CN115710695A - Integrated wafer-level hydrogen sulfide gas-sensitive film and preparation method of single MEMS hydrogen sulfide gas-sensitive film - Google Patents
Integrated wafer-level hydrogen sulfide gas-sensitive film and preparation method of single MEMS hydrogen sulfide gas-sensitive film Download PDFInfo
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- CN115710695A CN115710695A CN202211393937.0A CN202211393937A CN115710695A CN 115710695 A CN115710695 A CN 115710695A CN 202211393937 A CN202211393937 A CN 202211393937A CN 115710695 A CN115710695 A CN 115710695A
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- hydrogen sulfide
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- sulfide gas
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- 239000007789 gas Substances 0.000 title claims abstract description 50
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000231 atomic layer deposition Methods 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000010408 film Substances 0.000 description 28
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 22
- 239000011787 zinc oxide Substances 0.000 description 11
- 239000002245 particle Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009223 counseling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000001548 drop coating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
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Abstract
The invention relates to the technical field of gas-sensitive film preparation, in particular to an integrated wafer-level hydrogen sulfide gas-sensitive film and a preparation method of a single MEMS hydrogen sulfide gas-sensitive film.
Description
Technical Field
The invention relates to the technical field of gas-sensitive film preparation, in particular to an integrated wafer-level hydrogen sulfide gas-sensitive film and a preparation method of a single MEMS hydrogen sulfide gas-sensitive film.
Background
Hydrogen sulfide gas (H) 2 S) has high toxicity, high volatility and inflammability and is a hazardous gas pollutant. It is readily released from industrial production of oil, gas and mines. Long term exposure to ppb level H 2 S may increase the risk of central nervous and respiratory symptoms. 8 hours H 2 S threshold limit Exposure of 10ppm, recommendation H established by the American conference of government Industrial hygienists and the scientific counseling Committee for toxic air pollutants 2 Acceptable atmospheric levels of S should be at<83ppb range, thus monitoring very low concentrations of H in real time 2 S gas is important.
Research reports that various gas-sensitive performance influence factors such as morphology, crystal face and size are reported, when the particle size of the nano sensitive material is larger than the Debye length, the influence of the particle size change on the sensitive performance is small, and the gas-sensitive response is gradually increased along with the reduction of the particle size. Therefore, reducing the diameter of the nanoparticles is one of effective means for improving the sensitivity.
Currently, various types of gas sensors have been developed to detect these gases, but it is difficult to fabricate a uniform thin film on a MEMS (micro electro mechanical system) by conventional fabrication methods such as a drop coating method, a spin coating method, and the like. The gas sensitive material close to the thickness of the electron depletion layer generally has smaller particle size and higher working temperature, so that the nanoparticles of the gas sensitive material are easy to agglomerate at the working temperature, and the response and the stability of the gas sensitive material are further reduced. Meanwhile, the sensitive film (the thickness is usually in micron level) prepared by the traditional dripping method increases the collision probability of gas molecules and sensitive materials due to particle accumulation, knudsen diffusion and other gas diffusion modes, but the bottom of the sensitive film is difficult to react with the gas molecules. Therefore, the construction of an integrated structure of the gas-sensitive film with the length close to Debye, the effective reduction of particle agglomeration while realizing the electron depletion of the MOS film is an important strategy for improving the sensing performance and stability of the gas-sensitive material.
Therefore, in order to solve the above problems, the invention provides an integrated wafer-level hydrogen sulfide gas-sensitive film and a preparation method of a single MEMS hydrogen sulfide gas-sensitive film, wherein an ALD (atomic layer deposition) technology is used to construct the zinc oxide integrated film, the size or thickness of nanoparticles is accurately controlled, the problems of slow gas diffusion, particle agglomeration and the like in the conventional dropping coating method for preparing the sensitive film are effectively reduced, and the thermodynamic stability and gas-sensitive performance of the gas-sensitive film are improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an integrated wafer-level hydrogen sulfide gas-sensitive film and a preparation method of a single MEMS hydrogen sulfide gas-sensitive film.
In order to achieve the purpose, the invention provides an integrated wafer-level hydrogen sulfide gas-sensitive film and a preparation method of a single MEMS hydrogen sulfide gas-sensitive film, which comprises the following steps:
s1, before ALD (atomic layer deposition), firstly cleaning and drying an MEMS wafer;
s2, transferring the MEMS into an ALD reactor;
s3, depositing a ZnO film by taking diethyl zinc and water as precursors;
and S4, controlling the cycle number of the ALD ZnO deposited on the MEMS to obtain ZnO films with different thicknesses.
The temperature of the precursor is 0-200 ℃.
The pulse time of the single circulation of the diethyl zinc is 0.0001-50 s respectively.
The temperature of the precursor water is 0-90 ℃.
The pulse time in the single circulation of the precursor water is 0.0001-100 s.
Compared with the prior art, the integrated ZnO ultrathin heterogeneous gas-sensitive film is constructed on the MEMS wafer in situ by ALD (atomic layer deposition), so that the preparation of the MEMS sensor with high bonding strength, high sensitivity and long-term stability is realized, the process can effectively improve the consistency of the MEMS sensor, realize high-throughput, consistency and uniformity preparation and improve the preparation efficiency of the MEMS hydrogen sulfide sensor.
Drawings
FIG. 1 is a schematic view of a microscopic SEM of a film prepared by a conventional method in the prior art.
FIG. 2 is a schematic diagram of a MEMS wafer and a MEMS cell according to the present invention.
FIG. 3 is a schematic diagram of the morphology and thickness of a ZnO film on the MEMS structure of the present invention.
FIG. 4 is a graph of data of the bonding strength of the ZnO thin film prepared by the present invention.
FIG. 5 is a schematic diagram of the uniformity and homogeneity of the ZnO thin film prepared by the present invention.
Detailed Description
The invention will now be further described with reference to the accompanying drawings.
Referring to fig. 1 to 5, the invention provides an integrated wafer-level hydrogen sulfide gas-sensitive film and a preparation method of a single MEMS hydrogen sulfide gas-sensitive film, comprising the following steps:
s1, before ALD (atomic layer deposition), firstly cleaning and drying a micro-electro-mechanical system (MEMS);
s2, transferring the MEMS into an ALD reactor;
s3, depositing a ZnO film by taking diethyl zinc and water as precursors;
and S4, controlling the cycle number of the ALD ZnO deposition on the MEMS to obtain ZnO films with different thicknesses.
The temperature of the precursor is 0-200 ℃.
The pulse time in the single circulation of the diethyl zinc is 0.0001-50 s respectively.
The temperature of the precursor water is 0-90 ℃.
The pulse time in the single circulation of the precursor water is 0.0001-100 s.
The above is only a preferred embodiment of the present invention, and is only used to help understand the method and the core idea of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
The invention solves the technical problems that nano particles are easy to agglomerate, and the response and stability of a gas sensitive material are reduced due to particle accumulation and Knudsen diffusion, so that the bottom of a sensitive film is difficult to react with gas molecules.
Claims (5)
1. An integrated wafer-level hydrogen sulfide gas-sensitive film and a preparation method of a single MEMS hydrogen sulfide gas-sensitive film are characterized by comprising the following steps:
s1, before ALD (atomic layer deposition), firstly cleaning and drying an MEMS wafer;
s2, transferring the MEMS into an ALD reactor;
s3, depositing a ZnO film by taking diethyl zinc and water as precursors;
and S4, controlling the cycle number of the ALD ZnO deposited on the MEMS to obtain ZnO films with different thicknesses.
2. The integrated wafer-level hydrogen sulfide gas-sensitive film and the preparation method of the single MEMS hydrogen sulfide gas-sensitive film according to claim 1, wherein the temperature of the precursor is 0-200 ℃.
3. The integrated wafer-level hydrogen sulfide gas-sensitive film and the preparation method of the single MEMS hydrogen sulfide gas-sensitive film as claimed in claim 1, wherein the pulse time of the single cycle of the diethyl zinc is 0.0001-50 s respectively.
4. The integrated wafer-level hydrogen sulfide gas-sensitive film and the preparation method of the single MEMS hydrogen sulfide gas-sensitive film as claimed in claim 1, wherein the temperature of the precursor water is 0-90 ℃.
5. The integrated wafer-level hydrogen sulfide gas-sensitive film and the preparation method of the single MEMS hydrogen sulfide gas-sensitive film as claimed in claim 4, wherein the pulse time in a single circulation of the precursor water is 0.0001-100 s.
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| CN202211393937.0A CN115710695A (en) | 2022-11-08 | 2022-11-08 | Integrated wafer-level hydrogen sulfide gas-sensitive film and preparation method of single MEMS hydrogen sulfide gas-sensitive film |
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| CN202211393937.0A CN115710695A (en) | 2022-11-08 | 2022-11-08 | Integrated wafer-level hydrogen sulfide gas-sensitive film and preparation method of single MEMS hydrogen sulfide gas-sensitive film |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130311108A1 (en) * | 2007-07-17 | 2013-11-21 | Kwj Engineering Inc. | Apparatus and Method for Microfabricated Multi-Dimensional Sensors and Sensing Systems |
| CN114152652A (en) * | 2021-12-07 | 2022-03-08 | 上海大学 | Preparation method of integrated MEMS hydrogen sensor |
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- 2022-11-08 CN CN202211393937.0A patent/CN115710695A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130311108A1 (en) * | 2007-07-17 | 2013-11-21 | Kwj Engineering Inc. | Apparatus and Method for Microfabricated Multi-Dimensional Sensors and Sensing Systems |
| CN114152652A (en) * | 2021-12-07 | 2022-03-08 | 上海大学 | Preparation method of integrated MEMS hydrogen sensor |
Non-Patent Citations (3)
| Title |
|---|
| JUN YANG等: "Characteristics of ALD-ZnO Thin Film Transistor Using H2O and H2O2 as Oxygen Sources", 《ADVANCED MATERIALS INTERFACES》, vol. 9, no. 15, 23 May 2022 (2022-05-23), pages 1 - 9 * |
| QINGMIN HU等: "Highly Sensitive ZnO MEMS Sensor Fabrication with Atomic Layer Deposition Technique", 《THE ELECTROCHEMICAL SOCIETY》, vol. 56, 31 May 2021 (2021-05-31), pages 1 - 5 * |
| S. I. BOYADJIEV等: "Preparation and characterization of ALD deposited ZnO thin films studied for gas sensors", 《APPLIED SURFACE SCIENCE》, vol. 387, 30 November 2016 (2016-11-30), pages 1 - 17 * |
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