CN103386483B - A kind of nano-graphene composite and preparation method thereof - Google Patents
A kind of nano-graphene composite and preparation method thereof Download PDFInfo
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- CN103386483B CN103386483B CN201310279884.4A CN201310279884A CN103386483B CN 103386483 B CN103386483 B CN 103386483B CN 201310279884 A CN201310279884 A CN 201310279884A CN 103386483 B CN103386483 B CN 103386483B
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Abstract
A kind of nano-graphene composite and preparation method thereof, provide a kind of elemental constituent Graphene: 25 ~ 75%, nickel: 23 ~ 71%, phosphorus: the composite of 2 ~ 4%, its preparation technology is by carrying out sensitization, activation to nano-graphene, be dissolved in nickeliferous mixed solution, carry out the processing steps such as reaction with sodium hypophosphite solution and obtain.Present invention process is simple, handled easily, reasonable mixture ratio of components, the product prepared by present invention process have thermal diffusivity good, conduct electricity the excellent properties such as fast, wear-resisting, anticorrosion, especially solve the chemical bond problem of Graphene and metal, make it effective and the combination of other Metal Phase.
Description
Technical field
The present invention relates to nano-powder material, be specially a kind of nano-graphene composite and preparation method thereof.
Background technology
Along with science and the continuous of research go deep into and develop, at Material Field, Graphene has become a kind of upstart, and Graphene is with sp by carbon atom
2a kind of carbonaceous new material of the monolayer carbon atom tightly packed one-tenth bi-dimensional cellular shape lattice structure that hydridization connects, its basic structural unit is benzene hexatomic ring the most stable in organic material.Graphene is two-dimensional material the thinnest in the world, and thickness is only 0.35nm; Its intensity is the highest in test material.
Get more and more along with to the research of Graphene, but according to the technique of present stage, the investigation and application of people to Graphene still has a difficult problem, and such as Graphene and metal can not organically combine, and this significantly limit the range of application of Graphene.
Summary of the invention
Technical problem solved by the invention is to provide a kind of nano-graphene composite and preparation method thereof, to solve the shortcoming in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A kind of nano-graphene composite, comprises the elemental constituent of following mass percent:
Graphene: 25 ~ 75%;
Nickel: 23 ~ 71%;
Phosphorus: 2 ~ 4%.
A preparation method for nano-graphene composite, its technological process comprises the following steps:
The first step: take nano-graphene 1 part according to weight, first, Graphene is put into deionized water, and ultrasonic vibration disperses, process 30min, suction filtration moves in sensitizer and carries out sensitized treatment, ultrasonic vibration 40 ~ 60min, suction filtration moves in activator and activates, ultrasonic vibration 40 ~ 60min, suction filtration also spends deionized water to neutral, and vacuum drying is for subsequent use;
Second step: take according to above-mentioned element ratio and nickeliferous easily dissolve compound, mix with ammonium chloride, natrium citricum, add deionized water and stirring and be mixed with solution, and regulate pH to 10 with ammoniacal liquor, in this step, described ammonium chloride addition is suitable with nickel compound containing, and natrium citricum addition is about the half of nickel compound containing;
3rd step: add nano-graphene prepared by the first step in the mixed solution of upwards step, ultrasonic disperse 30min, then slowly adds the sodium hypophosphite aqueous solution of 5%, adjustment pH to 10,60min is stirred at 40 DEG C, after reacting completely, deionized water is washed, and suction filtration is dry, namely product is obtained, for the black powder of slightly metallic luster, in this step, the mixed proportion of described mixed solution and the sodium hypophosphite aqueous solution is volume 7:3.
In the present invention, described sensitizer is saturated SnCl
2solution, described activator is the PbCl of 1g/mL
2solution.
beneficial effect:
Present invention process is simple, handled easily, reasonable mixture ratio of components, the product prepared by present invention process have thermal diffusivity good, conduct electricity the excellent properties such as fast, wear-resisting, anticorrosion, especially solve the chemical bond problem of Graphene and metal, make it effective and the combination of other Metal Phase.
Detailed description of the invention
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below by embodiment, the present invention being specifically described:
Weigh 0.1g graphene oxide/Graphene and join the saturated SnCl of 100ml
2in liquid, the ultrasonic 50min of room temperature carries out sensitized treatment.After sensitization, carry out vacuum filtration with water pump on filter membrane, deionized water washing is to neutral.Vacuum drying is for subsequent use.
The Graphene that sensitized treatment is good is joined the PbCl that 100ml concentration is 1g/mL
2activate in activating solution, activation temperature is room temperature, and the time is 50min, keeps ultrasonic vibration in process.After activation, carry out vacuum filtration with water pump on filter membrane, deionized water washing, to neutral, obtains black oxidation Graphene/graphene powder.
Take nickelous sulfate 1.15g, ammonium chloride 1.59g, natrium citricum 0.54g, joined in beaker successively by above-mentioned solid, and be configured to the solution of 70ml clear, solution colour becomes green.In continuous whipping process, regulate solution ph to 10 with the concentrated ammonia liquor of 28%, solution colour becomes blue.In above-mentioned solution, add the pretreated Graphene of 0.1g, stir, ultrasonic, make its dispersion as far as possible.After ultrasonic, beaker is transferred in oil bath pan, in beaker, adds the aqueous solution that 30ml has dissolved 1.78g sodium hypophosphite, and under 40 DEG C of conditions stirring reaction 1h.After completion of the reaction, use filter membrane vacuum filtration, deionized water is washed, and drying obtains the powder of black slightly metallic luster.
More than show and describe general principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (2)
1. a nano-graphene composite, comprises the elemental constituent of following mass percent: Graphene 25 ~ 75%, nickel 23 ~ 71%, phosphorus 2 ~ 4%; It is characterized in that, described nano-graphene composite is made up of following preparation method:
The first step: take nano-graphene 1 part according to weight, first, Graphene is put into deionized water, and ultrasonic vibration disperses, process 30min, suction filtration moves in sensitizer and carries out sensitized treatment, ultrasonic vibration 40 ~ 60min, suction filtration moves in activator and activates, ultrasonic vibration 40 ~ 60min, suction filtration also spends deionized water to neutral, and vacuum drying is for subsequent use;
Second step: take according to the elemental constituent of described mass percent and nickeliferous easily dissolve compound, mix with ammonium chloride, natrium citricum, add deionized water and stirring and be mixed with solution, and regulate pH to 10 with ammoniacal liquor, in this step, described ammonium chloride addition is suitable with nickel compound containing, and natrium citricum addition is about the half of nickel compound containing;
3rd step: add nano-graphene prepared by the first step in the mixed solution of upwards step, ultrasonic disperse 30min, then slowly adds the sodium hypophosphite aqueous solution of 5%, adjustment pH to 10,60min is stirred at 40 DEG C, after reacting completely, deionized water is washed, and suction filtration is dry, namely product is obtained, for the black powder of slightly metallic luster, in this step, the mixed proportion of described mixed solution and the sodium hypophosphite aqueous solution is volume 7:3.
2. a kind of nano-graphene composite according to claim 1, is characterized in that, described sensitizer is saturated SnCl
2solution, described activator is the PbCl of 1g/mL
2solution.
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| CN103386483B true CN103386483B (en) | 2016-03-30 |
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| CN103736993B (en) * | 2014-01-03 | 2015-12-09 | 上海交通大学 | The preparation method of graphene/copper composite material |
| CN106348284A (en) * | 2015-07-15 | 2017-01-25 | 湖南元素密码石墨烯高科技有限公司 | Methods for preparing graphene and graphene composite from artificial diamond |
| CN111690324B (en) * | 2020-07-21 | 2023-03-21 | 宁波计氏金属新材料有限公司 | Corrosion-resistant chromium-free coating and surface treatment process thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857221A (en) * | 2010-05-21 | 2010-10-13 | 哈尔滨工业大学 | Method for preparing graphene compounds and graphene oxide compounds with high efficiency |
| CN102254582A (en) * | 2010-05-18 | 2011-11-23 | 国家纳米科学中心 | Graphite alkenyl conductive material and preparation method thereof |
| CN102385938A (en) * | 2011-11-10 | 2012-03-21 | 电子科技大学 | Metal matrix graphene composite electrical contact material and preparation method thereof |
| CN102731258A (en) * | 2012-05-21 | 2012-10-17 | 中国科学院大连化学物理研究所 | Method for preparing low carbon polyol by internal circulating catalysis and conversion of carbohydrate |
| KR20120139959A (en) * | 2011-06-20 | 2012-12-28 | 이재환 | High density nano coating compositions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102254582A (en) * | 2010-05-18 | 2011-11-23 | 国家纳米科学中心 | Graphite alkenyl conductive material and preparation method thereof |
| CN101857221A (en) * | 2010-05-21 | 2010-10-13 | 哈尔滨工业大学 | Method for preparing graphene compounds and graphene oxide compounds with high efficiency |
| KR20120139959A (en) * | 2011-06-20 | 2012-12-28 | 이재환 | High density nano coating compositions |
| CN102385938A (en) * | 2011-11-10 | 2012-03-21 | 电子科技大学 | Metal matrix graphene composite electrical contact material and preparation method thereof |
| CN102731258A (en) * | 2012-05-21 | 2012-10-17 | 中国科学院大连化学物理研究所 | Method for preparing low carbon polyol by internal circulating catalysis and conversion of carbohydrate |
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Effective date of registration: 20160316 Address after: 410000 Hunan province Changsha Furong District Road No. 98 Building 2 male incubator building 508 room Patentee after: HUNAN YUANSU MIMA GRAPHENE High-technology Co., Ltd. Address before: 410000 Hunan province city Changsha benevolent Park Furong District Yi Xin Yuan building 201 room 2 Patentee before: Tan Bin |
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