Preparation method for multi-layer metal oxide porous film nano gas-sensitive material

Patent metadata

Field	Value
Publication number	US-9816176-B2
Application number	US-201415030893-A
Country	US
Kind code	B2
Filing date	Apr 8, 2014
Priority date	Oct 21, 2013
Publication date	Nov 14, 2017
Grant date	Nov 14, 2017

Abstract

The present invention discloses a method for preparing a multilayer metal oxide nano-porous thin film gas sensitive material, in which the microsphere aqueous solution is self-assembled on a substrate covered with an insulating layer, to form a compact single-layer array template; the surface of these microspheres are etched by using a plasma etching method to reduce the pitches between the microspheres; the metal oxide thin film is deposited by a physical deposition method; the template is removed by ultrasonic treatment with a solvent to prepare a porous array metal oxide thin film; and annealing is performed in air atmosphere to obtain the metal oxide porous thin film gas sensitive material. The present invention can be used for preparing a regular porous array thin film gas sensitive material; the pore size of the prepared porous thin film material is uniform and controllable; and the combination of these materials is controllable.

First claim

What is claimed is:

1. A method for preparing a multilayer metal oxide nano-porous film gas sensitive material, comprising the following steps:
Step 1-self-assembling the polystyrene microsphere single-layer template on a Si substrate covered with SiO 2 by using a solution evaporation method;
Step 2-etching the polystyrene microsphere template by using a reactive ion etching method, to reduce the pitches between PSs;
Step 3-depositing, on the substrate processed in Step 2, 40 nm Cu 2 O+40 nm In 2 O 3 with indium oxide being in the bottom layer, and cuprous oxide being in the top layer, 40 nm In 2 O 3 +40 nm Cu 2 O with cuprous oxide being in the bottom layer, and indium oxide being in the top layer, 30 nm Cu 2 O+20 nm In 2 O 3 , +30 nm Cu 2 O with indium oxide being in the intermediate layer, and 30 nm In 2 O 3 +20 nm Cu 2 O+30 nm In 2 O 3 with cuprous oxide being in the intermediate layer, using a magnetron sputter physical deposition method; and
Step 4-placing the processed substrate of step 3 in toluene for ultrasonic treatment to remove the polystyrene microsphere template, and performing annealing for 4 h in air atmosphere at the temperature of 550° C.

2. The method for preparing a multilayer metal oxide nano-porous film gas sensitive material according to claim 1 , wherein the thickness of SiO 2 in Step 1 is between 100 nm and 10 μm.

3. The method for preparing a multilayer metal oxide nano-porous film gas sensitive material according to claim 1 , wherein in Step 2, the flow rate of the fed plasma gas O 2 is controlled to be 40 sccm, the pressure in the reaction cavity is controlled to be 37 mTorr, the power applied to excite the O 2 plasma is controlled to be 90 W, and the O 2 plasma etching time is controlled to be 1 min.

4. The method for preparing a multilayer metal oxide nano-porous film gas sensitive material according to claim 1 , wherein in Step 3, the target material used for magnetron sputtering is a ceramics target material of indium oxide or cuprous oxide, the power for exciting the Ar plasma is 80 W, and the pressure in the cavity is 3 mTorr.

Assignees

• Univ Soochow

Inventors

• Sun Xuhui
• Zhang Pingping
• Zhang Shumin

Classifications

• C23C14/086

  of zinc, germanium, cadmium, indium, tin, thallium or bismuth · CPC title

• C23C14/087

  of copper or solid solutions thereof · CPC title

• C23C14/352 Primary

  using more than one target (C23C14/56 takes precedence) · CPC title

• G01N27/127 Primary

  comprising nanoparticles · CPC title

• B82Y15/00

  Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors · CPC title