CN113913822A - Chalcogenide glass lens plated with hard film and processing technology thereof - Google Patents
Chalcogenide glass lens plated with hard film and processing technology thereof Download PDFInfo
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- 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
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- 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
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Abstract
The invention discloses a chalcogenide glass lens plated with a hard film and a processing technology thereof. A chalcogenide compound glass lens plated with a hard film is characterized in that a first anti-pollution film layer, a first yttrium fluoride film layer, a second anti-pollution film layer, a second yttrium fluoride film layer, a third anti-pollution film layer and a hard film layer are sequentially arranged on the surface of the chalcogenide compound glass lens from inside to outside. Also discloses a processing technology of the chalcogenide glass lens plated with the hard film, which comprises the following steps: 1) plating an anti-reflection film; 2) plating and adding a hard film. The method for plating the hardened film adopts a stepped plating method which is carried out in steps, and the step-by-step plating method meets the requirement that the required optical spectrum specification requires that the average transmittance Tave is more than or equal to 90 percent in the range of 6-13 mu m, thereby improving the problems that the film is easy to strip and the quality defect of film breakage is easily caused due to the influence of film thickness stress, and improving the product quality of chalcogenide glass lenses.
Description
Technical Field
The invention relates to a chalcogenide glass lens plated with a hard film and a processing technology thereof.
Background
The far infrared glass is material glass (also called chalcogenide glass) formed by taking anti-pollution, As, Se and Sb As main elements, and the chalcogenide glass is infrared optical glass with wide infrared application because the special structure and components of the chalcogenide glass have the advantages of good transmittance, extremely low refractive index, temperature coefficient of heat, dispersibility, easiness in preparation and the like between 2 and 14 mu m, and is used in military optical systems, infrared thermal imagers, civil vehicle-mounted night vision and other related fields.
In practical use, the window sheet of the exposed lens of the chalcogenide glass lens is scratched or scratched due to uneven thickness caused by the friction between dust, wind sand and other foreign matters and the surface of the glass during use; the beauty of the lens and the strength of the window sheet are directly influenced, and the optical transmittance of the infrared lens is reduced. Aiming at the problems, the method can be improved by plating the diamond-like carbon film super-hard film; if the material of the infrared lens is an anti-pollution material or other non-infrared chalcogenide glass single chip, a DLC (Diamond-like carbon) film can be directly plated on the surface of the glass, so that the hardness of the surface of the glass can be increased to protect the surface of the lens glass.
For infrared lens chalcogenide glass lens, the chalcogenide glass lens is different from the anti-pollution material or other single crystal infrared lens in characteristics. If the hard film is directly plated by using the prior art method, the following defects which affect the performance of the infrared lens can be generated on the surface of chalcogenide glass: 1) the requirement that the optical spectrum specification of the chalcogenide glass lens requires 6-13 mu m average transmittance spectrum Tave is more than or equal to 90 percent can not be obtained by directly plating and adding a hard film on the surface of the chalcogenide glass lens; 2) in the process of optical film forming and plating, the infrared chalcogenide glass is greatly influenced by stress along with the increase of the hardened film thickness, and the film layer is easily broken and has poor quality according to the prior art.
The existing DLC plating technology can not directly realize surface plating on chalcogenide glass, the requirement that the average transmittance Tave of 6-13 mu m of the required optical spectrum transmittance is more than or equal to 90 percent can not be met after direct plating, and film stripping and film breakage are easy to generate due to the influence of film thickness stress. Therefore, there is a need to develop a chalcogenide glass lens hard film plating technology to solve the above problems, so as to improve the quality of the product.
Disclosure of Invention
The invention aims to provide a chalcogenide glass lens plated with a hard film and a processing technology thereof.
The technical scheme adopted by the invention is as follows:
a chalcogenide compound glass lens plated with a hard film is characterized in that a first anti-pollution film layer, a first yttrium fluoride film layer, a second anti-pollution film layer, a second yttrium fluoride film layer, a third anti-pollution film layer and a hard film layer are sequentially arranged on the surface of the chalcogenide compound glass lens from inside to outside.
The thickness of the first anti-pollution film layer is 205-215 nm, the thickness of the first yttrium fluoride film layer is 310-330 nm, the thickness of the second anti-pollution film layer is 618-633 nm, the thickness of the second yttrium fluoride film layer is 1178-1930 nm, the thickness of the third anti-pollution film layer is 69-88 nm, and the thickness of the hardening film layer is 300-460 nm.
A processing technology of a chalcogenide glass lens plated with a hard film comprises the following steps:
1) plating an antireflection film: sequentially evaporating a first anti-pollution film, a first yttrium fluoride film, a second anti-pollution film, a second yttrium fluoride film and a third anti-pollution film on the surface of a chalcogenide glass lens to be plated to obtain a substrate plated with an AR film;
2) plating and adding a hard film: and (3) placing the substrate plated with the AR film in deposition equipment, introducing inorganic gas to clean the substrate under a vacuum condition, introducing alkane gas to perform radio frequency glow ionization, and depositing dissociated alkane gas on the surface of the substrate plated with the AR film to form a hard film layer so as to prepare the chalcogenide glass lens plated with the hard film.
In the processing step 2), the deposition equipment is a carbon film machine.
In the step 2) of the processing technology, the introduction amount of the inorganic gas is 20-40 sccm.
In the processing step 2), the inorganic gas is argon.
In the step 2) of the processing technology, the introduction amount of the alkane gas is 30-50 sccm.
In step 2) of the process, the alkane gas is C4H 10.
In the processing step 2), the deposition time of the hardened film is 300-600 seconds.
In the processing technology step 2), the gas pressure of the system before the inorganic gas is introduced is less than 3 multiplied by 10 < -3 > Pa, the gas pressure of the system when the inorganic gas is introduced for cleaning is 3-6 Pa, and the gas pressure of the system when the alkane gas is introduced for deposition is 8-20 Pa.
The invention has the beneficial effects that:
the method for plating the hardened film adopts a stepped plating method which is carried out in steps, and the step-by-step plating method meets the requirement that the required optical spectrum specification requires that the average transmittance Tave is more than or equal to 90 percent in the range of 6-13 mu m, thereby improving the problems that the film is easy to strip and the quality defect of film breakage is easily caused due to the influence of film thickness stress, and improving the product quality of chalcogenide glass lenses.
Specifically, the method comprises the following steps:
1. the chalcogenide glass lens adopts the film system design of AR (anti-pollution + yttrium fluoride + anti-pollution) + DLC, and has the following advantages: firstly, due to the characteristics of chalcogenide glass materials, the adhesion of the optical film can be influenced by the surface film layer bonding stress, and the anti-pollution film material and the substrate are used as the first layer of the AR dielectric film for priming, so that the film layer bonding stress is reduced to a certain extent, the film and the substrate are bonded more tightly, and the bonding firmness of the film and the substrate is favorably improved; secondly, the film material of the film system has a high (pollution-resistant) and low (yttrium fluoride) refractive index matching mode, which is beneficial to realizing the specification requirement of the spectrum transmittance of the infrared optical film; and the membrane system designed by matching AR + DLC is beneficial to better stabilizing the requirement of the thickness of the hard membrane added in each plating process, thereby ensuring the spectral repeatability and quality stability of the optical thin film after the hard membrane is added in each plating process.
2. The method uses the C4H10 gas, so that glow ionization can be carried out in a short time during the plating of the hard film to obtain enough carbon element rapid deposition hard film, the hard film can be deposited and plated after one plating for 300-600 seconds, and compared with other hard film plating methods, the method needs about 1800 seconds, thereby greatly saving the plating time and being beneficial to improving the production efficiency.
Detailed Description
A chalcogenide compound glass lens plated with a hard film is characterized in that a first anti-pollution film layer, a first yttrium fluoride film layer, a second anti-pollution film layer, a second yttrium fluoride film layer, a third anti-pollution film layer and a hard film layer are sequentially arranged on the surface of the chalcogenide compound glass lens from inside to outside. Wherein the first anti-pollution film layer, the first yttrium fluoride film layer, the second anti-pollution film layer, the second yttrium fluoride film layer and the third anti-pollution film layer form an AR film.
Preferably, the thickness of the first anti-pollution film layer is 205-215 nm, the thickness of the first yttrium fluoride film layer is 310-330 nm, the thickness of the second anti-pollution film layer is 618-633 nm, the thickness of the second yttrium fluoride film layer is 1178-1930 nm, the thickness of the third anti-pollution film layer is 69-88 nm, and the thickness of the hardening film layer is 300-460 nm.
A processing technology of a chalcogenide glass lens plated with a hard film comprises the following steps:
1) plating an antireflection film: sequentially evaporating a first anti-pollution film, a first yttrium fluoride film, a second anti-pollution film, a second yttrium fluoride film and a third anti-pollution film on the surface of a chalcogenide glass lens to be plated to obtain a substrate plated with an AR film;
2) plating and adding a hard film: and (3) placing the substrate plated with the AR film in deposition equipment, introducing inorganic gas to clean the substrate under a vacuum condition, introducing alkane gas to perform radio frequency glow ionization, and depositing dissociated alkane gas on the surface of the substrate plated with the AR film to form a hard film layer so as to prepare the chalcogenide glass lens plated with the hard film.
In the processing step 2), preferably, the deposition equipment is a carbon film machine.
In the processing step 2), preferably, the introduction amount of the inorganic gas is 20 to 40 sccm.
In process step 2), the inorganic gas is preferably argon.
In the step 2) of the processing technology, preferably, the introduction amount of the alkane gas is 30-50 sccm.
In process step 2), the preferred alkane gas is C4H 10.
In the processing step 2), preferably, the deposition time of the hardened film is 300 to 600 seconds.
In the processing technology step 2), the gas pressure of the system before the inorganic gas is introduced is less than 3 multiplied by 10 < -3 > Pa, the gas pressure of the system when the inorganic gas is introduced for cleaning is 3-6 Pa, and the gas pressure of the system when the alkane gas is introduced for deposition is 8-20 Pa.
The AR (Anti-Reflection) film is an antireflection film.
The present invention will be described in further detail with reference to specific examples.
The film materials used for evaporating the anti-pollution layer and the yttrium fluoride layer in the embodiments 1 to 4 are common optical film materials in the field, and can be purchased from the market.
Example 1:
example 1 the process for manufacturing a chalcogenide glass lens coated with a hard film comprises:
1) plating an antireflection film: sequentially evaporating a first anti-pollution film with the thickness of 210nm, a first yttrium fluoride film with the thickness of 323nm, a second anti-pollution film with the thickness of 624nm, a second yttrium fluoride film with the thickness of 1185nm and a third anti-pollution film with the thickness of 69nm on the surface of a chalcogenide compound glass lens to be plated to obtain a substrate plated with an AR film;
2) plating and adding a hard film: placing the substrate coated with the AR film in a carbon film machine, vacuumizing until the system pressure is 2 x 10 < -3 > Pa, introducing 25sccm argon to enable the system pressure to be 3-5 Pa, starting a radio frequency high-voltage system to enable argon glow discharge to carry out AR film bombardment cleaning on the substrate, then introducing 35sccm C4H10 gas to enable the system pressure to be 9-10 Pa, starting radio frequency glow discharge, forming plasma glow dissociation C4H10 gas in the area above the substrate, and depositing the dissociated C4H10 gas on the surface of the substrate coated with the AR film for 500 seconds to form a hardened film layer with the thickness of 329 nm.
Example 2:
example 2 the process for manufacturing a chalcogenide glass lens coated with a hard film comprises:
1) plating an antireflection film: sequentially evaporating a first anti-pollution film with the thickness of 212nm, a first yttrium fluoride film with the thickness of 328nm, a second anti-pollution film with the thickness of 629nm, a second yttrium fluoride film with the thickness of 1190nm and a third anti-pollution film with the thickness of 74nm on the surface of a chalcogenide compound glass lens to be plated to obtain a substrate plated with an AR film;
2) plating and adding a hard film: placing the substrate coated with the AR film in a carbon film machine, vacuumizing until the system pressure is 2 x 10 < -3 > Pa, introducing 25sccm argon to enable the system pressure to be 3-5 Pa, starting a radio frequency high-voltage system to enable argon glow discharge to carry out AR film bombardment cleaning on the substrate, then introducing 35sccm C4H10 gas to enable the system pressure to be 9-10 Pa, starting radio frequency glow discharge, forming plasma glow dissociation C4H10 gas in the area above the substrate, and depositing the dissociated C4H10 gas on the surface of the substrate coated with the AR film for 450 seconds to form a hardened film layer with the thickness of 308 nm.
Example 3:
example 3 the process for manufacturing a chalcogenide glass lens coated with a hard film comprises:
1) plating an antireflection film: sequentially evaporating a first anti-pollution film with the thickness of 205nm, a first yttrium fluoride film with the thickness of 315nm, a second anti-pollution film with the thickness of 620nm, a second yttrium fluoride film with the thickness of 1180nm and a third anti-pollution film with the thickness of 70nm on the surface of a chalcogenide compound glass lens to be plated to obtain a substrate plated with an AR film;
2) plating and adding a hard film: placing the substrate plated with the AR film in a carbon film machine, vacuumizing until the system pressure is 2 x 10 < -3 > Pa, introducing 35sccm argon to enable the system pressure to be 4-6 Pa, starting a radio frequency high-voltage system to enable argon glow discharge to carry out AR film bombardment cleaning on the substrate, then introducing 45sccm C4H10 gas to enable the system pressure to be 15-18 Pa, starting radio frequency glow discharge, forming plasma glow dissociation C4H10 gas in the area above the substrate, and depositing the dissociated C4H10 gas on the surface of the substrate plated with the AR film for 400 seconds to form a hardened film layer with the thickness of 335 nm.
Example 4:
example 4 the process for manufacturing a chalcogenide glass lens coated with a hard film is as follows:
1) plating an antireflection film: sequentially evaporating a first anti-pollution film with the thickness of 214nm, a first yttrium fluoride film with the thickness of 328nm, a second anti-pollution film with the thickness of 633nm, a second yttrium fluoride film with the thickness of 1920nm and a third anti-pollution film with the thickness of 87nm on the surface of a chalcogenide glass lens to be plated to obtain a substrate plated with an AR film;
2) plating and adding a hard film: placing the substrate plated with the AR film in a carbon film machine, vacuumizing until the system pressure is 2 x 10 < -3 > Pa, introducing 35sccm argon to enable the system pressure to be 4-6 Pa, starting a radio frequency high-voltage system to enable argon glow discharge to carry out AR film bombardment cleaning on the substrate, then introducing 45sccm C4H10 gas to enable the system pressure to be 15-18 Pa, starting radio frequency glow discharge, forming plasma glow dissociation C4H10 gas in the area above the substrate, and depositing the dissociated C4H10 gas on the surface of the substrate plated with the AR film for 550 seconds to form a hardened film layer with the thickness of 456 nm.
Comparative example 1:
only one layer of a 329nm thick hardened film was deposited on a chalcogenide glass lens to be coated as a comparative example, and the remaining conditions were the same as those of example 1.
Tests show that the transmittance Tave of the chalcogenide glass lens only plated with the hard film in the comparative example 1 is lower than 80% in the range of the infrared wavelength of 6-13 μm, and the transmittance Tave of the chalcogenide glass lens plated with the AR + hard film in the example 1 is higher than 90% in the range of the infrared wavelength of 6-13 μm. In example 2, the transmittance Tave is greater than 90% in the infrared wavelength range of 6 to 13 μm. In the infrared wavelength range of 6 to 13 μm, the average value of the transmittance Tave of example 1 is 96.17%, and the average value of the transmittance of example 2 is 94.10%.
The diamond-coated chalcogenide glass lenses of examples 1 to 4 were subjected to an adhesion test, a friction test, a low-temperature test, a high-temperature and high-humidity test, a high-low-temperature impact test, a salt spray test, and a dust test, respectively, according to GB/T32559-2016.
1. Adhesion test
Testing the tool: LP-24 adhesive tape
The test method comprises the following steps: adhering the film layer surface of the plating-accompanying sheet by using LP-24 adhesive tape, wherein the adhesive tape is adhered at the diagonal line or diameter of the plating-accompanying sheet, and then rapidly pulling up the film layer surface by a force perpendicular to the film layer surface for 2 times.
And (3) testing results: the surface quality of the film layer of the plated film is checked by visual inspection under a 11W desk lamp, and in the examples 1-4, no change and no film stripping are caused after the test, and the adhesion test is qualified.
2. Friction force test
Testing the tool: friction-resistant test rod
The test method comprises the following steps: the wear-resistant rod provided with the wear-resistant eraser is held by a hand, the pen point is wrapped by clean degreasing cloth, 1Kg of force is kept to be vertical to the surface of the film layer, the film layer accompanied with the plating is rubbed, the stroke length is about 2 times of the diameter of the friction head, and the film layer is rubbed 500 times (250 times of back and forth) along the same track.
And (3) testing results: the surface quality of the film layer of the plated sheet is checked by reflection visual inspection under an 11W table lamp, no change and no film damage are caused after the friction force test in the embodiments 1 to 4, and the friction force test is qualified.
3. Low temperature testing
Testing equipment: constant temperature and humidity testing machine
And (3) testing conditions are as follows: low temperature experiment (-40 ℃, 72h)
And (3) testing results: the surface quality of the plated film layer is checked by visual inspection of reflection under an 11W desk lamp, and then the adhesive force is tested. The results show that the surfaces of the films in examples 1-4 have no change after low-temperature testing; the adhesive force is not changed and the film is not peeled before and after the test, and the adhesive force is qualified. Therefore, the low temperature tests of examples 1 to 4 were acceptable.
4. High temperature high humidity test
Testing equipment: constant temperature and humidity testing machine
And (3) testing conditions are as follows: high temperature and humidity experiment (60 ℃ 90% RH, 72h)
And (3) testing results: the surface quality of the plated film layer is checked by visual inspection of reflection under an 11W desk lamp, and then the adhesive force is tested. The results show that the surfaces of the film layers in the examples 1 to 4 are unchanged after the high-temperature and high-humidity test; the adhesive force is not changed and the film is not peeled before and after the test, and the adhesive force is qualified. Therefore, the high temperature and high humidity tests of examples 1 to 4 were satisfactory.
5. High and Low temperature impact test
Testing equipment: cold and hot impact testing machine
And (3) testing conditions are as follows: high and low temperature impact test (20 min each at 70 ℃ to-40 ℃, 3 cycles)
And (3) testing results: the surface quality of the plated film layer is checked by visual inspection of reflection under an 11W desk lamp, and then the adhesive force is tested. The results show that the surfaces of the film layers in the examples 1-4 are not changed after the high-low temperature impact test; the adhesive force is not changed and the film is not peeled before and after the test, and the adhesive force is qualified. Therefore, the high and low temperature impact tests of examples 1 to 4 were acceptable.
6. Salt spray test
Testing equipment: salt spray testing machine
And (3) testing conditions are as follows: the temperature is 35 ℃ plus or minus 2 ℃, the concentration of the salt solution is 5 plus or minus 1 percent, the sedimentation rate is 1-3 ml/80cm2 & h, the spraying is continued for 24h, and the drying is carried out for 24h at the temperature of 30 ℃ and 40 percent RH.
And (3) testing results: the surface quality of the plated film layer is checked by visual inspection of reflection under an 11W desk lamp, and then the adhesive force is tested. The results show that the surfaces of the film layers in the examples 1 to 4 are unchanged after the salt spray test; the adhesive force is not changed and the film is not peeled before and after the test, and the adhesive force is qualified. Therefore, the salt spray tests of examples 1 to 4 were acceptable.
7. Dust test
Testing equipment: programmable sand dust test box
And (3) testing conditions are as follows: the temperature is 70 +/-2 ℃, the humidity is 25-30% RH, and the talcum powder is blown for 90 min.
And (3) testing results: the surface quality of the plated film layer is checked by visual inspection of reflection under an 11W desk lamp, and then the adhesive force is tested. The results show that in the examples 1-4, the surface of the film layer is unchanged after the sand dust test; the adhesive force is not changed and the film is not peeled before and after the test, and the adhesive force is qualified. Therefore, the sand dust tests of examples 1 to 4 were passed.
In summary, in order to solve the abrasion resistance and corrosion resistance of the optical film on the surface of the chalcogenide glass window sheet of the infrared lens, the obtained film is subjected to 500 times of back-and-forth abrasion-resistant wiping and wind-sand-and-salt-fog-resistant film testing under the force of 1kg/cm2 of a special tool. Meanwhile, the DLC film realized by the infrared lens chalcogenide glass DLC stepped plating method can meet the requirement that the average transmittance Tave of 6-13 mu m required by the spectrum transmission specification of the infrared optical film is more than or equal to 90 percent, and various tests such as an adhesive force test, a friction force test, a low-temperature test, a high-temperature high-humidity test, a high-low-temperature impact test, a salt spray test and a sand dust test all meet the required requirements.
Claims (10)
1. A chalcogenide glass lens plated with a hard film is characterized in that: the surface of the chalcogenide compound glass lens is sequentially provided with a first anti-pollution film layer, a first yttrium fluoride film layer, a second anti-pollution film layer, a second yttrium fluoride film layer, a third anti-pollution film layer and a hardened film layer from inside to outside.
2. The hard-coated chalcogenide glass lens according to claim 1, wherein: the thickness of the first anti-pollution film layer is 205-215 nm, the thickness of the first yttrium fluoride film layer is 310-330 nm, the thickness of the second anti-pollution film layer is 618-633 nm, the thickness of the second yttrium fluoride film layer is 1178-1930 nm, the thickness of the third anti-pollution film layer is 69-88 nm, and the thickness of the hardening film layer is 300-460 nm.
3. The process for processing a chalcogenide glass lens coated with a hard film according to claim 1, which comprises the following steps: the method comprises the following steps:
1) plating an antireflection film: sequentially evaporating a first anti-pollution film, a first yttrium fluoride film, a second anti-pollution film, a second yttrium fluoride film and a third anti-pollution film on the surface of a chalcogenide glass lens to be plated to obtain a substrate plated with an AR film;
2) plating and adding a hard film: and (3) placing the substrate plated with the AR film in deposition equipment, introducing inorganic gas to clean the substrate under a vacuum condition, introducing alkane gas to perform radio frequency glow discharge, and depositing dissociated alkane gas on the surface of the substrate plated with the AR film to form a hard film layer so as to prepare the chalcogenide glass lens plated with the hard film.
4. The process for processing a chalcogenide glass lens coated with a hard film according to claim 3, wherein the process comprises the following steps: in the step 2), the deposition equipment is a carbon film machine.
5. The process for processing a chalcogenide glass lens coated with a hard film according to claim 3, wherein the process comprises the following steps: in the step 2), the introduction amount of the inorganic gas is 20-40 sccm.
6. The process for processing a chalcogenide glass lens coated with a hard film according to claim 5, wherein the process comprises the following steps: in the step 2), the inorganic gas is argon.
7. The process for processing a chalcogenide glass lens coated with a hard film according to claim 3, wherein the process comprises the following steps: in the step 2), the introduction amount of the alkane gas is 30-50 sccm.
8. The process for manufacturing a chalcogenide glass lens coated with a hard film according to claim 7, wherein: in the step 2), the alkane gas is C4H 10.
9. The process for processing a chalcogenide glass lens coated with a hard film according to claim 3, wherein the process comprises the following steps: in the step 2), the deposition time of the hardened film is 300-600 seconds.
10. The process for processing a chalcogenide glass lens coated with a hard film according to claim 3, wherein the process comprises the following steps: in the step 2), the gas pressure of the system before the inorganic gas is introduced is less than 3 multiplied by 10 < -3 > Pa, the gas pressure of the system when the inorganic gas is introduced for cleaning is 3-6 Pa, and the gas pressure of the system when the alkane gas is introduced for deposition is 8-20 Pa.
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