CN109585825A - The Ni/NiFe of bimetallic MOF precursor synthesis2O4Lithium ion battery negative material and preparation method thereof - Google Patents
The Ni/NiFe of bimetallic MOF precursor synthesis2O4Lithium ion battery negative material and preparation method thereof Download PDFInfo
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- CN109585825A CN109585825A CN201811431176.7A CN201811431176A CN109585825A CN 109585825 A CN109585825 A CN 109585825A CN 201811431176 A CN201811431176 A CN 201811431176A CN 109585825 A CN109585825 A CN 109585825A
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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
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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
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of Ni/NiFe of bimetallic MOF precursor synthesis2O4Lithium ion battery negative material and preparation method thereof.The Ni/NiFe2O4Electrode material is by simple substance Ni and NiFe2O4Compound composition, preparation method are using soluble nickel salt and molysite as main material, and amino terephthalic acid (TPA) is ligand, constructs Ni-Fe-MOFs presoma using solvent-thermal method, further obtains Ni/NiFe through drying and roasting2O4Electrode material.The Ni/NiFe synthesized using the method for the present invention2O4, material morphology and of uniform size, about 200~400nm, wherein Ni and NiFe2O4Dispersed precipitate, and there is high-specific surface area and high porosity, therefore existing good electronic conductivity, and good transmission channel can be provided for lithium ion, so showing excellent structural stability, cycle performance and high rate performance when as lithium ion battery negative material.The method of the present invention simple process, low for equipment requirements, at low cost, obtained Ni/NiFe2O4Lithium ion battery negative material has a good application prospect.
Description
Technical field
The invention discloses bimetallic MOF precursor synthesis Ni/NiFe2O4Lithium ion battery negative material and its preparation side
Method belongs to lithium ion battery electrode material field.
Background technique
Transition metal oxide is a kind of important functional material, is being catalyzed, the numerous areas such as semiconductor and battery have
Wide application prospect.With the fast development of science and technology, metal oxide obtains comprehensive, deep understanding.Lithium-ion electric
Representative one of of the pond as novel green energy storage device, transition metal oxide are considered as potential negative electrode material.
NiFe2O4Have the characteristics that high specific capacity, safety are good and environmental-friendly.However it is the same with big poly-metal deoxide,
NiFe2O4There are problems that two in practical applications: first is that electronic conductivity is low；Second is that biggish during charge and discharge cycles
Volume change destroys material structure integrality, and active material dusting even falls off from collector, eventually leads to material
The capacity attenuation of material is obvious, and cycle performance is deteriorated.Disadvantages described above greatly hinders NiFe2O4In electrode material of lithium battery field
Business application.
Document, which generallys use, at present introduces various carbon materials or other materials cladding preparation NiFe2O4Composite material.
CN103700842A discloses a kind of NiFe2O4The preparation method of/C negative electrode material, but the NiFe synthesized2O4/ C negative electrode material table
Reveal poor cyclical stability.CN104051729A discloses a kind of using the compound NiFe of two-step method synthesizing graphite alkene2O4Material
Preparation method, the synthesis cost of the invention is high, and step is more many and diverse, is not easy to industrialized implementation.CN108039479A is disclosed
A kind of LiPON coats NiFe2O4Membrane electrode, which goes out excellent charging and discharging circulation reversibility (specific capacity
Be maintained at 872mAh/g), 50 times circulation after capacity obviously do not decay, but this method need to using special equipment implement, to equipment
It is more demanding.In the above patent, the introducing of carbon material or other materials improves the electrochemistry of lithium ion battery negative material
Performance, but materials synthesis is complex, higher cost, and equipment requirement is higher.Therefore, a kind of simple and easy preparation side is found
Method makes NiFe2O4Material has good cycle performance and security and stability has a very important significance.
Metal-organic framework material (MOFs) has high porosity and high-specific surface area and receives significant attention.MOFs is by gold
Belong to network structure obtained by ion and organic ligand self assembly, it is considered to be the ideal template of synthesis high porosity functional material.
Compared to monometallic MOF structure, coordination of the bimetallic in same frame structure promotes the generation of more defects, this is certain
It is Li in degree+Provide more reaction sites.The MOF structure that bimetallic coexists not only increases the complexity of material structure
Property, while also having expanded special performance and application that more metal ions are brought.Therefore, the present invention is with bimetallic MOF network structure
Based on synthesize NiFe2O4Combination electrode material, then Ni/NiFe is prepared by roasting2O4Composite material.The composite material
Have MOF material high specific surface area and pore structure abundant provides good Li+Transmission channel, Ni and NiFe2O4Disperse
Distribution can effectively improve NiFe2O4Electronic conductivity, the final electrochemical stability for improving electrode material.
Summary of the invention
The object of the present invention is to provide a kind of simple and easy, at low cost and electrochemical performance bimetallic MOF
Precursor synthesis Ni/NiFe2O4Lithium ion battery negative material and preparation method thereof, to solve NiFe2O4Conductivity is low, body
The problems such as poor circulation caused by product is changed significantly.
Bimetallic MOF precursor synthesis Ni/NiFe provided by the invention2O4Lithium ion battery negative material, it is characterised in that
The composite material of lithium ion battery cathode is made of simple substance Ni and NiFe2O4, simple substance Ni and NiFe2O4Two-phase is in Dispersed precipitate,
Ni/NiFe2O4Composite gauge is 200~400nm；
Bimetallic MOF precursor synthesis Ni/NiFe provided by the invention2O4Lithium ion battery negative material and its preparation side
Method, it is characterised in that using soluble ferric iron salt and nickel salt as main material, using amino terephthalic acid (TPA) as ligand, N-N dimethyl formyl
Amine (DMF) is reaction medium, obtains Ni-Fe-MOFs presoma using solvent-thermal method, then roasting direct obtains Ni/NiFe2O4
Composite material, the specific steps are as follows:
(1) according to the molar ratio 1:2 of Ni:Fe by nickel salt and iron salt dissolved in DMF, persistently stir 1h or more form it into
Uniform, stable solution；
(2) it is added in mixed solution obtained by amino-terephthalic acid (TPA) to step (1), persistently it is molten to obtain rufous by stirring 1h
Liquid.Wherein the molar ratio of amino-terephthalic acid (TPA) and nickel ion, iron ion is 2:1:2；
(3) it is added in mixed solution obtained by sodium hydroxide solution to step (2), continues to stir 2h.It then will be before acquisition
Liquid solution solvent thermal reaction 6~for 24 hours at 120 DEG C is driven,
(4) step (3) is cooled to room temperature after the reaction was completed, is washed three times respectively using DMF and deionized water, then will precipitating
In lower 80 DEG C of vacuum condition dry 12h, Ni-Fe-MOF presoma is obtained；By gained Ni-Fe-MOF presoma 500~700
2~4h is calcined at DEG C, then cooled to room temperature obtains Ni/NiFe2O4Composite material.
Nickel salt described in the step (1) is nickel nitrate；Molysite is iron chloride；Added DMF dosage is 50mL.
In the step (2), the substance withdrawl syndrome of sodium hydroxide solution is 0.4mol/L.
In the step (3), heating rate is 5 DEG C/min.
Compared with prior art, the present invention has the beneficial effect that:
(1) Ni/NiFe of the method for the present invention preparation2O4The features such as combination electrode material, high-ratio surface and high porosity can
The volume change for sufficiently alleviating active material in charge and discharge process shows good structural stability, and has good follow
Ring performance, discharge capacity is maintained at 653.7mAh/g after 70 circulations.
(2) Ni/NiFe of the method for the present invention preparation2O4Combination electrode material, since the presence of Ni phase effectively improves
NiFe2O4Conductivity meter reveals good high rate performance, and after 2000mA/g high current circulation, specific capacity is stilled remain in
312mAh/g is 641mAh/g when electric current restores 100mA/g specific discharge capacity.
(3) Ni/NiFe of the method for the present invention preparation2O4Combination electrode material, product property is good, and synthesis technology is simple, the party
Method is low for equipment requirements, at low cost.
Detailed description of the invention:
Fig. 1 is to prepare Ni/NiFe in the embodiment of the present invention 12O4The SEM of combination electrode material schemes；
Fig. 2 is to prepare Ni/NiFe in the embodiment of the present invention 12O4The XRD diagram of combination electrode material；
Fig. 3 is to prepare Ni/NiFe in the embodiment of the present invention 12O4The 1st time, the 2nd time and the 70th time constant current of combination electrode material
Charging and discharging curve；
Fig. 4 is to prepare Ni/NiFe in the embodiment of the present invention 12O4The cycle performance figure of combination electrode material；
Fig. 5 is to prepare Ni/NiFe in the embodiment of the present invention 12O4Combination electrode material is forthright again under different current densities
It can figure；
Specific embodiment:
Below with reference to embodiment and attached drawing, the invention will be further described.
Embodiment 1
(1) six water nickel nitrate of 0.727g is weighed respectively, and 1.352g ferric chloride (FeCl36H2O) is dissolved in 50mL DMF, and magnetic force stirs
1h is mixed to forming uniform, stable solution；Then 0.453g amino terephthalic acid (TPA) and 6mL sodium hydroxide solution are sequentially added,
Wherein naoh concentration is 0.4moL/L.
(2) reaction kettle is then placed in 120 DEG C of heat preservations by the autoclave of solution transfer polytetrafluoroethylliner liner
24h.It is cooled to room temperature, is centrifuged after the reaction was completed, washing (three times using DMF washing), 80 DEG C of dry 12h obtain brown Ni-
Fe-MOFs presoma.
(3) obtained brown Ni-Fe-MOFs presoma is placed in Muffle furnace, is warming up to 500 DEG C with 5 DEG C/min, and protect
Temperature processing 2h, then cools to room temperature, finally obtains Ni/NiFe2O4Composite material.
Embodiment 2
(1) six water nickel nitrate of 1.454g is weighed respectively, and 2.704g ferric chloride (FeCl36H2O) is dissolved in 50mL DMF, and magnetic force stirs
1h is mixed to forming uniform, stable solution；Then 0.906g amino terephthalic acid (TPA) and 12mL sodium hydroxide solution are sequentially added,
Wherein naoh concentration is 0.4moL/L.
(2) reaction kettle is then placed in 120 DEG C of heat preservations by the autoclave of solution transfer polytetrafluoroethylliner liner
24h.It is cooled to room temperature, is centrifuged after the reaction was completed, washing (three times using DMF washing), 80 DEG C of dry 12h obtain brown Ni-
Fe-MOFs presoma.
(3) obtained brown Ni-Fe-MOFs presoma is placed in Muffle furnace, is warming up to 500 DEG C with 5 DEG C/min, and protect
Temperature processing 2h, then cools to room temperature, finally obtains Ni/NiFe2O4Composite material.
Embodiment 3
(1) six water nickel nitrate of 0.727g is weighed respectively, and 1.352g ferric chloride (FeCl36H2O) is dissolved in 50mL DMF, and magnetic force stirs
1h is mixed to forming uniform, stable solution；Then 0.453g amino terephthalic acid (TPA) and 6mL sodium hydroxide solution are sequentially added,
Wherein naoh concentration is 0.4moL/L.
(2) reaction kettle is then placed in 120 DEG C of heat preservations by the autoclave of solution transfer polytetrafluoroethylliner liner
24h.It is cooled to room temperature, is centrifuged after the reaction was completed, washing (three times using DMF washing), 80 DEG C of dry 12h obtain brown Ni-
Fe-MOFs presoma.
(3) obtained brown Ni-Fe-MOFs presoma is placed in Muffle furnace, is warming up to 500 DEG C with 5 DEG C/min, and protect
Temperature processing 4h, then cools to room temperature, finally obtains Ni/NiFe2O4Composite material.
Embodiment 4
(1) six water nickel nitrate of 0.727g is weighed respectively, and 1.352g ferric chloride (FeCl36H2O) is dissolved in 50mL DMF, and magnetic force stirs
1h is mixed to forming uniform, stable solution；Then 0.453g amino terephthalic acid (TPA) and 6mL sodium hydroxide solution are sequentially added,
Wherein naoh concentration is 0.4moL/L.
(2) reaction kettle is then placed in 120 DEG C of heat preservations by the autoclave of solution transfer polytetrafluoroethylliner liner
12h.It is cooled to room temperature, is centrifuged after the reaction was completed, washing (three times using DMF washing), 80 DEG C of dry 12h obtain brown Ni-
Fe-MOFs presoma.
(3) obtained brown Ni-Fe-MOFs presoma is placed in Muffle furnace, is warming up to 700 DEG C with 5 DEG C/min, and protect
Temperature processing 4h, then cools to room temperature, finally obtains Ni/NiFe2O4Composite material.
Ni nanoparticle@NiFe2O4Chemical property as lithium ion battery negative material is with the assessment of CR2032 button cell.
Cell assembling processes are as follows: by active material: binder: conductive agent 7:2:1 in mass ratio is uniformly mixed, and a certain amount of N- is added
Uniform slurry is made in methyl pyrrolidone.Then slurry is spread evenly across on copper foil and is dried for 24 hours under 80 DEG C of vacuum conditions,
The load capacity of active material is 3~4mg on each pole piece.Battery assemble sequence are as follows: anode cover-spring leaf-gasket-lithium piece-electricity
Liquid-diaphragm-electrolyte-cathode pole piece-negative electrode casing is solved, the battery assembled is tested using new prestige battery test system.
Ni/NiFe2O4Chemical property as lithium ion battery negative material is tested with CR2032 button cell in new prestige
It is tested on instrument.In electrode preparation, by active material: binder: conductive agent 7:2:1 in mass ratio is uniformly mixed slurrying and applies
Cloth dries for 24 hours on copper foil and under 80 DEG C of vacuum conditions, and the load capacity of active material is 3~4mg on pole piece.Battery assemble sequence
Are as follows: anode cover-spring leaf-gasket-lithium piece-electrolyte-diaphragm-electrolyte-cathode pole piece-negative electrode casing.Lithium piece is used as to electrode
And reference electrode, with the LiPF of 1mol/L6The mixed solution of/EC-DEC (volume ratio 1:1) is electrolyte, and diaphragm selects C2400
Polypropylene porous film.
Fig. 1 is the Ni/NiFe obtained using the present embodiment method2O4The SEM of composite material schemes, as shown, sample is presented
Preferable dispersing uniformity, having a size of 200nm~400nm.
Fig. 2 is the Ni/NiFe obtained using the present embodiment method2O4The XRD diagram of composite material.30 °, 35 °, 43 °,
There is apparent characteristic diffraction peak, with NiFe at 57 °, 62 °2O4(JCPDS No.54-0964) matches, and respectively represents
NiFe2O4(220), (311), (400), (511) and (440) crystal face.The diffraction maximum occurred at 44 ° and 51 ° then respectively corresponds
(111) and (200) crystal face of Ni (JCPDS No. 04-0850).
Fig. 3 is 500 DEG C and calcines obtained Ni/NiFe2O4The constant current charge-discharge that composite material is the 1st time, the 2nd time and the 70th time
Curve.Current density is 100mA/g, and voltage range is 0.01V~3V.As seen from the figure, exist in discharge curve for the first time very bright
Aobvious discharge platform (~0.75V), this corresponds to Ni in process of intercalation2+And Fe3+Reduction.Otherwise charging process corresponds to metal
The oxidation process of oxide.In addition, putting charging capacity for the first time is respectively 846mAh/g and 600mAh/g, coulombic efficiency is for the first time
71%.2nd discharge capacity is 610mAh/g, and irreversible loss capacity may be attributed to the irreversible reaction of electrolyte and consolidate
The formation of body electrolyte interface film (SEI).But after 70 circulations, decaying does not occur not only in battery capacity to be presented instead
The trend risen, discharge capacity reach 663mAh/g.
Fig. 4 is the Ni/NiFe obtained using the present embodiment method2O4The cycle performance figure of composite material.The electrode material
Capacity attenuation is very slow, and as the trend risen is presented in the increase of cycle-index, capacity, illustrates using the method for the present invention
The Ni/NiFe of synthesis2O4Composite material cyclical stability is good.
Fig. 5 is 500 DEG C and calcines obtained Ni/NiFe2O4High rate performance figure of the composite material under different current densities, choosing
Select 100 mA/g, 300mA/g, 500mA/g, the current density progress high rate performance test of 1000mA/g and 2000mA/g.Such as figure
Shown in 5, Ni/NiFe2O4Composite material capacity attenuation under each current density is unobvious, or even follows in 2000mA/g high current
Capacity retention ratio is still higher after ring 10 times, and when current density is restored to 100mA/g, capacity still shows the trend risen,
Show good high rate performance.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills
Art field, is included within the scope of the present invention.
Claims (7)
1. the Ni/NiFe of bimetallic MOF precursor synthesis2O4Lithium ion battery negative material, it is characterised in that: the lithium-ion electric
Pond cathode composite material is by simple substance Ni and NiFe2O4It constitutes.
2. the Ni/NiFe of bimetallic MOF precursor synthesis according to claim 12O4Lithium ion battery negative material,
It is characterized in that: simple substance Ni and NiFe2O4Two-phase is in Dispersed precipitate.
3. the Ni/NiFe of bimetallic MOF precursor synthesis according to claim 12O4Lithium ion battery negative material,
Be characterized in that: the combination electrode material has high specific surface area and high porosity, and pattern is more uniform, having a size of 200
~400nm.
4. the Ni/NiFe of bimetallic MOF precursor synthesis according to claim 12O4Lithium ion battery negative material,
Be characterized in that: discharge capacity is maintained at 653.7mAh/g after 70 circulations, after 2000mA/g high current circulation, specific volume
Amount stills remain in 312mAh/g, is 641mAh/g when electric current restores 100mA/g specific discharge capacity.
5. the Ni/NiFe of bimetallic MOF precursor synthesis according to claim 12O4Lithium ion battery negative material,
Be characterized in that: with iron chloride, nickel nitrate is main material, and amino terephthalic acid (TPA) is ligand, and N-N dimethylformamide (DMF) is
Reaction medium obtains Ni-Fe-MOFs presoma using solvent-thermal method, and then Ni/NiFe is prepared in roasting direct2O4Composite wood
Material, its step are as follows:
(1) iron chloride is weighed, nickel nitrate and amino terephthalic acid (TPA) are successively dissolved in N-N dimethylformamide (DMF), and room temperature is stirred
It mixes and uniformly forms it into uniform, stable solution；
(2) 0.4mol/L sodium hydroxide solution 6mL is added, persistently stirs 1h and obtains brown precursor solution, then by acquisition
Precursor solution solvent thermal reaction 6~for 24 hours at 120 DEG C, is cooled to room temperature after the reaction was completed, sediment using DMF and go from
Sub- water respectively washs three times, then obtains Ni-Fe-MOF presoma in 80 DEG C of vacuum drying 12h；
(3) by Ni-Fe-MOF presoma obtained by step (2) in air atmosphere, 2~4h is roasted at 500~700 DEG C, obtains Ni/
NiFe2O4Composite material.
6. preparation method according to claim 5, which is characterized in that in step (1), amino terephthalic acid (TPA) and iron from
The ratio between amount of substance of son, nickel ion is 2:2:1.
7. preparation method according to claim 5, which is characterized in that in step (3), heating rate is 5 DEG C/min.
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