Cerium oxide particles, making process thereof and use thereof in chemical mechanical polishing

Patent metadata

Field	Value
Publication number	US-2024158251-A1
Application number	US-202218550272-A
Country	US
Kind code	A1
Filing date	Mar 10, 2022
Priority date	Mar 12, 2021
Publication date	May 16, 2024
Grant date	—

Abstract

The invention relates to cerium oxide particles having a roughness index RI of at least 5, to a making process thereof and to the use thereof in chemical mechanical polishing applications.

First claim

1 . A process for producing cerium oxide particles, comprising the following steps:
(a) contacting, under an inert atmosphere, (i) an aqueous solution of a base, (ii) an aqueous solution comprising NO 3 − , Ce III , optionally CO IV , and (iii) an organic acid or a salt thereof to obtain a mixture, wherein the organic acid is a substituted or unsubstituted, C1-C20 -alkyl, -alkenyl or -alkynyl carboxylic acid; (b) subjecting the mixture obtained in step (a) to a thermal treatment carried out at a temperature ranging from 75° C. to 95° C.; (c) optionally acidifying the mixture obtained in step (b); (d) optionally washing with water the solid material obtained at the end of step (b) or (c); (e) optionally subjecting the solid material obtained at the end of step (d) to a mechanical treatment to deagglomerate the particles.

2 . The process according to claim 1 , wherein the organic acid is a substituted or unsubstituted C1-C12 alkyl carboxylic acid.

3 . (canceled)

4 . (canceled)

5 . (canceled)

6 . (canceled)

7 . (canceled)

8 . (canceled)

9 . (canceled)

10 . (canceled)

11 . (canceled)

12 . (canceled)

13 . (canceled)

14 . (canceled)

15 . (canceled)

16 . (canceled)

17 . (canceled)

18 . Cerium oxide particles characterized in that said particles are spheroidal in shape and exhibit a roughness index RI of at least 2, wherein RI is defined by the formula:

RI
=

TEM
⁢

size

SSA
⁢

size

wherein “TEM size” denotes the average size of the particles measured on transmission electron microscopy images from at least 80 particles and “SSA size” denotes the theoretical average size of the particles according to the following formula:

SSA
⁢

size

=

6

SSA
×
ρ

wherein SSA denotes the BET specific surface area of the particles determined by nitrogen adsorption and ρ denotes the density of cerium(IV) oxide and is equal to 7.22 g/cm 3 and in that said particles exhibit a carbon weight ratio ranging from 0.001 wt % to 5 wt %, in particular from 0.1 wt % to 2.5 wt %.

19 . The cerium oxide particles according to claim 18 , characterized in that said particles exhibit a sphericity ratio SR between 0.8 and 1.0 wherein SR is calculated from the measured perimeter P and area A of the particles projection using the following equation:

SR
=

4
⁢
π
⁢

A

P
2

and determined by a Dynamic Image Analysis (DIA), notably pursuant to ISO 13322-2 (2006).

20 . (canceled)

21 . (canceled)

22 . The cerium oxide particles according to claim 18 , characterized in that said particles exhibit a specific surface area comprised between 15 and 100 m 2 /g.

23 . The cerium oxide particles according to claim 22 characterized in that said particles exhibit a specific surface area comprised between 20 and 40 m 2 /g.

24 . The cerium oxide particles according to claim 18 , characterized in that said particles exhibit an average size from 30 to 500 nm, said average size being measured from TEM images.

25 . The cerium oxide particles according to claim 24 characterized in that said particles exhibit an average size which is comprised between 140 and 300 nm.

26 . The cerium oxide particles according to any one of claim 18 , which are obtained by the process according to comprising the following steps:
(a) contacting, under an inert atmosphere, (i) an aqueous solution of a base, (ii) an aqueous solution comprising NO 3 − , Ce III , optionally Ce IV , and (iii) an organic acid or a salt thereof to obtain a mixture, wherein the organic acid is a substituted or unsubstituted, C1-C20 -alkyl, -alkenyl or -alkynyl carboxylic acid; (b) subjecting the mixture obtained in step (a) to a thermal treatment carried out at a temperature ranging from 75° C. to 95° C.; (c) optionally acidifying the mixture obtained in step (b); (d) optionally washing with water the solid material obtained at the end of step (b) or (c); (e) optionally subjecting the solid material obtained at the end of step (d) to a mechanical treatment to deagglomerate the particles.

27 . A dispersion of cerium oxide particles according to of claim 18 in a liquid medium.

28 . A method of preparing a polishing composition the method comprising the addition of different ingredients other than the cerium oxide particles of claim 26 or a dispersion of the cerium oxide particles in a liquid medium.

29 . A polishing composition comprising the cerium oxide particles characterized in that said particles exhibit a sphericity ratio SR between 0.8 and 1.0, wherein SR is calculated from the measured perimeter P and area A of the particles projection using the following equation:

SR
=

4
⁢
π
⁢

A

P
2

and determined by a Dynamic Image Analysis (DIA), notably pursuant to ISO 13322-2 (2006) or the dispersion of claim 27 .

30 . A method for removing a portion of a substrate, comprising polishing the substrate with a polishing composition according to claim 29 .

31 . The cerium oxide particles according to claim 18 , characterized in that said roughness index RI is of at least 3.5.

32 . The cerium oxide particles according to claim 18 , characterized in that said particles exhibit a carbon weight ratio ranging from 0.1 wt % to 2.5 wt %.

Assignees

• Rhodia Operations

Inventors

• Plissonneau Marie
• Toth Réka
• D'Alencon Lauriane
• Buissette Valérie
• Boudot Mickaël

Classifications

• C01F17/235 Primary

  Cerium oxides or hydroxides · CPC title

• C01F1/00

  Methods of preparing compounds of the metals beryllium, magnesium, aluminium, calcium, strontium, barium, radium, thorium, or the rare earths, in general · CPC title

• C09G1/02

  containing abrasives or grinding agents {(abrasives as such C09K3/14; polishing of semi-conductors H10P52/40)} · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01P2004/51

  Particles with a specific particle size distribution · CPC title