CN109811177A - A kind of preparation method of highly conductive high-intensitive silver-graphene composite material - Google Patents

A kind of preparation method of highly conductive high-intensitive silver-graphene composite material Download PDF

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Publication number
CN109811177A
CN109811177A CN201910148616.6A CN201910148616A CN109811177A CN 109811177 A CN109811177 A CN 109811177A CN 201910148616 A CN201910148616 A CN 201910148616A CN 109811177 A CN109811177 A CN 109811177A
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China
Prior art keywords
graphene
obtains
silver
powder
graphene composite
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CN201910148616.6A
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Chinese (zh)
Inventor
王松
谢明
刘满门
王塞北
陈松
侯攀
胡洁琼
李爱坤
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Kunming Institute of Precious Metals
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Kunming Institute of Precious Metals
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Priority to CN2018113743392 priority
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Publication of CN109811177A publication Critical patent/CN109811177A/en
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Abstract

The invention discloses a kind of preparation methods of highly conductive high-intensitive silver-graphene composite material, graphene content is 0.5wt%~5wt% in silver-graphene composite material, surplus is Ag and inevitable impurity, the preparation method is as follows: weighing Ag powder in proportion and graphene powder is placed in 2~8h of sonic oscillation in dehydrated alcohol and obtains Ag- graphene mixed solution;Mixed solution is placed in ball milling 10 in ball mill~obtain mixed slurry for 24 hours;Mixed slurry is dried in vacuo at 30~80 DEG C and obtains Ag- graphene composite powder;Composite granule isostatic cool pressing at 150~300MPa obtains preform;Preform vacuum microwave at 600~800 DEG C, which is sintered and cools to room temperature with the furnace, obtains silver-graphene composite material.Have high conductivity and high intensity using the silver-graphene composite material of this method preparation: conductivity is greater than 90%IACS, and tensile strength is greater than 290MPa.

Description

A kind of preparation method of highly conductive high-intensitive silver-graphene composite material
Technical field
The present invention relates to a kind of preparation methods of highly conductive high-intensitive silver-graphene composite material, belong to metal-based compound Field of material preparation.
Background technique
Compared with flaky graphite, carbon nanotube, carbon fiber etc., graphene is due to its unique structure and excellent performance Have become optimal carbonaceous material reinforcement in current metal-base composites.
Graphene partial size is small, large specific surface area, surface can be high, there is very strong reunions tendency, it is traditional direct mechanical to mix It closes technique and graphene can not be well dispersed in metallic matrix and firm with metallic matrix by forming sintering technology with nanoscale Consolidation is closed.
In order to solve the problems, such as graphene full and uniform dispersion in metallic matrix, a kind of patent of invention specification " metal Graphene is added in the salting liquid of parent metal in base matrix graphene composite electrical contact material preparation method (CN102385938B) ", It is mixed after being deposited metallochemistry reduction on the surface of graphene using hydrazine hydrate with parent metal, passes through vacuum melting method and prepare gold Belong to base matrix graphene composite electrical contact material.This method is although easy to operate, technique is easy to control, but in vacuum melting graphene with Parent metal is easy to happen reaction and generates brittlement phase, reduces the plasticity and toughness of composite material.Patent of invention specification " graphene Enhance the preparation method (CN102329976A) of metal-base composites " graphene oxide is dispersed in the table of flaky metal powder Simultaneously electronation handles to obtain graphene/composite metal powder in face, obtains graphene enhancing Metal Substrate using powder metallurgical technique Composite material.Although this method can regulate and control the content of graphene, induction graphene forms distribution of orientations, flake graphite alkene/ The defects of composite metal powder formability is poor, is easy to appear crackle and layering during the preparation process, material conductivity is poor.
Sonic oscillation, ball milling slurrying, vacuum drying, isostatic cool pressing and vacuum microwave sintering technology are applied to by the present invention In the preparation process of silver-graphene composite material, reduction method chemical contamination can be avoided, reduce the production cycle, be suitble to high-volume Industrialized production, and the silver-graphene composite material tissue height prepared is uniform, has high conductivity and high intensity.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the present invention provides a kind of highly conductive high-intensitive silver-graphene is compound The preparation method of material, graphene content is 0.5wt%~5wt% in silver-graphene composite material, and surplus is Ag and can not keep away Exempt from impurity.The present invention passes through sonic oscillation, ball milling slurrying, vacuum drying, isostatic cool pressing using graphene powder and Ag powder as raw material With the process flow of vacuum microwave sintering, highly conductive high-intensitive silver-graphene composite material is made.
The present invention the specific process steps are as follows:
(1) Ag powder is weighed in proportion and graphene powder is placed in 2~8h of sonic oscillation in dehydrated alcohol and obtains Ag- graphene Mixed solution;
(2) mixed solution is placed in ball mill, uses diameter for the zirconium oxide balls of 2~10mm, rotational speed of ball-mill 100~ Mechanical ball mill 10 under 400r/min, ball material mass ratio 5:1~30:1~obtain mixed slurry for 24 hours;
(3) mixed slurry is dried in vacuo at 30~80 DEG C and obtains Ag- graphene composite powder;
(4) composite granule isostatic cool pressing at 150~300MPa obtains preform;
(5) preform vacuum microwave at 600~800 DEG C is sintered and cools to room temperature with the furnace to obtain silver-graphene multiple Condensation material, 1~5h of vacuum microwave sintered heat insulating time, 0.5~350GHz of microwave frequency, microwave source output power 200~ 8000W, vacuum degree is less than 1 × 10-2Pa。
Compared with prior art, the beneficial effects of the present invention are: preparation silver-graphene composite material even tissue (see Fig. 1), have high conductivity and high intensity: conductivity is greater than 90%IACS, and tensile strength is greater than 290MPa, can be widely applied to The electrical contact of mesolow load appliance, the commutator material of micro machine, rotor wire of turbogenerator etc..
Detailed description of the invention
Fig. 1 is highly conductive high-intensitive silver-graphene composite material microstructure stereoscan photograph prepared by the present invention.
Specific embodiment
Embodiment 1
1. weighing 99g Ag powder respectively and 1g graphene powder being placed in sonic oscillation 4h in 500ml dehydrated alcohol and obtains Ag- Graphene mixed solution;
2. Ag- graphene mixed solution is placed in ball mill, use diameter for the zirconium oxide balls of 3mm, turns in ball milling Mechanical ball mill 15h obtains mixed slurry under fast 350r/min, ball material mass ratio 15:1;
3. mixed slurry is dried in vacuo at 50 DEG C and obtains Ag- graphene composite powder;
4. composite granule isostatic cool pressing at 200MPa obtains preform;
5. preform vacuum microwave at 700 DEG C, which is sintered and cools to room temperature with the furnace, obtains silver-graphene composite material, Vacuum microwave sintered heat insulating time 3h, microwave frequency 5GHz, microwave source output power 800W, vacuum degree is less than 1 × 10-2Pa。
Embodiment 2
1. weighing 96g Ag powder respectively and 4g graphene powder being placed in sonic oscillation 8h in 500ml dehydrated alcohol and obtains Ag- Graphene mixed solution;
2. mixed solution is placed in ball mill, use diameter for the zirconium oxide balls of 6mm, rotational speed of ball-mill 300r/min, Mechanical ball mill 15h obtains mixed slurry under ball material mass ratio 20:1;
3. mixed slurry is dried in vacuo at 70 DEG C and obtains Ag- graphene composite powder;
4. composite granule isostatic cool pressing at 250MPa obtains preform;
5. preform vacuum microwave at 750 DEG C, which is sintered and cools to room temperature with the furnace, obtains silver-graphene composite material; Vacuum microwave sintered heat insulating time 1.5h, microwave frequency 100GHz, microwave source output power 5000W, vacuum degree is less than 1 × 10- 2Pa。
1 embodiment material properties test of table
Performance Embodiment 1 Embodiment 2
Consistency (%) 99.8 99.6
Conductivity (%IACS) 96 92
Tensile strength (MPa) 297 323
Elongation after fracture (%) 17 15

Claims (3)

1. a kind of preparation method of highly conductive high-intensitive silver-graphene composite material, graphene contains in silver-graphene composite material Amount is 0.5wt%~5wt%, and surplus is Ag and inevitable impurity, it is characterised in that is prepared by following processing steps:
(1) Ag powder is weighed in proportion and graphene powder is placed in 2~8h of sonic oscillation in dehydrated alcohol and obtains the mixing of Ag- graphene Solution;
(2) mixed solution is placed in ball mill, uses diameter for the zirconium oxide balls of 2~10mm, rotational speed of ball-mill 100~ Mechanical ball mill 10 under 400r/min, ball material mass ratio 5:1~30:1~obtain mixed slurry for 24 hours;
(3) mixed slurry is dried in vacuo at 30~80 DEG C and obtains Ag- graphene composite powder;
(4) composite granule isostatic cool pressing at 150~300MPa obtains preform;
(5) preform vacuum microwave at 600~800 DEG C, which is sintered and cools to room temperature with the furnace, obtains silver-graphene composite wood Material, 1~5h of vacuum microwave sintered heat insulating time, 0.5~350GHz of microwave frequency, microwave source 200~8000W of output power, very Reciprocal of duty cycle is less than 1 × 10-2Pa。
2. a kind of preparation method of highly conductive high-intensitive silver-graphene composite material according to claim 1, it is characterised in that The granularity for the Ag powder that the step (1) uses is 10~100 μm, purity is greater than 99.95%, and the graphene powder used is surface Silver-plated multi-layer graphene.
3. a kind of preparation method of highly conductive high-intensitive silver-graphene composite material, it is characterised in that by following processing steps into Row preparation:
1) weighs 99g Ag powder respectively and 1g graphene powder is placed in sonic oscillation 4h in 500ml dehydrated alcohol and obtains Ag- graphite Alkene mixed solution;
2) Ag- graphene mixed solution is placed in ball mill by, uses diameter for the zirconium oxide balls of 3mm, in rotational speed of ball-mill Mechanical ball mill 15h obtains mixed slurry under 350r/min, ball material mass ratio 15:1;
3) mixed slurry is dried in vacuo at 50 DEG C and obtains Ag- graphene composite powder;
4) composite granule isostatic cool pressing at 200MPa obtains preform;
5) preform vacuum microwave at 700 DEG C, which is sintered and cools to room temperature with the furnace, obtains silver-graphene composite material, very Empty microwave sintering soaking time 3h, microwave frequency 5GHz, microwave source output power 800W, vacuum degree is less than 1 × 10-2Pa。
CN201910148616.6A 2018-11-19 2019-02-28 A kind of preparation method of highly conductive high-intensitive silver-graphene composite material Pending CN109811177A (en)

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CN2018113743392 2018-11-19

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110284019A (en) * 2019-07-11 2019-09-27 长飞光纤光缆股份有限公司 A method of orienting doped graphite in a metal
CN110964365A (en) * 2019-12-16 2020-04-07 广东南海启明光大科技有限公司 Preparation method of nano-silver-loaded graphene and graphene PTC slurry
CN111235424A (en) * 2020-01-16 2020-06-05 西安理工大学 AgZrB with excellent material transfer resistance2-Gr contact material and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105385877A (en) * 2015-11-09 2016-03-09 昆明贵金属研究所 Novel silver-based electrical contact composite material and preparing method thereof
CN105428097A (en) * 2015-12-24 2016-03-23 济南大学 Silver-based electrical contact composite material and preparation method therefor
CN105575684A (en) * 2015-12-24 2016-05-11 周懿涵 Silver based electrical contact composite material and preparation method thereof
CN105861865A (en) * 2016-06-03 2016-08-17 南昌航空大学 Method for preparing graphene reinforced aluminum matrix composite material by microwave sintering
US20170225233A1 (en) * 2016-02-09 2017-08-10 Aruna Zhamu Chemical-free production of graphene-reinforced inorganic matrix composites
CN108677048A (en) * 2018-04-20 2018-10-19 西安理工大学 A kind of silver-based composite material of nitrogen-doped graphene and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105385877A (en) * 2015-11-09 2016-03-09 昆明贵金属研究所 Novel silver-based electrical contact composite material and preparing method thereof
CN105428097A (en) * 2015-12-24 2016-03-23 济南大学 Silver-based electrical contact composite material and preparation method therefor
CN105575684A (en) * 2015-12-24 2016-05-11 周懿涵 Silver based electrical contact composite material and preparation method thereof
US20170225233A1 (en) * 2016-02-09 2017-08-10 Aruna Zhamu Chemical-free production of graphene-reinforced inorganic matrix composites
CN105861865A (en) * 2016-06-03 2016-08-17 南昌航空大学 Method for preparing graphene reinforced aluminum matrix composite material by microwave sintering
CN108677048A (en) * 2018-04-20 2018-10-19 西安理工大学 A kind of silver-based composite material of nitrogen-doped graphene and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110284019A (en) * 2019-07-11 2019-09-27 长飞光纤光缆股份有限公司 A method of orienting doped graphite in a metal
CN110964365A (en) * 2019-12-16 2020-04-07 广东南海启明光大科技有限公司 Preparation method of nano-silver-loaded graphene and graphene PTC slurry
CN111235424A (en) * 2020-01-16 2020-06-05 西安理工大学 AgZrB with excellent material transfer resistance2-Gr contact material and preparation method thereof

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