CN116657120A - Preparation method of deposited diamond-like film of polycarbonate lens - Google Patents
Preparation method of deposited diamond-like film of polycarbonate lens Download PDFInfo
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- CN116657120A CN116657120A CN202310653651.XA CN202310653651A CN116657120A CN 116657120 A CN116657120 A CN 116657120A CN 202310653651 A CN202310653651 A CN 202310653651A CN 116657120 A CN116657120 A CN 116657120A
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- 238000012512 characterization method Methods 0.000 claims abstract description 20
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- 238000012360 testing method Methods 0.000 claims abstract description 15
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims abstract description 12
- 239000011521 glass Substances 0.000 claims abstract description 11
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 238000005259 measurement Methods 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 44
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 30
- 239000010936 titanium Substances 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 23
- 229910052786 argon Inorganic materials 0.000 claims description 22
- 239000000758 substrate Substances 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 230000003287 optical effect Effects 0.000 claims description 12
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- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000004744 fabric Substances 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 238000001069 Raman spectroscopy Methods 0.000 claims description 7
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- ZFMITUMMTDLWHR-UHFFFAOYSA-N Minoxidil Chemical compound NC1=[N+]([O-])C(N)=CC(N2CCCCC2)=N1 ZFMITUMMTDLWHR-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
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- 238000005299 abrasion Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- JKNDTQVYGQBATP-UHFFFAOYSA-N argon;methane Chemical compound C.[Ar] JKNDTQVYGQBATP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- 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
- C23C16/44—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 method of coating
- C23C16/50—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 method of coating using electric discharges
- C23C16/505—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 method of coating using electric discharges using radio frequency discharges
-
- 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
- C23C14/20—Metallic material, boron or silicon on organic substrates
- C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
-
- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
- C23C16/0245—Pretreatment of the material to be coated by cleaning or etching by etching with a plasma
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
- C23C16/0281—Deposition of sub-layers, e.g. to promote the adhesion of the main coating of metallic sub-layers
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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
- 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
- C23C28/32—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
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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
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- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a preparation method of a deposited diamond-like film of a polycarbonate lens, which comprises the following steps: step 1: sample treatment, including sample cleaning and sample pretreatment; step 2: the sample deposition DLC film and test analysis comprises a glass lens DLC film experiment, a resin lens DLC experiment with curvature, a plane resin lens low-temperature DLC experiment, a resin lens Ti transition layer plating experiment and a plane resin lens DLC plating experiment containing a Ti transition layer; step 3: characterization measurement of DLC film; step 4: and adjusting and optimizing the process parameters according to the characterization and measurement structure of the film, and finally determining the optimal process parameters through different process parameter combinations. According to the invention, by using a plasma enhanced chemical vapor deposition system, the influence of process conditions such as different powers, different process gas formulas, different deposition temperatures, different deposition times and the like on the film performance is researched, so that the process conditions are optimized; and meanwhile, the adhesive force of the film is increased by adopting different transition layer materials.
Description
Technical Field
The invention relates to the technical field of lens film preparation, in particular to a preparation method of a deposited diamond-like film of a polycarbonate lens.
Background
Polycarbonate (PC resin) is a novel optical plastic with excellent comprehensive performance, and a lens made of PC material is called a space lens, and has the advantages of light weight, easy molding, good optical performance and the like, so that the Polycarbonate resin gradually replaces glass lenses to become the first-choice material of various optical lenses in recent years, and has very good development prospect. However, the PC resin lens has larger defects, which are mainly characterized by low surface hardness, easy abrasion, poor scratch resistance and poor temperature resistance (below 100 ℃), and the defects influence the service life of the lens and restrict the application range of the lens. In order to overcome the defects of PC lenses, hard films are mainly plated on the surfaces of the lenses through various coating processes at present so as to improve the wear resistance of the surfaces of the lenses, solve the damage caused by scraping and prolong the service life of the lenses.
The diamond-like carbon (DiamondlikeCarbon, DLC) is a novel film, has graphite structure sp2 bonds and diamond structure sp3 bonds, so DLC has a plurality of properties similar to diamond, such as light, electricity, sound, heat, machinery and the like, such as high hardness, wide optical transmission range (refractive index is generally 1.5-2.6), good electrical property (resistivity can reach 1000 ohm cm), good biocompatibility and the like. Meanwhile, the film has the characteristics of properties different from those of a diamond film, such as low film forming temperature (which can be reduced to 25 ℃ at room temperature), high surface smoothness, good friction and wear properties (friction coefficient is reduced to below 0.2) and the like. Therefore DLC has great application value in optics, medicine, acoustics, microelectronics, mechanical engineering, aerospace, and nuclear technology, and its industrial application has been in front of diamond films. Especially, DLC film is deposited on the surface of PC lens as antiwear hardening layer, so that the surface hardness of the lens can be obviously raised, the wear resistance is increased, the service life of the lens is prolonged, the visible light transparency of the lens is raised, ultraviolet rays are effectively absorbed and prevented, and the lens is beneficial to vision protection.
The major difficulty in depositing DLC films on PC lenses today is the problem of film-based bonding. In the DLC film deposition process, the bombardment of ions on the surface of the matrix causes larger compressive stress on the surface of the film, and simultaneously, the stress caused by the mismatching of film-matrix properties reduces the bonding strength of the film and the PC resin matrix and also limits the thickness of the film.
Disclosure of Invention
1. Technical problem to be solved
The invention aims to solve the problem that in the prior art, in the DLC film deposition process, the impact of ions on the surface of a substrate causes larger compressive stress on the surface of the film, and meanwhile, the stress is caused by mismatching of film-substrate properties.
2. Technical proposal
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing a deposited diamond-like film of a polycarbonate lens, comprising the following steps:
step 1: sample treatment, including sample cleaning and sample pretreatment, wherein the sample cleaning requires cleaning the substrate before the substrate is placed in the PECVD vacuum chamber;
step 2: the sample deposition DLC film and test analysis comprises a glass lens DLC film experiment, a resin lens DLC experiment with curvature, a plane resin lens low-temperature DLC experiment, a resin lens Ti transition layer plating experiment and a plane resin lens DLC plating experiment containing a Ti transition layer;
step 3: the characterization measurement of the DLC film comprises morphology structure characterization and performance characterization, wherein the morphology structure characterization mainly comprises: scanning electron microscope SEM, raman spectrometer Raman, X-ray diffractometer XRD, X-ray photoelectron spectrometer XPS, atomic force microscope AFM; the performance characterization included wear resistance: evaluating the wear resistance of the film by adopting a dust-free cloth in a friction manner; degree of bonding: testing the bonding degree of the film by adopting 3M glue in a sticking and tearing mode; transparency: quantitatively analyzing the transparency by adopting a naked eye observation method;
step 4: and adjusting and optimizing the process parameters according to the characterization and measurement structure of the film, and finally determining the optimal process parameters through different process parameter combinations.
Preferably, the sample cleaning in step 1 mainly comprises the following steps:
s1: placing a sample wafer to be washed into a clean beaker, adding a proper amount of detergent and deionized water, placing the sample wafer into an ultrasonic cleaner, and performing ultrasonic treatment for 10 minutes to remove oil stains and large-particle impurities on the surface;
s2: placing the sample wafer into a proper amount of acetone solution, sealing the beaker to prevent volatilization, and then ultrasonically cleaning for 10 minutes to remove organic impurities on the surface;
s3: placing the sample into a proper amount of absolute ethyl alcohol, sealing to prevent volatilization, then ultrasonically cleaning for 10 minutes, and removing organic solvents such as acetone and the like on the surface of the sample;
s4: placing the sample into a proper amount of deionized water, ultrasonically cleaning for 10 minutes, and removing absolute ethyl alcohol on the surface of the sample;
s5: purging the surface of the sample by using nitrogen, removing deionized water on the surface, and keeping the sample dry and clean;
s6: after drying in an oven at 50 ℃ for about 20 hours, the mixture was put into a vacuum drying oven for standby.
Preferably, the sample pretreatment in step 1 includes bombarding the substrate with argon plasma for 10 minutes to remove impurities on the surface before introducing carbon source gas, and generating groups containing unsaturated bonds on the surface of the substrate to improve the surface activity of the substrate so as to ensure the adhesion of the film firmly combined between the substrate and the film layer.
Preferably, the main process parameters of the PECVD vacuum chamber in the step 1 are set as background vacuum: 8.0X10-4 Pa, radio frequency power: 100W, ar flow: 30sccm, glow-starting pressure: 3Pa.
Preferably, the main process parameters adopted in the DLC film experiment of the glass lens in the step 3 are as follows: sample: 4 quartz glass sheets; cleaning: according to a standard cleaning flow; a mixed gas of methane (CH 4, purity 99.995%) and argon (Ar, purity 99.999%); distance between upper and lower polar plates: 70mm; radio frequency power: 200W; chamber background vacuum: 3.6X10-3 Pa; glow starting pressure: 5Pa, process pressure: the molecular pump gate valve is fully opened and kept at 3Pa.
Preferably, the main process parameters adopted in the DLC test of the resin lens with curvature in the step 3 are as follows: sample: 4 resin lenses; cleaning: according to a standard cleaning flow; a mixed gas of methane (CH 4, purity 5N) and argon (Ar, purity 5N); distance between upper and lower polar plates: 70mm; the lower polar plate sample table is not heated; chamber background vacuum: 8.0 x 10-4; glow starting pressure: 5Pa, process pressure: the molecular pump gate valve is fully opened and kept at 3Pa.
Preferably, the main process parameters of the low-temperature DLC test of the planar resin lens in the step 3 are as follows: sample: the planar resin lenses 16 are divided into 4 groups of 4 sheets each; cleaning: according to a standard cleaning flow; a mixed gas of methane (CH 4, purity 5N) and argon (Ar, purity 5N); distance between upper and lower polar plates: 70mm; the lower polar plate sample table is not heated; radio frequency power: 100w; CH4: ar=60 sccm:20sccm; chamber background vacuum: 8.0 x 10-4; glow starting pressure: 5Pa, process pressure: the molecular pump gate valve is fully opened and kept at 3Pa.
Preferably, the main experimental parameters of the Ti-plating transition layer experiment of the resin lens in the step 3 are as follows: sample: 6 planar resin sheets; the device comprises: magnetron sputtering, namely a Beijing-created micro-nano MSP-300BI magnetron sputtering instrument; and (3) target material: titanium target, beijing minoxidil, purity 4.5N; process gas: pure argon 40sccm; chamber background vacuum: 2 x 10-3; the sample table is not heated and is at the normal temperature of 25 ℃; dc target power: 80W, rate 0.1176nm/s; glow starting pressure: 5Pa, process pressure: regulating a molecular pump gate valve, and keeping 0.68Pa; sputtering time: 2s, 5s, 10s, 15s, 20s, 25s.
Preferably, the DLC plating experiment main technological parameters of the planar resin lens containing the Ti transition layer are as follows: sample: an optical resin lens with 6 titanium bonding layers (2.5 nm); a mixed gas of methane (CH 4, purity 5N) and argon (Ar, purity 5N); the lower polar plate is not heated and is at the normal temperature of 25 ℃; distance between upper and lower polar plates: 70mm; radio frequency power: 100w; chamber background vacuum: 4 x 10-4; glow starting pressure: 3.4Pa, process pressure: and regulating a molecular pump gate valve to keep 3Pa.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
in the invention, the influence of process conditions such as different powers, different process gas formulas, different deposition temperatures, different deposition times and the like on the film performance is researched by using a plasma enhanced chemical vapor deposition system, so that the process conditions are optimized; and meanwhile, the adhesive force of the film is increased by adopting different transition layer materials.
Drawings
FIG. 1 is a flow chart of a film process technology of a method for preparing a diamond-like film deposited on a polycarbonate lens according to the present invention;
FIG. 2 is a sample cleaning flow chart of a method for preparing a diamond-like film deposited on a polycarbonate lens according to the present invention;
FIG. 3 is a glow starting diagram of a PECVD DLC film coated according to the present invention;
FIG. 4 is a Raman spectrum of a glass sample wafer according to the present invention;
FIG. 5 is an AFM test chart of a 4# plate according to the present invention;
FIG. 6 is a schematic view of a DLC film deposited curvature resin lens (left to right 1# to 4# according to the present invention);
FIG. 7 shows the surface morphology of a No. 2 resin lens before and after wiping;
FIG. 8 is a chart showing the adhesive tape bonding force test of a No. 2 resin lens according to the present invention;
FIG. 9 is a schematic diagram of a DLC film deposited planar resin lens according to the present invention (left to right, groups 1 to 4);
FIG. 10 is a Raman spectrum of a group 4 planar resin lens according to the present invention;
FIG. 11 is a graph showing the results of wiping a sample wafer in accordance with the present invention;
FIG. 12 shows the experimental results of plating Ti film on a planar resin lens according to the present invention;
FIG. 13 shows the results of DLC film plating on a planar resin fine product containing Ti bonding layer according to the present invention;
FIG. 14 shows microscopic results after wiping of lenses 1-3 according to the present invention;
fig. 15 shows microscopic results after wiping of lenses # 4 and # 5 in accordance with the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Example 1:
referring to fig. 1-2, a method for preparing a deposited diamond-like film for a polycarbonate lens, comprising the steps of:
step 1: sample treatment, including sample cleaning and sample pretreatment, wherein the sample cleaning requires cleaning the substrate before the substrate is placed in the PECVD vacuum chamber;
the sample cleaning mainly comprises the following steps:
s1: placing a sample wafer to be washed into a clean beaker, adding a proper amount of detergent and deionized water, placing the sample wafer into an ultrasonic cleaner, and performing ultrasonic treatment for 10 minutes to remove oil stains and large-particle impurities on the surface;
s2: placing the sample wafer into a proper amount of acetone solution, sealing the beaker to prevent volatilization, and then ultrasonically cleaning for 10 minutes to remove organic impurities on the surface;
s3: placing the sample into a proper amount of absolute ethyl alcohol, sealing to prevent volatilization, then ultrasonically cleaning for 10 minutes, and removing organic solvents such as acetone and the like on the surface of the sample;
s4: placing the sample into a proper amount of deionized water, ultrasonically cleaning for 10 minutes, and removing absolute ethyl alcohol on the surface of the sample;
s5: purging the surface of the sample by using nitrogen, removing deionized water on the surface, and keeping the sample dry and clean;
s6: after drying in an oven at 50 ℃ for about 20 hours, the mixture was put into a vacuum drying oven for standby.
The sample pretreatment comprises that before introducing carbon source gas, argon plasma is used for bombarding a matrix for 10 minutes to remove impurities on the surface, and groups containing unsaturated bonds are generated on the surface of a substrate to improve the surface activity of the matrix so as to ensure the firm adhesion of the film between the matrix and the film layer; the main process parameters of the PECVD vacuum chamber are set as background vacuum: 8.0X10-4 Pa, radio frequency power: 100W, ar flow: 30sccm, glow-starting pressure: 3Pa;
step 2: the sample deposition DLC film and test analysis comprises a glass lens DLC film experiment, a resin lens DLC experiment with curvature, a plane resin lens low-temperature DLC experiment, a resin lens Ti transition layer plating experiment and a plane resin lens DLC plating experiment containing a Ti transition layer;
step 3: the characterization measurement of the DLC film comprises morphology structure characterization and performance characterization, wherein the morphology structure characterization mainly comprises: scanning electron microscope SEM, raman spectrometer Raman, X-ray diffractometer XRD, X-ray photoelectron spectrometer XPS, atomic force microscope AFM; the performance characterization included wear resistance: evaluating the wear resistance of the film by adopting a dust-free cloth in a friction manner; degree of bonding: testing the bonding degree of the film by adopting 3M glue in a sticking and tearing mode; transparency: quantitatively analyzing the transparency by adopting a naked eye observation method;
step 4: and adjusting and optimizing the process parameters according to the characterization and measurement structure of the film, and finally determining the optimal process parameters through different process parameter combinations.
In the invention, the influence of process conditions such as different powers, different process gas formulas, different deposition temperatures, different deposition times and the like on the film performance is researched by using a plasma enhanced chemical vapor deposition system, so that the process conditions are optimized; and meanwhile, the adhesive force of the film is increased by adopting different transition layer materials.
Example 2:
the DLC film experiment of the glass lens adopts main technological parameters:
(1) Sample: quartz glass 4 pieces.
(2) Cleaning: the cleaning process is carried out according to the standard.
(3) Methane (CH 4, 99.995% purity) and argon (Ar, 99.999% purity).
(4) Distance between upper and lower polar plates: 70mm.
(5) Radio frequency power: 200W;
(6) Chamber background vacuum: 3.6X10-3 Pa.
(7) Glow starting pressure: 5Pa, process pressure: the molecular pump gate valve is fully opened and kept at 3Pa. The glow is initiated as shown in FIG. 3.
The components of the diamond-like film are controlled by changing the heating temperature of the lower polar plate sample table, the flow rates of methane and argon and the deposition time parameters, so that the performance of the film is changed. On the basis of a large number of experiments, the optimal technological parameters are found out, and the design of the experimental parameters is shown in table 1.
TABLE 1 Experimental parameters for DLC film on glass sheets
Experimental results and analysis:
(1) The 4 samples were all successfully deposited with DLC film and the deposited lenses were as shown. The film has a theaflavine color, the deposition color of the No. 4 sample wafer is deep, and the light transmittance is good; the 1# to 4# sheets were tested using a microscopic confocal raman spectrometer, and the spectral diagram is shown in fig. 4. The sample wafers are consistent at the bimodal position on the Raman spectrum, and the peak near the 1380cm < -1 > position is a D peak representing the SP2 structure of the graphite phase; the peak near the 1600cm-1 position is a G peak representing the sp3 structure of diamond, and the spectral lines of the sample wafer are seen to have characteristic peaks of typical diamond-like films by contrast with the characteristic peaks of the spectral lines of diamond and graphite, indicating that DLC films are deposited on the sample wafer substrate.
(2) AFM for the 4# plate is shown in fig. 5:
DLC, estimated deposition rate about 11.7nm/min; the dust-free cloth is repeatedly rubbed for 20 times, and the dust-free cloth has no obvious scratch after being observed under a metallographic microscope, which proves that the wear resistance is better; the 3M adhesive tape is repeatedly pulled and torn at an angle of 90 degrees, and the DLC film does not fall off, which indicates that the bonding degree is good.
The experimental results show that the DLC film with good performance can be obtained on the deposition process conditions of 30 minutes and more for the glass lens, and the process preparation is carried out for the next resin-plated lens.
Example 3:
the DLC experiment of the resin lens with curvature adopts main technological parameters:
(1) Sample: resin lens 4 sheets.
(2) Cleaning: the cleaning process is carried out according to the standard.
(3) A mixed gas of methane (CH 4, purity 5N) and argon (Ar, purity 5N).
(4) Distance between upper and lower polar plates: 70mm.
(5) The lower plate sample stage was not heated.
(6) Chamber background vacuum: 8.0*10-4.
(7) Glow starting pressure: 5Pa, process pressure: the molecular pump gate valve is fully opened and kept at 3Pa.
Because the resin lens has low temperature resistance (100 ℃), the electrode plate sample table is not heated under PECVD, and is deposited at low temperature of about 25 ℃ at normal temperature. The main parameters to be regulated are: radio frequency power, gas flow ratio, and deposition time parameters. On the basis of a large number of experiments, the optimal technological parameters are found out, and the design of the experimental parameters is shown in table 2.
Table 2 parameters of DLC film experiments for curvature resin lenses
Experimental results and analysis:
(1) The DLC film is successfully deposited on all the 4 samples, and the deposited lenses are shown in FIG. 6; as can be seen from the figure, the resin sheet was excellent in light transmittance, and the film was dark brown in color, and the color gradually increased with increasing power and deposition time.
(2) The 1# sample wafer has large radio frequency power, long deposition time, molten center of the resin lens, dark color film and a large number of cracks, and can not be used; at reduced power to 150W, deposition time was reduced to 20 minutes, the resin lens was intact, dark brown film, and no cracking (see sheet 4), indicating that this parameter is a critical parameter for depositing resin sheets.
(3) The 2# and 3# sheets were deposited at moderate power for 30 minutes with the resin lenses intact, no cracks, and the film color was pale brown.
(4) The 4 kinds of sample pieces are repeatedly wiped for 20 times by using dust-free cloth, and have no obvious scratches when observed under a metallographic microscope, which shows that the wear resistance is better (see figure 7).
(5) The 4 samples were repeatedly pulled and torn at 90 degrees using a 3M tape, and the DLC film did not fall off (see fig. 8), demonstrating good bonding.
(6) The colors of the center and the edge films of the 4 curvature sample wafers are not obviously different, which indicates that the film thicknesses are consistent.
The experimental results show that the curved resin lens has better deposition effect under the medium power below 100W. In theory, the hardness of the film can be increased by increasing the proportion of argon, but in the experiment, the DLC film with better hardness can be obtained by adopting the methane-argon ratio of 1:1 and 3:1, and the wear resistance requirement of the lens is met. The curvature of the resin lens has no obvious effect on the thickness of the deposited DLC film. To mitigate the color depth of the film, this can be achieved by reducing the deposition time under medium power conditions.
Example 4:
a planar resin lens low temperature DLC experiment (deposition time, power, gas flow conditions); the main technological parameters of the planar circular optical resin lens are as follows:
(1) Sample: the planar resin lenses 16 are divided into 4 groups of 4 sheets each.
(2) Cleaning: the cleaning process is carried out according to the standard.
(3) A mixed gas of methane (CH 4, purity 5N) and argon (Ar, purity 5N).
(4) Distance between upper and lower polar plates: 70mm.
(5) The lower plate sample stage was not heated.
(6) Radio frequency power: 100w.
(7)CH4：Ar＝60sccm：20sccm。
(8) Chamber background vacuum: 8.0*10-4.
(9) Glow starting pressure: 5Pa, process pressure: the molecular pump gate valve is fully opened and kept at 3Pa.
Since the optical resin lens requires the DLC film to be plated to be colorless by naked eye observation, film thickness is controlled by adjusting deposition time under medium radio frequency power. On the basis of a large number of experiments, the optimal technological parameters are found out, and the design of the experimental parameters is shown in table 3.
Table 3 parameters of DLC film experiments for planar optical resin lenses
Experimental results and analysis:
(1) Four sets of deposited lenses were each observed as shown in fig. 9. 1-3 groups of sample sheets, compared with the uncoated lens, the fourth group of lens has no obvious color and little chromatic aberration.
(2) Raman spectra were performed on four groups of samples, except that the 4 th group had a double peak (see fig. 10), and the other 3 groups did not show that the nano-scale DLC film could be successfully coated at a power of 60 watts for more than 10 minutes.
(3) The first sample piece was repeatedly rubbed 20 times with dust-free cloth, and when seen in bare eyes, the first sample piece had obvious scratches and some DLC films were peeled off, as shown in fig. 11. The film is thinner and the binding force is poor due to the short deposition time.
The above experimental results show that when the nano DLC film is plated on the planar resin lens, a transition layer is needed to increase the adhesive force and wear resistance of the film.
Example 5:
experiment of Ti-plated transition layer of resin lens: because certain internal stress exists when the DLC film with high hardness is combined with the lens, the stress is influenced by synthesis process parameters and a film tissue structure, and the stress becomes a main cause for weakening the film interface bonding force. Currently, research into improving the bond strength of the film interface to the lens matrix interface and enhancing the frictional wear resistance of the film has focused on the design and preparation of the transition layer. Firstly, a Ti functional film is deposited on a substrate on a lens by adopting a radio frequency magnetron sputtering technology to serve as a transition layer, and then a DLC film is prepared on the Ti transition layer. Experimental results show that the properties of the film are greatly improved compared with the film directly coated on the substrate.
The main experimental parameters are as follows:
(1) Sample: 6 planar resin sheets;
(2) The device comprises: magnetron sputtering, namely a Beijing-created micro-nano MSP-300BI magnetron sputtering instrument;
(3) And (3) target material: titanium target, beijing minoxidil, purity 4.5N;
(4) Process gas: pure argon 40sccm;
(5) Chamber background vacuum: 2 x 10-3;
(6) The sample table is not heated and is at the normal temperature of 25 ℃;
(7) Dc target power: 80W, rate 0.1176nm/s;
(8) Glow starting pressure: 5Pa, process pressure: and regulating a molecular pump gate valve to maintain 0.68Pa.
(9) Sputtering time: 2s, 5s, 10s, 15s, 20s, 25s
Ti film plating experiments for various times on the coupons are shown in fig. 12.
Experimental results and analysis:
(1) The 6 samples were well transparent and were all conducted by IV testing using the semiconductor parameter tester 4200, indicating success of Ti film plating.
(2) The Ti film with the sputtering time of 25s can be obviously observed by naked eye observation, in order not to influence the transparency of the lens and consider a certain film thickness, the Ti film sputtered for 20s is taken and tested by a step-by-step instrument, and the thickness of the Ti film is 2.5nm.
(3) The 6 sample pieces are repeatedly pulled and torn at an angle of 90 degrees by using a 3M adhesive tape, and the Ti film does not fall off, which indicates that the bonding degree is good.
(4) And then 6 plane resin lenses are taken, sputtered for 20s and plated with Ti film for standby.
Example 6:
DLC plating experiment of a planar resin lens containing a Ti transition layer: the main technological parameters of the optical resin lens with the transition layer are as follows:
(1) Sample: optical resin lens with 6 titanium bonding layers (2.5 nm)
(2) A mixed gas of methane (CH 4, purity 5N) and argon (Ar, purity 5N).
(3) The lower polar plate is not heated and is at normal temperature of 25 ℃.
(4) Distance between upper and lower polar plates: 70mm.
(5) Radio frequency power: 100w;
(6) Chamber background vacuum: 4*10-4.
(7) Glow starting pressure: 3.4Pa, process pressure: and regulating a molecular pump gate valve to keep 3Pa.
The experiment keeps the PECVD radio frequency power 100W unchanged, and the optimal technological parameters are found out on the basis of a large number of experiments mainly by adjusting the deposition time and the gas flow ratio, and the experimental parameter design is shown in table 4.
TABLE 4 Experimental parameters for DLC film of optical resin lens containing transition layer
Experimental results: the deposition rate was 1nm/s, the light color DLC film, the mirror cloth was scratched, but not rubbed off.
(1) The 6 samples were all successfully deposited with DLC film and had good light transmittance, and the deposited lenses are shown in FIG. 13. Except for 6# tablets, the tablets had pale tea color, and all the other 5 tablets had no obvious color film.
(2) The # 1, # 2 and # 3 lenses were scratched but not rubbed off, indicating that a decrease in the argon ratio affected the film hardness (see fig. 14).
(3) The 4# and 5# mirror cloths were wiped free of scratches (as shown in fig. 15), and the scratches were not removed, indicating that the argon gas ratio was increased and the film hardness was increased.
The experimental results show that under the condition of considering a certain film thickness, the radio frequency power is 100W, CH4: ar=100 sccm:100sccm, and the DLC film is stable under the process condition of depositing for 5 minutes, and has good comprehensive effect.
In the invention, a method combining theory and experiment is adopted, and for different DLC film coating requirements, a large number of experiments and tests are mainly carried out to obtain the optimal technological parameters of the DLC film. The main process parameters are summarized as follows:
under the condition of no strict requirement on the color of the DLC film, the film with better combination degree and wear resistance can be realized by adjusting the deposition time of a coating film under the condition of medium power, and the process parameters are recommended: rf power 100w, ch4: ar=100 sccm:100sccm, 3Pa, and deposition time of 30 minutes.
Under the condition that no obvious color is required to be observed in naked eyes on the color of the DLC film, a magnetron sputtering coating instrument is used for sputtering a Ti transition film with the thickness of 2.5nm, DLC is deposited on the transition film, and the technological parameters are recommended: rf power 100w, ch4: ar=100 sccm:100sccm, 3Pa, and 5 minutes of deposition time.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (9)
1. A method for preparing a deposited diamond-like film of a polycarbonate lens, comprising the steps of:
step 1: sample treatment, including sample cleaning and sample pretreatment, wherein the sample cleaning requires cleaning the substrate before the substrate is placed in the PECVD vacuum chamber;
step 2: the sample deposition DLC film and test analysis comprises a glass lens DLC film experiment, a resin lens DLC experiment with curvature, a plane resin lens low-temperature DLC experiment, a resin lens Ti transition layer plating experiment and a plane resin lens DLC plating experiment containing a Ti transition layer;
step 3: the characterization measurement of the DLC film comprises morphology structure characterization and performance characterization, wherein the morphology structure characterization mainly comprises: scanning electron microscope SEM, raman spectrometer Raman, X-ray diffractometer XRD, X-ray photoelectron spectrometer XPS, atomic force microscope AFM; the performance characterization included wear resistance: evaluating the wear resistance of the film by adopting a dust-free cloth in a friction manner; degree of bonding: testing the bonding degree of the film by adopting 3M glue in a sticking and tearing mode; transparency: quantitatively analyzing the transparency by adopting a naked eye observation method;
step 4: and adjusting and optimizing the process parameters according to the characterization and measurement structure of the film, and finally determining the optimal process parameters through different process parameter combinations.
2. The method for preparing a diamond-like film deposited on a polycarbonate lens according to claim 1, wherein the sample cleaning in step 1 mainly comprises the following steps:
s1: placing a sample wafer to be washed into a clean beaker, adding a proper amount of detergent and deionized water, placing the sample wafer into an ultrasonic cleaner, and performing ultrasonic treatment for 10 minutes to remove oil stains and large-particle impurities on the surface;
s2: placing the sample wafer into a proper amount of acetone solution, sealing the beaker to prevent volatilization, and then ultrasonically cleaning for 10 minutes to remove organic impurities on the surface;
s3: placing the sample into a proper amount of absolute ethyl alcohol, sealing to prevent volatilization, then ultrasonically cleaning for 10 minutes, and removing organic solvents such as acetone and the like on the surface of the sample;
s4: placing the sample into a proper amount of deionized water, ultrasonically cleaning for 10 minutes, and removing absolute ethyl alcohol on the surface of the sample;
s5: purging the surface of the sample by using nitrogen, removing deionized water on the surface, and keeping the sample dry and clean;
s6: after drying in an oven at 50 ℃ for about 20 hours, the mixture was put into a vacuum drying oven for standby.
3. The method according to claim 1, wherein the sample pretreatment in step 1 comprises removing impurities on the surface of the substrate by bombardment with argon plasma for 10 minutes before introducing the carbon source gas, and generating groups containing unsaturated bonds on the surface of the substrate to improve the surface activity of the substrate, so as to ensure the adhesion of the film firmly combined between the substrate and the film.
4. A method for preparing a diamond-like film deposited on a polycarbonate lens according to claim 3, wherein the main process parameters of the PECVD vacuum chamber in step 1 are set as background vacuum: 8.0X10-4 Pa, radio frequency power: 100W, ar flow: 30sccm, glow-starting pressure: 3Pa.
5. The method for preparing a diamond-like film deposited on a polycarbonate lens according to claim 1, wherein the main process parameters adopted in the step 3 of the experiment of DLC film of a glass lens are as follows: sample: 4 quartz glass sheets; cleaning: according to a standard cleaning flow; a mixed gas of methane (CH 4, purity 99.995%) and argon (Ar, purity 99.999%); distance between upper and lower polar plates: 70mm; radio frequency power: 200W; chamber background vacuum: 3.6X10-3 Pa; glow starting pressure: 5Pa, process pressure: the molecular pump gate valve is fully opened and kept at 3Pa.
6. The method for preparing a diamond-like film deposited on a polycarbonate lens according to claim 1, wherein the main process parameters adopted in the DLC test of the resin lens with curvature in the step 3 are as follows: sample: 4 resin lenses; cleaning: according to a standard cleaning flow; a mixed gas of methane (CH 4, purity 5N) and argon (Ar, purity 5N); distance between upper and lower polar plates: 70mm; the lower polar plate sample table is not heated; chamber background vacuum: 8.0 x 10-4; glow starting pressure: 5Pa, process pressure: the molecular pump gate valve is fully opened and kept at 3Pa.
7. The method for preparing the diamond-like film deposited on the polycarbonate lens according to claim 1, wherein the main process parameters of the low-temperature DLC test of the planar resin lens in the step 3 are as follows: sample: the planar resin lenses 16 are divided into 4 groups of 4 sheets each; cleaning: according to a standard cleaning flow; a mixed gas of methane (CH 4, purity 5N) and argon (Ar, purity 5N); distance between upper and lower polar plates: 70mm; the lower polar plate sample table is not heated; radio frequency power: 100w; CH4: ar=60 sccm:20sccm; chamber background vacuum: 8.0 x 10-4; glow starting pressure: 5Pa, process pressure: the molecular pump gate valve is fully opened and kept at 3Pa.
8. The method for preparing a diamond-like film deposited on a polycarbonate lens according to claim 1, wherein the experimental parameters of the Ti-plating transition layer of the resin lens in the step 3 are as follows: sample: 6 planar resin sheets; the device comprises: magnetron sputtering, namely a Beijing-created micro-nano MSP-300BI magnetron sputtering instrument; and (3) target material: titanium target, beijing minoxidil, purity 4.5N; process gas: pure argon 40sccm; chamber background vacuum: 2 x 10-3; the sample table is not heated and is at the normal temperature of 25 ℃; dc target power: 80W, rate 0.1176nm/s; glow starting pressure: 5Pa, process pressure: regulating a molecular pump gate valve, and keeping 0.68Pa; sputtering time: 2s, 5s, 10s, 15s, 20s, 25s.
9. The method for preparing the diamond-like film deposited on the polycarbonate lens according to claim 1, wherein the DLC plating experiment of the planar resin lens containing the Ti transition layer comprises the following main technological parameters: sample: an optical resin lens with 6 titanium bonding layers (2.5 nm); a mixed gas of methane (CH 4, purity 5N) and argon (Ar, purity 5N); the lower polar plate is not heated and is at the normal temperature of 25 ℃; distance between upper and lower polar plates: 70mm; radio frequency power: 100w; chamber background vacuum: 4 x 10-4; glow starting pressure: 3.4Pa, process pressure: and regulating a molecular pump gate valve to keep 3Pa.
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