CN112593109A - Graphene additive and preparation method thereof - Google Patents
Graphene additive and preparation method thereof Download PDFInfo
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- CN112593109A CN112593109A CN202011375356.5A CN202011375356A CN112593109A CN 112593109 A CN112593109 A CN 112593109A CN 202011375356 A CN202011375356 A CN 202011375356A CN 112593109 A CN112593109 A CN 112593109A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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Abstract
The invention relates to a graphene additive and a preparation method thereof, wherein the graphene additive is prepared from graphene, a metal with conductivity and an organic solvent, and the volume ratios of the graphene, the metal and the organic solvent are preferably 0.28%, 14.24% and 85.48% respectively. When the graphene additive is used for manufacturing a conductor material, graphene can be successfully added into metal in a melting state in a melting furnace, and multilayer graphene is formed in a metal matrix of the manufactured conductor material, so that the conductivity of the conductor material is greatly improved.
Description
Technical Field
The invention belongs to the technical field of additives and conductive materials, and particularly relates to a graphene additive and a preparation method thereof.
Background
At present, silver, copper, gold, aluminum, tungsten, nickel, iron, lead and the like are commonly used as conductive materials. However, the applicant found that: the existing conductive materials have higher resistivity, so that the conductivity is lower, the self energy consumption is higher, the heat productivity is large, and the service life is greatly shortened.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a graphene additive which can successfully add graphene into molten metal in a smelting furnace and form multilayer graphene in a metal matrix of a prepared conductor material, so that the conductivity of the conductor material is greatly improved, and a preparation method of the graphene additive.
In order to solve the technical problems, the invention adopts the following technical scheme:
a graphene additive is prepared from graphene, a metal with conductivity and an organic solvent, wherein the volume ratio of the graphene, the metal and the organic solvent is preferably 0.28%, 14.24% and 85.48%, respectively.
Further, the particle size of the graphene is 1-10 nm.
Further, the organic solvent is one of absolute ethyl alcohol, 1-3 butanediol and water, and the absolute ethyl alcohol is preferred.
Further, the metal is Al or Cu.
The invention also provides a preparation method of the graphene additive, which comprises the following steps:
a1. dispersing graphene in an organic solvent to obtain a mixed solution A;
a2. adding metal into the mixed solution A, and mixing to obtain a mixed solution B;
a3. centrifuging the mixed solution B, and taking the lower layer powder A;
a4. vacuum drying the obtained lower layer powder A, and filling hydrogen at high temperature for reduction to obtain powder B;
a5. adding a smelting additive into the powder B for grinding to obtain powder C;
a6. and pressing and forming the powder C to obtain the graphene additive.
Further, the mixing time in step a2 is above 3h, and the rotational speed of the mixer is above 2000 rpm.
Further, the rotation speed of the centrifuge in the step a3 is 5000rpm, and the centrifugation time is 1 h.
Further, the drying temperature in step a4 was 120 ℃, the drying time was 24h, the reduction temperature was 200 ℃, and the reduction time was 30 minutes.
The invention mainly has the following beneficial effects:
according to the technical scheme, the graphene can be successfully added into the metal in a melting state in the melting furnace when the conductor material is manufactured, and the multilayer graphene is formed in the metal matrix of the manufactured conductor material, so that the conductivity of the conductor material is greatly improved.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of a graphene additive according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The graphene additive is prepared from graphene, a metal with conductivity and an organic solvent, and the volume ratios of the graphene, the metal and the organic solvent are preferably 0.28%, 14.24% and 85.48%, respectively. The particle size of the graphene is 1-10 nm, the metal can be Al or Cu, and the organic solvent is one of absolute ethyl alcohol, 1-3 butanediol and water (preferably absolute ethyl alcohol).
As shown in fig. 1, the preparation method of the graphene additive of the present invention includes the following steps:
and S100, dispersing graphene in an organic solvent to obtain a mixed solution A.
S200, adding metal into the mixed solution A, and mixing to obtain a mixed solution B; specifically, the mixed solution A after the metal is added is mixed by a mixer to obtain a mixed solution B, the mixing time is preferably more than 3h, and the rotating speed of the mixer is preferably more than 2000 rpm.
S300, carrying out centrifugal treatment on the mixed solution B, and taking the lower-layer powder A; the method specifically comprises the following steps: and centrifuging the mixed solution B by using a centrifuge, and taking the lower layer of powder A, wherein the rotation speed of the centrifuge is preferably 5000rpm, and the centrifuging time is preferably 1 h.
S400, after the obtained lower-layer powder A is dried in vacuum (for example, the lower-layer powder A is dried in a vacuum drying furnace), hydrogen is filled at high temperature for reduction to obtain powder B; wherein the drying temperature is preferably 120 ℃, the drying time is preferably 24 hours, the reduction temperature is preferably 200 ℃, and the reduction time is preferably 30 minutes.
S500, adding a smelting additive (such as a refiner, wherein the smelting additive is completely volatilized in the grinding process) into the powder B for grinding to obtain powder C;
and S600, pressing and forming the powder C to obtain the graphene additive.
When the graphene additive is used for manufacturing a conductor material, graphene can be successfully added into molten metal in a smelting furnace, and multilayer graphene is formed in a metal matrix of the manufactured conductor material, so that the conductivity of the conductor material is greatly improved.
The graphene additive and the preparation method of the present invention are further described in the following by specific examples.
Example 1：
In this embodiment 1, a graphene additive is prepared from graphene, Cu powder and absolute ethyl alcohol, and the specific steps include:
1) dispersing a proper amount of graphene additive in absolute ethyl alcohol to obtain a mixed solution A;
2) adding 50g of Cu powder into the mixed solution A, and mixing for more than 3h at the rotating speed of more than 2000rpm by adopting a mixer to obtain a mixed solution B;
3) centrifuging the mixed solution B for 1h at the rotating speed of 5000rpm by using a centrifuge, and taking the lower-layer powder A;
4) putting the obtained lower layer powder A into a vacuum drying furnace, carrying out vacuum drying for 24 hours at the temperature of 120 ℃, and then filling hydrogen at the high temperature of 200 ℃ for reduction for 30 minutes to obtain powder B;
5) adding a smelting additive into the powder B for grinding to obtain powder C;
6) and pressing and forming the powder C to obtain the graphene additive.
The graphene additive prepared in the embodiment 1 and Al are prepared into a conductor material, and the specific preparation process comprises the following steps: firstly, putting Al into a smelting furnace for smelting; and then adding the graphene additive into a smelting furnace, mixing with the molten Al, and finally stirring and preserving heat for 1h to obtain the conductive material.
Example 2：
In this embodiment 2, a graphene additive is prepared from graphene, Cu powder and absolute ethyl alcohol, and the specific steps are as follows:
1) dispersing a proper amount of graphene additive in absolute ethyl alcohol to obtain a mixed solution A;
2) adding 50g of Cu powder into the mixed solution A, and mixing for more than 3h at the rotating speed of more than 2000rpm by adopting a mixer to obtain a mixed solution B;
3) centrifuging the mixed solution B for 1h at the rotating speed of 5000rpm by using a centrifuge, and taking the lower-layer powder A;
4) putting the obtained lower layer powder A into a vacuum drying furnace, carrying out vacuum drying for 24 hours at the temperature of 120 ℃, and then filling hydrogen at the high temperature of 200 ℃ for reduction for 30 minutes to obtain powder B;
5) adding a smelting additive into the powder B for grinding to obtain powder C;
6) and pressing and forming the powder C to obtain the graphene additive.
The graphene additive prepared in the embodiment 2 and Cu are prepared into a conductor material, and the specific preparation process comprises the following steps: firstly, putting Cu into a smelting furnace for melting; and then adding the graphene additive into a smelting furnace, mixing with the molten Cu, and finally stirring and preserving heat for 1h to prepare the conductive material.
The test of the materials college of university of south China's university of committee in committee on the examples 1-2 and the conventional aluminum sheet as comparative examples specifically comprises the following steps: detecting by adopting a detection device of the American quantum PPMS-9, detecting items and conditions: resistivity (300K), the results are shown in table 1 below.
TABLE 1
As can be seen from the above table, when the graphene additive of the present invention is used to prepare the conductor material of examples 1-2, it is possible to form multi-layer graphene in the Al matrix and the Cu matrix, such that the electrical resistivity of the conductor material is significantly reduced and the electrical conductivity is greatly improved compared to the conventional aluminum sheet.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (8)
1. A graphene additive is prepared from graphene, a metal with conductivity and an organic solvent, wherein the volume ratio of the graphene to the metal to the organic solvent is preferably 0.28%, 14.24% and 85.48%, respectively.
2. The graphene additive according to claim 1, wherein the graphene has a particle size of 1 to 10 nm.
3. The graphene additive according to claim 1, wherein the organic solvent is one of absolute ethanol, 1-3 butanediol, and water, preferably absolute ethanol.
4. The graphene additive of claim 1, wherein the metal is Al or Cu.
5. A method for preparing the graphene additive according to any one of claims 1 to 4, comprising the steps of:
a1. dispersing graphene in an organic solvent to obtain a mixed solution A;
a2. adding metal into the mixed solution A, and mixing to obtain a mixed solution B;
a3. centrifuging the mixed solution B, and taking the lower layer powder A;
a4. vacuum drying the obtained lower layer powder A, and filling hydrogen at high temperature for reduction to obtain powder B;
a5. adding a smelting additive into the powder B for grinding to obtain powder C;
a6. and pressing and forming the powder C to obtain the graphene additive.
6. The method according to claim 5, wherein the mixing time in step a2 is 3 hours or more and the rotational speed of the mixer is 2000rpm or more.
7. The method according to claim 5, wherein the rotation speed of the centrifuge in the step a3 is 5000rpm, and the centrifugation time is 1 h.
8. The method according to claim 5, wherein the drying temperature in step a4 is 120 ℃, the drying time is 24h, the reduction temperature is 200 ℃, and the reduction time is 30 minutes.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011375356.5A CN112593109A (en) | 2020-11-30 | 2020-11-30 | Graphene additive and preparation method thereof |
| PCT/CN2020/139974 WO2022110455A1 (en) | 2020-11-30 | 2020-12-28 | Graphene additive and preparation method therefor |
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| CN202011375356.5A CN112593109A (en) | 2020-11-30 | 2020-11-30 | Graphene additive and preparation method thereof |
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| CN112593109A true CN112593109A (en) | 2021-04-02 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112575216A (en) * | 2020-12-07 | 2021-03-30 | 深圳量子态材料有限公司 | Method for adding graphene into molten metal solution |
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| CN117144081B (en) * | 2023-10-30 | 2024-01-16 | 金鼎重工有限公司 | Rolling method of hot rolled H-shaped steel for Nb-containing low temperature resistant structure |
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| CN109371276A (en) * | 2018-12-18 | 2019-02-22 | 苏州大学 | The method that batch founding prepares graphene enhancing aluminium alloy based nano composite material |
| CN110055444A (en) * | 2019-06-13 | 2019-07-26 | 中国矿业大学 | A kind of preparation method of highly conductive graphene/aluminum based composites |
Family Cites Families (1)
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| CN112575216A (en) * | 2020-12-07 | 2021-03-30 | 深圳量子态材料有限公司 | Method for adding graphene into molten metal solution |
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- 2020-11-30 CN CN202011375356.5A patent/CN112593109A/en active Pending
- 2020-12-28 WO PCT/CN2020/139974 patent/WO2022110455A1/en active Application Filing
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952588A (en) * | 2014-05-08 | 2014-07-30 | 江西理工大学 | High-strength and high-conductivity graphene copper-based composite material and preparation method thereof |
| CN105624457A (en) * | 2016-03-22 | 2016-06-01 | 北京工业大学 | Graphene enhanced magnesium-based composite and preparing method thereof |
| CN107058786A (en) * | 2017-04-19 | 2017-08-18 | 哈尔滨理工大学 | A kind of preparation method of magnesium-based graphene composite material |
| CN107164647A (en) * | 2017-04-28 | 2017-09-15 | 哈尔滨赫兹新材料科技有限公司 | High heat conduction rigidity graphene/copper nano composite material fin and preparation method thereof |
| CN107012355A (en) * | 2017-05-05 | 2017-08-04 | 哈尔滨工业大学 | A kind of preparation method of single-layer graphene reinforced aluminum matrix composites |
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| CN109371276A (en) * | 2018-12-18 | 2019-02-22 | 苏州大学 | The method that batch founding prepares graphene enhancing aluminium alloy based nano composite material |
| CN110055444A (en) * | 2019-06-13 | 2019-07-26 | 中国矿业大学 | A kind of preparation method of highly conductive graphene/aluminum based composites |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112575216A (en) * | 2020-12-07 | 2021-03-30 | 深圳量子态材料有限公司 | Method for adding graphene into molten metal solution |
| WO2022121004A1 (en) * | 2020-12-07 | 2022-06-16 | 梁海 | Method for adding graphene to molten metal solution |
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| WO2022110455A1 (en) | 2022-06-02 |
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