# US 4,399,232 A · Continuous inorganic fibers and process for production thereof

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- Number: US 4,399,232 A
- Document ID: US4399232A
- Status: Granted
- Kind: A
- Application number: 06/382,320
- Filed: 1982-05-26
- Granted: 1983-08-16
- Earliest claimed: 1979-06-28
- Assignees: Ube Industries, Ltd.
- Inventors: Seishi Yajima; Kiyohito Okamura; Yoshio Hasegawa; Takemi Yamamura
- Web page: https://patentgrep.com/patent/US4399232A

## CPC

- C04B 35/62272: {based on non-oxide ceramics (carbon nanotubes C01B32/15; carbon fibers D01F9/12)}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C01B 32/956: Silicon carbide
- C01B 32/977: Preparation from organic compounds containing silicon
- C03C 13/00: Fibre or filament compositions (manufacture of fibres or filaments C03B37/00)
- C04B 35/571: obtained from {Si-containing} polymer precursors {or organosilicon monomers}
- C04B 35/6325: {based on organo-metallic compounds}
- C08G 77/42: Block-or graft-polymers containing polysiloxane sequences (polymerising aliphatic unsaturated monomers on to a polysiloxane C08F283/12)
- C08G 77/60: in which all the silicon atoms are connected by linkages other than oxygen atoms
- C08G 79/00: Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon {with or without the latter elements in the main chain of the macromolecule}
- C08G 81/00: Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers (involving only carbon-to-carbon unsaturated bond reactions C08F299/00 {; polyester-amides C08G69/44; polyester-imides C08G73/16; polyamides-imides C08G73/14; block- or graft polymers containing polysiloxane sequences C08G77/42})
- D01F 9/10: by decomposition of organic substances (D01F9/12 takes precedence)
- C01P 2002/54: one element only
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/10: extending in one dimension, e.g. needle-like
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2006/90: Other properties not specified above
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- D01F: CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Continuous inorganic fibers consisting substantially of Si, Ti and C and optionally of O, said fibers being composed of (1) an amorphous material consisting substantially of Si, Ti and C and optionally of O, or (2) an aggregate consisting substantially of ultrafine crystalline particles of .beta.-SiC, TiC, a solid solution of .beta.-SiC and TiC and TiC.sub.1-x wherein 0<x<1 and having a particle diameter of not more than 500 A, in which amorphous SiO.sub.2 and TiO.sub.2 sometimes exist in the neighborhood of these ultrafine crystalline particles, or (3) a mixture of said amorphous material (1) and said aggregate (2) of ultrafine crystalline particles. The aforesaid continuous inorganic fibers can be produced by the following steps: a first step of preparing a semi-inorganic block copolymer comprising polycarbosilane blocks having a main chain skeleton composed mainly of carbosilane units of the formula --Si-CH.sub.2 --, each silicon atom of said carbosilane units having bonded thereto a side-chain group selected from the class consisting of hydrogen, lower alkyl and phenyl, and titanoxane units of the formula --Ti--O--; a second step of preparing a spinning dope of said semi-inorganic block copolymer; a third step of subjecting the resulting fibers to a treatment of rendering them infusible under tension or under no tension; and a fourth step of firing the infusible fibers at a temperature of 800.degree. to 1800.degree. C. in vacuum or in an atmosphere of an inert gas or a reducing gas.

## Claims

### Claim 1

Continuous inorganic fibers consisting substantially of Si, Ti and C and optionally of O, said fibers being composed of
(1) an amorphous material consisting substantially of Si, Ti and C and optionally of O, or
(2) an aggregate consisting substantially of ultrafine crystalline particles of .beta.-SiC, TiC, a solid solution of .beta.-SiC and TiC and TiC.sub.1-x wherein 0<x<1 and having a particle diameter of not more than 500 A, in which amorphous SiO.sub.2 and TiO.sub.2 sometimes exist in the neighborhood of these ultrifine crystalline particles, or
(3) a mixture of said amorphous material (1) and said aggregate (2) of ultrafine crystalline particles.

### Claim 2 (depends on 1)

The fibers of claim 1 which consist substantially of an amorphous material composed substantially of Si, Ti and C.

### Claim 3 (depends on 1)

The fibers of claim 1 which consist substantially of an amorphous material composed substantially of Si, Ti, C and O.

### Claim 4 (depends on 1)

The fibers of claim 1 which consist substantially of an aggregate of ultrafine crystalline particles of .beta.-SiC, TiC, a solid solution of .beta.-SiC and TiC and TiC.sub.1-x wherein 0<x<1 and having a particle diameter of not more than 500 A.

### Claim 5 (depends on 1)

The fibers of claim 1 which consist substantially of an aggregate of ultrafine crystalline particles of .beta.-SiC, TiC, a solid solution of .beta.-SiC and TiC and TiC.sub.1-x wherein 0<x<1 and having a particle diameter of not more than 500 A, in which amorphous SiO.sub.2 and TiO.sub.2 exist in the neighborhood of the ultrafine crystalline particles.

### Claim 6 (depends on 1)

The fibers of claim 1 which consist of a mixture of an amorphous material composed substantially of Si, Ti and C and an aggregate composed substantially of ultrafine crystalline particles of .beta.-SiC, TiC, a solid solution of .beta.-SiC and TiC and TiC.sub.1-x wherein 0<x<1 and having a particle diameter of not more than 500 A.

### Claim 7 (depends on 1)

The fibers of claim 1 which consist of a mixture of an amorphous material composed substantially of Si, Ti, C and O and an aggregate composed substantially of ultrafine crystalline particles of .beta.-SiC, TiC, a solid solution of .beta.-SiC and TiC and TiC.sub.1-x wherein 0<x<1 and having a particle diameter of not more than 500 A, in which amorphous SiC.sub.2 and TiO.sub.2 exist in the neighborhood of the ultrafine crystalline particles.