CN104900877A - Preparing method for LiFexMn(1-x)PO4/C for lithium-ion batteries - Google Patents
Preparing method for LiFexMn(1-x)PO4/C for lithium-ion batteries Download PDFInfo
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- CN104900877A CN104900877A CN201510319010.6A CN201510319010A CN104900877A CN 104900877 A CN104900877 A CN 104900877A CN 201510319010 A CN201510319010 A CN 201510319010A CN 104900877 A CN104900877 A CN 104900877A
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- aqueous solution
- lithium
- preparation
- raw material
- reaction
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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
- H01M4/5805—Phosphides
-
- 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
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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
-
- 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 provides a preparing method for LiFexMn(1-x)PO4/C. The method includes the following steps: 1), preparing raw materials including Li<+>, Fe<3+> and PO4<3-> into water solutions respectively; 2), using a metering pump to inject the water solutions obtained in the step (1) into a normal pressure reaction still for reaction, filtering and collecting a solid matter I after the reaction is completed, washing and drying to obtain a precursor; 3), performing solvent thermal reaction between the precursor and the raw material including Mn<2+>, collecting a solid matter II after the reaction is completed, washing and drying to obtain an intermediate product; 4), cladding the intermediate product by an organic matter, and at the same time, adding a lithium compound, and performing thermal treatment at a protective atmosphere to obtain a primary product, wherein the organic matter is glucose, cane sugar, starch or cellulose; 5), smashing and sieving the primary product to obtain the LiFexMn(1-x)PO4/C. The product prepared through adopting the method is excellent in performance and outstanding in cycling stability.
Description
Technical field
The present invention relates to anode material for lithium ion battery field, particularly relate to a kind of preparation method of lithium-ion-power cell high-performance lithium manganese phosphate material.
Background technology
Lithium ion battery is the secondary cell that a kind of energy density is high, power density is high, the life-span is long, plays an important role in modern society.In the mini-plant such as mobile phone, notebook computer, lithium ion battery applications is very extensive.Meanwhile, along with the fast development of the industry such as electric automobile, intelligent grid, the demand of lithium-ion-power cell sharply rises, and day by day improves its performance requirement.The positive electrode be applied in lithium ion battery is the deciding factor of its performance and cost.As anode material for lithium-ion batteries, lithium manganese phosphate has the advantages such as operating voltage is high, electric discharge is steady, cost is low, fail safe is good, is highly suitable for lithium ion power system.Lithium manganese phosphate material is applied to lithium-ion-power cell, will the energy density of battery system be made to obtain larger raising, and amount of monomer of connecting under identical group of output voltage reduces, and contributes to the reliability improving battery pack.
The key issue that the poorly conductive of lithium manganese phosphate need solve when being its application.Meanwhile, the oxidation state common due to manganese element is more, and in lithium manganese phosphate building-up process, the oxidation state of manganese element easily changes and makes material impure, degradation.Though lithium manganese phosphate material is closely similar with LiFePO4 structure, its preparation method and LiFePO4 have relatively big difference, and the some factors affecting this material property is also that it is distinctive.Conductive agent is coated, element doping and reduction primary particle particle diameter are the main method improving conductivity.Preparation method aspect, high temperature solid-state method and solvent-thermal method are conventional methods.But the performance of the lithium manganese phosphate material that existing method obtains can not be fully up to expectations.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of lithium-ion-power cell LiFe
xmn
1-xpO
4the preparation method of/C, the LiFe that the method is obtained
xmn
1-xpO
4/ C excellent performance, cyclical stability is given prominence to.
For this reason, technical scheme of the present invention is as follows:
A kind of LiFe
xmn
1-xpO
4the preparation method of/C, comprises the steps:
1) will containing Li
+, Fe
3+, PO
4 3-raw material be mixed with the aqueous solution respectively;
2) with measuring pump by step 1) aqueous solution that obtains injects normal-pressure reaction kettle and reacts; After having reacted, collecting by filtration solid content I, then washs it, dry, obtains presoma;
3) by described presoma and containing Mn
2+raw material carry out solvent thermal reaction, after question response completes, collect solid content II, then it washed, dry, obtain intermediate products;
4) carry out coated with organic substance to described intermediate products, add lithium-containing compound simultaneously, heat-treat under protective atmosphere, obtain Primary product; Described organic substance is glucose, sucrose, starch or cellulose;
5) described Primary product is carried out pulverize, sieve, obtain described LiFe
xmn
1-xpO
4/ C.
Step 2) solution remembers wherein Li respectively in normal-pressure reaction kettle
+, Fe
3+, PO
4 3-amount of substance be n
1, n
2, n
3, meet
and n
2: n
3=(0.005 ~ 0.5): 1.
Step 1) in containing Li
+, Fe
3+raw material be soluble-salt or hydroxide; Containing PO
4 3-raw material be phosphoric acid or soluble phosphate.
Described containing Li
+raw material be lithium hydroxide or lithium acetate; Containing Fe
3+raw material be ferric trichloride, ferric sulfate or ferric nitrate; Described soluble phosphate is ammonium phosphate, ammonium dihydrogen phosphate or lithium dihydrogen phosphate.
Step 2) in the aqueous solution to inject the mode of normal-pressure reaction kettle be one of following five kinds of modes:
A) at injection PO
4 3-in the process of the aqueous solution, alter least-squares Fe simultaneously
3+the aqueous solution and Li
+the aqueous solution, Fe
3+the aqueous solution first adds, until PO
4 3-the aqueous solution has injected; Or
B) at injection PO
4 3-in the process of the aqueous solution, alter least-squares Li simultaneously
+the aqueous solution and Fe
3+the aqueous solution, Li
+the aqueous solution first adds, until PO
4 3-the aqueous solution has injected; Or
C) at injection PO
4 3-in the process of the aqueous solution, the Li simultaneously slowly injected
+the aqueous solution, then slowly injects Fe
3+the aqueous solution, until PO
4 3-the aqueous solution has injected; Or
D) at injection PO
4 3-in the process of the aqueous solution, the Fe simultaneously slowly injected
3+the aqueous solution, then slowly injects Li
+the aqueous solution, until PO
4 3-the aqueous solution has injected; Or
E) inject 3 kinds of aqueous solution simultaneously.
Described step 3) reaction medium of solvent thermal reaction is the mixture of any one and water in the polyethylene glycol of ethylene glycol, glycerol and the degree of polymerization >=2.
Described step 3) in containing Mn
2+raw material be Mn
2+soluble salt, can be specifically manganese sulfate, manganese chloride or manganese acetate.
Described step 3) in containing Mn
2+the addition of raw material and presoma in Fe
3+, PO
4 3-the pass of content is: n (Mn
2+)=n (PO
4 3-) – n (Fe
3+).
Described step 3) condition of solvent thermal reaction is 100 ~ 200 DEG C, the reaction time is 2 ~ 24h.
Described step 4) organic quality is 10 ~ 50% of intermediate products quality.
Described step 4) lithium-containing compound is labile lithium salts, oxide or hydroxide, its addition ensures Li
+amount of substance be 1.05 times of ferro element amount of substance, that is: addition n (Li)=1.05*n (Fe).
Described lithium-containing compound is lithium carbonate, lithium acetate, lithium nitrate, lithia or oxygen lithium hydride.
Described step 4) protective atmosphere is argon gas or nitrogen.
Described step 4) heat treated temperature is 400 ~ 600 DEG C, heat treatment time is 0.5 ~ 5h.
The invention has the beneficial effects as follows: adopt crystallization control legal system for presoma, modify with ferro element to presoma, then adopt solvent-thermal method to prepare lithium manganese phosphate, carbon is coated obtains final products finally to adopt organic precursor pyrolysis to carry out lithium manganese phosphate.Lithium manganese phosphate material excellent performance prepared by the method, cyclical stability is given prominence to.The method, from aspects such as size controlling, doping and preparation flows, improves apparent electronics and the ionic conductivity of material, improves the performance of material.
Accompanying drawing explanation
Fig. 1 is LiFe provided by the invention
xmn
1-xpO
4the process chart of the preparation method of/C;
Fig. 2 is step 2) aqueous solution feed postition figure;
Fig. 3 is the different schematic cross-sections injecting the presoma primary particle that standard obtains.
Embodiment
The present invention adopts crystallization control legal system for presoma, presoma ferro element is modified, standard is added by setting different raw materials, control position and the effect of ferro element, reach induction presoma nucleation, doping, the effect such as coated, the particle diameter of presoma can be controlled simultaneously, and then control the particle diameter of end product primary particle.This presoma mixes with manganese salt, adopts solvent-thermal method to prepare lithium manganese phosphate, and carbon is coated obtains final products finally to adopt organic matter pyrolysis to carry out lithium manganese phosphate.The lithium manganese phosphate material excellent performance that the method is obtained, cyclical stability is given prominence to.0.1C specific discharge capacity can reach 150mAhg
-1, 100 times circulation volume conservation rate is greater than 98%.Fig. 2 gives containing Li
+, Fe
3+, PO
4 3-the different feed postition of the aqueous solution, Fig. 3 gives the schematic cross-section of the presoma primary particle that different feed postition in Fig. 2 obtains, and as seen from the figure, the pattern of different dosing methods on presoma has vital impact.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in detail.
Embodiment 1
Prepare the following aqueous solution: 3.0moldm
-3liOH solution, 1.0moldm
-3h
3pO
4solution, 1.0moldm
-3fe (NO
3)
3solution.Add liquid at the bottom of appropriate amount of deionized water (not having the minimum paddle of reactor) in a kettle., temperature sets 35 DEG C.Adopt Fig. 2 method 4) add reactant.H
3pO
4solution charge velocity is set as 1.0dm
3min
-1, inject 30dm altogether
3; LiOH solution charge velocity is set as 1.0dm
3min
-1, with H
3pO
4solution starts to inject simultaneously, injects 28dm altogether
3; After LiOH solution has been annotated, with 1.0dm
3min
-1speed inject Fe (NO
3)
3solution, injects 3dm altogether
3.After reactant has added, precipitation 30min, filters, spends deionized water and precipitate 5 times, dries and obtains presoma.Measure the phosphorus element content in this presoma and iron content, mix with moderate amount of sulfuric acid manganese, make n (Mn
2+)=n (PO
4 3-) – n (Fe
3+) obtain mixture.Add the glycerin solution (volume ratio of glycerol and water is 1:1) that quality is this mixture quality 3 times, fully mix, carry out the solvent thermal reaction of 4h at 190 DEG C.Filter, spend deionized water and precipitate 4 times, wash 1 time with ethanol, drying is intermediate products.Get glucose that quality is this intermediate products quality 1/4 and intermediate products mixing and ball milling obtains the reactant after mixing; the amount of lithium hydroxide meets n (Li)=1.05*n (Fe); by this reactant heat treatment 5h under 450 DEG C of nitrogen protections, obtain Primary product.This Primary product is carried out pulverize, sieve, obtain target product.
The product 0.1C specific discharge capacity that the present embodiment obtains reaches 150mAhg
-1, 1C specific discharge capacity reaches 130mAhg
-1.
Embodiment 2
Prepare the following aqueous solution: 2.5moldm
-3liOH solution, 1.0moldm
-3h
3pO
4solution, 0.2moldm
-3fe
2(SO
4)
3solution.Add liquid at the bottom of appropriate amount of deionized water (not having the minimum paddle of reactor) in a kettle., temperature sets 40 DEG C.Fig. 2 standard 5 is adopted to add reactant.LiOH solution and H
3pO
4solution charge velocity is set as 1.0dm
3min
-1, Fe
2(SO
4)
3solution charge velocity is set as 0.5dm
3min
-1, start filling simultaneously.Reactant adds 30min altogether, precipitation 20min.Filter, spend deionized water and precipitate 5 times, dry and obtain presoma.Measure phosphorus element content and the iron content of this presoma, mix with moderate amount of sulfuric acid manganese, make n (Mn
2+)=n (PO
4 3-) – n (Fe
3+).Add the vinyl alcohol aqueous solution (volume ratio of ethylene glycol and water is 2:1) of this mixture quality 2.5 times, fully after mixing, carry out 24h solvent thermal reaction at 120 DEG C.Filter, spend deionized water and precipitate 3 times, wash 2 times with ethanol, dry intermediate products.Be the reactant that the sucrose of intermediate products quality 30% and intermediate products and lithium acetate mixing and ball milling obtain mixing by quality; the amount of lithium acetate meets n (Li)=1.05*n (Fe), by this reactant heat treatment 3h under 550 DEG C of argon shields.Finally carry out pulverizing, sieving, obtain target product.
The product 0.1C specific discharge capacity of the present embodiment reaches 155mAhg
-1, 1C specific discharge capacity reaches 135mAhg
-1.
Embodiment 3
Prepare the following aqueous solution: 3.2moldm
-3liOH solution, 1.0moldm
-3h
3pO
4solution, 1.0moldm
-3feCl
3solution.Add liquid at the bottom of appropriate amount of deionized water (not having the minimum paddle of reactor) in a kettle., temperature sets 35 DEG C.Fig. 2 standard 2 is adopted to add reactant.H
3pO
4solution charge velocity is set as 1.0dm
3min
-1, inject 30dm altogether
3; LiOH solution and FeCl
3solution charge velocity is set as 1.0dm
3min
-1, with H
3pO
4solution starts to inject simultaneously, and first annotate LiOH solution 6min, and then annotate FeCl
3solution 4min, said process carries out 3 times altogether.After reactant has added, precipitation 30min.Filter, spend deionized water and precipitate 5 times, dry and obtain presoma.Measure phosphorus element content and the iron content of presoma, be mixed to get mixture with moderate amount of sulfuric acid manganese, make n (Mn
2+)=n (PO
4 3-) – n (Fe
3+).Add the PEG400 aqueous solution (volume ratio of PEG400 and water is 1:1) of this mixture quality 2 times, fully after mixing, carry out 10h solvent thermal reaction at 160 DEG C.Filter, spend deionized water and precipitate 4 times, wash 1 time with ethanol, dry intermediate products.Be that the starch of intermediate products quality 1/4 and intermediate products and lithium carbonate mixing and ball milling obtain the reactant after mixing by quality; the amount of lithium carbonate meets n (Li)=1.05*n (Fe); by this reactant heat treatment 2h under 600 DEG C of argon shields, obtain Primary product.This Primary product is carried out pulverize, sieve, obtain target product.
The product 0.1C specific discharge capacity of the present embodiment reaches 155mAhg
-1, 1C specific discharge capacity reaches 138 mAhg
-1.
Claims (10)
1. a LiFe
xmn
1-xpO
4the preparation method of/C, is characterized in that comprising the steps:
1) will containing Li
+, Fe
3+, PO
4 3-raw material be mixed with the aqueous solution respectively;
2) with measuring pump by step 1) aqueous solution that obtains injects normal-pressure reaction kettle and reacts; After having reacted, collecting by filtration solid content I, then washs it, dry, obtains presoma;
3) by described presoma and containing Mn
2+raw material carry out solvent thermal reaction, after question response completes, collect solid content II, then it washed, dry, obtain intermediate products;
4) carry out coated with organic substance to described intermediate products, add lithium-containing compound simultaneously, heat-treat under protective atmosphere, obtain Primary product; Described organic substance is glucose, sucrose, starch or cellulose;
5) described Primary product is carried out pulverize, sieve, obtain described LiFe
xmn
1-xpO
4/ C.
2. preparation method as claimed in claim 1, is characterized in that: step 2) solution remembers wherein Li respectively in normal-pressure reaction kettle
+, Fe
3+, PO
4 3-amount of substance be n
1, n
2, n
3, meet
and n
2: n
3=(0.005 ~ 0.5): 1.
3. preparation method as claimed in claim 1, is characterized in that: step 1) in containing Li
+, Fe
3+raw material be soluble-salt or hydroxide; Containing PO
4 3-raw material be phosphoric acid or soluble phosphate, preferably described containing Li
+raw material be lithium hydroxide or lithium acetate; Containing Fe
3+raw material be ferric trichloride, ferric sulfate or ferric nitrate; Described soluble phosphate is ammonium phosphate, ammonium dihydrogen phosphate or lithium dihydrogen phosphate.
4. preparation method as claimed in claim 1, is characterized in that: step 2) in the aqueous solution mode of injecting normal-pressure reaction kettle be one of following five kinds of modes:
A) at injection PO
4 3-in the process of the aqueous solution, alter least-squares Fe simultaneously
3+the aqueous solution and Li
+the aqueous solution, Fe
3+the aqueous solution first adds, until PO
4 3-the aqueous solution has injected; Or
B) at injection PO
4 3-in the process of the aqueous solution, alter least-squares Li simultaneously
+the aqueous solution and Fe
3+the aqueous solution, Li
+the aqueous solution first adds, until PO
4 3-the aqueous solution has injected; Or
C) at injection PO
4 3-in the process of the aqueous solution, the Li simultaneously slowly injected
+the aqueous solution, then slowly injects Fe
3+the aqueous solution, until PO
4 3-the aqueous solution has injected; Or
D) at injection PO
4 3-in the process of the aqueous solution, the Fe simultaneously slowly injected
3+the aqueous solution, then slowly injects Li
+the aqueous solution, until PO
4 3-the aqueous solution has injected; Or
E) inject 3 kinds of aqueous solution simultaneously.
5. preparation method as claimed in claim 1, is characterized in that: described step 3) reaction medium of solvent thermal reaction is the mixture of any one and water in the polyethylene glycol of ethylene glycol, glycerol and the degree of polymerization >=2.
6. preparation method as claimed in claim 1, is characterized in that: described step 3) in containing Mn
2+raw material be Mn
2+soluble salt, preferably sulfuric acid manganese, manganese chloride or manganese acetate.
7. preparation method as claimed in claim 1, is characterized in that: described step 3) in containing Mn
2+the addition of raw material and presoma in Fe
3+, PO
4 3-the pass of content is: n (Mn
2+)=n (PO
4 3-) – n (Fe
3+).
8. preparation method as claimed in claim 1, is characterized in that: described step 4) lithium-containing compound is labile lithium salts, oxide or hydroxide, its addition ensures Li
+amount of substance be 1.05 times of ferro element amount of substance, that is: addition n (Li)=1.05*n (Fe); Preferred described lithium-containing compound is lithium carbonate, lithium acetate, lithium nitrate, lithia or oxygen lithium hydride.
9. preparation method as claimed in claim 1, is characterized in that: described step 3) condition of solvent thermal reaction is 100 ~ 200 DEG C, the reaction time is 2 ~ 24h.
10. preparation method as claimed in claim 1, is characterized in that: described step 4) organic quality is 10 ~ 50% of intermediate products quality.
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|---|---|---|---|
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ID=54033394
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|---|---|---|---|---|
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| CN103700855A (en) * | 2013-12-12 | 2014-04-02 | 天津巴莫科技股份有限公司 | Preparation method of high-performance lithium manganese phosphate material for lithium-ion power batteries |
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| CN104577114A (en) * | 2014-12-23 | 2015-04-29 | 山东精工电子科技有限公司 | Lithium ion battery positive electrode material lithium iron manganese phosphate and liquid phase preparation method thereof |
-
2015
- 2015-06-09 CN CN201510319010.6A patent/CN104900877A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101673819A (en) * | 2009-09-25 | 2010-03-17 | 清华大学 | Method for preparing manganese lithium phosphate/carbon composite material by manganese phosphate |
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