Metal oxide macroscopic fiber and preparation method thereof

Patent metadata

Field	Value
Publication number	US-2018258554-A1
Application number	US-201515760254-A
Country	US
Kind code	A1
Filing date	Sep 16, 2015
Priority date	Sep 16, 2015
Publication date	Sep 13, 2018
Grant date	—

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

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

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 − 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.

10 . A metal oxide macroscopic fiber is obtained by the method for preparing metal oxide macroscopic fiber of claim 1 .

Assignees

• Univ Soochow

Inventors

• Geng Fengxia
• Hou Junyu
• Zheng Yuanchuan

Classifications

• D01F9/08

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

• C04B2235/3258

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

• C04B2235/3268

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

• C04B2235/3253

  Substoichiometric niobium or tantalum oxides, e.g. NbO · CPC title

• C04B2235/3255

  Niobates or tantalates, e.g. silver niobate · CPC title