Method for preparing antibacterial and dust-removal membrane

Patent metadata

Field	Value
Publication number	US-9815029-B2
Application number	US-201515028854-A
Country	US
Kind code	B2
Filing date	Jul 20, 2015
Priority date	Apr 28, 2015
Publication date	Nov 14, 2017
Grant date	Nov 14, 2017

Abstract

This invention discloses a method for preparing an antibacterial and dust-removal membrane. The method comprises the following steps: depositing a layer of nano-ZnO on the immersed membrane surface as the seed crystal with the atomic layer deposition instrument (ALD instrument); vertically immersing the membrane covered with nano-ZnO layer in a hydrothermal reactor filled with crystal growth solution, heating it for a period of time, taking the membrane out and cooling it to the room temperate, and removing it from the substrate; finally, heating this membrane in a drier, and purging it with nitrogen to remove the paraffin within the membrane pore to obtain the porous membrane with nano-ZnO arrays growing on the surface.

First claim

We claim:

1. A method for preparing an antibacterial and dust-removal membrane, comprising:
(1) performing a pretreatment step including: washing an AAO porous membrane with an ethanol solution, and melting a paraffin solution for future use;
(2) performing a pore blocking step including: adhering the pretreated AAO porous membrane on a substrate horizontally to prepare a sample, clamping the sample on a glass slide with a clamping slot, and immersing the glass slide having the sample in the paraffin solution and vibrating, taking the sample out after a period of time, cooling the sample to the room temperature with a surface exposed to the paraffin upward, using a hot smooth iron sheet to remove most of the paraffin on the surface of porous membrane, and removing the residual solid paraffin on the surface through plasma etching;
(3) performing a crystal seeding step including: placing the AAO membrane in the reaction chamber of ALD instrument after it is ultrasonically cleaned with acetone, ethanol and deionized water, using diethylzinc and deionized water as a precursor source respectively to provide zinc and oxygen required for the growth of ZnO, and using high purity nitrogen as a carrier and purging gas, starting deposition after it reaches to 15˜20 Pa, and keeping the deposition for a few hundreds cycles;
(4) performing a crystal growth step including: preparing a mixed solution of hexamethylene tetramine and zinc nitrate of at certain concentration in proportion as a growth solution, pouring the growing solution into a hydrothermal reactor, vertically placing the substrate with the AAO porous membrane covered with ZnO layer in the hydrothermal reactor, placing the hydrothermal reactor in a drier for treatment for a period of time, cooling naturally, taking the membrane out, washing the membrane-with deionized water, and drying it to obtain the porous membrane with nano-ZnO arrays on the surface;
(5) performing a pore cleaning step including: removing the porous membrane obtained in Step (4) from the substrate, horizontally placing the membrane in a drier and ensuring that the side is covered with nano-ZnO arrays upwards, heating for a period of time, purging the membrane with nitrogen, cooling and obtaining a porous membrane with nano-ZnO arrays growing on the surface and having uniform permeable pores.

2. The method for preparing an antibacterial and dust-removal membrane of claim 1 , wherein the pore diameter of AAO porous membrane in Step (1) is 0.1-10 μm; and the mass concentration of the ethanol solution is 80˜95%.

3. The method for preparing an antibacterial and dust-removal membrane of claim 1 , wherein the immersion temperature in Step (2) is 60˜90° C., the immersion time is 3˜5 h; and the temperature of said hot iron sheet is 60˜70° C. and a gas mixture of CH 4 , H 2 and Ar is adopted for said plasma etching, in which the molar ratio of the gases is 1:7:5; the flow of the gas is 26˜78 sccm; a bias power is 80˜90 W; a radio-frequency power is 250˜300 W; etching speed is 10˜25 nm/min, and etching time is 1˜2 h.

4. The method for preparing an antibacterial and dust-removal membrane of claim 1 , wherein pulse time and washing time of said diethylzinc in Step (3) are 0.1˜0.2 s and 3˜4 s respectively; pulse time and washing time of the deionized water are 0.1˜0.2 s and 4˜5 s respectively; the flows of carrier gas of diethylzinc and deionized water respectively are 100˜150 sccm and 150˜200 sccm; temperature of the substrate is 200˜280° C.; and number of times for growing is 100˜200 cycles.

5. The method for preparing an antibacterial and dust-removal membrane of claim 1 , wherein the concentrations of hexamethylene tetramine and zinc nitrate in said mixed solution in Step (4) are both 0.003˜0.1 mol/L; the molar ratio of hexamethylene tetramine and zinc nitrate in the solution is 1:1; and the addition dose of the mixed solution is 100˜500 ml.

6. The method for preparing an antibacterial and dust-removal membrane of claim 1 , wherein the temperature of said drier in Step (4) is 80˜100° C., and the treatment time is 2˜4 h.

7. The method for preparing an antibacterial and dust-removal membrane of claim 1 , wherein the temperature of said drier in Step (5) is 60˜90° C.; the flow rate of nitrogen is 0.4˜0.5 m/s, and the pressure is 0.5˜0.6 MPa.

Assignees

• Nanjing University Of Technology

Inventors

• Zhong Zhaoxiang
• Wu Xibo
• Yao Zhong

Classifications

• B01D67/0051 Primary

  by controlled crystallisation, e,.g. hydrothermal growth · CPC title

• B01D67/009

  with wave-energy, particle-radiation or plasma · CPC title

• B01D67/0083

  Thermal after-treatment · CPC title

• B01D2323/286

  Closing of pores, e.g. for membrane sealing · CPC title

• C23C16/56

  After-treatment · CPC title