CN107434250A - A kind of preparation method of the graphene of nickel-loaded - Google Patents
A kind of preparation method of the graphene of nickel-loaded Download PDFInfo
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- CN107434250A CN107434250A CN201710631435.XA CN201710631435A CN107434250A CN 107434250 A CN107434250 A CN 107434250A CN 201710631435 A CN201710631435 A CN 201710631435A CN 107434250 A CN107434250 A CN 107434250A
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- nickel
- graphene
- sodium chloride
- nickel salt
- glucose
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The present invention relates to a kind of preparation method for the graphene for preparing load nickel particle, the precursor powder of self assembly is dried to obtain after nickel salt, glucose and sodium chloride are well mixed in certain proportion using spray dryer, calcining reduction handles to obtain the composite powder of the graphene of nickel-loaded under atmosphere of hydrogen in tube furnace afterwards.The method that this method is peeled off relative to the method and machine of redox graphene is more cost-effective and can realize prepared by magnanimity；Secondly realize simultaneously and load nickel particle in graphenic surface, substantially increase the wetability and associativity between graphene and metallic matrix.
Description
Technical field
The present invention relates to it is a kind of using spray drying and chemical vapour deposition technique combine a step realize graphene growth and
The method of the area load of nickel particle, belong to the preparation field of graphene.
Background technology
And since 2004, the scientist Geim and Morozov of Britain are by mechanically pulling off method and mono-layer graphite piece have been made
Afterwards, people just expand substantial amounts of research to graphene.Graphene has the two dimensional crystal structure of monoatomic layer, it special
Structure makes it have excellent physical property and mechanical property.The theoretical specific surface area of graphene is up to 2630m2/ g, it strong
Degree is highest in known material, can reach 130GPa, be more than 100 times of Steel material；Young's modulus 1100GPa, with
One-dimensional CNT is suitable.Graphene theory carrier mobility is 15000cm2V-1s-1, it is the carrier mobility being currently known
Twice of the indium antimonide materials of rate highest is commercial silicon chip more than 10 times；Thermal conductivity is 5000Wm-1·K-1, it is diamond
3 times, therefore graphene is described as the preferable reinforcement of metal-base composites.
The preparation method of graphene mainly has micromechanics stripping method, liquid phase stripping method, CVD, SiC pyrolysismethods, oxygen at present
Graphite alkene reducing process.Micromechanics stripping method and liquid phase stripping method are exactly to be peeled off original crystalline flake graphite using the effect of mechanical force
Open, this method time consumption and energy consumption is more, hardly results in the graphene of individual layer.CVD and SiC pyrolysis rule are decomposed using carbon source
Deposition forms graphene, and this method production efficiency is very low, is difficult to the commercial application of graphene.For current research
For, it is exactly that graphene oxide reducing process prepares graphene that application is the most ripe also the most convenient.Graphite oxide reducing process is
By the way that native graphite is carried out into oxidation processes and ultrasonic disperse, the oxidation stone that a large amount of oxy radicals are contained by surface and edge is obtained
The graphene oxide solution of black alkene piece composition, then removes graphene oxide layer surface by thermal reduction or chemical reduction method
With the oxygen-containing group at edge, the method for finally giving graphene, the graphene that this method obtains still has certain structure
Defect, the performance for being not so good as to be obtained with CVD method in terms of electric conductivity is good, and time-consuming multi-step is cumbersome, it is necessary to substantial amounts of chemistry
Reagent.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the graphene of simple and easy preparation load nickel particle.Should
Method can prepare graphene fast and stable and uniformly load nickel particle at it, and this method process is simple, made
The graphene and nickel associativity obtained is good.To achieve the above object, the present invention is to be realized by the following technical programs,
A kind of preparation method of the graphene of nickel-loaded, its feature include procedure below：
(1) spray-on process prepares presoma：
Water is dissolved in after nickel salt, glucose, sodium chloride three are mixed with certain proportion and is stirred, and utilizes spraying afterwards
Drying machine sprays drying at 150 DEG C, that is, obtains the presoma of sodium chloride, glucose and nickel salt self-assembled structures.
(2) generation of the graphene-structured of nickel-loaded
The precursor powder of self-assembled structures made from step (1) is forged in 700-750 DEG C of hydrogen atmosphere pipe type stove
Burn 2 hours, wash away the graphene-structured of sodium chloride and drying to obtain area load nickel particle afterwards.
Preferably, step (1) by nickel salt, glucose, sodium chloride three with (0.3-2):1：The molar ratio of (50-300)
Mixing.Further, when the selection of step (1) nickel salt is nickel nitrate, nickel salt, glucose, the mol ratio of sodium chloride are 0.45:1:60；
When nickel salt selection is nickel chloride, nickel salt, glucose, the mol ratio of sodium chloride are 2:1:240.
Step (2) calcining heat may be selected to be 730 degrees Celsius, hydrogen flowing quantity 100ml/min.
The present invention has been implemented in combination with the graphene of area load nickel particle using spray drying process and chemical vapour deposition technique
Magnanimity prepare, obtained graphenic surface nickel particle Load Balanced is firmly combined with, and graphene crystallinity is preferable, is answered in Metal Substrate
The application of the reinforcement of condensation material etc. has preferable prospect.With advantages below：This method raw materials first are honest and clean
Valency is easy to get, and method is also relatively easy, and the method peeled off relative to the method and machine of redox graphene is more cost-effective
And it can realize prepared by magnanimity；Secondly we realize simultaneously loads nickel particle in graphenic surface, substantially increases graphite
Wetability and associativity between alkene and metallic matrix, are more suitable as metal-base composites reinforcement；This method can
To regulate and control the pattern of the content of nickel and graphene by regulating and controlling different ratios, different occasions can should be applied to.
Brief description of the drawings
Fig. 1 a are the pattern under the ESEM of the self assembly presoma after being spray-dried in embodiment 1.
Fig. 1 b are pattern under ESEM of the presoma after high-temperature calcination reduces in embodiment 1.
Fig. 1 c are the stereoscan photograph of the graphene of the nickel-loaded obtained in embodiment 1.
Fig. 1 d are the transmission electron microscope photo of the graphene of the nickel-loaded obtained in embodiment 1.
Fig. 1 e are that the graphene of the graphene-supported nickel of the nickel-loaded obtained in embodiment 1 is applied in Cu-base composites
Obtained stress-strain diagram.
Fig. 2 a are the transmission electron microscope photo of the graphene of nickel-loaded in embodiment 2.
Fig. 2 b are the XRD test results of the graphene of nickel-loaded in embodiment 2.
Fig. 2 c are the Raman test result of the graphene of nickel-loaded in embodiment 2.
Fig. 3 is the stereoscan photograph of the graphene of the nickel-loaded obtained in embodiment 3.
Embodiment
The present invention is further illustrated with reference to embodiment, these embodiments are served only for the explanation present invention, are not intended to limit this
Invention.
Embodiment 1
By nickel chloride (3.37g), glucose (1.28g) and sodium chloride (100g) mixing are dissolved in 400ml deionized waters and stirred
Mix uniformly (three's mol ratio be 2:1:240).Uniform mixed solution is spray-dried under conditions of 150 degree afterwards, obtained
The precursor powder of self assembly, two hours, Zhi Houyong are calcined by 730 degree of hydrogen (hydrogen flowing quantity 150ml/min) conditions
Deionized water washes away sodium chloride and is dried in vacuo, that is, obtains the graphene-structured of surface uniform load nickel.By being spray-dried
To the SEM patterns of self assembly presoma see Fig. 1 a, the pattern after the calcining of self assembly presoma is shown in Fig. 1 b, the load finally obtained
The SEM photograph and TEM photos of the graphene of nickel are shown in Fig. 1 c and Fig. 1 d respectively, the graphene of obtained nickel-loaded are applied to copper-based
The stress-strain diagram obtained in composite is shown in Fig. 1 e.
Embodiment 2
By nickel nitrate (0.6186g), glucose (1.8g) and sodium chloride (35g) mixing are dissolved in 150ml deionized waters and stirred
Mix uniformly (three's mol ratio be 0.46:1:60).Uniform mixed solution is spray-dried under conditions of 150 degree afterwards, obtained
To the precursor powder of self assembly, two hours are calcined by 730 degree of hydrogen (hydrogen flowing quantity 150ml/min) conditions, afterwards
Sodium chloride is washed with deionized water and is dried in vacuo, that is, obtains the graphene-structured of surface uniform load nickel.Obtained nickel-loaded
Graphene TEM patterns see Fig. 2 a, the XRD spectrum of the powder finally obtained is shown in Fig. 2 b, and Raman, which characterizes, sees Fig. 2 c.
Embodiment 3
By nickel nitrate (0.4124g), glucose (1.8g) and sodium chloride (35g) mixing are dissolved in 150ml deionized waters and stirred
Mix uniformly (three's mol ratio be 0.30:1:60).Uniform mixed solution is spray-dried under conditions of 150 degree afterwards, obtained
To the precursor powder of self assembly, two hours are calcined by 730 degree of hydrogen (hydrogen flowing quantity 150ml/min) conditions, afterwards
Sodium chloride is washed with deionized water and is dried in vacuo, that is, obtains the graphene-structured of surface uniform load nickel.Obtained graphene
SEM patterns see Fig. 3.
Claims (4)
1. a kind of preparation method of the graphene of nickel-loaded, its feature include procedure below：
(1) spray-on process prepares presoma：
Water is dissolved in after nickel salt, glucose, sodium chloride three are mixed with certain proportion and is stirred, and utilizes spray drying afterwards
Machine sprays drying at 150 DEG C, that is, obtains the presoma of sodium chloride, glucose and nickel salt self-assembled structures.
(2) generation of the graphene-structured of nickel-loaded
It is small that the precursor powder of self-assembled structures made from step (1) is calcined in 700-750 DEG C of hydrogen atmosphere pipe type stove to 2
When, the graphene-structured of sodium chloride and drying to obtain area load nickel particle is washed away afterwards.
2. according to the method for claim 1, it is characterised in that step (1) by nickel salt, glucose, sodium chloride three with
(0.3-2):1：The molar ratio mixing of (50-300).
3. according to the method for claim 1, it is characterised in that when the selection of step (1) nickel salt is nickel nitrate, nickel salt, grape
Sugar, the mol ratio of sodium chloride are 0.45:1:60；When nickel salt selection is nickel chloride, nickel salt, glucose, the mol ratio of sodium chloride are
2:1:240。
4. according to the method for claim 1, it is characterised in that the selection of step (2) calcining heat is 730 degrees Celsius, hydrogen
Flow is 100ml/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793130A (en) * | 2018-07-15 | 2018-11-13 | 天津大学 | The method that spray-on process prepares graphene |
| CN108817727A (en) * | 2018-07-19 | 2018-11-16 | 河南科技大学 | Pyrolysismethod synthesis is by force in conjunction with the high-strength Sn-Ag-Cu-RE system composite soldering and preparation method of the enhancing of copper-plated graphite alkene |
| CN112194119A (en) * | 2020-10-13 | 2021-01-08 | 河北医科大学 | Method for synthesizing three-dimensional graphene from solid sugar |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756167A (en) * | 2016-12-02 | 2017-05-31 | 天津大学 | Fabricated in situ three-dimensional grapheme strengthens the preparation method of nickel-base composite material |
-
2017
- 2017-07-28 CN CN201710631435.XA patent/CN107434250A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756167A (en) * | 2016-12-02 | 2017-05-31 | 天津大学 | Fabricated in situ three-dimensional grapheme strengthens the preparation method of nickel-base composite material |
Non-Patent Citations (2)
| Title |
|---|
| JIAN QIN ET AL.: "Graphene Networks Anchored with Sn@Graphene as Lithium Ion Battery Anode", 《ACS NANO》 * |
| 孙翠: "喷雾干燥法制备锡及锡氧化物-石墨烯复合材料及其电化学性能研究", 《中国学位论文全文数据库》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793130A (en) * | 2018-07-15 | 2018-11-13 | 天津大学 | The method that spray-on process prepares graphene |
| CN108817727A (en) * | 2018-07-19 | 2018-11-16 | 河南科技大学 | Pyrolysismethod synthesis is by force in conjunction with the high-strength Sn-Ag-Cu-RE system composite soldering and preparation method of the enhancing of copper-plated graphite alkene |
| CN112194119A (en) * | 2020-10-13 | 2021-01-08 | 河北医科大学 | Method for synthesizing three-dimensional graphene from solid sugar |
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