CN112394090A - Nitrogen dioxide gas sensor element and preparation method thereof - Google Patents
Nitrogen dioxide gas sensor element and preparation method thereof Download PDFInfo
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- CN112394090A CN112394090A CN201910757333.1A CN201910757333A CN112394090A CN 112394090 A CN112394090 A CN 112394090A CN 201910757333 A CN201910757333 A CN 201910757333A CN 112394090 A CN112394090 A CN 112394090A
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- 239000007789 gas Substances 0.000 title claims abstract description 68
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 title claims abstract description 55
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims abstract description 74
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 14
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000010931 gold Substances 0.000 claims abstract description 12
- 229910052737 gold Inorganic materials 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 239000010703 silicon Substances 0.000 claims abstract description 11
- 229910003446 platinum oxide Inorganic materials 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 238000004544 sputter deposition Methods 0.000 claims description 38
- 239000010408 film Substances 0.000 claims description 36
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000009304 pastoral farming Methods 0.000 claims description 9
- 239000013077 target material Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 abstract description 16
- 230000010354 integration Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract description 2
- 238000004377 microelectronic Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
Abstract
The invention discloses a nitrogen dioxide gas sensor element and a preparation method thereof. The nitrogen dioxide gas sensor element comprises a tungsten trioxide film, a platinum film and a gold interdigital electrode which are sequentially deposited on a silicon substrate with an oxide layer on the surface; wherein the tungsten trioxide film and the platinum film are respectively deposited by adopting a glancing angle magnetron sputtering method, and the glancing angles are respectively 10-30 degrees. The platinum/tungsten trioxide composite film in the nitrogen dioxide gas sensor element has lower overall resistivity, and the gold interdigital electrode is arranged on the surface of the platinum film, so that the test resistance is further reduced, and the element integration and test are facilitated. Meanwhile, compared with the traditional powder material, the platinum/tungsten trioxide composite film prepared by adopting the glancing angle magnetron sputtering has good uniformity, high consistency, high adhesion between the film and a substrate, high sensitivity and good selectivity, and can detect low-concentration (0.1ppm) nitrogen dioxide gas at the temperature of below 200 ℃.
Description
Technical Field
The invention relates to a nitrogen dioxide gas sensor element and a preparation method thereof, belonging to the field of gas sensors.
Background
With the development of modern industry, the ecological environment of the earth is increasingly worsened by the combustion of various fossil fuels and the toxic and harmful gases discharged in the industrial production process. Nitrogen dioxide is a common atmospheric pollutant, is one of main substances forming acid rain and photochemical smog, and is extremely harmful to human bodies after being exposed to a high-concentration nitrogen dioxide environment for a long time. Therefore, the method has important significance and development prospect for the research of the nitrogen dioxide gas sensor element.
The tungsten trioxide gas-sensitive material has received extensive attention from researchers due to the advantages of high sensitivity to nitrogen dioxide, fast response speed and the like. At present, the gas sensor is generally prepared by using powdered tungsten trioxide in industrial production, but the powdered tungsten trioxide is incompatible with a microelectronic process, and meanwhile, the powdered tungsten trioxide inevitably can be polluted in the process of transferring the powdered tungsten trioxide to a sensor element, so that the gas-sensitive performance is reduced. The tungsten trioxide film grows in situ on the sensor chip by adopting methods such as magnetron sputtering and the like, so that the problems of process compatibility and material pollution can be solved, and lower working temperature can be realized more easily, so that the method has higher research value. However, the tungsten trioxide film prepared by the conventional magnetron sputtering method and other methods is compact and does not meet the characteristics of porosity and large specific surface area of the gas-sensitive material, so that the gas-sensitive performance of the tungsten trioxide film is low, and the high-performance tungsten trioxide film prepared by the anodic oxidation method and other auxiliary methods has complex process and high cost and is not suitable for industrial large-scale production, so that further research is still needed on how to prepare the high-performance gas-sensitive film by adopting the simple process. In addition, the single tungsten trioxide film has higher resistivity, which is not beneficial to the integration and detection of the gas sensor element, and the noble metal film is compounded on the surface of the tungsten trioxide film, so that the overall resistivity of the film can be reduced, and the gas-sensitive property of the sensor element can be improved.
Disclosure of Invention
The invention aims to provide a nitrogen dioxide gas sensor element. The nitrogen dioxide gas sensor element has the advantages of low working temperature, high sensitivity, good selectivity, compatibility with microelectronic process, easy realization of silicon-based integration, and suitability for industrial mass production.
Another object of the present invention is to provide a method for manufacturing the nitrogen dioxide gas sensor element.
In order to achieve the purpose, the invention adopts the following technical scheme:
a nitrogen dioxide gas sensor element comprises a tungsten trioxide film, a platinum film and a gold interdigital electrode which are sequentially deposited on a silicon substrate with an oxide layer on the surface; wherein the tungsten trioxide film and the platinum film are respectively deposited by adopting a glancing angle magnetron sputtering method, and the glancing angles are respectively 10-30 degrees.
In the present invention, when the glancing angle is less than 10 ° or more than 30 °, the gas-sensitive performance of the prepared platinum/tungsten trioxide composite film may be significantly reduced, resulting in a great decrease in the sensitivity of the sensor element. Preferably, the glancing angle is between 15 ° and 20 °.
A method for producing the nitrogen dioxide gas sensor element, the method comprising the steps of:
(1) depositing tungsten trioxide thin film
Adopting metal tungsten as a target material, adopting argon and oxygen as working gases, and adopting a grazing angle magnetron sputtering to deposit a tungsten trioxide film on a silicon substrate with an oxide layer on the surface, wherein the grazing angle is 10-30 degrees;
(2) deposition of platinum films
Adopting metal platinum as a target material, adopting argon as working gas, and adopting a grazing angle magnetron sputtering to deposit a platinum film on the surface of the silicon substrate deposited with the tungsten trioxide, wherein the grazing angle is 10-30 degrees;
(3) preparation of gas sensor element
And placing the substrate deposited with the platinum/tungsten trioxide composite film in a muffle furnace for heat treatment, sputtering a gold interdigital electrode on the substrate subjected to heat treatment by taking gold as a target material and argon as a working gas to obtain the nitrogen dioxide gas sensor element.
Wherein, the sputtering working pressure, the oxygen volume fraction, the sputtering power and the sputtering time in the step (1), the sputtering working pressure, the sputtering power and the sputtering time in the step (2), and the heat treatment temperature and the heat treatment time in the step (3) can obviously influence the gas-sensitive performance of the film.
Preferably, the background vacuum degree in the step (1) is less than 5X 10-4Pa, the sputtering working pressure is 0.5-3 Pa, the volume fraction of oxygen is 20-60%, the sputtering power is 50-200W, and the sputtering time is 4-16 min.
Preferably, the background vacuum degree in the step (2) is less than 5X 10-4Pa, the sputtering working pressure is 0.5-3 Pa, the sputtering power is 50-150W, and the sputtering time is 5-20 s.
Preferably, the heat treatment temperature in the step (3) is 300-600 ℃, the temperature rise speed is 2 ℃/min, and the heat treatment time is 2-5 h.
Preferably, the background vacuum degree in the step (3) is less than 5X 10-4Pa, the sputtering working pressure is 1.5Pa, the sputtering power is 60W, and the sputtering time is 5 min.
The invention has the advantages that:
the platinum/tungsten trioxide composite film in the nitrogen dioxide gas sensor element has lower overall resistivity, and the gold interdigital electrode is arranged on the surface of the platinum film, so that the test resistance is further reduced, and the element integration and test are facilitated. Compared with the traditional powder material, the platinum/tungsten trioxide composite film prepared by adopting the glancing angle magnetron sputtering has the advantages of good uniformity, high consistency, high adhesion between the film and a substrate, high sensitivity and good selectivity, can detect low-concentration (0.1ppm) nitrogen dioxide gas at the temperature of below 200 ℃, is simple in preparation process, is compatible with a silicon-based microelectronic process, is easy to realize integration, and is suitable for industrial large-scale production.
Drawings
Fig. 1 is a schematic view of the structure of a nitrogen dioxide gas sensor element of the present invention.
Fig. 2 is a graph of the sensitivity of the nitrogen dioxide gas sensor element of example 1 to 1ppm nitrogen dioxide versus operating temperature.
Fig. 3 is a graph of the response/recovery of the nitrogen dioxide gas sensor element of example 1 at 150 c for different concentrations of nitrogen dioxide.
Fig. 4 is a schematic illustration of the selectivity of the nitrogen dioxide gas sensor element of example 1 for 1ppm of different gases at 150 c.
Detailed Description
The present invention is further illustrated with reference to the following figures and examples, which are not meant to limit the scope of the invention.
Example 1
(1) Depositing tungsten trioxide thin film
Depositing a tungsten trioxide film on the surface of the silicon oxide wafer by adopting a glancing angle magnetron sputtering method, wherein the glancing angle is 15 degrees. The target material is metal tungsten with the mass purity of 99.95 percent, the working gas is argon and oxygen with the purity of 99.999 percent, wherein the flow of the argon is 30mL/min, the flow of the oxygen is 20mL/min, the background vacuum degree is 2 x 10 < -4 > Pa, the sputtering pressure is 1Pa, the sputtering power is 100W, and the sputtering time is 8 min.
(2) Deposition of platinum films
And (3) adopting glancing angle magnetron sputtering to deposit a platinum film on the surface of the substrate deposited with the tungsten trioxide, wherein the glancing angle is 15 degrees. The target material is metal platinum with the mass purity of 99.95 percent, the working gas is argon with the purity of 99.999 percent, the argon flow is 20mL/min, the background vacuum degree is 2 x 10 < -4 > Pa, the sputtering pressure is 1.5Pa, the sputtering power is 60W, and the sputtering time is 10 s.
(3) Preparation of gas sensor element
And (3) placing the substrate deposited with the platinum/tungsten trioxide composite film in a muffle furnace for heat treatment at the temperature of 450 ℃ for 3 h. And then sputtering gold interdigital electrodes on the substrate after heat treatment by adopting conventional magnetron sputtering, wherein the used target material is gold with the mass purity of 99.95 percent, the working gas is argon with the purity of 99.999 percent, the argon flow is 20mL/min, the background vacuum degree is 2 x 10 < -4 > Pa, the sputtering pressure is 1.5Pa, the sputtering power is 60W, and the sputtering time is 5 min. The prepared nitrogen dioxide gas sensor element is shown in figure 1, wherein 1 is a silicon substrate, an oxide layer 2 grows on the surface of the silicon substrate, a tungsten trioxide thin film 3 and a platinum thin film 4 are deposited upwards, and the uppermost layer is a gold interdigital electrode 5.
The invention adopts a dynamic gas distribution method to measure the sensitivity of a nitrogen dioxide gas sensor element to gas to be measured at different temperatures, and defines the sensitivity S-Rg/R0 under oxidizing atmosphere (such as nitrogen dioxide) and the sensitivity S-R0/Rg under reducing atmosphere (such as ammonia gas), wherein R0 and Rg are the resistance values of the gas sensor element in dry air and the gas to be measured respectively.
The sensitivity of the nitrogen dioxide gas sensor element obtained in example 1 to 1ppm of nitrogen dioxide at room temperature, 100 ℃, 150 ℃, 200 ℃ and 250 ℃ operating temperatures was 1.21, 6.44, 9.37, 4.62 and 1.61, respectively, as shown in fig. 2. The nitrogen dioxide gas sensor element is suitable for working at low temperature (less than 200 ℃), and the optimal working temperature is 150 ℃.
The dynamic response curves of the nitrogen dioxide gas sensor element prepared in example 1 at the operating temperature of 150 ℃ for different concentrations of nitrogen dioxide are shown in fig. 3, and the sensitivity to 0.1ppm, 0.5ppm, 1ppm, 2ppm, 5ppm and 10ppm of nitrogen dioxide is 1.52, 5.73, 9.37, 48.46, 270.71 and 1135.62, respectively, and the response time to 1ppm of nitrogen dioxide is 24 s. The nitrogen dioxide gas sensor element has higher sensitivity to low-concentration nitrogen dioxide and has faster response characteristic.
The sensitivity of the nitrogen dioxide gas sensor element obtained in example 1 to 1ppm of nitrogen dioxide, ammonia gas, carbon monoxide, acetone, and ethanol at an operating temperature of 150 ℃ was 9.37, 1.36, 1.02, 1.04, and 1.01, respectively, as shown in fig. 4. It is shown that the nitrogen dioxide gas sensor element of the present invention has excellent selectivity for low concentrations of nitrogen dioxide.
Example 2
The present embodiment is different from embodiment 1 in that: the sputtering time of tungsten trioxide in step (1) was 16min, and the sensitivity of the prepared nitrogen dioxide gas sensor element to 1ppm of nitrogen dioxide at 150 ℃ was 5.45.
Example 3
The present embodiment is different from embodiment 1 in that: the sputtering time of platinum in the step (2) was 20s, and the sensitivity of the prepared nitrogen dioxide gas sensor element to 1ppm of nitrogen dioxide at 150 ℃ was 3.32.
Example 4
The present embodiment is different from embodiment 1 in that: the glancing angle in the deposition process of the platinum and tungsten trioxide films is 30 degrees, and the sensitivity of the prepared nitrogen dioxide gas sensor element to 1ppm of nitrogen dioxide at 150 ℃ is 1.85.
Claims (7)
1. A nitrogen dioxide gas sensor element is characterized by comprising a tungsten trioxide film, a platinum film and a gold interdigital electrode which are sequentially deposited on a silicon substrate with an oxide layer on the surface; wherein the tungsten trioxide film and the platinum film are respectively deposited by adopting a glancing angle magnetron sputtering method, and the glancing angles are respectively 10-30 degrees.
2. The nitrogen dioxide gas sensor element according to claim 1, wherein the grazing angle is 15 ° to 20 °.
3. A method for producing a nitrogen dioxide gas sensor element according to claim 1 or 2, characterized by comprising the steps of:
(1) depositing tungsten trioxide thin film
Adopting metal tungsten as a target material, adopting argon and oxygen as working gases, and adopting a grazing angle magnetron sputtering to deposit a tungsten trioxide film on a silicon substrate with an oxide layer on the surface, wherein the grazing angle is 10-30 degrees;
(2) deposition of platinum films
Adopting metal platinum as a target material, argon as a working gas, and adopting a grazing angle magnetron sputtering to deposit a platinum film on the surface of the substrate deposited with the tungsten trioxide, wherein the grazing angle is 10-30 degrees;
(3) preparation of gas sensor element
And placing the silicon substrate deposited with the platinum/tungsten trioxide composite film in a muffle furnace for heat treatment, sputtering a gold interdigital electrode on the heat-treated substrate by taking gold as a target material and argon as a working gas, and obtaining the nitrogen dioxide gas sensor element.
4. The method for producing a nitrogen dioxide gas sensor element according to claim 3, wherein the steps are(1) Vacuum degree of middle background is less than 5 x 10-4Pa, the sputtering working pressure is 0.5-3 Pa, the volume fraction of oxygen is 20-60%, the sputtering power is 50-200W, and the sputtering time is 4-16 min.
5. The method for producing a nitrogen dioxide gas sensor element according to claim 3, wherein the background vacuum degree in the step (2) is less than 5 x 10-4Pa, the sputtering working pressure is 0.5-3 Pa, the sputtering power is 50-150W, and the sputtering time is 5-20 s.
6. The method for manufacturing a nitrogen dioxide gas sensor element according to claim 3, wherein the heat treatment temperature in the step (3) is 300 to 600 ℃, the temperature rise rate is 2 ℃/min, and the heat treatment time is 2 to 5 hours.
7. The method for producing a nitrogen dioxide gas sensor element according to claim 3, wherein the background vacuum degree in the step (3) is less than 5 x 10-4Pa, the sputtering working pressure is 1.5Pa, the sputtering power is 60W, and the sputtering time is 5 min.
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Application publication date: 20210223 |