CN112813391A - Preparation method of ultra-wide waveband infrared long-wave pass cut-off light filtering film - Google Patents
Preparation method of ultra-wide waveband infrared long-wave pass cut-off light filtering film Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001914 filtration Methods 0.000 title description 2
- 239000000758 substrate Substances 0.000 claims abstract description 58
- 239000000463 material Substances 0.000 claims abstract description 49
- 230000003287 optical effect Effects 0.000 claims abstract description 24
- 238000009501 film coating Methods 0.000 claims abstract description 21
- 238000001704 evaporation Methods 0.000 claims abstract description 20
- 230000008020 evaporation Effects 0.000 claims abstract description 20
- 239000007888 film coating Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000004140 cleaning Methods 0.000 claims abstract description 15
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000007747 plating Methods 0.000 claims abstract description 12
- 229910009520 YbF3 Inorganic materials 0.000 claims abstract description 9
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 7
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 7
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 238000009504 vacuum film coating Methods 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 184
- 238000000034 method Methods 0.000 claims description 71
- 238000013461 design Methods 0.000 claims description 16
- 239000012788 optical film Substances 0.000 claims description 11
- 238000010884 ion-beam technique Methods 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 6
- 230000037452 priming Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000010409 thin film Substances 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 235000012149 noodles Nutrition 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 2
- 229910009518 YbF Inorganic materials 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 12
- 239000012528 membrane Substances 0.000 abstract description 10
- 239000011248 coating agent Substances 0.000 abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 238000002834 transmittance Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000001771 vacuum deposition Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
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- 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
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- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/208—Filters for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation
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Abstract
The invention discloses a preparation method of an ultra-wide waveband infrared long wave pass cut-off filter membrane, which adopts the technical scheme that: (1) designing a film system formula by taking infrared material silicon (Si) as a substrate; calculating the physical thickness value of each layer of film; (2) cleaning the plated substrate; (3) heating and baking the substrate; (4) bombarding the substrate with an ion source before and during coating; (5) putting ZnS film material into a rotary evaporation-resistant evaporation source, putting three film materials of Si, Ge and YbF3 into a rotary electron gun evaporation source crucible, and finishing film coating by using an optical vacuum film coating machine according to the formula sequence and the thickness value in the step (1); (6) and (5) annealing treatment. The invention solves the technical problem of plating the ultra-wide waveband long-wave-pass cut-off filter on the infrared material Si substrate.
Description
Technical Field
The invention belongs to the technical field of optical thin film plating, and relates to a preparation method of an ultra-wide waveband infrared long-wave pass cut-off filter film, which is used for realizing the design and preparation of the ultra-wide waveband infrared long-wave pass cut-off filter film for cutting off visible light (0.4-0.8 um), near infrared (0.8-3 um), middle infrared (3-5 um) and high-transmittance far infrared (7.5-13.5 um).
Background
The infrared film is widely applied to various optical and infrared components, solar cells and high-power laser systems. At present, many different types of infrared films can meet part of practical applications in the optical and infrared technical fields, and the requirements of wider practical applications on the comprehensive performance of the infrared films are continuously improved.
With the emergence and gradual increase of new coronary pneumonia epidemic situation, the patent technology of the invention is a key component of an infrared temperature measuring instrument, and is widely used (mainly used for testing the temperature of a human body) when resisting the epidemic situation; the indexes of the patent technology of the invention require that all light transmission is cut off before the middle infrared ray is 5um, and the transmittance is increased when the far infrared ray is 7.5-13.5 um.
The infrared film of the optical wave band not only requires that the film layer is very firmly plated and covered on the infrared material Si substrate, but also requires that the visible light (0.4-0.8 um), the near infrared (0.8-3 um) and the middle infrared (3-5 um) are deeply cut off, and the far infrared (7.5-13.5 um) is as high as possible. However, in the prior art, the infrared film materials which can be selected by the infrared-related broadband infrared film are few, and the film system design and the process are difficult. At present, conventional visible light and near infrared films are plated on a hard material substrate, the number of designed layers of the film layers is small, and the variety of available medium film materials is large (dozens); the ultra-wide band infrared long wave pass cut-off filter film required by the invention has only a plurality of types, the designed thickness of the film system is very thick, the firm requirement of the film is high, the process difficulty is large, the film is not comparable with the conventional infrared film system at present, otherwise, the ultra-wide band infrared long wave pass cut-off filter film product cannot be used in the field and in the air for a long time.
Disclosure of Invention
Objects of the invention
In order to overcome the defect that the conventional infrared film plating technology is only limited to plating infrared films by using a dielectric material in a single-point wavelength or narrow wavelength range, the invention provides a preparation method of an ultra-wide wavelength band infrared long-wave pass cut-off filter film, which can meet the requirements that a film layer plated on a Si substrate is hard and firm and can be used for a long time in the field and air.
(II) technical scheme
In order to solve the technical problem, the invention provides a preparation method of an ultra-wide waveband infrared long wave pass cut-off filter film, which comprises the following steps:
(1) taking Si as a substrate, the formula of a film system to be plated on two surfaces is as follows:
face 1G/100.0M 140.2H 359.4L 268.6H 489.9L 229.2H 495.3L 207.5H 467.4L 245.0H 508.5L 237.5H 442.9L 192.0H 592.8L 262.6H 699.7L 348.2H 617.3L 352.0H 766.3L 275.6H 812.9L 351.4H 534.2L 445.8H 687.6L 180.9H 473.0L 755.9N 88.1L 64.6H 20.0M/A;
face 2G/100.0M 69.1H 260.8L 195.7H 284.1L 148.2H 349.4L 207.8H 344.4L 157.9H 288.9L 163.9H 290.8L 183.1H 477.4L 126.6H 309.8L 124.3H 381.7L 31.3H 338.6L 121.2H 254.5L 131.2H 219.8L 105.1H 209.0L 146.2H 132.3L 312.3H 180.1L 73.9H 262.2L 95.9H 247.3L 118.6H 323.5L 755.9N 88.1L 64.6H 20.0M/A;
calculating the physical thickness value of each layer of film and tabulating in sequence; wherein G is a Si substrate and M isSi film material, H is Ge film material, L is ZnS film material, and N is YbF3A is an air medium with refractive index NA equal to 1, the reference wavelength λ c of the film system is equal to 800nm, M, H, N film materials are sequentially put into an electron gun evaporation source crucible of a vacuum chamber of a film coating machine for standby, and L film materials are put into a rotary evaporation resistant source.
(2) In the ultrasonic cleaning process of the coated substrate, cleaning the coated substrate with cleaning solution, drying the coated substrate by blowing, and placing the coated substrate into a vacuum chamber for vacuumizing and waiting to be coated;
(3) heating and baking the substrate, and gradually heating and baking at the temperature of 30-160 ℃ in a vacuum environment;
(4) in the optical film bonding priming process and the stress matching process, Si, Ge and YbF are mixed according to the optical thickness value of each film calculated by the film system design formula and the table sequence3Sequentially putting the three types of film materials into a rotary electron gun evaporation source crucible, putting the ZnS film material into a rotary evaporation resistance source, and then finishing film coating by using an optical vacuum film coating machine according to the formula list sequence and the thickness value in the step (1);
(5) in the ion source auxiliary evaporation process, an ion source is used for bombarding a substrate before and during film coating, and ion beams generated by the ion source are always used for bombarding the substrate until the film coating is finished;
(6) in the high-low temperature annealing process, the coated Si substrate is naturally cooled to room temperature in a vacuum chamber and then is annealed.
(III) advantageous effects
The preparation method of the ultra-wide waveband infrared long wave pass cut-off filter film provided by the technical scheme has the following beneficial effects:
(1) the existing infrared film (the reflectivity R is more than or equal to 95 percent) is generally plated in a single-point wavelength (such as 532nm or 1064nm) or a wave band range of hundreds of nanometers (< 1 um).
The ultra-wide waveband infrared long-wave pass cut-off filter film has the waveband range exceeding four thousand nanometers (larger than 4um), cuts off visible light (0.4-0.8 um), near infrared (0.8-3 um) and middle infrared (3-5 um) wavebands deeply, and solves the problems of narrow cutoff degree and low transmittance of infrared film waveband ranges in the prior art, wherein the infrared long-wave pass cut-off filter film has the advantages of narrow cutoff degree and low transmittance.
(2) The invention solves the process problem of firmness of the infrared film with super-thickness in the far infrared band.
In the prior art, the infrared film has a small range, so that the relative number of layers in the film system design is small, and the film layer is not too thick (generally less than 1 um). The preparation time of the coating process is short (about 1 hour generally), so that the firmness of the coated infrared film is easy to solve. The ultra-wide waveband infrared long-wavelength-pass cut-off filter film covers visible light (0.4-0.8 um), near infrared (0.8-3 um), middle infrared (3-5 um) and far infrared (7.5-13.5 um) wavebands, the design thickness of the film system is very thick and reaches more than 12um, and the preparation time of a film coating process is as long as more than 10 hours. Therefore, the ultra-wide waveband infrared long wave pass cut-off filter film with super thickness is a remarkable problem of the existing optical thin film technology in order to solve the problems of depth cut-off and high transmittance in the plating process and the firmness of a product used in a severe environment.
A, ultrasonic substrate cleaning process; B. a koffman ion source assisted evaporation process; C. matching process of optical film tensile stress and compressive stress; D. a special film layer bonding priming process; E. the film firmness and the process difficulty of the ultra-wide waveband infrared long wave pass cut-off filter film are solved by special process technologies such as a high-temperature preheating process and an annealing process.
Drawings
FIG. 1 is a schematic diagram of complete cut-off of light transmission before the middle infrared ray is 5um, and light transmission and high anti-reflection at the far infrared ray is 7.5-13.5 um as much as possible.
Fig. 2A and 2B are graphs showing the results of testing various characteristics of the plating layers of examples 1 to 3.
Detailed Description
In order to make the objects, contents and advantages of the present invention clearer, the following detailed description of the embodiments of the present invention will be made in conjunction with the accompanying drawings and examples.
Example 1
First, the optimized film system meeting the specification requirements of the present invention was designed using the advanced optical thin film design software (TFCalc) in the united states. Coating a film on the surface of a substrate by using optically processed Si, and designing a formula by using a film system:
noodle 1: G/100.0M 140.2H 359.4L 268.6H 489.9L 229.2H 495.3L 207.5H 467.4L 245.0H 508.5L 237.5H 442.9L 192.0H 592.8L 262.6H 699.7L 348.2H 617.3L 352.0H 766.3L 275.6H 812.9L 351.4H 534.2L 445.8H 687.6L 180.9H 473.0L 755.9N 88.1L 64.6H 20.0M/A;
face 2: G/100.0M 69.1H 260.8L 195.7H 284.1L 148.2H 349.4L 207.8H 344.4L 157.9H 288.9L 163.9H 290.8L 183.1H 477.4L 126.6H 309.8L 124.3H 381.7L 31.3H 338.6L 121.2H 254.5L 131.2H 219.8L 105.1H 209.0L 146.2H 132.3L 312.3H 180.1L 73.9H 262.2L 95.9H 247.3L 118.6H 323.5L 755.9N 88.1L 64.6H 20.0M/A;
the optical thickness values for each film were calculated and tabulated in order. Wherein G represents a Si substrate and the refractive index NG3.4, M is the refractive index NMSi film material of 3.4, H is refractive index NHGe film material of 4.2, L is refractive index NL2.2 ZnS film material, N being refractive index NL1.45 YbF3Film material, A is refractive index N A1 air medium, film system reference wavelength lambdac800 nm. The M, H, L, N above are all granular film materials with purity of 99.9%.
The film system consists of a surface 1 and a surface 2, and the physical thickness values of the surface 1 and the surface 2 are calculated according to the formula, namely the surface 1 and the surface 2 are designed:
face 1 (list of theoretical mean values of physical thickness calculated according to film system formula in example 1)
| Film layer number | Layer 1M | Layer 2H | Layer 3L | Layer 4H | Layer 5L | Layer 6H |
| Physical thickness of film (nm) | 100.0 | 140.2 | 389.4 | 268.6 | 489.9 | 229.2 |
| Film layer number | Layer 7L | Layer 8H | Layer 9L | Layer 10H | Layer 11L | Layer 12H |
| Physical thickness of film (nm) | 495.3 | 207.5 | 467.4 | 245.0 | 508.5 | 237.5 |
| Film layer number | Layer 13L | Layer 14H | Layer 15L | Layer 16H | Layer 17L | 18 th layer H |
| Physical thickness of film (nm) | 442.9 | 192.0 | 592.8 | 262.6 | 699.7 | 348.2 |
| Film layer number | Layer 19L | Layer 20H | Layer 21L | Layer 22H | Layer 23L | Layer 24H |
| Physical thickness of film (nm) | 617.3 | 352.0 | 766.3 | 275.6 | 812.9 | 351.4 |
| Film layer number | Layer 25L | Layer 26H | Layer 27L | Layer 28H | Layer L of 29 th | Layer 30N |
| Physical thickness of film(nm) | 534.2 | 445.8 | 687.6 | 180.9 | 473.0 | 755.9 |
| Film layer number | Layer 31L | Layer 32H | Layer 33M | |||
| Film optical thickness (nm) | 88.1 | 64.6 | 20.0 |
Face 2 (list of theoretical mean values of physical thickness calculated according to film system formula in example 1)
Note: only one bit after the decimal point is taken, and the precision is enough to reach the design scheme.
Description of membrane system design formula:
(1) the surface 1 and the surface 2 are lists of theoretical values of physical thickness calculated according to a film system design formula by taking a Si substrate.
(2) In order to ensure the film firmness, the arrangement sequence of the four film materials M, H, L and N in the film system design formula should meet the technical requirements of the processes such as the optical film bonding priming process, the optical film stress matching process and the like. The optical film bonding priming process is to plate a 100M film material (Si) bonded with a Si substrate on a first layer, and can play a key role in the firmness of the whole film. The stress matching process of the optical film layer comprises the following steps: in the aspect of membrane system design and membrane material arrangement, the M, H, L and N four kinds of membrane materials are alternately arranged (stress matching) according to the stress properties of the membrane materials, so that the firmness of the whole membrane layer can be played an important role.
The process of finishing the surface 1 and the surface 2 can be finished by common vacuum coating equipment (such as a box type vacuum coating machine produced by Chengdu modern south light factory), and the main process conditions comprise that:
the special equipment for optical coating comprises: the vacuum coating machine can be used for vacuumizing the vacuum chamber to 10 DEG by using a vacuum pump－2～10－4Pa magnitude order, forming vapor molecules by various film materials which are put into a crucible of a vacuum chamber in advance under the action of an electron gun (generating high-pressure and high-temperature electron beams), and sequentially attaching (growing) the vapor molecules on the surface of the substrate of the optical part according to the design requirement.
And crystal control, namely a quartz crystal oscillation film thickness control system. The crystal control instrument is converted into an optical thickness value according to the principle that the oscillation frequency of a quartz crystal is in direct proportion to the attachment thicknesses (weights) of different coating materials, and is also used for detecting the geometric thickness value of an optical coating in a vacuum chamber.
The ion source can be a koffman type ion source assisted deposition device. During the coating process in the vacuum chamber, the device can generate high-energy ion beams to assist the rapid and high-energy deposition of coating material molecules on the surface of the substrate. It is an important means for improving the firmness of the film layer.
The electron gun is an e-type electron beam evaporation source. Is the most commonly used copper crucible for circular porous evaporation of the membrane material, and the electron beam emitted by a high-pressure filament is irradiated on the membrane material at an angle of 270 degrees to evaporate the membrane material.
The baking can be realized by a heating baking device. The common resistance wire or quartz tube electrifying heating device can be selected for heating the temperature of the vacuum chamber (including the film coating substrate).
The plating process comprises the following steps:
(1) the vacuum chamber is cleaned and filled with film material. After the large cleaning is finished in a vacuum chamber of a film coating machine, four film materials in the film system design formula are mixed: m is Si, H is Ge, N is YbF3L is ZnS, and is a granular crystal film material with the purity of 99.99 percent, Si, Ge and YbF3The three kinds of film materials are sequentially put into a crucible of a rotary electron gun evaporation source, and the ZnS film material is put into a rotary evaporation-resistant evaporation source to be used when the subsequent film coating is evaporated.
(2) Cleaning the plated substrate, putting Si into an ultrasonic cleaning machine which takes ethanol (analytically pure with purity more than or equal to 99.5%) as cleaning fluid, and cleaning for 8 minutes by using a middle gear; cleaning with acetone (analytically pure with purity not less than 99.5%) for 8 min, blowing with high-purity nitrogen, placing in clean vacuum chamber carrying tray frame, closing the door, and vacuumizing.
(3) Baking the substrate while heating, and evacuating to 10 deg.C－3When the pressure is in Pa magnitude, the heating and baking device is started. Heating and baking are carried out from 30 ℃, the temperature is slowly increased, uniform heating and no cracking of the Si substrate can be ensured, the temperature is maintained for 60-90 minutes when the temperature is increased to 160 ℃, and in the whole heating process, a carrying disc provided with the Si substrate uniformly rotates at the speed of 20 revolutions per minute.
(4) Bombarding the substrate before ion source plating: before formal film coating, adjusting the ion source parameters of the auxiliary deposition device of the Koffman type ion source to: the voltage of a screen electrode is 500-550V, the beam current is 70-75 mA, high-purity argon Ar with the purity of four 9 is filled, and the vacuum degree is controlled to be 8.5 multiplied by 10 by using an air filling and vacuum control system－3～9.5×10－3Pa, the ion beam generated by the ion source was allowed to bombard the Si substrate for 30 minutes.
(5) And (3) completing film material evaporation in sequence: starting to coat the film according to the film system design formula from the optical thickness value of each film calculated by the surface 1 and the table. And the physical thickness value of each layer film is shown by crystal control. Meanwhile, the auxiliary deposition device of the Kaufman type ion source is always in the working state, and the parameters are completely the same as the step (4). In the whole evaporation process of the film material, the vacuum degree in the vacuum chamber of the film coating machine is 8.5 multiplied by 10－3～9.5×10－3Pa, "electron gun" evaporation rate is: si 0.3-0.4 nm/s, Ge 0.3-0.4 nm/s, YbF30.8-1.0 nm/s; the evaporation rate of the rotary evaporation resistance is as follows: ZnS is 1-1.5 nm/s. The rotation speed of the Si substrate film carrying disc workpiece is 100-120 revolutions per minute. Keeping the ion source parameters unchanged in the next whole film coating process, allowing the ion beams generated by the ion source to bombard the substrate until the film coating is finished, continuing to bombard the substrate for 7 minutes by the ion beams after the film coating is finished, keeping the temperature constant for 20 minutes, reducing the baking temperature from 160 ℃, closing the high vacuum valve, and stopping the diffusion pump from naturally cooling to the room temperature. In the whole cooling process, the carrying disc of the Si substrate of the device uniformly rotates at the speed of 20 revolutions per minute.
(6) And (4) taking out the Si substrate after the surface 1 is plated, and repeating the plating process steps except for changing the surface 1 in the step (5) into the surface 2 and changing the constant temperature for 20 minutes into 60 minutes.
(7) Annealing treatment: and naturally cooling the Si substrates plated with the surfaces 1 and 2 to room temperature in a vacuum chamber, filling high-purity nitrogen into the vacuum chamber, opening a door, taking out, transferring to a common drying oven, and carrying out annealing treatment. Heating up from 40 ℃, keeping the temperature at 10 ℃ per liter for 10 minutes, heating up to 130 ℃ once, keeping the temperature for 3-5 hours, cooling down, keeping the temperature for 10 minutes after cooling down to 10 ℃, cooling down to 40 ℃ at normal temperature, and taking out for detection for later use.
Example 2
Repeating the method of experimental example 1 according to the physical thickness values of the layers calculated and designed in the surface 2 and the surface 1, and adopting the optimized film system formula and the optical thicknesses of the layers of the surface 2 and the surface 1, in the coating process steps:
(1) the process step (1) in example 1 was repeated;
(2) the process step (2) in example 1 was repeated;
(3) the process step (3) in example 1 was repeated; except that the temperature of the heated baked substrate was finally held constant for 90 minutes.
(4) The process step (4) in example 1 was repeated; before formal coating in parameter aspect, ion source parameters are adjusted to the conditions that the voltage of a screen electrode is fixed to be 550V, the fast flow is fixed to be 75mA, four 9-purity high-purity argon Ar are filled, and the vacuum degree is controlled and fixed to be 8.5 multiplied by 10－ 3Pa, the generated ion beam bombards the Si substrate for 30 minutes.
(5) The process step (5) in example 1 was repeated; parameter aspect: the vacuum degree is fixed at 8.5X 10 during evaporation－3Pa, fixed evaporation rate: si 0.4nm/s, Ge 0.4nm/s, YbF31.0nm/s ZnS 1.5 nm/s. The workpiece rotation rate was fixed at 100 rpm.
Recording the actual physical thickness of each layer of film after the film coating is finished, wherein the actual physical thickness is shown on a surface 2 and a surface 1:
face 2 (Table of actual physical thickness values of film series in example 2)
| Film layer number | Layer 1M | Layer 2H | Layer 3L | Layer 4H | Layer 5L | Layer 6H | |
| Physical thickness of film (nm) | 99.7 | 69.3 | 260.5 | 195.9 | 284.5 | 148.7 | |
| Film layer number | Layer 7L | Layer 8H | Layer 9L | Layer 10H | Layer 11L | Layer 12H | |
| Physical thickness of film (nm) | 349.1 | 207.5 | 344.7 | 157.5 | 288.6 | 163.5 | |
| Film layer number | Layer 13L | Layer 14H | Layer | Layer 16H | 17 th layer L | 18 th layer L | |
| Physical thickness of film (nm) | 290.9 | 183.5 | 477.7 | 126.1 | 309.4 | 124.6 | |
| Film layer number | Layer 19L | Layer 20H | Layer 21L | Layer 22H | Layer 23L | Layer 24L | |
| Physical thickness of film (nm) | 381.9 | 31.0 | 338.9 | 121.6 | 254.3 | 131.0 | |
| Film layer number | Layer 25L | Layer 26H | Layer 27L | Layer 28H | Layer L of 29 th | Layer 30L | |
| Physical thickness of film (nm) | 219.7 | 105.2 | 209.3 | 146.5 | 132.1 | 312.6 | |
| Film layer number | Layer 31L | Layer 32H | Layer 33L | Layer 34H | 35 th layer L | 36 th layer L | |
| Film optical thickness (nm) | 180.0 | 73.7 | 262.5 | 96.1 | 247.0 | 118.5 | |
| Film layer number | Layer 37L | Layer 38N | 39 th layer L | Layer 40H | Layer 41M | ||
| Physical thickness of film (nm) | 325.1 | 756.3 | 88.5 | 64.1 | 20.1 |
Face 1 (Table of actual physical thickness values of film series in example 2)
Note: the values after the bit decimal point are not taken because the precision is sufficient to reach the design.
(6) Annealing treatment: the process step (7) in example 1 was repeated except that after the annealing was carried out to a temperature of 130 ℃ and the temperature was held constant for 5 hours, the temperature was lowered.
Example 3:
repeating the method of experimental example 1 according to the physical thickness values of the layers calculated and designed in the above-mentioned surfaces 1 and 2, and adopting the optimized film system formula of the invention and the optical thicknesses of the layers of the surfaces 1 and 2, in the coating process steps:
(1) the process step (1) in example 1 was repeated;
(2) the process step (2) in example 1 was repeated;
(3) the process step (3) in example 1 was repeated; except that the temperature of the heated baked substrate was finally held constant for 60 minutes.
(4) The process step (4) in example 1 was repeated; before formal coating on parameter aspect, ion source parameters are adjusted to the conditions that the voltage of a screen electrode is fixed to be 500V, the fast flow is fixed to be 70mA, high-purity argon Ar with the purity of four 9 is filled, and the vacuum degree is controlled and fixed to be 9.5 multiplied by 10－3Pa, the generated ion beam bombards the quartz substrate for 30 minutes.
(5) The process step (5) in example 1 was repeated; parameter aspect: the vacuum degree is fixed at 9.5X 10 during evaporation－3Pa, fixed evaporation rate: si 0.3nm/s, Ge 0.3nm/s, YbF30.8nm/s, ZnS 1 nm/s. The workpiece rotation rate was fixed at 120 rpm.
The actual physical thickness of each layer of film recorded after the film coating is finished is seen on the surface 1 and the surface 2:
face 1 (actual physical thickness value list of film series in example 3)
Face 2 (actual physical thickness value list of film series in example 3)
| Film layer number | Layer 1M | Layer 2H | Layer 3L | Layer 4H | Layer 5L | Layer 6H | |
| Physical thickness of film (nm) | 100.1 | 69.5 | 260.9 | 195.4 | 284.7 | 148.5 | |
| Film layer number | Layer 7L | Layer 8H | Layer 9L | Layer 10H | Layer 11L | Layer 12H | |
| Physical thickness of film (nm) | 349.2 | 207.5 | 344.6 | 157.9 | 288.5 | 163.7 | |
| Film layer number | Layer 13L | Layer 14H | Layer | Layer 16H | 17 th layer L | 18 th layer L | |
| Physical thickness of film (nm) | 290.4 | 183.6 | 477.1 | 126.9 | 309.4 | 124.7 | |
| Film layer number | Layer 19L | Layer 20H | Layer 21L | Layer 22H | Layer 23L | Layer 24L | |
| Physical thickness of film (nm) | 381.9 | 31.6 | 338.1 | 121.7 | 254.3 | 131.6 | |
| Film layer number | Layer 25L | Layer 26H | Layer 27L | Layer 28H | Layer L of 29 th | Layer 30L | |
| Physical thickness of film (nm) | 219.7 | 105.4 | 209.3 | 146.5 | 132.1 | 312.2 | |
| Film layer number | Layer 31L | Layer 32H | Layer 33L | Layer 34H | 35 th layer L | 36 th layer L | |
| Film optical thickness (nm) | 180.5 | 74.2 | 262.5 | 95.7 | 247.1 | 118.9 | |
| Film layer number | Layer 37L | Layer 38N | 39 th layer L | Layer 40H | Layer 41M | ||
| Physical thickness of film (nm) | 325.1 | 755.7 | 88.0 | 64.1 | 20.5 |
Note: the values after the bit decimal point are not taken because the precision is sufficient to reach the design.
(6) Annealing treatment: the process step (7) in example 1 was repeated except that after the annealing was carried out to a temperature of 130 ℃ and the temperature was held constant for 3 hours, the temperature was lowered.
The test results of various characteristic indexes of the plating film layer of the embodiment are as follows: (FIG. 2A and FIG. 2B)
(1) The transmittance of the Si substrate coated with the ultra-wide waveband infrared long wave pass cut-off filter film is as follows:
visible light, near infrared, mid-infrared: 0.4-5.0 um average transmittance T is 0.1% (T is less than or equal to 0.5%);
far infrared band: 7.5-13.5 um, and the average transmittance T is 85.3% (T is more than or equal to 70%);
(2) film firmness and laser damage resistance test: all meet the requirements specified by the national standard of optical films and pass the aviation standard + 70-55 ℃ high and low temperature impact test.
(3) The moisture resistance of the film layer is as follows: the requirements of national standards of optical films are met, and multiple experiments such as field use and water immersion prove that the Si cut-off filter with the ultra-wide waveband infrared long-wave pass cut-off filter film prepared by the embodiment has a very good moisture-proof protection effect and can be used for a long time in air flight and in severe environment in the field.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of an ultra-wide waveband infrared long wave pass cut-off filter film is characterized by comprising the following steps:
(1) si is used as a substrate, and the film system formula of the films plated on the two side surfaces is as follows:
face 1G/100.0M 140.2H 359.4L 268.6H 489.9L 229.2H 495.3L 207.5H 467.4L 245.0H 508.5L 237.5H 442.9L 192.0H 592.8L 262.6H 699.7L 348.2H 617.3L 352.0H 766.3L 275.6H 812.9L 351.4H 534.2L 445.8H 687.6L 180.9H 473.0L 755.9N 88.1L 64.6H 20.0M/A;
face 2G/100.0M 69.1H 260.8L 195.7H 284.1L 148.2H 349.4L 207.8H 344.4L 157.9H 288.9L 163.9H 290.8L 183.1H 477.4L 126.6H 309.8L 124.3H 381.7L 31.3H 338.6L 121.2H 254.5L 131.2H 219.8L 105.1H 209.0L 146.2H 132.3L 312.3H 180.1L 73.9H 262.2L 95.9H 247.3L 118.6H 323.5L 755.9N 88.1L 64.6H 20.0M/A;
calculating the physical thickness value of each layer of film and tabulating in sequence; wherein G is Si substrate, M is Si film material, H is Ge film material, L is ZnS film material, N is YbF3Film material, A is refractive index NA1 air medium, film system reference wavelength lambdacSequentially putting the M, H, N film materials into an electron gun evaporation source crucible of a vacuum chamber of a film coating machine for later use, and putting the L film materials into a rotary evaporation-resistant evaporation source;
(2) in the ultrasonic cleaning process of the coated substrate, cleaning the coated substrate with cleaning solution, drying the coated substrate by blowing, and placing the coated substrate into a vacuum chamber for vacuumizing and waiting to be coated;
(3) heating and baking the substrate, and gradually heating and baking at the temperature of 30-160 ℃ in a vacuum environment;
(4) in the optical film bonding priming process and the stress matching process, Si, Ge and YbF are mixed according to the optical thickness value of each film calculated by the film system design formula and the table sequence3Sequentially putting the three types of film materials into a rotary electron gun evaporation source crucible, putting the ZnS film material into a rotary evaporation resistance source, and then finishing film coating by using an optical vacuum film coating machine according to the formula list sequence and the thickness value in the step (1);
(5) in the ion source auxiliary evaporation process, an ion source is used for bombarding a substrate before and in the film coating process; the ion beam generated by the ion beam bombards the substrate until the film coating is finished;
(6) in the high-low temperature annealing process, the coated ball cover is naturally cooled to room temperature in a vacuum chamber and then is annealed.
2. The method for preparing an infrared long-wave pass cut-off filter film of an ultra-wide waveband as claimed in claim 1, wherein the method comprises the following steps: the ultrasonic cleaning process of the coated Si substrate comprises the steps of putting the substrate into an ultrasonic cleaning machine containing ethanol as cleaning liquid, selecting a middle gear for cleaning for 10 minutes, then cleaning with acetone cleaning liquid for 10 minutes, drying with high-purity nitrogen, putting the substrate into a clean vacuum chamber carrier plate frame, closing a door, vacuumizing and waiting for plating.
3. The method for preparing an infrared long-wave pass cut-off filter film of an ultra-wide waveband as claimed in claim 1, wherein the method comprises the following steps: the optical film layer bonding and priming process is characterized in that 1.0M film material bonded with a Si substrate is plated on a first layer.
4. The method for preparing an infrared long-wave pass cut-off filter film of an ultra-wide waveband as claimed in claim 1, wherein the method comprises the following steps: the stress matching process of the optical film layer is characterized in that M, H, L, N four film materials are alternately arranged according to the stress properties detected by the film materials.
5. The method for preparing an infrared long-wave pass cut-off filter film of an ultra-wide waveband as claimed in claim 1, wherein the method comprises the following steps: when the substrate is baked at a warm temperature, the vacuum is pumped to 10－3When the pressure is in Pa magnitude order, baking is carried out from 30 ℃, the temperature is slowly raised to 160 ℃, the temperature is kept for 60 minutes, and the workpiece rotates for 20 revolutions per minute.
6. The method for preparing an infrared long-wave pass cut-off filter film of an ultra-wide waveband as claimed in claim 1, wherein the method comprises the following steps: the ion source auxiliary evaporation process is characterized in that ion source parameters are adjusted to: the voltage of the screen electrode is 500V, the beam current is 70mA, high-purity argon with the purity of four 9 is filled, and the vacuum degree is controlled to be 1.0 multiplied by 10－2Pa, bombarding the dome base with the generated ion beam for 20 minutes.
7. The method for preparing an infrared long-wave pass cut-off filter film of an ultra-wide waveband as claimed in claim 1, wherein the method comprises the following steps: the high-low temperature annealing process is that the Si substrate after film plating is naturally cooled to room temperature and then transferred to a drying oven from a vacuum chamber for annealing treatment: heating up from 40 ℃, keeping the temperature at 10 ℃ per liter for 10 minutes, heating up to 130 ℃ once, keeping the temperature for 8-10 hours, cooling down, keeping the temperature at 10 ℃ for 10 minutes each time, cooling down to 30 ℃ at normal temperature, taking out and detecting for later use.
8. The method for preparing an infrared long-wave pass cut-off filter film of an ultra-wide waveband as claimed in claim 1, wherein the method comprises the following steps: the film system is composed of 45 film from inside to outside, and the physical thickness value of each film is calculated and designed according to the formula in the step (1).
9. The method for preparing an infrared long-wave pass cut-off filter film of an ultra-wide waveband as claimed in claim 8, wherein: the physical thickness values of the films are shown in the following table:
noodle 1:
Face 2:
10. the use of the method of any of claims 1-9 in the field of optical thin film coating technology.
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| CN114047571B (en) * | 2021-11-23 | 2023-09-19 | 中国航空工业集团公司洛阳电光设备研究所 | Infrared short wave cut-off filter |
| CN114325911A (en) * | 2021-12-31 | 2022-04-12 | 苏州厚朴传感科技有限公司 | Intermediate infrared double-color optical filter and preparation method thereof |
| CN114325911B (en) * | 2021-12-31 | 2024-01-30 | 苏州厚朴传感科技有限公司 | Middle-infrared double-color filter and preparation method thereof |
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| CN112813391B (en) | 2022-08-12 |
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