Borosilicate nanoparticles and method for making the same

Patent metadata

Field	Value
Publication number	US-2016376419-A1
Application number	US-201414901476-A
Country	US
Kind code	A1
Filing date	Jun 20, 2014
Priority date	Jun 27, 2013
Publication date	Dec 29, 2016
Grant date	—

Abstract

Borosilicate nanoparticles and method of making borosilicate nanoparticles. Advantages of the method include making the borosilicate nanoparticles at temperatures not greater than 200 C. The nanoparticles made are useful, for example, as fillers in coatings, adhesives, and composite articles.

First claim

1 . A plurality of borosilicate nanoparticles, wherein a majority of the boron of the borosilicate is tetragonally coordinated.

2 . A composite comprising the plurality of borosilicate nanoparticles of claim 1 .

3 . The composite of claim 2 that includes a thermoplastic polymer matrix.

4 . The composite of claim 2 that includes a thermoset polymer matrix.

5 . The composite of claim 2 in the form of a layer.

6 . A method of making borosilicate nanoparticles, the method comprising:
heating at least
(a) at least one of a boron compound selected from a metaborate ester having the formula (RO) 3 (BO) 3 or an alkoxy borane having the formula B(OR) 3 , where R is an alkyl; and
(b) at least one of a silane compound having the formula Si(OR) 4 or a silane compound having the formula RSi(OR′) 3 , where R is an alkyl, phenyl or a reactive group and R′ is a alkyl or phenyl group

at at least one temperature and for a time sufficient to provide boroxine-silane adduct;
acidifying the boroxine-silane adduct to provide a borosilicate network; and
hydrolyzing the borosilicate network with ammonia

to provide the borosilicate nanoparticles.

7 . The method of claim 6 further comprising diluting the boroxine-silane adduct with at least one solvent prior to acidifying the boroxine-silane adduct.

8 . The method of claim 6 , wherein the solvent is at least one of a ketone, ester, alcohol, or chlorocarbon.

9 . The method of claim 6 , wherein acidifying the boroxine-silane adduct is conducted with a carboxylic acid.

10 . The method of claim 6 , wherein the ratio of B to Si in the boroxine-silane adduct is in a range from 0.2 to 1.5.

11 . The method of claim 6 , wherein the heating is conducted at any temperature not greater than 200° C.

12 . The method of claim 6 , wherein the heating is conducted at any temperature not greater than 100° C.

13 . The method of claim 6 , wherein the heating is conducted at any temperature not greater than 50° C.

14 . The method of claim 6 further comprising adding a surfactant of non-ionic, cationic, or anionic to the boroxine-silane adduct prior to providing the borosilicate network.

15 . The method of claim 6 , wherein the nanoparticles have particle sizes in a range in size from 5 nanometers to 1000 nanometers.

16 . The method of claim 6 , wherein a majority of the boron of the borosilicate is tetragonally coordinated.

Assignees

• 3M Innovative Properties Co

Inventors

• Devasenapathi Appuswamy
• Rajagopal Rama V

Classifications

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• C01P2002/82

  by IR- or Raman-data · CPC title

• C09K21/02

  Inorganic materials · CPC title

• C08K2201/005

  Additives being defined by their particle size in general · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title