CN109205588A - The preparation method of ferrousphosphate lithium material - Google Patents
The preparation method of ferrousphosphate lithium material Download PDFInfo
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- CN109205588A CN109205588A CN201811270999.6A CN201811270999A CN109205588A CN 109205588 A CN109205588 A CN 109205588A CN 201811270999 A CN201811270999 A CN 201811270999A CN 109205588 A CN109205588 A CN 109205588A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
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- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The present invention provides a kind of preparation methods of ferrousphosphate lithium material.The preparation method of the ferrousphosphate lithium material is the following steps are included: S1, according to the molar ratio of elemental lithium and P elements be that 1.8~2.2:1 prepares LP；It is that 2~2.2:1 prepares FP according to the molar ratio of ferro element and P elements；S2, it is that 1:1:1 mixes the LP and the FP according to the mass ratio of elemental lithium, ferro element and P elements, obtains LFP mixed powder；S3, it LFP mixed powder is transferred in sand mill is sanded, the D50 of LFP is at 1.2~1.5 μm after control is sanded；S4, the LFP after sand milling is dried, is granulated, and be transferred to sintering preparation in sintering furnace and obtain ferrousphosphate lithium material.The synthesis technology that the preparation method of ferrousphosphate lithium material of the invention passes through each synthesis material in control ferrousphosphate lithium material production process, and synthetic parameters in ferrousphosphate lithium material synthesis process are further controlled, so that the ferrousphosphate lithium material discharge capacity with higher and higher circulating ratio of preparation.
Description
Technical field
The present invention relates to a kind of preparation methods of ferrousphosphate lithium material, belong to cell positive material technical field.
Background technique
Ferrousphosphate lithium material is a kind of anode material for lithium-ion batteries risen 21 century, and theoretical specific capacity can reach
170mAh/g, operating voltage can reach 3V, and cycle life has good safety, while LiFePO 4 up to up to ten thousand times
The material low manufacture cost capability of sustainable development is strong, is widely regarded as optimal power battery anode material.
The method of synthesizing lithium iron phosphate materials has much in the prior art, common are solid phase method, liquid phase method, hydro-thermal
Method, sol-gal process and coprecipitation etc..Wherein, solid phase method mostly uses iron-containing compound, phosphorous compound and containing lithium
Compound be raw material, be sufficiently mixed, grind, be sintered after prepare ferrousphosphate lithium material.
However Mixture drying method is complicated during the preparation process for material in ferrous phosphate in the prior art, causes sintered
The discharge capacity of ferrousphosphate lithium material is low, is unfavorable for promoting the use of in industrial circle.
In view of this, it is necessary to provide a kind of preparation method of ferrousphosphate lithium material, to solve the above problems.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of ferrousphosphate lithium material, use ferrous phosphate of the invention
The ferrousphosphate lithium material circulating ratio with higher of the preparation method preparation of lithium material.
For achieving the above object, the present invention provides a kind of preparation method of ferrousphosphate lithium material, the phosphoric acid
The preparation method of ferrous lithium material the following steps are included:
The preparation of S1, LP and FP: being that 1.8~2.2:1 prepares LP according to the molar ratio of elemental lithium and P elements；According to iron member
The molar ratio of element and P elements is that 2~2.2:1 prepares FP；
The preparation of S2, LFP: the mass ratio according to elemental lithium, ferro element and P elements is 1:1:1 by the LP and the FP
It is mixed, obtains LFP mixed powder；
The sand milling of S3, LFP: LFP mixed powder being transferred in sand mill and is sanded, and the D50 of LFP exists after control is sanded
1.2~1.5 μm；
The sintering of S4, LFP: the LFP after sand milling being dried, is granulated, and is transferred to sintering preparation in sintering furnace and is obtained
Ferrousphosphate lithium material.
As a further improvement of the present invention, the step S1 is specifically included:
The preparation of S11, LP slurry: taking lithium salts to be dissolved in deionized water, prepare elemental lithium mass fraction be 18%~
22% lithium salt solution, and phosphoric acid is added into the lithium salt solution and prepares LP slurry, control elemental lithium and phosphorus member in LP slurry
The molar ratio of element is 1.8~2.2:1；
The drying of S12, LP slurry: the LP slurry in step S11 is dehydrated, dry LP is obtained；
The preparation of S13, FP slurry: taking molysite to be dissolved in deionized water, prepare ferro element mass fraction be 15%~
20% iron salt solutions prepare the phosphate solution that the mass fraction of P elements is 60%~65%, and the phosphate is molten
Liquid is sprayed in the iron salt solutions, prepares FP slurry, and control in FP slurry the molar ratio of ferro element and P elements be 2~
2.2:1；
The drying of S14, FP slurry: the FP slurry in the step S13 is dehydrated, obtain catch up with FP.
As a further improvement of the present invention, the step S2 specifically:
S21, practical LP ratio and practical FP ratio in the LP and the FP are calculated separately, and according to elemental lithium: ferro element:
The mass ratio of P elements is that 1:1:1 weighs LP and FP；
S22, by after weighing LP and FP be transferred in mixing machine and mix, incorporation time control in 30~45min.
As a further improvement of the present invention, the step S3 specifically:
S31, LFP and sanding media are mixed according to the mass ratio of 1:2；
S32, it the material in the step S31 is transferred in sand mill according to the charging rate of 5L/min is sanded,
120min is sanded in circulation；
After 120min is sanded in S33, circulation, every the granularity D50 of 30min measurement LFP, until the granularity D50 of LFP is 1.2
Stop being sanded between~1.5 μm.
As a further improvement of the present invention, in the step S3, the sanding media is second of the concentration 90% or more
Alcohol, the sanding media are that partial size is zirconium oxide bead between 0.15~0.3cm.
As a further improvement of the present invention, the step S4 specifically: the LFP after grinding is transferred to double cone dryer
In be dried, the heating temperature of double cone dryer described in drying process is 90~98 DEG C；The internal pressure of double-cone dryer
Between -0.75~-0.93MPa.
The beneficial effects of the present invention are: the preparation method of ferrousphosphate lithium material of the invention passes through control LiFePO 4
The synthesis technology of each synthesis material in Material Manufacturing Process, and further control and synthesized in ferrousphosphate lithium material synthesis process
Parameter, so that the ferrousphosphate lithium material discharge capacity with higher and higher circulating ratio of preparation.
Detailed description of the invention
Fig. 1 is the process flow chart of ferrousphosphate lithium material synthesis of the present invention.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, right in the following with reference to the drawings and specific embodiments
The present invention is described in detail.
Refering to Figure 1, present invention discloses a kind of preparation method 100 of ferrousphosphate lithium material, LiFePO 4
The preparation method 100 of material the following steps are included:
The preparation of S1, LP and FP: being that 1.8~2.2:1 prepares LP according to the molar ratio of elemental lithium and P elements；According to iron member
The molar ratio of element and P elements is that 2~2.2:1 prepares FP；
The preparation of S2, LFP: the mass ratio according to elemental lithium, ferro element and P elements is 1:1:1 by the LP and the FP
It is mixed, obtains LFP mixed powder；
The sand milling of S3, LFP: LFP mixed powder being transferred in sand mill and is sanded, and the D50 of LFP exists after control is sanded
1.2~1.5 μm；
The sintering of S4, LFP: the LFP after sand milling being dried, is granulated, and is transferred to sintering preparation in sintering furnace and is obtained
Ferrousphosphate lithium material.
Preparation method 100 to the ferrousphosphate lithium material is described in detail for following description part.
The step S1 is specifically included:
The preparation of S11, LP slurry: taking lithium salts to be dissolved in deionized water, prepare elemental lithium mass fraction be 18%~
22% lithium salt solution, and phosphoric acid is added into the lithium salt solution and prepares LP slurry, control elemental lithium and phosphorus member in LP slurry
The molar ratio of element is 1.8~2.2:1；
The drying of S12, LP slurry: the LP slurry in step S11 is dehydrated, dry LP is obtained；
The preparation of S13, FP slurry: taking molysite to be dissolved in deionized water, prepare ferro element mass fraction be 15%~
20% iron salt solutions prepare the phosphate solution that the mass fraction of P elements is 60%~65%, and the phosphate is molten
Liquid is sprayed in the iron salt solutions, prepares FP slurry, and control in FP slurry the molar ratio of ferro element and P elements be 2~
2.2:1；
The drying of S14, FP slurry: the FP slurry in the step S13 is dehydrated, obtain catch up with FP.
In the step S11, the dissolution of the lithium salts carries out in a kettle, in the course of dissolution of the lithium salts,
Solvent is deionized water of the temperature between 38~42 DEG C, the solution rate that can effectively ensure that the lithium salts is arranged such, simultaneously
Prevent lithium salts from change of properties occurring at high operating temperatures.Further, in the present invention, the lithium salts is monohydrate lithium hydroxide,
And the mass fraction of elemental lithium is 18%~22% in lithium salt solution after dissolving.
The phosphoric acid solution is that concentrated phosphoric acid is prepared through dilution, in the present invention, the mass fraction of the phosphoric acid solution
It is 18%~23%.Further, the step S11 further includes that the phosphoric acid solution is sprayed in the lithium salt solution, with
The LP slurry is prepared, specifically, phosphoric acid solution is added into the lithium salt solution by the way of spray, it is ensured that phosphoric acid
Solution contacts uniformly with the lithium salt solution, guarantees that rapid reaction effectively carries out, and elemental lithium and phosphorus member in the LP slurry
The molar ratio of element is 1.8~2.2:1.
It further include adding additive into the LP slurry in the step S11, in the present invention, the additive
For phosphor-included additive, further, in the present invention the additional amount of the additive be the lithium salts quality 0.55%~
0.7%, it is preferred that in one embodiment of the invention, the usage amount of the additive is the 0.6% of the lithium salts quality,
Continue to stir 30~45min of the LP slurry after to additive addition, until the phosphoric acid solution, the lithium salts original are molten
Liquid and the additive sufficiently react, and the preparation of the LP slurry terminates.
The step S12 is specially to dehydrate the LP slurry in step S11, obtains dry LP；The step
In rapid S12, the dehydration of the LP slurry is carried out by band filter, and the operating rate of the band filter is 1m/min,
Further, in the dehydration of the LP slurry, the discharge velocity of the LP slurry should be controlled constantly, to guarantee the LP
Slurry considers the thickness taken in band filter and is no more than 1.5cm, while in the dehydration of the LP slurry, can pass through institute
It states band filter to wash the LP slurry, to remove free phosphate radical remaining in LP slurry.
Dewatered LP slurry, which is transferred in dry bipyramid, to be dried, and is controlled in drying process true in the dry bipyramid
Reciprocal of duty cycle is between -0.09~-0.098MPa, and the temperature for adjusting the dry bipyramid is at 92 DEG C or more, continues drying out 12h to double
Vacuum degree is not changing in cone, stops drying, naturally cools to 25 DEG C with bottom discharge, the drying of the LP slurry terminates.
In the step S13, the preparation of the FP slurry specifically: dissolve molysite in a kettle, the iron
When salt dissolves, deionized water should be transferred in reaction kettle first, molysite is then transferred to the reaction kettle equipped with deionized water
In, and open reaction kettle and be stirred continuously, until molysite is completely dissolved, iron salt solutions are made, the matter of ferro element in the iron salt solutions
Measuring score is 15%~20%.
It should be noted that in one embodiment of the invention, the molysite is green vitriol, ferrous oxalate
Or any one of di-iron trioxide, it is preferred that the molysite is green vitriol in one embodiment of the invention,
And the temperature of the deionized water is 35~37 DEG C.
The phosphatic dissolution also carries out in a kettle, further, molten to phosphate progress using reaction kettle
Deionized water need to be transferred in reaction kettle by Xie Shi first, then the phosphate transfection is moved in reaction kettle be stirred it is molten
Solution, with preparing phosphoric acid salting liquid, specifically, the mass fraction of P elements is 60% in the phosphate solution in the present invention
~65%；Simultaneously in the phosphatic course of dissolution, the temperature of the deionized water should be controlled at 35~40 DEG C, preferably
, in the present invention, the temperature of the deionized water is 37 DEG C, and in one embodiment of the invention, the phosphate tool
Body is diammonium hydrogen phosphate.
In the step S13, the phosphate solution prepared in the step S12 is sprayed in the iron salt solutions,
To produce iron salt solutions；In this process, reaction kettle should be used constantly to be stirred to the iron salt solutions, to prevent the phosphorus
When acid salt solution is reacted in being sprayed to the iron salt solutions, the local concentration of phosphate solution is excessively high, then causes FP
The resulting anomaly of slurry.
Further, after phosphate spray, continue after stirring 15~30min of the molysite slurry, to the molysite
Antioxidant is added in slurry, the additional amount of the antioxidant is the 0.3%~0.4% of the molysite quality, preferably in this hair
In bright, the antioxidant is ascorbic acid, and the additional amount of the ascorbic acid is the 0.36% of molysite quality.
After the ascorbic acid is added, the pH value of the molysite slurry need to be adjusted, in the present invention, the pH tune
Section agent is ammonium hydroxide, and further, the ammonium hydroxide is mixed by the way of spray with the molysite slurry in the present invention, is had
For body, the concentration of the ammonium hydroxide is 3% in the present invention, specifically, in being carried out using ammonium hydroxide to the molysite slurry
And when, when the pH value of the molysite slurry reaches 6.5 or more, reduce the spray flow of the ammonium hydroxide, it is preferred that of the invention
In one embodiment, the spray rate of the ammonium hydroxide can be controlled by adding solenoid valve in the pipeline of ammonia spray.To
When the pH of the molysite slurry reaches 7, stop spraying ammonium hydroxide into the molysite slurry, continues to stir 30min, molysite slurry
PH value is constant, then antioxidant is added into the FP mixed liquor in FP slurry antioxidant, and adjusts the pH value of the FP mixed liquor
It is 7, the preparation of the FP slurry terminates.
The step S14 is mainly the drying of FP slurry, and the drying of FP slurry in the present invention mainly includes dehydration and does
Dry two steps, the dehydration of the FP slurry are main are as follows: and the FP slurry is put into centrifuge and is dehydrated, centrifugal dehydration process
In, when the water of leakage fluid dram position in centrifuge is not under plume, the FP slurry is washed using deionized water, is repeated
Three times, the washing dehydration of FP slurry terminates for washing, and the amount that can effectively reduce the phosphate radical to dissociate in FP slurry is arranged such, and guarantees
The stability of subsequent LFP preparation.
Further, the step S14 further includes that dewatered FP slurry is transferred in dry double cone dryer to carry out
It is dry；The FP slurry when being dried using double cone dryer, control the double cone dryer internal temperature be 105 ±
5℃；Further, vacuumize process should be carried out constantly in the drying process so that the pressure in the double cone dryer-
Between 0.07~-0.1MPa, after the dry 10h of bipyramid, continues to be evacuated to -0.09MPa and continue drying, if bipyramid is dry in 30min
The dry of the unchanged then FP slurry of pressure in dry machine is completed, and is continued to guarantee that the pressure in double cone dryer is constant at this time, be stopped
Heating, until discharging when the temperature in double cone dryer drops to 25 DEG C or less, with the FP of acquisition.
The step S2 specifically:
S21, practical lithium phosphorus ratio and actual iron phosphorus ratio in the LP and the FP are calculated separately, and according to elemental lithium: iron
Element: the mass ratio of P elements is that 1:1:1 weighs LP and FP；
S22, by after weighing LP and FP be transferred in mixing machine and mix, incorporation time control in 30~45min.
In the step S22, to guarantee that the FP and LP is uniformly mixed, the mixed process in batch mixer into
Row, and after the FP and the LP are fed into the batch mixer, it should continue to stir 45min~120min, to guarantee batch mixer
In FP and LP be uniformly mixed, finally to obtain LFP.
The step S3 specifically:
S31, LFP and sanding media are mixed according to the mass ratio of 1:2；
S32, it the material in the step S31 is transferred in sand mill according to the charging rate of 5L/min is sanded,
120min is sanded in circulation；
After 120min is sanded in S33, circulation, every the granularity D50 of 30min measurement LFP, until the granularity D50 of LFP is 1.2
Stop being sanded between~1.5 μm.
In the step S3, abrasive media is added in sand mill first, and opens sand mill operation preheating, further
, it is zirconium oxide bead between 0.15~0.3cm that the abrasive media, which is partial size, in the present invention.Then, according to the quality of 1:2
Than mixing LFP with sanding media, the sanding media is ethyl alcohol of the concentration 90% or more in the present invention；Finally,
Mixed LFP and sanding media are transferred in sand mill and are sanded；Need to illustrate when, in the present invention, the sand
The charging rate of grinding machine is 5L/min, further, after 120min is sanded in the LFP and sanding media mixed material circulation,
Every the granularity D50 of 30min measurement LFP, until the granularity D50 of LFP stops being sanded between 1.2~1.5 μm.
The step S4 is the sintering of LFP, in the step S4, carries out bipyramid drying to the LFP in S3 first, dry
The heating temperature of the double cone dryer is 90~98 DEG C in the process；The internal pressure of double-cone dryer -0.75~-
Between 0.93MPa, then, the LFP after drying is granulated, the LFP material after granulation is transferred to sintering after granulation
It is sintered in furnace, should continue to be passed through inert gas into the sintering equipment in sintering process, such as argon gas, nitrogen, further,
The sintering equipment is pipe type sintering furnace in the present invention, and the heating rate of the pipe type sintering furnace is 5 DEG C/min, and described
The sintering temperature of LFP is to keep the temperature cooled to room temperature after 7.5h, it should be noted that in cooling from room temperature to 800 DEG C
During should be always ensured that the sintering of the pipe type sintering furnace is intracavitary full of inert gas, to prevent the LiFePO 4 material
Material is oxidized in temperature-fall period.
It please join the material property table that table 1 is ferrousphosphate lithium material prepared by the present invention.
| Granularity (D50) μm | 1.25~2.75 |
| Specific capacity mAh/g | 155~160 |
| Specific surface area m2/g | 13~15 |
| Tap density g/cm3 | 1.7~1.8 |
| 1C discharge capacity mAh/g | 155~163 |
Table 1: ferrousphosphate lithium material performance table
In conclusion the preparation method 100 of ferrousphosphate lithium material of the invention is raw by control ferrousphosphate lithium material
The synthesis technology of each synthesis material during production, and synthetic parameters in ferrousphosphate lithium material synthesis process are further controlled,
So that the ferrousphosphate lithium material discharge capacity with higher and higher circulating ratio of preparation, then make the present invention
The ferrousphosphate lithium material for preparing of preparation method 100 of the ferrousphosphate lithium material there is stronger usability, be suitable for dynamic
Use in power battery.
The above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferred embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that, it can modify to technical solution of the present invention
Or equivalent replacement, without departing from the spirit and scope of the technical solution of the present invention.
Claims (6)
1. a kind of preparation method of ferrousphosphate lithium material, which comprises the following steps:
The preparation of S1, LP and FP: being that 1.8~2.2:1 prepares LP according to the molar ratio of elemental lithium and P elements；According to ferro element with
The molar ratio of P elements is that 2~2.2:1 prepares FP；
The preparation of S2, LFP: the mass ratio according to elemental lithium, ferro element and P elements is that 1:1:1 carries out the LP and FP
Mixing obtains LFP mixed powder；
The sand milling of S3, LFP: LFP mixed powder being transferred in sand mill and is sanded, and the D50 of LFP is 1.2 after control is sanded
~1.5 μm；
The sintering of S4, LFP: the LFP after sand milling being dried, is granulated, and is transferred to sintering preparation in sintering furnace and is obtained phosphoric acid
Ferrous lithium material.
2. the preparation method of ferrousphosphate lithium material according to claim 1, which is characterized in that the step S1 is specifically wrapped
It includes:
The preparation of S11, LP slurry: taking lithium salts to be dissolved in deionized water, and the mass fraction for preparing elemental lithium is 18%~22%
Lithium salt solution, and phosphoric acid is added into the lithium salt solution and prepares LP slurry controls rubbing for elemental lithium and P elements in LP slurry
You are than being 1.8~2.2:1；
The drying of S12, LP slurry: the LP slurry in step S11 is dehydrated, dry LP is obtained；
The preparation of S13, FP slurry: taking molysite to be dissolved in deionized water, and the mass fraction for preparing ferro element is 15%~20%
Iron salt solutions, the mass fraction for preparing P elements is 60%~65% phosphate solution, and the phosphate solution is sprayed
To in the iron salt solutions, FP slurry is prepared, and controlling the molar ratio of ferro element and P elements in FP slurry is 2~2.2:1；
The drying of S14, FP slurry: the FP slurry in the step S13 is dehydrated, obtain catch up with FP.
3. the preparation method of ferrousphosphate lithium material according to claim 1, it is characterised in that: the step S2 is specific
Are as follows:
S21, practical LP ratio and practical FP ratio in the LP and the FP are calculated separately, and according to elemental lithium: ferro element: phosphorus member
The mass ratio of element is that 1:1:1 weighs LP and FP；
S22, by after weighing LP and FP be transferred in mixing machine and mix, incorporation time control in 30~45min.
4. the preparation method of ferrousphosphate lithium material according to claim 1, it is characterised in that: the step S3 is specific
Are as follows:
S31, LFP and sanding media are mixed according to the mass ratio of 1:2；
S32, it the material in the step S31 is transferred in sand mill according to the charging rate of 5L/min is sanded, recycle
120min is sanded；
After 120min is sanded in S33, circulation, every the granularity D50 of 30min measurement LFP, until the granularity D50 of LFP is 1.2~1.5
Stop being sanded between μm.
5. the preparation method of ferrousphosphate lithium material according to claim 4, it is characterised in that: in the step S3, institute
Stating sanding media is ethyl alcohol of the concentration 90% or more, and the sanding media is that partial size is zirconium oxide between 0.15~0.3cm
Pearl.
6. the preparation method of ferrousphosphate lithium material according to claim 1, it is characterised in that: the step S4 is specific
Are as follows: the LFP after grinding is transferred in double cone dryer and is dried, the heating temperature of double cone dryer described in drying process
It is 90~98 DEG C；The internal pressure of double-cone dryer is between -0.75~-0.93MPa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101645504A (en) * | 2008-08-07 | 2010-02-10 | 赵兵 | Method for preparing lithium iron phosphate of anode material of lithium ion battery |
| CN102491303A (en) * | 2011-11-14 | 2012-06-13 | 日照华轩新能源有限公司 | Method for preparing lithium ion phosphate, cathode material of lithium ion battery |
| JP2015195163A (en) * | 2013-09-25 | 2015-11-05 | 国立大学法人 東京大学 | nonaqueous secondary battery |
-
2018
- 2018-10-29 CN CN201811270999.6A patent/CN109205588A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101645504A (en) * | 2008-08-07 | 2010-02-10 | 赵兵 | Method for preparing lithium iron phosphate of anode material of lithium ion battery |
| CN102491303A (en) * | 2011-11-14 | 2012-06-13 | 日照华轩新能源有限公司 | Method for preparing lithium ion phosphate, cathode material of lithium ion battery |
| JP2015195163A (en) * | 2013-09-25 | 2015-11-05 | 国立大学法人 東京大学 | nonaqueous secondary battery |
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