Metal oxide macroscopic fiber and preparation method thereof

Patent metadata

Field	Value
Publication number	US-10655245-B2
Application number	US-201515760254-A
Country	US
Kind code	B2
Filing date	Sep 16, 2015
Priority date	Sep 16, 2015
Publication date	May 19, 2020
Grant date	May 19, 2020

Abstract

A metal oxide macroscopic fiber and a preparation method thereof, the method including: adding, as a spinning dope, an anionic metal oxide aqueous colloidal solution into wet spinning equipment, extruding the spinning dope from the spinning equipment into a thread, injecting the extruded thread into a coagulating bath containing a flocculating agent to obtain as-spun fiber, and repeatedly washing the resulted as-spun fiber with deionized water and drying same, thereby obtaining a metal oxide fiber. Said method makes the process simple and controllable, being adaptable to production on a large scale. The prepared metal oxide fiber having special physical and chemical properties is widely applicable in terms of intelligent spinning, biomedicine, energy recycling and conversion, and the field of microelectronic devices and the like.

First claim

The invention claimed is:

1. A method for preparing metal oxide macroscopic fiber, characterized in that it comprises the following steps:
providing an anionic metal oxide colloidal aqueous solution;
obtaining an as-spun fiber by wet spinning the anionic metal oxide colloidal aqueous solution in a coagulating bath; and
washing the as-spun fiber with deionized water and drying the same, thereby obtaining the metal oxide macroscopic fiber;
wherein said coagulation bath contains a flocculant with the mass fraction being between 0.5% to 5%, and speed of the wet spinning is between 0.1 ml/min to 5 ml/min; the anionic metal oxide colloidal aqueous solution consists of 0.1 mg/ml to 20 mg/ml of anionic metal oxide dispersed in water.

2. The method for preparing metal oxide macroscopic fiber of claim 1 , wherein the anionic metal oxide is manganese oxide, ruthenium oxide, titanium oxide, niobium oxide, tantalum oxide, tungsten oxide, cesium tungsten oxide, calcium niobium oxide, titanium niobium oxide or a mixture thereof.

3. The method for preparing metal oxide macroscopic fiber of claim 2 , wherein the manganese oxide is MnO 2 x− , 0<x<1, or A 2 Na y−3 MnO 3y+1 − , in which A is Ca, Sr, Ba, 3≤y≤6, said tantalum oxide is TaO 3− , SrTa 2 O 7 2− , La 0.7 Tb 0.3 Ta 2 O 7 − or Eu 0.56 Ta 2 O 7 2− , said tungsten oxide is W 2 O 7 2− , said cesium tungsten oxide is Cs 4 W 11 O 36 2− , said ruthenium oxide is RuO 2.1 z− or RuO 2 z− , 0<z<1, said niobium oxide is Nb 6 O 17 4− , Nb 3 O 8 − , LaNb 2 O 7 − or La 0.9 Eu 0.05 Nb 2 O 7 − , said titanium oxide is Ti 1-n O 2 4n− , 0<n<1, Ti 0.8 Co 0.2 O 2 0.4− , Bi 4 Ti 3 O 12 2− , Ti 0.6 Fe 0.4 O 2 0.4− , Ti 0.8−m/4 Fe m/2 Co 0.2−m/4 O 2 0.4− , 0≤m≤0.8, Ti (5.2−2i)/6 Mn i/2 O 2 (3.2−1)/6− , 0≤i≤0.4 or RE 2 Ti 3 O 10 2− , in which RE is La, Pr, Sm, Nd, Eu, Gd, Tb or Dy, said calcium niobium oxide is Ca 2 Nb 3 O 10 − , said titanium niobium oxide is TiNbO 5 − , Ti 2 NbO 7 − or Ti 5 NbO 14 3− .

4. The method for preparing metal oxide macroscopic fiber of claim 3 , wherein the anionic metal oxide is Ti 0.87 O 2 0.52− , W 2 O 7 2− , TiNb 6 O 5 5− , Ca 2 Nb 3 O 10 − , TaO 3− , Nb 6 O 17 4− , Nb 3 O 8 − , RuO 2.1 0.2− , RuO 2 0.2− , SrTa 2 O 7 2− , LaNb 2 O 7 − , Cs 4 W 11 O 36 2− or a mixture thereof.

5. The method for preparing metal oxide macroscopic fiber of claim 1 , wherein the coagulating bath comprises water, methanol, ethanol, acetone or a mixture thereof.

6. The method for preparing metal oxide macroscopic fiber of claim 1 , wherein the flocculant is lanthanum salt, aluminum salt, ferric salt, copper salt, calcium salt, magnesium salt, zinc salt, sodium salt, Lithium salt, potassium salt, acetic acid, polyvinyl alcohol, polyethylene glycol, cellulose, chitosan, sodium dodecylsulphate, cetyl trimethyl ammonium bromide, concentrated sulfuric acid, or mixture thereof.

7. The method for preparing metal oxide macroscopic fiber of claim 6 , wherein the flocculant is lanthanum chloride, aluminum chloride, ferric nitrate, copper sulphate, calcium chloride, magnesium sulphate, zinc chloride, sodium chloride, lithium fluoride, potassium sulphate, acetic acid, cellulose, polyethylene glycol, chitosan, sodium dodecylsulphate, cetyl trimethyl ammonium bromide, or a mixture thereof.

8. The method for preparing metal oxide macroscopic fiber of claim 1 , wherein the as-spun fiber is washed by deionized water after drawing, and the draw ratio is between 2 to 8.

9. The method for preparing metal oxide macroscopic fiber of claim 1 , wherein the as-spun fiber is washed by deionized water until the pH of washing waste water is 7, and the conditions for drying are drying for 0.5 h to 72.0 h between 15° C. to 80° C.

Assignees

• Univ Soochow

Inventors

• Geng Fengxia
• Hou Junyu
• Zheng Yuanchuan

Classifications

• C04B35/6264

  Mixing media, e.g. organic solvents · CPC title

• C04B2235/3289

  Noble metal oxides · CPC title

• C04B2235/3268

  Manganates, manganites, rhenates or rhenites, e.g. lithium manganite, barium manganate, rhenium oxide · CPC title

• C04B2235/3258

  Tungsten oxides, tungstates, or oxide-forming salts thereof · CPC title

• D01F9/08

  of inorganic material (working or processing of metal wire B21F; from softened glass, minerals or slags C03B37/00) · CPC title