CN113608289B - Infrared filter for nitrogen trifluoride gas detection and preparation method thereof - Google Patents
Infrared filter for nitrogen trifluoride gas detection and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an infrared filter for detecting nitrogen trifluoride gas, which comprises a substrate, a main film system structure and a cut-off film system structure; the main film system structure is as follows: sub/HLHL2HLHLHLHL2HLH0.08M/Air; the stop film system structure is as follows: sub/0.18 (HL) ≡5.265 (HL) ≡0.38 (HL) ≡7.52 (HL) ≡0.73 (HL) ≡7.43 (0.5LH0.5L) ≡7.1M/Air; the central wavelength of the infrared filter is 11050+/-100 nm, the bandwidth is 380+/-60 nm, the peak transmittance is more than or equal to 78%, and the maximum transmittance of the cut-off region of 2000-18000 nm is less than 1%. The invention also provides a corresponding preparation method and an infrared gas sensor.
Description
Technical Field
The invention relates to the technical field of infrared gas detectors, in particular to an infrared filter for detecting nitrogen trifluoride gas, a preparation method and application thereof.
Background
Nitrogen trifluoride, formula NF 3 The relative molecular weight is 71.002, the gas is colorless and toxic at normal temperature, the melting point is-206.8 ℃, and the boiling point is-129 ℃. The nitrogen trifluoride gas is a fluorine source of a high-energy chemical laser and is also a plasma etching gas in the microelectronics industry, and has good selectivity and etching rate for plasma etching of a silicon substrate. In particular, the amount of nitrogen trifluoride gas used has been rapidly increasing in recent years with the development of the semiconductor industry. But at the same time, the mixed gas of nitrogen trifluoride and water, hydrogen, ammonia, carbon monoxide or hydrogen sulfide can be exploded violently when meeting sparks. And meanwhile, nitrogen trifluoride is easy to react with hemoglobin, and the risk is high after the nitrogen trifluoride is inhaled into a human body. Therefore, the leakage problem of the gas is needed to be closely concerned in the production, the preparation, the storage and the use of the nitrogen trifluoride, otherwise, serious safety accidents are easily caused. While an infrared gas sensor using NDIR technology is an important means for monitoring nitrogen trifluoride gas, as shown in fig. 1, at an incident light intensity I according to lambert-beer's law 0 (λ), gas absorption coefficient α (λ), and optical path L are unchanged, and the emitted light intensity I (λ) =i 0 (λ)exp[-α(λ)CL]Only with respect to the gas concentration C. The function of the filter in the structure is to only allow the light of the nitrogen trifluoride infrared absorption area to enter the detector, and the light of other wave bands is totally cut off. However, no infrared filter specially designed for detecting nitrogen trifluoride gas exists in the market at present, which affects popularization and application of the nitrogen trifluoride gas infrared sensor.
CN 109870408A, an optical filter for nondispersive infrared detection of nitrogen trifluoride, application thereof and detection method of nitrogen trifluoride, uses sapphire optical filter to realize the filtering effect of high transmissivity of 10-12 μm wave band, contradicts with optical common sense, so the optical filter provided by the patent cannot be realized. It is known that to achieve a high transmission effect in a certain band, a material should be selected for design that has no or low absorption in that band, whereas sapphire materials should belong to the contraindicated materials in the 10-12 μm band. Since sapphire has strong optical absorption characteristics in this band, resulting in its complete absorption cutoff (i.e., light-tight). Referring specifically to fig. 2, a transmittance spectrum of sapphire with a thickness of 1mm, which was self-measured by the inventors; reference may also be made to Yu Huai, second edition of "Infrared optics", page 68, which shows that 7 μm later is not available, for the text of figures 2-30 to 2-33 and tables 2-8; reference may also be made to FIG. 3, which shows the transmittance spectrum of sapphire, which is disclosed for CRYSTRAN, UK, and which is derived fromhttps://www.crystran.co.uk/optical-materials/sapphire-al2o3. Reference may also be made to the data relating to sapphire disclosed by the german schottky (schott) company, which explicitly indicates that sapphire can be used with a transmission spectrum in the 250 to 5000nm band. Therefore, based on the common knowledge of the optics, the optical filter disclosed in the patent has 10-12 μm that other spectral patterns in the transmission spectrum area cannot be realized. Next, in this patent, plating barium fluoride of 0.4 to 1mm on a silicon wafer also fails to achieve the effect of a bandpass filter, and fig. 8 is a transmission spectrum of this solution simulated using film system design software. In addition, plating of barium fluoride films of 0.4-1 mm on silicon wafers is not in line with the general technical knowledge, so-called film thickness is usually in the order of nanometers and micrometers, if the film thickness in the order of millimeters is higherCost, in this case, barium fluoride flake is generally used directly instead.
Disclosure of Invention
The invention aims at solving the problems and provides an infrared filter for detecting nitrogen trifluoride gas, and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme of the infrared filter for detecting nitrogen trifluoride 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 film system structure is as follows:
Sub/HLHL2HLHLHLHL2HLH0.08M/Air, where Sub represents the substrate, air represents Air, H is a quarter wavelength optical thickness Ge film, L is a quarter wavelength optical thickness ZnS film, M is a quarter wavelength optical thickness YbF 3 The number of the film layer in the film system structure is the film thickness coefficient, and the design wavelength is 11050nm;
the stop film system structure is as follows:
sub/0.18 (HL) ≡5.265 (HL) ≡0.38 (HL) ≡7.52 (HL) ≡7.73 (HL) ≡7.43 (0.5LH0.5L) ≡7.1M/Air, wherein Sub represents a substrate, air represents Air, H is a Ge film layer of quarter wavelength optical thickness, L is a ZnS film layer of quarter wavelength optical thickness, M is YbF of quarter wavelength optical thickness 3 The film layers, the numbers of the repetition times of the film stacks are the film thickness coefficient, and the design wavelength is 11050nm;
the central wavelength of the infrared filter is 11050+/-100 nm, the bandwidth is 380+/-60 nm, the peak transmittance is more than or equal to 78%, and the maximum transmittance of the cut-off region of 2000-18000 nm is less than 1%.
Preferably, the substrate is single crystal silicon or single crystal germanium with the thickness of 0.5mm and polished on two sides.
The invention also provides a method for preparing the infrared filter for detecting nitrogen trifluoride gas, which comprises the following steps:
(1) Placing the substrate into a clamp, placing the clamp into a vacuum chamber of a coating machine, and vacuumizing;
(2) Baking the substrate;
(3) Ion bombarding the substrate;
(4) Plating a main film system structure layer by layer on one side of the substrate according to the film layer required by the main film system structure;
(5) Turning over the substrate, repeating the steps (1) - (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 after plating, breaking the blank and taking out the workpiece.
Preferably, the step (1) specifically includes:
loading a monocrystalline silicon wafer or monocrystalline germanium wafer substrate material with thickness of 0.5mm and smoothness of 40/20 standard into a fixture, placing into a vacuum chamber of a coating machine, and pumping the background vacuum degree to 8×10 -4 Pa；
The step (2) is specifically as follows:
baking the substrate material at 200-300 ℃ and keeping the constant temperature for more than 120 min;
the step (3) is specifically as follows:
ion bombarding the substrate material for 5-15 min by adopting a Hall ion source, wherein the ion source uses high-purity argon, and the gas flow is 15-25 sccm;
the step (6) is specifically as follows:
and after plating, the baking temperature is reduced to 20-40 ℃ to break the blank and take out the workpiece.
Preferably, the step (4) specifically includes:
coating the main film system structure layer by layer according to the film layer required by the main film system structure, and evaporating the Ge film material and YbF by adopting an electron beam evaporation process 3 The film material is evaporated by adopting a resistance evaporation process, wherein the film coating rate of the Ge film is 0.4-0.6 nm/s and YbF 3 The film coating speed is 0.4-0.6 nm/s, the ZnS film coating speed is 2.0-3.0 nm/s, and the film thickness and speed are controlled by combining indirect light control and crystal control in the deposition process.
Preferably, the step (5) specifically includes:
reversing the substrate plated with the main film system structure, repeating the steps (1) - (3), plating the 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, and evaporating the Ge film material and YbF by adopting an electron beam evaporation process 3 Film material, the film coating rate of Ge film is 0.4-0.6 nm/s, ybF 3 The film coating speed is 0.4-0.6 nm/s, the ZnS film material is evaporated by adopting a resistance evaporation process, the film coating speed of the ZnS film is 2.0-3.0 nm/s, and the film thickness and speed are controlled by using indirect light control and crystal control in combination in the deposition process.
Preferably, the method further comprises the steps of:
(7) Placing the plated infrared filter into an annealing furnace for annealing at the annealing temperature of 250-350 ℃ for 7-9 hours at the heating/cooling speed of 1 ℃/min;
(8) The transmittance spectrum at normal incidence of the filter was measured using a PE spectral two fourier transform infrared spectrometer.
The invention also provides an infrared temperature measuring sensor, wherein the infrared thermometer is provided with the infrared filter for detecting nitrogen trifluoride gas.
The infrared filter for detecting nitrogen trifluoride gas, the preparation method and the application thereof, provided by the invention, use a regular film system, are favorable for positioning the center wavelength and the bandwidth of the passband of the filter by using a light control technology, ensure the accuracy of a transmission peak, and use fluoride YbF in the outermost layer 3 The film material can ensure the accuracy of spectrum and has the effect of resisting nitrogen trifluoride reaction, and the service life of the optical filter is prolonged.
Drawings
Fig. 1 is a schematic structural view of an NDIR infrared sensor.
Fig. 2 is a graph of the transmittance spectrum of sapphire having a thickness of 1mm, which was self-measured by the inventors.
Fig. 3 is a transmittance spectrum of sapphire disclosed by CRYSTRAN company, UK.
Fig. 4 is a schematic structural view of an infrared filter for detecting nitrogen trifluoride gas according to the present invention.
FIG. 5 is a spectrum of a narrow band infrared filter of the present invention having a center wavelength of 11000 nm.
FIG. 6 is a partial enlarged spectrum view of a narrow band infrared filter with a center wavelength of 11000nm according to the present invention.
Fig. 7 is a transmission spectrum of the infrared band of single crystal silicon.
Fig. 8 is a transmission spectrum of CN 109870408A solution simulated using film system design software.
Detailed Description
In order to make the technical contents of the present invention more clearly understood, the following examples are specifically described.
As shown in fig. 4, in order to solve the problem that there is no special filter for detecting nitrogen trifluoride gas in the market at present, the invention provides an embodiment of an infrared filter for detecting nitrogen trifluoride gas, wherein the infrared filter comprises a substrate, a main film system structure and a stop film system structure, and the main film system structure and the stop film system structure are respectively arranged at two sides of the substrate. The main film system structure and the stop film system structure use alternating Ge film layers and ZnS film layers, and ytterbium fluoride (YbF 3) is used as the outermost layer, so that the accuracy of spectrum is ensured, and the corrosion of nitrogen trifluoride can be prevented.
Specifically, the main film system structure is as follows: sub/HLHL2HLHLHLHL2HLH0.08M/Air, where Sub represents the substrate, air represents Air, H is a quarter wavelength optical thickness Ge film, L is a quarter wavelength optical thickness ZnS film, M is a quarter wavelength optical thickness YbF 3 The number of the film layer in the film system structure is the film thickness coefficient, and the design wavelength is 11050nm;
the stop film system structure is as follows: sub/0.18 (HL) ≡5.265 (HL) ≡0.38 (HL) ≡7.52 (HL) ≡7.73 (HL) ≡7.43 (0.5LH0.5L) ≡7.1M/Air, wherein Sub represents a substrate, air represents Air, H is a Ge film layer of quarter wavelength optical thickness, L is a ZnS film layer of quarter wavelength optical thickness, M is YbF of quarter wavelength optical thickness 3 The film layers, the numbers of the repetition times of the film stacks are the film thickness coefficient, and the design wavelength is 11050nm;
according to the infrared absorption spectrum of nitrogen trifluoride gas, there is a deep absorption peak at 11.05+ -0.2 μm, so the high transmission region of the filter is set in this band, but at the same time, the wider the use bandwidth is, the larger the gas absorption coefficient is, the more easily absorption saturation occurs under the same optical path condition, i.e., the larger α (λ), the emitted light intensity I (λ) approaches zero and is insensitive to concentration variation. As shown in fig. 5 and 6, the center wavelength of the narrow-band infrared filter is 11050+/-100 nm, the bandwidth is 380+/-60 nm, the peak transmittance is more than or equal to 78%, and the maximum transmittance of a cut-off region (except a pass band) of 2000-18000 nm is less than 1%. The transmission passband of the invention is 380nm, which is significantly different from the projection passband of CN 109870408A, 2000 nm.
The substrate is monocrystalline silicon or monocrystalline germanium with the thickness of 0.5mm and polished on two sides. As shown in FIG. 7, the single crystal silicon is used as a base material, which has the advantage of a broad infrared transmission spectrum (2-18 μm transmission) and a low cost. In addition, single crystal germanium can be used as a substrate material, but is expensive and is not suitable for mass production.
The invention also provides an embodiment of a method for preparing the infrared filter for nitrogen trifluoride gas detection, which comprises the following steps:
(1) Loading monocrystalline silicon wafer substrate material with thickness of 0.5mm, diameter of 100mm and smoothness of 40/20 standard into fixture, placing into vacuum chamber of film plating machine, and pumping background vacuum degree to 8×10 -4 Pa; when the main film system structure is plated, the substrate is preferentially placed at a position with better film thickness uniformity, and the outermost ring station of the rotary substrate table is generally avoided.
(2) Baking the substrate material at 200-300 ℃ and keeping the constant temperature for more than 120 min; preferably the baking temperature is 250 ℃;
(3) Ion bombarding the substrate material for 5-15 min by adopting a Hall ion source, wherein the ion source uses high-purity argon, and the gas flow is 15-25 sccm; the bombardment time is preferably 10min;
(4) On one side of the substrate, plating a main film system structure layer by layer according to the film layer required by the main film system structure, and evaporating the Ge film material and YbF by adopting an electron beam evaporation process 3 The film material is evaporated by adopting a resistance evaporation process, wherein the film coating rate of the Ge film is excellentSelected to be 0.5nm/s, ybF 3 The film coating speed is preferably 0.5nm/s, the ZnS film coating speed is 2.5nm/s, and the film thickness and speed are controlled by combining indirect light control and crystal control in the deposition process;
(5) Reversing the substrate plated with the main film system structure, repeating the steps (1) - (3), plating the 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, and evaporating the Ge film material and YbF by adopting an electron beam evaporation process 3 The film material, the film coating rate of the Ge film is preferably 0.5nm/s, ybF 3 The film coating speed is preferably 0.5nm/s, a resistance evaporation process is adopted to evaporate ZnS film material, the film coating speed of the ZnS film is 2.5nm/s, and the film thickness and speed are controlled by using indirect light control and crystal control in the deposition process;
(6) And after plating, the baking temperature is reduced to 30 ℃, and blank breaking and workpiece taking are carried out.
(7) Placing the plated infrared filter into an annealing furnace for annealing, wherein the annealing temperature is preferably 300 ℃, the constant temperature time is preferably 8 hours, and the heating/cooling speed is 1 ℃/min;
(8) The transmittance spectrum at normal incidence of the filter was measured using a PE spectral two fourier transform infrared spectrometer.
The invention also provides an infrared temperature measuring sensor, wherein the infrared thermometer is provided with the infrared filter for detecting nitrogen trifluoride gas.
The infrared filter for detecting nitrogen trifluoride gas, the preparation method and the application thereof, provided by the invention, use a regular film system, are favorable for positioning the center wavelength and the bandwidth of the passband of the filter by using a light control technology, ensure the accuracy of a transmission peak, and use fluoride YbF in the outermost layer 3 The film material can ensure the accuracy of spectrum and has the effect of resisting nitrogen trifluoride reaction, and the service life of the optical filter is prolonged.
In this specification, the invention has been described with reference to specific embodiments thereof. It will be apparent, however, that various modifications and changes may be made without departing from the 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 nitrogen trifluoride 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 film system structure is as follows:
Sub/HLHL2HLHLHLHL2HLH0.08M/Air, where Sub represents the substrate, air represents Air, H is a quarter wavelength optical thickness Ge film, L is a quarter wavelength optical thickness ZnS film, M is a quarter wavelength optical thickness YbF 3 The number of the film layer in the film system structure is the film thickness coefficient, and the design wavelength is 11050nm;
the stop film system structure is as follows:
sub/0.18 (HL) ≡5.265 (HL) ≡0.38 (HL) ≡7.52 (HL) ≡7.73 (HL) ≡7.43 (0.5LH0.5L) ≡7.1M/Air, wherein Sub represents a substrate, air represents Air, H is a Ge film layer of quarter wavelength optical thickness, L is a ZnS film layer of quarter wavelength optical thickness, M is YbF of quarter wavelength optical thickness 3 The film layers, the numbers of the repetition times of the film stacks are the film thickness coefficient, and the design wavelength is 11050nm;
the central wavelength of the infrared filter is 11050+/-100 nm, the bandwidth is 380+/-60 nm, the peak transmittance is more than or equal to 78%, and the maximum transmittance of the cut-off region of 2000-18000 nm except the passband is less than 1%.
2. The infrared filter for detecting nitrogen trifluoride gas as defined in claim 1, wherein said substrate is 0.5mm thick, double-sided polished single crystal silicon or single crystal germanium.
3. A method for producing the infrared filter for nitrogen trifluoride gas detection as claimed in claim 1 or 2, characterized by comprising the steps of:
(1) Placing the substrate into a clamp, placing the clamp into a vacuum chamber of a coating machine, and vacuumizing;
(2) Baking the substrate;
(3) Ion bombarding the substrate;
(4) Plating a main film system structure layer by layer on one side of the substrate according to the film layer required by the main film system structure;
(5) Turning over the substrate, repeating the steps (1) - (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 after plating, breaking the blank and taking out the workpiece.
4. The method for manufacturing an infrared filter for nitrogen trifluoride gas detection as claimed in claim 3, wherein said step (1) is specifically:
loading a monocrystalline silicon wafer or monocrystalline germanium wafer substrate material with thickness of 0.5mm and smoothness of 40/20 standard into a fixture, placing into a vacuum chamber of a coating machine, and pumping the background vacuum degree to 8×10 -4 Pa；
The step (2) is specifically as follows:
baking the substrate material at 200-300 ℃ and keeping the constant temperature for more than 120 min;
the step (3) is specifically as follows:
ion bombarding the substrate material for 5-15 min by adopting a Hall ion source, wherein the ion source uses high-purity argon, and the gas flow is 15-25 sccm;
the step (6) is specifically as follows:
and after plating, the baking temperature is reduced to 20-40 ℃ to break the blank and take out the workpiece.
5. The method for manufacturing an infrared filter for nitrogen trifluoride gas detection as recited in claim 3, wherein said step (4) is specifically:
coating the main film system structure layer by layer according to the film layer required by the main film system structure, and evaporating the Ge film material and YbF by adopting an electron beam evaporation process 3 The film material is evaporated by adopting a resistance evaporation process, wherein the film coating rate of the Ge film is 0.4-0.6 nm/s and YbF 3 The film coating rate of the film is 0.4-0.6 nm/s, and the ZnS film coating rate is2.0-3.0 nm/s, and the film thickness and the film speed are controlled by using indirect light control and crystal control in the deposition process.
6. The method for manufacturing an infrared filter for nitrogen trifluoride gas detection as recited in claim 3, wherein said step (5) is specifically:
reversing the substrate plated with the main film system structure, repeating the steps (1) - (3), plating the 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, and evaporating the Ge film material and YbF by adopting an electron beam evaporation process 3 Film material, the film coating rate of Ge film is 0.4-0.6 nm/s, ybF 3 The film coating speed is 0.4-0.6 nm/s, the ZnS film material is evaporated by adopting a resistance evaporation process, the film coating speed of the ZnS film is 2.0-3.0 nm/s, and the film thickness and speed are controlled by using indirect light control and crystal control in combination in the deposition process.
7. The method for manufacturing an infrared filter for nitrogen trifluoride gas detection as recited in claim 3, further comprising the steps of:
(7) Placing the plated infrared filter into an annealing furnace for annealing at the annealing temperature of 250-350 ℃ for 7-9 hours at the heating/cooling speed of 1 ℃/min;
(8) The transmittance spectrum at normal incidence of the filter was measured using a PE spectral two fourier transform infrared spectrometer.
8. An infrared temperature sensor, characterized in that the infrared temperature sensor is provided with the infrared filter for detecting nitrogen trifluoride gas according to claim 1 or 2.
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| CN210514674U (en) * | 2019-07-03 | 2020-05-12 | 上海欧菲尔光电技术有限公司 | Germanium-based infrared long-wave pass filter |
| CN111596396A (en) * | 2020-07-21 | 2020-08-28 | 上海翼捷工业安全设备股份有限公司 | Infrared filter for chloroethylene gas detection, gas sensor and preparation method |
| CN112255721A (en) * | 2020-11-12 | 2021-01-22 | 深圳市美思先端电子有限公司 | Double-bandpass filter and manufacturing method thereof |
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