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Method for preparing graphene/copper/cuprous oxide composite powder through low-energy ball mill

A cuprous oxide and composite powder technology, applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., can solve the problems of destroying the hexagonal structure of graphene carbon atoms, lengthy and cumbersome process, and difficulty in mass production , to achieve good powder dispersion effect, simple process steps and improved overall performance

Active Publication Date: 2019-09-13
湖南华瑞康源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main methods for preparing composite powders include high-energy ball milling, in-situ polymerization, electrochemical deposition, and chemical vapor deposition, but these methods have more or less problems, such as destroying the carbon of graphene. Atomic hexagonal structure, the introduction of other impurities, the process is too long and cumbersome, it is difficult to prepare in large quantities, etc.

Method used

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  • Method for preparing graphene/copper/cuprous oxide composite powder through low-energy ball mill
  • Method for preparing graphene/copper/cuprous oxide composite powder through low-energy ball mill
  • Method for preparing graphene/copper/cuprous oxide composite powder through low-energy ball mill

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Graphene with a purity of 99.0wt% is immersed in a mixed acid with a volume ratio of hydrochloric acid and nitric acid of 1:1 for 1.5h. After cleaning and drying, it is ultrasonically dispersed in deionized water for 40min to obtain a mass concentration of 0.3wt%. Graphene dispersion liquid;

[0028] (2) Copper powder is placed in the polytetrafluoroethylene ball mill jar that zirconia ball is housed, and ball material ratio is 1:1, carries out pre-ball milling 1h under the condition of 30r / min and mixes with graphene dispersion liquid, described The quality of graphene accounts for 1wt% of the copper powder mass, and its pH is adjusted to 3.0 by using 10wt% dilute hydrochloric acid, and then the mixed slurry is obtained after secondary ball milling for 1h under the condition of 30r / min;

[0029] (3) The mixed slurry was diluted to neutral with deionized water, then stirred and reacted at 70° C. for 15 minutes, and the graphene / copper / cuprous oxide composite powder ...

Embodiment 2

[0031] (1) the graphene that purity is 99.0wt% is soaked 3h in the mixed acid that hydrochloric acid and nitric acid volume ratio are 3:1, after cleaning, drying, obtain mass concentration after ultrasonic dispersion 60min in deionized water and be 0.5wt% Graphene dispersion;

[0032] (2) Copper powder is placed in the polytetrafluoroethylene ball mill jar that zirconia ball is housed, and ball material ratio is 2:1, carries out pre-ball milling 1.5h under the condition of 60r / min and mixes with graphene dispersion liquid, so The quality of the graphene accounts for 3wt% of the copper powder quality, adopting 10wt% dilute hydrochloric acid to adjust its pH to 4.0, and then performing secondary ball milling for 1.5h under the condition of 60r / min to obtain the mixed slurry;

[0033] (3) Dilute the mixed slurry to neutral with deionized water, then stir and react at 80°C for 20 minutes, and after suction filtration and freeze-drying, the graphene / copper / cuprous oxide composite p...

Embodiment 3

[0035] (1) the graphene that purity is 99.0wt% is soaked 3h in the mixed acid that hydrochloric acid and nitric acid volume ratio are 1:3, after cleaning, drying, obtain mass concentration after ultrasonic dispersion 80min in deionized water and be 0.8wt% Graphene dispersion;

[0036] (2) Copper powder is placed in the agate ball mill jar that agate ball is housed, and ball-to-material ratio is 3:1, carries out pre-ball milling 1.5h under the condition of 100r / min and mixes with graphene dispersion liquid after, described graphene The mass accounts for 3wt% of the copper powder mass, and the pH is adjusted to 4.0 by using 10wt% dilute hydrochloric acid, and then the mixed slurry is obtained after secondary ball milling under the condition of 100r / min for 8.0h;

[0037] (3) Dilute the mixed slurry to neutral with deionized water, then stir and react at 80°C for 20 minutes, and after suction filtration and freeze-drying, the graphene / copper / cuprous oxide composite powder is obta...

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Abstract

A method for preparing graphene / copper / cuprous oxide composite powder through a low-energy ball mill includes the following steps that firstly, graphene dispersion liquid is obtained by conducting mixing acid leaching, washing and drying on graphene and then conducting ultrasonic dispersion on the graphene in deionized water; secondly, copper powder is mixed with the graphene dispersion liquid after being subjected to pre-ball-milling under the condition of 10-150 r / min, pH is regulated to 2.5-4.5, and then mixed slurry is obtained after secondary ball milling is conducted under the conditionof 10-150 r / min; and thirdly, the mixed slurry is stirred and reacts at the temperature being 60-90 DEG C after being regulated to neutral, and the graphene / copper / cuprous oxide composite powder is obtained after filtering and drying. The graphene structure in the graphene / copper / cuprous oxide composite powder prepared through the method is kept complete, dispersion is uniform, no other impurity is introduced, particles are tiny, the relative proportion between copper and cuprous oxide can be controlled, the process is simple, the repetition rate is high, and large-scale production can be achieved.

Description

technical field [0001] The invention belongs to the fields of material preparation and chemical engineering, and in particular relates to a method for preparing graphene / copper / cuprous oxide composite powder by low-energy ball milling. Background technique [0002] Graphene / copper / cuprous oxide composites have excellent electrical conductivity, thermal conductivity, electrochemical properties, catalytic properties and good mechanical properties, and have high potentials in capacitor materials, electrode materials, catalysts, biosensors and lubricating additives. Its application value is a research hotspot in the field of graphene composite materials. However, how to disperse the graphene structure completely and uniformly into the copper powder matrix is ​​a difficult problem that is currently focused on research. At present, the main methods for preparing composite powders include high-energy ball milling, in-situ polymerization, electrochemical deposition, and chemical va...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/04B22F1/00C01B32/194
CPCB22F1/0003B22F9/04C01B32/194B22F2009/043
Inventor 贺国华
Owner 湖南华瑞康源科技有限公司
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