CN107275618A - A kind of preparation method of carbon-coated antimony porous material for ion battery negative pole - Google Patents
A kind of preparation method of carbon-coated antimony porous material for ion battery negative pole Download PDFInfo
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- CN107275618A CN107275618A CN201710541003.XA CN201710541003A CN107275618A CN 107275618 A CN107275618 A CN 107275618A CN 201710541003 A CN201710541003 A CN 201710541003A CN 107275618 A CN107275618 A CN 107275618A
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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
- H01M4/366—Composites as layered products
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
A kind of preparation method of carbon-coated antimony porous material for ion battery negative pole, belongs to the preparation method of carbon-coated antimony porous material.The preparation method of carbon-coated antimony porous material is regulated and controled technical parameter in course of reaction, prepares the structure of porous carbon-coated antimony, obtained carbon-coated antimony porous material using antimony source solution and carbon source stirring absorption, dispersed mixing, carburising step;Using carbon-coated antimony porous material as ion battery cathode material, electrode slice is fabricated to;Specifically:Antimony source involvement solvent is added slowly in carbon source make antimony source fully spread mixing by stirring and being continuously added dispersant, antimony source and carbon source ratio are about 1:10 to 1:1, and be carbonized 1 10 hours in an inert atmosphere, material requested is dried to obtain after cleaning.Advantage:Method is simple, and raw material is cheap and easy to get, and operating procedure controllability is high, by regulating and controlling the parameter in course of reaction, realizes cheap, large-scale production to carbon-coated antimony material, and by it using the negative material for doing ion battery.
Description
Technical field
It is particularly a kind of for ion battery negative pole the present invention relates to a kind of preparation method of carbon-coated antimony porous material
The preparation method of carbon-coated antimony porous material.
Background technology
As a member in carbon coating field, porous carbon-coated antimony nano material because its have dimensional effect, quantum effect,
The important characteristic such as skin effect, in catalysis, the field such as electrochemical energy storage has a wide range of applications.Due to the particle diameter and shape of material
Looks structure has a strong impact on for the physics of material, chemical property, therefore conjunction is controlled to material it is necessary to autotelic
Into to obtain desired premium properties.
Because exploration of the fast development to lithium ion battery of lithium ion battery never stops, but it is due to the scarcity of lithium source
Cause it unconfined can not provide stable support for new energy battery.
Lithium ion battery is replaced to be researcher using the close kalium ion battery of chemical property or sodium-ion battery
The target constantly pursued.It is several times as much as lithium ion yet with the ionic radius of potassium ion or sodium ion and is required during deintercalation
Space it is just bigger, and potassium ion or sodium ion be also always potassium the problem of volumetric expansion is violent during alloying from
The problem of can not ignore on sub- battery Commercial road.These shortcomings are all reflected in the unstable of kalium ion battery or sodium-ion battery
Cycle performance and the characteristics of low specific capacity on.The deintercalation space of potassium ion or sodium ion and carried based on this shortcoming in order to expand
On the premise of height ratio capacity, antimony, by extensive concern, but is due to that antimony exists as a kind of metal for expanding battery capacity that can stablize
Volumetric expansion is big during alloying influences its stability, and capability retention is low the problem of be also facing in industry.
The content of the invention
It is easy to get the invention aims to providing a kind of raw material, preparation method is simple, easily operated be used for ion battery
The preparation method of the carbon-coated antimony porous material of negative pole.
The object of the present invention is achieved like this:The preparation method of the carbon-coated antimony porous material of the present invention using antimony source and
Technical parameter in carbon source stirring absorption, dispersed mixing, carburising step, regulation and control course of reaction, prepares porous carbon coating
The structure of antimony, obtains carbon-coated antimony porous material;Using carbon-coated antimony porous material as ion battery cathode material, electricity is fabricated to
Pole piece.
The preparation method of carbon-coated antimony porous material, is comprised the following steps that:
(1) antimony source is added in the antimony source solvent of 1-10 mol/Ls and is made into antimony source solution;It is then slowly added to water suction
In property high molecular polymer carbon source, until all being absorbed by carbon source, mixed material is obtained;With after in vacuum freezing drying oven,
Dry 1-20 hours;
(2) freeze-dried rear product in step (1) is moved in tube-type atmosphere furnace, the 1-15 that is carbonized in ar gas environment is small
When, 300-1200 degrees Celsius of carburizing temperature, 1-10 degrees/min of programming rate;
(3) product after being carbonized in step (2) is cleaned up and separated with wash solution, be then put into vacuum refrigeration and do
In dry case, dry 1-15 hours, obtain carbon-coated antimony porous material.
Described antimony source is the compound of antimony, selected from stibnite (Sb2S3), antimony fluoride (SbF3), antimony chloride (SbCl3), bromine
Change antimony (SbBr3), antimony iodide (SbI3)。
Described carbon source is selected from the absorbent polymer polymer such as PMA, polyacrylic acid potassium, Sodium Polyacrylate
In one or more.
In the step (1), antimony source solvent is deionized water (H2O), acetone (CH3COCH3), absolute ethyl alcohol (C2H5OH in)
One or more.
In the step (1), carbon source quality:Antimony source quality=1:10-10:Between 1.
In the step (1), the preferred deionized water (H of antimony source solvent2) or absolute ethyl alcohol (C O2H5OH)。
In the step (1), the preferred stibnite (Sb in antimony source2S3), bromination antimony (SbBr3) or antimony chloride (SbCL3)。
In the step (1), the water imbibition high score such as the preferred PMA of carbon source, polyacrylic acid potassium, Sodium Polyacrylate
Sub- polymer.
In the step (2), carburizing temperature is preferably 450-800 degree;Time is 5-10 hours.
In the step (3), wash solution is the one or more in deionized water, alcohol, watery hydrochloric acid, and using centrifugation
Separation or the separation of Buchner funnel suction filtration.
The method of application that the carbon-coated antimony porous material is used for ion battery negative pole is:
(1) it is 70 by weight:20:10 ratio weighs carbon-coated antimony porous material, carbon black and Kynoar respectively
And mix, 1-METHYLPYRROLIDONE solution is then added into mixed material, is fully ground or stirred 1-10 hours, will
To pasty mixture be uniformly coated on copper foil, and under the conditions of 40-120 DEG C dry, afterwards to scribbling said mixture
Copper foil rolled, cut obtained electrode slice;
(2) in the environment full of argon gas, electrode slice, barrier film and sheet metal are assembled into button cell simultaneously in conventional manner
Carry out constant current charge-discharge capacity and cycle performance test;Described ion battery includes lithium ion battery, kalium ion battery and sodium
Ion battery.
Described sheet metal is lithium piece, sodium piece or potassium piece.
Beneficial effect:Raw materials used cheap and easy to get, synthetic method is simply easily operated, it is easy to large-scale industrial production.
Meanwhile, the porous carbon-coated antimony porous material is shown into excellent chemical property as ion battery cathode material, both
The low shortcoming of the traditional carbon negative pole material specific capacity of commercialization ion battery is overcome, but also with traditional antimony metal negative material
The excellent cycling stability not possessed, has directive function to exploitation novel ion battery electrode material.
Advantage:The synthetic technology for being mixed and being carbonized using stirring at normal temperature uniform pickup prepares a kind of with uniform carbon bag
Structural composite material is covered, method therefor is simple, and raw material is cheap and easy to get, and operating procedure controllability is high, by regulating and controlling in course of reaction
Parameter, realize cheap, large-scale production to carbon-coated antimony material, and the negative material of ion battery is done into its application, obtain
Good chemical property is arrived.
Brief description of the drawings:
Fig. 1 is the powder X-ray diffraction pattern figure of the porous carbon-coated antimony of the embodiment of the present invention 1.
Fig. 2 is the electron scanning micrograph of the porous carbon-coated antimony of the embodiment of the present invention 1.
Fig. 3 is that carbon-coated antimony porous material of the present invention is used for the charge and discharge cycles figure of kalium ion battery.
Fig. 4 is that carbon-coated antimony porous material of the present invention is used for the charge and discharge cycles figure of sodium-ion battery.
Fig. 5 is that carbon-coated antimony porous material of the present invention is used for the charge and discharge cycles figure of lithium ion battery.
Embodiment
The preparation method of the carbon-coated antimony porous material of the present invention absorbed using antimony source and carbon source stirring, dispersed mixed
Technical parameter in conjunction, carburising step, regulation and control course of reaction, prepares the structure of porous carbon-coated antimony, obtains carbon-coated antimony many
Porous materials;Using carbon-coated antimony porous material as ion battery cathode material, electrode slice is fabricated to.
The preparation method of carbon-coated antimony porous material, is comprised the following steps that:
(1) antimony source is added in the antimony source solvent of 1-10 mol/Ls and is made into antimony source solution;It is then slowly added to water suction
In property high molecular polymer carbon source, until all being absorbed by carbon source, mixed material is obtained;With after in vacuum freezing drying oven,
Dry 1-20 hours;
(2) freeze-dried rear product in step (1) is moved in tube-type atmosphere furnace, the 1-15 that is carbonized in ar gas environment is small
When, 300-1200 degrees Celsius of carburizing temperature, 1-10 degrees/min of programming rate;
(3) product after being carbonized in step (2) is cleaned up and separated with wash solution, be then put into vacuum refrigeration and do
In dry case, dry 1-15 hours, obtain carbon-coated antimony porous material.
Described antimony source is the compound of antimony, selected from stibnite (Sb2S3), antimony fluoride (SbF3), antimony chloride (SbCl3), bromine
Change antimony (SbBr3), antimony iodide (SbI3)。
Described carbon source is selected from the absorbent polymer polymer such as PMA, polyacrylic acid potassium, Sodium Polyacrylate
In one or more.
In the step (1), antimony source solvent is deionized water (H2O), acetone (CH3COCH3), absolute ethyl alcohol (C2H5OH in)
One or more.
In the step (1), carbon source quality:Antimony source quality=1:10-10:Between 1.
In the step (1), the preferred deionized water (H of antimony source solvent2) or absolute ethyl alcohol (C O2H5OH)。
In the step (1), the preferred stibnite (Sb in antimony source2S3), bromination antimony (SbBr3) or antimony chloride (SbCL3)。
In the step (1), it is high that carbon source preferably is selected from the water imbibitions such as PMA, polyacrylic acid potassium, Sodium Polyacrylate
One or more in Molecularly Imprinted Polymer.
In the step (2), carburizing temperature is preferably 450-800 degree;Time is 5-10 hours.
In the step (3), wash solution is the one or more in deionized water, alcohol, watery hydrochloric acid, and using centrifugation
Separation or the separation of Buchner funnel suction filtration.
The method of application that the carbon-coated antimony porous material is used for ion battery negative pole is:
(1) it is 70 by weight:20:10 ratio weighs carbon-coated antimony porous material, carbon black and Kynoar respectively
And mix, 1-METHYLPYRROLIDONE solution is then added into mixed material, is fully ground or stirred 1-10 hours, will
To pasty mixture be uniformly coated on copper foil, and under the conditions of 40-120 DEG C dry, afterwards to scribbling said mixture
Copper foil rolled, cut obtained electrode slice;
(2) in the environment full of argon gas, electrode slice, barrier film and sheet metal are assembled into button cell simultaneously in conventional manner
Carry out constant current charge-discharge capacity and cycle performance test;Described ion battery includes lithium ion battery, kalium ion battery and sodium
Ion battery.
Described sheet metal is lithium piece, sodium piece or potassium piece.
Embodiment 1:Taking 0.6g antimony source to be dissolved in stirring in 2ml absolute ethyl alcohol dissolves it, then slow thereto to add
Enter 1g high molecular polymer simultaneously with this stirring, solution is fully absorbed.And then it is slowly added to 8ml anhydrous second
Alcohol, ensures that absolute ethyl alcohol fully spreads during addition, obtains the composite 1. of white puff flakes while stirring
Composite 1 is put into freezing in vacuum freeze drier and obtains within 10 hours white powder composite 2. and then by composite 2 600
Degree, carbonization obtains black powder composite 3. for 10 hours composite 3 is cleaned for several times with deionized water and cloth is used in ar gas environment
Family name's funnel suction filtration obtains uniform black powder composite 4. composite 4 is placed in vacuum freeze drier to dry 10 hours
To black powder product.Product is through Bruker D8 ADVANCE x-ray powder diffraction instruments with Cu K alpha ray (wavelengthScanning leg speed is 0.08 °/sec) Sb (Fig. 1) is accredited as, match with JCPDS card standard values No.35-0517,
Occur without other impurities peak.
Fig. 1 is the powder X-ray diffraction pattern of porous carbon-coated antimony;Wherein left ordinate is relative intensity
(Intensity), abscissa is angle of diffraction (2 θ).
Using the pattern of the porous carbon-coated antimony nano particle of JSF-6700 scanning electron microscopic observations, as shown in Figure 2.
Electrochemical property test:It is 70 by weight:20:10 ratio weighs carbon-coated antimony, carbon black, polyvinylidene fluoride respectively
Alkene, then adds 1-METHYLPYRROLIDONE solution, is fully ground or stirs 2-3 hours, the mixture of pasty state is uniformly coated with
On copper foil, dried at 60 ± 20 DEG C, the copper foil for scribbling said mixture is rolled afterwards, obtained electrode slice is cut;
In the environment full of argon gas, electrode slice, barrier film and potassium piece are assembled into button cell in conventional manner and constant current charge and discharge is carried out
Capacitance and cycle performance test.Its chemical property is as shown in Figure 3.
Embodiment 2:Taking 0.6g antimony source to be dissolved in stirring in 2ml deionized water dissolves it, then slow thereto to add
Enter 1g high molecular polymer simultaneous stirring, solution is fully absorbed.And then it is slowly added to 8ml anhydrous second
Alcohol, ensures that absolute ethyl alcohol fully spreads during addition, obtains the composite 1. of white puff flakes while stirring
Composite 1 is put into freezing in vacuum freeze drier and obtains within 10 hours white powder composite 2. and then by composite 2 600
Degree, carbonization obtains black powder composite 3. for 10 hours composite 3 is cleaned for several times with deionized water and cloth is used in ar gas environment
Family name's funnel suction filtration obtains uniform black powder composite 4. composite 4 is placed in vacuum freeze drier to dry 10 hours
To black powder product.
Electrochemical property test:It is 70 by weight:20:10 ratio weighs carbon-coated antimony, carbon black, polyvinylidene fluoride respectively
Alkene, then adds 1-METHYLPYRROLIDONE solution, is fully ground or stirs 2-3 hours, the mixture of pasty state is uniformly coated with
On copper foil, dried at 60 ± 20 DEG C, the copper foil for scribbling said mixture is rolled afterwards, obtained electrode slice is cut;
In the environment full of argon gas, electrode slice, barrier film and sodium piece are assembled into button cell in conventional manner and constant current charge and discharge is carried out
Capacitance and cycle performance test.Its chemical property is as shown in Figure 4.
Embodiment 3:Taking 0.6g antimony source to be dissolved in stirring in 2ml absolute ethyl alcohol dissolves it, then slow thereto to add
Enter 1g high molecular polymer simultaneous stirring.And then 8ml absolute ethyl alcohol is slowly added to, ensures nothing while stirring
Water-ethanol fully spreads during addition, and obtaining the composite 1. of white puff flakes, that composite 1 is put into vacuum is cold
Freezing obtains white powder composite 2. for 10 hours and then by composite 2 at 800 degree in lyophilizer, is carbonized 10 in ar gas environment
Hour obtains black powder composite 3. and composite 3 is cleaned for several times with deionized water and is obtained uniformly with Buchner funnel suction filtration
Composite 4 is placed on drying in vacuum freeze drier and obtains black powder product in 10 hours by black powder finished product 4..
Electrochemical property test:It is 70 by weight:20:10 ratio weighs carbon-coated antimony, carbon black, polyvinylidene fluoride respectively
Alkene, then adds 1-METHYLPYRROLIDONE solution, is fully ground or stirs 2-3 hours, the mixture of pasty state is uniformly coated with
On copper foil, dried at 60 ± 20 DEG C, the copper foil for scribbling said mixture is rolled afterwards, obtained electrode slice is cut;
In the environment full of argon gas, electrode slice, barrier film and lithium piece are assembled into button cell in conventional manner and constant current charge and discharge is carried out
Capacitance and cycle performance test.Its chemical property is as shown in Figure 5.
Claims (8)
1. a kind of preparation method of carbon-coated antimony porous material for ion battery negative pole, it is characterized in that:Carbon-coated antimony is porous
The preparation method of material regulates and controls technology in course of reaction using antimony source and carbon source stirring absorption, dispersed mixing, carburising step
Parameter, prepares the structure of porous carbon-coated antimony, obtains carbon-coated antimony porous material;Using carbon-coated antimony porous material as from
Sub- cell negative electrode material, is fabricated to electrode slice.
2. a kind of preparation method of carbon-coated antimony porous material for ion battery negative pole according to claim 1, its
It is characterized in:The preparation method of carbon-coated antimony porous material, is comprised the following steps that:
(1)Antimony source solution is made into the antimony source solvent that antimony source is added to 1-10 mol/Ls;It is then slowly added to water imbibition high
In Molecularly Imprinted Polymer carbon source, until all being absorbed by carbon source, mixed material is obtained;With after in vacuum freezing drying oven, dry
1-20 hours;
(2)By step(1)In freeze-dried rear product move in tube-type atmosphere furnace, in ar gas environment be carbonized 1-15 hours,
300-1200 degrees Celsius of carburizing temperature, 1-10 degrees/min of programming rate;
(3)By step(2)Product after middle carbonization is cleaned up and separated with wash solution, is then put into vacuum freezing drying oven
In, dry 1-15 hours, obtain carbon-coated antimony porous material.
3. a kind of preparation method of carbon-coated antimony porous material for ion battery negative pole according to claim 1 or 2,
It is characterized in that:Described antimony source is the compound of antimony, selected from stibnite(Sb2S3), antimony fluoride(SbF3), antimony chloride(SbCl3)、
Bromination antimony(SbBr3), antimony iodide(SbI3).
4. a kind of preparation method of carbon-coated antimony porous material for ion battery negative pole according to claim 1 or 2,
It is characterized in that:Described carbon source is selected from the absorbent polymer polymer such as PMA, polyacrylic acid potassium, Sodium Polyacrylate
In one or more.
5. a kind of preparation method of carbon-coated antimony porous material for ion battery negative pole according to claim 2, its
It is characterized in:The step(1)In, antimony source solvent is deionized water(H2O), acetone(CH3COCH3), absolute ethyl alcohol(C2H5OH)In
One or more;
The step(1)In, carbon source quality:Antimony source quality=1:10-10:Between 1.
6. a kind of preparation method of carbon-coated antimony porous material for ion battery negative pole according to claim 2, its
It is characterized in:The step(3)In, wash solution is the one or more in deionized water, alcohol, watery hydrochloric acid, and using centrifugation
Separation or the separation of Buchner funnel suction filtration.
7. a kind of application process of carbon-coated antimony porous material for ion battery negative pole described in claim 1 or 2, it is special
Levying is:The method of application that the carbon-coated antimony porous material is used for ion battery negative pole is:
(1)It is 70 by weight:20:10 ratio weighs carbon-coated antimony porous material, carbon black and Kynoar and mixed respectively
Close, 1-METHYLPYRROLIDONE solution is then added into mixed material, is fully ground or stirred 1-10 hours, by what is obtained
Pasty mixture is uniformly coated on copper foil, and is dried under the conditions of 40-120 DEG C, afterwards to scribbling the copper of said mixture
Paper tinsel is rolled, and cuts obtained electrode slice;
(2)In the environment full of argon gas, electrode slice, barrier film and sheet metal are assembled into button cell in conventional manner and carried out
Constant current charge-discharge capacity and cycle performance test;Described ion battery includes lithium ion battery, kalium ion battery and sodium ion
Battery.
8. a kind of preparation method of carbon-coated antimony porous material for ion battery negative pole according to claim 7, its
It is characterized in:Described sheet metal is lithium piece, sodium piece or potassium piece.
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CN108390033A (en) * | 2018-02-08 | 2018-08-10 | 陕西科技大学 | A kind of preparation method and applications preparing anode material of lithium-ion battery carbon-coated antimony nano-tube material |
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