CN105185968B - A kind of preparation method of lithium ion battery molybdenum oxide/nickel carbon composite negative pole material - Google Patents

A kind of preparation method of lithium ion battery molybdenum oxide/nickel carbon composite negative pole material Download PDF

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CN105185968B
CN105185968B CN201510661685.9A CN201510661685A CN105185968B CN 105185968 B CN105185968 B CN 105185968B CN 201510661685 A CN201510661685 A CN 201510661685A CN 105185968 B CN105185968 B CN 105185968B
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negative pole
moo
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lithium ion
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CN105185968A (en
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赵海雷
夏青
杜志鸿
高春辉
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Jiadao Material Technology Jiaxing Co ltd
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University of Science and Technology Beijing USTB
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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
    • 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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • 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
    • H01M4/626—Metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
    • 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

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Abstract

The invention discloses a kind of preparation method of lithium ion battery molybdenum oxide/nickel carbon composite negative pole material, belong to new material and electrochemical field, problem to be solved is to provide the composite negative pole material of a kind of high specific capacity and cyclical stability and economically viable preparation technology.Using ammonium molybdate tetrahydrate as molybdenum source, nickel nitrate is nickel source, and presoma is prepared by hydro-thermal method, using the method for chemical vapor deposition, prepares MoO2/ Ni/C composites.The advantage of the invention is that cost of material is low, preparation technology is simple.MoO prepared by the method2/ Ni/C composite material compositions are evenly distributed, and have higher reversible specific capacity, preferable cyclical stability and longer cycle life, can play MoO2, the respective advantage of Ni, C, be a kind of preferable composite cathode material for lithium ion cell, can be widely applied to the fields such as various portable electric appts, electric automobile and Aero-Space.

Description

A kind of preparation method of lithium ion battery molybdenum oxide/nickel carbon composite negative pole material
Technical field
The invention belongs to new material and electrochemical field, and in particular to a kind of MoO of high reversible specific capacity2/ Ni/C lithiums from Sub- battery composite cathode material and preparation method thereof.
Technical background
With the development of science and technology, energy crisis and increasingly highlight the problem of environmental pollution, the exploration of novel energy is Through as the task of top priority.Lithium ion battery has extended cycle life because it has energy density high, memory-less effect and environment-friendly etc. Advantage, the fields such as portable electric appts, Aero-Space, military affairs have been widely used in it.At present, notebook mobile phone etc. all becomes Minimized in portability so that the battery of more height ratio capacity turns into the focus of research.
There is some drawbacks for commercial wide variety of graphite-like carbon negative pole material：The current potential of carbon electrode and lithium metal Current potential is very close to (0.01V vs.Li+/ Li), the easy precipitating metal lithium in surface forms dendrite, potential safety hazard be present；Discharged first Generation SEI films are reacted in journey with electrolyte, initial coulomb efficiency is low；Lithium ion is repeatedly during deintercalation, and material structure is by broken It is bad to cause special capacity fade, reduce its service life cycle；Above all its theoretical specific capacity is very low, only 372mAhg-1.Then, novel anode material has become current focus of attention.
The focus studied at present is concentrated mainly on the alloy materials such as Si, Sn, Sb.It is general relative to carbon material, metal material Have preferable compatibility with higher specific capacity, while with electrolyte, but would generally cause during the deintercalation of lithium compared with Big volumetric expansion, cause motor efflorescence to fail, make cycle performance of battery poor.In addition, metal material and carbon material is compound Negative pole is also one of focus, but generally preparation technology is complicated, and cost is higher.The deficiency for more than, the present invention are proposed with MoO2 Material is as lithium ion battery negative material.
Molybdenum oxide, including MoO2, MoO3, their resistance are low, and fusing point is high, while has good chemically and thermally stability. In addition, MoO2There is higher theoretical specific capacity (838mAh/g).MoO2As lithium ion battery negative material, have very big Application prospect, but it there is also certain shortcoming：Its electronic conductance and ionic conductance is poor, while the meeting during removal lithium embedded Generation volumetric expansion causes active material to come off, and causes capacity attenuation.Following method is mainly proposed to be improved at present：
(1) highly conductor phase is introduced, it is generally compound with carbon.The electronic conductance and ionic conductance of molybdenum oxide are poor, and introducing carbon can To improve the electric conductivity of molybdenum oxide.Xiaolin Liu et al. synthesize uniform hollow MoO by simple soft template hydro-thermal method2@ Carbon composites, the discharge and recharge under 0.5C current density, specific capacity still keep 800mAhg when circulating for 100 times-1, follow Ring excellent in stability (Liu X, Wu D, Ji W, et al.Uniform MoO2@carbon hollow nanospheres with superior lithium-ion storage properties[J].Journal of Materials Chemistry A,2015,3(3):968-972.).Yun Xu et al. prepare MoO using solvent-thermal method2/ GO composite negative pole materials Material, in 100mAg-1Current density under, 30 times circulation when still have 726mAhg-1(Xu Y,Yi R,Yuan B,et al.High capacity MoO2/graphite oxide composite anode for lithium-ion batteries[J].The Journal of Physical Chemistry Letters,2012,3(3):309-314.)。
(2) nano-scale particle is prepared, shortens lithium ion diffusion path, buffer volumes expansion.Xianfa Zhang et al. are used Solvent-thermal method is prepared for the MoO with hollow core shell structure2Particle.Almost no capacity declines in the negative material charge and discharge cycles Subtract, in 50mAg-1Current density under, 50 times circulation when still have 847.5mAhg-1(Zhang X,Song X,Gao S,et al.Facile synthesis of yolk-shell MoO2microspheres with excellent electrochemical performance as a Li-ion battery anode[J].Journal of Materials Chemistry A,2013,1(23):6858-6864.)。
The content of the invention
It is an object of the invention to provide a kind of even particle distribution, regular appearance, has of a relatively high reversible specific volume The MoO of amount, preferable cyclical stability and longer cycle life2/ Ni/C composite cathode material for lithium ion cell.
A kind of preparation method of lithium ion battery molybdenum oxide/nickel carbon composite negative pole material, it is characterised in that：Composite negative pole Material is by MoO2, tri- kinds of components of Ni, C form, wherein Ni is in MoO2Weight/mass percentage composition in/Ni/C composite negative pole materials is 5 ~30%, C are in MoO2Weight/mass percentage composition in/Ni/C composite negative pole materials is 5~50%, and remaining is MoO2。
It is concretely comprised the following steps：
(1) solution is configured：By ammonium molybdate (NH4)6Mo7O24·4H2O is as molybdenum source, and in deionized water, stirring is equal for dissolving It is even, clear transparent solutions a is made, the wherein addition of molybdenum is 0.1mM~5mM；
Using the inorganic salts containing nickel element as nickel source, it is dissolved in solution a, stirs according to Mo/Ni mol ratio=0.01~10 Mix uniformly, solution b is made.
A certain amount of urea is added in solution b, stirs to abundant dissolving, obtains solution c, the addition of wherein urea is 0.2~100g/mL.
(2) after solution c is stirred, 150~200 DEG C of 1~24h of hydro-thermal in baking oven is placed in hydro-thermal tank, are sunk Form sediment；
(3) by pelleting centrifugation obtained by step (2), centrifuged with deionized water and ethanol wash repeatedly, 50~90 in baking oven DEG C drying, can obtain presoma.
(4) presoma obtained by step (3) is placed in tube furnace, leads to inert gas, by toluene solution, in 400~700 DEG C heat treatment 0.5~12h, MoO2/Ni/C composites can be obtained.
The addition sequence of molybdenum source, nickel source, urea described in step (1) also can be adjusted voluntarily according to the order.
The inorganic salts containing nickel element described in step (1) are one or both of Ni (NO3) 26H2O, NiCl2.
Inert gas described in step (4) is one or both of nitrogen, argon gas.
Consideration is taken into account from capacity and electric conductivity, mass ratioes of the C in MoO2/Ni/C composite negative pole materials is preferably 8 ~25%, if because carbon content is too low, the electron conduction of material can not be fundamentally improved, carbon content is too high, then The specific capacity of material can be reduced.
MoO2Material has higher specific capacity；Ni is uniformly embedded among particle, is formed good inner conductive network, is carried The high electron conduction of material；Agraphitic carbon is evenly coated at MoO2Surface, it is possible to reduce the inhomogeneities of electric charge, alleviating should The Volume Changes that power inequality is brought；Graphene is attached to surface and the surrounding of particle, plays a part of elastic housing, and padded coaming takes off Volumetric expansion in process of intercalation, prevent active material powder of detached.MoO after compound2/ Ni/C composites play several persons Respective advantage.
The negative material prepared in this way has advantages below：
(1) particle is uniform, regular appearance；
(2) there is of a relatively high specific capacity, cyclical stability and longer cycle life；
(3) each component can play respective advantage.
The present invention synthesizes MoO by hydro-thermal method combination chemical vapour deposition technique2/ Ni/C composites.Carbon and nickel are deposited Effectively improving MoO2Electron conduction, make circulation more stable；Nano active MoO2Particle has of a relatively high specific volume Amount.MoO2/ Ni/C materials have height ratio capacity, high circulation stability and long circulation life, be a kind of lithium of good performance from Sub- cell negative electrode material.
The invention has the advantages that in the building-up process of material, flexibly, simply, reaction condition is gentle for operation, generates powder grain Footpath smaller particle is uniform, and technique simply can be mass-produced.
MoO2/ Ni/C composites are a kind of composite cathode material for lithium ion cell of good performance, this material and its system Preparation Method is there is not yet document and patent report.
Brief description of the drawings
Fig. 1 is the MoO of embodiment 12/ Ni/C cyclic curve figure
Embodiment
With reference to embodiment, the present invention will be further described, but is not limited to protection scope of the present invention：
Embodiment 1：
Weigh the pure ammonium molybdate (purity >=99.0%) of 0.177g analyses to be dissolved in 50ml deionized waters, stir, make Into clear transparent solutions；0.291g Ni (NO are added in the solution3)2·6H2O, continue stirring until forming homogeneous solution；Weigh 0.3g urea is added in solution, is stirred to abundant dissolving；Transfer the solution into hydro-thermal tank that to be placed in baking oven 160 DEG C of insulations 12 small When, obtain greenish precipitate；60 DEG C of drying, obtain presoma after centrifuge washing；Presoma is subjected to chemical vapor deposition process, 600 DEG C are incubated 0.5 hour, obtain MoO2/ Ni/C materials.
By obtained MoO2/ Ni/C composite negative pole materials, 15wt.% acetylene black, 15wt.% PVDF are well mixed, Slurry is made, is coated uniformly on copper foil, circular electrode pole piece is stamped into after vacuum drying, using lithium metal as to electrode, 1mol/ L LiPF6/ EMC+DC+DEC (volume ratios 1:1:1) it is electrolyte, Celgard2400 is barrier film, forms test cell.To electricity Pond carries out constant current charge-discharge test, and current density 100mA/g, charging/discharging voltage scope is 0.01~3.0V.As a result show, its Initial coulomb efficiency is 42%, and after 150 circulations, specific capacity is maintained at 680mAh/g or so.
Embodiment 2：
Weigh the pure ammonium molybdate (purity >=99.0%) of 0.354g analyses to be dissolved in 50ml deionized waters, stir, make Into clear transparent solutions；0.582g Ni (NO are added in the solution3)2·6H2O, continue stirring until forming homogeneous solution；Weigh 0.5g urea is added in solution, is stirred to abundant dissolving；Transfer the solution into hydro-thermal tank that to be placed in baking oven 180 DEG C of insulations 2 small When, obtain greenish precipitate；60 DEG C of drying, obtain presoma after centrifuge washing；Presoma is subjected to chemical vapor deposition process, 600 DEG C are incubated 0.5 hour, obtain MoO2/ Ni/C materials.
By obtained MoO2/ Ni/C composite negative pole materials, 15wt.% acetylene black, 15wt.% PVDF are well mixed, Slurry is made, is coated uniformly on copper foil, circular electrode pole piece is stamped into after vacuum drying, using lithium metal as to electrode, 1mol/ L LiPF6/ EMC+DC+DEC (volume ratios 1:1:1) it is electrolyte, Celgard2400 is barrier film, forms test cell.To electricity Pond carries out constant current charge-discharge test, and current density 100mA/g, charging/discharging voltage scope is 0.01~3.0V.As a result show, its Initial coulomb efficiency is 51%, and after 100 circulations, specific capacity is maintained at 500mAh/g or so.
Embodiment 3：
Weigh the pure ammonium molybdate (purity >=99.0%) of 17.7g analyses to be dissolved in 500ml deionized waters, stir, make Into clear transparent solutions；29.1g Ni (NO are added in the solution3)2·6H2O, continue stirring until forming homogeneous solution；Weigh 20g urea is added in solution, is stirred to abundant dissolving；Transfer the solution into hydro-thermal tank that to be placed in baking oven 160 DEG C of insulations 2 small When, obtain greenish precipitate；60 DEG C of drying, obtain presoma after centrifuge washing；Presoma is subjected to chemical vapor deposition process, 600 DEG C are incubated 0.5 hour, obtain MoO2/ Ni/C materials.
By obtained MoO2/ Ni/C composite negative pole materials, 15wt.% acetylene black, 15wt.% PVDF are well mixed, Slurry is made, is coated uniformly on copper foil, circular electrode pole piece is stamped into after vacuum drying, using lithium metal as to electrode, 1mol/ L LiPF6/ EMC+DC+DEC (volume ratios 1:1:1) it is electrolyte, Celgard2400 is barrier film, forms test cell.To electricity Pond carries out constant current charge-discharge test, and current density 100mA/g, charging/discharging voltage scope is 0.01~3.0V.As a result show, its Initial coulomb efficiency is 49%, and after 100 circulations, specific capacity is maintained at 400mAh/g or so.

Claims (6)

  1. A kind of 1. preparation method of lithium ion battery molybdenum oxide/nickel carbon composite negative pole material, it is characterised in that：Composite negative pole material Material is by MoO2, tri- kinds of components of Ni, C form, wherein Ni is in MoO2Weight/mass percentage composition in/Ni/C composite negative pole materials for 5 ~ 30%, C are in MoO2Weight/mass percentage composition in/Ni/C composite negative pole materials is 5 ~ 50%, and remaining is MoO2, concrete technology step is：
    (1) solution is configured：By ammonium molybdate (NH4)6Mo7O24·4H2O in deionized water, stirs as molybdenum source, dissolving, makes Into clear transparent solutions a；
    It is dissolved in solution a, stirs using the inorganic salts containing nickel element as nickel source, solution b is made；
    A certain amount of urea is added in solution b, stirs to abundant dissolving, obtains solution c；
    (2) after solution c is stirred, 150 ~ 200 DEG C of h of hydro-thermal 1 ~ 24 in baking oven is placed in hydro-thermal tank, are precipitated；
    (3) by pelleting centrifugation obtained by step (2), multiple, 50 ~ 90 DEG C of bakings in baking oven are centrifuged with deionized water and ethanol wash It is dry, it can obtain presoma；
    (4) presoma obtained by step (3) is placed in tube furnace, leads to inert gas, by toluene solution, in 400 ~ 700 DEG C of heat 0.5 ~ 12 h is handled, MoO can be obtained2/ Ni/C composites.
  2. 2. the preparation method of lithium ion battery molybdenum oxide according to claim 1/nickel carbon composite negative pole material, its feature It is：The addition of molybdenum is the mM of 0.1 mM ~ 5 in clear transparent solutions a described in step (1).
  3. 3. the preparation method of lithium ion battery molybdenum oxide according to claim 1/nickel carbon composite negative pole material, its feature It is：The Ni mol ratios in the Mo and nickel source in solution b described in step (1) are：Mo/Ni mol ratio=0.01 ~ 10.
  4. 4. the preparation method of lithium ion battery molybdenum oxide according to claim 1/nickel carbon composite negative pole material, its feature It is：The addition of urea is 0.2 ~ 100 g/mL in step (1).
  5. 5. the preparation method of lithium ion battery molybdenum oxide according to claim 1/nickel carbon composite negative pole material, its feature It is：The inorganic salts containing nickel element described in step (1) are Ni (NO3)2·6H2O、NiCl2One or both of.
  6. 6. the preparation method of lithium ion battery molybdenum oxide according to claim 1/nickel carbon composite negative pole material, its feature It is：Inert gas described in step (4) is argon gas.
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CN104241624A (en) * 2014-09-24 2014-12-24 南京大学 Method for preparing anode material of molybdenum oxide lithium ion battery by controlling oxidation

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