IP Library Granted Patent US 12,355,067
Granted Patent B2
US 12,355,067 · App. 18/472,214 · Granted Jul 8, 2025

Carbon-silicon three-dimensional structural composite material and preparation method thereof

Inventors: Xuelian Wu (Fujian, CN); Enqiang Zhang (Fujian, CN)
Assignee: Hithium Tech HK Lmited
H01M4/364C01B32/184C01B32/198H01M4/386H01M4/587B82Y30/00B82Y40/00C01B2204/22
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Quick Facts
Patent No.
US 12,355,067
App. No.
18/472,214
Granted
Jul 8, 2025
Kind
B2
Abstract

Provided are a carbon-silicon three-dimensional structural composite material and a preparation method thereof. The preparation method includes: dissolving graphene quantum dots in ultrapure water, dropwise adding a CuCl 2 or ZnCl 2 solution, and performing oscillation to generate a mixed emulsifier; mixing the mixed emulsifier with a graphite oxide aqueous solution and a cyclohexane solution containing nanosilicon spheres, and performing homogenization to form a uniform oil-in-water emulsion; adding hydrazine hydrate into the obtained emulsion for reduction, and performing a hydrothermal reaction to obtain a reduced emulsion; and freeze-drying the reduced emulsion, performing washing with a washing liquid, and performing vacuum drying to obtain a carbon-silicon three-dimensional structural composite material.

Claims (23)

1. A preparation method of a carbon-silicon three-dimensional structural composite material, comprising the following steps:

a first step of dissolving 0.05 g of graphene quantum dots in 4 ml to 6 ml of ultrapure water, dropwise adding 0.75 ml of a CuCl2 or ZnCl2 solution having a concentration of 0.25 mol/ml, and performing oscillation to generate a mixed emulsifier;

a second step of mixing the mixed emulsifier obtained in the first step with 15 ml of a graphite oxide aqueous solution having a concentration of 15 mg/ml and 15 ml of a cyclohexane solution containing 0.15 g of nanosilicon spheres, and performing homogenization for 25 s to form a uniform oil-in-water emulsion;

a third step of adding 0.9 g hydrazine hydrate into the emulsion obtained in the second step for reduction, and performing a hydrothermal reaction to obtain a reduced emulsion; and

a fourth step of freeze-drying the reduced emulsion obtained in the third step, performing washing with a washing liquid, and performing vacuum drying, to obtain the carbon-silicon three-dimensional structural composite material.

2. The preparation method of the carbon-silicon three-dimensional structural composite material according to claim 1 , wherein the graphene quantum dots in the first step are prepared by:

uniformly dissolving 1 g of citric acid and 0.03 g of histidine in 20 ml of ultrapure water under a heating condition of a 45° C. water bath,

performing pyrolysis at 180° C. for 3 h to form a mixture,

filtering the mixture,

pouring a filtrate in a dialysis bag for dialysis treatment, and

performing freeze-drying at −40° C. after the dialysis treatment to obtain the graphene quantum dots.

3. The preparation method of the carbon-silicon three-dimensional structural composite material according to claim 1 , wherein the graphite oxide in the second step is prepared by a Hummer method.

4. The preparation method of the carbon-silicon three-dimensional structural composite material according to claim 1 , wherein the nanosilicon spheres in the second step have a particle diameter denoted by r, where r satisfies 50 nm.

5. The preparation method of the carbon-silicon three-dimensional structural composite material according to claim 1 , wherein the cyclohexane solution containing the nanosilicon spheres in the second step is prepared by:

adding the nanosilicon spheres into a mixed solution prepared by acetone, ethanol, and water according to a ratio of 1:1:1,

performing ultrasonic treatment for 30 min,

performing washing with ethanol and ultrapure water for three times after the ultrasonic treatment, performing centrifugal separation, and taking a lower layer of solid,

performing vacuum drying at 60° C. to obtain treated silicon spheres, and

uniformly dispersing 0.15 g of the treated nanosilicon spheres in 15 ml of a cyclohexane solution.

6. The preparation method of the carbon-silicon three-dimensional structural composite material according to claim 1 , wherein the hydrothermal reaction in the third step is performed at a temperature of 63° C. for 9 h.

7. The preparation method of the carbon-silicon three-dimensional structural composite material according to claim 1 , wherein the freeze-drying in the fourth step is performed at a temperature of −40° C.

8. The preparation method of the carbon-silicon three-dimensional structural composite material according to claim 1 , wherein the washing liquid in the fourth step is ethanol.

9. The preparation method of the carbon-silicon three-dimensional structural composite material according to claim 1 , wherein the vacuum drying in the fourth step is performed at a temperature of 60° C.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 11, 2025
From: XIAMEN HITHIUM ENERGY STORAGE TECHNOLOGY CO., LTD.
To: HITHIUM TECH HK LIMITED
Reel/Frame 070462/0648 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 12, 2023
From: WU, XUELIAN; ZHANG, ENQIANG
To: XIAMEN HITHIUM ENERGY STORAGE TECHNOLOGY CO., LTD.
Reel/Frame 065190/0008 →
Priority Claims (1)
CN 202110863229.8 · Jul 29, 2021 · national
Continuity (2)
Division 17875611 · Jul 28, 2022
Related Publication 20240014383A1 · Jan 11, 2024
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