CN106058193A - Novel negative electrode material of sodium-ion battery as well as preparation method and application thereof - Google Patents
Novel negative electrode material of sodium-ion battery as well as preparation method and application thereof Download PDFInfo
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- CN106058193A CN106058193A CN201610575911.6A CN201610575911A CN106058193A CN 106058193 A CN106058193 A CN 106058193A CN 201610575911 A CN201610575911 A CN 201610575911A CN 106058193 A CN106058193 A CN 106058193A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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 the technical field of new energies and discloses a novel negative electrode material of a sodium-ion battery as well as a preparation method and an application of the novel negative electrode material. The preparation method comprises the following steps: dissolving a carbon source and a molybdenum source in a solvent, heating to ensure a reaction to obtain a precursor Mo3(BTC)2, implementing in-situ carbonization to obtain a composition of a carbonization-molybdenum nanoparticle and an ultrathin graphene shell. The specific structure of the negative electrode material is that the carbonization-molybdenum nanoparticle is coated by the ultrathin graphene shell, wherein the diameter of the carbonization-molybdenum nanoparticle is 1-10nm. In the electrochemical reaction process of the negative electrode material with sodium, the conversion reaction with a sodium ion achieves disembedding of the sodium ion, the reversible disembedding sodium capacity, the excellent sodium storage performance, higher reversible capacity and better cycle performance are achieved, the preparation method is simple, the cost is low, the preparation method is environmentally friendly and can be applied to the sodium-ion battery, and more possibilities for the exploration of the negative electrode material of the sodium-ion battery are provided.
Description
Technical field
The invention belongs to technical field of new energies, particularly to a kind of novel anode material of lithium-ion battery and preparation side thereof
Method and application.
Background technology
Energy problem of current various countries growing tension, and demand is still continuing increase, in the last few years, along with the progress of science and technology
And reform and innovation, electronic equipment, electric power tool, electric automobile etc. is also fast-developing, explores efficient, portable, the storage of safe green
Energy material becomes the certainty of development.Lithium ion battery is big due to energy density, through obtaining commercial applications widely, especially
At power vehicle, compact power, the aspect such as electronic equipment has played its advantage, but lithium resource is limited, expensive, and right
The demand of lithium is also being continuously increased, the relatively costly large-scale application limiting lithium ion battery.Therefore researchers start by
Sight has been moved to sodium-ion battery, for comparing lithium (0.006%), and sodium rich reserves, account for 2.64%, in terms of extensive energy storage
Tool has great advantage, and has boundless application prospect.
Metallic sodium and lithium belong to same main group, have similar physicochemical properties, therefore develop the sodium of excellent from
Sub-battery has bigger application prospect, thus explores the anode material of lithium-ion battery of the excellent properties such as high power capacity, stable circulation
Become the focus of current research field.But bigger sodium ion radius makes deintercalation sodium process slow, current commercialization should
Graphite cathode, sodium ion can not as at lithium ion the most embedding sodium, formed NaC64Capacity is the lowest.Alloy anode storage sodium
Capacity is higher, but there is the biggest bulk effect, and cycle performance is poor, therefore needs exist for finding one and has high power capacity, surely
Qualitative good, negative material that safety is good.
One carbonization one molybdenum (MoC) is as a kind of typical magnesium-yttrium-transition metal compound, and it is as cell negative electrode material the most not
Have relevant report, present invention applicant first by carbonization one molybdenum (MoC) materials application in anode material of lithium-ion battery, its
Reaction mechanism in the battery is similar to other magnesium-yttrium-transition metal compounds, by holding with the contribution of sodium ion generation conversion reaction
Amount.Conversion reaction is one of electrochemical energy storage form, other also include deintercalation reaction, alloying reaction.Conversion reaction and its
His two kinds of reaction mechanism differences, it is a kind of reversible redox reaction, and therefore a carbonization one molybdenum (MoC) is that a class has very much
The anode material of lithium-ion battery of potentiality.
Summary of the invention
In order to overcome the present Research of above-mentioned prior art anode material of lithium-ion battery, there is capacity low, cycle performance
The shortcoming of difference is with not enough, and the primary and foremost purpose of the present invention is to provide a kind of novel anode material of lithium-ion battery.
The negative material of the present invention is the complex (MoC@GS) of a carbonization one molybdenum nanoparticle and ultra-thin Graphene shell, its
In a molybdenum carbide (MoC) nanoparticle a diameter of 1～10nm.
Another object of the present invention is to provide the preparation method of a kind of above-mentioned novel anode material of lithium-ion battery.
Preparation method of the present invention uses two-step method to prepare negative material, first prepares presoma Mo3(BTC)2(a kind of
Metal-organic framework materials containing molybdenum, Mo-MOF), then carry out in-situ carburization and obtain negative material.
Still a further object of the present invention is the application providing above-mentioned novel anode material of lithium-ion battery in sodium-ion battery.
The purpose of the present invention is realized by following proposal:
A kind of novel anode material of lithium-ion battery, is the complex of a carbonization one molybdenum nanoparticle and ultra-thin Graphene shell
(MoC@GS), concrete structure is that ultra-thin Graphene shell is coated with a carbonization one molybdenum nanoparticle, wherein, carbonization one molybdenum (MoC) nanometer
A diameter of the 1～10nm of grain.
The present invention also provides for the preparation method of a kind of above-mentioned novel anode material of lithium-ion battery, comprises the following steps:
Carbon source and molybdenum source are dissolved in a solvent, reacting by heating, obtain presoma Mo3(BTC)2, then carry out in-situ carburization,
Obtain the complex (MoC@GS) of a carbonization one molybdenum nanoparticle and ultra-thin Graphene shell.
Wherein in an embodiment, described carbon source is trimesic acid (H3BTC), aniline (C6H7And terephthaldehyde N)
Acid (C8H6O4At least one in).
Wherein in an embodiment, described carbon source is trimesic acid (H3BTC)。
Wherein in an embodiment, described molybdenum source is hexacarbonylmolybdenum (Mo (CO)6), three carbonyl cycloheptatriene base molybdenums
(C11H14MoO3), ammonium molybdate (H8MoN2O4) and sodium molybdate (Na2MoO4At least one in).
Wherein in an embodiment, described molybdenum source is hexacarbonylmolybdenum (Mo (CO)6)。
Wherein in an embodiment, molybdenum source used and mol ratio 1:10 of carbon source～1:15.
Wherein in an embodiment, molybdenum source used and mol ratio 1:13.6 of carbon source.
Wherein in an embodiment, the temperature of described reacting by heating is 100～200 DEG C.
Wherein in an embodiment, the temperature of described reacting by heating is 150～160 DEG C.
Wherein in an embodiment, the temperature of described reacting by heating is 155 DEG C.
Wherein in an embodiment, the time of described reacting by heating is 3 days or more than 3 days.
Wherein in an embodiment, the time of described reacting by heating is 5 days or more than 5 days.
Wherein in an embodiment, the temperature of described carbonization is 500～1000 DEG C.
Wherein in an embodiment, the temperature of described carbonization is 700～900 DEG C.
Wherein in an embodiment, the time of described carbonization is 2～8h.
Wherein in an embodiment, the time of described carbonization is 5h.
Wherein in an embodiment, one or more in the organic solvent of esters of described solvent.
Wherein in an embodiment, described solvent is dimethyl fumarate (DMF).
Wherein in an embodiment, described solvent is the dimethyl fumarate (DMF) of deoxygenation.
The product obtained after described in-situ carburization, is dried to obtain the product of purification again after available solvent washing.Described wash
The solvent washed is preferably the dimethyl fumarate (DMF) of deoxygenation.Described dry temperature be 100 DEG C or more than, preferably 135 DEG C.
The present invention also provides for a kind of sodium-ion battery negative pole based on above-mentioned negative material, and this negative pole includes described novel sodium
Ion battery cathode material, binding agent and conductive agent；Described negative pole is by by described novel anode material of lithium-ion battery, bonding
Agent and conductive agent are mixed and made into slurry in a solvent, coat, be dried, obtain electrode.
Wherein in an embodiment, described binding agent is Kynoar (PVDF), polyacrylic acid (PAA), carboxylic first
At least one in base sodium cellulosate (CMC), sodium alginate (SA), butadiene-styrene rubber (SBR).
Wherein in an embodiment, described solvent is at least one in water and N-Methyl pyrrolidone (NMP).
Wherein in an embodiment, conductive agent used is at least one in white carbon black, Super-P, Ketjen black.
Wherein in an embodiment, described sodium-ion battery negative pole also includes other additives.
The present invention also provides for a kind of sodium-ion battery based on above-mentioned sodium-ion battery negative pole, including described sodium-ion battery
Negative pole, to electrode metal sodium, three parts of electrolyte system.
Wherein in an embodiment, described electrolyte system is organic solvent electrolyte or polyelectrolyte.
Wherein in an embodiment, described electrolyte system is organic solvent electrolyte.
Wherein in an embodiment, described electrolyte system is the organic solvent electrolyte of sodium salt.
Wherein in an embodiment, in described electrolyte system, the concentration of sodium salt is 1M.
Wherein in an embodiment, described sodium salt is NaPF6、NaClO4、NaBF4, in NaTf, NaFSI and NaTFSI
At least one, preferably NaPF6、NaClO4。
Wherein in an embodiment, described organic solvent is PC, EC, DMC, DME, DEC, THF and 2,2'-ethylenedioxybis(ethanol). diformazan
The mixed solvent of at least one in ether, preferably PC Yu EC.
Wherein in an embodiment, described electrolyte system is possibly together with additive.
The novel anode material of lithium-ion battery of the present invention can be applicable in sodium-ion battery.
The novel anode material of lithium-ion battery of the present invention, with the electrochemical reaction process of sodium, occurs to turn with sodium ion
Change reaction and realize the deintercalation of sodium ion, and electrochemical data shows that it has reversible deintercalation sodium capacity.And the negative pole of the present invention
Material has good storage sodium performance, has higher reversible capacity and preferable cycle performance, and preparation method is simple, low cost
Honest and clean, environmental friendliness, the exploration for later anode material of lithium-ion battery provides more possibility.
Accompanying drawing explanation
Fig. 1 is carbonization one molybdenum (MoC) nanoparticle complex (MoC@GS) with ultra-thin Graphene shell of embodiment 1
X-ray diffractogram.
Fig. 2 is carbonization one molybdenum (MoC) nanoparticle complex (MoC@GS) with ultra-thin Graphene shell of embodiment 1
Scanning electron microscope (SEM) photograph.
Fig. 3 is carbonization one molybdenum (MoC) nanoparticle complex (MoC@GS) with ultra-thin Graphene shell of embodiment 1
Transmission electron microscope picture.
Fig. 4 is carbonization one molybdenum (MoC) nanoparticle complex (MoC@GS) with ultra-thin Graphene shell of embodiment 1
Cyclic curve.
Fig. 5 is carbonization one molybdenum (MoC) nanoparticle complex (MoC@GS) with ultra-thin Graphene shell of embodiment 1
First charge-discharge curve.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention do not limit
In this.
In following embodiment, described reagent the most commercially obtains with material.
Embodiment 1
It is synthesized by two-step process complex (MoC@GS) the negative pole material of a carbonization one molybdenum nanoparticle and ultra-thin Graphene shell
Material.First presoma Mo is prepared3(BTC)2, then precursor product is carried out under argon gas atmosphere in quartz ampoule in-situ carburization,
To the complex (MoC@GS) of end product one carbonization one molybdenum nanoparticle Yu ultra-thin Graphene shell, nanoparticle a diameter of 1～
10nm。
Concrete operations are as follows:
The hexacarbonylmolybdenum of mol ratio 1:13.6, trimesic acid are dissolved in dimethyl fumarate, under an argon atmosphere
Back flow reaction more than 5 days at 155 DEG C, through filtering, washing, after drying, obtain presoma Mo3(BTC)2, then presoma is placed in stone
In English pipe, 700～900 DEG C of in-situ carburization 5h under argon gas atmosphere, are cooled to room temperature, utilize dimethyl fumarate washing, dried,
Obtain the complex (MoC@GS) of a carbonization one molybdenum nanoparticle and ultra-thin Graphene shell.
Embodiment 2
It is synthesized by two-step process complex (MoC@GS) the negative pole material of a carbonization one molybdenum nanoparticle and ultra-thin Graphene shell
Material.First presoma Mo is prepared3(BTC)2, then precursor product is carried out under argon gas atmosphere in quartz ampoule in-situ carburization,
To the complex (MoC@GS) of end product one carbonization one molybdenum nanoparticle Yu ultra-thin Graphene shell, nanoparticle a diameter of 1～
10nm。
Concrete operations are as follows:
The hexacarbonylmolybdenum of mol ratio 1:10, trimesic acid are dissolved in dimethyl fumarate, under an argon atmosphere 100
Back flow reaction more than 5 days at DEG C, through filtering, washing, after drying, obtain presoma Mo3(BTC)2, then presoma is placed in quartz
In pipe, 500～1000 DEG C of in-situ carburization 2h under argon gas atmosphere, are cooled to room temperature, utilize dimethyl fumarate washing, dried,
Complex (MoC@GS) to a carbonization one molybdenum nanoparticle Yu ultra-thin Graphene shell.
Embodiment 3
It is synthesized by two-step process complex (MoC@GS) the negative pole material of a carbonization one molybdenum nanoparticle and ultra-thin Graphene shell
Material.First presoma Mo is prepared3(BTC)2, then precursor product is carried out under argon gas atmosphere in quartz ampoule in-situ carburization,
To the complex (MoC@GS) of end product one carbonization one molybdenum nanoparticle Yu ultra-thin Graphene shell, nanoparticle a diameter of 1～
10nm。
Concrete operations are as follows:
The hexacarbonylmolybdenum of mol ratio 1:15, trimesic acid are dissolved in dimethyl fumarate, under an argon atmosphere 200
Back flow reaction more than 3 days at DEG C, through filtering, washing, after drying, obtain presoma Mo3(BTC)2, then presoma is placed in quartz
In pipe, 500～1000 DEG C of in-situ carburization 8h under argon gas atmosphere, are cooled to room temperature, utilize dimethyl fumarate washing, dried,
Complex (MoC@GS) to a carbonization one molybdenum nanoparticle Yu ultra-thin Graphene shell.
Embodiment 4: performance characterization
According to the preparation method of conventional sodium-ion battery, carbonization one molybdenum nanoparticle embodiment 1 prepared is with super
The complex (MoC@GS) of thin Graphene shell and metallic sodium are assembled into sodium-ion battery, when electric current density is 500mA/g, its
Discharge capacity is 288.1mAh/g first.
Structural characterization, XRD test result such as Fig. 1 is carried out by X-ray diffraction analysis instrument (Bruker D8, Cu K alpha ray)
Shown in, product is a purer carbonization one molybdenum (MoC).
With the scanning electron microscope (SEM) complex (the MoC@to a carbonization one molybdenum nanoparticle Yu ultra-thin Graphene shell
GS) carry out surface appearance feature to characterize, result as in figure 2 it is shown, carbonization one molybdenum (MoC) diameter of nano particles be 1～
10nm。
With the transmission electron microscope (TEM) complex (the MoC@to a carbonization one molybdenum nanoparticle Yu ultra-thin Graphene shell
GS) carry out more specifically Characterization of morphology and structure, result as it is shown on figure 3, carbonization one molybdenum (MoC) diameter of nano particles be 1～
10nm, the number of plies of Graphene thin layer is 1～3 layer.
The chemical property of complex (the MoC@GS) negative material of one carbonization one molybdenum nanoparticle and ultra-thin Graphene shell
Characterize:
By complex (MoC@GS) and the Super-of the carbonization one molybdenum nanoparticle for preparing and ultra-thin Graphene shell
P, sodium alginate (SA) 8:1:1 in mass ratio uniformly mix, and solvent is deionized water, make slurry and are coated uniformly on Copper Foil afflux
On body, making pole piece after vacuum drying, metallic sodium is to electrode, glass fiber filter (Whatman company of Britain GF/D) conduct
Barrier film, electrolyte is 1M NaClO4EC:PC=1:1 (volume ratio), 5%FEC are additive, assemble and obtain in glove box
CR2016 button cell.
The battery of above-mentioned assembling carries out on LAND charge-discharge test instrument constant current charge-discharge test, and discharge and recharge interval is 3
～0.01V.
As shown in Figure 4 and Figure 5, battery has higher discharge capacity first to the result of charge-discharge test and preferably circulation is steady
Qualitative.When electric current density is 500mA/g, its first discharge capacity be 288.1mAh/g, coulombic efficiency is 48.8%, circulation
After 200 times, discharge capacity remains at 105.8mAh/g.Can draw, in the present invention preparation a carbonization one molybdenum nanoparticle with
The complex (MoC@GS) of ultra-thin Graphene shell, as anode material of lithium-ion battery, has good chemical property.
Embodiment 5
Different from embodiment 4 being, the charging and discharging currents density of the present embodiment is 100mA/g, and other conditions are the most identical, group
Dress sodium-ion battery test its chemical property, its first discharge capacity be 495.4mAh/g, coulombic efficiency is 46.4%, circulation
After 40 times, discharge capacity remains at 188.1mAh/g.
Embodiment 6
Different from embodiment 4 being, the charging and discharging currents density of the present embodiment is 1A/g, and other conditions are the most identical, and it is first
Secondary discharge capacity is 268.2mAh/g, and coulombic efficiency is 56.8%, and after circulating 450 times, discharge capacity remains at 87.6mAh/
G, result shows the chemical property all under different electric current densities with excellence, and still has preferable electricity when big electric current
Chemism.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (10)
1. the preparation method of a novel anode material of lithium-ion battery, it is characterised in that comprise the following steps:
Carbon source and molybdenum source are dissolved in a solvent, reacting by heating, obtain presoma Mo3(BTC)2, then carry out in-situ carburization, obtain
One carbonization one molybdenum nanoparticle and the complex of ultra-thin Graphene shell.
The preparation method of novel anode material of lithium-ion battery the most according to claim 1, it is characterised in that: described carbon
Source is at least one in trimesic acid, aniline and p-phthalic acid；Described molybdenum source is hexacarbonylmolybdenum, three carbonyl cycloheptyls three
At least one in thiazolinyl molybdenum, ammonium molybdate and sodium molybdate.
The preparation method of novel anode material of lithium-ion battery the most according to claim 1, it is characterised in that: described carbon
Source is trimesic acid；Described molybdenum source is hexacarbonylmolybdenum.
The preparation method of novel anode material of lithium-ion battery the most according to claim 1, it is characterised in that: molybdenum source used
Mol ratio 1:10～1:15 with carbon source；The temperature of described reacting by heating is 100～200 DEG C；The time of described reacting by heating is 3
It or more than 3 days；The temperature of described carbonization is 500～1000 DEG C；The time of described carbonization is 2～8h.
The preparation method of novel anode material of lithium-ion battery the most according to claim 1, it is characterised in that: molybdenum source used
Mol ratio 1:13.6 with carbon source；The temperature of described reacting by heating is 150～160 DEG C；The time of described reacting by heating be 5 days or
More than 5 days；The temperature of described carbonization is 700～900 DEG C；The time of described carbonization is 5h.
6. a novel anode material of lithium-ion battery, it is characterised in that according to the novel sodium described in any one of Claims 1 to 5
The preparation method of ion battery cathode material obtains.
Novel anode material of lithium-ion battery the most according to claim 6, it is characterised in that described material is a carbonization one
Molybdenum nanoparticle and the complex of ultra-thin Graphene shell, concrete structure is that ultra-thin Graphene shell is coated with a carbonization one molybdenum nanoparticle,
Wherein, a diameter of the 1～10nm of a carbonization one molybdenum nanoparticle.
8. a sodium-ion battery negative pole based on the novel anode material of lithium-ion battery described in claim 6, its feature exists
In including novel anode material of lithium-ion battery, binding agent and conductive agent described in claim 6.
9. a sodium-ion battery based on the sodium-ion battery negative pole described in claim 8, it is characterised in that include that right is wanted
Seek the sodium-ion battery negative pole described in 8, to electrode metal sodium, three parts of electrolyte system.
The novel anode material of lithium-ion battery the most according to claim 6 application in sodium-ion battery.
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