CN114460677A - Infrared filter for MEMS black body packaging and preparation method thereof - Google Patents
Infrared filter for MEMS black body packaging and preparation method thereof Download PDFInfo
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- CN114460677A CN114460677A CN202210381588.4A CN202210381588A CN114460677A CN 114460677 A CN114460677 A CN 114460677A CN 202210381588 A CN202210381588 A CN 202210381588A CN 114460677 A CN114460677 A CN 114460677A
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- blackbody
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- 238000004806 packaging method and process Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 80
- 239000000758 substrate Substances 0.000 claims abstract description 58
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 23
- 238000004857 zone melting Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 34
- 238000001704 evaporation Methods 0.000 claims description 22
- 239000007888 film coating Substances 0.000 claims description 22
- 238000009501 film coating Methods 0.000 claims description 22
- 230000003287 optical effect Effects 0.000 claims description 15
- 238000007747 plating Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 14
- 239000010703 silicon Substances 0.000 claims description 14
- 229910009520 YbF3 Inorganic materials 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 9
- 229910052732 germanium Inorganic materials 0.000 claims description 9
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 238000005566 electron beam evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 239000012459 cleaning agent Substances 0.000 claims description 7
- 238000005137 deposition process Methods 0.000 claims description 7
- 238000002834 transmittance Methods 0.000 claims description 7
- 238000000411 transmission spectrum Methods 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 238000001745 non-dispersive infrared spectroscopy Methods 0.000 abstract description 6
- 239000010410 layer Substances 0.000 description 52
- 229910052984 zinc sulfide Inorganic materials 0.000 description 20
- 235000012431 wafers Nutrition 0.000 description 10
- 230000003595 spectral effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- 239000005083 Zinc sulfide Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 239000002210 silicon-based material Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 1
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 1
- 229910001632 barium fluoride Inorganic materials 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- 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
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
- C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Inorganic Chemistry (AREA)
- Optical Filters (AREA)
Abstract
The invention relates to an infrared filter for MEMS black body packaging and a preparation method thereof, wherein the infrared filter comprises a substrate material and antireflection film series structures, and the antireflection film series structures are arranged on two sides of the substrate material; the antireflection film system structure is as follows: sub/0.26M1.34H0.92M1.65H1.33M1.27H1.87M0.67H3.3M 1.62.62 1.62M1.27L1.06M3.44L0.44M/Air, the infrared filter for the MEMS black body packaging takes high-resistance zone-melting monocrystalline silicon as a substrate, the transmissivity T is more than 70% within the wavelength range of 2.0-15 mu m, wherein the transmissivity T is more than 85% within the wavelength range of 2.5-12 mu m, the infrared filter can meet the requirements of an NDIR infrared gas sensor, and the market blank is filled.
Description
Technical Field
The invention relates to the field of blackbody light sources, in particular to the technical field of infrared filters, and specifically relates to an infrared filter for MEMS blackbody packaging and a preparation method thereof.
Background
In NDIR infrared gas sensors, halogen bulbs or MEMS blackbodies are typically used as the infrared light source. As shown in fig. 1a, since the halogen bulb emission spectrum can only cover visible light to the mid-infrared 6.0 μm, the application in the mid-long infrared band is limited. Such as SF6Infrared gas detectors for gases typically use a 10.56 μm wavelength as the operating wavelength, where halogen bulbs cannot be used as the light source for the sensor. The MEMS blackbody source has an ideal radiation spectrum close to a blackbody, and can cover the medium and long wavelength bands well, as shown in fig. 1b, which is a radiation spectrum curve of the blackbody source. Generally, in order TO ensure the working stability and the service life of the MEMS black body light source, the MEMS black body chip needs TO be packaged by using a TO tube cap, and meanwhile, a 2-15 mu m waveband high-transmission optical filter is used as a window piece. In the wave band range, barium fluoride or calcium fluoride crystals, optical filters with silicon, germanium and zinc selenide crystals as substrates and the like can be selected. However, the performance and economic benefits of several schemes are comprehensively considered, and the filter scheme using single crystal silicon as a substrate has the most cost performance. But researches find that no filter designed for the MEMS black body light source exists in the domestic market at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an infrared filter for the blackbody packaging of MEMS and a preparation method thereof.
In order to achieve the purpose, the infrared filter for the MEMS blackbody packaging comprises a substrate material and antireflection film series structures, wherein the antireflection film series structures are arranged on two sides of the substrate material;
the antireflection film system structure is as follows:
sub/0.26 M1.34H0.92M1.65H1.33M1.27H1.87M0.67H3.3M1.62M1.27L1.06M3.44L0.44M/Air, where Sub represents the substrate material, Air represents Air, H is a Ge film layer of quarter-wavelength optical thickness, M is a ZnS film layer of quarter-wavelength optical thickness, and L is YbF of quarter-wavelength optical thickness3The number in the film system structure is the film thickness coefficient, and the central wavelength is 1000 nm.
Preferably, the 9 th layer and the 10 th layer of the antireflection film series structure are located at different light control points, and the YbF is3Both sides of the film layer are ZnS film layers.
The infrared filter for the MEMS black body packaging has the following spectral characteristics: the transmissivity is more than 70% in the range of 2-15 mu m of the infrared transmission waveband, and the transmissivity is more than 85% in the range of 2.5-12 mu m of the high-transmissivity waveband.
Preferably, the substrate material is optical-grade high-resistance zone melting monocrystalline silicon or monocrystalline germanium material, but monocrystalline germanium is expensive, and monocrystalline silicon material is preferentially used in production.
Preferably, the high resistance zone-melting monocrystalline silicon requires: the resistivity is more than or equal to 10000 omega cm, the thickness is 0.4-0.5 mm, and the transmissivity at the wavelength of 9 mu m is more than 51%.
The preparation method of the infrared filter for the MEMS black body packaging is mainly characterized by comprising the following steps of:
(1) cleaning and drying the substrate material with two polished surfaces, then loading the substrate material into a special fixture, placing the substrate material on a DOME station of a vacuum chamber, and vacuumizing the vacuum chamber;
(2) baking the substrate material at 190-210 ℃, and keeping the temperature constant;
(3) bombarding the substrate material by using Hall ion source ions for 6-10 minutes, wherein the gas flow is 15-30 sccm;
(4) respectively plating antireflection film series structures on two surfaces of the base material layer by layer according to the film layer thickness required by a preset film series structure;
(5) and after the plating is finished, breaking the cavity when the baking temperature is reduced to 30 ℃, and taking out the infrared filter.
Preferably, the cleaning process of the substrate material in the step (1) is as follows: firstly, using a cleaning agent to carry out ultrasonic cleaning for 3-5 minutes, then putting a silicon wafer into pure water to carry out ultrasonic cleaning for 2-3 minutes, finally spraying the pure water for 1 minute, then blowing the pure water to dry by nitrogen, wherein the solvent ratio of the cleaning agent is ammonia water: hydrogen peroxide: pure water 5:15: 80.
preferably, the vacuum degree in the step (1) is 5 × 10-4Pa～8×10-4Pa。
Preferably, the constant temperature time in the step (2) is 100 to 120 minutes.
Preferably, the ion source in the step (3) is high-purity oxygen, and the anode voltage is 150-200V.
Preferably, the plating process in the step (4) specifically includes:
(4.1) performing first-side plating, evaporating the Ge film material by adopting an electron beam evaporation process, and evaporating the ZnS film material and YbF by adopting a resistance evaporation process3Coating the anti-reflection film system structure on one surface of the base material layer by layer according to the required film thickness;
wherein the film coating rate of the Ge film is 0.5nm/s, the film coating rate of the ZnS film is 1.0nm/s, and YbF3The film coating rate of the film is 1.0nm/s, and the thickness and rate of the film are controlled by combining indirect light control and crystal control in the deposition process;
(4.2) turning over the substrate material coated with the first surface and loading the substrate material into a jig, evaporating Ge film material by electron beam evaporation process, and evaporating ZnS film material and YbF by resistance evaporation process3Coating the other surface of the substrate material with an antireflection film system structure layer by layer according to the required film layer thickness;
wherein the film coating rate of the Ge film is 0.5nm/s, the film coating rate of the ZnS film is 1.0nm/s, and YbF3The film coating speed of the film is 1.0nm/s, and the thickness and speed of the film layer are controlled by combining indirect light control and crystal control in the deposition processAnd (4) rate.
Preferably, the step (5) further comprises the following steps:
(6) the transmission spectrum at normal incidence of the filter was measured using a fourier transform infrared spectrometer.
Preferably, the step (6) further comprises the following steps:
(7) scribing with a scriber and a resin blade, wherein the main shaft rotation speed of the scriber is as follows: 30000rpm, a feed speed of 20mm/s, and a size of the filter after dicing of 5X 5 mm.
Preferably, the step (7) further comprises the following steps:
(8) the filter is encapsulated on the cap window using a dispenser.
Preferably, the substrate material in the step (1) is a monocrystalline silicon wafer, the thickness is 0.4-0.5 mm, and the diameter is 100 mm.
According to the requirements of an MEMS black body light source on an NDIR infrared gas sensor, the invention designs and prepares the infrared filter which takes high-resistance zone-melting monocrystalline silicon as a substrate and has the transmissivity T of more than 70 percent within the wavelength range of 2.0-15 mu m, wherein the transmissivity T of more than 85 percent within the wavelength range of 2.5-12 mu m, can meet the requirements of the NDIR infrared gas sensor and fill the market blank.
Drawings
FIG. 1a is a diagram of an infrared light source emission spectrum of a halogen bulb.
FIG. 1b is a graph of the radiation spectrum of a MEMS blackbody light source.
Fig. 2 is a schematic structural diagram of an infrared filter for MEMS blackbody packaging according to the present invention.
FIG. 3 is a graph of transmission spectra for Czochralski single crystal silicon and float-zone single crystal silicon.
Fig. 4 is a transmittance spectrum of an infrared filter for MEMS black body packaging of the present invention.
FIG. 5 is a block diagram of a MEMS blackbody light source of the present invention.
Reference numerals:
1 MEMS black body light source chip
2 Infrared filter
3 base
4 metal pipe cap
5 stitches.
Detailed Description
In order to more clearly describe the technical contents of the present invention, the following further description is given in conjunction with specific embodiments.
As shown in fig. 2, the infrared filter 2 for MEMS blackbody packaging of the present invention includes a substrate material and an antireflection film structure, wherein the antireflection film structure is disposed on two sides of the substrate material;
the antireflection film system structure is as follows:
sub/0.26 M1.34H0.92M1.65H1.33M1.27H1.87M0.67H3.3M1.62M1.27L1.06M3.44L0.44M/Air, where Sub represents the substrate material, Air represents Air, H is a Ge film layer of quarter-wavelength optical thickness, M is a ZnS film layer of quarter-wavelength optical thickness, and L is YbF of quarter-wavelength optical thickness3The number in the film system structure is the film thickness coefficient, and the central wavelength is 1000 nm.
In a preferred embodiment of the present invention, the 9 th layer and the 10 th layer of the antireflection film structure are located at different photo-control points, and the YbF is3Both sides of the film layer are ZnS film layers.
As shown in fig. 4, the infrared filter 2 for MEMS black body encapsulation has the following spectral characteristics: the transmissivity is more than 70% in the range of 2-15 mu m of the infrared transmission waveband, and the transmissivity is more than 85% in the range of 2.5-12 mu m of the high-transmissivity waveband.
In a preferred embodiment of the present invention, the substrate material is optical-grade high-resistance zone-melting monocrystalline silicon or monocrystalline germanium material, but monocrystalline germanium is expensive, and monocrystalline silicon material is preferentially used in production.
In a preferred embodiment of the present invention, the high resistance float-zone silicon single crystal requires: the resistivity is more than or equal to 10000 omega cm, the thickness is 0.4-0.5 mm, and the transmissivity at the wavelength of 9 mu m is more than 51%.
The invention discloses a preparation method of an infrared filter 2 for MEMS black body packaging, which comprises the following steps:
(1) cleaning and drying the substrate material with two polished surfaces, then loading the substrate material into a special fixture, placing the substrate material on a DOME station of a vacuum chamber, and vacuumizing the vacuum chamber;
(2) baking the substrate material at 190-210 ℃, and keeping the temperature constant;
(3) bombarding the substrate material by using Hall ion source ions for 6-10 minutes, wherein the gas flow is 15-30 sccm;
(4) respectively plating antireflection film series structures on two surfaces of the base material layer by layer according to the film layer thickness required by a preset film series structure;
(5) and after the plating is finished, breaking the air when the baking temperature is reduced to 30 ℃, and taking out the infrared filter 2.
As a preferred embodiment of the present invention, the cleaning process of the substrate material in step (1) is: firstly, using a cleaning agent to carry out ultrasonic cleaning for 3-5 minutes, then putting a silicon wafer into pure water to carry out ultrasonic cleaning for 2-3 minutes, finally spraying the pure water for 1 minute, then blowing the pure water to dry by nitrogen, wherein the solvent ratio of the cleaning agent is ammonia water: hydrogen peroxide: pure water 5:15: 80.
as a preferred embodiment of the present invention, the degree of vacuum in the step (1) is 5X 10-4Pa～8×10-4Pa。
In a preferred embodiment of the present invention, the constant temperature time in the step (2) is 100 to 120 minutes.
In a preferred embodiment of the present invention, in the step (3), the ion source is high-purity oxygen, and the anode voltage is 150 to 200V.
As a preferred embodiment of the present invention, the plating process in the step (4) specifically includes:
(4.1) performing first-side plating, evaporating the Ge film material by adopting an electron beam evaporation process, and evaporating the ZnS film material and YbF by adopting a resistance evaporation process3Coating materials, namely plating an anti-reflection film system structure on one surface of the base material layer by layer according to the required film layer thickness;
wherein the Ge film has a film-coating rate of 0.5nm/s, the ZnS film has a film-coating rate of 1.0nm/s, and YbF3The film coating rate of the film is 1.0nm/s, and the thickness and rate of the film are controlled by combining indirect light control and crystal control in the deposition process;
(4.2) turning over the substrate material coated with the first surface and loading the substrate material into a jig, evaporating Ge film material by electron beam evaporation process, and evaporating ZnS film material and YbF by resistance evaporation process3Coating the other surface of the substrate material with an antireflection film system structure layer by layer according to the required film layer thickness;
wherein the film coating rate of the Ge film is 0.5nm/s, the film coating rate of the ZnS film is 1.0nm/s, and YbF3The film coating speed of the film is 1.0nm/s, and the thickness and speed of the film are controlled by combining indirect light control and crystal control in the deposition process.
As a preferred embodiment of the present invention, the step (5) further comprises the following steps:
(6) the transmission spectrum at normal incidence of the filter was measured using a fourier transform infrared spectrometer.
As a preferred embodiment of the present invention, the step (6) further comprises the following steps:
(7) scribing with a scriber and a resin blade, wherein the main shaft rotation speed of the scriber is as follows: 30000rpm, a feed speed of 20mm/s, and a size of the filter after dicing of 5X 5 mm.
As a preferred embodiment of the present invention, the step (7) further comprises the following steps:
(8) the filter is encapsulated on the cap window using a dispenser.
As a preferred embodiment of the invention, the substrate material in the step (1) is a monocrystalline silicon wafer, the thickness is 0.4-0.5 mm, and the diameter is 100 mm.
In a preferred embodiment, as shown in fig. 2, the infrared filter 2 for MEMS black body encapsulation of the present invention includes a substrate material and an anti-reflection film structure, wherein the anti-reflection film structure is disposed on two sides of the substrate material;
the antireflection film system structure is as follows:
Sub/0.26M1.34H0.92M1.65H1.33M1.27H1.87M0.67H3.3M1.62M1.27L1.06M3.44L0.44M [ a/Air ] wherein, Sub represents a base material, Air represents Air, H is a Ge film layer of a quarter-wavelength optical thickness, M is a ZnS film layer of a quarter-wavelength optical thickness, and L is YbF of a quarter-wavelength optical thickness3The number in the film system structure is the film thickness coefficient, and the design wavelength is 1000 nm.
The invention does not allow YbF when using light control to monitor the film thickness3Film layer as first film layer, YbF3The two sides of the film layer are both zinc sulfide film layers, which is beneficial to improving the bonding force of the film layer. Wherein the 9 th layer and the 10 th layer are both zinc sulfide film layers, but the two layers are positioned on two different light control points, so that YbF is aimed at3The film layer is not used as the first film layer of the light control point.
The film system structure has YbF3The two sides of the film layer are both zinc sulfide film layers, the purpose is to enhance the binding force of the film layer and simultaneously prevent YbF3The film layer is exposed on the outermost side (air side). The experiment proves that when Ge-YbF appears3Interface and YbF3The stripping phenomenon is easy to occur at the Air interface, which is not beneficial to the scribing process of the optical filter at the later stage.
The infrared filter 2 for the MEMS black body packaging has the following spectral characteristics: the transmissivity is more than 70% in the range of 2-15 mu m of the infrared transmission waveband, and the transmissivity is more than 85% in the range of 2.5-12 mu m of the high-transmissivity waveband.
As shown in FIG. 3, in which the broken line represents the transmittance curve of Czochralski silicon (CZ-Si) and the solid line represents the transmittance curve of float-zone silicon (FZ-Si), both silicon wafers have the same thickness, it can be seen from FIG. 3 that Czochralski silicon has a large depression at 9000nm, i.e., a significant absorption peak at 9 μm, whereas float-zone silicon does not have a significant absorption peak, so that the substrate should preferably be float-zone silicon in both silicon wafers.
In a preferred embodiment, the substrate material is optical-grade high-resistance zone-melting monocrystalline silicon or monocrystalline germanium material, but monocrystalline germanium is expensive, and monocrystalline silicon material is preferentially used in production.
In a preferred embodiment, the high resistance zone-melting monocrystalline silicon requires: the resistivity is more than or equal to 10000 omega cm, the thickness is 0.4mm, and the transmissivity at the wavelength of 9 mu m is more than 51 percent.
Fig. 4 shows a transmittance spectrogram of the infrared filter 2 for MEMS black body encapsulation according to the present invention, which embodies the spectral characteristics of the infrared filter 2, and shows that the infrared filter 2 satisfies the various indexes of the present invention, i.e. fig. 4 shows that the transmittance T of the infrared filter 2 according to the present invention is greater than 70% in the wavelength range of 2000-15000 nm, wherein the transmittance T is greater than 85% in the wavelength range of 2500-12000 nm, so that the infrared filter 2 according to the present invention can effectively meet the requirement of detecting an MEMS black body light source.
Specifically, when the substrate material is made of a monocrystalline silicon wafer, the antireflection film structure is Si/0.26 M1.34H0.92M1.65H1.33M1.27H1.87M0.67H3.3M1.62M1.27L1.06M3.44L0.44M/Air, and similarly, when the substrate material is made of a monocrystalline germanium material, the antireflection film structure is Ge/0.26 M1.34H0.92M1.65H1.33M1.27H1.87M0.67H3.3M1.62M1.27L1.06M3.44L0.44M/Air.
The infrared filter 2 for the MEMS black body package may be prepared by the following preparation method:
(1) cleaning a monocrystalline silicon wafer with the thickness of 0.4mm and the diameter of 100mm, and polished on two sides: firstly, ultrasonically cleaning for 3-5 minutes by using a cleaning agent (the solvent ratio is ammonia water: hydrogen peroxide: pure water =5:15: 80), then ultrasonically cleaning for 2-3 minutes by putting the silicon wafer into pure water, finally spraying for 1 minute by using the pure water, and then drying by using nitrogen;
(2) putting the cleaned and dried silicon wafer into a special fixture, putting the fixture on a DOME station of a vacuum chamber, and vacuumizing to 5-8 multiplied by 10-4Pa；
(3) Baking the substrate at 200 +/-10 ℃ and keeping the constant temperature for 100-120 minutes;
(4) the substrate is bombarded by Hall ion source ions for about 6-10 minutes, the ion source uses high-purity oxygen (99.99%), anode voltage is 150-200V, and gas flow is 15-30 sccm;
(5) plating the first surface, evaporating Ge film material by electron beam evaporation process, and evaporating ZnS film material and YbF by resistance evaporation process3Coating the film material layer by layer according to the thickness of the film layer as shown in the table 1, wherein the coating rate of the Ge film is 0.5nm/s, and the coating rate of the ZnS film isThe ratio is 1.0nm/s, YbF3The film coating speed of the film is 1.0nm/s, and the thickness and speed of the film are controlled by combining indirect light control and crystal control in the deposition process.
(6) Coating the second surface, turning over the substrate coated with the first surface, loading into a fixture, and coating layer by layer according to the requirement of the film system structure shown in Table 1, wherein the Ge film material is evaporated by electron beam evaporation process with a film coating rate of 0.5nm/s, and ZnS film material and YbF are evaporated by resistance evaporation process3The film coating rate of the film material and the ZnS film is 1.0nm/s, YbF3The film coating speed of the film is 1.0nm/s, and the thickness and speed of the film are controlled by combining indirect light control and crystal control in the deposition process.
TABLE 1 film layer Structure
(7) And after the plating is finished, breaking the blank and taking the workpiece when the baking temperature is reduced to the room temperature.
(8) The transmission spectrum at normal incidence of the filter was measured using a fourier transform infrared spectrometer.
(9) Dicing was performed using a dicing saw and a resin blade (spindle rotation speed: 30000rpm, feed speed 20 mm/s), and the size of the filter after dicing was 5X 5 mm.
(10) The filter is encapsulated on the cap window using a dispenser.
Fig. 5 is a structural diagram of an infrared light source using the MEMS blackbody light source, in which the MEMS blackbody light source chip 1 is fixed on the base 3, and the pin 5 is used to supply power to the light source. The metal cap 4 has a conical inner structure, one end with a larger opening is packaged with the infrared filter 2, and the other end is sealed with the base 3. After the MEMS black body light source chip 1 emits infrared light, part of the light is directly emitted through the infrared filter, and the other part of the light is reflected by the conical surface and then emitted through the infrared filter. By the structure shown in FIG. 5, the MEMS black body light source can be used as a light source of an infrared gas sensor, and the infrared filter disclosed by the invention can well meet the spectral characteristics of the MEMS black body light source.
According to the requirements of an MEMS black body light source on an NDIR infrared gas sensor, the invention designs and prepares the infrared filter which takes high-resistance zone-melting monocrystalline silicon as a substrate and has the transmissivity T of more than 70 percent within the wavelength range of 2.0-15 mu m, wherein the transmissivity T of more than 85 percent within the wavelength range of 2.5-12 mu m, can meet the requirements of the NDIR infrared gas sensor and fill the market blank.
In this specification, the invention has been described with reference to specific embodiments thereof. It will, however, be evident that various modifications and changes may be made thereto without departing from the broader spirit and scope of the invention. The description is thus to be regarded as illustrative instead of limiting.
Claims (15)
1. The infrared filter for the MEMS blackbody packaging is characterized by comprising a substrate material and antireflection film series structures, wherein the antireflection film series structures are arranged on two sides of the substrate material;
the antireflection film system structure is as follows:
sub/0.26 M1.34H0.92M1.65H1.33M1.27H1.87M0.67H3.3M1.62M1.27L1.06M3.44L0.44M/Air, where Sub represents the substrate material, Air represents Air, H is a Ge film layer of quarter-wavelength optical thickness, M is a ZnS film layer of quarter-wavelength optical thickness, and L is YbF of quarter-wavelength optical thickness3The number in the film system structure is the film thickness coefficient, and the central wavelength is 1000 nm.
2. The infrared filter for the blackbody packaging of the MEMS as claimed in claim 1, wherein the 9 th layer and the 10 th layer of the antireflection film structure are located at different photo-control points, and the YbF is3Both sides of the film layer are ZnS film layers.
3. The infrared filter for the blackbody packaging of the MEMS as claimed in claim 1, wherein the transmittance of the infrared filter in the infrared transmission band of 2 to 15 μm is greater than 70%, and the transmittance in the high transmission band of 2.5 to 12 μm is greater than 85%.
4. The infrared filter for the blackbody packaging of the MEMS according to claim 1, wherein the substrate material is optical-grade high-resistance zone-melting single crystal silicon or single crystal germanium material.
5. The infrared filter for the blackbody packaging of the MEMS according to claim 4, wherein the high-resistance zone-melting monocrystalline silicon requires: the resistivity is more than or equal to 10000 omega cm, the thickness is 0.4-0.5 mm, and the transmissivity at the wavelength of 9 mu m is more than 51%.
6. A method for manufacturing the infrared filter for the blackbody packaging of the MEMS according to any one of claims 1 to 5, wherein the method comprises the following steps:
(1) cleaning and drying the substrate material with two polished surfaces, then loading the substrate material into a special fixture, placing the substrate material on a DOME station of a vacuum chamber, and vacuumizing the vacuum chamber;
(2) baking the substrate material at 190-210 ℃, and keeping the temperature constant;
(3) bombarding the substrate material by using Hall ion source ions for 6-10 minutes, wherein the gas flow is 15-30 sccm;
(4) respectively plating antireflection film series structures on two surfaces of the base material layer by layer according to the film layer thickness required by a preset film series structure;
(5) and after the plating is finished, breaking the cavity when the baking temperature is reduced to 30 ℃, and taking out the infrared filter.
7. The method for manufacturing an infrared filter for blackbody packaging of MEMS according to claim 6, wherein the cleaning process of the substrate material in the step (1) is as follows: firstly, using a cleaning agent to carry out ultrasonic cleaning for 3-5 minutes, then putting a silicon wafer into pure water to carry out ultrasonic cleaning for 2-3 minutes, finally spraying the pure water for 1 minute, then blowing the pure water to dry by nitrogen, wherein the solvent ratio of the cleaning agent is ammonia water: hydrogen peroxide: pure water 5:15: 80.
8. the method for preparing an infrared filter for blackbody packaging of MEMS according to claim 6, wherein the degree of vacuum in step (1) is 5 x 10-4Pa～8×10-4Pa。
9. The method for preparing the infrared filter for the blackbody packaging of the MEMS according to claim 6, wherein the constant temperature time in the step (2) is 100-120 minutes.
10. The method for preparing the infrared filter for the blackbody packaging of the MEMS according to claim 6, wherein in the step (3), the ion source is high-purity oxygen, and the anode voltage is 150-200V.
11. The method for manufacturing the infrared filter for the blackbody packaging of the MEMS according to claim 6, wherein the plating process in the step (4) specifically comprises:
(4.1) performing first-side plating, evaporating the Ge film material by adopting an electron beam evaporation process, and evaporating the ZnS film material and YbF by adopting a resistance evaporation process3Coating the anti-reflection film system structure on one surface of the base material layer by layer according to the required film thickness;
wherein the film coating rate of the Ge film is 0.5nm/s, the film coating rate of the ZnS film is 1.0nm/s, and YbF3The film coating rate of the film is 1.0nm/s, and the thickness and rate of the film are controlled by combining indirect light control and crystal control in the deposition process;
(4.2) turning over the substrate material coated with the first surface and loading the substrate material into a jig, evaporating Ge film material by electron beam evaporation process, and evaporating ZnS film material and YbF by resistance evaporation process3Coating the other surface of the substrate material with an antireflection film system structure layer by layer according to the required film layer thickness;
wherein the film coating rate of the Ge film is 0.5nm/s, the film coating rate of the ZnS film is 1.0nm/s, and YbF3The film coating speed of the film is 1.0nm/s, and the thickness and speed of the film are controlled by combining indirect light control and crystal control in the deposition process.
12. The method for preparing an infrared filter for the blackbody packaging of the MEMS according to claim 6, wherein the step (5) is followed by the following steps:
(6) the transmission spectrum at normal incidence of the filter was measured using a fourier transform infrared spectrometer.
13. The method for manufacturing an infrared filter for MEMS black body package as claimed in claim 12, wherein the step (6) is further followed by the steps of:
(7) and (3) scribing by using a scribing machine and a resin blade, wherein the rotating speed of a main shaft of the scribing machine is 30000rpm, the feed speed is 20mm/s, and the size of the scribed filter is 5 multiplied by 5 mm.
14. The method for manufacturing an infrared filter for the blackbody packaging of the MEMS according to claim 13, wherein the step (7) is followed by the steps of:
(8) the filter is encapsulated on the cap window using a dispenser.
15. The method for manufacturing an infrared filter for the blackbody packaging of an MEMS according to claim 6, wherein the substrate material in the step (1) is a monocrystalline silicon wafer, the thickness of the monocrystalline silicon wafer is 0.4-0.5 mm, and the diameter of the monocrystalline silicon wafer is 100 mm.
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