Method for preparation of plasma-treated nanofiber-based hydrogen gas sensing material

Patent metadata

Field	Value
Publication number	US-12258703-B2
Application number	US-202017906072-A
Country	US
Kind code	B2
Filing date	Dec 24, 2020
Priority date	Mar 12, 2020
Publication date	Mar 25, 2025
Grant date	Mar 25, 2025

Abstract

The present disclosure provides a preparation method of a plasma-treated nanofiber-based hydrogen gas sensing material, including the following steps: (1) stirring a mixed solution of absolute ethanol, polyvinyl pyrrolidone (PVP), N,N-dimethylformamide, SnCl 2 ·H 2 O, and Zn(CH 3 COO) 2 ·2H 2 O uniformly on a constant-temperature magnetic stirrer to obtain a spinning solution; (2) electrospinning the spinning solution and depositing on an aluminum foil to obtain a spinning fiber; (3) annealing the spinning fiber in a muffle furnace to obtain a hydrogen gas sensing material sample; and (4) subjecting the hydrogen gas sensing material sample to a vacuum argon plasma treatment with a Hall ion source to obtain the nanofiber-based hydrogen gas sensing material. In the method, nanofibers are prepared by electrospinning and subjected to the vacuum argon plasma treatment through the Hall ion source. The prepared sensing material has an extremely large specific surface area, and gas-sensing properties of rapid response and high sensitivity to hydrogen gas.

First claim

What is claimed is:

1. A method for preparation of a plasma-treated nanofiber-based hydrogen gas sensing material, comprising the following steps:
(1) stirring a mixed solution of absolute ethanol, polyvinyl pyrrolidone (PVP), N,N-dimethylformamide (DMF), SnCl 2 ·H 2 O, and Zn(CH 3 COO) 2 ·2H 2 O uniformly on a constant-temperature magnetic stirrer to obtain a spinning solution;
(2) electrospinning the spinning solution and depositing on an aluminum foil to obtain a spinning fiber;
(3) annealing the spinning fiber in a muffle furnace to obtain a hydrogen gas sensing material sample; and
(4) subjecting the hydrogen gas sensing material sample to a vacuum argon plasma treatment with a Hall ion source to obtain the nanofiber-based hydrogen gas sensing material,
wherein in step (1), the SnCl 2 ·H 2 O and the Zn(CH 3 COO) 2 ·2H 2 O have a mass ratio of (1-1.6):(1-1.6), and the absolute ethanol, the DMF, and the PVP have a volume ratio of (1-1.5):(1-1.5):(1-1.5), and
wherein in step (4), the vacuum argon plasma treatment comprises the following steps: placing the hydrogen gas sensing material sample into a vacuum chamber; conducting vacuumization with an air pump and a molecular pump to a vacuum degree of 5×10 −3 Pa, and introducing 3 sccm to 5 sccm of argon gas into the vacuum chamber to keep the vacuum degree at 1×10 −2 Pa to 5×10 −2 Pa; turning on the Hall ion source, adjusting an anode voltage and an anode current, starting timing, and recording a cathode voltage and a cathode current; and when the treatment is completed, turning off the Hall ion source, introducing nitrogen gas, opening the vacuum chamber, and removing the sample to complete the vacuum argon plasma treatment; wherein the vacuum argon plasma treatment is conducted at a cathode voltage of 10 V to 15 V, a cathode current of 8.0 A to 10.0 A, an anode voltage of 120 V to 150 V, and an anode current of 1.0 A to 1.9 A for 5 min to 20 min.

2. The method for preparation of a plasma-treated nanofiber-based hydrogen gas sensing material according to claim 1 , wherein step (1) specifically comprises the following steps: mixing 0.5 g to 0.8 g of the SnCl 2 ·H 2 O, 0.5 g to 0.8 g of the Zn(CH 3 COO) 2 ·2H 2 O, 5 mL to 7.5 mL of the absolute ethanol, and 5 mL to 7.5 mL of the DMF, and stirring the mixed solution on the constant-temperature magnetic stirrer at 50° C. and 300 r/min; after mixing uniformly by the stirring, adding 5 mL to 7.5 mL of the PVP to an obtained mixture, and continuing stirring at 50° C. and 300 r/min for 6 h to mix uniformly, to obtain the spinning solution.

3. The method for preparation of a plasma-treated nanofiber-based hydrogen gas sensing material according to claim 1 , wherein in step (2), a temperature is controlled at 40° C. to 60° C. and a relative humidity is controlled at 35% before the electrospinning; and the electrospinning is conducted by a flat plate winding method, with a needle as a positive electrode at a voltage range of 10 kV to 15 kV, and the aluminum foil as a negative electrode at a voltage range of 2 kV to 3 kV.

4. The method for preparation of a plasma-treated nanofiber-based hydrogen gas sensing material according to claim 1 , wherein in step (3), the spinning fiber is annealed in a muffle furnace by the following three stages:
a first stage of heating: heating the muffle furnace from a room temperature to 600° C. within 3 h;
a second stage of maintaining a constant-temperature: maintaining the muffle furnace at 600° C. for 2 h; and
a third stage of cooling: reducing a power of the muffle furnace to 0, and naturally cooling to the room temperature.

5. The method for preparation of a plasma-treated nanofiber-based hydrogen gas sensing material according to claim 1 , wherein the vacuum argon plasma treatment is conducted at the cathode voltage of 14.2 V, the cathode current of 10.0 A, the anode voltage of 150 V, and the anode current of 1.9 A.

6. The method for preparation of a plasma-treated nanofiber-based hydrogen gas sensing material according to claim 1 , wherein the vacuum argon plasma treatment is conducted at the cathode voltage of 15 V, the cathode current of 8 A, the anode voltage of 145 V, and the anode current of 1.2 A for 20 min.

Assignees

• Univ Chongqing

Inventors

• Wang Feipeng
• Hu Kelin
• Shen Zijia
• Liu Hongcheng
• Xiong Jianglin
• Li Jian
• Wang Youyuan
• Chen Weigen
• Du Lin
• Wang Kaizheng
• Zhao Qi

Classifications

• G01N33/005 Primary

  H2 · CPC title

• D10B2505/00

  Industrial · CPC title

• D10B2401/16

  antistatic; conductive · CPC title

• D10B2321/08

  polymers of unsaturated carboxylic acids or unsaturated organic esters, e.g. polyacrylic esters, polyvinyl acetate · CPC title

• D06M2101/18

  Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds · CPC title