Method of making inorganic, metal oxide spheres using microstructured molds

Patent metadata

Field	Value
Publication number	US-9527768-B2
Application number	US-201514788863-A
Country	US
Kind code	B2
Filing date	Jul 1, 2015
Priority date	Aug 21, 2006
Publication date	Dec 27, 2016
Grant date	Dec 27, 2016

Abstract

A process for making inorganic, metal oxide spheres that includes exposing solidified, molded microparticles that include a glass precursor composition to a temperature sufficient to transform the molded microparticles into molten glass and cooling the molten glass to form inorganic, metal oxide spheres.

First claim

What is claimed is:

1. A process for making inorganic, metal oxide spheres, the process comprising:
forming a glass precursor composition comprising glass precursor particles dispersed in a vehicle such that the composition forms a dispersion, the vehicle including at least one of water, an organic liquid, and a binder;
positioning the glass precursor composition in a plurality of mold cavities;
solidifying the glass precursor composition in the plurality of mold cavities to form solidified, molded microparticles;
demolding the solidified, molded microparticles from the plurality of mold cavities;
exposing the solidified, molded microparticles, after demolding, to a temperature sufficient to transform the molded microparticles into molten droplets; and
cooling the molten droplets to form inorganic, metal oxide spheres.

2. The process of claim 1 , wherein the inorganic, metal oxide spheres comprise glass.

3. The process of claim 1 , wherein the exposing comprises:
passing the molded microparticles through a chamber having a temperature sufficient to melt the solidified, molded microparticles;
melting the molded microparticles; and
rendering the melted particles substantially spherical.

4. The process of claim 1 , further comprising maintaining the molten droplets at or above the temperature sufficient to transform the molded microparticles into molten droplets for a sufficient period of time, such that the molten droplets form into spherical molten droplets.

5. The process of claim 1 , wherein the exposing comprises exposing the molded microparticles to a temperature of at least 2000K.

6. The process of claim 1 , wherein solidifying the glass precursor composition includes exposing the composition to an energy source to at least partially solidify the composition.

7. The process of claim 1 , wherein the vehicle comprises a binder comprising at least one of cellulose, thermoplastic polymer, and actinic radiation curable resin.

8. The process of claim 1 , wherein each mold cavity defines a volume no greater than about 880,000,000 cubic micrometers.

9. The process of claim 1 , wherein each solidified, molded microparticle has a volume of no greater than 8,000,000,000 μm 3 .

10. The process of claim 1 , wherein the plurality of mold cavities is present on a three-dimensional body having at least one continuous surface comprising a plurality of openings at least some of which provide access to the mold cavities, the mold cavities extending into the three-dimensional body.

11. The process of claim 1 , wherein the glass precursor comprises particles comprising oxides of at least one of silicon, aluminum, zirconium, titanium, boron, lanthanum, sodium, potassium, calcium, magnesium, and barium.

12. The process of claim 1 , wherein the inorganic, metal oxide spheres have an average cross-sectional dimension no greater than about 500 micrometers.

13. The process of claim 1 , wherein the inorganic, metal oxide spheres have an average cross-sectional dimension no greater than 100 micrometers.

14. The process of claim 1 , wherein the molded microparticles exhibit a shape comprising at least one of polyhedron, parallelepiped, diamond, cylinder, arcuate, arcuate terminated cylinder, sphere, hemisphere, gumdrop, bell, cone, and frusto-conical cone.

15. The process of claim 1 , wherein the inorganic, metal oxide spheres have a mean sphere diameter, and wherein the inorganic, metal oxide spheres exhibit an average absolute deviation from the mean sphere diameter of less than 20% prior to a screening step.

16. The process of claim 1 , wherein the inorganic, metal oxide spheres have a mean sphere diameter, and wherein the inorganic, metal oxide spheres exhibit an average absolute deviation from the mean sphere diameter of less than 10% prior to a screening step.

17. The process of claim 1 , wherein the inorganic, metal oxide spheres have an index of refraction of at least about 1.2.

18. The process of claim 1 , wherein the inorganic, metal oxide spheres comprise microbubbles or microbeads.

19. The process of claim 1 , wherein the plurality of mold cavities is formed in a production tool, and wherein the production tool is formed of a polyolefin, a polyamide, a polyimide, a metal, a ceramic, or a combination thereof.

20. The process of claim 1 , wherein the vehicle is present in the glass precursor composition in an amount of at least 20% by weight.

21. The process of claim 1 , wherein placing the glass precursor composition in the plurality of mold cavities includes at least one of partially filling one or more of the plurality of mold cavities and completely filling one or more of the plurality of mold cavities.

22. The process of claim 1 , wherein the plurality of mold cavities includes mold cavities that abut.

23. The process of claim 1 , wherein the plurality of mold cavities includes mold cavities of different shapes, different sizes, or a combination thereof.

24. The process of claim 1 , wherein the glass precursor composition is in the form of a slurry.

25. The process of claim 1 , wherein exposing the solidified, molded microparticles, after demolding, to a temperature sufficient to transform the molded microparticles into molten droplets includes exposing the solidified, molded microparticles, after demolding, to a flame.

26. The process of claim 25 , further comprising adjusting the flame based on a target size of the inorganic, metal oxide spheres.

27. The process of claim 1 , further comprising partially embedding the inorganic, metal oxide spheres in a layer of binder material.

28. A process for making a retroreflective article, the process comprising:
partially embedding the inorganic, metal oxide spheres formed according to the process of claim 1 in a layer of binder material.

29. The process of claim 1 , wherein the molten droplets comprise homogeneous molten droplets.

Assignees

• 3M Innovative Properties Co

Inventors

• Kramlich David C
• Vandenberg John L
• Frey Matthew H
• Culler Scott R
• Schakel-Carlson Kathleen M

Classifications

• C08K2003/2241

  Titanium dioxide · CPC title

• C03C12/02 Primary

  Reflective beads · CPC title

• C08K2003/265

  Calcium, strontium or barium carbonate · CPC title

• G02B5/128

  transparent spheres being embedded in matrix · CPC title

• C08K3/38

  Boron-containing compounds · CPC title