CN108054360B - Fluorinated lithium iron sulfate cathode material for low-temperature lithium battery and preparation method thereof - Google Patents
Fluorinated lithium iron sulfate cathode material for low-temperature lithium battery and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of novel electrochemical energy storage materials, in particular to a fluorinated lithium iron sulfate cathode material for a low-temperature lithium battery and a preparation method thereof, wherein the preparation method comprises the following steps: (1) weighing ferrous sulfate heptahydrate, heating, and putting the ferrous sulfate heptahydrate, titanium oxide and tin oxide into a ball mill for ball milling; (2) adding lithium fluoride, dispersing the mixture in an organic solvent, performing reflux reaction, drying and grinding into powder; (3) dispersing the powder into aqueous epoxy resin emulsion, carrying out ultrasonic treatment, and heating to obtain a solid mixture; (4) carrying out flame quenching treatment to obtain the fluorinated lithium iron sulfate; according to the invention, the titanium oxide and the tin oxide are used for doping modification of the fluorinated lithium iron sulfate, so that the conductive channel in the fluorinated lithium iron sulfate is improved, meanwhile, an organic polymer is coated outside the fluorinated lithium iron sulfate and is calcined at a high temperature to obtain an organic carbon coating, and the charge and discharge performance of the anode material at a low temperature is improved.
Description
Technical Field
The invention relates to the technical field of novel electrochemical energy storage materials and preparation thereof, in particular to a fluorinated lithium iron sulfate cathode material for a low-temperature lithium battery and a preparation method thereof.
Background
A lithium ion battery, which is a chemical power source, uses two compounds capable of reversibly intercalating and deintercalating lithium ions as positive and negative electrodes, respectively, and lithium ions are deintercalated from the positive electrode and intercalated into the negative electrode when the battery is charged, and vice versa when the battery is discharged. The lithium ion battery mainly comprises a pole core and a non-aqueous electrolyte, wherein the pole core is sealed in a battery shell and comprises a battery electrode and a diaphragm, the battery electrode comprises a positive pole and a negative pole, and the positive pole comprises a current collector and a positive pole material coated and/or filled on the current collector.
LiCoO is a common lithium battery cathode material at present2、LiMn2O4、LiFePO4And LiNi1/3Co1/3Mn1/3O2Etc. in which LiMn2O4And LiFePO4Suitable for power batteries, LiCoO2And LiNi1/3Co1/3Mn1/3O2It is suitable for 3C electronic products. LiFeSO4F as a novel sulfate polyanion material not only has the outstanding advantages of low price, environmental protection and the like, but also is in common use with the layered material LiCoO2And spinel type material LiMn2O4Compared with the anode material, LiFeSO4F has better safety, and in the field of power batteries, the advantages enable LiFeSO4F becomes a novel anode material with great development potential. Lithium iron phosphate (LiFePO) at 3.45V4) Fluorine ions are introduced into the anion groups of the cathode material, and the lithium iron fluorophosphate (LiFePO) with the Tavorite structure can be obtained4F) The ion conductivity is improved by more than two orders of magnitude, but the working potential is reduced to 2.8V. If SO4 is used2-Radical substitution of PO43-Lithium iron fluorosulfate (LiFeSO) with two structures can be obtained4F) One is a Tavorite structure, and the voltage platform is 3.6V; the other is a Triplite structure, and the voltage platform is 3.9V. The latter having an ionic conductivity of 7X 10 at 25 deg.C-11S/cm, 4X 10 of ionic conductivity at 147 deg.C-6S/cm, which provides favorable precondition for preparing the lithium ion battery with excellent cycle performance and rate performance, good thermal stability and high safety.
However, LiFeSO4The electronic conductivity and the ion diffusion rate of F are low, so that the charge and discharge capacity of F under high rate is hindered, and particularly LiFeSO is formed at low temperature4F has poor charge and discharge properties.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a fluorinated lithium iron sulfate anode material for a low-temperature lithium battery, and the prepared fluorinated lithium iron sulfate has higher electronic conductivity and greatly improves the charge and discharge performance at low temperature.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a fluorinated lithium iron sulfate anode material for a low-temperature lithium battery comprises the following steps:
(1) weighing ferrous sulfate heptahydrate, heating to 60-80 ℃, preserving heat for 3-4 hours, and then mixing with titanium oxide and tin oxide according to a weight ratio of 1: (0.2-0.8) putting the mixture into a ball mill together, and ball-milling for 3-5 h at the speed of 100-300 r/min;
(2) adding lithium fluoride into the mixture obtained in the step (1), continuously performing ball milling for 1-3 hours, dispersing the mixture into an organic solvent, refluxing for 3-5 hours at 240-280 ℃, cooling to room temperature, cleaning with an acetone solution, and then placing into a vacuum oven for drying and crushing into powder for later use;
(3) dispersing the powder in the step (2) into an aqueous epoxy resin emulsion, carrying out ultrasonic treatment for 1-2 h, and heating to 60-90 ℃ while carrying out ultrasonic treatment to obtain a solid mixture;
(4) and (3) carrying out flame quenching treatment on the solid mixture to carbonize a surface coating layer of the solid mixture to obtain the fluorinated lithium iron sulfate.
According to the preparation method provided by the invention, titanium oxide and tin oxide are doped in the preparation of the lithium iron fluoride sulfate, and a conductive channel is formed inside the lithium iron fluoride sulfate anode material due to the existence of the two phases, so that the internal electron mobility of the anode material is improved; an epoxy resin cladding is introduced on the surface of the modified fluorinated lithium iron sulfate, and organic carbon is formed after high-temperature calcination, so that the co-permeation of the electrolyte to the anode material is reduced, and the charge and discharge performance of the electrolyte under the low-temperature condition is improved.
Further, according to the invention, in order to prevent the heating dehydration process of the ferrous sulfate heptahydrate from being influenced by the outside, the heating dehydration process is carried out in an atmosphere protected by inert gas, specifically, argon and nitrogen can be used for protection; the ferrous sulfate heptahydrate loses crystal water after being heated to form ferrous sulfate monohydrate; the ball milling is carried out after the iron oxide and the tin oxide are mixed, so that the particle size distribution is reduced, and the reaction efficiency is improved.
The organic solvent in the step (2) is used for providing a reaction medium, the organic solvent is tetraethyleneglycol, and the iron oxide, the tin oxide, the ferrous sulfate monohydrate and the lithium fluoride which are ground and refined are mixed in the organic solvent to be repeatedly refluxed, so that the lithium fluoride and the ferrous sulfate are subjected to an addition reaction, and the iron oxide and the tin oxide are doped in the organic solvent.
According to the invention, in the step (1), the weight ratio of the ferrous sulfate heptahydrate to the total weight of the mixture of the titanium oxide and the tin oxide is 1: (0.5-0.8).
According to the invention, in the step (2), the addition amount of the lithium fluoride is 0.1-0.3 times of the weight of the ferrous sulfate heptahydrate.
In the step (3), in order to improve the dispersibility of the powder in the aqueous epoxy resin emulsion, the powder is dispersed in the aqueous epoxy resin emulsion and then subjected to ultrasonic treatment, wherein the frequency of the ultrasonic treatment is 20-30 kHz.
In the step (4), the flame quenching temperature is 800-1500 ℃. The thermal decomposition temperature of the fluorinated lithium iron sulfate is lower and is about 450 ℃, so that the conventional carbon coating technology is not suitable for the fluorinated lithium iron sulfate, and in order to carry out carbonization treatment on the organic polymer coated on the surface of the fluorinated lithium iron sulfate, the flame quenching treatment mode is adopted to carbonize the organic polymer coating on the surface of the fluorinated lithium iron sulfate so as to form the fluorinated lithium iron sulfate material coated by organic carbon. Wherein, the titanium oxide, the tin oxide and the fluorinated lithium iron sulfate close to the outer layer are mixed and sintered to form a doped phase. And (2) after coating the aqueous epoxy resin emulsion, calcining at high temperature, doping a mixed phase of titanium oxide and tin oxide in the fluorinated lithium iron sulfate, and forming an organic carbon coating layer on the outer side.
The invention also provides a fluorinated lithium iron sulfate cathode material prepared by the preparation method, and the electronic conductivity of the fluorinated lithium iron sulfate cathode material can reach 3.2-4.5 multiplied by 10-11S/cm。
Compared with the prior art, the invention improves the conductive channel in the lithium iron fluoride sulfate by doping modification of titanium oxide and tin oxide, and simultaneously, the raw material for obtaining the lithium iron fluoride sulfate by reaction is ground and refined, so that the obtained finished product has small particle size; organic polymers are coated outside the fluorinated lithium iron sulfate and are calcined at high temperature to obtain organic carbon coating, so that the charge and discharge performance of the cathode material at low temperature is improved.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified with the specific embodiments.
Example 1
A preparation method of a fluorinated lithium iron sulfate cathode material for a low-temperature lithium battery comprises the following steps:
(1) weighing 1000g of ferrous sulfate heptahydrate, heating to 70 ℃, preserving heat for 3h, putting the ferrous sulfate heptahydrate and a mixture of 450g of titanium oxide and 250g of tin oxide into a ball mill together, and ball-milling for 4h at the speed of 200 r/min;
(2) adding 200g of lithium fluoride into the mixture obtained in the step (1), continuing ball milling for 2h, dispersing the mixture into tetraethyleneglycol, refluxing for 4h at 260 ℃, cooling to room temperature, washing with an acetone solution, and then putting into a vacuum oven for drying and grinding into powder for later use;
(3) dispersing the powder in the step (2) into aqueous epoxy resin emulsion, carrying out ultrasonic treatment for 1h, wherein the frequency of the ultrasonic treatment is 25kHz, and then heating to 70 ℃ while carrying out the ultrasonic treatment to obtain a solid mixture;
(4) and (3) carrying out flame quenching treatment on the solid mixture, wherein the temperature of the flame quenching treatment is 1200 ℃, and carbonizing the surface coating layer of the solid mixture to obtain the fluorinated lithium iron sulfate.
Example 2
A preparation method of a fluorinated lithium iron sulfate cathode material for a low-temperature lithium battery comprises the following steps:
(1) weighing 1000g of ferrous sulfate heptahydrate, heating to 70 ℃, preserving heat for 3h, putting the mixture together with 580g of titanium oxide and 120g of tin oxide into a ball mill, and ball-milling for 4h at the speed of 200 r/min;
(2) adding 200g of lithium fluoride into the mixture obtained in the step (1), continuing ball milling for 2h, dispersing the mixture into tetraethyleneglycol, refluxing for 4h at 260 ℃, cooling to room temperature, washing with an acetone solution, and then putting into a vacuum oven for drying and grinding into powder for later use;
(3) dispersing the powder in the step (2) into aqueous epoxy resin emulsion, carrying out ultrasonic treatment for 1h, wherein the frequency of the ultrasonic treatment is 25kHz, and then heating to 70 ℃ while carrying out the ultrasonic treatment to obtain a solid mixture;
(4) and (3) carrying out flame quenching treatment on the solid mixture, wherein the temperature of the flame quenching treatment is 1200 ℃, and carbonizing the surface coating layer of the solid mixture to obtain the fluorinated lithium iron sulfate.
Example 3
A preparation method of a fluorinated lithium iron sulfate cathode material for a low-temperature lithium battery comprises the following steps:
(1) weighing 1000g of ferrous sulfate heptahydrate, heating to 70 ℃, preserving heat for 3h, putting the ferrous sulfate heptahydrate and a mixture of 400g of titanium oxide and 300g of tin oxide into a ball mill together, and ball-milling for 4h at the speed of 200 r/min;
(2) adding 200g of lithium fluoride into the mixture obtained in the step (1), continuing ball milling for 2h, dispersing the mixture into tetraethyleneglycol, refluxing for 4h at 260 ℃, cooling to room temperature, washing with an acetone solution, and then putting into a vacuum oven for drying and grinding into powder for later use;
(3) dispersing the powder in the step (2) into aqueous epoxy resin emulsion, carrying out ultrasonic treatment for 1h, wherein the frequency of the ultrasonic treatment is 25kHz, and then heating to 70 ℃ while carrying out the ultrasonic treatment to obtain a solid mixture;
(4) carrying out flame quenching treatment on the solid mixture, wherein the temperature of the flame quenching treatment is 1200 ℃, and carbonizing the surface coating layer of the solid mixture to obtain the fluorinated lithium iron sulfate
Example 4
A preparation method of a fluorinated lithium iron sulfate cathode material for a low-temperature lithium battery comprises the following steps:
(1) weighing 1000g of ferrous sulfate heptahydrate, heating to 60 ℃, preserving heat for 3h, putting the mixture and a mixture of 330g of titanium oxide and 170g of tin oxide into a ball mill together, and ball-milling for 5h at the speed of 100 r/min;
(2) adding 100g of lithium fluoride into the mixture obtained in the step (1), continuing ball milling for 1h, dispersing the mixture into tetraethyleneglycol, refluxing for 5h at 240 ℃, cooling to room temperature, washing with an acetone solution, and then putting into a vacuum oven for drying and grinding into powder for later use;
(3) dispersing the powder in the step (2) into aqueous epoxy resin emulsion, carrying out ultrasonic treatment for 1h, wherein the frequency of the ultrasonic treatment is 20kHz, and then heating to 60 ℃ while carrying out the ultrasonic treatment to obtain a solid mixture;
(4) and (3) carrying out flame quenching treatment on the solid mixture, wherein the temperature of the flame quenching treatment is 800 ℃, and carbonizing the surface coating layer of the solid mixture to obtain the lithium iron fluoride sulfate.
Example 5
A preparation method of a fluorinated lithium iron sulfate cathode material for a low-temperature lithium battery comprises the following steps:
(1) weighing 1000g of ferrous sulfate heptahydrate, heating to 80 ℃, preserving heat for 4h, putting the mixture and a mixture of 500g of titanium oxide and 300g of tin oxide into a ball mill together, and ball-milling for 3h at the speed of 300 r/min;
(2) adding 300g of lithium fluoride into the mixture obtained in the step (1), continuing ball milling for 3h, dispersing the mixture into tetraethyleneglycol, refluxing for 3h at 280 ℃, cooling to room temperature, washing with an acetone solution, and then putting into a vacuum oven for drying and grinding into powder for later use;
(3) dispersing the powder in the step (2) into aqueous epoxy resin emulsion, carrying out ultrasonic treatment for 2h, wherein the frequency of the ultrasonic treatment is 30kHz, and then heating to 60 ℃ while carrying out the ultrasonic treatment to obtain a solid mixture;
(4) and (3) carrying out flame quenching treatment on the solid mixture, wherein the temperature of the flame quenching treatment is 1500 ℃, and carbonizing the surface coating layer of the solid mixture to obtain the fluorinated lithium iron sulfate.
And (3) performance testing:
1. conductivity of material
The samples of the examples were pressed into a sheet having a thickness of 1cm, coated with square conductive silver paste on both sides of the sheet and bonded with conductive silver wires, connected to an impedance analyzer (Solartron 1260 type impedance analyzer) to perform the test, and the test results were recorded in table 1.
2. Electrochemical performance test
Preparing the positive electrode material, the conductive additive (Super P) and the adhesive (polyvinylidene fluoride) obtained in the above embodiment into an electrode sheet: dissolving polyvinylidene fluoride into N-methyl pyrrolidone to prepare glue with the mass fraction of 7%, then uniformly mixing a positive electrode material, a conductive auxiliary agent and an adhesive according to the mass ratio of 7:2:1, grinding the mixture into paste, uniformly coating the paste on an aluminum foil, drying the aluminum foil under a baking lamp, finally baking the aluminum foil in a vacuum oven at the temperature of 120 ℃ for 5 hours, cooling the aluminum foil to the room temperature, and cutting the aluminum foil into pieces with the size of 8 multiplied by 8mm2The electrode sheet of (1);
a lithium sheet is used as a negative electrode, a polypropylene film is used as a diaphragm, lithium hexafluorophosphate is used as a solute, a solution in which ethylene carbonate and ethylene carbonate are mixed and used as a solvent is used as an electrolyte, a button cell is assembled in a glove box under an argon protective atmosphere, a charge-discharge tester is used for carrying out constant-current charge-discharge test on the button cell under the room temperature condition, the test result is recorded in a table 1, and a low-temperature incubator (a GX-3000-80L high-low temperature incubator of Gaoxin detection equipment in Dongguan city) is used for setting and meeting the low-temperature condition required by the test.
The test results are recorded in table 1, using the positive electrode material in example 1 of chinese patent "a positive electrode material, a lithium ion battery containing the positive electrode material, and a method for manufacturing the same" disclosed in application No. CN 201710610430.9 "as a control group.
Table 1:
from the data, it can be seen that the fluorinated lithium iron sulfate provided by the invention has excellent charge and discharge performance at low temperature.
The foregoing shows and describes the general principles, essential features, and inventive features of this invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A preparation method of a fluorinated lithium iron sulfate anode material for a low-temperature lithium battery is characterized by comprising the following steps of: the method comprises the following steps:
(1) weighing ferrous sulfate heptahydrate, heating to 60-80 ℃, preserving heat for 3-4 hours, and mixing with a mixture of titanium oxide and tin oxide according to a weight ratio of 1: (0.2-0.8), mixing, putting into a ball mill together, and ball-milling for 3-5 h at the speed of 100-300 r/min;
(2) adding lithium fluoride into the mixture obtained in the step (1), continuously performing ball milling for 1-3 hours, dispersing the mixture into an organic solvent, refluxing for 3-5 hours at 240-280 ℃, cooling to room temperature, cleaning with an acetone solution, and then placing into a vacuum oven for drying and crushing into powder for later use;
(3) dispersing the powder in the step (2) into an aqueous epoxy resin emulsion, carrying out ultrasonic treatment for 1-2 h, and heating to 60-90 ℃ while carrying out ultrasonic treatment to obtain a solid mixture;
(4) and (3) carrying out flame quenching treatment on the solid mixture to carbonize a surface coating layer of the solid mixture to obtain the fluorinated lithium iron sulfate.
2. The method for preparing the fluorinated lithium iron sulfate cathode material for the low-temperature lithium battery as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the heating of the ferrous sulfate heptahydrate is carried out in the atmosphere protected by inert gas.
3. The method for preparing the fluorinated lithium iron sulfate cathode material for the low-temperature lithium battery as claimed in claim 1, wherein the method comprises the following steps: the weight ratio of the ferrous sulfate heptahydrate to the total weight of the mixture of titanium oxide and tin oxide is 1: (0.5-0.8).
4. The method for preparing the fluorinated lithium iron sulfate cathode material for the low-temperature lithium battery as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the addition amount of the lithium fluoride is 0.1-0.3 times of the weight of the ferrous sulfate heptahydrate.
5. The method for preparing the fluorinated lithium iron sulfate cathode material for the low-temperature lithium battery as claimed in claim 1, wherein the method comprises the following steps: in the step (3), the frequency of ultrasonic treatment is 20-30 kHz.
6. The method for preparing the fluorinated lithium iron sulfate cathode material for the low-temperature lithium battery as claimed in claim 1, wherein the method comprises the following steps: in the step (4), the flame quenching temperature is 800-1500 ℃.
7. The fluorinated lithium iron sulfate cathode material for the low-temperature lithium battery is characterized in that: the fluorinated lithium iron sulfate cathode material is prepared by the preparation method of any one of claims 1 to 6.
8. The fluorinated lithium iron sulfate cathode material for a low-temperature lithium battery as claimed in claim 7, wherein: the electronic conductivity of the fluorinated lithium iron sulfate anode material is 3.2-4.5 multiplied by 10-11S/cm。
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| CN101935072A (en) * | 2010-08-26 | 2011-01-05 | 中国科学院化学研究所 | Ferrous lithium sulphate fluoride as well as preparation method and application thereof |
| CN102332580A (en) * | 2011-03-15 | 2012-01-25 | 中国科学院物理研究所 | Fluorinated ferric sulfate salt compound as well as preparation method and application thereof |
| CN102939262A (en) * | 2010-05-17 | 2013-02-20 | 国立科学研究中心 | Method for preparing alkali metal and transition metal fluorosulfates |
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| CN102939262A (en) * | 2010-05-17 | 2013-02-20 | 国立科学研究中心 | Method for preparing alkali metal and transition metal fluorosulfates |
| CN101935072A (en) * | 2010-08-26 | 2011-01-05 | 中国科学院化学研究所 | Ferrous lithium sulphate fluoride as well as preparation method and application thereof |
| CN102332580A (en) * | 2011-03-15 | 2012-01-25 | 中国科学院物理研究所 | Fluorinated ferric sulfate salt compound as well as preparation method and application thereof |
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