Aerogels, calcined and crystalline articles and methods of making the same

Patent metadata

Field	Value
Publication number	US-10052266-B2
Application number	US-201815895459-A
Country	US
Kind code	B2
Filing date	Feb 13, 2018
Priority date	Oct 10, 2011
Publication date	Aug 21, 2018
Grant date	Aug 21, 2018

Abstract

Aerogel, calcined articles, and crystalline articles comprising ZrO 2 . Exemplary uses of the crystalline metal oxide articles include dental articles (e.g., restoratives, replacements, inlays, onlays, veneers, full and partial crowns, bridges, implants, implant abutments, copings, anterior fillings, posterior fillings, and cavity liner, and bridge frameworks) and orthodontic appliances (e.g., brackets, buccal tubes, cleats, and buttons).

First claim

What is claimed is:

1. A crack-free, calcined metal oxide article comprising a metal oxide; and having x, y, and z dimensions of at least 5 mm, a density in a range from 30 to 95 percent of theoretical density, and an average connected pore size in a range from 10 nm to 100 nm, wherein at least 70 mole percent of the metal oxide is crystalline ZrO 2 , and wherein the crystalline ZrO 2 has an average grain size less than 100 nm.

2. The crack-free, calcined metal oxide article of claim 1 , wherein the crack-free, calcined metal oxide article has x, y, and z dimensions of at least 10 mm.

3. The crack-free, calcined metal oxide article of claim 1 , wherein at least 75 mole percent of the metal oxide is crystalline ZrO 2 .

4. The crack-free, calcined metal oxide article of claim 1 , wherein the metal oxide comprises 1 to 15 mole percent of crystalline Y 2 O 3 .

5. The crack-free, calcined metal oxide article of claim 1 , wherein the metal oxide further comprises at least one of crystalline metal oxides of Y 2 O 3 and La 2 O 3 .

6. The crack-free, calcined metal oxide article of claim 1 , wherein the metal oxide further comprises at least one of crystalline metal oxides of CeO 2 , Pr 2 O 3 , Nd 2 O 3 , Pm 2 O 3 , Sm 2 O 3 , Eu 2 O 3 , Gd 2 O 3 , Tb 2 O 3 , Dy 2 O 3 , Ho 2 O 3 , Er 2 O 3 , Tm 2 O 3 , Yb 2 O 3 , Fe 2 O 3 , MnO 2 , Co 2 O 3 , Cr 2 O 3 , NiO, CuO, Bi 2 O 3 , Ga 2 O 3 , and Lu 2 O 3 .

7. The crack-free, calcined metal oxide article of claim 1 , wherein the metal oxide further comprises at least one of crystalline metal oxides of Fe 2 O 3 , MnO 2 , Co 2 O 3 , Cr 2 O 3 , NiO, CuO, Bi 2 O 3 , Ga 2 O 3 , Er 2 O 3 , Pr 2 O 3 , Eu 2 O 3 , Dy 2 O 3 , Sm 2 O 3 , and CeO 2 .

8. The crack-free, calcined metal oxide article of claim 1 , wherein the metal oxide further comprises crystalline Al 2 O 3 .

9. The crack-free, calcined metal oxide article of claim 1 having a sulfate equivalent less than 5 ppm and a chloride equivalent less than 5 ppm.

10. A method of making a crack-free, calcined metal oxide article comprising a metal oxide; and having x, y, and z dimensions of at least 5 mm, a density in as range from 30 to 95 percent of theoretical density, and an average connected pore size in a range from 10 nm to 100 nm, wherein at least 70 mole percent of the metal oxide is crystalline ZrO 2 , and wherein the crystalline ZrO 2 has an average grain size less than 100 nm, the method comprising heating a monolithic aerogel for a time and at a temperature sufficient to provide the crack-free, calcined metal oxide article, wherein the monolithic aerogel comprises organic material and crystalline metal oxide particles, wherein the crystalline metal oxide particles are in a range from 3 to 20 volume percent, based on the total volume of the monolithic aerogel, wherein at least 70 mole percent of the crystalline metal oxide particles is ZrO 2 .

11. The method of claim 10 , further comprising chemically treating the calcined metal oxide to remove volatile ions.

12. The method of claim 10 , further comprising chemically treating the calcined metal oxide article to remove chloride ions or sulfate ions.

13. The method of claim 10 , wherein the crystalline metal oxide particles further comprises at least one of Y 2 O 3 and La 2 O 3 .

14. The method of claim 10 , wherein the aerogel has a surface area in a range of 100 to 300 m 2 /g.

Assignees

• 3M Innovative Properties Co

Inventors

• Kolb Brant U
• Feisel Bryan C
• Goetzinger Martin
• Hall Philip S
• Hauptmann Holger
• Hendrickson Mark J
• Humpal Kathleen M
• Longabach John W
• Mathers James P
• Naujok Roberta R
• Pennington Paul D
• Schechner Gallus

Classifications

• A61K6/887

  Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds · CPC title

• A61K6/818 Primary

  comprising zirconium oxide · CPC title

• A61K6/822

  comprising rare earth metal oxides · CPC title

• A61K6/824

  comprising transition metal oxides · CPC title

• C01G25/00 Primary

  Compounds of zirconium · CPC title