Producing semi-crystalline pulverulent polycarbonate and use thereof in additive manufacturing

Patent metadata

Field	Value
Publication number	US-11634546-B2
Application number	US-202117190030-A
Country	US
Kind code	B2
Filing date	Mar 2, 2021
Priority date	Mar 3, 2020
Publication date	Apr 25, 2023
Grant date	Apr 25, 2023

Abstract

Ways of preparing a partially crystalline polycarbonate powder are provided that include dissolving an amorphous polycarbonate in a polar aprotic solvent to form a first solution of solubilized polycarbonate at a first temperature. The first solution is then cooled to a second temperature, the second temperature being lower than the first temperature, where a portion of the solubilized polycarbonate precipitates from the first solution to form a second solution including the partially crystalline polycarbonate powder. Certain partially crystalline polycarbonate powders resulting from such methods are particularly useful in additive manufacturing processes, including powder bed fusion processes.

First claim

What is claimed is:

1. A method of preparing a partially crystalline polycarbonate powder, the method comprising:
dissolving an amorphous polycarbonate in a polar aprotic solvent to form a first solution of solubilized polycarbonate at a first temperature below the boiling point of the solvent; and
cooling the first solution to a second temperature, the second temperature being lower than the first temperature, wherein a portion of the solubilized polycarbonate precipitates from the first solution to form a slurry comprised of the partially crystalline polycarbonate powder and a less-than-saturated or saturated solution of the polycarbonate, the second temperature being room temperature.

2. The method of claim 1 , further comprising separating the partially crystalline polycarbonate powder from the slurry.

3. The method of claim 2 , wherein, prior to or during the separating, a low molecular weight miscible solvent that does not dissolve the polycarbonate is added to the slurry.

4. The method of claim 3 , wherein the low molecular weight miscible solvent is a C 1 to C 4 alcohol and the separation is performed using filtration.

5. The method of claim 1 , further comprising repeating the dissolving step using the remainder of the second solution as the polar aprotic solvent and repeating the cooling step to form the second solution including another partially crystalline polycarbonate powder, wherein at least a portion of the polycarbonate dissolved is leftover from the prior dissolving and precipitating.

6. The method of claim 1 , wherein the polar aprotic solvent is comprised of one or more of the following: dimethyl sulfoxide; diphenyl ether; or anisole.

7. The method of claim 1 , wherein the dissolving step includes heating the amorphous polycarbonate in the polar aprotic solvent to form the first solution of solubilized polycarbonate at the first temperature, the first temperature being greater than room temperature.

8. The method of claim 7 , wherein the cooling step includes cooling the first solution to the second temperature at a cooling rate, the second temperature being room temperature and the cooling rate being at most about 5° C./min.

9. The method of claim 1 , wherein the partially crystalline polycarbonate powder has one or more of: (i) a D 90 particle size of less than about 150 μm, (ii) a D 10 of at least 10 μm or (iii) an average particle size of about 30 μm to about 40 μm.

10. The method of claim 9 , wherein the partially crystalline polycarbonate powder has at least about 90% of the particles by number having a circularity of 0.65 or greater.

11. The method of claim 10 , wherein the partially crystalline polycarbonate powder has a crystallinity of at least about 20% to 35%.

12. A powder composition comprising a partially crystalline polycarbonate powder having a D 90 particle size of less than about 150 μm, an average particle diameter from about 30 μm to about 40 μm, and a crystallinity between about 20% and about 35%.

13. The powder composition of claim 12 , wherein the partially crystalline polycarbonate powder has a flowability of at least about 0.5 g/s as determined by Method A of ASTM D 1895 using a 15 mm nozzle.

14. The powder composition of claim 12 , wherein the partially crystalline polycarbonate powder has a circularity such that at least about 90% of the particles by number have a circularity of 0.65 or greater.

15. An object prepared by an additive manufacturing process comprising:
fusing the powder composition of claim 12 in a powder bed fusion process to form the object.

16. The method of claim 1 , wherein the concentration of the polycarbonate in the first solution is about 5% to about 30% by weight.

17. The powder composition of claim 12 , wherein the partially crystalline polycarbonate powder has a D 10 of at least 10 μm.

18. The method of claim 1 , wherein the first temperature is from about 100° C. to 150° C.

19. The method of claim 18 , wherein the first temperature is at most about 145° C.

20. The method of claim 1 , wherein the dissolving and cooling are carried out under a pressure within 1% of atmospheric pressure.

Assignees

• Jabil Inc

Inventors

• Gardner Thomas
• Hislop Travis
• Pyle Victoria H

Classifications

• B33Y40/10

  Pre-treatment · CPC title

• B29C64/153

  using layers of powder being selectively joined, e.g. by selective laser sintering or melting · CPC title

• C08J2369/00

  Characterised by the use of polycarbonates; Derivatives of polycarbonates · CPC title

• C08G64/40

  Post-polymerisation treatment · CPC title

• B29C64/314

  Preparation · CPC title