CN107572495A - The technique that a kind of homogeneous grain diameter combination mechanical alloying prepares LiFePO4 - Google Patents
The technique that a kind of homogeneous grain diameter combination mechanical alloying prepares LiFePO4 Download PDFInfo
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- CN107572495A CN107572495A CN201710809405.3A CN201710809405A CN107572495A CN 107572495 A CN107572495 A CN 107572495A CN 201710809405 A CN201710809405 A CN 201710809405A CN 107572495 A CN107572495 A CN 107572495A
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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
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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
A kind of homogeneous grain diameter combination mechanical alloying prepares the technique of LiFePO4, it is characterized in that, comprise the following steps：1) wet ball grinding：Various raw materials are blended in, ball milling 35 hours in ball mill by wet process, after ball milling raw material particle size control in 100 mesh, raw material Fe, Li, PO43, dispersant, talcum powder and mix element mol ratio be 1: 1: 1: 0.01 0.015: 2: 0.005 0.007；2) dry：By the raw material drying after ball milling；3) pre-burning：By dried raw material at 300 400 DEG C pre-burning 46 hours；4) dry ball milling：1 2wt% starch, dry ball milling to 300 mesh are added into above-mentioned raw materials；5) high temperature sintering：Sintered 8 hours at being 650 700 DEG C in temperature；6) LiFePO4 finished product is crushed to obtain.The technique of the present invention is suitable for industrial-scale preparation, and product cut size is homogeneous, conducts electricity very well.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, specifically a kind of liquid phase cocrystallization granularity is equal
One technique for preparing LiFePO4 with reference to mechanical alloying.
Background technology
LiFePO4 (the LiFePO of crystallographic system olivine-type4) material is due to high, cheap, dirty without environment with specific capacity
Dye, the advantages that security and heat endurance are good and turn into a kind of most potential lithium-ion-power cell material.
In the prior art, the method for synthesizing iron lithium phosphate mainly has：Solid phase method, hydrothermal synthesis method, sol-gel process, water
Phase co-electrodeposition method etc..
Solid phase method is more in a kind of synthetic method of the LiFePO 4 powder used earliest, and first stage commercial Application
The method of use.Its equipment, technique are simple, are industrialized beneficial to realizing, its weak point is：Product grain is big, and thing is mutually uneven,
Calcination time is grown, and crystal shape is irregular, and particle size distribution range is larger, and chemical property is poor.
Hydrothermal synthesis method is by carrying out chemical reaction preparation in the fluid such as the aqueous solution or vapor under high temperature, high pressure
A kind of method of powder body material, it has the advantages that, and thing is mutually homogeneous, diameter of particle is small, process is simple.But it is only limited to a small amount of powder
Prepared by body, because the design and manufacture difficulty of large-scale high temperature high voltage resistant reactor is big, cost is high, therefore in high-volume industrial production
In by a definite limitation.
Sol-gel process is also only applicable to a small amount of powder and prepared, large quantities of because gel digestion time is long, dries and shrinks greatly
It is big to measure industrially prepared difficulty.
The content of the invention
The present invention provides the technique that a kind of homogeneous grain diameter combination mechanical alloying prepares LiFePO4, its use liquid phase with
The mode that solid phase reaction combines prepares LiFePO 4 powder, suitable for large batch of industrial application.
The technical scheme that specifically uses of the present invention is：
A kind of homogeneous grain diameter combination mechanical alloying prepares the technique of LiFePO4, it is characterized in that, comprise the following steps：
1) wet ball grinding：Various raw materials are blended in, the ball milling 3-5 hours in ball mill by wet process, raw material particle size controls after ball milling
Fe, Li, PO in 100 mesh, raw material4 3-, dispersant, talcum powder and mix element mol ratio be 1: 1: 1: 0.01-0.015: 2
: 0.005-0.007, wherein,
Source of iron is derived from：Ferric oxalate, di-iron trioxide or ferrous phosphate
Lithium source is derived from：LiH2PO4Or Li2CO3
Phosphorus source is derived from：NH4H2PO4Or LiH2PO4
Dispersant is：Cetyl trimethylammonium bromide；
Mix any mixture that element is yittrium oxide, titanium oxide and chromium oxide；
2) dry：By the raw material drying after ball milling；
3) pre-burning：By dried raw material at 300-400 DEG C pre-burning 4-6 hours；
4) dry ball milling：1-2wt% starch, dry ball milling to 300 mesh are added into above-mentioned raw materials；
5) high temperature sintering：Sintered 8 hours at being 650-700 DEG C in temperature；
6) LiFePO4 finished product is crushed to obtain.
Compared with prior art, it is an advantage of the invention that：
1) technique of the invention is suitable for industrial-scale preparation；
2) in the present invention, chromium can increase the rigidity of product；Titanium dioxide and yittrium oxide can guarantee that the product grain after high temperature sintering
Footpath is homogeneous；
3) conductive carbon is converted to after the starch sintering of addition, improves the electric conductivity of product.
Embodiment
Embodiment
1) composition of raw materials：
Ferric oxalate 46.6Kg, lithium carbonate 7.4Kg, NH4H2PO411.5kg, cetyl trimethylammonium bromide 3.64Kg, oxidation
Yttrium 0.7Kg, titanium oxide 0.08Kg, chromium oxide 0.15Kg, talcum powder 34Kg.
2) wet ball grinding：Above-mentioned raw materials are mixed, add the purified water of infiltration amount, ball milling 3-5 is small in ball mill by wet process
When, after ball milling raw material particle size control in 100 mesh,
2) dry：By the raw material drying after ball milling；
3) pre-burning：By dried raw material at 300-400 DEG C pre-burning 4-6 hours；
4) dry ball milling：1.4Kg starch, dry ball milling to 300 mesh are added into above-mentioned raw materials；
5) high temperature sintering：Sintered 8 hours at being 650-700 DEG C in temperature；
6) LiFePO4 finished product is crushed to obtain.
Claims (1)
1. a kind of homogeneous grain diameter combination mechanical alloying prepares the technique of LiFePO4, it is characterized in that, comprise the following steps：
1) wet ball grinding：Various raw materials are blended in, the ball milling 3-5 hours in ball mill by wet process, raw material particle size controls after ball milling
Fe, Li, PO in 100 mesh, raw material4 3-, dispersant, talcum powder and mix element mol ratio be 1: 1: 1: 0.01-0.015: 2
: 0.005-0.007, wherein,
Source of iron is derived from：Ferric oxalate, di-iron trioxide or ferrous phosphate
Lithium source is derived from：LiH2PO4Or Li2CO3
Phosphorus source is derived from：NH4H2PO4Or LiH2PO4
Dispersant is：Cetyl trimethylammonium bromide；
Mix any mixture that element is yittrium oxide, titanium oxide and chromium oxide；
2) dry：By the raw material drying after ball milling；
3) pre-burning：By dried raw material at 300-400 DEG C pre-burning 4-6 hours；
4) dry ball milling：1-2wt% starch, dry ball milling to 300 mesh are added into above-mentioned raw materials；
5) high temperature sintering：Sintered 8 hours at being 650-700 DEG C in temperature；
6) LiFePO4 finished product is crushed to obtain.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710809405.3A CN107572495A (en) | 2017-09-10 | 2017-09-10 | The technique that a kind of homogeneous grain diameter combination mechanical alloying prepares LiFePO4 |
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| CN201710809405.3A CN107572495A (en) | 2017-09-10 | 2017-09-10 | The technique that a kind of homogeneous grain diameter combination mechanical alloying prepares LiFePO4 |
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| CN107572495A true CN107572495A (en) | 2018-01-12 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275887A (en) * | 2011-01-17 | 2011-12-14 | 横店集团东磁股份有限公司 | Preparation method of high capacity high compacted density lithium iron phosphate material and product thereof |
| CN102664265A (en) * | 2011-05-25 | 2012-09-12 | 淄博赛动能源材料有限公司 | Process for preparing lithium iron phosphate by using liquid phase cocrystallization and mechanical alloying |
| CN102709619A (en) * | 2012-05-07 | 2012-10-03 | 杭州金马能源科技有限公司 | Preparation method for recycling lithium iron phosphate |
| CN103165886A (en) * | 2012-11-23 | 2013-06-19 | 杭州金马能源科技有限公司 | Preparation method for lithium iron phosphate materials with high tap density |
-
2017
- 2017-09-10 CN CN201710809405.3A patent/CN107572495A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275887A (en) * | 2011-01-17 | 2011-12-14 | 横店集团东磁股份有限公司 | Preparation method of high capacity high compacted density lithium iron phosphate material and product thereof |
| CN102664265A (en) * | 2011-05-25 | 2012-09-12 | 淄博赛动能源材料有限公司 | Process for preparing lithium iron phosphate by using liquid phase cocrystallization and mechanical alloying |
| CN102709619A (en) * | 2012-05-07 | 2012-10-03 | 杭州金马能源科技有限公司 | Preparation method for recycling lithium iron phosphate |
| CN103165886A (en) * | 2012-11-23 | 2013-06-19 | 杭州金马能源科技有限公司 | Preparation method for lithium iron phosphate materials with high tap density |
Non-Patent Citations (1)
| Title |
|---|
| 朱林泉 等: "《快速成型与快速制造技术》", 31 January 2003 * |
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