CN109360981A - Cell positive material LiCrxMn2-xO4-yFyAnd the preparation method of positive plate - Google Patents
Cell positive material LiCrxMn2-xO4-yFyAnd the preparation method of positive plate Download PDFInfo
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- CN109360981A CN109360981A CN201811033505.2A CN201811033505A CN109360981A CN 109360981 A CN109360981 A CN 109360981A CN 201811033505 A CN201811033505 A CN 201811033505A CN 109360981 A CN109360981 A CN 109360981A
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
- H01M4/48—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
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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
- H01M4/582—Halogenides
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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 the preparation method of a kind of cell positive material and positive plate, the positive electrode is to mix chromium, fluorine composite spinelle type oxide LiCr x Mn2‑x O4‑y F y (0≤x≤ 0.5,0≤y≤ 0.3).Using step mixing by the compound of lithium, chrome green, the compound of manganese and lithium fluoride proportionally n (Li): n (Cr): n (Mn): n (F)=1:x:2‑x:yIt is uniformly mixed, then the 100-200 DEG C of drying 5-10h in drying box, in air 530-550 DEG C of heat treatment 5-10h, continues to be warming up to 650-750 DEG C, keep the temperature 10-20h, be finally slowly cooled to room temperature.The product purity is high, and good for stability in thermal cell, voltage is steady, and capacity is big, with 10mA/cm at 250 DEG C2Current density electric discharge, surveyed highest discharge capacity reaches 842 mAh/g.Applied in underground heat or petroleum-natural gas exploration drilling device, continued smooth can power under the rigor conditions such as high temperature, high pressure.Preparation method of the present invention is simple, and production and manufacturing cost are cheap.
Description
Technical field
The invention belongs to energy technology fields, are related to a kind of cell positive material LiCr x Mn2-x O4-y F y (0≤x≤ 0.5,0
≤y≤ 0.3) preparation, in particular to thermal cell positive electrode spinel-type LiCr x Mn2-x O4-y F y Preparation, this preparation method
Obtained thermal cell positive electrode capacity is significantly promoted, voltage stabilization.
Background technique
As in the widely applied thermal cell of military industry field, there is storage time length, safe and reliable, high-energy-density, structure
The features such as compact.And with the transformation now to the wilderness demand of the energy and energy resource structure, to cleaning and renewable energy
Development and utilization is more and more paid attention to.Required battery will bear high temperature in underground heat and deep-well oil-gas mining environment
The critical conditions such as high pressure, therefore using improving the advantages of thermal cell and to it and got growing concern at present.
For the temperature of the exploration and developments such as deep-well petroleum, natural gas at 200 DEG C or so, underground heat production temperature can be higher.But mesh
Preceding commercial Li-ion battery operating temperature only has -55 DEG C~70 DEG C.Li-Mg/SOCl2The operating temperature of organic electrolyte cell
Reach 180 DEG C, expensive vacuum Dewar bottle must be installed at higher temperatures and be protected.Thermal cell (high temperature modified
Battery) heat that can use institute's working environment activated and worked, and can simplify battery structure, reduce battery manufacture at
This.
LiM x Mn2-x O4-y F y Positive electrode has research in traditional lithium-ion battery, and Doped ions are mainly for raising mangaic acid
The cycle performance of lithium material.Choi W et al. (Journal of the Electrochemical Society, 2007,154
(8): A792-A797) by raw material Li2CO3, Mn2O3And TiO2Or NiO is sintered 48h at 800 DEG C and obtains LiMn2−y− z Li y M z O4, then with NH4HF2It mixes and 450 DEG C of sintering 5h obtains LiMn in air atmosphere2−y−z Li y M z O4−ηFη.This preparation method
Substep is needed to carry out, and NH4HF2It can decompose and distil at high temperature, inconvenience control.Bao S.J. et al. (Materials
Chemistry and Physics, 2006,95 (1): 188-192) use sol-gal process using citric acid as chelating agent, with
LiNO3, Mn (NO3)2, LiF and CrO3LiCr is made for raw material x Mn2−x O4−yFy .This preparation method is raw materials used relatively high, and
Complex process is unfavorable for productionization.
Summary of the invention
The purpose of the present invention is using convenient and fast operating method, easy preparation process prepares high capacity, high-purity, property
The excellent electrode material of energy, simplifies the existing process for preparing material, and be able to satisfy mass production.
To achieve the above object, LiCr of the present invention x Mn2-x O4-y F y The preparation step of battery material are as follows:
(1) by the compound of the compound of lithium, the compound of chromium, the compound of manganese and fluorine proportionally n (Li): n (Cr): n
(Mn): n(F)=1:x:2-x:yIt is uniformly mixed, wherein 0≤x≤ 0.5,0≤y≤0.3；
(2) ball-milling method mixing material 1-3h, revolving speed 150-300r/min are used；
(3) gained mixture 100-200 DEG C of drying, 5-10h in drying box or heat-treatment furnace；
(4) 530-550 DEG C of heat treatment 5-10h, heating rate are 0.1-5 DEG C/min in air；
(5) continue to be warming up to 650-750 DEG C, keep the temperature 10-20h, heating rate is 0.1-5 DEG C/min；
(6) it is cooled to room temperature, cooling rate obtains LiCr in 0.1-2 DEG C/min x Mn2-x O4-y F y Cell positive material.
Specifically, the compound of the lithium uses lithium carbonate, lithium hydroxide or lithium nitrate, preferably lithium carbonate and hydrogen-oxygen
Change lithium.
The compound of the chromium uses chrome green.
The compound of the manganese uses mangano-manganic oxide, manganese dioxide, preferably manganese dioxide.
The compound of the fluorine uses lithium fluoride.
The present invention also provides a kind of methods for preparing positive plate: by gained positive electrode grinding sieve with 100 mesh sieve, then with together
The conductive agent and electrolyte that sample sieves with 100 mesh sieve are uniformly mixed, this mixture is pressed into positive plate using powder compressing machine.
In positive plate, positive electrode: electrolyte: conductive agent=7:2:1(mass ratio).Wherein electrolyte uses low melting point nitre
Hydrochlorate, such as LiNO3-KNO3, conductive agent is using carbon materials such as graphite powder, carbon blacks.
Cathode uses lithium alloy piece.
Cell positive material LiCr prepared by this preparation method x Mn2-x O4-y F y It has the following advantages that and effect:
(1) preparation method of the present invention disposably mixes raw material, is obtained later by high temperature sintering, and preparation process is simpler
Just, practical handling strong, it can largely generate.
(2) the positive electrode LiCr that preparation method of the present invention obtains x Mn2-x O4-y F y With undoped spinel lithium manganate
Structure is identical, i.e., with the atom in foreign atom substitution original structure.
(3) the positive electrode LiCr that preparation method of the present invention obtains x Mn2-x O4-y F y Purity is high, stability is good,
With 10mA/cm under 250 °C2Current density electric discharge, surveyed highest discharge capacity reaches 842 mAh/g, and voltage is steady, capacity
Greatly.Applied in underground heat or petroleum-natural gas exploration drilling device, can persistently be put down under the rigor conditions such as high temperature, high pressure
Steady power supply, increases equipment cruise duration, while reducing battery volume, to there is bigger specific energy.
(4) preparation method of the present invention is simple, raw materials used relative moderate, reduces battery production and manufacturing cost.
Detailed description of the invention
The discharge curve of prepared battery in Fig. 1, embodiment 1；
The discharge curve of prepared battery in Fig. 2, embodiment 2；
The discharge curve of prepared battery in Fig. 3, embodiment 3；
The discharge curve of prepared battery in Fig. 4, embodiment 4；
The X ray diffracting spectrum of material prepared in Fig. 5, embodiment 1-4；
The scanning electron microscope (SEM) photograph of material prepared in Fig. 6, embodiment 1；
The scanning electron microscope (SEM) photograph of material prepared in Fig. 7, embodiment 2；
The scanning electron microscope (SEM) photograph of material prepared in Fig. 8, embodiment 3；
The scanning electron microscope (SEM) photograph of material prepared in Fig. 9, embodiment 4.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1: raw materials LiOHH2O, Cr2O3, MnO2, LiF, purity it is all analysis it is pure, according to mole
Above-mentioned four kinds of reagents are weighed than 1:0.05:1.9:0；Weighed amount reagent is fitted into alumina balls grinding jar, and 230r/min's
Ball milling mixing two hours under revolving speed；By uniformly mixed material, dry 6h, heating rate are 5 DEG C/min at 150 DEG C, are then existed
550 DEG C of heat preservation 6h, heating rate are 5 DEG C/min, then are heat-treated 12h at 750 DEG C, are cooled to room temperature, cooling rate is 1 DEG C/
Min obtains black powder.Resulting materials grinding is sieved with 100 mesh sieve, then is mixed with the conductive agent and electrolyte equally sieved with 100 mesh sieve
It closes uniformly, this mixture is pressed into positive plate using powder compressing machine.In positive plate, positive electrode active materials: electrolyte: conductive agent
=7:2:1(mass ratio), wherein electrolyte uses LiNO3-KNO3(mass fraction is respectively 33.2% and 66.8%), conductive agent use
Graphite.Positive plate and electrolyte and cathode are assembled into single battery.Single battery is at 250 DEG C with 10mA/cm2Electric current it is close
Degree electric discharge, test results are shown in figure 1.
Embodiment 2: raw materials LiOHH2O, Cr2O3, MnO2, LiF, purity it is all analysis it is pure, according to mole
Above-mentioned four kinds of reagents are weighed than 0.9:0.05:1.9:0.1；Weighed amount reagent is fitted into alumina balls grinding jar, and in 230r/
Ball milling mixing two hours under the revolving speed of min；By uniformly mixed material, dry 6h, heating rate are 5 DEG C/min at 150 DEG C,
Then in 550 DEG C of heat preservation 6h, heating rate is 5 DEG C/min, then is heat-treated 12h at 750 DEG C, is cooled to room temperature, cooling rate
For 1 DEG C/min, black powder is obtained.Resulting materials grinding is sieved with 100 mesh sieve, then with the conductive agent and electricity that equally sieve with 100 mesh sieve
It solves matter to be uniformly mixed, this mixture is pressed into positive plate using powder compressing machine.In positive plate, positive electrode active materials: electrolyte:
Conductive agent=7:2:1(mass ratio), wherein electrolyte uses LiNO3-KNO3(mass fraction is respectively 33.2% and 66.8%), it is conductive
Agent uses graphite.Positive plate and electrolyte and cathode are assembled into single battery.Single battery is at 250 DEG C with 10mA/cm2's
Current density electric discharge, test results are shown in figure 2.
Embodiment 3: raw materials LiOHH2O, Cr2O3, MnO2, LiF, purity it is all analysis it is pure, according to mole
Above-mentioned four kinds of reagents are weighed than 0.8:0.05:1.9:0.2；Weighed amount reagent is fitted into alumina balls grinding jar, and in 230r/
Ball milling mixing two hours under the revolving speed of min；By uniformly mixed material, dry 6h, heating rate are 5 DEG C/min at 150 DEG C,
Then in 550 DEG C of heat preservation 6h, heating rate is 5 DEG C/min, then is heat-treated 12h at 750 DEG C, is cooled to room temperature, cooling rate
For 1 DEG C/min, black powder is obtained.Resulting materials grinding is sieved with 100 mesh sieve, then with the conductive agent and electricity that equally sieve with 100 mesh sieve
It solves matter to be uniformly mixed, this mixture is pressed into positive plate using powder compressing machine.In positive plate, positive electrode active materials: electrolyte:
Conductive agent=7:2:1(mass ratio), wherein electrolyte uses LiNO3-KNO3(mass fraction is respectively 33.2% and 66.8%), it is conductive
Agent uses graphite.Positive plate and electrolyte and cathode are assembled into single battery.Single battery is at 250 DEG C with 10mA/cm2's
Current density electric discharge, test results are shown in figure 3.
Embodiment 4: raw materials LiOHH2O, Cr2O3, MnO2, LiF, purity it is all analysis it is pure, according to mole
Above-mentioned four kinds of reagents are weighed than 0.7:0.05:1.9:0.3；Weighed amount reagent is fitted into alumina balls grinding jar, and in 230r/
Ball milling mixing two hours under the revolving speed of min；By uniformly mixed material, dry 6h, heating rate are 5 DEG C/min at 150 DEG C,
Then in 550 DEG C of heat preservation 6h, heating rate is 5 DEG C/min, then is heat-treated 12h at 750 DEG C, is cooled to room temperature, cooling rate
For 1 DEG C/min, black powder is obtained.Resulting materials grinding is sieved with 100 mesh sieve, then with the conductive agent and electricity that equally sieve with 100 mesh sieve
It solves matter to be uniformly mixed, this mixture is pressed into positive plate using powder compressing machine.In positive plate, positive electrode active materials: electrolyte:
Conductive agent=7:2:1(mass ratio), wherein electrolyte uses LiNO3-KNO3(mass fraction is respectively 33.2% and 66.8%), it is conductive
Agent uses graphite.Positive plate and electrolyte and cathode are assembled into single battery.Single battery is at 250 DEG C with 10mA/cm2's
Current density electric discharge, test results are shown in figure 4.
The discharge initiation voltage and discharge capacity of embodiment 1-4 is listed in Table 1 below.
The step hybrid manipulation that the present invention uses is easy, is obtaining the battery of function admirable just by mixing and calcining later
Pole material.The LiCr as made from this method x Mn2-x O4-y F y Specific discharge capacity is up to 842 mAh/g(embodiments 4).This reality
Border discharge capacity is than the FeS that uses in Conventional thermoelectric pond2The theoretical discharge capacity (446 mAh/g) of positive electrode almost improves
One times.At the same time, LiCr made from this method x Mn2-x O4-y F y Discharge voltage is relatively steady, and main there are two big voltages to put down
Platform (2.7-2.8V；1.6-2.3V), high voltage potential can reduce battery volume while meeting voltage requirements, improve electricity
Pond energy density per unit volume reduces monocell and stacks quantity, improves battery safety.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (6)
1. a kind of cell positive material LiCr x Mn2-x O4-y F y Preparation method, which comprises the steps of:
(1) by the compound of the compound of lithium, the compound of chromium, the compound of manganese and fluorine according to molar ratio n (Li): n
(Cr):n(Mn): n(F)=1:x:2-x:yIt is uniformly mixed, wherein 0≤x≤ 0.5,0≤y≤0.3；
(2) ball-milling method mixing material 1-3h, revolving speed 150-300r/min are used；
(3) gained mixture 100-200 DEG C of drying, 5-10h in drying box or heat-treatment furnace；
(4) 530-550 DEG C of heat treatment 5-10h, heating rate are 0.1-5 DEG C/min in air；
(5) continue to be warming up to 650-750 DEG C, keep the temperature 10-20h, heating rate is 0.1-5 DEG C/min；
(6) it is cooled to room temperature, cooling rate obtains LiCr in 0.1-2 DEG C/min x Mn2-x O4-y F y Cell positive material.
2. cell positive material LiCr as described in claim 1 x Mn2-x O4-y F y Preparation method, which is characterized in that the lithium
Compound using lithium carbonate or lithium hydroxide or lithium nitrate；The compound of chromium uses chrome green；The compound of the manganese
Using mangano-manganic oxide or manganese dioxide；The compound of the fluorine uses lithium fluoride.
3. cell positive material LiCr as claimed in claim 2 x Mn2-x O4-y F y Preparation method, which is characterized in that the change of lithium
It closes object and uses lithium carbonate or lithium hydroxide；The compound of manganese is manganese dioxide.
4. a kind of preparation method of positive plate, which is characterized in that by the described in any item cell positive materials of claim 1 ~ 3
LiCr x Mn2-x O4-y F y Grinding sieves with 100 mesh sieve, then is uniformly mixed with the conductive agent and electrolyte equally sieved with 100 mesh sieve, utilizes powder
This mixture is pressed into positive plate by tablet press machine；It counts in mass ratio, positive electrode: electrolyte: conductive agent=7:2:1.
5. the preparation method of positive plate as claimed in claim 4, which is characterized in that electrolyte uses low melting point nitrate；It leads
Electric agent uses graphite powder or carbon black.
6. the preparation method of positive plate as claimed in claim 5, which is characterized in that electrolyte uses LiNO3-KNO3。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111987299A (en) * | 2020-08-29 | 2020-11-24 | 中北大学 | Si @ SnO used as high-temperature lithium battery positive electrode material2Preparation method of @ C microspheres |
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