CN115469390A - Infrared filter for detecting diethyl carbonate gas and preparation method thereof - Google Patents

Infrared filter for detecting diethyl carbonate gas and preparation method thereof Download PDF

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CN115469390A
CN115469390A CN202211323386.0A CN202211323386A CN115469390A CN 115469390 A CN115469390 A CN 115469390A CN 202211323386 A CN202211323386 A CN 202211323386A CN 115469390 A CN115469390 A CN 115469390A
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system structure
substrate
layer
film system
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张�杰
何虎
许晴
于海洋
张敏敏
王爽
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Shanghai Aegis Industrial Safety Corp
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract

The invention relates to an infrared filter for detecting diethyl carbonate gas, which comprises a substrate, a main film system structure and a cut-off film system structure, wherein the main film system structure and the cut-off film system structure are respectively arranged on two sides of the substrate; the main membrane system structure is as follows: si/0.11L1.23H1.07H0.98H0.98L2.00H 0.99L0.98H1.02L1.09H1.01L0.99H0.98L1.99H0.99H0.83H0.44L/Air; the structure of the cut-off film system is as follows: si/0.26L 0.32 (0.5HL0.5H) ^60.48 (0.5HL0.5H) ^ 6.70 (0.5HL0.5H) ^ 6.35 (0.5LH0.5L) ^ 5.7 (0.5LH0.5L) ^ 5/Air), and the design wavelength is 7900nm. The invention also provides a corresponding preparation method and an infrared gas sensor.

Description

Infrared filter for detecting diethyl carbonate gas and preparation method thereof
Technical Field
The invention relates to the technical field of infrared gas detectors, and relates to an infrared filter for detecting diethyl carbonate gas, and a preparation method and application thereof.
Background
In recent years, with the promotion of new energy policy in China, the lithium ion battery industry has developed explosively. Meanwhile, the industry of diethyl carbonate (DEC) electrolyte matched with the electrolyte is rapidly developed. However, DEC is a colorless liquid that is toxic, flammable and volatile, and therefore its leakage should be monitored rigorously during manufacture, transport and use.
The industry generally selects a PID sensor to monitor the gas concentration (liquid leakage volatilization) of DEC, and although this type of sensor has the advantages of low cost and sensitive response, it also has the disadvantages of susceptibility to interference from other organic compounds and short service life. Among many gas detection technologies, non-dispersive infrared (NDIR) is becoming more and more popular in the market due to its non-toxic, anti-jamming and long life. Therefore, there is a need for an NDIR gas sensor that can be used to detect DEC gas.
Non Dispersive InfraRed sensing (NDIR) is a method of detecting gas concentration using two or more different InfraRed bands. The basic principle follows lambert beer's law:
I＝I 0 ·exp(-μCL)；
wherein I 0 Represents the light intensity when no gas is absorbed, I represents the light intensity when gas is absorbed, mu is the gas molecule absorption coefficient (constant at normal temperature and normal pressure), and L represents the optical path(i.e., the length of the sensor optical path, which is a constant) and C is the concentration of the gas to be measured. The two filters of different wave bands represent the light intensity channel I without absorption 0 (reference channel) and the intensity channel with absorption I (measurement channel), so that the ratio of the two channels is related only to the gas concentration,
ln(I 0 /I)＝μCL；
i.e. the gas concentration is proportional to the ratio of the signal intensities of the reference channel and the measurement channel.
In general, reference channel filters are easier to select (e.g., 3900nm/90nm filters), and the measurement channels must be determined based on the specific absorption peaks of the different gases.
In a chinese patent application CN 114895395A, a far infrared filter and a preparation method thereof are proposed, which have a center wavelength of 7800nm and a bandwidth of 160nm, and are suitable for detecting CF4 (refrigerant R14) gas. Among them, the filter (7800 nm/160 nm) in CN 114895395A cannot be directly or simply modified for detecting diethyl carbonate (DEC) gas, mainly because, based on the filter, the infrared absorption peak coincidence degree is low and the bandwidth is too small, the signal-to-noise ratio obtained by the sensor is too low to be used for detecting diethyl carbonate; in the film system design, a single crystal germanium base material with high price is used, and the germanium substrate material is more brittle and is not suitable for manufacturing a large-area germanium sheet; 3 coating materials, namely germanium, zinc selenide and zinc sulfide, are used in the design of a film system, so that the problem that one coating material is used is caused, and the materials are easily mixed in the preparation and production processes (zinc sulfide is a light yellow crystal, and zinc selenide is an orange crystal).
Disclosure of Invention
The invention mainly aims to solve the problems and provide an infrared filter for detecting diethyl carbonate gas and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the infrared filter for detecting the diethyl carbonate gas adopted by the invention is as follows:
the infrared filter comprises a substrate, a main film system structure and a cut-off film system structure, wherein the main film system structure and the cut-off film system structure are respectively arranged on two sides of the substrate;
the main membrane system structure is as follows:
Si/0.11L1.23H1.07H0.98H0.98L2.00H0.99L0.98H1.02L1.09H1.01L0.99H0.98L1.99H0.99L0.83H0.44L/Air；
the structure of the cut-off film system is as follows:
Si/0.26L 0.32(0.5HL0.5H)^6 0.48(0.5HL0.5H)^6 0.70(0.5HL0.5H)^6 1.35(0.5LH0.5L)^5 1.7(0.5LH0.5L)^5/Air；
wherein Si represents an optical-grade monocrystalline silicon substrate material, air represents Air, H is a Ge film layer with a quarter-wavelength optical thickness, L is a ZnS film layer with a quarter-wavelength optical thickness, and ^5 and ^6 are the repetition times of a film stack, the number before the film stack is a film thickness coefficient, and the design wavelength is 7900nm.
Preferably, the center wavelength of the infrared filter is 7900 +/-50 nm, the bandwidth is 280 +/-20 nm, the peak transmittance is more than 80%, and the transmittance of the wave bands of the cut-off regions 1500-7300 nm and 8500-16000 nm is less than 1%.
The invention also provides a method for preparing the infrared filter for detecting diethyl carbonate gas, which comprises the following steps:
(1) Putting the substrate into a fixture, placing the fixture into a vacuum chamber of a film coating machine, and vacuumizing;
(2) Baking the substrate;
(3) Ion bombardment of the substrate;
(4) Coating a main film system structure on one side of the substrate layer by layer according to the film layer required by the main film system structure;
(5) Turning over the substrate, repeating the steps (1) to (3), and plating a cut-off film system structure layer by layer on the other side of the substrate according to the film layer required by the cut-off film system structure;
(6) And (5) breaking the hollow part after the plating is finished, and taking the part.
Preferably, the step (1) is specifically:
loading the substrate material of single crystal silicon wafer into fixture, placing it in vacuum chamber of film-plating machine, and pumping the vacuum degree to 8X 10 -4 Pa；
The step (2) is specifically as follows:
baking the substrate material at 190-210 ℃ and keeping the constant temperature for 100-120 minutes;
the step (3) is specifically as follows:
bombarding the substrate material by using Hall ion source ions for 6-10 min, wherein the ion source uses high-purity oxygen, and the gas flow is 15-30 sccm;
the step (6) is specifically as follows:
after the plating is finished, the baking temperature is reduced to 20-40 ℃, and the workpiece is broken and taken out.
Preferably, the step (4) is specifically:
the main film system structure is plated layer by layer according to the film layer required by the main film system structure, the Ge film material is evaporated by adopting an electron beam evaporation process, the ZnS film material is evaporated by adopting a resistance evaporation process, wherein the film plating rate of the Ge film is 0.4-0.6 nm/s, the film plating rate of the ZnS film is 1.0-3.0 nm/s, the film thickness is monitored and judged by using light control in the deposition process, and the crystal control is used for monitoring the film plating rate.
Preferably, the step (5) is specifically:
and (2) reversing the substrate plated with the main film system structure, repeating the steps (1) to (3), plating a cut-off film system structure on the other side of the substrate layer by layer according to a film layer required by the cut-off film system structure, evaporating Ge film materials by adopting an electron beam evaporation process, wherein the film coating rate of the Ge film is 0.4-0.6 nm/s, evaporating ZnS film materials by adopting a resistance evaporation process, the film coating rate of the ZnS film is 1.0-3.0 nm/s, performing film thickness monitoring and judging by using light control in the deposition process, and monitoring the film coating rate by using crystal control.
Preferably, the method further comprises the steps of:
(7) The transmittance spectra at normal incidence of the filters were measured using a PE spectra two fourier transform infrared spectrometer.
The invention provides an infrared pyroelectric sensor which is mainly characterized in that the infrared pyroelectric sensor is provided with an infrared filter for detecting diethyl carbonate gas.
The infrared filter for detecting diethyl carbonate gas and the preparation method thereof can be well used for monitoring the concentration of gas volatilized by DEC.
Drawings
FIG. 1 is a chart of diethyl carbonate gas absorption spectra tested in accordance with the present invention.
FIG. 2 is the transmittance of a 0.5mm thick silicon wafer.
FIG. 3 is a transmittance spectrum of the host film system structure.
Fig. 4 is a transmittance spectrum of the cut-off film system structure.
Fig. 5a and 5b are a global and a partial magnified view, respectively, of an infrared spectrum of the 7900NBP filter.
FIG. 6 is a response graph of the measured signal of DEC gas.
Detailed Description
In order to clearly understand the technical contents of the present invention, the following examples are given in detail.
The infrared filter for detecting diethyl carbonate gas comprises a substrate, a main film system structure and a cut-off film system structure, wherein the main film system structure and the cut-off film system structure are respectively arranged on two sides of the substrate;
the main membrane system structure is as follows:
Si/0.11L1.23H1.07H0.98H0.98L2.00H0.99L0.98H1.02L1.09H1.01L0.99H0.98L1.99H0.99L0.83H0.44L/Air；
the structure of the cut-off film system is as follows:
Si/0.26L 0.32(0.5HL0.5H)^6 0.48(0.5HL0.5H)^6 0.70(0.5HL0.5H)^6 1.35(0.5LH0.5L)^5 1.7(0.5LH0.5L)^5/Air；
wherein Si represents an optical-grade monocrystalline silicon substrate material, in particular to an optical-grade czochralski monocrystalline silicon substrate material, air represents Air, H is a Ge film layer with a quarter-wavelength optical thickness, L is a ZnS film layer with a quarter-wavelength optical thickness, ^5 and ^6 are the repetition times of a film stack, the number in front of the film stack is a film thickness coefficient, and the design wavelength is 7900nm.
As shown in fig. 1, diethyl carbonate (DEC) gas was tested to have a significant absorption peak at 7.9 μm and a large bandwidth (about 300 nm). As shown in fig. 3 to 5b, through a plurality of tests, it is found that: the spectral characteristics of the infrared filter are: the central wavelength is 7900 +/-50 nm, the bandwidth is 280 +/-20 nm, the peak transmittance is more than 80%, and the use requirements are best met when the transmittance of the wave bands of 1500-7300 nm and 8500-16000 nm is less than 1%.
In the infrared filter of the present invention, optical grade czochralski silicon is used, the transmittance of the infrared filter is shown in fig. 2, the infrared filter has the advantages of lower cost (about one tenth of germanium), easier processing into large silicon wafers (such as 4 inches or 6 inches), and higher utilization rate of large-area substrates for subsequent filter scribing. The monocrystalline silicon with lower cost is used as a substrate material, so that the cost performance of the product is improved
In the infrared filter, the main film system and the cut-off film system both use non-regular film system structures (the thickness of the film layer is not integral multiple of a quarter wavelength), so that fewer film layers can be used to obtain an ideal spectrum, and the film coating time and the consumption of film materials are reduced.
The invention provides a method for preparing an infrared filter for detecting diethyl carbonate gas, which comprises the following steps:
(1) Putting the substrate into a fixture, placing the fixture into a vacuum chamber of a film coating machine, and vacuumizing; the method specifically comprises the following steps:
cleaning a monocrystalline silicon wafer base material with the thickness of 0.5mm and the diameter of 100mm, wherein the monocrystalline silicon wafer base material is polished on two sides: firstly, ultrasonic cleaning is carried out for 10 minutes by using a cleaning agent (the solvent ratio is ammonia water: hydrogen peroxide: pure water =5: 80), then the silicon wafer is put into the pure water for ultrasonic cleaning for 5 minutes, finally the pure water is used for spraying for 1 minute, then nitrogen is used for drying, the silicon wafer is put into a clamp and is placed into a vacuum chamber of a film coating machine, and the background vacuum degree is pumped to 8 multiplied by 10 -4 Pa；
(2) Baking the substrate; the method comprises the following specific steps:
baking the substrate material at 200 +/-10 ℃ and keeping the constant temperature for 100-120 minutes;
(3) Ion bombardment of the substrate; the method specifically comprises the following steps:
bombarding the substrate material by using Hall ion source ions for 6-10 min, wherein the ion source uses high-purity oxygen (99.99%), the anode voltage is 150-200V, and the gas flow is 15-30 sccm;
(4) Coating a main film system structure on one side of the substrate layer by layer according to the film layer required by the main film system structure; the method specifically comprises the following steps:
coating a main film system structure layer by layer according to a film layer required by the main film system structure, evaporating a Ge film material by adopting an electron beam evaporation process, evaporating a ZnS film material by adopting a resistance evaporation process, wherein the film coating rate of the Ge film is 0.5nm/s, the film coating rate of the ZnS film is 2.0nm/s, and the film thickness monitoring and judging are carried out by using light control in the deposition process, and the crystal control is used for monitoring the film coating rate;
(5) Turning over the substrate, repeating the steps (1) to (3), and plating a cut-off film system structure on the other side of the substrate layer by layer according to the film layer required by the cut-off film system structure; the method comprises the following specific steps:
reversing the substrate plated with the main film system structure, repeating the steps (1) to (3), plating a cut-off film system structure on the other side of the substrate layer by layer according to a film layer required by the cut-off film system structure, evaporating a Ge film material by adopting an electron beam evaporation process, wherein the film plating rate of the Ge film is 0.5nm/s, evaporating a ZnS film material by adopting a resistance evaporation process, the film plating rate of the ZnS film is 2.0nm/s, and performing film thickness monitoring and judging by using light control in the deposition process, wherein the crystal control is used for monitoring the film plating rate;
(6) After plating, breaking the hollow space and taking out the workpiece; the method comprises the following specific steps:
after plating, the baking temperature is reduced to 30 ℃, and then the workpiece is broken and taken out;
(7) The transmittance spectrum at normal incidence of the filter was measured using a PE spectrum two fourier transform infrared spectrometer.
In the method, the optical thickness of the film layer is monitored by using the light control system, so that the repeatability of batch production is improved, and the process robustness is better.
Wherein, the main film structure and the light control parameters thereof are shown in the following table 1:
TABLE 1
Figure BDA0003911429330000061
The structure of the cut-off film system and the light control parameters thereof are shown in the following table 2:
TABLE 2
Figure BDA0003911429330000071
The manufactured optical filter is manufactured into the infrared pyroelectric sensor through the following steps:
(8) Scribing with a Disco scriber and a resin blade (spindle rotation speed: 35000rpm, feed speed 8 mm/s), the size of the filter after scribing is 3 × 3mm;
(9) Packaging the 3900NBP and 7900NBP optical filters after slicing on a tube cap window by using a Wucang dispenser;
(10) And packaging the double-element tube cap and the pyroelectric sensitive element into the pyroelectric detector by using a capping machine in a high-purity nitrogen environment.
The pyroelectric sensor can be assembled as an infrared sensor for diethyl carbonate (DEC) gas detection according to the method in patent CN 215066148U.
As shown in fig. 6, the infrared sensor for detecting diethyl carbonate gas of the present invention, which uses 7900NBP filter and 3900NBP filter, can be well used for monitoring the concentration of gas volatilized by DEC.
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 specification and drawings are, accordingly, to be regarded in an illustrative rather than a restrictive sense.

Claims (8)

1. The infrared filter for detecting diethyl carbonate gas is characterized by comprising a substrate, a main film system structure and a cut-off film system structure, wherein the main film system structure and the cut-off film system structure are respectively arranged on two sides of the substrate;
the main membrane system structure is as follows:
Si/0.11L1.23H1.07H0.98H0.98L2.00H0.99L0.98H1.02L1.09H1.01L0.99H0.98L1.99H0.99L0.83H0.44L/Air；
the structure of the cut-off film system is as follows:
Si/0.26L 0.32(0.5HL0.5H)^6 0.48(0.5HL0.5H)^6 0.70(0.5HL0.5H)^61.35(0.5LH0.5L)^5 1.7(0.5LH0.5L)^5/Air；
wherein Si represents an optical-grade monocrystalline silicon substrate material, air represents Air, H is a Ge film layer with a quarter-wavelength optical thickness, L is a ZnS film layer with a quarter-wavelength optical thickness, and ^5 and ^6 are the repetition times of a film stack, the number before the film stack is a film thickness coefficient, and the design wavelength is 7900nm.
2. The infrared filter for detecting diethyl carbonate gas as claimed in claim 1, wherein the infrared filter has a center wavelength of 7900 ± 50nm, a bandwidth of 280 ± 20nm, a peak transmittance of > 80%, and a transmittance of < 1% in the cutoff regions of 1500-7300 nm and 8500-16000 nm.
3. A method for preparing the infrared filter for detecting diethyl carbonate gas of claim 1 or 2, comprising the steps of:
(1) Putting the substrate into a fixture, placing the fixture into a vacuum chamber of a film coating machine, and vacuumizing;
(2) Baking the substrate;
(3) Ion bombardment of the substrate;
(4) Coating a main film system structure on one side of the substrate layer by layer according to the film layer required by the main film system structure;
(5) Turning over the substrate, repeating the steps (1) to (3), and plating a cut-off film system structure on the other side of the substrate layer by layer according to the film layer required by the cut-off film system structure;
(6) And (5) breaking the hollow part after the plating is finished, and taking the part.
4. The method according to claim 3, wherein the step (1) is specifically:
loading the substrate material of single crystal silicon wafer into fixture, placing it in vacuum chamber of film-plating machine, and pumping the vacuum degree to 8X 10 - 4 Pa；
The step (2) is specifically as follows:
baking the substrate material at 190-210 ℃ and keeping the constant temperature for 100-120 minutes;
the step (3) is specifically as follows:
bombarding the substrate material by using Hall ion source ions for 6-10 min, wherein the ion source uses high-purity oxygen, and the gas flow is 15-30 sccm;
the step (6) is specifically as follows:
after the plating is finished, the baking temperature is reduced to 20-40 ℃, and the workpiece is broken and taken out.
5. The method according to claim 3, wherein the step (4) is specifically:
the method comprises the steps of coating a main film system structure layer by layer according to a film layer required by the main film system structure, evaporating Ge film materials by adopting an electron beam evaporation process, evaporating ZnS film materials by adopting a resistance evaporation process, wherein the film coating rate of a Ge film is 0.4-0.6 nm/s, the film coating rate of a ZnS film is 1.0-3.0 nm/s, carrying out film thickness monitoring and judging by using light control in a deposition process, and using crystal control for monitoring the film coating rate.
6. The method according to claim 3, wherein the step (5) is specifically:
and (2) reversing the substrate plated with the main film system structure, repeating the steps (1) to (3), plating a cut-off film system structure on the other side of the substrate layer by layer according to a film layer required by the cut-off film system structure, evaporating Ge film materials by adopting an electron beam evaporation process, wherein the film coating rate of the Ge film is 0.4-0.6 nm/s, evaporating ZnS film materials by adopting a resistance evaporation process, the film coating rate of the ZnS film is 1.0-3.0 nm/s, performing film thickness monitoring and judging by using light control in the deposition process, and monitoring the film coating rate by using crystal control.
7. The method of claim 3, further comprising the steps of:
(7) The transmittance spectrum at normal incidence of the filter was measured using a PE spectrum two fourier transform infrared spectrometer.
8. An infrared pyroelectric sensor, characterized in that the pyroelectric sensor is provided with the infrared filter for detecting diethyl carbonate gas as claimed in claim 1 or 2.
CN202211323386.0A 2022-10-27 2022-10-27 Infrared filter for detecting diethyl carbonate gas and preparation method thereof Pending CN115469390A (en)

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