IP Library Granted Patent US 10,183,863
Granted Patent B2
US 10,183,863 · App. 15/531,708 · Granted Jan 22, 2019

Porous hollow shell WO

Inventors: Jianfeng Huang (Shaanxi, CN); Xin Wang (Shaanxi, CN); Liyun Cao (Shaanxi, CN); Jiayin Li (Shaanxi, CN); Haibo Ouyang (Shaanxi, CN); Cuiyan Li (Shaanxi, CN); Wei Hao (Shaanxi, CN); Zhanwei Xu (Shaanxi, CN); Jie Fei (Shaanxi, CN); Chunyan Yao (Shaanxi, CN)
Assignee: Shaanxi University of Science & Technology
B82Y30/00B01J13/02C01G41/00C01G41/02H01M4/364H01M4/48H01M4/483H01M4/58H01M4/5815B01J13/0017B01J13/0021B01J13/0039B01J13/0047B01J13/04B22F9/24B82Y40/00C01P2002/72C01P2004/03C01P2004/34C01P2004/64C01P2004/80C01P2006/12C01P2006/16C01P2006/40H01M10/054
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Quick Facts
Patent No.
US 10,183,863
App. No.
15/531,708
Granted
Jan 22, 2019
Kind
B2
Abstract

Provided is a method for the preparation of a porous hollow shell WO 3 /WS 2 nanomaterial, comprising: (1) adding a hexavalent tungsten salt to a sol A comprising mesocarbon microbeads, and stirring to obtain a sol B; (2) drying and grinding the sol B, and then heating a resulting powder at 200-500° C. for 0.5-2 hours to obtain a porous hollow shell WO 3 nanocrystalline material; (3) placing the porous hollow shell WO 3 nanocrystalline material obtained by Step 2 and a sulfur powder separately in a vacuum furnace, controlling such that a degree of vacuum is −0.01 to −0.1 MPa and a temperature is 200-500° C., and reacting for 0.5-3 hours to obtain a WO 3 /WS 2 porous hollow shell nanocrystalline material. Also provided is a porous hollow shell WO 3 /WS 2 nanocrystalline material obtained by the method.

Claims (13)

1. A method for preparing a WO 3 /WS 2 porous hollow shell nanocrystalline anode material, comprising the steps of:

1) adding a hexavalent tungsten salt to a sol A comprising mesocarbon microbeads, and stirring to obtain a sol B, wherein a concentration of the mesocarbon microbeads in the sol A is 0.002˜0.2 g/mL, and a concentration of the W6+in the sol B is 0.01˜2.0 mol/L;

2) drying and grinding the sol B obtained by Step 1, and then heating a resulting powder at 200-500° C. for 0.5-2 hours to obtain a porous hollow shell WO 3 nanocrystalline material; and

3) placing the porous hollow shell WO 3 nanocrystalline material obtained by Step 2 and a sulfur powder separately into a vacuum tube furnace, controlling such that a degree of vacuum is −0.01 to −0.1 MPa and a temperature is 200-500° C., and reacting for 0.5-3 hours to sulfurize some WO 3 of the porous hollow shell WO 3 nanocrystalline material into WS 2 to obtain a WO 3 /WS 2 porous hollow shell nanocrystalline anode material.

2. The method according to claim 1 , characterized in that a solvent of the sol A is at least one of anhydrous ethanol, isopropyl alcohol, ethylene glycol, and distilled water, the sol A further comprises a dispersant, the dispersant being at least one of polyvinyl alcohol, carboxymethylcellulose sodium, lauryl sodium sulfate, and polyethylene glycol, and a concentration of the dispersant in the sol A is 0.006˜0.25 g/mL.

3. The method according to claim 2 , characterized in that the sol A is obtained by adding a dispersant to the solvent and stirring to dissolve, followed by adding the mesocarbon microbeads thereto and stirring to disperse, and then placing a resulting mixture in a 300˜1000 W ultrasonic generator for ultrasonic vibration for 20˜60 minutes.

4. The method according to claim 1 , characterized in that the sol B is obtained by adding the hexavalent tungsten salt to the sol A and stirring, then placing a resulting mixture in a 300˜1000 W ultrasonic generator for ultrasonic vibration and aging for 60˜180 minutes.

5. The method according to claim 1 , characterized in that, in Step 2, the sol B is dried in a vacuum drying oven at 40-70° C. for 2-6 hours, followed by being ground.

6. The method according to claim 1 , characterized in that a mass ratio of the porous hollow shell WO 3 nanocrystalline material to the sulfur powder is 0.1-10 g porous hollow shell WO 3 nanocrystalline material to 0.1-4.0 g sulfur powder.

7. The method according to claim 1 , characterized in that the hexavalent tungsten salt is at least one of tungsten hexachloride, sodium tungstate, ammonium tungstate, and sodium polytungstate.

8. A WO 3 /WS 2 porous hollow shell nanocrystalline anode material obtained by the method according to claim 1 , in which a porous hollow shell presents a honeycomb structure with a pore size of 0.2˜2.0 μm and a shell wall thickness of 40-150 nm, and nanoparticles attached thereon have a particle size of 30-100 nm.

9. The WO 3 /WS 2 porous hollow shell nanocrystalline anode material according to claim 8 , characterized in that a mass ratio of WO 3 to WS 2 in the WO 3 /WS 2 porous hollow shell nanocrystalline anode material is at least 1 part WO 3 to 9 parts WS 2 and at most 9 parts WO 3 to 1 part WS 2 .

10. The WO 3 /WS 2 porous hollow shell nanocrystalline anode material according to claim 8 , characterized in that a specific surface area of the WO 3 /WS 2 porous hollow shell nanocrystalline anode material is 300-700 m 2 /g.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 30, 2017
From: HUANG, JIANFENG; WANG, XIN; CAO, LIYUN; LI, JIAYIN; OUYANG, HAIBO; LI, CUIYAN; HAO, WEI; XU, ZHANWEI; FEI, JIE; YAO, CHUNYAN
To: SHAANXI UNIVERSITY OF SCIENCE & TECHNOLOGY
Reel/Frame 042533/0903 →
Priority Claims (1)
CN 2015 1 0243715 · May 13, 2015 · national
Continuity (1)
Related Publication 20170341935A1 · Nov 30, 2017