CN105655583B - A kind of processing method of phosphate metal lithium salt material and the phosphate metal lithium salt material obtained by this method - Google Patents
A kind of processing method of phosphate metal lithium salt material and the phosphate metal lithium salt material obtained by this method Download PDFInfo
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- CN105655583B CN105655583B CN201610124003.5A CN201610124003A CN105655583B CN 105655583 B CN105655583 B CN 105655583B CN 201610124003 A CN201610124003 A CN 201610124003A CN 105655583 B CN105655583 B CN 105655583B
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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 present invention relates to field of lithium ion battery, the phosphate metal lithium salt material for disclosing a kind of processing method of phosphate metal lithium salt material and being obtained by this method.The method of the present invention includes：Phosphate metal lithium salt material is heat-treated under weak oxide atmosphere.Phosphate metal lithium salt material is handled using the method for the present invention, hardly deteriorates the chemical properties such as the specific capacity of electric discharge gram first of material, but can substantially reduce specific surface area, saturated water adsorptive value and the absorption speed of material.
Description
Technical field
The present invention relates to field of lithium ion battery, in particular it relates to a kind of processing method of phosphate metal lithium salt material and
The phosphate metal lithium salt material obtained by this method.
Background technology
Phosphate metal lithium salt material (such as ferrousphosphate lithium material) is present anode material for lithium-ion batteries market both at home and abroad
On one of mainstay material, be the preferred material of current Prospect of EVS Powered with Batteries because of its remarkable security performance, cycle performance
Material.But, because the characteristics of its own structure, compared with traditional cobalt acid lithium, LiMn2O4, three element materials, its electronic conduction
Rate and ionic conductivity are all poor, therefore in practical application, in addition to carbon coating processing is carried out, typically also need to phosphoric acid gold
Belong to lithium salt material and carry out nanosizing processing, the deficiency of electric conductivity is made up by shortening electronics and ion transmission path.However, material
The nanosizing of material can be brought using upper shortcoming, and wherein specific surface area, which is substantially increased, can cause phosphate metal lithium salt material especially to hold
It is hygroscopic, then need more binding agents to ensure the bonding between active material and collector when carrying out battery pole piece coating
Power.Therefore, reduce the specific surface area of phosphate metal lithium salt material and solve to be caused greatly by phosphate metal lithium salt material specific surface area
Water imbibition the problem of rise, the problem of be urgent need to resolve in current phosphate metal lithium salt material application.
The content of the invention
The invention aims to overcome phosphate metal lithium salt material specific surface area of the prior art big and thus draw
The phosphoric acid gold that the defect that the water imbibition risen rises is obtained there is provided a kind of processing method of phosphate metal lithium salt material and by this method
Belong to lithium salt material.
To achieve these goals, in a first aspect, the invention provides a kind of processing method of phosphate metal lithium salt material,
Methods described includes：Phosphate metal lithium salt material is heat-treated under weak oxide atmosphere.
Second aspect, the invention provides the phosphate metal lithium salt material that methods described is obtained.
The method of the present invention, can not only by being heat-treated under weak oxide atmosphere to phosphate metal lithium salt material
The part surplus carbon on phosphate metal lithium salt material surface is removed in weak oxide atmosphere, but also phosphate metal lithium will not be aoxidized
Metal (such as ferrous iron) in salt material, specifically, the part surplus carbon on phosphate metal lithium salt material surface is in weak oxide
It is oxidized in atmosphere and becomes gas and escaped with carrier gas, the metal (such as ferrous iron) in simultaneous oxidation phosphate metal lithium salt material is again
It is not oxidized.
Phosphate metal lithium salt material is handled using the method for the present invention, hardly deteriorates the electric discharge gram specific volume first of material
The chemical properties such as amount, but specific surface area, saturated water adsorptive value and the absorption speed of material can be substantially reduced, and control can be passed through
The temperature and time of processing is heated to regulate and control the amplitude of specific surface area reduction.
Other features and advantages of the present invention will be described in detail in subsequent embodiment part.
Embodiment
The embodiment to the present invention is described in detail below.It should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
In a first aspect, the invention provides a kind of processing method of phosphate metal lithium salt material, methods described includes：By phosphorus
Sour metal lithium salt material is heat-treated under weak oxide atmosphere.
In the method for the present invention, for weak oxide atmosphere, there is no particular limitation, as long as can be by phosphate metal lithium salts
The part surplus carbon of material surface is oxidized to gas, while again will not be by the metal in phosphate metal lithium salt material (such as ferrous iron)
Aoxidized, under preferable case, weak oxide atmosphere is carbon dioxide atmosphere or sulfur trioxide atmosphere, is more preferably
Carbon dioxide atmosphere.Weak oxide atmosphere of the present invention can be 99.99% weak oxide atmosphere.
In the method for the present invention, the present inventor has found under study for action, the suitable temperature and time of control heat treatment
Can be in the case where not causing material electrochemical performance substantially to deteriorate, hence it is evident that specific surface area, the saturated absorption amount of reduction material
And absorption speed.Under preferable case, the condition of heat treatment includes：Temperature is 650-800 DEG C, and the time is 0.5-20h, further excellent
Selection of land, the condition of heat treatment includes：Temperature is 700-750 DEG C, and the time is 2-10h.
Process of the present invention it is preferred in the case of, the condition of heat treatment also includes：Gas flow is 1-20L/min, enters one
Step is preferably 4-10L/min.It will be understood by those skilled in the art that when being heat-treated, controlling These gases flow
It may be such that weak oxide atmosphere is excessive.
In the method for the present invention, for phosphate metal lithium salts, there is no particular limitation, can be common various in this area
Under phosphate metal lithium salts, preferable case, phosphate metal lithium salts is LixMyPO4Or the Li of metal-doped modificationxMyPO4,
LixMyPO4In, the M is selected from least one of Fe, Mn, Co and Ni, and x is 0.9-1.1, and y is 0.9-1.1.Mixed for described
There is no particular limitation for the species of the metal of miscellaneous modification, can be the common various metals in this area, for example can selected from Mg,
At least one of Al, Ti, Na, Ca, Zn, yttrium (Y), lanthanum (La) and samarium (Sm).It is further preferred that LixMyPO4For
LiFeaCobNicMndPO4, wherein 0≤a, b, c, d≤1, and 0.95≤a+b+c+d≤1.1, it is further preferred that LixMyPO4
For LiFePO4、LiMnPO4、LiCoPO4、LiNiPO4、LiFe0.4Mn0.6PO4、LiFe0.4Co0.6PO4、LiFe0.4Co0.3Ni0.3PO4
And LiFe0.3Co0.3Ni0.3Mn0.1PO4At least one of.It will be understood by those skilled in the art that LixMyPO4In, M choosings
From in Fe, Mn, Co and Ni at least two when, y for two kinds of elements of wherein at least stoichiometric proportion sum.
In the method for the present invention, for the Li of metal-doped modificationxMyPO4The amount of the metal ion of middle doping is not special
Restriction, can be the common various consumptions in this area, this is well known to those skilled in the art, and will not be repeated here.Moreover,
Foregoing Li in the present inventionxMyPO4Or the Li of metal-doped modificationxMyPO4Can voluntarily it prepare or commercially available.
In the method for the present invention, phosphate metal lithium salt material is to handle the phosphate metal handled with nanosizing by carbon coating
Lithium salt material.There is no particular limitation for the method handled for cladding processing and nanosizing, can be respectively commonly used in the art
Various methods, this is well known to the skilled person, and will not be repeated here.In the method for the present invention, at carbon coating
The phosphate metal lithium salt material that reason and nanosizing are handled can be prepared voluntarily or by commercially available.
Second aspect, the invention provides the phosphate metal lithium salt material that the above method is obtained.
Embodiment
The present invention will be described in detail by way of examples below, but and is not so limited the present invention.
In following examples, LiFePO4、LiMnPO4, Mg doping LiCoPO4、LiNiPO4、LiFe0.4Mn0.6PO4、
LiFe0.4Co0.6PO4、LiFe0.4Co0.3Ni0.3PO4And LiFe0.3Co0.3Ni0.3Mn0.1PO4By carbon coating processing and nanosizing
Processing, and Guizhou Anda Technology Energy Co., Ltd. is purchased from, wherein,
LiFePO4Carbon content be 1.62 weight %, specific surface area is 16.3m2/ g, under 23 DEG C, 45% relative humidity
(climatic chamber) absorbs water in 1 hour reaches saturation, and saturated water adsorptive value is 6384ppm, the CR2025 button cells being assembled into
The specific capacity of electric discharge gram first under 0.1C charge-discharge magnifications is 160.3mAh/g；
LiMnPO4Carbon content be 2.78 weight %, specific surface area is 23.4m2/ g, under 23 DEG C, 45% relative humidity
(climatic chamber) absorbs water in 30 minutes reaches saturation, and saturated water adsorptive value is 9236ppm, the CR2025 button cells being assembled into
The specific capacity of electric discharge gram first under 0.1C charge-discharge magnifications is 112mAh/g；
LiNiPO4Carbon content be 3.42 weight %, specific surface area is 26.8m2/ g, under 23 DEG C, 45% relative humidity
(climatic chamber) absorbs water in 28 minutes reaches saturation, and saturated water adsorptive value is 9176ppm, the CR2025 button cells being assembled into
The specific capacity of electric discharge gram first under 0.1C charge-discharge magnifications is 115mAh/g；
The LiCoPO of Mg doping4Carbon content be that 3.13 weight %, Mg contents are 0.05 weight %, specific surface area is
26.2m2/ g, (climatic chamber) absorbs water in 32 minutes under 23 DEG C, 45% relative humidity reaches saturation, and saturated water adsorptive value is
The specific capacity of electric discharge gram first under 8945ppm, the CR2025 button cell 0.1C charge-discharge magnifications being assembled into is 117mAh/g；
LiFe0.4Mn0.6PO4Carbon content be 2.52 weight %, specific surface area is 21.8m2/ g, at 23 DEG C, 45% is relatively wet
(climatic chamber) absorbs water in 45 minutes under degree reaches saturation, and saturated water adsorptive value is 7239ppm, the CR2025 buttons electricity being assembled into
The specific capacity of electric discharge gram first under the 0.1C charge-discharge magnifications of pond is 144mAh/g；
LiFe0.4Co0.6PO4Carbon content be 2.77 weight %, specific surface area is 20.9m2/ g, at 23 DEG C, 45% is relatively wet
(climatic chamber) absorbs water in 48 minutes under degree reaches saturation, and saturated water adsorptive value is 6365ppm, the CR2025 buttons electricity being assembled into
The specific capacity of electric discharge gram first under the 0.1C charge-discharge magnifications of pond is 128mAh/g；
LiFe0.4Co0.3Ni0.3PO4Carbon content be 3.11 weight %, specific surface area is 27.1m2/ g, in 23 DEG C, 45% phase
Saturation is reached to water suction in (climatic chamber) under humidity 33 minutes, saturated water adsorptive value is 8543ppm, the CR2025 buttons being assembled into
The specific capacity of electric discharge gram first under formula battery 0.1C charge-discharge magnifications is 125mAh/g；
LiFe0.3Co0.3Ni0.3Mn0.1PO4Carbon content be 3.05 weight %, specific surface area is 25.7m2/ g, at 23 DEG C,
(climatic chamber) absorbs water in 37 minutes under 45% relative humidity reaches saturation, and saturated water adsorptive value is 7922ppm, is assembled into
The specific capacity of electric discharge gram first under CR2025 button cell 0.1C charge-discharge magnifications is 129mAh/g.
The specific surface area of phosphate metal lithium salt material is used passes through BET specific surface area detection method (GB/T than Surface Tester
19587-2004) it is measured.
The carbon content of phosphate metal lithium salt material passes through carbon dioxide infrared absorption spectroscopy (YB/ using carbon and sulfur analytical instrument
T5339-2006) it is measured.
The saturated water adsorptive value and absorption speed of phosphate metal lithium salt material pass through karr using karr-Fei Xiu moisture testers
Fischer's method (GB/T 6283-2008) is measured.
The method of testing of gram specific capacity of electric discharge first under CR2025 button cell 0.1C charge-discharge magnifications includes：By button
Battery is with 0.1C electric current constant-current charge to given voltage VL, shelve 5 minutes, then keep VLConstant-voltage charge is until electric current is equal to
0.01C, is shelved 5 minutes, then with 0.1C electric current constant-current discharge to 2.5V；
Wherein, for the Li of carbon coatingxFeaCobNicMndPO4(metallic element can be doped or undoped) material, if a is not
0, b, c, d are all 0, then VL=3.8V；If d is not all 0 for 0, c, b, then VL=4.2V；If b or c are not 0, VL=5.0V.
The preparation method of CR2025 button cells includes：
(1) the phosphate metal lithium salt material for preparing 2.125g the inventive method, 0.25g adhesive HSV900 (methods
State's Ah's Kerma (unit of kinetic energy)) and 0.125g conductive agent Super-P (Switzerland Te Migao) mixing, specific method is：, will be viscous first using NMP as solvent
Mixture dissolves, and is separately added with agitation phosphate metal lithium salt material and conductive agent, and stirring forms uniform slurry after mixing；
The slurry is uniformly poured into glass surface ware, then dried at 100 DEG C, crush, weigh tabletting, diameter is made
For 15.5mm positive plate, wherein the quality of phosphate metal lithium salt material is about 0.068g in positive plate.
(2) assembling of battery
It is positive pole by above-mentioned positive plate, using lithium piece as negative pole, using polypropylene screen as barrier film, is assembled into battery core component, with
Afterwards by LiPF6EC/DMC=1 is dissolved in by the concentration of 1 mol/L:The in the mixed solvent formation nonaqueous electrolytic solution of 1 (volume ratio),
So that barrier film and both positive and negative polarity complete wetting to be defined, then by cell sealing, CR2025 button cells are made in the addition of electrolyte.
Embodiment 1
The present embodiment is used for the processing method for illustrating the phosphate metal lithium salt material of the present invention.
By 100g LiFePO4It is heat-treated in tube-type atmosphere furnace, heat treatment condition includes：Locate under 750 DEG C of constant temperature
Reason 5 hours, atmosphere is 99.99% carbon dioxide, and gas flow is 6L/min, obtains sample A, and be made using sample A
CR2025 button cells.
After measured, the sample A obtained carbon content is 1.02 weight %；Specific surface area is 10.7m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 7 hours under relative humidity reaches saturation, and saturated water adsorptive value is 1835ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, gram specific capacity of discharging first is 159.6mAh/g.
Embodiment 2
The present embodiment is used for the processing method for illustrating the phosphate metal lithium salt material of the present invention.
By 100g LiMnPO4It is heat-treated in tube-type atmosphere furnace, heat treatment condition includes：Locate under 720 DEG C of constant temperature
Reason 2 hours, atmosphere is 99.99% sulfur trioxide (using 60 DEG C of hot nitrogens as carrier gas), and gas flow is 4L/min, obtains sample
Product B, and CR2025 button cells are made using sample B.
After measured, the sample B obtained carbon content is 2.16 weight %；Specific surface area is 16.5m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 1 hour under relative humidity reaches saturation, and saturated water adsorptive value is 5945ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 110.8mAh/g.
Embodiment 3
The present embodiment is used for the processing method for illustrating the phosphate metal lithium salt material of the present invention.
By 100g LiNiPO4It is heat-treated in tube-type atmosphere furnace, heat treatment condition includes：Locate under 700 DEG C of constant temperature
Reason 10 hours, atmosphere is 99.99% carbon dioxide, and gas flow is 10L/min, obtains sample C, and be made using sample C
CR2025 button cells.
After measured, the sample C obtained carbon content is 2.33 weight %；Specific surface area is 18.2m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 55 minutes under relative humidity reaches saturation, and saturated water adsorptive value is 6521ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 114.1mAh/g.
Embodiment 4
According to the method for embodiment 1, unlike, the temperature of heat treatment is 800 DEG C, obtains sample D, and utilize sample D
CR2025 button cells are made.
After measured, the sample D obtained carbon content is 0.64 weight %；Specific surface area is 5.6m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 16 hours under relative humidity reaches saturation, and saturated water adsorptive value is 1059ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 82.5mAh/g.
Embodiment 5
According to the method for embodiment 1, unlike, the temperature of heat treatment is 650 DEG C, obtains sample E, and utilize sample E
CR2025 button cells are made.
After measured, the sample E obtained carbon content is 1.58 weight %；Specific surface area is 15.2m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 1 hour under relative humidity reaches saturation, and saturated water adsorptive value is 6083ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 160.2mAh/g.
Embodiment 6
According to the method for embodiment 1, unlike, the time of heat treatment is 0.5h, obtains sample F, and utilize sample F system
Into CR2025 button cells.
After measured, the carbon content of the sample F obtained is 1.55 weight %；Specific surface area is 15.5m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 1 hour under relative humidity reaches saturation, and saturated water adsorptive value is 6122ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 159.9mAh/g.
Embodiment 7
According to the method for embodiment 1, unlike, the time of heat treatment is 15h, obtains sample G, and utilize sample G systems
Into CR2025 button cells.
After measured, the sample G obtained carbon content is 0.86 weight %；Specific surface area is 7.5m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 12 hours under relative humidity reaches saturation, and saturated water adsorptive value is 1152ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 108.4mAh/g.
Embodiment 8
According to the method for embodiment 1, unlike, phosphate metal lithium salts is the LiCoPO that Mg adulterates4, sample H is obtained, and
CR2025 button cells are made using sample H.
After measured, the sample H obtained carbon content is 2.03 weight %；Specific surface area is 17.7m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 1 hour under relative humidity reaches saturation, and saturated water adsorptive value is 6491ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 115.3mAh/g.
Embodiment 9
According to the method for embodiment 1, unlike, phosphate metal lithium salts is LiFe0.4Mn0.6PO4, obtain sample Q, and profit
CR2025 button cells are made with sample Q.
After measured, the sample Q obtained carbon content is 1.73 weight %；Specific surface area is 14.0m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 2 hours under relative humidity reaches saturation, and saturated water adsorptive value is 4654ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 143.5mAh/g.
Embodiment 10
According to the method for embodiment 1, unlike, phosphate metal lithium salts is LiFe0.4Co0.6PO4, obtain sample X, and profit
CR2025 button cells are made with sample X.
After measured, the sample X obtained carbon content is 1.83 weight %；Specific surface area is 13.6m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 2 hours under relative humidity reaches saturation, and saturated water adsorptive value is 4310ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 127.7mAh/g.
Embodiment 11
According to the method for embodiment 1, unlike, phosphate metal lithium salts is LiFe0.4Co0.3Ni0.3PO4, sample Y is obtained,
And CR2025 button cells are made using sample Y.
After measured, the sample Y obtained carbon content is 2.05 weight %；Specific surface area is 16.4m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 2 hours under relative humidity reaches saturation, and saturated water adsorptive value is 5012ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 124.3mAh/g.
Embodiment 12
According to the method for embodiment 1, unlike, phosphate metal lithium salts is LiFe0.3Co0.3Ni0.3Mn0.1PO4, obtain sample
Product Z, and CR2025 button cells are made using sample Z.
After measured, the sample Z obtained carbon content is 1.97 weight %；Specific surface area is 17.3m2/g；In 23 DEG C, 45%
(climatic chamber) absorbs water in 2 hours under relative humidity reaches saturation, and saturated water adsorptive value is 5341ppm；The CR2025 buttons being made
Under formula battery 0.1C charge-discharge magnifications, its gram specific capacity of discharging first is 128.8mAh/g.
Embodiment 1 is compared with embodiment 4-5 and understood, when the temperature of heat treatment is 700-750 DEG C, material can not caused
In the case of expecting that chemical property substantially deteriorates, specific surface area, saturated absorption amount and the absorption speed of material are further reduced.
Embodiment 1 is compared with embodiment 6-7 and understood, when the time of heat treatment is 2-10h, material electricity can not caused
In the case that chemical property substantially deteriorates, specific surface area, saturated absorption amount and the absorption speed of material are further reduced.
Phosphate metal lithium salt material is handled using the method for the present invention, hardly deteriorates the electric discharge gram specific volume first of material
The chemical properties such as amount, but can substantially reduce specific surface area, saturated water adsorptive value and the absorption speed of material.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (8)
1. a kind of processing method of phosphate metal lithium salt material, it is characterised in that methods described includes：By phosphate metal lithium salts material
Material is heat-treated under weak oxide atmosphere；
Wherein, the condition of the heat treatment includes：Temperature is 700-750 DEG C, and the time is 2-10h；
The phosphate metal lithium salt material is to handle the phosphate metal lithium salt material handled with nanosizing by carbon coating；It is described weak
Oxidizing atmosphere is carbon dioxide atmosphere or sulfur trioxide atmosphere.
2. according to the method described in claim 1, wherein, the weak oxide atmosphere be carbon dioxide atmosphere.
3. according to the method described in claim 1, wherein, the condition of the heat treatment also includes：Gas flow is 1-20L/
min。
4. according to the method described in claim 1, wherein, the condition of the heat treatment also includes：Gas flow is 4-10L/
min。
5. according to the method described in claim 1, wherein, the phosphate metal lithium salts be LixMyPO4Or metal-doped modification
LixMyPO4, in LixMyPO4In, the M is selected from least one of Fe, Mn, Co and Ni, and x is 0.9-1.1, and y is 0.9-1.1.
6. method according to claim 5, wherein, the LixMyPO4For LiFeaCobNicMndPO4, wherein 0≤a, b, c,
D≤1, and 0.95≤a+b+c+d≤1.1.
7. the method according to claim 5 or 6, wherein, LixMyPO4For LiFePO4、LiMnPO4、LiCoPO4、LiNiPO4、
LiFe0.4Mn0.6PO4、LiFe0.4Co0.6PO4、LiFe0.4Co0.3Ni0.3PO4And LiFe0.3Co0.3Ni0.3Mn0.1PO4In at least one
Kind.
8. the phosphate metal lithium salt material that any one methods described is obtained in claim 1-7.
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| CN103274386B (en) * | 2013-05-24 | 2014-11-05 | 厦门大学 | Aperture-controllable porous electrode and preparation method thereof |
| EP2835349A1 (en) * | 2013-08-09 | 2015-02-11 | Basf Se | Process for the preparation of an electrode material and its use in lithium-ion batteries |
| CN105132657A (en) * | 2015-09-29 | 2015-12-09 | 邢台钢铁有限责任公司 | Method for decreasing decarburized layers on surfaces of high-carbon-chromium bearing steel wires |
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Denomination of invention: A treatment method of phosphate metal lithium salt material and phosphate metal lithium salt material obtained by the method Effective date of registration: 20220627 Granted publication date: 20170905 Pledgee: Kaiyang sub branch of Bank of Guiyang Co.,Ltd. Pledgor: GUIZHOU ANDA TECHNOLOGY ENERGY CO.,LTD. Registration number: Y2022980008988 |
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Address after: 550,306 Bai Anying Village, Xicheng Sub district Office, Kaiyang County, Guiyang City, Guizhou Province Patentee after: GUIZHOU ANDA TECHNOLOGY ENERGY CO.,LTD. Address before: 550300 Ping Shang, Chengxi village, Chengguan Town, Kaiyang County, Guiyang City, Guizhou Province Patentee before: GUIZHOU ANDA TECHNOLOGY ENERGY CO.,LTD. |