# US 12,110,377 B1 · Aerogel with hierarchical pore structure formed using pulsed laser technology, and preparation method and use thereof

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- Number: US 12,110,377 B1
- Document ID: US12110377B1
- Status: Granted
- Kind: B1
- Application number: 18/524,186
- Filed: 2023-11-30
- Published: 2024-10-03
- Granted: 2024-10-08
- Earliest claimed: 2023-03-27
- Assignees: Ocean University of China
- Applicants: Ocean University of China
- Inventors: Hongzhi Cui; Ruiqi Xu; Na Wei; Minggang Zhao; Aiping Wang; Jun Zhao
- Web page: https://patentgrep.com/patent/US12110377B1

## CPC

- C08J 9/283: {a discontinuous liquid phase emulsified in a continuous macromolecular phase}
- B23K 26/0622: by shaping pulses
- B23K 26/389: {of fluid openings, e.g. nozzles, jets}
- B23K 26/402: involving non-metallic material, e.g. isolators
- C02F 1/14: using solar energy
- C08J 3/075: Macromolecular gels
- C08J 3/212: {and solid additives}
- C08J 9/0066: {Use of inorganic compounding ingredients}
- C08J 9/36: After-treatment (C08J9/22 takes precedence)
- C08K 3/34: Silicon-containing compounds
- C08L 5/12: {Agar or} agar-agar {, i.e. mixture of agarose and agaropectin}; Derivatives thereof
- F24S 70/16: made of ceramic; made of concrete; made of natural stone
- C02F 2103/08: Seawater, e.g. for desalination
- C08J 2201/026: Crosslinking before of after foaming
- C08J 2201/0484: the liquid phase being aqueous
- C08J 2205/026: Aerogel, i.e. a supercritically dried gel
- C08J 2205/04: characterised by the foam pores
- C08J 2305/12: Agar-agar; Derivatives thereof
- C08J 2329/04: Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
- C08J 2405/12: Agar-agar; Derivatives thereof
- C08J 2429/04: Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
- C08K 2201/001: Conductive additives
- C08K 2201/011: Nanostructured additives
- C08L 2203/14: used for foams
- C08L 2312/00: Crosslinking
- Y02A 20/124: Water desalination
- Y02A 20/212: Solar-powered wastewater sewage treatment, e.g. spray evaporation
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- B23K: SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- F24S: SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS (for producing mechanical power from solar energy F03G6/00)
- Y02A: TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE

## Abstract

Disclosed are an aerogel with a hierarchical pore structure formed using a pulsed laser technology, and a preparation method and use thereof. In the preparation method, a nano silicon-containing inorganic material as a freezing element, a biomass polymer as a cross-linking agent, and deionized water as a solvent are mixed and a resulting mixture is left to stand and gelatinized to obtain a hydrogel; the hydrogel is frozen to form ice crystals therein, and the ice crystals are removed by freeze-drying to obtain a micron-nano porous aerogel; the micron-nano porous aerogel is subjected to customized millimeter-scale punching using a pulsed laser to obtain an aerogel with a millimeter-micron-nano hierarchical pore structure.

## Claims

### Claim 1

An aerogel with a hierarchical pore structure formed using a pulsed laser technology, the aerogel being a silicon-containing inorganic-organic composite aerogel with a millimeter-micron-nano hierarchical pore structure, and being formed by subjecting a micron-nano silicon-containing inorganic-organic composite aerogel to customized millimeter-scale punching using a pulsed laser,
wherein the micron-nano silicon-containing inorganic-organic composite aerogel is prepared by a process comprising:
mixing a nano silicon-containing inorganic material, a biomass polymer, and deionized water as a solvent to obtain a mixture, leaving the mixture to stand, and gelatinizing to obtain a nano silicon-containing inorganic-organic composite hydrogel, the biomass polymer comprising polyvinyl alcohol, agar, and glutaraldehyde; and
freezing the nano silicon-containing inorganic-organic composite hydrogel to form ice crystals therein, and removing the ice crystals therein by freeze-drying to obtain the micron-nano silicon-containing inorganic-organic composite aerogel; and
wherein a size, a shape, and a number of millimeter-scale pores in the aerogel with the hierarchical pore structure are controlled by the pulsed laser, thereby obtaining the silicon-containing inorganic-organic composite aerogel with the millimeter-micron-nano hierarchical pore structure.

### Claim 2 (depends on 1)

The aerogel with the hierarchical pore structure formed using the pulsed laser technology as claimed in claim 1, wherein the nano silicon-containing inorganic material comprises at least one of MoSi2, SiO2, and Si3N4.

### Claim 3 (depends on 1)

A method for preparing the aerogel with the hierarchical pore structure formed using the pulsed laser technology as claimed in claim 1, comprising the steps of:
step 1), preparing the nano silicon-containing inorganic-organic composite hydrogel, comprising:
providing polyvinyl alcohol and agar, adding deionized water thereto, and dissolving the polyvinyl alcohol and the agar by heating to obtain a homogeneous solution; adding a glutaraldehyde solution into the homogeneous solution, and subjecting a resulting mixture to cross-linking to obtain a cross-linked solution; adding a nano silicon-containing inorganic powder into the cross-linked solution to obtain a nano silicon-containing inorganic-organic composite colloidal sol; and leaving the nano silicon-containing inorganic-organic composite colloidal sol to stand, and gelatinizing to obtain the nano silicon-containing inorganic-organic composite hydrogel;
step 2), preparing the micron-nano silicon-containing inorganic-organic composite aerogel, comprising:
freezing the nano silicon-containing inorganic-organic composite hydrogel obtained in step 1) to form the ice crystals therein, and vacuum freeze-drying to remove the ice crystals and obtain the micron-nano silicon-containing inorganic-organic composite aerogel; and
step 3), producing the silicon-containing inorganic-organic composite aerogel with a millimeter-micron-nano hierarchical pore structure, comprising:
subjecting the micron-nano silicon-containing inorganic-organic composite aerogel to punching processing using the pulsed laser technology to form the millimeter-scale pore structure,
wherein the punching processing is performed by:
setting the pulsed laser with a frequency of 20 Hz, a pulse-width of 5,000 ps, a scanning speed of 50 mm/s to 150 mm/s, a laser power of 3% to 8%, and a laser spot of 1 mm; selecting a millimeter-scale pore shape; and punching the micron-nano silicon-containing inorganic-organic composite aerogel from top to bottom using a laser light source to form the millimeter-scale pores, wherein the size, the shape, and the number of the millimeter-scale pores in the aerogel with the hierarchical pore structure are controlled by the pulsed laser, thereby forming the silicon-containing inorganic-organic composite aerogel with the millimeter-micron-nano hierarchical pore structure.

### Claim 4 (depends on 3)

The method as claimed in claim 3, wherein in step 1) the nano silicon-containing inorganic-organic composite colloidal sol comprises 1 wt % to 4 wt % of the polyvinyl alcohol, 1 wt % to 2 wt % of the agar, and 0.02 wt % to 1 wt % of the nano silicon-containing inorganic powder.

### Claim 5 (depends on 3)

The method as claimed in claim 3, wherein in step 2) the nano silicon-containing inorganic-organic composite hydrogel is frozen at a temperature of −30° C. to −80° C.

### Claim 6 (depends on 3)

The method as claimed in claim 3, wherein the millimeter-scale pore shape comprises at least one of a square, a circle, and a polygon.

### Claim 7 (depends on 3)

The method as claimed in claim 3, wherein the nano silicon-containing inorganic powder comprises at least one of MoSi2, SiO2, and Si3N4.

### Claim 8 (depends on 1)

A solar-driven method for desalinating seawater, comprising the steps of:
combining the aerogel with the hierarchical pore structure formed using the pulsed laser technology as claimed in claim 1, a polystyrene foam as a thermal insulation layer, and a fiber absorbent paper, and assembling into an evaporator, wherein the aerogel is to absorb solar energy, and the fiber absorbent paper is to transport seawater; and
evaporating the seawater by using the evaporator to obtain fresh water.
