Nitrogen oxide gas sensor based on sulfur doped graphene and preparation method thereof

Patent metadata

Field	Value
Publication number	US-10908107-B2
Application number	US-201615774007-A
Country	US
Kind code	B2
Filing date	Jan 6, 2016
Priority date	Nov 11, 2015
Publication date	Feb 2, 2021
Grant date	Feb 2, 2021

Abstract

A nitrogen oxide gas sensor based on sulfur-doped graphene and a preparation method therefor. The method includes the following steps: 1) providing graphene and a micro heater platform substrate, and transferring the graphene onto the micro heater platform substrate; 2) putting the micro heater platform substrate covered with the graphene into a chemical vapor deposition reaction furnace; 3) performing gas feeding and exhausting treatment to the reaction furnace by using inert gas; 4) simultaneously feeding inert gas and hydrogen gas into the reaction furnace at a first temperature; 5) feeding inert gas, hydrogen gas and sulfur source gas into the reaction furnace at a second temperature for reaction to perform sulfur doping to the graphene; and 6) stopping feeding the sulfur source gas, and performing cooling in a hydrogen gas and insert gas shielding atmosphere.

First claim

What is claimed is:

1. A preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene, characterized in that the method comprises the following steps:
1) providing graphene and a micro heater platform substrate, and transferring the graphene onto the micro heater platform substrate;
2) putting the micro heater platform substrate covered with the graphene into a chemical vapor deposition reaction furnace;
3) performing gas feeding and exhausting treatment to the reaction furnace by using inert gas;
4) simultaneously feeding inert gas and hydrogen gas into the reaction furnace at a first temperature;
5) feeding inert gas, hydrogen gas and sulfur source gas into the reaction furnace at a second temperature for reaction to perform sulfur doping to the graphene; and
6) stopping feeding the sulfur source gas, and performing cooling to the reaction furnace in a hydrogen gas and insert gas shielding atmosphere.

2. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that, in step 1), the graphene is intrinsic graphene.

3. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that, in step 1), the micro heater platform substrate is a single micro heater platform or a wafer level substrate.

4. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that, in step 1), a test electrode and a heater are provided on the micro heater platform substrate, and the graphene at least covers the test electrode.

5. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that, in step 1), the graphene is transferred onto the micro heater platform substrate by adopting a direct transfer method or PMMA method.

6. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that, in step 3), the flow rate of the inert gas is 500 sccm-5000 sccm, and the gas feeding and exhausting treatment time is 2 min-30 min.

7. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that, in step 4), the first temperature is 200° C.-700° C.; the flow rate of mixed gas of the hydrogen gas and the inert gas is 100 sccm-5000 sccm; and the mixing ratio of the hydrogen gas to the inert gas is 10%-90%.

8. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that, in step 5), the second temperature is 300° C.-900° C.; the flow rate of the inert gas is 500 sccm-5000 sccm, the flow rate of the hydrogen gas is 10 sccm-100 sccm and the flow rate of the sulfur source gas is 0.5 sccm-50 sccm; and the doping time is 10 min-50 min.

9. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 8 , characterized in that the sulfur source gas comprises one or more of hydrogen sulfide and carbonyl sulfide.

10. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that the sulfur source gas comprises one or more of hydrogen sulfide and carbonyl sulfide.

11. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that, in step 5), temperature is increased from the first temperature to the second temperature, the temperature is kept at the second temperature for 5 min-20 min, and then the sulfur source gas is fed into the reaction furnace.

12. The preparation method for nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 1 , characterized in that, in step 6), the flow rate of the inert gas is 50 sccm-300 sccm, and the flow rate of the hydrogen gas is 10 sccm-40 sccm.

13. A nitrogen oxide gas sensor based on sulfur-doped graphene comprising:
a micro heater platform substrate with a first surface and a second surface;
a test electrode located on the first surface of the micro heater platform substrate;
a heater located on the second surface of the micro heater platform substrate; and
a sulfur-doped graphene located on the first surface of the micro heater platform substrate covering the test electrode and the first surface of the micro heater platform substrate.

14. The nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 13 , wherein the micro heater platform substrate is a single micro heater platform, the number of the test electrode is one pair, the number of the heater is one, and the pair of test electrode is disposed above the heater.

15. The nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 13 , wherein the micro heater platform substrate is a wafer level substrate, a plurality of test electrodes and a plurality of heaters are respectively distributed in an array on the first surface and the second surface, and the plurality of test electrodes correspond to the plurality of heaters one to one in location.

16. A nitrogen oxide gas sensor based on sulfur-doped graphene comprising:
a micro heater platform substrate with a first surface and a second surface;
a heater located on the first surface of the micro heater platform substrate;
an insulating layer located on the heater;
a test electrode located on the insulating layer;
a sulfur-doped graphene located on the first surface of the micro heater platform substrate covering the test electrode and the first surface of the micro heater platform substrate.

17. The nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 16 , wherein the micro heater platform substrate is a single micro heater platform, the number of the test electrode is one pair, the number of the heater is one, and the pair of test electrode is disposed above the heater.

18. The nitrogen oxide gas sensor based on sulfur-doped graphene according to claim 16 , wherein the micro heater platform substrate is a wafer level substrate, a plurality of test electrodes and a plurality of heaters are respectively distributed in an array on the first surface of the micro heater platform substrate, and the plurality of test electrodes correspond to the plurality of heaters one to one in location.

Assignees

• Shanghai Inst Microsystem & Information Tech Cas
• Shanghai Institute Of Microsystem And Information Tech Chinese Academy Of Science

Inventors

• Li Tie
• Guo Lianfeng
• Liang Chen
• Wang Yuelin

Classifications

• G01N33/0037

  NOx · CPC title

• C23C16/22

  characterised by the deposition of inorganic material, other than metallic material · CPC title

• G01N27/125 Primary

  Composition of the body, e.g. the composition of its sensitive layer · CPC title

• Y02A50/20

  Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters · CPC title