CN108417773A - A kind of LiFePO4 combination electrode and its preparation method and application - Google Patents
A kind of LiFePO4 combination electrode and its preparation method and application Download PDFInfo
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- CN108417773A CN108417773A CN201810112026.3A CN201810112026A CN108417773A CN 108417773 A CN108417773 A CN 108417773A CN 201810112026 A CN201810112026 A CN 201810112026A CN 108417773 A CN108417773 A CN 108417773A
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- 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
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/043—Processes of manufacture in general involving compressing or compaction
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- 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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Abstract
The invention belongs to field of lithium ion battery material preparation, and in particular to a kind of LiFePO4 combination electrode and its preparation method and application, the preparation process of LiFePO4 combination electrode is：Aluminium ion is deposited on by iron phosphate lithium electrode surface in oil-based solvent system by electrochemical deposition method first, LiFePO4 combination electrode A is obtained after drying, lithium salts is deposited on the surfaces combination electrode A using electrochemical deposition method in oil-based solvent system later, LiFePO4 combination electrode B is obtained after cleaning, drying.It prepares material has many advantages, such as that ionic conductivity is high, consistency is high, the strong gram volume and its high rate performance for improving its material of structural stability using the lithium salts of flexible, its electron transfer rate is improved by the high characteristic of middle layer deposition foamed aluminium conductivity simultaneously, the combination electrode prepared and energy density, high rate performance and its cycle performance that its lithium ion battery can be improved applied to ferric phosphate lithium cell.
Description
Technical field
The invention belongs to field of lithium ion battery material preparation, and in particular to a kind of LiFePO4 combination electrode and its preparation
Methods and applications.
Background technology
LiFePO4 has been developed in recent years a kind of novel anode material, high, the environmental-friendly, valence with its security performance
The advantages that lattice are cheap and its have extended cycle life and applied to the fields such as car, but issued as National Ministry of Finance announces《It closes
The notice of fiscal support policy is promoted and applied in 2016-2020 new-energy automobiles》, it is desirable that ferric phosphate lithium cell has higher
Energy density, to reach highest subsidy standard.And lithium iron phosphate positive material is the chief component of LiFePO4, property
The quality of energy plays a key effect to the multiplying power, cycle and its energy density of ferric phosphate lithium cell.Current LiFePO4 is just
The gram volume of pole material is generally in 150-160mAh/g, and pole piece compaction density is in 2.3-2.4g/cm2Between, cause its ferric phosphate
The energy density of lithium is relatively low, influences the course continuation mileage of its electric vehicle.And lithium iron phosphate positive material energy density is improved at present
Method mainly have：The gram volume and compacted density of material are improved, material gram volume is improved and compacted density major way is
Doped metallic elements, material nano and its materials such as cladding consistency height and the good carbon of compatibility of electrolyte.Such as patent
（CN201310570094.1）A kind of production method of high-capacity high-compaction lithium iron phosphate anode material is disclosed, by using more
The method of secondary compacting and sintering prepares high-capacity high-compaction lithium iron phosphate anode material, has effectively achieved and improves LiFePO4 pressure
The purpose of real density, electrochemistry gram volume and cycle performance, but it uses solid phase method that there are clad consistency is low and its lithium
The transmission rate of ion is relatively low, influences the gram volume of its material and its further increasing for compacted density.
Invention content
The shortcomings that overcome the prior art, the present invention provides a kind of preparation method of LiFePO4 combination electrode, the party
Method is efficient, can improve the compacted density of iron phosphate lithium electrode, gram volume and its high rate performance.
To achieve the above object, the present invention uses following technical scheme:
A kind of preparation method of LiFePO4 combination electrode, using following steps：
（1）1g~5g organic aluminium salts are added to（10~30）Ml benzene and（70~90）The mixed organic solvents of ml tetrahydrofurans
In, it stirring evenly, is then to electrode by working electrode, platinum filament of compression moulding LiFePO4, saturation calomel is reference electrode,
1min~30min is deposited using electrochemical deposition method on the working electrode (s, then cleans, be dried to obtain LiFePO4 combination electrode
A；
（2）1g~5g lithium salts is added in the ethylene carbonate of 100ml and is uniformly mixing to obtain organic solvent system, later with phosphorus
Sour iron lithium combination electrode A is used as to electrode, saturation calomel as working electrode, platinum electrode as reference electrode, and using electrification
Method is in working electrode surface electro-deposition lithium salts, sedimentation time 1min~30min, after, using ethylene carbonate cleaning, dry
It is dry to obtain iron phosphate lithium electrode B, as the LiFePO4 combination electrode.
Further, step（1）Described in molding LiFePO4 preparation method be：First by the ferric phosphate of 80g~95g
The N-Methyl pyrrolidone of lithium powder, 5g~20g Kynoar and 50ml~100ml obtains grume glue after mixing
Body obtains blocky iron phosphate lithium electrode later by tablet press machine compression moulding after dry.
Preferably, step（1）Described in aluminium salt be aluminium ethide, butyl aluminium, aluminium acetate, aluminium triformate, oxalic acid aluminium and propionic acid
One kind in aluminium.
Preferably, step（1）And step（2）Described in electrochemical deposition method be cyclic voltammetry, constant-voltage method, constant flow method
With one kind in impulse method.
Preferably, step（2）Described in lithium salts be lithium carbonate, lithium hydroxide, lithium metaaluminate, lithium perchlorate and lithium zirconate
In one kind.
LiFePO4 combination electrode prepared by above-mentioned preparation method, which is characterized in that the LiFePO4 combination electrode is
By LiFePO4 and its it is deposited on the aluminium salt on surface and its lithium salts forms, mass ratio is：LiFePO4：Aluminium salt：Lithium salts is
100：1~5：1~5.
Application in above-mentioned LiFePO4 combination electrode, which is characterized in that the ferric phosphate lithium cell is mainly by phosphoric acid
Iron lithium combination electrode, graphite cathode material, ceramic diaphragm and its functional electrolyte composition.
And electrochemical process has the characteristics that preparation process is fast, consistency is high, consistency is high and its process is easy to control, and prepares
The material gone out has many advantages, such as that sedimentary is thin, consistency is high, and structural stability is strong, is such as applied to LiFePO4 and prepares, Ke Yi great
Amplitude improves the tap density of its material, and improves the gram volume and its high rate performance of its material.
Advantageous effect
（1）For the present invention by depositing aluminium salt on the surfaces iron phosphate lithium electrode A, aluminium salt is foamed aluminium, and is coated on LiFePO4
Surface improves the electronic conductivity of LiFePO4 and its reduces its specific surface area and its reduce active site, improves its first charge discharge efficiency；
Organic aluminium salt has preferable compatibility with LiFePO4 simultaneously, can uniformly, firmly be deposited on its surface.
（2）In outermost layer by electrochemical deposition lithium salts, its material is improved by the high characteristic of lithium salts lithium ion conducting rate
The transmission rate of lithium ion in charge and discharge process, while middle layer foamed aluminium has nano aperture structure, and do not influence charge and discharge
The transmission rate of lithium ion in electric process.
（3）The present invention is using electrochemical process deposition aluminium salt and lithium salts, with preparation process is fast, consistency is high, consistency is high
And its process the features such as being easy to control, the material prepared has many advantages, such as that sedimentary is thin, consistency is high, and structural stability is strong,
Such as be applied to LiFePO4 prepare, the tap density of its material can be increased substantially, and improve its material gram volume and its
High rate performance.
Description of the drawings
Fig. 1 is the cyclic curve figure for the ferric phosphate lithium cell that embodiment is prepared with comparative example.
Specific implementation mode
The present invention is further illustrated with comparative example in conjunction with the embodiments, it should explanation, following the description be only for
It explains the present invention, its content is not defined.
Embodiment 1
The preparation method of blocky iron phosphate lithium electrode is：
The N-Methyl pyrrolidone of the iron phosphate powder of 90g, 10g Kynoar and 80ml is obtained after mixing first
Grume colloid, and coated on foamed aluminium, be pressed into after dry and by tablet press machine in the case where pressure is the pressure of 10Mpa
Type, then obtain blocky iron phosphate lithium electrode after temperature is 80 DEG C dry.
1）3g aluminium ethides are added in the mixed organic solvents of 20ml benzene and 80ml tetrahydrofurans, conduct after stirring evenly
Deposition solution is later to electrode by working electrode, platinum filament of compression moulding bulk LiFePO4, and saturation calomel is reference electricity
Pole uses cyclic voltammetry later in deposition solution（Voltage range -2V-2V, surface sweeping rate：5mV/s）On the working electrode (s
20min is deposited, the ethylene carbonate cleaning of 0.1mol/L is used later, is dried to obtain LiFePO4 combination electrode A；
2）3g lithium hydroxides are added in the ethylene carbonate of 100ml and are uniformly mixing to obtain organic solvent system, later with phosphorus
Sour iron lithium combination electrode A is used as to electrode, saturation calomel as working electrode, platinum electrode as reference electrode, and using cycle
Voltammetry（Voltage range -2V-2V, surface sweeping rate：5mV/s）In working electrode surface electro-deposition lithium salts, sedimentation time 20min,
After, using ethylene carbonate cleaning, it is dried to obtain LiFePO4 combination electrode B.
Embodiment 2
The preparation method of blocky iron phosphate lithium electrode is：
The N-Methyl pyrrolidone of the iron phosphate powder of 80g, 20g Kynoar and 50ml is obtained after mixing first
Grume colloid, and coated on foamed aluminium, be pressed into after dry and by tablet press machine in the case where pressure is the pressure of 10Mpa
Type, then obtain blocky iron phosphate lithium electrode after temperature is 80 DEG C dry.
1）1g butyl aluminium is added in the mixed organic solvents of 10ml benzene and 90ml tetrahydrofurans, conduct after stirring evenly
Deposition solution is later to electrode by working electrode, platinum filament of compression moulding LiFePO4, and saturation calomel is reference electrode,
Deposition solution uses constant-voltage method（Voltage 2V）1min is deposited on the working electrode (s, uses the ethylene carbonate of 0.1mol/L clear later
It washes, be dried to obtain LiFePO4 combination electrode A；
2）1g lithium carbonates are added in the ethylene carbonate of 100ml and are uniformly mixing to obtain organic solvent system, later with phosphoric acid
Iron lithium combination electrode A is used as to electrode, saturation calomel as working electrode, platinum electrode as reference electrode, and using using permanent
Platen press（Voltage 2V）In working electrode surface electro-deposition lithium salts, sedimentation time 1min, after, using ethylene carbonate cleaning,
It is dried to obtain LiFePO4 combination electrode B.
Embodiment 3
The preparation method of blocky iron phosphate lithium electrode is：
The N-Methyl pyrrolidone of the iron phosphate powder of 95g, 5g Kynoar and 100ml is obtained after mixing first
Grume colloid, and coated on foamed aluminium, be pressed into after dry and by tablet press machine in the case where pressure is the pressure of 10Mpa
Type, then obtain blocky iron phosphate lithium electrode after temperature is 80 DEG C dry.
1）5g aluminium acetates are added in the mixed organic solvents of 30ml benzene and 70ml tetrahydrofurans, conduct after stirring evenly
Deposition solution is later to electrode by working electrode, platinum filament of compression moulding LiFePO4, and saturation calomel is reference electrode,
Deposition solution uses constant flow method（1mA/cm2）30min is deposited on the working electrode (s, uses the ethylene carbonate of 0.1mol/L later
It cleans, be dried to obtain LiFePO4 combination electrode A；
2）5g lithium metaaluminates are added in the ethylene carbonate of 100ml and are uniformly mixing to obtain organic solvent system, later with phosphorus
Sour iron lithium combination electrode A is used as working electrode, platinum electrode and uses constant current as reference electrode to electrode, saturation calomel
Method（1mA/cm2）In working electrode surface electro-deposition lithium salts, sedimentation time 30min, after, using ethylene carbonate cleaning,
It is dried to obtain LiFePO4 combination electrode B.
Comparative example：
As a comparison case with the LiFePO4 purchased in the market（Model：N1, producer：Jiangsu Leneng Battery Co., Ltd.）
1）Button cell makes：
In mass ratio 0.9: 0.05: 0.05 weighs the positive-active that 2.0000g Examples 1 to 3 and comparative example are prepared respectively
Substance iron phosphate lithium electrode, 0.1111g conductive blacks, 0.1111gPVDF mixing, add and 2.5g organic solvents NMP are added
(N-Methyl pyrrolidone) is sufficiently mixed uniformly.The film that thickness is 140 microns, 120 DEG C of vacuum dryings are painted on aluminium foil
2h breaks into the disk of 5mm using card punch, and using tablet press machine in 10Mpa lower sheetings, 120 DEG C of vacuum heat-preserving 12h weigh anode
Sheet weight.It is assembled into button cell in the glove box of argon gas protection, using metal lithium sheet as cathode, electrolyte is volume ratio 1: 1
EC (ethylene carbonate), DMC ((1,2- dimethyl carbonate) solvent, electrolyte LiPF6, diaphragm Celgard2400
Microporous polyethylene film.The battery installed is tested into electrical property on blue electric tester.In 2.5V~4.2V voltage ranges, with
0.2C constant current charge/discharge, test specific capacity prepare button cell A1, A2, A3 and B1 as shown in table 1.
Table 1, embodiment and comparative example buckle electrical test results comparison
As can be seen from Table 1, the discharge capacity and first charge discharge efficiency for the LiFePO 4 material that embodiment is prepared are apparently higher than comparison
Example, the reason for this is that embodiment material surface doping has the transmission rate that lithium salts provides lithium ion in charge and discharge process in material, from
And improve first charge discharge efficiency and the gram volume performance of its material；Intermediate layer of material is coated with the high aluminum material of electronic conductivity simultaneously,
Improve the electric conductivity of its material.
2）Soft-package battery makes：
It is negative with artificial graphite respectively using embodiment 1, embodiment 2, embodiment 3 and comparative example resulting materials as positive electrode
Pole material, using LiPF6/EC+DEC（Volume ratio 1: 1）For electrolyte, 2400 films of Celgard are diaphragm, prepare 2.5Ah circles
Column battery C1, C2, C3 and D1, and the high rate performance of its material is tested, rate of charge 0.3C, discharge-rate 0.3C,
0.5C、1.0C、5.0C、10.0C、20.0C。
Table 2, embodiment are compared with the multiplying power discharging of comparative example
As can be seen from Table 2, the high rate performance for the battery that embodiment material preparation goes out is substantially better than comparative example, the reason for this is that implementing
Material surface is coated with lithium salts substance in example, for the lithium ion for providing sufficient in charge and discharge process, improves in its charge and discharge process
Multiplying power discharging property.
Table 3 is the circulation of embodiment and soft-package battery, and wherein parameter is：Multiplying power is charged and discharged non-2.0C/2.0C,
Voltage range 2.5-4.2V, 25 ± 3 DEG C of temperature, cycle-index 500 times, while calculating the energy density of battery.
Table 3, embodiment are compared with the energy density of comparative example
As can be seen from Table 3, the energy density for the battery that embodiment is prepared is substantially better than comparative example, the reason for this is that embodiment
Material has the energy density that higher specific capacity and its tap density improve its material.LiFePO 4 material has densification simultaneously
The lithium ion that degree is high, structural stability is strong and its sufficient, to improve its cycle performance.
Claims (7)
1. a kind of preparation method of LiFePO4 combination electrode, which is characterized in that use following steps：
（1）1g~5g organic aluminium salts are added to（10~30）Ml benzene and（70~90）The mixed organic solvents of ml tetrahydrofurans
In, it stirring evenly, is then to electrode by working electrode, platinum filament of compression moulding LiFePO4, saturation calomel is reference electrode,
1min~30min is deposited using electrochemical deposition method on the working electrode (s, then cleans, be dried to obtain LiFePO4 combination electrode
A；
（2）1g~5g lithium salts is added in the ethylene carbonate of 100ml and is uniformly mixing to obtain organic solvent system, later with phosphorus
Sour iron lithium combination electrode A is used as to electrode, saturation calomel as working electrode, platinum electrode as reference electrode, and using electrification
Method is in working electrode surface electro-deposition lithium salts, sedimentation time 1min~30min, after, using ethylene carbonate cleaning, dry
It is dry to obtain iron phosphate lithium electrode B, as the LiFePO4 combination electrode.
2. according to preparation method described in claim 1, which is characterized in that step（1）Described in be molded LiFePO4 preparation side
Method is：First by the N- methylpyrroles of the iron phosphate powder of 80g~95g, 5g~20g Kynoar and 50ml~100ml
Alkanone obtains grume colloid after mixing, and later by tablet press machine compression moulding, blocky ferric phosphate is obtained after dry
Lithium electrode.
3. preparation method according to claim 1, which is characterized in that step（1）Described in aluminium salt be aluminium ethide, butyl
One kind in aluminium, aluminium acetate, aluminium triformate, oxalic acid aluminium and propionic acid aluminium.
4. according to preparation method described in claim 1, which is characterized in that step（1）And step（2）Described in electrochemical deposition
Method is one kind in cyclic voltammetry, constant-voltage method, constant flow method and impulse method.
5. according to preparation method described in claim 1, which is characterized in that step（2）Described in lithium salts be lithium carbonate, hydroxide
One kind in lithium, lithium metaaluminate, lithium perchlorate and lithium zirconate.
6. a kind of LiFePO4 combination electrode prepared by claim 1-6 any one of them preparation methods, which is characterized in that
The LiFePO4 combination electrode is by LiFePO4 and its is deposited on the aluminium salt on surface and its lithium salts forms, and mass ratio is：
LiFePO4：Aluminium salt：Lithium salts is 100：1~5：1~5.
7. application of the LiFePO4 combination electrode in LiFePO4 combination electrode described in a kind of claim 6, feature exist
In the ferric phosphate lithium cell is mainly by LiFePO4 combination electrode, graphite cathode material, ceramic diaphragm and its functional electric
Solve liquid composition.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109244463A (en) * | 2018-11-20 | 2019-01-18 | 贵州大学 | A kind of preparation method of LITHIUM BATTERY material ferric lithium phosphate |
| CN113611836A (en) * | 2021-08-03 | 2021-11-05 | 中山大学 | High-power high-energy-density lithium iron phosphate composite electrode material and preparation method thereof |
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| CN113611836B (en) * | 2021-08-03 | 2023-09-15 | 中山大学 | High-power high-energy-density lithium iron phosphate composite electrode material and preparation method thereof |
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