CN109713357B - Preparation method of ferrotitanium lithium battery - Google Patents

Preparation method of ferrotitanium lithium battery Download PDF

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CN109713357B
CN109713357B CN201711015730.9A CN201711015730A CN109713357B CN 109713357 B CN109713357 B CN 109713357B CN 201711015730 A CN201711015730 A CN 201711015730A CN 109713357 B CN109713357 B CN 109713357B
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titanium silicon
silicon carbon
iron phosphate
rotating speed
lithium iron
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CN109713357A (en
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吴彬杰
李海军
蔡惠群
魏银仓
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Yinlong New Energy Co Ltd
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    • Y02E60/10—Energy storage using batteries
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Abstract

The invention discloses a preparation method of a ferrotitanium lithium battery, which comprises the steps of preparing titanium silicon carbon negative electrode slurry and lithium iron phosphate positive electrode slurry, then respectively and uniformly coating the lithium iron phosphate positive electrode slurry and the titanium silicon carbon negative electrode slurry on a positive current collector and a negative current collector, drying and pressing to obtain positive and negative pole pieces, and finally assembling to obtain the ferrotitanium lithium battery; thus, the invention adopts titanium silicon carbon as the cathode material, and can utilize the shell, the core and the pomegranate coat in the shell-core pomegranate structure of the titanium silicon carbon to ensure that the titanium silicon carbon cathode material is more stable and reliable than the conventional graphite in the charging and discharging process, thereby further improving the safety and reliability of the battery, prolonging the cycle life of the battery and simultaneously improving the mass ratio energy of the battery.

Description

Preparation method of ferrotitanium lithium battery
Technical Field
The invention belongs to the technical field of lithium ion preparation, and particularly relates to a preparation method of a ferrotitanium lithium battery.
Background
With the development of the technology, the lithium ion battery has a good application prospect in the fields of electric automobiles and energy storage, and will certainly have a profound influence on the life of people in the future.
The cathode of the existing lithium iron phosphate battery generally adopts a pure graphite material, and the hexagonal layered structure of the graphite material is not beneficial to maintaining the stable structure in the charging and discharging process; graphite is a combustible substance and is not beneficial to controlling the stability of the battery under the thermal runaway state; meanwhile, particle pulverization failure is caused by expansion and contraction of graphite in charging and discharging, the cycle life of the manufactured battery is relatively short, and the requirement for improving the energy density of the battery cannot be met; in addition, the layered structure of graphite results in a long ion migration path during charging and discharging, which makes it impossible to realize high-rate charging, and the discharge capacity under low temperature conditions is also affected.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a ferrotitanium lithium battery.
The invention is realized by the following steps:
step 1: sequentially adding a thickening agent, a first conductive agent, a second conductive agent, a binder and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon negative electrode slurry;
step 2: sequentially adding an adhesive, a first conductive agent, a second conductive agent and a nano lithium iron phosphate active substance into a solvent, and uniformly mixing to obtain lithium iron phosphate anode slurry;
and step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
In the scheme, the titanium silicon carbon cathode slurry in the step 1 comprises the following components in parts by weight: titanium silicon carbon active material: 86.0-99.0 parts of thickening agent: 1.0-5.0 parts of a first conductive agent: 0.2-6.0 parts of a second conductive agent: 0.5-5.0 parts of adhesive: 0.2 to 5.0 parts.
Preferably, the titanium silicon carbon active material is formed by D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm.
In the scheme, the lithium iron phosphate positive electrode slurry in the step 2 comprises the following components in parts by weight: nano lithium iron phosphate active material: 85.0-98.0 parts of adhesive: 1.0-10.0 parts of a first conductive agent: 0.2-4.0 parts of a second conductive agent: 0.5 to 5.0 parts.
Preferably, the nano lithium iron phosphate active material consists of D10Lithium iron phosphate powder, D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mu m, and D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m.
In the scheme, the thickening agent and the adhesive are one or more of polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, polyacrylonitrile, polyacrylate, styrene butadiene rubber emulsion or sodium carboxymethylcellulose.
In the above scheme, the first conductive agent and the second conductive agent are both one or more of carbon nanotubes, amorphous carbon, graphite, graphene, or solid electrolyte.
In the scheme, the solvent is one or more of deionized water, N-methyl pyrrolidone, alcohol or acetone.
In the above scheme, step 1 specifically comprises: step 101, adding a thickening agent into a solvent, and vacuumizing and stirring for 60-120 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
102, adding a first conductive agent into the solution obtained in the step 101, and vacuumizing and stirring for 60-120 min at a revolution speed of 50-200r/min and a rotation speed of 1000-;
103, adding a second conductive agent into the solution obtained in the step 102, and vacuumizing and stirring for 20-100 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
104, adding an adhesive into the solution obtained in the step 103, and vacuumizing and stirring for 20-100 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-5000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa to obtain a solution;
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring for 20-100 min at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa to obtain a solution;
and 106, adjusting the viscosity of the solution obtained in the step 105 to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity is 2000-28000 mPa.S.
In the above scheme, step 2 specifically comprises: step 201, adding an adhesive into a solvent, and vacuumizing and stirring for 60-120 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
step 202, adding a first conductive agent into the solution obtained in the step 201, and vacuumizing and stirring for 60-120 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
step 203, adding a second conductive agent into the solution obtained in the step 202, and performing vacuum pumping and stirring for 20-100 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20 to 100 minutes at a revolution speed of 20 to 200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa to obtain a solution;
and step 205, adjusting the viscosity of the solution obtained in the step 204 to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa · S.
Compared with the prior art, the invention provides a preparation method of a ferrotitanium lithium battery, which comprises the steps of preparing titanium silicon carbon negative electrode slurry and lithium iron phosphate positive electrode slurry, then respectively and uniformly coating the lithium iron phosphate positive electrode slurry and the titanium silicon carbon negative electrode slurry on a positive current collector and a negative current collector, drying and pressing to obtain positive and negative pole pieces, and finally assembling to obtain the ferrotitanium lithium battery; thus, the invention adopts titanium silicon carbon as the cathode material, and can utilize the shell, the core and the pomegranate coat in the shell-core pomegranate structure of the titanium silicon carbon to ensure that the titanium silicon carbon cathode material is more stable and reliable than the conventional graphite in the charging and discharging process, thereby further improving the safety and reliability of the battery, prolonging the cycle life of the battery and simultaneously improving the mass ratio energy of the battery.
Drawings
FIG. 1 is a flow chart of a method for preparing a ferrotitanium lithium battery provided in an embodiment of the present invention;
fig. 2 is a rate charge test chart of a ferrotitanium lithium battery of the method for preparing a ferrotitanium lithium battery provided in embodiment 1 of the present invention;
FIG. 3 is a low-temperature-30 ℃ charge-discharge characteristic curve diagram of a method for preparing a ferrotitanium lithium battery provided in embodiment 1 of the present invention;
fig. 4 is a graph of a 1C charge cycle test of a ferrotitanium lithium battery according to the method for preparing a ferrotitanium lithium battery provided in embodiment 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of a ferrotitanium lithium battery, which is a flow chart and is shown in figure 1, and the method is realized by the following steps:
step 1: sequentially adding a thickening agent, a first conductive agent, a second conductive agent, a binder and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon negative electrode slurry;
wherein the titanium silicon carbon cathode slurry in the step 1 comprises the following components in parts by weight: titanium silicon carbon active material: 86.0-99.0 parts of thickening agent: 1.0-5.0 parts of a first conductive agent: 0.2-6.0 parts of a second conductive agent: 0.5-5.0 parts of adhesive: 0.2 to 5.0 parts.
The step 1 is realized by the following steps: wherein the ambient humidity in the whole preparation process is 1-20% RH, and the ambient temperature is 25 +/-5 ℃.
Step 101, adding a thickening agent into a solvent, and vacuumizing and stirring for 60-120 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
wherein the thickening agent is one or more of polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, polyacrylonitrile, polyacrylate, styrene-butadiene rubber emulsion or sodium carboxymethylcellulose; the solvent is one or more of deionized water, N-methyl pyrrolidone, alcohol or acetone; the thickening agent can provide the stability of the slurry, prevent sedimentation and facilitate the uniform mixing of the subsequent auxiliary agents.
102, adding a first conductive agent into the solution obtained in the step 101, and vacuumizing and stirring for 60-120 min at a revolution speed of 50-200r/min and a rotation speed of 1000-;
wherein the first conductive agent is one or more of carbon nanotubes, amorphous carbon, graphite, graphene or solid electrolyte.
103, adding a second conductive agent into the solution obtained in the step 102, and vacuumizing and stirring for 20-100 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
wherein the second conductive agent is one or more of carbon nanotubes, amorphous carbon, graphite, graphene or solid electrolyte.
The first conductive agent and the second conductive agent are added in sequence according to different powder densities, so that the conductive agents are conveniently dispersed.
104, adding an adhesive into the solution obtained in the step 103, and vacuumizing and stirring for 20-100 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-5000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa to obtain a solution;
wherein the adhesive is one or more of polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, polyacrylonitrile, polyacrylate, styrene butadiene rubber emulsion or sodium carboxymethylcellulose, and the adhesive is added to help the slurry to be well adhered to the foil during coating in the step 3.
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring for 20-100 min at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa to obtain a solution;
wherein the titanium silicon carbon active substance is formed by D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm.
And 106, adjusting the viscosity of the solution obtained in the step 105 to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity is 2000-28000 mPa.S.
Wherein, the viscosity adjusting process comprises the following steps: the mixture is stirred for 20-100 min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa and the revolution rotating speed is 50-200r/min and the rotation rotating speed is 1000-8000 r/min.
Step 2: sequentially adding an adhesive, a first conductive agent, a second conductive agent and a nano lithium iron phosphate active substance into a solvent, and uniformly mixing to obtain lithium iron phosphate anode slurry;
wherein the lithium iron phosphate anode slurry in the step 2 comprises the following components in parts by weight: nano lithium iron phosphate active material: 85.0-98.0 parts of adhesive: 1.0-10.0 parts of a first conductive agent: 0.2-4.0 parts of a second conductive agent: 0.5 to 5.0 parts.
The step 2 is realized by the following steps:
step 201, adding an adhesive into a solvent, and vacuumizing and stirring for 60-120 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
wherein, the adhesive is one or more of polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, polyacrylonitrile, polyacrylate, styrene-butadiene rubber emulsion or sodium carboxymethylcellulose; the solvent is one or more of deionized water, N-methyl pyrrolidone, alcohol or acetone; the binder serves to adhere the powder to the foil and also to prevent settling for slurry stability.
Step 202, adding a first conductive agent into the solution obtained in the step 201, and vacuumizing and stirring for 60-120 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
wherein the first conductive agent is one or more of carbon nanotubes, amorphous carbon, graphite, graphene or solid electrolyte.
Step 203, adding a second conductive agent into the solution obtained in the step 202, and performing vacuum pumping and stirring for 20-100 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
wherein the second conductive agent is one or more of carbon nanotubes, amorphous carbon, graphite, graphene or solid electrolyte.
The first conductive agent and the second conductive agent are added in sequence according to different powder densities, so that the conductive agents are conveniently dispersed.
Step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20 to 100 minutes at a revolution speed of 20 to 200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa to obtain a solution;
wherein the nano lithium iron phosphate active material is composed of D10Lithium iron phosphate powder, D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mu m, and D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m.
And step 205, adjusting the viscosity of the solution obtained in the step 204 to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa · S.
Wherein, the viscosity adjusting process comprises the following steps: the mixture is stirred for 20-100 min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa and the revolution rotating speed is 50-200r/min and the rotation rotating speed is 1000-8000 r/min.
And step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
The invention has proposed a ferrotitanium lithium preparation method of cell, at first, adopt titanium silicon carbon negative pole material, can utilize "shell", "core" and "pomegranate overcoat" in its "shell-core pomegranate structure", in order to guarantee the silicon carbon negative pole material is more stable and more reliable than the conventional graphite in the course of charging and discharging, in this way, make the safe reliability of the battery promoted on the one hand, on the other hand make the battery cycle life made prolong; secondly, the difference between the 'core-shell-pomegranate structure' of the titanium silicon carbon negative electrode material and the conventional graphite (the ions migrate and are embedded from the graphite layer in a single direction) is that the migration and embedding mode of ions in the charging and discharging process is multi-directional (the ions can migrate and are embedded from any direction of the 'pomegranate structure' to the center of the 'core'), so that the titanium silicon carbon material has higher gram specific capacity than the graphite, and in addition, the powder shell is coated by a titanium-containing substance, so that the titanium silicon carbon negative electrode material has lower temperature discharging capacity and quick charging capacity; finally, the theoretical capacity of the silicon reaches 4200Ah/kg, which is far higher than that of the existing graphite, so that the mass specific energy of the battery is further improved.
Example 1
Step 1: the titanium silicon carbon cathode slurry comprises the following components in parts by weight: titanium silicon carbon active material: 92.0 parts, polytetrafluoroethylene: 3.0 parts, carbon nanotube: 3.0 parts, graphene:2.8 parts of epoxy resin: 2.6 parts; sequentially adding polytetrafluoroethylene, a carbon nanotube, graphene, epoxy resin and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon cathode slurry; wherein the titanium silicon carbon active substance is formed by D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm; wherein the solvent is deionized water and N-methyl pyrrolidone.
The step 1 is realized by the following steps:
step 101, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
102, adding carbon nanotubes into the solution obtained in the step 101, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
103, adding graphene into the solution obtained in the step 102, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
104, adding epoxy resin into the solution obtained in the step 103, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
and step 106, performing viscosity adjustment on the solution obtained in the step 105 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform, so as to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity of the titanium silicon carbon negative electrode slurry is 2000-28000 mPa & S.
Step 2: the lithium iron phosphate anode slurry comprises the following components in parts by weight: nano lithium iron phosphate active material: 91.0 parts of polytetrafluoroethylene: 5.0 parts, carbon nanotube: 2.0 part, graphene: 2.8 parts of polytetrafluoroethylene, a carbon nanotube, graphene and a nano lithium iron phosphate active material are sequentially added into a solvent and uniformly mixed to obtain lithium iron phosphate anode slurry; wherein the nano lithium iron phosphate active material is composed of D10Lithium iron phosphate powder, D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mu m, and D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m, and the solvent is deionized water and N-methyl pyrrolidone.
The step 2 is realized by the following steps:
step 201, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa;
202, adding carbon nanotubes into the solution obtained in the step 201, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 203, adding graphene into the solution obtained in the step 202, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 20-200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
step 205, performing viscosity adjustment on the solution obtained in the step 204 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa & S;
and step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
As shown in fig. 2, it can be seen from the graph that the rate charge test chart of the ferrotitanium lithium battery prepared by the method for preparing a ferrotitanium lithium battery provided in embodiment 1 of the present invention shows that the 1C charging efficiency, the 2C charging efficiency, the 3C charging efficiency and the 4C charging efficiency can all reach more than 90%; a charge-discharge characteristic curve diagram at the low temperature of minus 30 ℃ is shown in figure 3, and it can be seen from the figure that the charge-discharge efficiency reaches 60 percent when the ferrotitanium lithium battery is charged and discharged at the low temperature of minus 30 ℃; the 1C charging cycle test curve diagram of the ferrotitanium lithium battery is a charging and discharging cycle test of the ferrotitanium lithium battery at normal temperature, and the graph shows that the capacity retention rate is more than 80% after 10000 cycles of 1C charging and discharging cycle; aiming at the safe reliability of the battery, a needling experiment is carried out on the ferrotitanium lithium battery, and the experiment shows that the ferrotitanium lithium battery has no phenomena of fire and explosion, so that the safe reliability of the ferrotitanium lithium battery can meet the application requirement.
Example 2
Step 1: the titanium silicon carbon cathode slurry comprises the following components in parts by weight: titanium silicon carbon active material: 86.0 parts of polytetrafluoroethylene: 3.0 parts, carbon nanotube: 6.0 parts, graphene: 2.8 parts of epoxy resin: 2.6 parts; sequentially adding polytetrafluoroethylene, a carbon nanotube, graphene, epoxy resin and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon cathode slurry; wherein the titanium silicon carbon active substance is formed by D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm; wherein the solvent is deionized water and N-methyl pyrrolidone.
The step 1 is realized by the following steps:
step 101, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
102, adding carbon nanotubes into the solution obtained in the step 101, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
103, adding graphene into the solution obtained in the step 102, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
104, adding epoxy resin into the solution obtained in the step 103, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
and step 106, performing viscosity adjustment on the solution obtained in the step 105 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform, so as to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity of the titanium silicon carbon negative electrode slurry is 2000-28000 mPa & S.
Step 2: the lithium iron phosphate anode slurry comprises the following components in parts by weight: nano lithium iron phosphate active material: 85.0 parts of polytetrafluoroethylene: 5.0 parts, carbon nanotube: 4.0 part, graphene: 2.8 parts of polytetrafluoroethylene, a carbon nanotube, graphene and a nano lithium iron phosphate active material are sequentially added into a solvent and uniformly mixed to obtain lithium iron phosphate anode slurry; wherein the nano lithium iron phosphate active material is composed of D10Lithium iron phosphate powder、D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mu m, and D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m, and the solvent is deionized water and N-methyl pyrrolidone.
The step 2 is realized by the following steps:
step 201, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa;
202, adding carbon nanotubes into the solution obtained in the step 201, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 203, adding graphene into the solution obtained in the step 202, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 20-200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
step 205, performing viscosity adjustment on the solution obtained in the step 204 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa & S;
and step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
The performance test of the ferrotitanium lithium battery prepared in the embodiment 2 is performed, the test result is similar to that of the embodiment 1, and the 1C charging efficiency, the 2C charging efficiency, the 3C charging efficiency and the 4C charging efficiency can reach more than 90%; the ferrotitanium lithium battery is charged and discharged at the low temperature of minus 30 ℃, and the charging and discharging efficiency reaches 60 percent; the ferrotitanium lithium battery is subjected to charge-discharge cycle test at normal temperature, and the capacity retention rate is more than 80% after 10000 cycles of 1C charge-discharge cycle; acupuncture experiments show that the ferrotitanium lithium battery has no phenomena of fire and explosion, so that the safety and reliability of the ferrotitanium lithium battery can meet the application requirements.
Example 3
Step 1: the titanium silicon carbon cathode slurry comprises the following components in parts by weight: titanium silicon carbon active material: 99.0 parts of polytetrafluoroethylene: 3.0 parts, carbon nanotube: 0.2 part, graphene: 2.8 parts of epoxy resin: 2.6 parts; sequentially adding polytetrafluoroethylene, a carbon nanotube, graphene, epoxy resin and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon cathode slurry; wherein the titanium silicon carbon active substance is formed by D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm; wherein the solvent is deionized water and N-methyl pyrrolidone.
The step 1 is realized by the following steps:
step 101, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
102, adding carbon nanotubes into the solution obtained in the step 101, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
103, adding graphene into the solution obtained in the step 102, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
104, adding epoxy resin into the solution obtained in the step 103, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
and step 106, performing viscosity adjustment on the solution obtained in the step 105 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform, so as to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity of the titanium silicon carbon negative electrode slurry is 2000-28000 mPa & S.
Step 2: the lithium iron phosphate anode slurry comprises the following components in parts by weight: nano lithium iron phosphate active material: 98.0 parts of polytetrafluoroethylene: 5.0 parts, carbon nanotube: 0.2 part, graphene: 2.8 parts of polytetrafluoroethylene, a carbon nanotube, graphene and a nano lithium iron phosphate active material are sequentially added into a solvent and uniformly mixed to obtain lithium iron phosphate anode slurry; wherein the nano lithium iron phosphate active material is composed of D10Lithium iron phosphate powder, D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mu m, and D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m, and the solvent is deionized water and N-methyl pyrrolidone.
The step 2 is realized by the following steps:
step 201, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa;
202, adding carbon nanotubes into the solution obtained in the step 201, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 203, adding graphene into the solution obtained in the step 202, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 20-200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
step 205, performing viscosity adjustment on the solution obtained in the step 204 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa & S;
and step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
The performance test of the ferrotitanium lithium battery prepared in the embodiment 3 is carried out, the test result is similar to that of the embodiment 1, and the 1C charging efficiency, the 2C charging efficiency, the 3C charging efficiency and the 4C charging efficiency can reach more than 90%; the ferrotitanium lithium battery is charged and discharged at the low temperature of minus 30 ℃, and the charging and discharging efficiency reaches 60 percent; the ferrotitanium lithium battery is subjected to charge-discharge cycle test at normal temperature, and the capacity retention rate is more than 80% after 10000 cycles of 1C charge-discharge cycle; acupuncture experiments show that the ferrotitanium lithium battery has no phenomena of fire and explosion, so that the safety and reliability of the ferrotitanium lithium battery can meet the application requirements.
Example 4
Step 1: of titanium silicon carbon cathode slurryComprises the following components in parts by weight: titanium silicon carbon active material: 92.0 parts, polytetrafluoroethylene: 1.0 part, carbon nanotube: 3.0 parts, graphene: 2.8 parts of epoxy resin: 5.0 parts of (B); sequentially adding polytetrafluoroethylene, a carbon nanotube, graphene, epoxy resin and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon cathode slurry; wherein the titanium silicon carbon active substance is formed by D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm; wherein the solvent is deionized water and N-methyl pyrrolidone.
The step 1 is realized by the following steps:
step 101, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
102, adding carbon nanotubes into the solution obtained in the step 101, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
103, adding graphene into the solution obtained in the step 102, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
104, adding epoxy resin into the solution obtained in the step 103, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
and step 106, performing viscosity adjustment on the solution obtained in the step 105 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform, so as to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity of the titanium silicon carbon negative electrode slurry is 2000-28000 mPa & S.
Step 2: the lithium iron phosphate anode slurry comprises the following components in parts by weight: nano lithium iron phosphate active material: 91.0 parts of polytetrafluoroethylene: 1.0 part, carbon nanotube: 2.0 part, graphene: 2.8 parts of polytetrafluoroethylene, a carbon nanotube, graphene and a nano lithium iron phosphate active material are sequentially added into a solvent and uniformly mixed to obtain lithium iron phosphate anode slurry; wherein the nano lithium iron phosphate active material is composed of D10Lithium iron phosphate powder, D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mu m, and D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m, and the solvent is deionized water and N-methyl pyrrolidone.
The step 2 is realized by the following steps:
step 201, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa;
202, adding carbon nanotubes into the solution obtained in the step 201, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 203, adding graphene into the solution obtained in the step 202, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 20-200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
step 205, performing viscosity adjustment on the solution obtained in the step 204 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa & S;
and step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
The performance test of the ferrotitanium lithium battery prepared in the embodiment 4 is carried out, the test result is similar to that of the embodiment 1, and the 1C charging efficiency, the 2C charging efficiency, the 3C charging efficiency and the 4C charging efficiency can reach more than 90%; the ferrotitanium lithium battery is charged and discharged at the low temperature of minus 30 ℃, and the charging and discharging efficiency reaches 60 percent; the ferrotitanium lithium battery is subjected to charge-discharge cycle test at normal temperature, and the capacity retention rate is more than 80% after 10000 cycles of 1C charge-discharge cycle; acupuncture experiments show that the ferrotitanium lithium battery has no phenomena of fire and explosion, so that the safety and reliability of the ferrotitanium lithium battery can meet the application requirements.
Example 5
Step 1: the titanium silicon carbon cathode slurry comprises the following components in parts by weight: titanium silicon carbon active material: 92.0 parts, polytetrafluoroethylene: 5.0 parts, carbon nanotube: 3.0 parts, graphene: 2.8 parts of epoxy resin: 0.2 part; sequentially adding polytetrafluoroethylene, a carbon nanotube, graphene, epoxy resin and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon cathode slurry; wherein the titanium silicon carbon active substance is formed by D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm; wherein the solvent is deionized water and N-methyl pyrrolidone.
The step 1 is realized by the following steps:
step 101, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
102, adding carbon nanotubes into the solution obtained in the step 101, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
103, adding graphene into the solution obtained in the step 102, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
104, adding epoxy resin into the solution obtained in the step 103, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
and step 106, performing viscosity adjustment on the solution obtained in the step 105 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform, so as to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity of the titanium silicon carbon negative electrode slurry is 2000-28000 mPa & S.
Step 2: the lithium iron phosphate anode slurry comprises the following components in parts by weight: nano lithium iron phosphate active material: 91.0 parts of polytetrafluoroethylene: 10.0 parts, carbon nanotube: 2.0 part, graphene: 2.8 parts of polytetrafluoroethylene, a carbon nanotube, graphene and a nano lithium iron phosphate active material are sequentially added into a solvent and uniformly mixed to obtain lithium iron phosphate anode slurry; wherein the nano lithium iron phosphate active material is composed of D10Lithium iron phosphate powder, D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mum, said D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m, and the solvent is deionized water and N-methyl pyrrolidone.
The step 2 is realized by the following steps:
step 201, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa;
202, adding carbon nanotubes into the solution obtained in the step 201, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 203, adding graphene into the solution obtained in the step 202, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 20-200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
step 205, performing viscosity adjustment on the solution obtained in the step 204 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa & S;
and step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
The performance test of the ferrotitanium lithium battery prepared in the embodiment 5 is carried out, the test result is similar to that of the embodiment 1, and the 1C charging efficiency, the 2C charging efficiency, the 3C charging efficiency and the 4C charging efficiency can reach more than 90%; the ferrotitanium lithium battery is charged and discharged at the low temperature of minus 30 ℃, and the charging and discharging efficiency reaches 60 percent; the ferrotitanium lithium battery is subjected to charge-discharge cycle test at normal temperature, and the capacity retention rate is more than 80% after 10000 cycles of 1C charge-discharge cycle; acupuncture experiments show that the ferrotitanium lithium battery has no phenomena of fire and explosion, so that the safety and reliability of the ferrotitanium lithium battery can meet the application requirements.
Example 6
Step 1: the titanium silicon carbon cathode slurry comprises the following components in parts by weight: titanium silicon carbon active material: 92.0 parts, polytetrafluoroethylene: 3.0 parts, carbon nanotube: 0.2 part, graphene: 5.0 parts of epoxy resin: 2.6 parts; sequentially adding polytetrafluoroethylene, a carbon nanotube, graphene, epoxy resin and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon cathode slurry; wherein the titanium silicon carbon active substance is formed by D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm; wherein the solvent is deionized water and N-methyl pyrrolidone.
The step 1 is realized by the following steps:
step 101, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
102, adding carbon nanotubes into the solution obtained in the step 101, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
103, adding graphene into the solution obtained in the step 102, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
104, adding epoxy resin into the solution obtained in the step 103, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
and step 106, performing viscosity adjustment on the solution obtained in the step 105 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform, so as to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity of the titanium silicon carbon negative electrode slurry is 2000-28000 mPa & S.
Step 2: the lithium iron phosphate anode slurry comprises the following components in parts by weight: nano lithium iron phosphate active material: 91.0 parts of polytetrafluoroethylene: 5.0 parts, carbon nanotube: 0.2 part, graphene: 5.0 parts of polytetrafluoroethylene, a carbon nanotube, graphene and a nano lithium iron phosphate active material are sequentially added into a solvent and uniformly mixed to obtain lithium iron phosphate anode slurry; wherein the nano lithium iron phosphate active material is composed of D10Lithium iron phosphate powder, D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mu m, and D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m, and the solvent is deionized water and N-methyl pyrrolidone.
The step 2 is realized by the following steps:
step 201, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa;
202, adding carbon nanotubes into the solution obtained in the step 201, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 203, adding graphene into the solution obtained in the step 202, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 20-200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
step 205, performing viscosity adjustment on the solution obtained in the step 204 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa & S;
and step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
The performance test of the ferrotitanium lithium battery prepared in the embodiment 6 is carried out, the test result is similar to that of the embodiment 1, and the 1C charging efficiency, the 2C charging efficiency, the 3C charging efficiency and the 4C charging efficiency can reach more than 90%; the ferrotitanium lithium battery is charged and discharged at the low temperature of minus 30 ℃, and the charging and discharging efficiency reaches 60 percent; the ferrotitanium lithium battery is subjected to charge-discharge cycle test at normal temperature, and the capacity retention rate is more than 80% after 10000 cycles of 1C charge-discharge cycle; acupuncture experiments show that the ferrotitanium lithium battery has no phenomena of fire and explosion, so that the safety and reliability of the ferrotitanium lithium battery can meet the application requirements.
Example 7
Step 1: the titanium silicon carbon cathode slurry comprises the following components in parts by weight: titanium silicon carbon active material: 92.0 parts, polytetrafluoroethylene: 3.0 parts, carbon nanotube: 6.0 parts, graphene: 0.5 part of epoxy resinFat: 2.6 parts; sequentially adding polytetrafluoroethylene, a carbon nanotube, graphene, epoxy resin and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon cathode slurry; wherein the titanium silicon carbon active substance is formed by D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm; wherein the solvent is deionized water and N-methyl pyrrolidone.
The step 1 is realized by the following steps:
step 101, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
102, adding carbon nanotubes into the solution obtained in the step 101, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
103, adding graphene into the solution obtained in the step 102, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
104, adding epoxy resin into the solution obtained in the step 103, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
and step 106, performing viscosity adjustment on the solution obtained in the step 105 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform, so as to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity of the titanium silicon carbon negative electrode slurry is 2000-28000 mPa & S.
Step 2: the lithium iron phosphate anode slurry comprises the following components in parts by weight: nano lithium iron phosphate active material: 91.0 parts of polytetrafluoroethylene: 5.0 parts, carbon nanotube: 4.0 part, graphene: 0.5 part of polytetrafluoroethylene, a carbon nanotube, graphene and a nano lithium iron phosphate active material are sequentially added into a solvent and uniformly mixed to obtain lithium iron phosphate anode slurry; wherein the nano lithium iron phosphate active material is composed of D10Lithium iron phosphate powder, D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mu m, and D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m, and the solvent is deionized water and N-methyl pyrrolidone.
The step 2 is realized by the following steps:
step 201, adding polytetrafluoroethylene into a solvent, and stirring for 60-120 min to be uniform at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa;
202, adding carbon nanotubes into the solution obtained in the step 201, and vacuumizing and stirring the solution for 60-120 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 203, adding graphene into the solution obtained in the step 202, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 50-200r/min and a rotation speed of 1000-;
step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20-100 min to be uniform at a revolution speed of 20-200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa;
step 205, performing viscosity adjustment on the solution obtained in the step 204 at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-8000r/min under a relative vacuum degree of less than or equal to-0.07 Mpa, vacuumizing and stirring for 20-100 min until the solution is uniform to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa & S;
and step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
The performance test of the ferrotitanium lithium battery prepared in the embodiment 7 is carried out, the test result is similar to that of the embodiment 1, and the 1C charging efficiency, the 2C charging efficiency, the 3C charging efficiency and the 4C charging efficiency can reach more than 90%; the ferrotitanium lithium battery is charged and discharged at the low temperature of minus 30 ℃, and the charging and discharging efficiency reaches 60 percent; the ferrotitanium lithium battery is subjected to charge-discharge cycle test at normal temperature, and the capacity retention rate is more than 80% after 10000 cycles of 1C charge-discharge cycle; acupuncture experiments show that the ferrotitanium lithium battery has no phenomena of fire and explosion, so that the safety and reliability of the ferrotitanium lithium battery can meet the application requirements.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.

Claims (7)

1. A preparation method of a ferrotitanium lithium battery is characterized by comprising the following steps:
step 1: sequentially adding a thickening agent, a first conductive agent, a second conductive agent, a binder and a titanium silicon carbon active substance into a solvent, and uniformly mixing to obtain titanium silicon carbon negative electrode slurry; the titanium silicon carbon anode slurry comprises the following components in parts by weight: titanium silicon carbon active material: 86.0-99.0 parts of thickening agent: 1.0-5.0 parts of a first conductive agent: 0.2-6.0 parts of a second conductive agent: 0.5-5.0 parts of adhesive: 0.2-5.0 parts;
the step 1 specifically comprises the following steps:
step 101, adding a thickening agent into a solvent, and vacuumizing and stirring for 60-120 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
102, adding a first conductive agent into the solution obtained in the step 101, and vacuumizing and stirring for 60-120 min at a revolution speed of 50-200r/min and a rotation speed of 1000-;
103, adding a second conductive agent into the solution obtained in the step 102, and vacuumizing and stirring for 20-100 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
104, adding an adhesive into the solution obtained in the step 103, and vacuumizing and stirring for 20-100 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-5000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa to obtain a solution;
105, adding a titanium silicon carbon active substance into the solution obtained in the step 104, and vacuumizing and stirring for 20-100 min at a revolution rotating speed of 20-200r/min and a rotation rotating speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa to obtain a solution;
106, adjusting the viscosity of the solution obtained in the step 105 to obtain titanium silicon carbon negative electrode slurry, wherein the solid content of the titanium silicon carbon negative electrode slurry is 40.0-75.0%, and the viscosity is 2000-28000 mPa & S;
step 2: sequentially adding an adhesive, a first conductive agent, a second conductive agent and a nano lithium iron phosphate active substance into a solvent, and uniformly mixing to obtain lithium iron phosphate anode slurry; the lithium iron phosphate anode slurry comprises the following components in parts by weight: nano lithium iron phosphate active material: 85.0-98.0 parts of adhesive: 1.0-10.0 parts of a first conductive agent: 0.2-4.0 parts of a second conductive agent: 0.5-5.0 parts;
and step 3: respectively and uniformly coating the lithium iron phosphate anode slurry and the titanium silicon carbon cathode slurry on an anode current collector and a cathode current collector, and drying and pressing to obtain an anode pole piece and a cathode pole piece;
and 4, step 4: and (3) performing diaphragm slitting, winding, casing and baking treatment on the positive pole piece and the negative pole piece to obtain an electric core, and performing liquid injection and formation treatment on the electric core and then assembling to obtain the ferrotitanium lithium battery.
2. A method of making an ilmenite lithium battery as claimed in claim 1, wherein the titanium silicon carbon active material is formed from D10Titanium silicon carbon powder, D50Titanium silicon carbon powder and D90Titanium silicon carbon powder composition, said D10The grain diameter of the titanium silicon carbon powder is 0.8-3.0 mu m, and D50The grain diameter of the titanium silicon carbon powder is 4.0-18.0 mu m, and D90The grain diameter of the titanium silicon carbon powder is less than 25.0 μm.
3. The method of claim 2, wherein the nano lithium iron phosphate active material is formed from D10Lithium iron phosphate powder, D50Lithium iron phosphate powder and D90Iron lithium phosphate powder composition, D10The particle diameter of the lithium iron phosphate powder is 0.8-2.0 mu m, and D50The particle diameter of the lithium iron phosphate powder is 4.0-15.0 mu m, and D90The particle size of the lithium iron phosphate powder is less than 23.0 mu m.
4. The method of claim 3, wherein the thickener and binder are at least one of polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, polyacrylonitrile, polyacrylate, styrene butadiene rubber emulsion, or sodium carboxymethylcellulose.
5. The method according to claim 4, wherein the first and second conductive agents are each at least one of carbon nanotubes, amorphous carbon, graphite, graphene, or solid-state electrolyte.
6. The method of claim 5, wherein the solvent is at least one of deionized water, N-methylpyrrolidone, alcohol, or acetone.
7. A method for preparing an ilmenite lithium battery according to any of claims 1-6, characterized in that the step 2 is specifically realized by the following steps:
step 201, adding an adhesive into a solvent, and vacuumizing and stirring for 60-120 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
step 202, adding a first conductive agent into the solution obtained in the step 201, and vacuumizing and stirring for 60-120 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
step 203, adding a second conductive agent into the solution obtained in the step 202, and performing vacuum pumping and stirring for 20-100 min at a revolution rotating speed of 50-200r/min and a rotation rotating speed of 1000-;
step 204, adding a nano lithium iron phosphate active substance into the solution obtained in the step 203, and vacuumizing and stirring the solution for 20 to 100 minutes at a revolution speed of 20 to 200r/min and a rotation speed of 1000-10000r/min under the condition that the relative vacuum degree is less than or equal to-0.07 Mpa to obtain a solution;
and step 205, adjusting the viscosity of the solution obtained in the step 204 to obtain lithium iron phosphate anode slurry, wherein the solid content of the lithium iron phosphate anode slurry is 40.0-75.0%, and the viscosity is 1800-26000 mPa · S.
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