is butane, carrier gas
Body is argon gas, butane concentration (C4H10/ Ar) it is 60% (percent by volume), deposition power 800W, sedimentation time 9min are obtained
To the unified diamond-like protective film of the silicon base for being applicable in 3~5 mu m wavebands of the invention, wherein electron beam evaporation deposition equipment is
II type coating machine of TianXing TXX1100-, apparatus for plasma chemical vapor deposition are TianXing TXHLWT700 type coating machine.
The test that transmitance and reflectivity are carried out to the unified diamond-like protective film of above-mentioned silicon base, it is complete to measure silicon base
Bore diamond-like protective film is 66.3% in the mean transmissivity of 3~5 mu m wavebands, average reflectance 2.6%, above-mentioned silicon substrate
The unified diamond-like protective film in bottom carries out light transmittance spectral curve obtained by the test of transmitance and reflectivity and sees Fig. 2, reflects
Rate spectral curve is shown in Fig. 3；
By the part according to national military standard GJB2485-1995 standard, to the unified diamond-like protective film of the silicon base into
Row surface quality, adhesive force, high/low temperature, damp and hot measurement test, after test, no marking, without stripping phenomenon.
Embodiment 2
Select 152mm × 114mm × 10mm silicon window as silicon substrate material, using double-sided elevated temperature adhesive tape by silicon base
It is fixed on workpiece plate, germanium articulamentum is coated with silicon substrate surface is unified using electron beam evaporation deposition equipment later, is coated with
Temperature is controlled at 167 DEG C, carries out ion auxiliary using ion source during being coated with.Using plasma chemical vapor deposition later
Equipment, the carbon-source gas in the silicon substrate surface plating diamond protective film for being coated with germanium articulamentum, deposition are butane, dilution
Gas is argon gas, butane concentration (C4H10/ Ar) it is 80% (percent by volume), deposition power 800W, sedimentation time is
8min30s obtains the unified diamond-like protective film of the silicon base for being applicable in 3~5 mu m wavebands of the invention.
The test that transmitance and reflectivity are carried out to the unified diamond-like protective film of silicon base, it is unified to measure silicon base
Diamond-like protective film is 66.5% in the mean transmissivity of 3~5 mu m wavebands, average reflectance 2.5%；
By the part according to national military standard GJB2485-1995 standard, to the unified diamond-like protective film of the silicon base into
Row surface quality, adhesive force, high/low temperature, damp and hot measurement test, after test, no marking, without stripping phenomenon.
Embodiment 3
Select the silicon lens of Φ 214mm × 9.48mm as silicon substrate material layer, using double-sided elevated temperature adhesive tape by silicon base
It is fixed on workpiece plate, germanium articulamentum is coated with silicon substrate surface is unified using electron beam evaporation deposition equipment later, is coated with
Temperature is controlled at 167 DEG C, carries out ion auxiliary using ion source during being coated with.Using plasma chemical vapor deposition later
Equipment, the carbon-source gas in the silicon substrate layer surface plating diamond protective film for being coated with germanium articulamentum, deposition is butane, dilute
Outgassing body is argon gas, butane concentration (C4H10/ Ar) it is 63% (percent by volume), deposition power 900W, sedimentation time is
8min.Obtain the unified diamond-like protective film of the silicon base for being applicable in 3~5 mu m wavebands of the invention.
The test that transmitance and reflectivity are carried out to the unified diamond-like protective film of the silicon base, it is complete to measure silicon base
Bore diamond-like protective film is 66.2% in the mean transmissivity of 3~5 mu m wavebands, average reflectance 2.9%；
By the part according to national military standard GJB2485-1995 standard, to the unified diamond-like protective film of the silicon base into
Row surface quality, adhesive force, high/low temperature, damp and hot measurement test, after test, no marking, without stripping phenomenon.
Embodiment 4
It selects the silicon window of Φ 96mm × 7mm as silicon substrate material layer, is fixed silicon base using double-sided elevated temperature adhesive tape
On workpiece plate, germanium articulamentum is coated with silicon substrate layer surface is unified using electron beam evaporation deposition equipment later, is coated with temperature
Degree control carries out ion auxiliary using ion source during being coated at 170 DEG C.Using plasma chemical vapor deposition is set later
Standby, the carbon-source gas in the silicon substrate layer surface plating diamond protective film for being coated with germanium articulamentum, deposition is butane, dilution
Gas is argon gas, butane concentration (C4H10/ Ar) it is 66% (percent by volume), deposition power 800W, sedimentation time is
8min50s.Obtain the unified diamond-like protective film of the silicon base for being applicable in 3~5 mu m wavebands of the invention.
The test that transmitance and reflectivity are carried out to the unified diamond-like protective film of the silicon base, it is complete to measure silicon base
Bore diamond-like protective film is 66.4% in the mean transmissivity of 3~5 mu m wavebands, average reflectance 2.8%；
By the part according to national military standard GJB2485-1995 standard, to the unified diamond-like protective film of the silicon base into
Row surface quality, adhesive force, high/low temperature, damp and hot measurement test, after test, no marking, without stripping phenomenon.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is 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 (8)
1. a kind of silicon base diamond-like protective film, which is characterized in that connected including silicon base, diamond-like protective film and germanium
Layer；The germanium articulamentum is set between silicon base and diamond-like protective film.
2. a kind of silicon base diamond-like protective film according to claim 1, which is characterized in that the diamond-like protection
Mean transmissivity >=66%, average reflectance≤3% of film.
3. a kind of silicon base diamond-like protective film according to claim 2, which is characterized in that the silicon base is used
Material be infrared optical material silicon.
4. a kind of preparation method of silicon base diamond-like protective film as claimed in any one of claims 1 to 3, feature exist
In including the following steps:
Step S1: silicon base is fixed on workpiece plate using double-sided elevated temperature adhesive tape；
Step S2: germanium articulamentum is coated with silicon substrate surface is unified using electron beam evaporation deposition equipment；
Step S3: using plasma chemical vapor depsotition equipment is coated with diamond-like in the silicon substrate surface for being coated with germanium articulamentum
Stone protective film.
5. a kind of preparation method of silicon base diamond-like protective film according to claim 4, which is characterized in that step S2
In coating temperature be 170 ± 5 DEG C, be coated with during using ion source carry out ion auxiliary.
6. a kind of preparation method of silicon base diamond-like protective film according to claim 4 or 5, which is characterized in that step
The carbon-source gas deposited in rapid S3 is butane, and diluent gas is argon gas.
7. a kind of preparation method of silicon base diamond-like protective film according to claim 6, which is characterized in that butane is dense
Degree is 60~150%.
8. a kind of preparation method of silicon base diamond-like protective film according to claim 7, which is characterized in that step S3
The deposition power of plasma chemical vapor depsotition equipment is 600~1500W, and sedimentation time is 7~13min.
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| CN201811574807.0A CN109576706A (en) | 2018-12-21 | 2018-12-21 | A kind of silicon base diamond-like protective film and preparation method thereof |
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| CN201811574807.0A CN109576706A (en) | 2018-12-21 | 2018-12-21 | A kind of silicon base diamond-like protective film and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210140037A1 (en) * | 2019-09-24 | 2021-05-13 | Adam Khan | Protective diamond coating system and method |
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| CN105296926A (en) * | 2015-12-04 | 2016-02-03 | 中国航空工业集团公司洛阳电光设备研究所 | Hard anti-reflection composite film type optical window and preparation method thereof |
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Cited By (2)
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| US20210140037A1 (en) * | 2019-09-24 | 2021-05-13 | Adam Khan | Protective diamond coating system and method |
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