CN105329867A - High-compaction preparation method of lithium ferric manganese phosphate - Google Patents
High-compaction preparation method of lithium ferric manganese phosphate Download PDFInfo
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- CN105329867A CN105329867A CN201510765883.XA CN201510765883A CN105329867A CN 105329867 A CN105329867 A CN 105329867A CN 201510765883 A CN201510765883 A CN 201510765883A CN 105329867 A CN105329867 A CN 105329867A
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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
- C01B25/265—General methods for obtaining phosphates
-
- 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
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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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
- C01B25/37—Phosphates of heavy metals
- C01B25/377—Phosphates of heavy metals of manganese
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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
- 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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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a high-compaction preparation method of lithium ferric manganese phosphate. The high-compaction preparation method includes the steps that raw material mixing is conducted, preforming is conducted, sintering is conducted, secondary preforming is conducted, sintering is conducted, semi-finished crushing treatment is conducted on the prepared lithium ferric manganese phosphate, preforming is conducted a third time, high-temperature sintering is conducted at the temperature of 700-900 DEG C the last time, sintering is conducted continuously for 6-10 hours, a product obtained after high-temperature sintering is subjected to crushing treatment, a lithium ferric manganese phosphate material of certain fineness is obtained, finally sieving and iron removing are conducted, and a finished product can be obtained. By means of the high-compaction preparation method, a lithium ion battery manufactured with the lithium ferric manganese phosphate material as the anode can have the advantages of being high in energy and density as well as safety, long in service life and beneficial to application and popularization.
Description
[technical field]
The present invention relates to the technical field, the particularly technical field of a kind of preparation method of high-pressure solid lithium ferric manganese phosphate of lithium ion battery processing.
[background technology]
Along with the raising of socioeconomic development and human living standard, the demand of various countries to the energy increases day by day, and the going from bad to worse of the minimizing of traditional fossil energy (coal, oil, Sweet natural gas) and global environment, become two large obstacles of survival and development of mankind, find new forms of energy, the energy storage transfer equipment of exploitation energy-conserving and environment-protective becomes one of hot subject of various countries' research.The device that battery transforms mutually as a kind of chemical energy and electric energy is the important medium of reasonable energy utilization, and the progress of society makes developing green, high energy, the power supply of safety becomes a kind of active demand.In numerous secondary cells, lithium-ion secondary cell (Lithium-ion
battery, be called for short LIB) and at the beginning of being born, just rely on its incomparable performance to become the focus of global extensive concern.Positive electrode material is the important component part of lithium ion battery, and it not only participates in electrochemical reaction as electrode materials, and is the supplier of lithium ion.Because the density of positive electrode material is far above negative material, therefore positive electrode material specific storage is larger on the impact of battery specific storage, and positive electrode material accounts for about 40% of lithium ion battery cost.Therefore, the performance of positive electrode material and price etc. are that restriction lithium ion battery is further to the bottleneck of high-energy, long lifetime and low cost development.
LiMPO
4(M=Fe, Mn, Co and Ni) series of electrode material belongs to polyanionic compound, completely different from the structure of ordinary oxide electrode materials, thus, has unique chemical property.This kind of electrode materials causes the great interest of numerous researchist in recent years, wherein, and LiFePO
4be one of current study hotspot, its theoretical capacity is about 170mAh/g, but it is only 3.4V relative to the electrode potential of Li+/Li.LiCoPO4 and LiNiPO
4voltage platform respectively 4.8 and 5.1V, beyond the scope that existing lithium-ion battery electrolytes can bear, research finds, LiMnPO in these materials
4be 4.1V relative to the electrode potential of Li+/Li, be applicable to existing lithium-ion electrolyte, but the intrinsic conductivity of this material be extremely low, than an iron lithium phosphate also low 2-3 order of magnitude.For above problem, there is scholar to propose and have LiFePO concurrently
4and LiMnPO
4liFe
0.5+xmn
0.5-xpO
4, this kind of material has high gram volume and high-voltage platform, and intrinsic conductivity is also much higher than LiMnPO simultaneously
4.The positive electrode material of lithium ion battery mainly contains cobalt acid lithium, lithium manganate, lithium nickelate, ternary material, iron lithium phosphate etc.Wherein cobalt acid lithium is the positive electrode material that current most lithium ion battery uses.LiFe
0.5+xmn
0.5-xpO
4p-O key in crystal is very firm, is difficult to decompose, even if also at high temperature or when overcharging can not lattice avalanche occur as cobalt acid lithium or form oxidizing species, therefore has good security.In order to meet Green Travel, country promotes the development of electromobile energetically, and power lithium-ion battery used for electric vehicle requires to have high-energy-density and high security concurrently.
[summary of the invention]
Object of the present invention solves the problems of the prior art exactly, a kind of high-pressure solid lithium ferric manganese phosphate and preparation method thereof is proposed, lithium ferric manganese phosphate material can be made to be the advantage that lithium ion battery that positive pole is made has high-energy-density and high security concurrently, and long service life, is beneficial to and applies.
For achieving the above object, the present invention proposes a kind of high-pressure solid lithium ferric manganese phosphate, its chemical molecular formula is LiFe
0.5+xmn
0.5-xpO
4, 0.1≤x≤0.4.
The preparation method of a kind of high-pressure solid lithium ferric manganese phosphate of the present invention, its preparation method comprises the following steps successively:
Step one: raw material mix: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1-1.1:0.5-0.9:0.1-0.5:1:0.03-0.1, and adopt planetary ball mill to mill mixing, obtain presoma;
Step 2: compressing tablet, sintering: use tabletting machine to suppress presoma prepared by step one, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 200-350 DEG C of sintering, continues sintering 3-5h;
Step 3: secondary compressing tablet, sintering: once sintered lithium ferric manganese phosphate work in-process step 2 prepared are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then spraying dry is carried out, warm 450-600 DEG C of sintering in compressing tablet and secondary is carried out to the powder obtained, continues sintering 3-5h;
Step 4: to the lithium ferric manganese phosphate work in-process pulverization process prepared in step 3, again carry out compressing tablet, carries out last high temperature 700-900 DEG C of sintering, continues sintering 6-10h;
Step 5: the product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieves, deironing can obtain the finished product.
In this method, preparation process comprises the following steps: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1.1:0.8:0.2:1:0.06, and adopts planetary ball mill to mill mixing, obtains presoma; Use tabletting machine to suppress presoma, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 250 DEG C of sintering, continue sintering 5h; Once sintered lithium ferric manganese phosphate work in-process are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then carry out spraying dry, temperature 500 DEG C of sintering in compressing tablet and secondary are carried out to the powder obtained, continues sintering 5h; To lithium ferric manganese phosphate work in-process pulverization process, again carry out compressing tablet, carry out last high temperature 800 DEG C sintering, continue sintering 8h; The product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieve, deironing can obtain the finished product.
In this method, preparation process comprises the following steps: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1:0.6:0.4:1:0.03, and adopts planetary ball mill to mill mixing, obtains presoma; Use tabletting machine to suppress presoma, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 200 DEG C of sintering, continue sintering 5h; Once sintered lithium ferric manganese phosphate work in-process are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then carry out spraying dry, temperature 450 DEG C of sintering in compressing tablet and secondary are carried out to the powder obtained, continues sintering 4h; To lithium ferric manganese phosphate work in-process pulverization process, again carry out compressing tablet, carry out last high temperature 800 DEG C sintering, continue sintering 7h; The product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieve, deironing can obtain the finished product.
In this method, preparation process comprises the following steps: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1.1:0.9:0.1:1:0.1, and adopts planetary ball mill to mill mixing, obtains presoma; Use tabletting machine to suppress presoma, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 350 DEG C of sintering, continue sintering 5h; Once sintered lithium ferric manganese phosphate work in-process are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then carry out spraying dry, temperature 600 DEG C of sintering in compressing tablet and secondary are carried out to the powder obtained, continues sintering 5h; To lithium ferric manganese phosphate work in-process pulverization process, again carry out compressing tablet, carry out last high temperature 900 DEG C sintering, continue sintering 10h; The product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieve, deironing can obtain the finished product.
Beneficial effect of the present invention: the present invention can make lithium ferric manganese phosphate material be the advantage that lithium ion battery that positive pole is made has high-energy-density and high security concurrently, and long service life, is beneficial to and applies.
Feature of the present invention and advantage will be described in detail by embodiment.
[embodiment]
A kind of high-pressure solid lithium ferric manganese phosphate of the present invention, its chemical molecular formula is LiFe
0.5+xmn
0.5-xpO
4, 0.1≤x≤0.4.
The preparation method of a kind of high-pressure solid lithium ferric manganese phosphate of the present invention, its preparation method comprises the following steps successively:
Step one: raw material mix: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1-1.1:0.5-0.9:0.1-0.5:1:0.03-0.1, and adopt planetary ball mill to mill mixing, obtain presoma;
Step 2: compressing tablet, sintering: use tabletting machine to suppress presoma prepared by step one, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 200-350 DEG C of sintering, continues sintering 3-5h;
Step 3: secondary compressing tablet, sintering: once sintered lithium ferric manganese phosphate work in-process step 2 prepared are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then spraying dry is carried out, warm 450-600 DEG C of sintering in compressing tablet and secondary is carried out to the powder obtained, continues sintering 3-5h;
Step 4: to the lithium ferric manganese phosphate work in-process pulverization process prepared in step 3, again carry out compressing tablet, carries out last high temperature 700-900 DEG C of sintering, continues sintering 6-10h;
Step 5: the product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieves, deironing can obtain the finished product.
Embodiment one: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1.1:0.8:0.2:1:0.06, and adopt planetary ball mill to mill mixing, obtain presoma; Use tabletting machine to suppress presoma, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 250 DEG C of sintering, continue sintering 5h; Once sintered lithium ferric manganese phosphate work in-process are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then carry out spraying dry, temperature 500 DEG C of sintering in compressing tablet and secondary are carried out to the powder obtained, continues sintering 5h; To lithium ferric manganese phosphate work in-process pulverization process, again carry out compressing tablet, carry out last high temperature 800 DEG C sintering, continue sintering 8h; The product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieve, deironing can obtain the finished product.
Embodiment two: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1:0.6:0.4:1:0.03, and adopt planetary ball mill to mill mixing, obtain presoma; Use tabletting machine to suppress presoma, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 200 DEG C of sintering, continue sintering 5h; Once sintered lithium ferric manganese phosphate work in-process are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then carry out spraying dry, temperature 450 DEG C of sintering in compressing tablet and secondary are carried out to the powder obtained, continues sintering 4h; To lithium ferric manganese phosphate work in-process pulverization process, again carry out compressing tablet, carry out last high temperature 800 DEG C sintering, continue sintering 7h; The product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieve, deironing can obtain the finished product.
Embodiment three: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1.1:0.9:0.1:1:0.1, and adopt planetary ball mill to mill mixing, obtain presoma; Use tabletting machine to suppress presoma, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 350 DEG C of sintering, continue sintering 5h; Once sintered lithium ferric manganese phosphate work in-process are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then carry out spraying dry, temperature 600 DEG C of sintering in compressing tablet and secondary are carried out to the powder obtained, continues sintering 5h; To lithium ferric manganese phosphate work in-process pulverization process, again carry out compressing tablet, carry out last high temperature 900 DEG C sintering, continue sintering 10h; The product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieve, deironing can obtain the finished product.
Above-described embodiment is to explanation of the present invention, is not limitation of the invention, anyly all belongs to protection scope of the present invention to the scheme after simple transformation of the present invention.
Claims (5)
1. a high-pressure solid lithium ferric manganese phosphate, is characterized in that: the chemical molecular formula of described high-pressure solid lithium ferric manganese phosphate is LiFe
0.5+xmn
0.5-xpO
4, 0.1≤x≤0.4.
2. a preparation method for high-pressure solid lithium ferric manganese phosphate, is characterized in that: described preparation method comprises the following steps successively:
Step one: raw material mix: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1-1.1:0.5-0.9:0.1-0.5:1:0.03-0.1, and adopt planetary ball mill to mill mixing, obtain presoma;
Step 2: compressing tablet, sintering: use tabletting machine to suppress presoma prepared by step one, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 200-350 DEG C of sintering, continues sintering 3-5h;
Step 3: secondary compressing tablet, sintering: once sintered lithium ferric manganese phosphate work in-process step 2 prepared are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then spraying dry is carried out, warm 450-600 DEG C of sintering in compressing tablet and secondary is carried out to the powder obtained, continues sintering 3-5h;
Step 4: to the lithium ferric manganese phosphate work in-process pulverization process prepared in step 3, again carry out compressing tablet, carries out last high temperature 700-900 DEG C of sintering, continues sintering 6-10h;
Step 5: the product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieves, deironing can obtain the finished product.
3. the preparation method of a kind of high-pressure solid lithium ferric manganese phosphate as claimed in claim 2, it is characterized in that: described preparation process comprises the following steps: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1.1:0.8:0.2:1:0.06, and adopt planetary ball mill to mill mixing, obtain presoma; Use tabletting machine to suppress presoma, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 250 DEG C of sintering, continue sintering 5h; Once sintered lithium ferric manganese phosphate work in-process are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then carry out spraying dry, temperature 500 DEG C of sintering in compressing tablet and secondary are carried out to the powder obtained, continues sintering 5h; To lithium ferric manganese phosphate work in-process pulverization process, again carry out compressing tablet, carry out last high temperature 800 DEG C sintering, continue sintering 8h; The product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieve, deironing can obtain the finished product.
4. the preparation method of a kind of high-pressure solid lithium ferric manganese phosphate as claimed in claim 2, it is characterized in that: described preparation process comprises the following steps: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1:0.6:0.4:1:0.03, and adopt planetary ball mill to mill mixing, obtain presoma; Use tabletting machine to suppress presoma, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 200 DEG C of sintering, continue sintering 5h; Once sintered lithium ferric manganese phosphate work in-process are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then carry out spraying dry, temperature 450 DEG C of sintering in compressing tablet and secondary are carried out to the powder obtained, continues sintering 4h; To lithium ferric manganese phosphate work in-process pulverization process, again carry out compressing tablet, carry out last high temperature 800 DEG C sintering, continue sintering 7h; The product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieve, deironing can obtain the finished product.
5. the preparation method of a kind of high-pressure solid lithium ferric manganese phosphate as claimed in claim 2, it is characterized in that: described preparation process comprises the following steps: lithium salts, molysite, manganese salt, P contained compound, carbon source are taken by the mol ratio of 1.1:0.9:0.1:1:0.1, and adopt planetary ball mill to mill mixing, obtain presoma; Use tabletting machine to suppress presoma, the presoma suppressed is carried out in the ar gas environment being mixed with trace hydrogen a low temperature 350 DEG C of sintering, continue sintering 5h; Once sintered lithium ferric manganese phosphate work in-process are pulverized, mix a certain proportion of admixed with additives and solvent simultaneously, pour sand mill into and carry out wet-mixed dispersion, then carry out spraying dry, temperature 600 DEG C of sintering in compressing tablet and secondary are carried out to the powder obtained, continues sintering 5h; To lithium ferric manganese phosphate work in-process pulverization process, again carry out compressing tablet, carry out last high temperature 900 DEG C sintering, continue sintering 10h; The product of high temperature sintering is carried out pulverization process, obtains the lithium ferric manganese phosphate material of certain fineness, finally sieve, deironing can obtain the finished product.
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| CN106904588A (en) * | 2017-03-22 | 2017-06-30 | 江苏元景锂粉工业有限公司 | A kind of lithium ion battery with high energy density positive electrode and preparation method thereof |
| CN109817945A (en) * | 2019-02-20 | 2019-05-28 | 惠州亿纬锂能股份有限公司 | A kind of nickelic positive electrode and preparation method thereof |
| CN110400917A (en) * | 2019-05-31 | 2019-11-01 | 宜春天赐高新材料有限公司 | A kind of high capacity type lithium ferric manganese phosphate positive electrode and preparation method thereof |
| CN113659133A (en) * | 2021-07-09 | 2021-11-16 | 江苏乐能电池股份有限公司 | Preparation method of high-compaction lithium ferric manganese phosphate cathode material |
| CN116598466A (en) * | 2023-06-20 | 2023-08-15 | 河北九丛科技有限公司 | Preparation method of metal oxide uniformly doped battery-level lithium manganese iron phosphate |
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