# US 5,352,642 A · Fabrication of Y.sub.3 Al.sub.5 O.sub.12 fibers from water soluble polymers

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- Number: US 5,352,642 A
- Document ID: US5352642A
- Status: Granted
- Kind: A
- Application number: 07/974,040
- Filed: 1992-11-10
- Granted: 1994-10-04
- Earliest claimed: 1992-11-10
- Assignees: The Babcock & Wilcox Company
- Inventors: Sung S. Pak; R. Allen Kimel
- Web page: https://patentgrep.com/patent/US5352642A

## CPC

- C04B 35/62236: {Fibres based on aluminium oxide}
- 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

## Abstract

A method for fabricating Y.sub.3 Al.sub.5 O.sub.12 (YAG) fibers from water soluble polymers includes a pre-YAG polymer synthesis, with solution viscosity adjustment followed by fiber spinning and heat treatment. The polymer synthesis employs polar solvents such as water or alcohol with a carboxylic acid containing at least two carboxyl groups.

## Claims

### Claim 1

A method for making an yttrium-aluminum water soluble polymer, comprising the steps of:
mixing an yttrium salt with an aluminum salt in an yttrium to aluminum molar ratio of about 3 to 5;
adding said yttrium and aluminum salt mixture to a solution containing a polar solvent and an acid having at least two carboxyl groups; and
refluxing said yttrium and aluminum salt solution for a time to allow polymerization among the yttrium and aluminum functional groups, and carboxyl groups for forming the yttrium and aluminum water soluble polymer.

### Claim 2 (depends on 1)

A method as recited in claim 1, wherein the ratio of the total number of carboxyl groups to that of the yttrium and aluminum functional groups is between about 0.1 to about 0.6.

### Claim 3 (depends on 2)

A method as recited in claim 2, further comprising the step of evaporating ligands from the polymer for increasing its viscosity.

### Claim 4 (depends on 1)

A method as recited in claim 1, wherein the refluxing step is performed for about twenty-four hours.

### Claim 5

A method for fabricating yttrium aluminum garnet fibers, comprising the steps of:
forming a water-soluble polymer solution from yttrium and aluminum salts mixed with a polar solvent and an acid having at least two carboxyl groups;
heating the water-soluble polymer solution to adjust the concentration thereof to provide an oxide char yield of at least 20 percent on a weight percent basis and a viscosity of at least 10.sup.5 centipoise; and
fabricating fibers from the adjusted water-soluble polymer in an inert atmosphere.

### Claim 6 (depends on 5)

A method as recited in claim 5, further comprising the step of pyrolyzing the fibers fabricated from the water-soluble polymer.

### Claim 7 (depends on 6)

A method as recited in claim 6, wherein the pyrolyzing step includes heating the fibers in air from room temperature to about 500.degree. C. at about 1.degree. C./minute.

### Claim 8 (depends on 7)

A method as recited in claim 7, further comprising the step of heating the fibers at about 10.degree. C./minute from about 500.degree. C. to about 875.degree. C. and holding at this temperature for about 30 minutes.

### Claim 9 (depends on 5)

A method as recited in claim 5, further comprising the step of heating the fibers at about 10.degree. C./minute from about 875.degree. C. to about 1000.degree. C.

### Claim 10 (depends on 5)

A method as recited in claim 5, wherein the polar solvent is a member selected from the group consisting of water, methanol, ethanol and isopropanol.

### Claim 11 (depends on 5)

A method as recited in claim 5, wherein the acid is a member selected from the group consisting of oxalic, tartaric, and citric acid.

### Claim 12 (depends on 5)

A method as recited in claim 5, wherein the fabricating step produces fibers of approximately 10 to 100 centimeters in length.

### Claim 13 (depends on 5)

A method as recited in claim 5, wherein the step of fabricating fibers includes the step of holding fibers in a zone of NH.sub.3 gas for forming a film on the fiber surface.

### Claim 14

A method for making yttrium aluminum garnet powder, comprising the steps of:
mixing an yttrium salt with an aluminum salt in an yttrium to aluminum molar ratio of about 3 to 5;
adding said yttrium and aluminum salt mixture to a solution containing NH.sub.3 and distilled water at room temperature to produce a precipitate in a suspension;
collecting and washing said precipitate;
drying the precipitate; and
calcining the precipitate to make yttrium aluminum garnet powder.

### Claim 15 (depends on 1)

A method as recited in claim 1 further comprising the steps of adding a yttrium aluminum garnet powder to the yttrium-aluminum water soluble polymer and mixing while heating at a temperature sufficient to allow for reaction and evaporation to make an improved yttrium aluminum garnet water soluble polymer and to raise its oxide char yield to about 60 percent on a weight percent basis.

### Claim 16 (depends on 1)

A method as recited in claim 1, wherein the yttrium salt and aluminum salt is a salt selected from the group consisting of nitrates, chlorides, and acetates.

### Claim 17 (depends on 14)

A method as recited in claim 14, wherein the yttrium salt and aluminum salt is a salt selected from the group consisting of nitrates, chlorides, and acetates.

### Claim 18 (depends on 5)

A method as recited in claim 5, wherein the yttrium salt and aluminum salt is a salt selected from the group consisting of nitrates, chlorides, and acetates.
