CN109473668A - A kind of modified prelithiation material and preparation method thereof and lithium battery - Google Patents
A kind of modified prelithiation material and preparation method thereof and lithium battery Download PDFInfo
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- CN109473668A CN109473668A CN201811255742.3A CN201811255742A CN109473668A CN 109473668 A CN109473668 A CN 109473668A CN 201811255742 A CN201811255742 A CN 201811255742A CN 109473668 A CN109473668 A CN 109473668A
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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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
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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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- 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 discloses a kind of modified prelithiation material and preparation method thereof and lithium batteries, comprising: the general formula of modified prelithiation material is Liz(CuxAy)O2, wherein x+y=1,0 < x <, 1,0 < y <, 1,0 < z < 2；A is the element that chemical valence is greater than+2；There are three characteristic peaks for tool in the X-ray diffraction XRD spectra of the modified prelithiation material, it is greater than 0.15 in 18.5 ° to 19.0 °, 26.0 ° to 27.0 ° and 32.0 ° to 33.0 °, (002) crystal face and the diffraction peak intensity ratio of (101) crystal face respectively；The granularity of the modified prelithiation material is 100nm-10um.
Description
Technical field
The present invention relates to lithium battery material technical field more particularly to a kind of modified prelithiation material and preparation method thereof and
Lithium battery.
Background technique
Output voltage is high, energy density is high, have extended cycle life, have a safety feature, memoryless effect because having for lithium ion battery
The features such as answering is successfully applied to mobile power source field as main energy storage device.For further satisfaction power grid energy storage, electronic
The demand of automobile and consumer electronics product to energy storage device, more long circulation life, safety is more preferable, energy density is higher
Electrode material and lithium battery system become research hotspot.
Commercial Li-ion battery cathode mainly uses graphite material at present, and the theoretical capacity of graphite material is in 372mAh/
G limits the specific capacity of lithium ion battery entirety.With the alloy material of cathode of higher theoretical capacity gradually replace graphite material at
For trend.However with lithium ion irreversible reaction occurs for most of height ratio capacity negative electrode material generally existing first weeks, to consume
Lithium source in lithium battery reduces battery entirety specific capacity.
Therefore solve the problems, such as that all low efficiencys of the head of the alloy material of cathode of height ratio capacity become key.Wherein prelithiation skill
Art proposes to become most possible solution in the first week supplement lithium ion of Battery formation.However existing prelithiation technology is big
The problems such as there are prelithiation amounts to be difficult to control for part, prelithiation amount is small, there are side reactions, therefore there is an urgent need to propose a kind of pre- lithium
Change material and preparation method thereof to make up this technical bottleneck.
Summary of the invention
The present invention provides a kind of modified prelithiation material and preparation method thereof and lithium battery, modification prelithiation of the invention
Material is greatly improved the capacity of lithium battery.Preparation method is simple, abundant raw materials low to environmental requirement, is suitable for greatly
Large-scale production.
In a first aspect, the embodiment of the invention provides a kind of modified prelithiation materials, comprising:
The general formula of the modified prelithiation material is Liz(CuxAy)O2, wherein x+y=1,0 < x <, 1,0 < y <, 1,0 < z
< 2；A is the element that chemical valence is greater than+2；
There are three characteristic peaks for tool in the X-ray diffraction XRD spectra of the modified prelithiation material, respectively extremely at 18.5 °
The diffraction peak intensity ratio of 19.0 °, 26.0 ° to 27.0 ° and 32.0 ° to 33.0 °, (002) crystal face and (101) crystal face is greater than 0.15；
The granularity of the modified prelithiation material is 100nm-10um.
Preferably, the A is the one or more of aluminium, titanium, iron, vanadium, tungsten, niobium, tantalum, zirconium or lanthanum.
Preferably, the Liz(CuxAy)O2In, 0.5 < x <, 0.9,0.1 < y <, 0.5,0 < z < 1.9；(002) crystal face
It is greater than 0.2 with the diffraction peak intensity ratio of (101) crystal face；The granularity of the modified prelithiation material is 100nm-5um.
It is further preferred that the Liz(CuxAy)O2In, 0.6 < x <, 0.8,0.2 < y <, 0.4,0 < z < 1.8；
(002) the diffraction peak intensity ratio of crystal face and (101) crystal face is greater than 0.3；The granularity of the modified prelithiation material is 100nm-
1um。
Preferably, the particle proterties of the modified prelithiation material be round, ellipse, sheet or polygon one kind or
It is a variety of.
Preferably, the de- lithium capacity of the modified prelithiation material is 300mAh/g-500mAh/g；De- lithium voltage is 3-
4.6V。
Second aspect, the embodiment of the invention provides a kind of preparation methods of modified prelithiation material, comprising:
The raw material of modified prelithiation material are put into mixing apparatus according to stoichiometric ratio and are uniformly mixed, are obtained
Mixture；Wherein, the raw material of the modified prelithiation material include the respective oxide of tri- kinds of elements of Li, Cu and A, hydroxide
Object, carbonate, phosphate, ammonium salt or organic salt, in the raw material, the stoichiometric ratio of the compound of three kinds of elements exists
(1.5-2): (0.5-1): (0.1-0.5), granularity is between 10nm-10um；A is the element that chemical valence is greater than+2；
The mixture is put into agglomerating plant and is sintered, sintering temperature between 300 DEG C -900 DEG C, obtain half at
Product material；
The semi-finished product material is put into crushing plant and carries out primary breakup；
Semifinished material investment disintegrating apparatus after the primary breakup is crushed to get the modified prelithiation is arrived
Material.
Preferably, the mixing apparatus includes: double movement mixers, three-dimensional mixer, V-Mixer, single cone double helix
One of mixing machine, slot type spiral ribbon mixer and horizontal Agravicmixer；
The agglomerating plant includes: one of batch-type furnace, tube furnace, roller-way cellar and rotary furnace；
The crushing plant includes: jaw crusher, gyratory crusher, impact breaker, hammer mill and roll-type
One of crusher；
The disintegrating apparatus includes: flat air flow crusher, fluidized bed airflow pulverizer, circulating air-flow crushing
Machine, impacting breakers, expansion type crusher, ball mill pulverizer, high speed rotation throwing type pulverizer and high speed rotation impacting type
One of pulverizer.
Preferably, the sintering specifically includes: in air atmosphere, vacuum atmosphere, nitrogen atmosphere, argon atmosphere, argon hydrogen
It is sintered under atmosphere or oxygen atmosphere.
The third aspect, the embodiment of the invention provides a kind of including modification prelithiation material described in above-mentioned first aspect
Lithium battery.
Modified prelithiation material provided by the invention, is greatly improved the capacity of lithium battery.Preparation method is simple, right
Environmental requirement is low, abundant raw materials, is suitable for large-scale production.
Detailed description of the invention
Below by drawings and examples, the technical solution of the embodiment of the present invention is described in further detail.
Fig. 1 is scanning electron microscope (SEM) figure of modified prelithiation material provided in an embodiment of the present invention；
Fig. 2 is X-ray diffraction (XRD) figure of modified prelithiation material provided in an embodiment of the present invention；
Fig. 3 is the preparation method flow chart of modified prelithiation material provided in an embodiment of the present invention；
Fig. 4 is the electrochemistry figure that the embodiment of the present invention one provides.
Specific embodiment
Below with reference to embodiment, the present invention is further described in detail, but is not intended to limit guarantor of the invention
Protect range.
The embodiment of the invention provides a kind of modified prelithiation material, general formula Liz(CuxAy)O2, wherein A is chemical combination
Valence is greater than+2 element, can specifically include the one or more of aluminium, titanium, iron, vanadium, tungsten, niobium, tantalum, zirconium or lanthanum；X+y in general formula
1,0 < y < of=1,0 < x <, 1,0 < z < 2.
The particle proterties of modified prelithiation material are the one or more of circle, ellipse, sheet or polygon, and granularity is
100nm-10um, shown in pattern SEM figure as shown in Figure 1.There are three characteristic peaks for tool in its X-ray diffraction XRD spectra, exist respectively
18.5 ° to 19.0 °, 26.0 ° to 27.0 ° and 32.0 ° to 33.0 °；(002) diffraction peak intensity of crystal face and (101) crystal face is than big
In 0.15.
In preferred example, modified prelithiation material Liz(CuxAy)O2, 0.5 < x <, 0.9,0.1 < y <, 0.5,0 < z
< 1.9；(002) the diffraction peak intensity ratio of crystal face and (101) crystal face is greater than 0.2；Granularity is 100nm-5um.
In preferred example, modified prelithiation material Liz(CuxAy)O2, 0.6 < x <, 0.8,0.2 < y < 0.4,0
< z < 1.8；(002) the diffraction peak intensity ratio of crystal face and (101) crystal face is greater than 0.3；Granularity is 100nm-1um.
The de- lithium capacity of modified prelithiation material provided in an embodiment of the present invention is 300mAh/g-500mAh/g, takes off lithium electricity
Pressure is 3-4.6V.It is applied in lithium battery, can greatly promote the capacity of lithium battery.
Correspondingly, the embodiment of the invention also provides the methods for preparing above-mentioned modified prelithiation material.Its preparation flow is such as
Shown in Fig. 3, mainly include the following steps:
Step 310, the raw material of modified prelithiation material are put into mixing apparatus according to stoichiometric ratio and are carried out uniformly
Mixing, obtains mixture；
Wherein, the raw material of modified prelithiation material include lithium source, copper source and doping element compound, respectively Li, Cu
With the respective oxide of tri- kinds of elements of A, hydroxide, carbonate, phosphate, ammonium salt or organic salt；In raw material, lithium source,
Copper source and the stoichiometric ratio of doping element compound are at (1.5-2): (0.5-1): (0.1-0.5), lithium source, copper source and doping member
The granularity of plain compound is between 10nm-10um；A be chemical valence be greater than+2 element, can specifically include aluminium, titanium, iron, vanadium,
Tungsten, niobium, tantalum, zirconium or lanthanum it is one or more；
Mixing apparatus used include: double movement mixers, three-dimensional mixer, V-Mixer, single cone double worm mixer,
One of slot type spiral ribbon mixer and horizontal Agravicmixer.
Step 320, mixture is put into agglomerating plant and is sintered, sintering temperature obtains between 300 DEG C -900 DEG C
Semi-finished product material；
Agglomerating plant used includes: one of batch-type furnace, tube furnace, roller-way cellar and rotary furnace.Being sintered environment is in sky
It is sintered in gas atmosphere, vacuum atmosphere, nitrogen atmosphere, argon atmosphere, argon nitrogen atmosphere or oxygen atmosphere.
Step 330, semi-finished product material is put into crushing plant and carries out primary breakup；
Crushing plant used includes: jaw crusher, gyratory crusher, impact breaker, hammer mill and roll-type
One of crusher.
Step 340, the semifinished material investment disintegrating apparatus after primary breakup is crushed to get modified prelithiation is arrived
Material.
Disintegrating apparatus used includes: flat air flow crusher, fluidized bed airflow pulverizer, circulating air-flow crushing
Machine, impacting breakers, expansion type crusher, ball mill pulverizer, high speed rotation throwing type pulverizer and high speed rotation impacting type
One of pulverizer.
Preparation method provided by the invention is simple, abundant raw materials low to environmental requirement, is suitable for large-scale production.
Below by specific example, technical solution of the present invention is further elaborated.
Embodiment 1
Present embodiments provide a kind of modified prelithiation material Li1.8(Cu0.8AL0.2)O2.Its preparation process is according to corresponding
Stoichiometric ratio weigh granularity be the lithium carbonate of 1um, the copper oxide of 500nm, 10nm alumina material.By three kinds of raw material
It is placed in the mixing of V cone screw mixer high speed, revolving speed 400rpm, incorporation time is 1 hour.Mixture is taken out, is placed
It is sintered in atmosphere batch-type furnace.It is passed through argon atmosphere, the specific procedure of sintering are as follows: room temperature is to 900 DEG C, 5 DEG C/min, heat preservation
24 hours, Temperature fall.Semi-finished product after sintering are crushed using jaw crusher, carry out powder using airslide disintegrating mill
It is broken, obtain modified prelithiation material.Its XRD spectrum is as shown in Figure 2.Fig. 4 is modification prelithiation material prepared by the present embodiment
Half-cell electrochemical property test result figure, its specific capacity of test result are 420mAh/g.
Embodiment 2
Present embodiments provide a kind of modified prelithiation material Li1.9(Cu0.9AL0.1)O2.Its preparation process is according to corresponding
Stoichiometric ratio weigh granularity be the lithium hydroxide of 5um, the copper oxide of 500nm, 10nm alumina material.By three kinds of former materials
Material, which is placed in ball mill, to be mixed, and water is added as dispersion machine, and revolution revolving speed is 600rpm, rotation revolving speed 300rpm, is mixed
Closing the time is 5 hours.Mixture is taken out, is placed in vacuum drying and is dried.It is box to be placed in atmosphere for mixture after drying
It is sintered in furnace.It is passed through argon atmosphere, the specific procedure of sintering are as follows: room temperature keeps the temperature 36 hours to 800 DEG C, 5 DEG C/min, from
So cooling.Semi-finished product after sintering are crushed using jaw crusher, is crushed, is changed using airslide disintegrating mill
Property prelithiation material.Its XRD spectrum is as shown in Figure 2.
Embodiment 3
Present embodiments provide a kind of modified prelithiation material Li1.8(Cu0.9Ti0.1)O2.Its preparation process is according to corresponding
Stoichiometric ratio weigh granularity be the lithium acetate of 5um, the copper acetate of 200nm, 10nm alumina material.By three kinds of raw material
It is placed in the mixing of V cone screw mixer high speed, revolving speed 400rpm, incorporation time is 1 hour.Mixture is placed in atmosphere
It is sintered in batch-type furnace.It is passed through nitrogen atmosphere, the specific procedure of sintering are as follows: for room temperature to 900 DEG C, 5 DEG C/min, heat preservation 36 is small
When, Temperature fall.Semi-finished product after sintering are crushed using jaw crusher, are crushed using airslide disintegrating mill,
Obtain modified prelithiation material.Its XRD spectrum is as shown in Figure 2.
Embodiment 4
Present embodiments provide a kind of modified prelithiation material Li1.8(Cu0.9Fe0.2)O2.Its preparation process is according to corresponding
Stoichiometric ratio weigh granularity be the lithium carbonate of 5um, the Kocide SD of 200nm, 10nm iron oxide.Three kinds of raw material are put
It is placed in the mixing of V cone screw mixer high speed, revolving speed 400rpm, incorporation time is 1 hour.Mixture is placed in atmosphere box
It is sintered in formula furnace.It is passed through air atmosphere, the specific procedure of sintering are as follows: room temperature keeps the temperature 72 hours to 900 DEG C, 5 DEG C/min,
Temperature fall.Semi-finished product after sintering are crushed using jaw crusher, is crushed, is obtained using airslide disintegrating mill
Modified prelithiation material.
Embodiment 5
Present embodiments providing a kind of modified prelithiation material is Li1.7(Cu0.7Fe0.3)O2.Its preparation process is according to phase
The stoichiometric ratio answered weighs the iron oxide that granularity is the lithium carbonate of 5um, the Kocide SD of 200nm, 10nm.By three kinds of raw material
It is placed in the mixing of V cone screw mixer high speed, revolving speed 400rpm, incorporation time is 1 hour.Mixture is placed in atmosphere
It is sintered in batch-type furnace.It is passed through air atmosphere, the specific procedure of sintering are as follows: for room temperature to 900 DEG C, 5 DEG C/min, heat preservation 72 is small
When, Temperature fall.Semi-finished product after sintering are crushed using jaw crusher, are crushed using airslide disintegrating mill,
Obtain modified prelithiation material.
Modified prelithiation material provided by the invention, is greatly improved the capacity of lithium battery.Preparation method is simple, right
Environmental requirement is low, abundant raw materials, is suitable for large-scale production.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of modified prelithiation material, which is characterized in that the general formula of the modified prelithiation material is Liz(CuxAy)O2, wherein
1,0 < y < of x+y=1,0 < x <, 1,0 < z < 2；A is the element that chemical valence is greater than+2；
Tool is there are three characteristic peak in the X-ray diffraction XRD spectra of the modified prelithiation material, respectively 18.5 ° to 19.0 °,
26.0 ° to 27.0 ° and 32.0 ° to 33.0 °, the diffraction peak intensity ratio of (002) crystal face and (101) crystal face is greater than 0.15；
The granularity of the modified prelithiation material is 100nm-10um.
2. modified prelithiation material according to claim 1, which is characterized in that the A be aluminium, titanium, iron, vanadium, tungsten, niobium,
Tantalum, zirconium or lanthanum it is one or more.
3. modified prelithiation material according to claim 1, which is characterized in that the Liz(CuxAy)O2In, 0.5 < x <
0.9,0.1 < y <, 0.5,0 < z < 1.9；(002) the diffraction peak intensity ratio of crystal face and (101) crystal face is greater than 0.2；The modification
The granularity of prelithiation material is 100nm-5um.
4. modified prelithiation material according to claim 3, which is characterized in that the Liz(CuxAy)O2In, 0.6 < x <
0.8,0.2 < y <, 0.4,0 < z < 1.8；(002) the diffraction peak intensity ratio of crystal face and (101) crystal face is greater than 0.3；The modification
The granularity of prelithiation material is 100nm-1um.
5. modified prelithiation material according to claim 1, which is characterized in that the graininess of the modified prelithiation material
Shape is the one or more of circle, ellipse, sheet or polygon.
6. modified prelithiation material according to claim 1, which is characterized in that the de- lithium of the modified prelithiation material holds
Amount is 300mAh/g-500mAh/g；De- lithium voltage is 3-4.6V.
7. a kind of preparation method of modified prelithiation material, which is characterized in that the described method includes:
The raw material of modified prelithiation material are put into mixing apparatus according to stoichiometric ratio and are uniformly mixed, are mixed
Object；Wherein, the raw material of the modified prelithiation material include the respective oxide of tri- kinds of elements of Li, Cu and A, hydroxide,
Carbonate, phosphate, ammonium salt or organic salt, in the raw material, the stoichiometric ratio of the compound of three kinds of elements is in (1.5-
2): (0.5-1): (0.1-0.5), granularity is between 10nm-10um；A is the element that chemical valence is greater than+2；
The mixture is put into agglomerating plant and is sintered, sintering temperature obtains semi-finished product between 300 DEG C -900 DEG C
Material；
The semi-finished product material is put into crushing plant and carries out primary breakup；
Semifinished material investment disintegrating apparatus after the primary breakup is crushed to get the modified prelithiation material is arrived
Material.
8. preparation method according to claim 7, which is characterized in that
The mixing apparatus includes: double movement mixers, three-dimensional mixer, V-Mixer, single cone double worm mixer, slot type
One of spiral ribbon mixer and horizontal Agravicmixer；
The agglomerating plant includes: one of batch-type furnace, tube furnace, roller-way cellar and rotary furnace；
The crushing plant includes: jaw crusher, gyratory crusher, impact breaker, hammer mill and roll crushing
One of machine；
The disintegrating apparatus includes: flat air flow crusher, fluidized bed airflow pulverizer, circulating airslide disintegrating mill, hits
Impact crusher, expansion type crusher, ball mill pulverizer, high speed rotation throwing type pulverizer and high speed rotation impacting type pulverizer
One of.
9. preparation method according to claim 7, which is characterized in that the sintering specifically includes: in air atmosphere, vacuum
It is sintered under atmosphere, nitrogen atmosphere, argon atmosphere, argon nitrogen atmosphere or oxygen atmosphere.
10. a kind of lithium battery including any modification prelithiation material of the claims 1-6.
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| CN112467139A (en) * | 2020-10-23 | 2021-03-09 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode pre-lithiation agent and preparation method and application thereof |
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| CN106058168A (en) * | 2016-02-03 | 2016-10-26 | 万向A二三系统有限公司 | Prelithiated positive electrode material for lithium ion secondary battery |
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| CN112467139A (en) * | 2020-10-23 | 2021-03-09 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode pre-lithiation agent and preparation method and application thereof |
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