CN107755691B - A kind of preparation method of carbon coating copper micro-nano granules composite material - Google Patents
A kind of preparation method of carbon coating copper micro-nano granules composite material Download PDFInfo
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- CN107755691B CN107755691B CN201710954647.1A CN201710954647A CN107755691B CN 107755691 B CN107755691 B CN 107755691B CN 201710954647 A CN201710954647 A CN 201710954647A CN 107755691 B CN107755691 B CN 107755691B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1241—Metallic substrates
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Abstract
The invention discloses a kind of preparation methods of carbon coating copper micro-nano granules composite material.The method that the present invention uses hydrothermal synthesis to combine with high temperature cabonization, is made carbon coating copper micro-nano granules composite material.By this method obtain compound carbon coating is good, operating process is simple, produced convenient for magnanimity.
Description
Technical field
The present invention relates to a kind of preparation methods of carbon coating copper micro-nano granules composite material, belong to carbon material synthetic technology
Field.
Background technique
There is very excellent physicochemical property using inorganic matter or organic matter as the core shell nanostructure of shell, cause
The great interest of vast researcher, wherein carbon-clad metal (M/C) structure, especially by taking Cu/C as an example, since its is cheap
And unique property, in biosensor, supercapacitor, the extensive use of fuel cell and catalyst etc. has been obtained
To further investigation.By carbon coating, the performances such as the unique electromagnetism optics of this Cu fine-grained particles are not only remained, and assign it
Better chemical stability, resistance to acid and alkali, biocompatibility and surface-functionalized various selective, but also can be to particle
Grain is modified, and then is expanded it and widely applied.Up to the present, the method that research and development synthesize this novel structure has very
It is more, such as spray-on process, microwave irradiation, electric arc, pulsed laser irradiation method, the heat of chemical vapour deposition technique and organo-metallic compound
Decompose etc..However above method the high requirements on the equipment, subsequent treatment process is complicated, and the reaction time is longer, energy consumption height and yield
Minimum, these significantly limit the large-scale production of carbon coating copper micro-nano granules composite material.
Summary of the invention
For the deficiency of a variety of methods of current research and development synthesis carbon coating copper micro-nano granules composite material, the present invention is provided
It is a kind of through the modes such as hydrothermal synthesis and high temperature cabonization, the method for preparing the composite materials of carbon coating copper micro-nano granules should
Method process is simple, produces convenient for magnanimity.
In the present invention, spherical copper powder particle can be tied after surfactant is surface-treated between organic carbon source
It closes, to coat organic carbon source lotion on the surface of copper, the product for then obtaining hydro-thermal reaction is under the atmosphere of inert gas
High-temperature roasting is carried out, during heating, the organic carbon source for being coated on copper surface is decomposed, high temperature cabonization, to generate carbon
Coated copper micro-nano granules compound.
Technical solution of the present invention is specifically described as follows.
The present invention provides a kind of preparation method of carbon coating copper micro-nano granules composite material, the specific steps are as follows:
(1) firstly, in a solvent by spherical copper powder and surfactant, 40~80min of mixing being stirred at room temperature, is subsequently added into
Organic carbon source continues 1~2h of stirring, obtains mixed emulsion；Then, mixed emulsion is transferred to polytetrafluoroethyllining lining
It in container, is placed in stainless steel cauldron, seals, carry out hydro-thermal process, control hydrothermal temperature is 50-200 DEG C, and the reaction time is
12-48h；After reaction, natural cooling is filtered, washing, and filter cake vacuum drying obtains organic matter/copper complex；Wherein:
The solvent is the mixture of deionized water or deionized water and dehydrated alcohol composition；
The spherical copper powder, surfactant, organic carbon source and solvent mass ratio be 1:(0.1-10): (0.2-10):
(10-100)；
(2) after roasting organic matter/copper complex obtained in step (1) under an inert atmosphere, room is naturally cooled to
Temperature obtains carbon coating copper micro-nano granules composite material.
In the present invention, in step (1), spherical copper powder is 100~500 mesh.
In the present invention, in step (1), the volume ratio of deionized water and dehydrated alcohol in solvent is 1:3~3:1.
In the present invention, in step (1), surfactant is selected from hexadecyltrimethylammonium chloride, cetyl trimethyl
One or more of ammonium bromide or polyvinylpyrrolidone.
In the present invention, in step (1), the organic carbon source is phenolic resin, saccharide compound or other macromolecule chemical combination
Object；Preferably, organic carbon source is phenolic resin, it is furthermore preferred that in phenol-formaldehyde resin or resorcinol-formaldehyde resin
It is one or two kinds of.
In the present invention, in step (1), hydrothermal temperature is 120-180 DEG C, reaction time 20-30h.
In the present invention, in step (1), vacuum drying temperature is 50~80 DEG C.
In the present invention, in step (2), calcination procedure is as follows: with heating rate for 1-5 DEG C/min, being warming up to 600-1000
DEG C, react 6-20h.
In the present invention, the carbon coating copper micro-nano granules composite material as made from above-mentioned preparation is dark brown black powder,
Powder diameter≤10 μm, are in chondritic and pattern is preferable, size distribution uniform, and product purity is high.And the prior art
It compares, the beneficial effects of the present invention are:
Simple using the method for the present invention apparatus and process, low in cost, the period is shorter and yield is higher, can continuous scale metaplasia
It produces, is easy to industrializing implementation.And obtained product structure uniform, controllable, crystallinity is good, has a good application prospect.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of carbon coating copper micro-nano granules compound prepared by embodiment 1.
Fig. 2 is the microphoto of the single carbon coating copper particle of carbon coating copper micro-nano granules compound prepared by embodiment 1.
Fig. 3 is carbon coating copper micro-nano granules compound X ray diffracting spectrum prepared by embodiment 1.
Specific embodiment
Below by way of specific implementation, in conjunction with attached drawing, the present invention will be further described, but the present invention is not limited in following reality
Apply example.
Method described in various embodiments of the present invention is conventional method unless otherwise instructed.
Raw material used in various embodiments of the present invention unless otherwise instructed, can be bought from disclosed commercial sources
It arrives.
The magnitude of chemical substance used in various embodiments of the present invention is determined by pre-set range, with
Gram, milliliter etc. is measurement unit.
Instrument used in various embodiments of the present invention or device model and the information of manufacturer are as follows:
Air dry oven, model DHG-9920A, manufacturer: Shanghai Yiheng Scientific Instruments Co., Ltd；
Vacuum oven, DZF-6030A, Shanghai Yiheng Scientific Instruments Co., Ltd；
Tube furnace, II type of SL1700, Shanghai Sheng Li test equipment Co., Ltd；
X-ray diffractometer (XRD), Panaco company, X PERT PRO Holland；
Scanning electron microscope (SEM), S-3400N Hitachi, Japan.
Embodiment 1
A kind of preparation method of carbon coating copper micro-nano granules composite material, specifically comprises the following steps:
(1) 2g copper powder (100 mesh) is scattered in 20g solvent, at room temperature high-speed stirred, and 0.2g surface-active is then added
Agent continues to stir 1h, 1g organic carbon source is then added, stirs 1.5h, mixed emulsion is made.Then, this liquid is transferred to poly-
It in the container of tetrafluoroethene liner, is placed in stainless steel cauldron, seals, carry out hydro-thermal process, controlled at 180 DEG C, instead
Should for 24 hours, after natural cooling, obtained reaction solution is filtered, clean after, filter cake in 60 DEG C vacuum drying to get to organic matter/
Copper complex；
The solvent is deionized water；
The surfactant is polyvinylpyrrolidone:
The organic carbon source is phenol-formaldehyde resin, and phenolic aldehyde is that 1:4 carries out reacting mixing obtained in mass ratio
Object, and it is configured to ethyl alcohol the mixed solution of 20wt%；
(2) by organic matter/copper complex obtained in step (1) under the atmosphere of nitrogen, control heating rate is 5
DEG C/min, 600 DEG C are warming up to, high-temperature roasting 8h is carried out.Then cooled to room temperature to get arrive carbon coating copper micro-nano granules
Composite material.
Above-mentioned obtained carbon coating copper micro-nano granules composite material, be dark brown black powder, powder diameter≤10 μm,
In chondritic and pattern it is preferable, size distribution uniform.After copper in carbon coating copper complex is removed, institute's carbon coated
The thickness of layer is in 50 rans.
Above-mentioned obtained carbon coating copper micro-nano granules composite material is observed using scanning electron microscope, it is obtained
Scanning electron microscope image is as depicted in figs. 1 and 2.Fig. 1 is the shape appearance figure of carbon coating copper micro-nano granules compound, and compound is in black
Or dark brown black powder, in spherical；Fig. 2 is the stereoscan photograph of carbon coating copper micro-nano granules compound, as it can be seen that copper in figure
Fine-grained particles surface is coated with apparent carbon-coating structure.
Above-mentioned obtained carbon coating copper micro-nano granules composite material is analyzed using x-ray diffractometer, gained
The wide-angle XRD that arrives is as shown in figure 3, as can be seen from Figure 3 43.169 ° of base peak, and 50.455 °, 74.089 ° are all elemental copper
Standard feature peak, diffraction maximum is sharp, the elemental copper with high crystallinity.
Embodiment 2
A kind of preparation method of carbon coating copper micro-nano granules composite material, specifically comprises the following steps:
(1) 1.5g copper powder (300 mesh) is scattered in 20g solvent, at room temperature high-speed stirred, and it is living that the surface 0.2g is then added
Property agent, continue stir 1h, then be added 0.8g organic carbon source, stir 1.5h, mixed emulsion is made.Then, this liquid is shifted
It to the container of polytetrafluoroethyllining lining, is placed in stainless steel cauldron, seals, hydro-thermal process is carried out, controlled at 180
DEG C, for 24 hours, after natural cooling, obtained reaction solution is filtered for reaction, and after cleaning, filter cake is in 60 DEG C of vacuum drying to get to having
Machine object/copper complex；
The solvent is deionized water；
The cationic surfactant is cetyl trimethylammonium bromide:
The organic carbon source is phenol-formaldehyde resin, and phenolic aldehyde is that 1:4 carries out reacting mixing obtained in mass ratio
Object, and it is configured to ethyl alcohol the mixed solution of 20wt%；
(2) in a nitrogen atmosphere by organic matter/copper complex obtained in step (1), control heating rate be 5 DEG C/
Min is warming up to 700 DEG C, carries out high-temperature roasting 8h.Then cooled to room temperature is to get multiple to carbon coating copper micro-nano granules
Condensation material.After copper in carbon coating copper complex is removed, the thickness of coated carbon-coating is in 20 rans.
Embodiment 3
A kind of preparation method of carbon coating copper micro-nano granules composite material, specifically comprises the following steps:
(1) 1.5g copper powder (500 mesh) is scattered in 20g solvent, at room temperature high-speed stirred, and 0.5g cation is then added
Surfactant continues to stir 1h, 1g organic carbon source is then added, stirs 1.5h, mixed emulsion is made.Then, by this liquid
It is transferred in the container of polytetrafluoroethyllining lining, is placed in stainless steel cauldron, seal, carry out hydro-thermal process, controlled at
180 DEG C, reaction for 24 hours, after natural cooling, obtained reaction solution is filtered, clean after, filter cake in 60 DEG C vacuum drying to get
To organic matter/copper complex；
The solvent is the mixed solution that deionized water and ethyl alcohol are 1:1 composition in mass ratio；
The cationic surfactant is hexadecyltrimethylammonium chloride:
The organic carbon source is phenol-formaldehyde resin, and phenolic aldehyde is that 1:4 carries out reacting mixing obtained in mass ratio
Object, and it is configured to ethyl alcohol the mixed solution of 20wt%；
(2) in a nitrogen atmosphere by organic matter/copper complex obtained in step (1), heating rate is 5 DEG C/min,
800 DEG C are warming up to, high-temperature roasting 8h is carried out.Then cooled to room temperature to get arrive carbon coating copper micro-nano granules composite wood
Material.After copper in carbon coating copper complex is removed, the thickness of coated carbon-coating is in 50 rans.
In conclusion carbon coating copper micro-nano granules composite material of the invention is not only retained due to the cladding by carbon
The performances such as the spherical morphology of this Cu fine-grained particles and unique electromagnetism optics, and its better chemical stability is assigned,
Resistance to acid and alkali, biocompatibility and surface-functionalized various selective, but also fine-grained particles can be modified, therefore this
The carbon coating copper micro-nano granules composite material of invention in biosensor, electrically conductive ink, supercapacitor, fuel cell and is urged
Agent etc. will have potential application prospect.
The above is only the citing to embodiments of the present invention, it is noted that for the general skill of the art
For art personnel, under the premise of not departing from this technology principle, several improvement and modification can also be made, these improve and become
Type is regarded as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of carbon coating copper micro-nano granules composite material, which is characterized in that specific step is as follows:
(1) it firstly, in a solvent by spherical copper powder and surfactant, 40~80min of mixing is stirred at room temperature, is subsequently added into organic
Carbon source continues 1~2h of stirring, obtains mixed emulsion；Then, mixed emulsion is transferred to the container of polytetrafluoroethyllining lining
It is interior, it is placed in stainless steel cauldron, seals, carry out hydro-thermal process, control hydrothermal temperature is 50-200 DEG C, reaction time 12-
48h；After reaction, natural cooling is filtered, washing, and filter cake vacuum drying obtains organic matter/copper complex；Wherein:
The solvent is the mixture of deionized water or deionized water and dehydrated alcohol composition；
The spherical copper powder, surfactant, organic carbon source and solvent mass ratio be 1:(0.1-10): (0.2-10): (10-
100)；
(2) after roasting organic matter/copper complex obtained in step (1) under an inert atmosphere, cooled to room temperature is obtained
To carbon coating copper micro-nano granules composite material.
2. preparation method according to claim 1, which is characterized in that in step (1), spherical copper powder is 100~500 mesh.
3. preparation method according to claim 1, which is characterized in that in step (1), deionized water in solvent and anhydrous
The volume ratio of ethyl alcohol is 1:3~3:1.
4. preparation method according to claim 1, which is characterized in that in step (1), surfactant is selected from cetyl
One or more of trimethyl ammonium chloride, cetyl trimethylammonium bromide or polyvinylpyrrolidone.
5. preparation method according to claim 1, which is characterized in that in step (1), organic carbon source is phenolic resin.
6. preparation method according to claim 1 or 5, which is characterized in that in step (1), organic carbon source is phenol-formaldehyde
One of resin or resorcinol-formaldehyde resin or two kinds.
7. preparation method according to claim 1, which is characterized in that in step (1), hydrothermal temperature is 120-180 DEG C, instead
It is 20-30h between seasonable.
8. preparation method according to claim 1, which is characterized in that in step (1), vacuum drying temperature is 50~80
℃。
9. preparation method according to claim 1, which is characterized in that in step (2), calcination procedure is as follows: with 1-5 DEG C/
The heating rate of min is warming up to 600-1000 DEG C, reacts 6-20h.
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| CN109550941B (en) * | 2018-11-15 | 2020-05-26 | 中国科学院过程工程研究所 | Carbon nano tube coated titanium spherical composite powder and preparation method thereof |
| CN110039043B (en) * | 2019-03-15 | 2021-07-06 | 上海大学 | Three-dimensional copper @ carbon core-shell nanoparticle, and preparation method and application thereof |
| CN110480004B (en) * | 2019-08-29 | 2021-11-09 | 南京理工大学 | Method for preparing carbon-coated nano aluminum powder by hydrothermal method |
| CN114559033B (en) * | 2022-03-04 | 2023-03-10 | 厦门大学 | Carbon-coated copper nanoparticles and preparation method thereof |
| US11801553B1 (en) | 2022-11-29 | 2023-10-31 | King Faisal University | Method for making carbon-coated copper nanoparticles |
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