CN101992303A - Method for preparing graphene/Ni nano composite material - Google Patents
Method for preparing graphene/Ni nano composite material Download PDFInfo
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- CN101992303A CN101992303A CN 201010523516 CN201010523516A CN101992303A CN 101992303 A CN101992303 A CN 101992303A CN 201010523516 CN201010523516 CN 201010523516 CN 201010523516 A CN201010523516 A CN 201010523516A CN 101992303 A CN101992303 A CN 101992303A
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Abstract
The invention relates to a method for preparing a graphene/Ni nano composite material and belongs to the field of preparation of nano composite materials. Natural scale graphite is used as a raw material, and the method comprises the following main steps of: oxidizing the raw material to prepare oxidized graphite by using a Hummers method; ultrasonically dissolving the oxidized graphite and nickel chloride in deionized water, adding hydrazine hydrate, regulating the pH value of the solution to be 10.5 to 11 by using sodium hydroxide, and performing reflux reaction at the temperature of 110 DEG C for 3 to 4 hours under the protection of nitrogen; and collecting the precipitate, washing and drying to prepare the graphene/Ni nano composite material. The Ni nano particles in the prepared graphene/Ni nano composite material are coated by graphene sheets, the Ni can be prevented from being oxidized by air, harmful effect generated by direct contact of Ni and organisms is avoided, and the composite material is an ideal material for targeted medicament delivery and thermal therapy. The method is simple and practicable in operation technology, short in reaction time, high in repeatability, low in cost and suitable for industrialization.
Description
Technical field
The invention belongs to the nano composite material preparation field, the preparation method of particularly a kind of Graphene/Ni nano composite material.
Background technology
Graphene is the mono-layer graphite crystal, and it is the basic structural unit that makes up other dimension carbonaceous materials (as zero dimension fullerene, one dimension CNT, three-dimensional graphite).Graphene has excellent electricity, calorifics and mechanical property, is expected in the acquisition extensive use of fields such as high-performance nano electronic device, composite, field emmision material, gas sensor and energy storage; Because its unique two-dimensional structure, Graphene has contained abundant and novel physical phenomenon, for the research of quantum-mechanical phenomenon provides ideal platform, has an important researching value, therefore, Graphene becomes one of material science and Condensed Matter Physics field hot research in recent years rapidly.
Nickel is a kind of important feeromagnetic metal, has good non-oxidizability and corrosion resistance, and the intensity and the plasticity of nickel are also fine simultaneously, are used for fields such as various types of stainless steels, magnetic material, battery and catalysis in a large number; With Graphene and the compound nano composite material of making of metallic nickel, have important use at biomedical sector and be worth, because Graphene itself has excellent biological compatibility on the one hand, and pliability is good, specific area is big, and medicine is had good suction-operated; Ni nano particle magnetic field navigation is effective on the other hand, target is good, absorbs electromagnetic wave efficient height, and heating effect is remarkable under the effect of alternating magnetic field; Graphene/Ni nano composite material can arrive diseased region as pharmaceutical carrier under introduction by magnetic field, thereby realize target administration or thermotherapy etc., this target administration can alleviate the toxic and side effect of medicine to normal structure, and strengthens drug effect, is the important research direction of new drug carrier system; The present invention prepares a kind of Graphene/Ni nano composite material, different with general graphene composite material, the just not simple surface of Ni nano particle in this Graphene/Ni nano composite material attached to graphene film, but be wrapped in by graphene film, so both can prevent the oxidation of Ni, can stop Ni to contact with the direct of organism again, be the ideal material of target administration and thermotherapy.
Summary of the invention
The object of the invention is to provide the preparation method of a kind of Graphene/Ni nano composite material, adopts following technical scheme:
1) with the natural flake graphite is raw material, its oxidation obtained graphite oxide with the Hummers method;
2) with graphite oxide and nickel chloride ultrasonic dissolution in deionized water, the concentration of graphite oxide is 0.3 ~ 0.5 g/L, the concentration of nickel chloride is 3 ~ 4 g/L;
3) dripping mass fraction is the hydrazine hydrate of 85 %, and it is 40 ~ 50 mL that every liter of solution needs the consumption of hydrazine hydrate;
4) with sodium hydrate regulator solution pH=10.5 ~ 11,110 ℃ of stirring and refluxing reaction 3 ~ 4 h under nitrogen protection;
5) after the cooling, filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
The Ni nano particle is not simple surface attached to Graphene in the Graphene/Ni nano composite material of the present invention's preparation, but wrapped up by graphene film, so both can prevent the oxidation of Ni, can stop Ni directly to contact the harmful effect that is produced again with organism, this method operating procedure is simple, and the reaction time is short, good reproducibility, cost is low, is easy to industrializing implementation.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the Graphene/Ni nano composite material of the embodiment of the invention 1 preparation, and wherein abscissa is the angle of diffraction (2
θ), unit for the degree (
0), ordinate is a diffracted intensity, unit is cps;
Fig. 2 and Fig. 3 are transmission electron microscope (TEM) photo of the Graphene/Ni nano composite material of the embodiment of the invention 1 preparation.
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are described in detail, but protection scope of the present invention is not limited to these embodiment.
Embodiment 1:
Take by weighing graphite oxide, 368 mg nickel chlorides that 40 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4.5 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection, after the cooling, filters, and uses deionized water and absolute ethanol washing respectively, with the product drying; Fig. 1 is the XRD figure of product, and all diffraction maximums all can belong to cubic system Ni(JCPDS 04-0850).The diffraction maximum of graphite does not appear in XRD figure, shows that the reunion of Graphene has obtained effective control; Fig. 2 and Fig. 3 are the TEM figure of product, can see that metal Ni nano particle is wrapped up by graphene film, and grain diameter is about 80 ~ 160 nm.
Embodiment 2:
Take by weighing graphite oxide, 300 mg nickel chlorides that 30 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 3:
Take by weighing graphite oxide, 300 mg nickel chlorides that 30 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dropwise 5 mL mass fraction is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 4:
Take by weighing graphite oxide, 300 mg nickel chlorides that 30 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=11,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 5:
Take by weighing graphite oxide, 300 mg nickel chlorides that 30 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 4 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 6:
Take by weighing graphite oxide, 300 mg nickel chlorides that 50 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 7:
Take by weighing graphite oxide, 300 mg nickel chlorides that 50 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dropwise 5 mL mass fraction is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 8:
Take by weighing graphite oxide, 300 mg nickel chlorides that 50 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=11,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 9:
Take by weighing graphite oxide, 300 mg nickel chlorides that 50 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 4 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 10:
Take by weighing graphite oxide, 400 mg nickel chlorides that 30 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 11:
Take by weighing graphite oxide, 400 mg nickel chlorides that 30 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dropwise 5 mL mass fraction is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 12:
Take by weighing graphite oxide, 400 mg nickel chlorides that 30 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=11,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 13:
Take by weighing graphite oxide, 400 mg nickel chlorides that 30 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 4 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 14:
Take by weighing graphite oxide, 400 mg nickel chlorides that 50 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 15:
Take by weighing graphite oxide, 400 mg nickel chlorides that 50 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dropwise 5 mL mass fraction is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 16:
Take by weighing graphite oxide, 400 mg nickel chlorides that 50 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=11,110 ℃ of stirring and refluxing are reacted 3 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Embodiment 17:
Take by weighing graphite oxide, 400 mg nickel chlorides that 50 mg prepare with the Hummers method, ultrasonic dissolution is in 100 mL deionized waters.Dripping 4 mL mass fractions is the hydrazine hydrate of 85 %, and with sodium hydrate regulator solution pH=10.5,110 ℃ of stirring and refluxing are reacted 4 h under nitrogen protection; after the cooling; filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
Claims (5)
1. the preparation method of Graphene/Ni nano composite material, it is characterized in that: with graphite oxide and nickel chloride is reactant, hydrazine hydrate is as reducing agent, with water as reaction medium, backflow prepared in reaction Graphene/Ni nano composite material under nitrogen protection.
2. the preparation method of a kind of Graphene as claimed in claim 1/Ni nano composite material may further comprise the steps:
1) graphite oxide and nickel chloride ultrasonic dissolution are obtained mixed aqueous solution in deionized water, the concentration of graphite oxide is 0.3 ~ 0.5 g/L, and the concentration of nickel chloride is 3 ~ 4 g/L;
2) dripping mass fraction is the hydrazine hydrate of 85 %, and it is 40 ~ 50 mL that every liter of mixed aqueous solution needs the consumption of hydrazine hydrate;
3) the pH value of adjusting mixed aqueous solution is 10.5 ~ 11, reacts 3 ~ 4 h in 110 ℃ of stirring and refluxing under nitrogen protection;
4) after the cooling, filter, use deionized water and absolute ethanol washing respectively, the product drying is obtained Graphene/Ni nano composite material.
3. the preparation method of a kind of Graphene as claimed in claim 1 or 2/Ni nano composite material is characterized in that: be raw material with the natural flake graphite, with the Hummers method its oxidation obtained graphite oxide.
4. the preparation method of a kind of Graphene as claimed in claim 2/Ni nano composite material is characterized in that: adopt NaOH to regulate the pH value of mixed aqueous solution.
5. the preparation method of a kind of Graphene as claimed in claim 1 or 2/Ni nano composite material is characterized in that: the metal Ni nano particle in described Graphene/Ni nano composite material is wrapped up by graphene film, and grain diameter is 80 ~ 160 nm.
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