CN106082167A - The carbon nano tube compound material of porous carbon supporting base end portion coated metal granule and the preparation method of derivant, product and application - Google Patents
The carbon nano tube compound material of porous carbon supporting base end portion coated metal granule and the preparation method of derivant, product and application Download PDFInfo
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- CN106082167A CN106082167A CN201610410595.7A CN201610410595A CN106082167A CN 106082167 A CN106082167 A CN 106082167A CN 201610410595 A CN201610410595 A CN 201610410595A CN 106082167 A CN106082167 A CN 106082167A
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses carbon nano tube compound material and the preparation method of derivant, product and the application of a kind of porous carbon supporting base end portion coated metal granule, with metal complex as presoma, the method deposited by chemical gaseous phase, high temperature reduction obtains the porous carbon materials rich in metal nanoparticle, then with the porous carbon materials rich in metal nanoparticle as catalyst, introduce carbon-source gas, be deposited on metallic particles growth CNT by chemical gaseous phase and obtain the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule.Then composite acid further is dissolved and obtain its derivant.The present invention can be at CNT end preserving capital metal particles, aperture is adjustable, and the advantages such as the features such as the high-specific surface area of porous carbon materials and unique pore passage structure and the high-modulus of CNT, high intensity, special electrical properties and good heat transfer property are incorporated into one, and the two kinds of grading materials making us obtain are with a wide range of applications in electrochemical field.
Description
Technical field
The invention belongs to field of nanometer material technology, the CNT being specifically related to porous carbon supporting base end portion coated metal granule is multiple
Condensation material and derivant and preparation method thereof.
Background technology
Porous carbon materials is owing to having specific area, low cost, unique pore passage structure and excellent chemical stability
Etc. feature, it is widely used in the fields such as gas separating medium, electrode material for super capacitor and catalyst carrier at present.Mesh
Before mainly have following several for the method for synthesizing porous material with carbon element: high polymer carbonizatin method, biological material carbonizatin method, physics and
Chemical activation method, chemical vapour deposition technique etc..CNT takes SP due to wherein carbon atom2Hydridization, compares SP3Hydridization, SP2
In hydridization, S orbital composition is bigger, makes CNT have high-modulus and high intensity.And the P electricity of carbon atom on CNT
Son forms large-scale delocalized pi-bond, and owing to conjugation is notable, CNT has the electrical properties that some are special.It addition, carbon
Nanotube has higher thermal conductivity, if the CNT of the trace that adulterates in the composite, the thermal conductivity of this composite
The biggest improvement will be likely to be obtained.Adulterated by hetero atom (such as N, P, S, B etc.), material with carbon element performance in terms of electro-catalysis
Also can be greatly improved.
Metal complex itself has great surface area, regulatable aperture and topological structure, and can be by selecting
Prepared by different metal ions and organic ligand.Recently, metal complex is applied to pyrolysis system as a kind of good template
Standby porous carbon materials.The CNT degree of graphitization that additionally prepared by chemical gaseous phase depositing process is at a relatively high, and has good
Electric conductivity.
So the technical program is with metal complex as template, the method deposited by chemical gaseous phase is obtained porous carbon and supports
The carbon nano tube compound material of end coated metal granule and its derivative classification material with carbon element, the hierarchical composite material obtained because
Metallic particles is packaged in CNT end, and its aperture is adjustable, and the technical program is by the high-specific surface area of porous carbon materials, low
The features such as cost, unique pore passage structure and the high-modulus of CNT and high intensity, special electrical properties and good
The advantages such as heat transfer property are incorporated into one, make two kinds of grading materials that we obtain in catalysis, capacitor, sensor, energy storage etc.
Field is with a wide range of applications.
Summary of the invention
In view of this, an object of the present invention is to provide the CNT of porous carbon supporting base end portion coated metal granule
Composite and the preparation method of derivant, can be successfully in the growth carbon nanometer of porous carbon materials situ by this method
Manage and CNT end package metals catalyst granules in situ, and it can obtain porous carbon by simple acid corrosion
Material-CNT hierarchy derivant；The two of the purpose of the present invention are to provide porous carbon supporting base end portion coated metal granule
Carbon nano tube compound material and derivant product；The three of the purpose of the present invention are to provide described product in electrochemical field
Application.
For reaching above-mentioned purpose, the concrete technical scheme of the present invention is as follows:
1, the preparation method of the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule, including walking as follows
Rapid:
1) rich in the preparation of porous carbon materials of metal nanoparticle: with metal complex as presoma, chemistry gas is used
The method deposited mutually, by metal complex presoma in reducing gas atmosphere, temperature is reduced under the conditions of being 500-950 DEG C,
Porous carbon materials rich in metal nanoparticle；
2) preparation of the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule: with rich in metal nano
The porous carbon materials of grain is raw material, and with it as catalyst, by raw material under carbon-source gas atmosphere, temperature is 500-
Carry out chemical gaseous phase deposition under the conditions of 950 DEG C, raw-material metal nanoparticle grows CNT, obtain porous carbon and prop up
The carbon nano tube compound material of support end coated metal granule.
Preferably, step 1) described metal complex is containing the one in metal Mn, Cu, La, Mo, Fe, Co, Ni, Cr
Or several coordination compound coordinated with organo units or metal-organic framework material.
Preferably, described organo units is glycerol or 1,3,5-1,3,5-Benzenetricarboxylic acids.
Preferably, in described organo units or carbon-source gas, doping N, P, S or B element form the carbon material of miscellaneous element doping
Material.
Preferably, step 1) described reducing gas is H2, step 2) and described carbon-source gas is hydrocarbon gas.
The carbon nano tube compound material of the porous carbon supporting base end portion coated metal granule that 2, prepared by described preparation method.
3, the carbon nano tube compound material of described porous carbon supporting base end portion coated metal granule answering in electro-catalysis is reduced
With.
4, the preparation method of the carbon nano tube compound material derivant of porous carbon supporting base end portion coated metal granule, by described
Carbon nano tube compound material immersion corrosion in acid of porous carbon supporting base end portion coated metal granule falls metal therein, obtains many
The carbon nano tube compound material derivant of hole carbon supporting base end portion coated metal granule.
Preferably, described acid be concentration be the sulphuric acid of 1-5mol/L, hydrochloric acid, nitric acid.
The carbon nano tube compound material of the porous carbon supporting base end portion coated metal granule that 5, prepared by described preparation method derives
Thing.
6, the carbon nano tube compound material derivant of described porous carbon supporting base end portion coated metal granule is in lithium battery
Application.
The beneficial effects of the present invention is: the present invention with metal complex as presoma, the side deposited by chemical gaseous phase
Method, first by metal complex presoma high temperature reduction in reducing gas, makes the porous rich in metal nanoparticle
Material with carbon element；In porous carbon materials rich in metal nanoparticle as catalyst, be passed through special gas simultaneously, pass through chemical gaseous phase
The metallic site in-situ growing carbon nano tube being deposited in porous carbon；The end obtaining the growth of porous carbon materials situ is coated with
The composite structure of carbon nano tube of metal catalyst particles；The composite being previously obtained is soaked in diluted acid and makes metal therein
Particle erosion is fallen, and then obtains growing in porous carbon the classification material with carbon element of CNT.The porous carbon synthesized by the method is propped up
Support CNT, can be at CNT end preserving capital metal particles, and aperture is adjustable, and by the high-ratio surface of porous carbon materials
The features such as long-pending and unique pore passage structure and the high-modulus of CNT, high intensity, special electrical properties and good biography
The advantages such as hot property are incorporated into one, and the two kinds of grading materials making us obtain are led in catalysis, capacitor, sensor, energy storage etc.
Territory is with a wide range of applications.
Accompanying drawing explanation
In order to make the purpose of the present invention, technical scheme and beneficial effect clearer, the present invention provides drawings described below:
In Fig. 1, a represents the scanning electron microscope (SEM) photograph implementing the 1 cobalt-glycerol complex precursors material obtained, and b represents by changing
The scanning electron microscope (SEM) photograph of the composite of metal simple-substance is contained after learning vapour deposition；
Fig. 2 represents the composite and the hydrogen reduction performance comparison figure of commercialization platinum that embodiment 1 obtains；
In Fig. 3, a represents the scanning electron microscope of the nickel-1,3,5-1,3,5-Benzenetricarboxylic acid complex precursors material that embodiment 2 obtains
Figure.B represent deposited by chemical gaseous phase after the scanning electron microscope (SEM) photograph of composite containing metal simple-substance, c represents and corroded metal
The scanning electron microscope (SEM) photograph of the derivant obtained after simple substance；
Fig. 4 represents that derivant carries sulfur as the lithium-sulfur cell negative material charge-discharge cycle when the electric current density of 0.5C
Can figure.
Detailed description of the invention
Below the preferred embodiments of the present invention are described in detail.The experiment side of unreceipted actual conditions in embodiment
Method, generally according to normal condition or according to the condition proposed by manufacturer.
Embodiment 1
The CNT end of the nitrogen-doping of porous carbon materials situ growth is packaged with answering of metal simple-substance granule
The preparation method of condensation material, comprises the following steps:
1) by 0.22g Co (NO3)2·6H2O and 4mL glycerol is dissolved in 40mL aqueous isopropanol simultaneously, continuous stirring simultaneously
2h is to obtain the solution of clarification；
2) solution obtained is moved into 180 DEG C of reaction 6h in 100mL politef reactor, be naturally cooling to room subsequently
Temperature.It is centrifuged repeatedly the product washing above-mentioned gained with ethanol, obtains pink powder at 60 DEG C of vacuum drying 6h；
3) by 2) in the pink powder that obtains as chemical gaseous phase deposition tube furnace in the middle of, be warming up under argon shield
Be passed through hydrogen gas (Ar:hydrogen=5:1) after 650 DEG C and keep 5 minutes making 2) in the metal organic frame material that obtains
Material reduction thoroughly, is passed through ethylene (350sccm) the most simultaneously and ammonia (100sccm) keeps 10 minutes simultaneously, with life in situ
Long CNT.It is naturally cooling to room temperature subsequently and obtains the black powder of composite；
Fig. 1 a is the surface sweeping Electronic Speculum figure of the Co-glycerate presoma that embodiment 1 prepares, and from figure, we are permissible
Observe that the Co-glycerate presoma that we synthesize is the diameter regular spheroid at about 300nm；Porous carbon in Fig. 1 b
The CNT end of material situ growth is packaged with the scanning electron microscope (SEM) photograph of the composite of metal simple-substance granule, can be bright in figure
Aobvious sees that metal simple-substance granule part has been pushed up one end of CNT.
The black powder prepared can be used for electrocatalytic oxidation reduction.Method particularly includes: 1) take 2mg composite powder
It is distributed in the mixed liquor of 1mL water and ethanol (1:1), and adds the Nafion solution of 20 μ L 5%, continuous ultrasound 10 subsequently
Minute, obtain dispersion liquid；2) disc electrode is gone back with the aluminium powder polishing rotation of particle diameter 0.3 μm and 0.05 μm respectively smooth, the most smooth, and
Rinse well with deionized water, dry standby；3) take 5 μ L step (1) gained dispersant liquid drops and rotate counter offer electrode centers, naturally dry
Dry, prepare hydrogen reduction test electrode.
Fig. 2 is the hydrogen reduction performance comparison figure with commercialization platinum of the composite that embodiment 1 obtains, as shown in FIG.,
The composite material exhibits that we obtain has gone out half spike potential of 26mV higher than commercialization platinum, and carrying current and commercialization platinum phase
Seemingly.Illustrate that the composite of gained exists the biggest potentiality in terms of electro-catalysis.
Embodiment 2
The preparation method of the CNT growing miscellaneous element doping of porous carbon materials situ, comprises the following steps:
1) by 0.372g Ni (NO3)2·6H2O and 0.182g 1,3,5-1,3,5-Benzenetricarboxylic acid is dissolved in 30mL dehydrated alcohol simultaneously
In, continuous stirring 2h simultaneously；
2) light green solution obtained is moved into 180 DEG C of reaction 12h in 50mL politef reactor, be naturally cooling to
Room temperature；
3) it is centrifuged repeatedly with ethanol and washs the product of above-mentioned gained, obtain shallow green powder at 60 DEG C of vacuum drying 6h；
4) by 3) in the shallow green powder that obtains as chemical gaseous phase deposition tube furnace in the middle of, be warming up under argon shield
Be passed through hydrogen gas (Ar:hydrogen=5:1) after 650 DEG C and keep 5 minutes making 3) in the metal organic frame material that obtains
Material reduction thoroughly, is passed through ethylene (350sccm) the most simultaneously and ammonia (100sccm) keeps 10 minutes simultaneously, with life in situ
Long CNT.It is naturally cooling to room temperature subsequently and obtains black powder；
5) by 4) in the powder sample that obtains at 2mol L-1Dilute hydrochloric acid in immersion corrosion 24h, obtain nitrogen-doping
The classifying porous material with carbon element of the growth CNT of porous carbon materials situ.
Fig. 3 a is the surface sweeping Electronic Speculum figure of the Ni-MOF presoma that embodiment 2 prepares, and we can observe that from figure
We Ni-MOF of synthesis is the diameter regular spheroid about 2 μm；Fig. 3 b deposits growth in situ carbon nanometer for chemical gaseous phase
Composite after pipe；Fig. 3 c grows CNT for the porous carbon materials situ after eroding nickel metal simple-substance further
Scanning electron microscope (SEM) photograph, from figure it may be seen that we obtained porous carbon materials situ grown CNT point
Level material with carbon element.
The classification material with carbon element prepared and sulfur simple substance are mixed with the ratio of 2:3 and grinds 30 minutes, subsequently at nitrogen
With 3 ° of min under gas shielded-1It is warming up to 155 DEG C keep 10 hours, using the C/S composite that obtains as lithium ion battery negative material
Material is tested for button cell.
Fig. 4 is the charge-discharge performance figure under the electric current density of 0.5C, we have seen that first circle discharge capacity from figure
For 1480mAh/g, and after having circulated 150 circles, there remains the discharge capacity of 825.51480mAh/g.This side is described
The classification material with carbon element that method obtains also has the biggest potentiality in terms of energy storage.
Finally illustrate, preferred embodiment above only in order to technical scheme to be described and unrestricted, although logical
Cross above preferred embodiment the present invention to be described in detail, it is to be understood by those skilled in the art that can be
In form and it is made various change, without departing from claims of the present invention limited range in details.
Claims (10)
1. the preparation method of the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule, it is characterised in that include
Following steps:
1) rich in the preparation of porous carbon materials of metal nanoparticle: with metal complex as presoma, chemical gaseous phase is used to sink
Long-pending method, by metal complex presoma in reducing gas atmosphere, temperature is reduced under the conditions of being 500-950 DEG C, must be rich in
The porous carbon materials of metal nanoparticle；
2) preparation of the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule: with rich in metal nanoparticle
Porous carbon materials is raw material, on raw material rich in metal nanoparticle as catalyst, by raw material at carbon-source gas atmosphere
Under enclosing, temperature carries out chemical gaseous phase deposition under the conditions of being 500-950 DEG C, and raw-material metal nanoparticle grows carbon nanometer
Pipe, obtains the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule.
The preparation side of the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule the most according to claim 1
Method, it is characterised in that step 1) described metal complex be containing the one in metal Mn, Cu, La, Mo, Fe, Co, Ni, Cr or
Several coordination compounds coordinated with organo units or metal-organic framework material.
The preparation side of the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule the most according to claim 2
Method, it is characterised in that doping N, P, S or B element form the carbon material of miscellaneous element doping in described organo units or carbon-source gas
Material.
The preparation side of the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule the most according to claim 1
Method, it is characterised in that step 1) described reducing gas is H2, step 2) and described carbon-source gas is hydrocarbon gas.
5. the carbon nanometer of the porous carbon supporting base end portion coated metal granule that prepared by preparation method described in any one of Claims 1 to 4
Pipe composite.
6. the carbon nano tube compound material of porous carbon supporting base end portion coated metal granule described in claim 5 is in electro-catalysis is reduced
Application.
7. the preparation method of the carbon nano tube compound material derivant of porous carbon supporting base end portion coated metal granule, its feature exists
In, carbon nano tube compound material immersion corrosion in acid of described porous carbon supporting base end portion coated metal granule is fallen gold therein
Belong to, obtain the carbon nano tube compound material derivant of porous carbon supporting base end portion coated metal granule.
The system of the carbon nano tube compound material derivant of porous carbon supporting base end portion coated metal granule the most according to claim 7
Preparation Method, it is characterised in that described acid be concentration be the sulphuric acid of 1-5mol/L, hydrochloric acid, nitric acid.
9. the CNT of the porous carbon supporting base end portion coated metal granule that prepared by preparation method described in claim 7 or 8 is combined
Material derived thing.
10. the carbon nano tube compound material derivant of porous carbon supporting base end portion coated metal granule described in claim 9 is at lithium sulfur
Application in battery.
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Cited By (13)
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|---|---|---|---|---|
| CN107946560A (en) * | 2017-11-10 | 2018-04-20 | 武汉理工大学 | Carbon confinement metal or metal oxide composite nanostructure material and its preparation method and application |
| CN108023084A (en) * | 2017-12-04 | 2018-05-11 | 广东工业大学 | A kind of silicon-carbon cathode material preparation method and lithium ion battery |
| CN108682821A (en) * | 2018-05-25 | 2018-10-19 | 江苏师范大学 | A kind of preparation method of lithium ion battery cobalt-based metal oxide composite electrode |
| KR20180133063A (en) * | 2017-06-05 | 2018-12-13 | 주식회사 엘지화학 | Catalytic site, positive electrode active material and lithium-sulfur battery comprising the same |
| CN109560294A (en) * | 2018-11-30 | 2019-04-02 | 深圳大学 | A kind of lithium oxygen battery positive electrode and preparation method thereof and lithium oxygen battery |
| CN109873158A (en) * | 2017-12-01 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of lithium-sulfur cell carbon material and its preparation and application |
| CN110190262A (en) * | 2019-06-14 | 2019-08-30 | 河北工业大学 | A kind of preparation method of lithium sulfur battery anode material |
| CN110787819A (en) * | 2019-08-19 | 2020-02-14 | 浙江工业大学 | Cobalt diselenide/nitrogen-doped carbon nano material composite electrode catalytic material and preparation method and application thereof |
| CN111864212A (en) * | 2020-08-31 | 2020-10-30 | 中航锂电技术研究院有限公司 | Composite carbon material, self-supporting current collector, preparation method and lithium-sulfur battery |
| CN113346040A (en) * | 2021-05-19 | 2021-09-03 | 北京化工大学 | Flexible integrated lithium-sulfur battery positive electrode material and preparation method thereof |
| CN115703633A (en) * | 2021-08-12 | 2023-02-17 | 西南大学 | Micron-sized embroidered spherical porous carbon material and preparation method and application thereof |
| CN115724420A (en) * | 2022-09-30 | 2023-03-03 | 重庆长安新能源汽车科技有限公司 | Bimetal doped porous carbon material, preparation method, application, coated positive electrode material and preparation method |
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| KR102183658B1 (en) * | 2017-06-05 | 2020-11-26 | 주식회사 엘지화학 | Catalytic site, positive electrode active material and lithium-sulfur battery comprising the same |
| KR20180133063A (en) * | 2017-06-05 | 2018-12-13 | 주식회사 엘지화학 | Catalytic site, positive electrode active material and lithium-sulfur battery comprising the same |
| CN107946560A (en) * | 2017-11-10 | 2018-04-20 | 武汉理工大学 | Carbon confinement metal or metal oxide composite nanostructure material and its preparation method and application |
| CN107946560B (en) * | 2017-11-10 | 2020-09-08 | 武汉理工大学 | Carbon-limited domain metal or metal oxide composite nano-structure material and preparation method and application thereof |
| CN109873158B (en) * | 2017-12-01 | 2021-07-09 | 中国科学院大连化学物理研究所 | Carbon material for lithium-sulfur battery and preparation and application thereof |
| CN109873158A (en) * | 2017-12-01 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of lithium-sulfur cell carbon material and its preparation and application |
| CN108023084B (en) * | 2017-12-04 | 2020-05-19 | 广东工业大学 | Preparation method of silicon-carbon negative electrode material and lithium ion battery |
| CN108023084A (en) * | 2017-12-04 | 2018-05-11 | 广东工业大学 | A kind of silicon-carbon cathode material preparation method and lithium ion battery |
| CN108682821A (en) * | 2018-05-25 | 2018-10-19 | 江苏师范大学 | A kind of preparation method of lithium ion battery cobalt-based metal oxide composite electrode |
| CN109560294A (en) * | 2018-11-30 | 2019-04-02 | 深圳大学 | A kind of lithium oxygen battery positive electrode and preparation method thereof and lithium oxygen battery |
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