# US 9,039,796 B2 · Method for producing abrasive grains, method for producing slurry, and method for producing polishing liquid

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- Number: US 9,039,796 B2
- Document ID: US9039796B2
- Status: Granted
- Kind: B2
- Application number: 13/582,961
- Filed: 2011-11-21
- Published: 2012-12-27
- Granted: 2015-05-26
- Earliest claimed: 2010-11-22
- Assignees: Hitachi Chemical Company, Ltd.
- Applicants: Tomohiro Iwano; Hisataka Minami; Hirotaka Akimoto
- Inventors: Tomohiro Iwano; Hisataka Minami; Hirotaka Akimoto
- Web page: https://patentgrep.com/patent/US9039796B2

## CPC

- C09G 1/02: containing abrasives or grinding agents {(abrasives as such C09K3/14; polishing of semi-conductors H10P52/40)}
- C09K 3/1409: {Abrasive particles per se (preparation of diamond C01B32/25)}
- C09K 3/1463: {Aqueous liquid suspensions}
- C09K 13/00: Etching, surface-brightening or pickling compositions (for glass C03C15/00, {C03C25/66; for mortars, concrete, artificial or natural stone or ceramics C04B41/5338}; for metallic material C23F, C23G1/00, C25F1/00; {for semi-conductors H10P52/40})
- H10P 95/062: {involving a dielectric removal step}
- C09G: POLISHING COMPOSITIONS (French polish C09F11/00); SKI WAXES
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10

## Abstract

In the production method for abrasive grains according to the invention, an aqueous solution of a salt of a tetravalent metal element is mixed with an alkali solution, under conditions such that a prescribed parameter is 5.00 or greater, to obtain abrasive grains including a hydroxide of the tetravalent metal element.

## Claims

### Claim 1

A production method for abrasive grains, comprising mixing a first liquid, which is an aqueous solution of at least one tetravalent metal element salt, and a second liquid which is a solution of at least one alkali, so as to form a liquid mixture, under conditions such that parameter Z in the following formula (1) is 5.00 or greater, to yield abrasive grains including a hydroxide of the tetravalent metal element, wherein during the mixing the liquid mixture is stirred using a stirring blade, wherein the tetravalent metal element is at least one kind selected from the group consisting of scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, promethium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium, and wherein the alkali is selected from the group consisting of ammonia, triethylamine, pyridine, piperidino, pyrrolidine, imidazole, chitosan, potassium hydroxide and sodium hydroxide:
Z=(1/(ΔpH×k)) ×(N/M)/1000 (1),
wherein in formula (1), ΔpH represents a variation in pH per minute in a reaction system of the liquid mixture, k represents a reaction temperature coefficient represented by the following formula (2), N represents a cycle count (min−1) represented by the following formula (3), and M represents a substitution count (min−1) represented by the following formula (5);
k=2((T−20)/10) (2),
wherein in formula (2), T represents a temperature (° C.) of the reaction system;
N=(u ×S)/Q (3),
wherein in formula (3), u represents a linear speed (m/min) represented by the following formula (4), for the stirring blade stirring the liquid mixture obtained by mixing the first liquid and the second liquid, S represents an area (m2) of the stirring blade, and Q represents a liquid volume (m3) of the liquid mixture;
u=2π×R×r (4),
wherein in formula (4), R represents a rotational speed (min−1) of the stirring blade, and r represents a radius of rotation (m) of the stirring blade; and
M=v/Q (5),
wherein in formula (5), v represents a mixing rate (m3/min) of the first liquid and second liquid, and Q represents a liquid volume (m3) of the liquid mixture, and
wherein:
the ΔpH is in the range of 0.001 to 5.00,
the cycle count N is in the range of 1.00 min−1 to 200.00 min−1,
the substitution count M is in the range of 1.0 ×10−5 min-1 to 1.0 min−1,
the linear speed u is in the range of 5.00 m/min to 200.00 m/min,
the mixing rate v is in the range of 1.00 ×10−7 m3/min to 1.00 ×10−2 m3/min, and
the rotational speed R is in the range of 30 min−1 to 1000 min−1.

### Claim 2 (depends on 1)

The production method according to claim 1, wherein a concentration of the at least one tetravalent metal element salt in the first liquid is 0.01 mol/L or greater.

### Claim 3 (depends on 1)

The production method according to claim 1, wherein an alkaline concentration of the second liquid is not greater than 15.0 mol/L.

### Claim 4 (depends on 1)

The production method according to claim 1, wherein a pH of the liquid mixture, after mixing the first liquid and the second liquid, is 2.0 to 7.0.

### Claim 5 (depends on 1)

The production method according to claim 1, wherein the tetravalent metal element of the at least one tetravalent metal element salt is tetravalent cerium.

### Claim 6 (depends on 1)

A production method for a slurry, wherein abrasive grains obtained by the production method according to claim 1 are mixed with water to obtain a slurry.

### Claim 7 (depends on 6)

A production method for a polishing liquid, wherein a slurry obtained by the production method according to claim 6 is mixed with an additive to obtain a polishing liquid.

### Claim 8 (depends on 1)

A production method for a polishing liquid, wherein abrasive grains obtained by the production method according to claim 1, an additive and water are mixed to obtain a polishing liquid.

### Claim 9 (depends on 5)

A production method for a slurry, wherein abrasive grains obtained by the production method according to claim 5 are mixed with water to obtain a slurry.

### Claim 10 (depends on 9)

A production method for a polishing liquid, wherein a slurry obtained by the production method according to claim 9 is mixed with an additive to obtain a polishing liquid.

### Claim 11 (depends on 5)

A production method for a polishing liquid, wherein abrasive grains obtained by the production method according to claim 5, an additive and water are mixed to obtain a polishing liquid.

### Claim 12 (depends on 1)

The production method according to claim 1, wherein the temperature T is in the range of 0° C. to 60° C.

### Claim 13 (depends on 1)

The production method for abrasive grains according to claim 1, wherein said first liquid is an aqueous solution of a tetravalent metal element salt, and said second liquid is a solution of an alkali.

### Claim 14 (depends on 1)

The production method for abrasive grains according to claim 1, wherein the mixing is conducted so as to react the at least one tetravalent metal element salt with the at least one alkali to obtain the tetravalent metal element hydroxide.

### Claim 15 (depends on 12)

The production method according to claim 12, wherein the liquid volume Q is 0.001 to 10.00 m3, and the radius of rotation r of the stirring blade is in the range of 0.001 m to 10 m.

### Claim 16 (depends on 15)

The production method according to claim 15, wherein the area S of the stirring blade is 0.0005 to 0.0340 m.

### Claim 17 (depends on 1)

The production method according to claim 1, wherein the mean particle size of the abrasive grains formed is 1-200 nm.

### Claim 18 (depends on 1)

The production method according to claim 1, wherein ΔpH is in the range of 0.001 to 1.00.

### Claim 19 (depends on 1)

The production method according to claim 1, wherein the tetravalent metal element is cerium, and the alkali is selected from the group consisting of ammonia and imidazole.