CN108584907A - A kind of hard carbon material and its preparation method and application - Google Patents
A kind of hard carbon material and its preparation method and application Download PDFInfo
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- CN108584907A CN108584907A CN201810602259.1A CN201810602259A CN108584907A CN 108584907 A CN108584907 A CN 108584907A CN 201810602259 A CN201810602259 A CN 201810602259A CN 108584907 A CN108584907 A CN 108584907A
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- hard carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 belongs to Material Fields more particularly to a kind of hard carbon material and its preparation method and application.The present invention provides a kind of preparation methods of hard carbon material, include the following steps:Citric acid is placed in protective atmosphere, pyrolytic reaction is carried out, obtains the hard carbon material.The present invention directly carries out a step pyrolytic reaction using citric acid under protective atmosphere; unique laminated structure and the hard carbon material containing a large amount of micropores, central hole structure is prepared, there is good chemical property using the hard carbon material as negative electrode of lithium ion battery made from negative electrode active material.Preparation method simple possible of the present invention, need not pre-process citric acid, and citric acid is spontaneous in pyrolytic process to be polymerize, and can simplify technique to greatest extent, while greatly reducing the manufacturing cost of hard carbon material.Also, citric acid is distributed very wide, synthesis technology maturation in nature, and raw material sources are abundant and economical.
Description
Technical field
The invention belongs to Material Fields more particularly to a kind of hard carbon material and its preparation method and application.
Background technology
Hard carbon material belongs to difficult graphited amorphous carbon material, by graphite microcrystal disordering arrangement form.Different from stone
Ink material, Storage mechanism of the lithium ion in hard carbon material are included in insertion-abjection mechanism of graphite microcrystal interlayer and in hard carbons
The adsorption-desorption mechanism on material micropore and surface, the microstructure of hard carbon material to its capacity, cycle performance and high rate performance all
It has a major impact.The precursor sources for preparing hard carbon material are abundant, common are carbohydrate, aromatic compounds, lipoid substance
And high molecular polymer etc., hard carbon material can be obtained by carrying out heat treatment to these presomas.Application number
201110383924.0 patent document is disclosed coat simultaneously heat to the dispersion of resinae and plant hard carbon presoma
Solution, is prepared spherical hard carbon particle, which has good high rate performance as lithium ion battery negative material.Firmly
The surface topography and internal microstructure of carbon material can all directly affect its chemical property, hard compared to the spherical shape in above-mentioned patent
Carbon, sheet hard carbon have more surface-active sites and higher specific surface area, have higher capacity and high rate performance.Shen
Please numbers 201510563682.1 patent document disclose using pitch and melamine mixture as presoma, by pitch and
Melamine is uniformly dispersed in heating reaction kettle high speed, is crushed after cooling, then calcines, sieved through ball milling in an inert atmosphere
And except the rich nitrogen type porous flake carbon material for preparing soft hard carbon combination after magnetic, but this method is pre- to hard carbon presoma
The process is more complicated for processing.
Invention content
In view of this, the present invention provides a kind of hard carbon material and its preparation method and application, for solving existing sheet
The complex problem of the preparation method of hard carbon.
The specific technical solution of the present invention is as follows:
A kind of preparation method of hard carbon material, includes the following steps:
Citric acid is placed in protective atmosphere, pyrolytic reaction is carried out, obtains the hard carbon material.
Preferably, the citric acid includes anhydrous citric acid and/or Citric Acid Mono.
Preferably, the pyrolytic reaction specifically includes:
1h~5h is kept the temperature at 800 DEG C~1300 DEG C, is cooled to 23 DEG C ± 2 DEG C.
Preferably, described before heat preservation 1h~5h, to further include at 800 DEG C~1300 DEG C:
It is warming up to 800 DEG C~1300 DEG C with 2 DEG C/min~5 DEG C/min.
Preferably, the protective atmosphere includes nitrogen and/or inert gas.
Preferably, the protective atmosphere further includes hydrogen;
Volume ratio of the hydrogen in the protective atmosphere is 1%~10%.
The present invention also provides hard carbon materials made from preparation method described in above-mentioned technical proposal.
The present invention also provides application of the hard carbon material described in above-mentioned technical proposal in the electrode of manufacture battery.
Preferably, the electrode is cathode or combination electrode.
The present invention also provides application of the hard carbon material described in above-mentioned technical proposal in manufacturing capacitor.
In conclusion the present invention provides the present invention provides a kind of preparation method of hard carbon material, include the following steps:
Citric acid is placed in protective atmosphere, pyrolytic reaction is carried out, obtains the hard carbon material.The present invention is directly being protected using citric acid
Shield atmosphere under carry out a step pyrolytic reaction, be prepared unique laminated structure and containing a large amount of micropores, central hole structure it is hard
Carbon material has good chemical property using the hard carbon material as negative electrode of lithium ion battery made from negative electrode active material.
Preparation method simple possible of the present invention, need not pre-process citric acid, and citric acid spontaneous generation in pyrolytic process is poly-
It closes, technique can be simplified to greatest extent, while greatly reducing the manufacturing cost of hard carbon material.Also, citric acid is in nature
Middle distribution is very wide, and synthesis technology is ripe, and raw material sources are abundant and economical.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described.
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the hard carbon material in the embodiment of the present invention;
Fig. 2 is scanning electron microscope (SEM) figure (bar=1 μm) of the hard carbon material in the embodiment of the present invention;
Fig. 3 is scanning electron microscope (SEM) figure (bar=5 μm) of the hard carbon material in the embodiment of the present invention;
Fig. 4 is Raman spectrum (Raman) figure of the hard carbon material in the embodiment of the present invention;
Fig. 5 is using the hard carbon material in the embodiment of the present invention as the first circle of lithium ion battery made from negative electrode active material
(1st) and the second circle (2nd) charge and discharge electrograph;
Fig. 6 is to be existed using the hard carbon material in the embodiment of the present invention as lithium ion battery made from negative electrode active material
The Capacity Plan of 2000 circle of cycle under 200mA/g current densities;
Fig. 7 is using the hard carbon material in the embodiment of the present invention as the multiplying power of lithium ion battery made from negative electrode active material
Charge and discharge cycles figure, current density are 50mA/g~1000mA/g.
Specific implementation mode
The present invention provides a kind of hard carbon material and its preparation method and application, the preparation for solving existing sheet hard carbon
The complex problem of method.
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects
It encloses.
A kind of preparation method of hard carbon material, includes the following steps:
Citric acid is placed in protective atmosphere, pyrolytic reaction is carried out, obtains hard carbon material.
The linear compounds that polymolecular linear condensation forms higher molecular weight can occur after heated for citric acid, or occur to divide
Dehydration is cyclic in sub, and the polymer that polymerization forms higher molecular weight occurs between ring molecule.During pyrolytic reaction, citric acid
Fusing, dehydration, polymerization occurs, final pyrolysis becomes the hard carbon material with two-dimensional structure.
The present invention directly carries out a step pyrolytic reaction using citric acid under protective atmosphere, and unique sheet knot is prepared
Structure and containing a large amount of micropores, central hole structure hard carbon material, using the hard carbon material as lithium made from negative electrode active material from
Sub- battery cathode has good chemical property.Preparation method simple possible of the present invention need not locate citric acid in advance
Reason, citric acid is spontaneous in pyrolytic process to be polymerize, and can simplify technique to greatest extent, while greatly reducing hard carbon material
Manufacturing cost.Also, citric acid is distributed very wide, synthesis technology maturation in nature, and raw material sources are abundant and economical.
In the present invention, citric acid and/or Citric Acid Mono.
In the present invention, pyrolytic reaction specifically includes:
1h~5h is kept the temperature at 800 DEG C~1300 DEG C, is cooled to 23 DEG C ± 2 DEG C.
Further, before keeping the temperature 1h~5h at 800 DEG C~1300 DEG C, further include:
It is warming up to 800 DEG C~1300 DEG C with 2 DEG C/min~5 DEG C/min.
In the present invention, protective atmosphere includes nitrogen and/or inert gas.
Further, protective atmosphere further includes hydrogen;
Volume ratio of the hydrogen in protective atmosphere is 1%~10%.
The present invention also provides hard carbon materials made from above-mentioned technical proposal preparation method.
The specific surface area of hard carbon material of the present invention is 1000m2/ g or more.Hard carbon material is two-dimensional sheet structure, hard carbon piece
Between width range is 1 μm~100 μm, thickness is less than 100nm, and certain curvature is presented in hard carbon piece.
The present invention also provides application of the above-mentioned technical proposal hard carbon material in the electrode of manufacture battery.
In the present invention, electrode is cathode or combination electrode.
Battery is preferably secondary cell and/or heavy-duty battery, and secondary cell is preferably lithium ion battery or sodium ion electricity
Pond.
The present invention also provides application of the above-mentioned technical proposal hard carbon material in manufacturing capacitor.
Capacitor is preferably ultracapacitor.
Lithium ion battery is because having many advantages, such as that energy density is high, operating voltage is high, cycle performance and high rate performance are excellent, quilt
It is widely used in the fields such as consumable electronic product, new-energy automobile and extensive energy storage.Negative material is as lithium-ion electric
Indispensable part in the device of pond, largely influences and limits the performance of battery.In view of material cost and stabilization
Property, most of commercial Li-ion battery use natural graphite or modified graphite as negative material, and theoretical specific capacity reaches
372mAh/g.The layer structure of graphite allows lithium ion embedded and abjection, but lithium ion can only by graphite crystal boundary diffusion,
Ion transmission path is long, and diffusion rate is small, limits the high rate performance of battery;In addition, the phase of this layer structure and electrolyte
Capacitive is poor, and the total insertion of solvent also be easy to cause graphite and occurs leafing, peeling and structure collapses etc. in charge and discharge process, leads
Cycle performance of battery is caused drastically to decline.
Contain a large amount of micropores and central hole structure inside hard carbon material of the present invention, there is bigger compared to spherical particle hard carbon
The regulation and control to hard carbon piece interlamellar spacing may be implemented in specific surface area, the temperature by adjusting pyrolytic reaction, are lithium ion, sodium ion storage
It deposits and more active sites is provided, improve diffusion rate of the ion in electrode material, to improve the specific capacity, forthright again of battery
The chemical properties such as energy, cycle performance.
Sheet hard carbon material interlamellar spacing 0.4nm or more provided by the present invention, compared to the stone that interlamellar spacing only has 0.335nm
Ink material is more advantageous to Na+On the one hand the deintercalation of graphite microcrystal interlayer can store more Na+To improve the specific volume of material
On the other hand amount, the rate charge-discharge stability for improving material prevent from caving in ion deinsertion process in which materials recurring structure, layer
Capacitance loss caused by separation or peeling.
For a further understanding of the present invention, with reference to specific embodiment, the present invention will be described in detail.
Embodiment 1
50g Citric Acid Monos are placed in tube furnace, carry out pyrolytic reaction under an argon atmosphere, pyrolytic reaction includes to rise
5 DEG C/min of warm rate is warming up to 900 DEG C, 2h is kept the temperature at 900 DEG C, cooled to room temperature, obtaining hard carbon material 1, (number is:
NCS-900C 2h)。
Embodiment 2
50g Citric Acid Monos are placed in tube furnace, carry out pyrolytic reaction under an argon atmosphere, pyrolytic reaction includes to rise
5 DEG C/min of warm rate is warming up to 1100 DEG C, 2h is kept the temperature at 1100 DEG C, cooled to room temperature, obtaining hard carbon material 2, (number is:
NCS-1100C 2h)。
Embodiment 3
50g Citric Acid Monos are placed in tube furnace, carry out pyrolytic reaction under an argon atmosphere, pyrolytic reaction includes to rise
5 DEG C/min of warm rate is warming up to 1300 DEG C, 2h is kept the temperature at 1300 DEG C, cooled to room temperature, obtaining hard carbon material 3, (number is:
NCS-1300C 2h)。
Embodiment 4
XRD tests are carried out to hard carbon material 1 to hard carbon material 3, as a result referring to Fig. 1, hard carbon material 1 is to hard carbon material 3
Significantly broadened diffraction maximum that there are two tools, and d002Interlamellar spacing is larger, and numerical value is more than 0.4nm, larger d002Interlamellar spacing is advantageous
In lithium ion or sodium ion insertion and abjection, illustrate hard carbon material of the present invention as lithium ion battery or sodium-ion battery cathode material
Higher charge-discharge magnification may be implemented in material.
Hard carbon material 1 is to the generally loose porous block structure of hard carbon material 3, and part is by a large amount of sclay texture groups
At.Its microscopic appearance is tested by scanning electron microscope (SEM) to hard carbon material 1, as a result please refers to Fig. 2 and Fig. 3, hard carbon material
Material 1 is two-dimensional sheet structure, and between hard carbon piece width range is 1 μm~100 μm, thickness is less than 100nm, and hard carbon piece presents certain
Curvature.
The hard carbon material 1 that embodiment 1 to embodiment 3 is prepared to hard carbon material 3 is amorphous carbon material (amorphous state),
Raman spectrum analysis is carried out to hard carbon material 1 to hard carbon material 3, as a result please refers to Fig. 3 and table 1.Hard carbon material 1 is to hard carbon material
3 D peak intensities are higher, the ratio (I at the peaks D and the peaks GD/IG) equally higher.
1 hard carbon material 1 of table to hard carbon material 3 physical property
Embodiment 5
The hard carbon material 1 prepared using the embodiment of the present invention 1 to embodiment 3 is pressed to hard carbon material 3 as negative electrode active material
According to negative electrode active material:Conductive black:Binder=8:1:1 mass ratio is mixed into negative material, using metal lithium sheet as pair
Electrode, electrolyte are 1mol/L LiPF6EC:DMC(1:1v/v), CR2032 button electricity is assembled in the glove box full of argon gas
Pond.The battery of assembling carries out charge-discharge test between 0.005V~3V, with the current density of 50-1000mA/g.
Referring to Fig. 5, for using the hard carbon material in the embodiment of the present invention as lithium-ion electric made from negative electrode active material
The first circle (1 in pondst) and the second circle (2nd) charge and discharge electrograph.Table 1 is please referred to, for using hard carbon material of the present invention as negative electrode active material
The charge and discharge data of lithium ion battery made from matter.The result shows that using hard carbon material 1 to hard carbon material 3 as negative electrode active material
Lithium ion battery made from matter has larger specific discharge capacity, and first circle coulombic efficiency is relatively low, absolutely proves hard carbon material 1 to hard
Carbon material 3 has the characteristic of bigger serface.In addition, using hard carbon material 1 to hard carbon material 3 as made from negative electrode active material
Lithium ion battery has different charging and discharging capacities, and first circle coulombic efficiency is different, can be realized to piece by adjusting holding temperature
Shape hard carbon material regulating microstructure is so as to improve material electrochemical performance.
Charge and discharge data of the table 2 using hard carbon material of the present invention as lithium ion battery made from negative electrode active material
Referring to Fig. 6, for using the hard carbon material in the embodiment of the present invention as lithium-ion electric made from negative electrode active material
Pond recycles the Capacity Plan of 2000 circles under 200mA/g current densities.The result shows that being made with the hard carbon material in the embodiment of the present invention
There is relatively stable long circulating stability for lithium ion battery made from negative electrode active material, specific capacity with cycle-index increase
The trend of reduction after first increasing is presented.In addition, using hard carbon material 1 to hard carbon material 3 as lithium made from negative electrode active material from
Sub- battery has different long circulating stabilities, can be realized to sheet hard carbon material regulating microstructure by adjusting holding temperature
So as to improve material electrochemical performance.
Referring to Fig. 7, for using the hard carbon material in the embodiment of the present invention as lithium-ion electric made from negative electrode active material
The rate charge-discharge cycle figure in pond, current density is 50mA/g~1000mA/g.Table 3 is please referred to, for hard carbon material of the present invention
Multiplying power and cycle performance data as lithium ion battery made from negative electrode active material.The result shows that with the embodiment of the present invention
In hard carbon material as lithium ion battery made from negative electrode active material have excellent rate charge-discharge performance, illustrate this hair
Bright sheet hard carbon material has excellent lithium ion quickly embedding de- ability as negative electrode of lithium ion battery.In addition, with hard carbon material 1
There is different rate charge-discharge performances as lithium ion battery made from negative electrode active material to hard carbon material 3, tune can be passed through
Holding temperature is saved to realize to sheet hard carbon material regulating microstructure so as to improve material electrochemical performance.
Multiplying power and cycle performance number of the table 3 using hard carbon material of the present invention as lithium ion battery made from negative electrode active material
According to
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of hard carbon material, which is characterized in that include the following steps:
Citric acid is placed in protective atmosphere, pyrolytic reaction is carried out, obtains the hard carbon material.
2. preparation method according to claim 1, which is characterized in that the citric acid includes anhydrous citric acid and/or one
Water citric acid.
3. preparation method according to claim 1, which is characterized in that the pyrolytic reaction specifically includes:
1h~5h is kept the temperature at 800 DEG C~1300 DEG C, is cooled to 23 DEG C ± 2 DEG C.
4. preparation method according to claim 3, which is characterized in that described to keep the temperature 1h~5h at 800 DEG C~1300 DEG C
Before, further include:
It is warming up to 800 DEG C~1300 DEG C with 2 DEG C/min~5 DEG C/min.
5. preparation method according to claim 1, which is characterized in that the protective atmosphere includes nitrogen and/or indifferent gas
Body.
6. preparation method according to claim 5, which is characterized in that the protective atmosphere further includes hydrogen;
Volume ratio of the hydrogen in the protective atmosphere is 1%~10%.
7. hard carbon material made from preparation method described in claim 1 to claim 6 any one.
8. application of the hard carbon material described in claim 7 in the electrode of manufacture battery.
9. application according to claim 7, which is characterized in that the electrode is cathode or combination electrode.
10. application of the hard carbon material described in claim 7 in manufacturing capacitor.
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CN110098407A (en) * | 2019-04-19 | 2019-08-06 | 上海大学 | Carbon-based storage sodium negative electrode material, its application and preparation method |
CN111211315A (en) * | 2020-02-26 | 2020-05-29 | 中国科学院山西煤炭化学研究所 | Asphalt substrate layer carbon material and preparation method and application thereof |
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