CN109494368A - A kind of preparation method and applications of carbonaceous nanocomposite - Google Patents
A kind of preparation method and applications of carbonaceous nanocomposite Download PDFInfo
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- CN109494368A CN109494368A CN201811470997.1A CN201811470997A CN109494368A CN 109494368 A CN109494368 A CN 109494368A CN 201811470997 A CN201811470997 A CN 201811470997A CN 109494368 A CN109494368 A CN 109494368A
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- carbonaceous
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation method and applications of carbonaceous nanocomposite, are related to Carbon Materials.A kind of preparation method of carbonaceous nanocomposite, step are as follows: the compound of boron-containing compound and metallic antimony is dissolved separately in the mixed solution of deionized water and dehydrated alcohol, high molecular material is added, is warming up to 80~100 DEG C, 0.5~2h of constant temperature, cooling obtained gel state substance;It is freeze-dried 10~48h, xerogel is made;It is placed in tube furnace, vacuumizes, inert gas is passed through with the speed of 100~300ml/min; after vacuumizing repeatedly, being passed through inertia protection destiny time; 600~1200 DEG C, 2~5h of constant temperature are warming up to 5~10 DEG C/min rate, is cooled to room temperature obtained carbonaceous nanocomposite.Preparation process of the present invention is simple, and cost of material is low, and non-environmental-pollution in preparation process, structure is controllable with performance, can get the carbonaceous nanocomposite of different storage sodium performances.
Description
Technical field
The present invention relates to Carbon Materials, and in particular to a kind of carbonaceous prepared based on hydro-thermal reaction and charring process is nano combined
The preparation method and applications of material.
Background technique
Conventional graphite material because to sodium ion deintercalation low efficiency, kinetic rate is slow, volume expansion is big, limit its
Direct application in sodium-ion battery leads to large capacity, high sodium diffusivity and good circulation performance anode material of lithium-ion battery
Serious scarcity.Since sodium ion size is bigger than lithium, most lithium ion battery negative materials are performed poor in sodium-ion battery,
There are Embedding efficiencies it is low, kinetic rate is slow and volume expansion is serious the problems such as, therefore, design and prepare novel sodium ion
Cell negative electrode material seems particularly critical.
In existing anode material of lithium-ion battery system (Carbon Materials, alloy material, metal oxide etc.), Carbon Materials are deposited
: at low cost, various structures, reversible capacity height, stable cycle performance, and have the advantages that characteristic is constructed in flexible space.Its
In, hard carbon has biggish carbon-coating spacing and unordered micropore, possesses more storage sodium sites, so that hard carbon is as storage sodium cathode
Material causes the very big concern of numerous researchers.
However storage sodium capacity, cycle performance and the high rate performance of hard carbon need to be improved, and are to research and develop one kind in the present invention
The carbonaceous nanocomposite of height storage sodium ability.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of carbonaceous nanocomposite.
It is a further object to provide the applications of carbonaceous nanocomposite.
Invention thinking of the invention is: utilizing hydro-thermal reaction and high temperature carbonization, preparation has high reversible capacity and multiplying power
The carbonaceous nanocomposite of performance, and it is used for the preparation of anode material of lithium-ion battery.
The present invention is achieved by the following technical solutions:
A kind of preparation method of carbonaceous nanocomposite, step are as follows:
1) it prepares gel state substance: the compound of boron-containing compound and metallic antimony is dissolved separately in deionized water and dehydrated alcohol
Mixed solution in, high molecular material is added, stirs evenly, is warming up to 80~100 DEG C, 0.5~2h of constant temperature, cooling obtained gel
State substance;
2) it prepares xerogel: by the dry 10~48h of gel state material freeze, xerogel is made;
3) it prepares carbonaceous nanocomposite: xerogel being placed in tube furnace, is vacuumized, with the speed of 100~300ml/min
It is passed through inert gas, after vacuumizing repeatedly, being passed through inertia protection destiny time, is warming up to 600~1200 with 5~10 DEG C/min rate
DEG C, 2~5h of constant temperature is cooled to room temperature obtained carbonaceous nanocomposite.
Further, the boron-containing compound is tetraphenylboron sodium, ammonium pentaborate or dimethylamino monoborane.
The compound of the metallic antimony is antimony acetate, antimony trichloride or antimony pentafluoride.
The volume ratio of the deionized water and dehydrated alcohol is 3~6:1.
The high molecular material is starch or cellulose.
The boron-containing compound: the compound of metallic antimony: the mass volume ratio of high molecular material is 12~26g:18g:
100mL。
The inert gas is high-purity argon gas or nitrogen.
Further, the present invention also provides the application of carbonaceous nanocomposite, the nano combined materials of the carbonaceous
Material may be used as anode material of lithium-ion battery.
The method that the present invention utilizes hydro-thermal reaction and high temperature carbonization, hetero atom boron element is introduced into hard carbon structure, as
The substitution position boron atom of electron acceptor enables to carbon structure to be easier to obtain electronics from sodium, enhances to alkali metal ion
Suction-operated, and broader carbon-coating spacing is produced, be conducive to more sodium ion absorption and quick deintercalation, and then improve
The energy density and multiplying power property of hard carbon cathode material, while will there is the antimony of high storage sodium capacity to be introduced into boron doped hard carbon material
Expect to form the carbonaceous nanocomposite for having high storage sodium ability, high reversible capacity and high rate performance, the composite wood in matrix
Material can be used as anode material of lithium-ion battery.
In order to verify the performance of carbonaceous nanocomposite, respectively to carbonaceous nanocomposite by scanning electron microscope, thoroughly
Radio mirror, x-ray photoelectron spectroscopy, X-ray diffraction spectrum, storage sodium performance are measured;Wherein Fig. 2 is carbonaceous nanocomposite
The microcosmic shape that carbonaceous nanocomposite obtained in the present invention is in jellyfish shape can be clearly seen in scanning electron microscopic picture from figure
Looks;Fig. 3 is carbonaceous nanocomposite transmission electron microscope picture, from transmission electron microscope photo shown in figure analysis shows carbonaceous nanometer
Composite material has the microstructure of jellyfish shape;Fig. 4 is carbonaceous nanocomposite x-ray photoelectron spectroscopy figure, can from figure
Contain carbon, boron, antimony, five kinds of oxygen, nitrogen elements in carbonaceous nanocomposite to obtain;Fig. 5 is carbonaceous nanocomposite X-ray
Diffraction spectrogram, by analyzing the object phase composition for preparing material in the present invention, it was demonstrated that in prepared material containing whether there is or not
Sizing carbon and metal simple-substance antimony;Fig. 6 is that carbonaceous nanocomposite stores up sodium performance, is as can be seen from the figure prepared in the present invention
Material has high specific capacity and excellent cyclical stability.
Compared with prior art, the invention has the following advantages:
(1) preparation process is simple, and cost of material is low, and without pre-processing to raw material, by hydro-thermal reaction and high temperature carbonization,
Carbonaceous anode material of lithium-ion battery can be obtained;
(2) non-environmental-pollution in preparation process, it is environmental friendly, exhaust gas, waste liquid, waste residue etc. are not generated;
(3) structure and performance are controllable, by the ratio of simple adjustment high molecular material and inert metal compound, can be obtained not
With the carbonaceous nanocomposite of storage sodium performance.
Detailed description of the invention
Fig. 1 is the flow chart of preparation method of the present invention.
Fig. 2 is the carbonaceous nanocomposite scanning electron microscopic picture prepared in the embodiment of the present invention 1.
Fig. 3 is the carbonaceous nanocomposite transmission electron microscope picture prepared in the embodiment of the present invention 1.
Fig. 4 is the carbonaceous nanocomposite x-ray photoelectron spectroscopy figure prepared in the embodiment of the present invention 1.
Fig. 5 is the carbonaceous nanocomposite X-ray diffraction spectrogram prepared in the embodiment of the present invention 1.
Fig. 6 is the carbonaceous nanocomposite storage sodium performance prepared in the embodiment of the present invention 1.
Specific embodiment
Clear, complete description is carried out to technical solution of the present invention below in conjunction with drawings and examples, it is clear that described
Embodiment be only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ability
Domain those of ordinary skill every other embodiment obtained without creative efforts, belongs to guarantor of the present invention
The range of shield.
Embodiment 1
5.300g tetraphenylboron sodium and 4.500g antimony acetate are dissolved separately in the mixed solution of 25ml deionized water and dehydrated alcohol
In (volume ratio 3:1), 13.500g starch is added, above-mentioned mixed solution is warming up to 80 DEG C after mixing evenly, constant temperature 0.5h
After be cooled into gel state substance;Xerogel is formd after freeze-dried 10h again;Xerogel after taking drying is placed in tubular type
In furnace, after vacuumizing, inert gas is passed through with the speed of 100 ml/min, after vacuumizing repeatedly, being passed through inertia protection destiny time,
600 DEG C are warming up to 5~10 DEG C/min rate, is cooled to room temperature after constant temperature 2h;Carbonaceous nanocomposite is finally obtained, and will
It is as active material for making sodium-ion battery cathode.
Embodiment 2
By 3.300g ammonium pentaborate, 2.000g dimethylamino monoborane and 4.500g antimony acetate are dissolved separately in 25ml deionized water
In the mixed solution (volume ratio 3:1) of dehydrated alcohol, 13.500g starch is added, it is after mixing evenly that above-mentioned mixing is molten
Liquid is warming up to 90 DEG C, and gel state substance has been cooled into after constant temperature 1.5h;It is freeze-dried again to form xerogel afterwards for 24 hours;It takes
Xerogel after drying is placed in tube furnace, after vacuumizing, is passed through inert gas with the speed of 150ml/min, vacuumize repeatedly,
After being passed through inertia protection destiny time, 900 DEG C are warming up to 5~10 DEG C/min rate, is cooled to room temperature after constant temperature 3.5h;Finally obtain
Carbonaceous nanocomposite is obtained, and as active material for making sodium-ion battery cathode.
Embodiment 3
5.300g dimethylamino monoborane and 2.000g antimony pentafluoride, 2.500g antimony acetate are dissolved separately in 25ml deionized water
In the mixed solution (volume ratio 4:1) of dehydrated alcohol, 13.500g cellulose is added, after mixing evenly by above-mentioned mixing
Solution is warming up to 100 DEG C, and gel state substance has been cooled into after constant temperature 2h;Xerogel is formd after freeze-dried 48h again;It takes
Xerogel after drying is placed in tube furnace, after vacuumizing, is passed through inert gas with the speed of 300ml/min, vacuumize repeatedly,
After being passed through inertia protection destiny time, is heated up 1200 DEG C with 5~10 DEG C/min rate, be cooled to room temperature after constant temperature 5h;Finally obtain
Carbonaceous nanocomposite, and as active material for making sodium-ion battery cathode.
Embodiment 4
4.800g dimethylamino monoborane and 4.500g antimony acetate are dissolved separately in the mixed of 25ml deionized water and dehydrated alcohol
It closes in solution (volume ratio 5:1), adds 12.500g starch, above-mentioned mixed solution is warming up to 100 DEG C after mixing evenly,
Gel state substance has been cooled into after constant temperature 1.5h;Xerogel is formd after freeze-dried 36h again;Xerogel after taking drying
It is placed in tube furnace, after vacuumizing, inert gas is passed through with the speed of 200 ml/min, vacuumize repeatedly, be passed through inertia protection
After destiny time, 1000 DEG C are warming up to 5~10 DEG C/min rate, is cooled to room temperature after constant temperature 4h;It is multiple finally to obtain carbonaceous nanometer
Condensation material, and as active material for making sodium-ion battery cathode.
Embodiment 5
The mixing that 4.300g ammonium pentaborate and 4.500g antimony trichloride are dissolved separately in 25ml deionized water and dehydrated alcohol is molten
In liquid (volume ratio 6:1), 4.500g starch, 7.000 celluloses are added, is after mixing evenly warming up to above-mentioned mixed solution
95 DEG C, gel state substance has been cooled into after constant temperature 0.5h;Xerogel is formd after freeze-dried 48h again;After taking drying
Xerogel is placed in tube furnace, after vacuumizing, is passed through inert gas with the speed of 300 ml/min, vacuumize repeatedly, be passed through it is lazy
Property protection destiny time after, be warming up to 1100 DEG C with 5~10 DEG C/min rate, be cooled to room temperature after constant temperature 3h;Finally obtain carbonaceous
Nanocomposite, and as active material for making sodium-ion battery cathode.
Embodiment 6
3.500g tetraphenylboron sodium and 4.500g antimony acetate are dissolved separately in the mixed solution of 25ml deionized water and dehydrated alcohol
In (volume ratio 3:1), 8.500g starch is added, above-mentioned mixed solution is warming up to 100 DEG C after mixing evenly, constant temperature 0.5h
After be cooled into gel state substance;Xerogel is formd after freeze-dried 48h again;Xerogel after taking drying is placed in tubular type
In furnace, after vacuumizing, inert gas is passed through with the speed of 100ml/min, after vacuumizing repeatedly, being passed through inertia protection destiny time,
800 DEG C are warming up to 5~10 DEG C/min rate, is cooled to room temperature after constant temperature 5h;Carbonaceous nanocomposite is finally obtained, and will
It is as active material for making sodium-ion battery cathode.
Embodiment 7
The mixing that 3.000g ammonium pentaborate and 4.500g antimony pentafluoride are dissolved separately in 25ml deionized water and dehydrated alcohol is molten
In liquid (volume ratio 5:1), 12.500g cellulose is added, above-mentioned mixed solution is warming up to 90 DEG C after mixing evenly, constant temperature
Gel state substance has been cooled into after 1.5h;Xerogel is formd after freeze-dried 36h again;Xerogel after taking drying is placed in
In tube furnace, after vacuumizing, inert gas is passed through with the speed of 200 ml/min, vacuumizes repeatedly, be passed through inertia protection destiny
After secondary, 1000 DEG C are warming up to 5~10 DEG C/min rate, is cooled to room temperature after constant temperature 2h;Finally obtain the nano combined material of carbonaceous
Material, and as active material for making sodium-ion battery cathode.
Embodiment 8
6.500g ammonium pentaborate and 4.500g antimony acetate are dissolved separately in the mixed solution of 25ml deionized water and dehydrated alcohol
In (volume ratio 3:1), 13.500g starch is added, above-mentioned mixed solution is warming up to 80 DEG C after mixing evenly, constant temperature 0.5h
After be cooled into gel state substance;Xerogel is formd after freeze-dried 48h again;Xerogel after taking drying is placed in tubular type
In furnace, after vacuumizing, inert gas is passed through with the speed of 300 ml/min, after vacuumizing repeatedly, being passed through inertia protection destiny time,
700 DEG C are warming up to 5~10 DEG C/min rate, is cooled to room temperature after constant temperature 3h;Carbonaceous nanocomposite is finally obtained, and will
It is as active material for making sodium-ion battery cathode.
Embodiment 9
The mixing that 6.000g ammonium pentaborate and 4.500g antimony trichloride are dissolved separately in 25ml deionized water and dehydrated alcohol is molten
In liquid (volume ratio 4:1), 12.500g cellulose is added, above-mentioned mixed solution is warming up to 90 DEG C after mixing evenly, constant temperature
Gel state substance has been cooled into after 1.5h;It is freeze-dried again to form xerogel afterwards for 24 hours;Xerogel after taking drying is placed in
In tube furnace, after vacuumizing, inert gas is passed through with the speed of 100ml/min, vacuumizes repeatedly, be passed through inertia protection destiny time
Afterwards, 900 DEG C are warming up to 5~10 DEG C/min rate, are cooled to room temperature after 2~5h of constant temperature;Finally obtain the nano combined material of carbonaceous
Material, and as active material for making sodium-ion battery cathode.
Embodiment 10
5.500g tetraphenylboron sodium and 4.500g antimony acetate are dissolved separately in the mixed solution of 25ml deionized water and dehydrated alcohol
In (volume ratio 6:1), 13.500g starch is added, above-mentioned mixed solution is warming up to 100 DEG C after mixing evenly, constant temperature
Gel state substance has been cooled into after 0.5h;Xerogel is formd after freeze-dried 48h again;Xerogel after taking drying is placed in
In tube furnace, after vacuumizing, inert gas is passed through with the speed of 300ml/min, vacuumizes repeatedly, be passed through inertia protection destiny time
Afterwards, 1200 DEG C are warming up to 5~10 DEG C/min rate, are cooled to room temperature after constant temperature 5h;Carbonaceous nanocomposite is finally obtained,
And as active material for making sodium-ion battery cathode.
The principles and effects of the invention, and the implementation that part uses only is illustrated in the above embodiments
Example, and is not intended to limit the present invention;It should be pointed out that for those of ordinary skill in the art, not departing from wound of the present invention
Under the premise of making design, various modifications and improvements can be made, and these are all within the scope of protection of the present invention.
Claims (8)
1. a kind of preparation method of carbonaceous nanocomposite, which is characterized in that step are as follows:
1) it prepares gel state substance: the compound of boron-containing compound and metallic antimony is dissolved separately in deionized water and dehydrated alcohol
Mixed solution in, high molecular material is added, stirs evenly, is warming up to 80~100 DEG C, 0.5~2h of constant temperature, cooling obtained gel
State substance;
2) it prepares xerogel: by the dry 10~48h of gel state material freeze, xerogel is made;
3) it prepares carbonaceous nanocomposite: xerogel being placed in tube furnace, is vacuumized, with the speed of 100~300ml/min
It is passed through inert gas, after vacuumizing repeatedly, being passed through inertia protection destiny time, is warming up to 600~1200 with 5~10 DEG C/min rate
DEG C, 2~5h of constant temperature is cooled to room temperature obtained carbonaceous nanocomposite.
2. a kind of preparation method of carbonaceous nanocomposite according to claim 1, which is characterized in that the boracic
Compound is any one or several mixtures of tetraphenylboron sodium, ammonium pentaborate, dimethylamino monoborane.
3. a kind of preparation method of carbonaceous nanocomposite according to claim 1 or 2, which is characterized in that described
The compound of metallic antimony is any one or several mixtures of antimony acetate, antimony trichloride, antimony pentafluoride.
4. a kind of preparation method of carbonaceous nanocomposite according to claim 1 or 2, which is characterized in that described
Deionized water and the volume ratio of dehydrated alcohol are 3~6:1.
5. a kind of preparation method of carbonaceous nanocomposite according to claim 1 or 2, which is characterized in that described
High molecular material is the mixture of starch, cellulose or the two.
6. a kind of preparation method of carbonaceous nanocomposite according to claim 1 or 2, which is characterized in that described
Boron-containing compound: the compound of metallic antimony: the mass volume ratio of high molecular material is 12~26g:18g:100mL.
7. a kind of preparation method of carbonaceous nanocomposite according to claim 1 or 2, which is characterized in that described
Inert gas is high-purity argon gas or nitrogen.
8. the application of carbonaceous nanocomposite described in claim 1, which is characterized in that the carbonaceous nanocomposite
As anode material of lithium-ion battery.
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