Zirconia-based particles doped with a lanthanide element

Patent metadata

Field	Value
Publication number	US-9950932-B2
Application number	US-201013512107-A
Country	US
Kind code	B2
Filing date	Dec 21, 2010
Priority date	Dec 29, 2009
Publication date	Apr 24, 2018
Grant date	Apr 24, 2018

Abstract

Zirconia-based particles, sols containing the zirconia-based particles, methods of making the sols and the zirconia-based particles, composites containing the zirconia-based particles in an organic matrix, and sintered bodies prepared from the zirconia-based particles are described. The zirconia-based particles are crystalline, have a primary particles size no greater than 100 nanometers, and are doped with a lanthanide element or with both a lanthanide element and yttrium.

First claim

We claim:

1. A zirconia-based particles comprising: a) 0.02 to 20 mole percent lanthanide element oxide based on total moles of inorganic oxide in the zirconia-based particles; b) 0.1 to 15 mole percent yttrium oxide based on total moles of inorganic oxide in the zirconia-based particles; and c) at least 80 mole percent zirconium oxide based on total moles of inorganic oxide in the zirconia-based particles; and wherein the zirconia-based particles are crystalline, doped with lanthanide element and yttrium, and have a volume-average size that is no greater than 50 nanometers, and wherein the zirconia-based particles are discrete and have an organic material sorbed on a surface in an amount up to 15 weight percent based on the weight of the zirconia-based particles.

2. The zirconia-based particles of claim 1 , wherein the zirconia-based particles have an average primary particle size that is no greater than 50 nanometers.

3. The zirconia-based particles of claim 1 , wherein the zirconia-based particles have an average primary particle size that is no greater than 30 nanometers.

4. The zirconia-based particles of claim 1 , wherein the zirconia-based particles comprise 0.1 to 10 mole percent lanthanide element oxide.

5. The zirconia-based particles of claim 1 , wherein the zirconia-based particles comprise 0.1 to 10 mole percent lanthanide element oxide and 1 to 15 mole percent yttrium oxide.

6. The zirconia-based particles of claim 1 , wherein the zirconia-based particles comprise 0.5 to 5 mole percent lanthanide element oxide and 5 to 15 mole percent yttrium oxide.

7. The zirconia-based particles of claim 1 , wherein the zirconia-based particles comprise 1 to 7 mole percent lanthanide element oxide and 1 to 7 mole percent yttrium oxide.

8. The zirconia-based particles of claim 1 , wherein the zirconia-based particles have a Z-average particle size determined by Photon Correlation Spectroscopy that is no greater than 70 nanometers.

9. The zirconia-based particles of claim 1 , wherein the zirconia-based particles have a crystal structure that is at least 70 percent cubic, tetragonal, or a combination thereof.

10. A sol comprising at least 3 weight percent of zirconia-based particles dispersed, suspended, or a combination thereof in an aqueous medium, the zirconia-based particles comprising: a) 0.02 to 20 mole percent lanthanide element oxide based on total moles of inorganic oxide in the zirconia-based particles; b) 0.1 to 15 mole percent yttrium oxide based on total moles of inorganic oxide in the zirconia-based particles; and c) at least 80 mole percent zirconium oxide based on total moles of inorganic oxide in the zirconia-based particles; and wherein the zirconia-based particles are crystalline, doped with lanthanide element and yttrium, and have a volume-average size that is no greater than 50 nanometers, wherein the zirconia-based particles are discrete and have an organic material sorbed on a surface in an amount up to 15 weight percent based on the weight of the zirconia-based particles, and wherein less than 5 weight percent of the zirconia-based particles in the sol settle when the sol is stored for one week at room temperature.

11. The sol of claim 10 , wherein the zirconia-based particle have an average primary particle size that is no greater than 50 nanometers.

12. The sol of claim 10 , wherein the zirconia-based particle have an average primary particle size that is no greater than 30 nanometers.

13. The sol of claim 10 , wherein the zirconia-based particles have a crystal structure that is at least 70 percent cubic, tetragonal, or a combination thereof.

14. A method of making a zirconia-based particles, the method comprising: preparing a feedstock comprising multiple salts dissolved, suspended, or a combination thereof in an aqueous-based medium, the multiple salts comprising a zirconium salt, a lanthanide element salt, and a yttrium salt, wherein the feedstock is acidic and wherein a majority of the multiple salts are carboxylate salts; subjecting the feedstock to a hydrothermal treatment to form a sol comprising at least 3 weight percent zirconia-based particles, wherein the zirconia-based particles comprise a) 0.02 to 20 mole percent lanthanide element oxide based on total moles of inorganic oxide in the zirconia-based particles; b) 0.1 to 15 mole percent yttrium oxide based on total moles of inorganic oxide in the zirconia-based particles; and c) at least 80 mole percent zirconium oxide based on total moles of inorganic oxide in the zirconia-based particles; and wherein the zirconia-based particles are crystalline, doped with lanthanide element and yttrium, and have a volume-average size that is no greater than 50 nanometers, wherein the zirconia-based particles are discrete and have an organic material sorbed on a surface in an amount up to 15 weight percent based on the weight of the zirconia-based particles, and wherein less than 5 weight percent of the zirconia-based particles in the sol settle when the sol is stored for one week at room temperature.

15. The method of claim 14 , which further comprises subjecting the sol to dialysis, distillation, diafiltration, or a combination thereof to at least partially remove a by-product of the hydrothermal treatment, wherein the by-product comprises a dissolved carboxylic acid, carboxylate anion, or mixture thereof.

16. A composite material comprising a zirconia-based particles dispersed, suspended, or a combination thereof in an organic matrix, the zirconia-based particles comprising: a) 0.02 to 20 mole percent lanthanide element oxide based on total moles of inorganic oxide in the zirconia-based particles; b) 0.1 to 15 mole percent yttrium oxide based on total moles of inorganic oxide in the zirconia-based particles; and c) at least 80 mole percent zirconium oxide based on total moles of inorganic oxide in the zirconia-based particles; and wherein the zirconia-based particles are crystalline, doped with lanthanide element and yttrium, and have a volume-average size that is no greater than 50 nanometers, and wherein the zirconia-based particles are discrete and have an organic material sorbed on a surface an amount up to 15 weight percent based on the weight of the zirconia-based particles.

17. A sintered body comprising a product formed by sintering a zirconia-based particles, the zirconia-based particles comprising a) 0.02 to 20 mole percent lanthanide element oxide based on total moles of inorganic oxide in the zirconia-based particles; b) 0.1 to 15 mole percent yttrium oxide based on total moles of inorganic oxide in the zirconia-based particles; and c) at least 80 mole percent zirconium oxide based on total moles of inorganic oxide in the zirconia-based particles; and wherein the zirconia-based particles are crystalline, doped with lanthanide element and yttrium, and have a volume-average size that is no greater than 50 nanometers, and wherein the zirconia-based particles have an organic material sorbed on a surface in an amount up to 15 weight percent based on the weight of the zirconia-based particles.

Assignees

• Kolb Brant U
• Hendrickson Mark J
• Mathers James P
• Humpal Kathleen M
• Sharma Neeraj
• Brostrom Myles L
• 3M Innovative Properties Co

Inventors

• Kolb Brant U
• Hendrickson Mark J
• Mathers James P
• Humpal Kathleen M
• Sharma Neeraj
• Brostrom Myles L

Classifications

• C04B2235/6562

  Heating rate · CPC title

• C08K3/22

  of metals · CPC title

• C01G25/00 Primary

  Compounds of zirconium · CPC title

• C01P2002/60

  Compounds characterised by their crystallite size · CPC title

• C04B2235/443

  Nitrates or nitrites · CPC title