Controlled microwave assisted synthesis of functionalized silica nanoparticles

Patent metadata

Field	Value
Publication number	US-10919777-B2
Application number	US-201815981248-A
Country	US
Kind code	B2
Filing date	May 16, 2018
Priority date	May 31, 2013
Publication date	Feb 16, 2021
Grant date	Feb 16, 2021

Abstract

A functionalized fiber. The functionalized fiber includes a fiber strand and silica nanoparticles at least partially encapsulating the fiber strand. The silica nanoparticles are synthesized by hydrolyzing a tetramethyl orthosilicate in hydrochloric acid to form silicic acid monomers. The silicic acid monomers are diluted in acetone and irradiated for a time that is less than 90 seconds with an energy source configured to generate microwave frequency energy to polymerize the silicic acid monomers into the silica nanoparticles.

First claim

What is claimed is:

1. A functionalized fiber comprising:
a fiber strand; and
silica nanoparticles at least partially encapsulating the fiber strand, the silica nanoparticles being synthesized by:
hydrolyzing a tetramethyl orthosilicate in hydrochloric acid to form silicic acid monomers;
diluting the silicic acid monomers in acetone;
irradiating the diluted silicic acid monomers for a time that is less than 90 seconds with an energy source configured to generate microwave frequency energy to polymerize the silicic acid monomers into the silica nanoparticles; and
complexing the silica nanoparticles with molybdenum by preparing a molybdic acid solution and titrating the silica nanoparticles with the molybdic acid solution.

2. The functionalized fiber of claim 1 , wherein the fiber strand comprises cotton.

3. The functionalized fiber of claim 1 , wherein the fiber strand comprises nanofiber.

4. The functionalized fiber of claim 1 , wherein the synthesis further comprises:
introducing a dopant to the silica nanoparticles before irradiating.

5. A functionalized fiber comprising:
a fiber strand;
a coating about at least a portion of the fiber strand, the coating comprising a first plurality of silica nanoparticles and a second plurality of silica nanoparticles that is not the first plurality of silica nanoparticles.

6. The functionalized fiber of claim 5 , wherein the first plurality of silica nanoparticles, the second plurality of silica nanoparticles, or both includes a dopant selected from the group consisting of a metal, a biocide, a chromophore, or flame retardant, or a semiconductor.

7. The functionalized fiber of claim 5 , wherein the first plurality of silica nanoparticles, the second plurality of silica nanoparticles, or both is synthesized from a water-soluble microwave reactive silicon species.

8. The functionalized fiber of claim 7 , wherein the water-soluble microwave reactive silicon species is tetraethyl orthosilicate or tetramethylorthosilicate.

9. The functionalized fiber of claim 5 , where the coating is synthesized by:
hydrolyzing a first water-soluble microwave reactive silicon species in acid to form first silicic acid monomers;
hydrolyzing a second water-soluble microwave reactive silicon species in acid to form second silicic acid monomers;
diluting the first and second silicic acid monomers in acetone; and
irradiating the first and second diluted silicic acid monomers for a time that is less than 90 seconds with an energy source configured to generate microwave frequency energy to polymerize the first and second silicic acid monomers into the first and second pluralities of silica nanoparticles, respectively.

Assignees

• Us Gov Air Force
• Us Air Force

Inventors

• Owens Jeffery Ray
• Lovingood Derek

Classifications

• C01B33/14 Primary

  Colloidal silica, e.g. dispersions, gels, sols · CPC title

• C01B33/18

  Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof (preparation of aerogels by dehydrating gels C01B33/158; treatment to enhance the pigmenting or filling properties C09C) · CPC title

• Y10T428/2933

  Coated or with bond, impregnation or core · CPC title

• D06M11/79

  with silicon dioxide, silicic acids or their salts · CPC title

• C01G39/02 Primary

  Oxides; Hydroxides · CPC title