IP Library Granted Patent US 11,913,092
Granted Patent B2
US 11,913,092 · App. 17/258,136 · Granted Feb 27, 2024

Magnesium-based alloy foam

Inventors: Kicheol Hong (Busan, KR); Hyeji Park (Seoul, KR); Teakyung Um (Seoul, KR); Heeman Choe (Walnut Creek, CA)
Assignee: CellMo Materials Innovation, Inc.
C22C1/08B22F1/06B22F1/10B22F3/11B22F3/222C22C23/00C22C23/02C22C23/04C22C23/06B22F3/10B22F2202/01B22F2301/058B22F2998/10C22C1/087
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Quick Facts
Patent No.
US 11,913,092
App. No.
17/258,136
Granted
Feb 27, 2024
Kind
B2
Abstract

Morphology, microstructure, compressive behavior, and biocorrosive properties of magnesium or magnesium alloy foams allow for their use in biodegradable biomedical, metal-air battery electrode, hydrogen storage, and lightweight transportation applications. Magnesium or Mg alloy foams are usually very difficult to manufacture due to the strong oxidation layer around the metallic particles; however, in this invention, they can be synthesized via a camphene-based freeze-casting process with the addition of graphite powder using precisely controlled heat-treatment parameters. The average porosity ranges from 45 to 85 percent and the median pore diameter is about a few tens to hundreds of microns, which are suitable for bio and energy applications utilizing their enhanced surface area. This invention based on powder-slurry freeze-casting method using camphene as a volatile solvent is also applicable for other metal foams such as iron, copper, or others to produce three-dimensional metal foams with high strut connectivity.

Claims (33)

1. A method comprising:

mixing magnesium or magnesium alloy powder having a particle size from about 36 microns to 45 microns in a solution of camphene to obtain a suspension solution containing about 3-6 weight-percent binder and about 1-3 weight-percent dispersant;

stirring or sonicating the suspension solution uniformly in water bath for about 30-60 minutes to obtain a slurry solution;

freeze casting the camphene-based magnesium or magnesium alloy powder slurry solution;

drying, via sublimation, camphene, a frozen green-body foam, by placing the frozen green-body foam in an air hood for about 3-7 days or in a freeze dryer for about 24-48 hours; and

after drying, sintering the frozen green-body foam comprising the magnesium or magnesium alloy, wherein the sintering comprises a two-step sintering process comprising burning of the binder and dispersant at about 300-450 degrees Celsius for about 3-5 hours, and sintering of the frozen green-body foam at about 500-650 degrees Celsius for about 3-10 hours in argon atmosphere, and

after sintering, a three dimensionally connected magnesium or magnesium alloy foam is produced of at least one of Mg—Al, Mg—Zn, Mg—Al, Mg—Mn, Mg—Si, Mg—Cu, Mg—Zr, or Mg-rare earth element, or any combination thereof.

2. The method of claim 1 wherein the binder is polystyrene and the dispersant is oligometric polyester powder.

3. The method of claim 1 comprising:

mechanically mixing powders of the magnesium and another element for from about 10 minutes to about 60 minutes to obtain a uniform particle mixing before mixing with liquid caphene, binder, and dispersant when the powders used are not prealloyed.

4. The method of claim 1 comprising:

freezing the slurry solution at a temperature from about −80-40 degrees Celsius.

5. The method of claim 1 comprising:

drying the slurry solution in a vacuum at a temperature from about −80 degrees Celsius to about room temperature.

6. The method of claim 1 comprising:

sintering the frozen green-body foam in an alumina crucible filled with graphite powder having a mean particle size of about 1-30 microns, thereby transforming the frozen green-body foam to the magnesium or magnesium alloy foam.

7. The method of claim 6 wherein the magnesium or magnesium alloy foam comprises a three-dimensional pore structure with uniformly distributed pores having diameters from about 1 micron to about 300 microns.

8. A method comprising:

mixing a magnesium alloy powder having a particle size from about 36 microns to 45 microns in a solution of camphene to obtain a suspension solution containing about 3-6 weight-percent binder comprising polystyrene and about 1-3 weight-percent dispersant comprising oligometric polyester powder;

stirring or sonicating the suspension solution uniformly in a water bath for about 30-60 minutes to obtain a slurry solution;

freeze casting the camphene-based magnesium alloy powder slurry solution;

drying camphene, a frozen green-body foam, by placing the frozen green-body foam in an air hood for about 3-7 days or in a freeze dryer for about 24-48 hours; and

after drying, sintering the frozen green-body foam comprising the magnesium alloy, wherein the sintering comprises a two-step sintering process comprising burning of the binder and dispersant at about 300-450 degrees Celsius for about 3-5 hours, and sintering of the frozen green-body foam at about 500-650 degrees Celsius for about 3-10 hours in argon atmosphere, and

after sintering, a three dimensionally connected magnesium alloy foam is produced of at least one of Mg—Al, Mg—Zn, Mg—Al, Mg—Mn, Mg—Si, Mg—Cu, Mg—Zr, or Mg-rare earth element, or any combination thereof.

9. A method comprising:

(i) mixing magnesium or magnesium alloy powder in a solution of liquid camphene to obtain a suspension solution containing about 3-6 weight-percent binder comprising polystyrene and about 1-3 weight-percent dispersant;

(ii) stirring or sonicating the suspension solution uniformly in warm-water bath at above degrees Celsius for about 30-60 minutes to obtain a slurry solution;

(iii) freeze casting the camphene-based magnesium or magnesium alloy powder slurry solution;

(iv) drying, via sublimation, camphene, a frozen green-body foam, by placing the frozen green-body foam in an air hood for about 3-7 days or in a freeze dryer for about 24-48 hours; and

(v) after drying, sintering the frozen green-body foam comprising the magnesium or magnesium alloy, and

after sintering, a three dimensionally connected magnesium or magnesium alloy foam is produced of at least one of Mg—Al, Mg—Zn, Mg—Al, Mg—Mn, Mg—Si, Mg—Cu, Mg—Zr, or Mg-rare earth element, or any combination thereof,

wherein the sintering the frozen green-body foam comprising the magnesium or magnesium alloy comprises a two-step sintering process comprising

burning of the binder and dispersant at about 300-450 degrees Celsius for about 3-5 hours, and sintering of the frozen green-body foam at about 500-650 degrees Celsius for about 3-10 hours in argon atmosphere.

Assignments (2)
CHANGE OF NAME Recorded Jun 26, 2023
From: CELLMOBILITY, INC.
To: CELLMO MATERIALS INNOVATION, INC.
Reel/Frame 064111/0581 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 5, 2021
From: HONG, KICHEOL; PARK, HYEJI; UM, TEAKYUNG; CHOE, HEEMAN
To: CELLMOBILITY, INC.
Reel/Frame 054819/0548 →