IP Library › Granted Patent US 10,780,411
Granted Patent B2
US 10,780,411 · App. 15/898,464 · Granted Sep 22, 2020

Multi-channel direct-deposit assembly method to high-throughput synthesize three-dimensional macroporous/mesoporous material array

Inventors: Xiaonao Liu (Frederick, MD); Yifeng Shi (Frederick, MD)
Assignee: TAO TREASURES, LLC
B01J19/0046C01B13/363B01J2219/00378B01J2219/00385B01J2219/00495B01J2219/00527B01J2219/00587B01J2219/00745B01J2219/00747B82Y30/00B82Y40/00
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Quick Facts
Patent No.
US 10,780,411
App. No.
15/898,464
Granted
Sep 22, 2020
Kind
B2
Abstract

A multi-channel direct-deposit assembly method is disclosed to high-throughput synthesize three-dimensional macroporous/mesoporous (3DMM) material array with precisely controlled composition, pore size, and pore structure. The macropore size of the synthesized 3DMM material is in the range of 50-1000 nm; the mesopore size of the synthesized 3DMM material is in the range of 1-50 nm. The surface area of the 3DMM material is in the range of 20-1000 m 2 /g. The 3DMM material array can be used for rapid synthesis, screening and manufacture of catalysts and nanosensors.

Claims (22)

1. A method of forming an array of structured material containing macropores and mesopores, comprising:

preparing a plurality of pore-forming template agent solutions, wherein each of the plurality of pore-forming template agent solutions comprises at least one macropore-forming template agent, at least one mesopore-forming template agent, and a first amphoteric solvent, wherein the macropore-forming template agent is silica nanoparticles and carbon nanospheres, and wherein the mesopore-forming template agent is a polymer;

preparing a plurality of precursor solutions, wherein each of the plurality of precursor solutions comprises a precursor selected from the group consisting of metal species metal nanoparticles, organosilicate, and a mixture thereof and a second amphoteric solvent; and

depositing, by inkjet printing, an as-synthesized array of dots onto a substrate, wherein each of the as-synthesized array of dots is a mixture of at least one of the plurality of precursor solutions and at least one of the plurality of pore-forming template agent solutions.

2. The method of claim 1 , further comprising:

filling each of a first set of channels in an inkjet printer with at least one of the plurality of precursor solutions;

filling each of a second set of channels in the inkjet printer with at least one of the plurality of pore-forming template agent solutions; and

during the depositing step, dispensing a first volume of the at least one of the plurality of precursor solutions from one of the first set of channels and a second volume of the at least one of the plurality of pore-forming template agent solutions in each dot in the as-synthesized array of dots.

3. The method of claim 1 , further comprising:

evaporating the as-synthesized array at 20-500° C. to remove the amphoteric solvent to form an as-synthesized film array.

4. The method of claim 3 , further comprising:

removing the pore-forming template agents in the as-synthesized film array by heating at 100-1000° C., by etching using a NaOH solution or a HF solution, or both to obtain the array of structured material.

5. The method of claim 2 , wherein, the first volume and the second volume is controlled according to a software program so that the a composition of each dot in the as-synthesized array of dots is controllable.

6. The method of claim 1 , wherein the first amphoteric solvent and the second amphoteric solvent are the same or different, each is chosen from water, alcohol, acid, alkali, acetone, or mixtures thereof.

7. The method of claim 6 , wherein said alcohol is chosen from methanol, ethanol, propanol, butanol, glycerol, or mixtures thereof.

8. The method of claim 6 , wherein said acid is chosen from formic acid, acetic acid, nitric acid, hydrochloric acid, sulfuric acid, citric acid, or mixtures thereof.

9. The method of claim 6 , wherein said alkali is chosen from ammonia, sodium hydroxide, potassium hydroxide, or mixtures thereof.

10. The method of claim 1 , wherein said metal species is one or more metals, metal salts, or metal alkoxide chosen from main group metals, transition metals, lanthanide metals, actinide metal, nitrates, carbonates, acetates, chlorates, or alkoxides.

11. The method of claim 1 , wherein said substrate is chosen from paper, membrane, glass, corundum, ceramic, silicon wafer, steel, wood, quarts, or a circuit board.

12. The method of claim 1 , wherein a size of the macropores in the structured material is in a range of 50-1000 nm, a size of the mesopores in the structured material is in a range of 1-50 nm, and wherein a surface area of the structured material is in a range of 20-1000 m 2 /g.

13. The method of claim 1 , wherein the structured material comprises metal oxide composites, metal/metal oxides composites, metal/reduced graphene oxide (rGO) composites, metal oxide/rGO composites, metal/carbon nanotube (CNT) composites, metal oxide/CNT composites, metal/Mxene composite, or metal oxide/Mxene composite.

14. The method of claim 1 , wherein the polymer is a block copolymer that is PEG-PPG-PEG or EO 96 PO 70 EO 96 .

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 7, 2019
From: LIU, XIAONAO
To: TAO TREASURES LLC DBA NANOBIOFAB
Reel/Frame 049411/0595 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 7, 2019
From: SHI, YIFENG
To: TAO TREASURES LLC DBA NANOBIOFAB
Reel/Frame 049411/0674 →
Continuity (3)
Provisional Application 62462297 · Feb 22, 2017
Provisional Application 62460735 · Feb 17, 2017
Related Publication 20190336932A1 · Nov 7, 2019
Cited By (1)
US 12,551,142