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CN-121992487-A - Preparation of Ag monoatomic modified In based on pulse voltage discharge2O3Single crystal film, method thereof and gas sensor

CN121992487ACN 121992487 ACN121992487 ACN 121992487ACN-121992487-A

Abstract

The invention discloses an Ag monoatomic modified In 2 O 3 monocrystalline film prepared based on pulse voltage discharge, a method and a gas sensor thereof, which comprise the following steps of 1) placing a substrate In a vacuum cavity of magnetron sputtering equipment, taking an indium oxide target as an In source, growing the indium oxide monocrystalline film on the substrate through a magnetron sputtering process to obtain the indium oxide monocrystalline film, wherein the substrate is yttria stabilized zirconia YSZ, 2) placing the indium oxide monocrystalline film obtained In the step 1) on a vacuum cavity sample table provided with a pulse voltage discharge electrode and an Ag target inside, evaporating Ag particles based on the pulse voltage discharge process, depositing on the surface of the indium oxide monocrystalline film material to form dispersed clusters, and annealing to obtain the Ag monoatomic modified In 2 O 3 monocrystalline film. The synthesis of sensitive materials with high atomic utilization rate and stable structure is realized, and the advanced NO 2 gas sensor with high sensitivity and high selectivity is obtained.

Inventors

  • ZHU LIPING
  • MAO JIANING
  • JIANG JIE
  • WU XINFENG
  • LI XINRAN
  • YU XIANLONG

Assignees

  • 浙江大学温州研究院
  • 浙江大学
  • 温州志感科技有限公司

Dates

Publication Date
20260508
Application Date
20260211

Claims (10)

  1. 1. The method for preparing the Ag monoatomic modified In 2 O 3 monocrystal film based on the pulse voltage discharge technology is characterized by comprising the following steps of: 1) Placing a substrate In a vacuum cavity of a magnetron sputtering device, taking an In 2 O 3 target as an In source, and growing an indium oxide In 2 O 3 monocrystal film on the substrate through a magnetron sputtering process, wherein the substrate is yttria stabilized zirconia YSZ; 2) Placing the indium oxide single crystal film obtained In the step 1) on a vacuum chamber sample table provided with a pulse voltage discharge electrode and an Ag target material, evaporating Ag particles based on a pulse voltage discharge process, depositing the Ag particles on the surface of the indium oxide single crystal film material to form dispersed clusters, and annealing to obtain the Ag monoatomic modified In 2 O 3 single crystal film.
  2. 2. The method for preparing the Ag monoatomic modified In 2 O 3 single crystal thin film based on the pulse voltage discharge technology according to claim 1, wherein In step 1), the substrate is washed with acetone, absolute ethyl alcohol, deionized water In sequence before being placed In a vacuum cavity of a magnetron sputtering device.
  3. 3. The method for preparing the Ag monoatomic modified In 2 O 3 single crystal film based on the pulse voltage discharge technology according to claim 1 is characterized In that In the step 1), the magnetron sputtering process specifically comprises the steps of S1, vacuumizing a vacuum cavity, and then heating the substrate to 400-600 ℃, wherein the temperature rising rate is 30 ℃ per minute; S2, setting the power of the magnetron sputtering equipment to be 80-100W, introducing argon, and cleaning the In 2 O 3 target by pre-sputtering for 2-5 min; And S3, introducing argon and oxygen into the vacuum cavity, and adjusting the argon-oxygen ratio in the vacuum cavity to be 10:1-5:1, wherein the total pressure is 0.40 Pa-2.0 Pa, the power is 80W-100W, and the sputtering time is 10 min-30 min.
  4. 4. The method for preparing the Ag monoatomic modified In 2 O 3 single crystal thin film based on the pulse voltage discharge technology according to claim 1, wherein In the step 2), an Ag target is used as a discharge cathode or is placed In front of the cathode, and the distance between a sample stage and the Ag target is 5-30 cm.
  5. 5. The method for preparing the Ag monoatomic modified In 2 O 3 monocrystalline film based on the pulse voltage discharge technology according to claim 1 is characterized In that In the step 2), ag particles are evaporated based on the pulse voltage discharge technology, and dispersed clusters are formed on the surface of an indium oxide monocrystalline film material by depositing the Ag particles on the surface of the indium oxide monocrystalline film material by firstly vacuumizing a vacuum chamber until the background vacuum degree is not higher than 1.0X10 -3 Pa, secondly, continuously introducing argon as working gas, maintaining the pressure of the chamber at 0.1-10 Pa, and then applying a high-voltage pulse power supply to the pulse voltage discharge electrode to evaporate the Ag particles, and depositing the Ag particles on the surface of the indium oxide monocrystalline film material.
  6. 6. The method for preparing Ag monoatomic modified In 2 O 3 single crystal thin film according to claim 5, wherein the specific pulse parameters of the high-voltage pulse power supply applied to the pulse voltage discharge electrode are pulse voltage 1-20 kV, pulse frequency 10-1000 Hz and pulse width 1-300 s。
  7. 7. The method for preparing a Ag monoatomic modified In 2 O 3 single crystal thin film based on pulse voltage discharge technology according to claim 1, wherein In step 2), the deposition time is 30 seconds to 30 minutes, and after the deposition is finished, the sample is subjected to vacuum or protective atmosphere annealing treatment at room temperature to 400 ℃.
  8. 8. An Ag monoatomic modified In 2 O 3 single crystal thin film prepared based on pulse voltage discharge technology, which is characterized In that the single crystal thin film is prepared by the method according to any one of claims 1-7.
  9. 9. A gas sensor for detecting low concentration NO 2 , characterized In that the Ag monoatomically modified In 2 O 3 single crystal thin film material according to claim 8 is used as a sensitive layer material.
  10. 10. The low concentration NO 2 detection gas sensor according to claim 9, wherein the low concentration is less than 100ppm.

Description

Ag monoatomic modified In 2O3 monocrystalline film prepared based on pulse voltage discharge, method thereof and gas sensor Technical Field The invention relates to the field of gas sensing material preparation and semiconductor devices, in particular to an Ag monoatomic modified In 2O3 monocrystalline film prepared based on pulse voltage discharge, a method thereof and a gas sensor. Background NO 2 is a major atmospheric pollutant, mainly derived from the combustion of automobile exhaust, industrial exhaust and fossil fuels. Long-term exposure to low concentration NO 2 can seriously harm human respiratory system, while high concentration NO 2 can cause environmental problems such as acid rain, photochemical smog, etc. Therefore, the development of the high-performance gas sensor capable of rapidly, accurately and real-time detecting the low-concentration NO 2 has urgent demands and important significance in the fields of environmental monitoring, industrial safety, intelligent home, medical diagnosis and the like. The noble metal monoatomic catalyst provides a revolutionary thought for greatly improving the performance of the sensing material by virtue of the extreme atomic utilization rate and the unique electronic structure. Among them, in 2O3 single crystal thin film is an ideal carrier material, but the surface of the thin film is high-efficiency, uniform and stable to load noble metal single atoms, which faces key technical challenges. The current mainstream single-atom preparation and loading technology, such as wet chemical method, is easy to cause atom aggregation, and the Atomic Layer Deposition (ALD) technology has the problems of complex technology, high cost, poor compatibility with thin film technology and the like. Based on the above, the invention provides an Ag monoatomic modified In 2O3 monocrystalline film prepared based on a pulse voltage discharge technology and a gas sensor, which can be effectively used In the field of NO 2 detection. Disclosure of Invention The invention aims to provide an Ag monoatomic modified In 2O3 monocrystalline film prepared based on pulse voltage discharge, a method thereof and a gas sensor, so as to realize efficient synthesis of sensitive materials with high atomic utilization rate and stable structure, and finally obtain an advanced NO 2 gas sensor with high sensitivity and high selectivity, thereby meeting urgent requirements of the fields of environmental monitoring, industrial safety and the like on accurate and real-time gas detection technology. The invention provides the following technical scheme: A method for preparing an Ag monoatomic modified In 2O3 monocrystalline film based on a pulse voltage discharge technology comprises the following steps: 1) Placing a substrate In a vacuum cavity of a magnetron sputtering device, taking an In 2O3 target as an In source, and growing an indium oxide In 2O3 monocrystal film on the substrate through a magnetron sputtering process, wherein the substrate is yttria stabilized zirconia YSZ; 2) Placing the indium oxide single crystal film obtained In the step 1) on a vacuum chamber sample table provided with a pulse voltage discharge electrode and an Ag target material, evaporating Ag particles based on a pulse voltage discharge process, depositing the Ag particles on the surface of the indium oxide single crystal film material to form dispersed clusters, and annealing to obtain the Ag monoatomic modified In 2O3 single crystal film. Further, in step 1), the substrate is washed with acetone, absolute ethyl alcohol and deionized water in sequence before being placed in a vacuum cavity of the magnetron sputtering device. In the step 1), the magnetron sputtering process specifically comprises the steps of S1, vacuumizing a vacuum cavity, and then heating the substrate to 400-600 ℃ with the temperature rising rate of 30 ℃ per minute; S2, setting the power of the magnetron sputtering equipment to be 80-100W, introducing argon, and cleaning the In 2O3 target by pre-sputtering for 2-5 min; and S3, introducing argon and oxygen into the vacuum cavity, and adjusting the argon-oxygen ratio in the vacuum cavity to be 10:1-5:1, wherein the total pressure is 0.40-2.0 Pa, the power is 80-100W, and the sputtering time is 10-30 min. Further, in step 2), the Ag target is used as a discharge cathode or is placed in front of the cathode, and the distance between the sample stage and the Ag target is 5-30 cm. Further, in the step 2), ag particles are evaporated based on a pulse voltage discharge process, and the Ag particles are deposited on the surface of the indium oxide single crystal film material to form dispersed clusters, wherein firstly, a vacuum chamber is vacuumized until the background vacuum degree is not higher than 1.0X10 -3 Pa, secondly, argon is introduced as working gas, the pressure of the chamber is maintained to be 0.1-10 Pa, and then a high-voltage pulse power supply is applied to the pulse voltage discharge electro