CN109728258B - Dispersing process of lithium iron phosphate cathode material - Google Patents
Dispersing process of lithium iron phosphate cathode material Download PDFInfo
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- CN109728258B CN109728258B CN201711035683.4A CN201711035683A CN109728258B CN 109728258 B CN109728258 B CN 109728258B CN 201711035683 A CN201711035683 A CN 201711035683A CN 109728258 B CN109728258 B CN 109728258B
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a dispersion process of a lithium iron phosphate positive electrode material containing a graphene conductive agent, aiming at effectively shortening the time of a homogenate dispersion process and saving the industrial production cost based on improvement of the specific energy and the cycle performance of the lithium iron phosphate battery. The method is characterized in that: the method comprises the steps of baking, obtaining a conductive agent, preparing conductive slurry, preparing conductive colloid and preparing lithium iron phosphate anode slurry. The conductive agent is prepared into the conductive colloid, so that the conductive colloid is fully fused without being laid aside, the time of a homogenate process is greatly shortened, the cost is reduced, and the resource waste is reduced. And the surface activity of the graphene is changed by dispersing for four times, including adding a dispersing agent, and continuously shearing by using the extreme shearing force of the superfine particle crusher, so that the prepared slurry is uniformly dispersed and has good stability.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a dispersion process of a lithium iron phosphate positive electrode material containing a graphene conductive agent.
Background
The lithium iron phosphate battery is a battery made of a lithium iron phosphate positive electrode material, has the advantages of high multiplying power, long cycle life, high safety performance, low cost and no environmental pollution, and is widely applied to the field of electric vehicles. With the development of the domestic electric vehicle industry and the implementation of the state of falling to the ground of new energy electric vehicle subsidy policy, the lithium ion battery as the heart of the electric vehicle is paid more and more attention and tests; according to the letter of industry and Ministry of science and technology and the finance department, namely the notice of technical innovation engineering project of new energy automobile industry in 2012 of organization declaration, the specific energy of the battery monomer is definitely required to reach more than 150Wh/kg, and the specific energy of the battery monomer reaches 300Wh/kg in 2020; therefore, the research on batteries with higher energy density and excellent cycle performance will be the focus of all battery enterprises.
Compared with a nickel-cobalt-manganese ternary material, the lithium iron phosphate material has an orthorhombic olivine structure, and after lithium ions are extracted/embedded, the crystal structure is hardly rearranged, so that the lithium iron phosphate material has high safety performance and long cycle life, and becomes a mainstream material of batteries for electric vehicles. But the conductivity of the lithium ion battery is poor, the lithium ion diffusion is slow, and the capacity of the lithium ion battery is difficult to effectively exert by adding a common conductive agent; the nano-scale conductive agent has large specific surface area and high activity, the traditional homogenizing process cannot effectively disperse, agglomeration and accumulation are easily caused, the consistency of the manufactured battery cannot be guaranteed, and potential safety hazards are caused in the charging and discharging test process in the module assembly.
Graphene is used as a two-dimensional crystal which is formed by carbon atoms and has only one layer of atom thickness, and is a novel nano material which is found to be strongest in electric conduction and heat conduction performances so far. The conductive agent is added into a lithium iron phosphate positive electrode material as a conductive agent, so that the diffusion transmission of lithium ions can be effectively improved, the internal resistance of the battery is reduced, the capacity and the cycle performance of the lithium iron phosphate battery are greatly improved, and the improvement on the specific energy of the battery and the improvement on the endurance mileage of an electric vehicle are essentially improved.
The traditional preparation process of the lithium iron phosphate anode slurry has long time, poor dispersion effect of the nano conductive agent and large energy consumption of equipment, causes cost waste for industrial production and is not beneficial to the green and environment-friendly concept of electric vehicle production.
Disclosure of Invention
The invention aims to effectively shorten the time of a homogenizing and dispersing process and save the industrial production cost while improving the specific energy and the cycle performance of the lithium iron phosphate battery.
The invention is realized by the following steps:
a dispersing process of a lithium iron phosphate positive electrode material specifically comprises the following steps:
the method comprises the following steps: and (3) respectively baking the lithium iron phosphate material, the conductive carbon black (Super P-Li), the graphite powder (KS-6) and the graphene for 8 hours in vacuum under the pressure of-0.095 MPa and the temperature of 120 +/-5 ℃. Respectively baking dispersant (Hypermer KD-1) and polyvinylidene fluoride under vacuum at-0.095 MPa and 80 + -5 deg.C for 3 hr. After the baking is finished, naturally cooling to below 50 ℃ for use.
Step two: adding conductive carbon black (Super P-Li), graphite powder (KS-6) and graphene into a ball-milling mixing tank according to the mass ratio of 1:1:1, wherein the total mass ratio of the conductive carbon black (Super P-Li), the graphite powder (KS-6) and the graphene to the total mass ratio of medium and small ceramic balls is 1:1, the diameter of the medium ceramic ball is 40mm, the diameter of the small ceramic ball is 20mm, the mass ratio of the medium and small ceramic balls is 1:1, and the ball-milling mixing tank is dispersed for 30-60 min at the rotating speed of 30r/min to obtain the conductive agent.
Step three: and (3) mixing the conductive agent (comprising conductive carbon black (Super P-Li), graphite powder (KS-6) and graphene), the dispersing agent and N-methylpyrrolidone after the second dispersion step is finished according to the weight ratio of 4.5: 0.5: adding 95 percent of the mixture into an ultrafine particle grinder; the superfine particle crusher is used for high-speed circulating dispersion for 30-60 min at the rotating speed of 2000-2500 r/min and the gap of 10-30 microns to prepare the conductive slurry.
Step four: and (3) adding polyvinylidene fluoride and the conductive slurry prepared in the third step into a planetary dispersing machine according to the mass ratio of 2-5%, performing vacuum dispersion at the rotating speed of revolution of 15-35 r/min and rotation of 1500-3500 r/min for 3-6 h, preparing a conductive colloid after the dispersion is completed, and taking out the conductive colloid from the planetary dispersing machine.
Step five: adding the lithium iron phosphate anode material into the prepared conductive colloid with the mass ratio of 30-70%, putting the conductive colloid into another planetary dispersion machine, and dispersing for 1-4 h at a revolution speed of 15-35 r/min and a rotation speed of 1000-3500 r/min. And after the dispersion is finished, adding 10% of N-methyl pyrrolidone, and performing vacuum dispersion for 0.5-3 h by using a revolution rotating speed of 15-35 r/min and a rotation rotating speed of 1000-3500 r/min to prepare the lithium iron phosphate anode slurry with required solid content and viscosity.
The polyvinylidene fluoride PVDF used above is us Solef 5130. The graphene is prepared by a graphite oxide reduction method. The dispersant used was British grass big Hypermer KD-1.
The invention has the beneficial effects that:
firstly, SP, KS-6 and graphene are preliminarily mixed by a ball milling and mixing method, so that the three conductive agents are subjected to primary dispersion mixing.
And secondly, adding the preliminarily dispersed conductive agent and the dispersing agent into the azomethine pyrrolidone, and performing high-speed shearing at micron-level gaps by using an ultrafine particle crusher to prepare uniformly dispersed conductive agent slurry.
And then, adding a polyvinylidene fluoride binder, and dispersing for the third time by using a planetary dispersing machine to obtain the conductive colloid after the dispersion is finished.
And then adding a lithium iron phosphate anode material, and performing high-efficiency high-viscosity dispersion by controlling the solid content of the slurry, so that the main material is fully fused with the conductive agent and the binder.
And finally, the nitrogen methyl pyrrolidone is added to adjust the viscosity of the slurry, so that the prepared lithium iron phosphate anode slurry has a good dispersing effect, moderate viscosity and excellent coating performance.
The conventional industrial production method needs 4-5 h of dispersed polyvinylidene fluoride and is used after being placed for 12-24 h. And the conductive agent is directly added into the solvent for planetary dispersion, so that the nano-scale conductive agent cannot be uniformly dispersed.
The conductive agent is prepared into the conductive colloid, so that the conductive colloid is fully fused without being laid aside, the time of a homogenate process is greatly shortened, the cost is reduced, and the resource waste is reduced. And the surface activity of the graphene is changed by dispersing for four times, including adding a dispersing agent, and continuously shearing by using the extreme shearing force of the superfine particle crusher, so that the prepared slurry is uniformly dispersed and has good stability.
Drawings
Fig. 1 is a comparison of the discharge capacity of a 5Ah pouch battery manufactured by the dispersion process of a lithium iron phosphate positive electrode material according to the present invention and a conventional battery using a material that does not contain a graphene conductive agent, wherein the upper curve is the discharge capacity of the battery manufactured by the process of the present invention;
fig. 2 is a comparison of the discharge capacity retention rate of a 5Ah soft package battery manufactured by the dispersion process of the lithium iron phosphate positive electrode material of the present invention and a conventional battery using a material not containing a graphene conductive agent for 1000 times, wherein the upper curve is the discharge capacity retention rate of the battery manufactured by the process of the present invention.
Detailed Description
The invention is further described below with reference to the figures and examples.
A dispersion process of a lithium iron phosphate positive electrode material containing a graphene conductive agent comprises the steps of carrying out vacuum baking on a lithium iron phosphate material, conductive carbon black (Super P-Li), graphite powder (KS-6) and graphene at 120 +/-5 ℃ for 8 hours. Hypermer KD-1, carrying out vacuum baking on polyvinylidene fluoride at 80 +/-5 ℃ for 3 h. And (4) timing when the temperature reaches the required temperature, and naturally cooling to below 50 ℃ for use after the baking is finished. Adding Super P-Li, KS-6 and graphene into a ball-milling mixing tank according to the mass ratio of 1:1:1, adding medium and small ceramic balls (with the diameter of 40mm and the diameter of 20mm) according to the material ratio of 1:1 (the ratio is 1:1), and dispersing for 30min at the rotating speed of 30 r/min. And (3) dispersing the conductive agent after the dispersion, Hypermer KD-1, N-methyl pyrrolidone in a mass ratio of 4.5: 0.5: 95, adding the mixture into an ultrafine particle grinder, using the mixture at 2000r/min, and performing high-speed circulating dispersion for 30min at a gap of 10 microns to prepare the conductive slurry. Polyvinylidene fluoride and the prepared conductive slurry are mixed according to the proportion of 3:97, and performing vacuum dispersion at revolution speed of 35r/min and rotation speed of 3500r/min for 3h to obtain conductive colloid. Adding the lithium iron phosphate anode material into the prepared conductive colloid, and dispersing at revolution speed of 25r/min and rotation speed of 1000r/min for 2h at a ratio of 6: 4. And after the dispersion is finished, adding a certain amount of N-methyl pyrrolidone, and performing vacuum dispersion for 30min by using a revolution rotating speed of 35r/min and a rotation rotating speed of 3500r/min to prepare the lithium iron phosphate anode slurry with required solid content and viscosity.
The invention firstly prepares a lithium iron phosphate anode material PT30 (Tianjin Stelan energy science and technology Co., Ltd.) graphene (self-made by Beijing Wanyuan industry Co., Ltd.) conductive carbon black (Super P-Li) graphite powder (KS-6)
(TIMCAL Co., Ltd.). Baking was carried out for 8 hours at 120 ℃ using a vacuum oven (Sharp electromechanical device, Inc., of Dongguan Co., Ltd.). Polyvinylidene fluoride (Solef 5130, USA), Hypermer KD-1 (British grass) is baked in a vacuum oven at 80 ℃ for 3 h. And (4) timing when the temperature reaches the required temperature, and naturally cooling to below 50 ℃ for use after the baking is finished. Adding Super P-Li, KS-6 and graphene into a ball-milling mixing tank according to the ratio of 1:1:1, adding medium and small ceramic balls (the diameter is 40mm and the diameter is 20mm) according to the material ratio (1:1) (the ratio is 1:1), and dispersing for 30min at the rotating speed of 30 r/min. And (3) mixing the dispersed conductive agent, Hypermer KD-1, N-methyl pyrrolidone in a ratio of 4.5: 0.5: 95 was charged into an ultrafine particle mill (Japan Zenghain industries Co., Ltd.), and high-speed circulation dispersion was carried out at a rate of 2000r/min with a gap of 10 μm for 30min to prepare a conductive paste. Polyvinylidene fluoride and the prepared conductive paste are added into a planetary dispersion machine (Sharp electromechanical equipment of Dongguan department Co., Ltd.) according to the proportion of 3:97, vacuum dispersion is carried out at the rotating speed of revolution of 35r/min and rotation of 3500r/min for 3h, and the conductive colloid is prepared after the dispersion is finished. Adding a lithium iron phosphate anode material PT3 into the prepared conductive colloid, and dispersing at a revolution speed of 25r/min and a rotation speed of 1000r/min for 2h at a ratio of 6: 4. After the dispersion is finished, adding a certain amount of N-methyl pyrrolidone, and performing vacuum dispersion for 30min at revolution speed of 35r/min and rotation speed of 3500r/min, wherein the vacuum degree is (-0.095MPa), the solid content of the obtained anode slurry is 40-50%, and the viscosity is 3000-8000 MPa; and (3) sieving by using a 150-mesh sieve, so that the finally prepared lithium iron phosphate anode slurry has excellent dispersion consistency and the finished battery has good performance.
The performance ratio of the 5Ah soft package battery prepared by using the dispersion process and the conventional battery prepared by using the graphene-free conductive agent are shown in Table 1, and the discharge capacity ratio is shown in FIG. 1:
TABLE 1 comparison of cell Performance
Compared with the conventional 5Ah soft package battery in a circulating mode, the capacity retention rate of the 5Ah soft package battery prepared by the dispersion process is 99.5% after 1000 times of 1C charging and discharging, and the capacity retention rate of the conventional battery is 91.6%. The cycling curves are shown in figure 2.
The method of carrying out the present invention has been described in detail with reference to the examples, but the present invention is not limited to the examples described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. The prior art can be adopted for the content which is not described in detail in the specification of the invention.
Claims (2)
1. A dispersing process of a lithium iron phosphate positive electrode material specifically comprises the following steps:
the method comprises the following steps: respectively baking the lithium iron phosphate material, the conductive carbon black, the graphite powder and the graphene for 8 hours in vacuum under the pressure of-0.095 MPa and the temperature of 120 +/-5 ℃; respectively baking the dispersing agent and the polyvinylidene fluoride under the pressure of-0.095 MPa and the temperature of 80 +/-5 ℃ for 3 hours in vacuum; naturally cooling to below 50 ℃ for use after baking is finished;
step two: adding conductive carbon black, graphite powder and graphene into a ball-milling material mixing tank according to the mass ratio of 1:1:1, wherein the total mass ratio of the conductive carbon black, the graphite powder and the graphene to the total mass ratio of medium and small ceramic balls is 1:1, the mass ratio of the medium ceramic ball to the small ceramic ball is 1:1, the ball-milling material mixing tank is used at the rotating speed of 30r/min, and the ball-milling material mixing tank is dispersed for 30-60 min to obtain a conductive agent;
step three: and (3) mixing the conductive agent, the dispersing agent and the N-methyl pyrrolidone after the dispersion in the second step is finished according to the weight ratio of 4.5: 0.5: adding 95 percent of the mixture into an ultrafine particle grinder; the superfine particle crusher is used for high-speed circulating dispersion for 30min to 60min by using a rotating speed of 2000r/min to 2500r/min and a gap of 10 microns to 30 microns to prepare conductive slurry;
step four: adding polyvinylidene fluoride and the conductive slurry prepared in the third step into a planetary dispersing machine according to the mass ratio of 2% -5%, performing vacuum dispersion at the rotating speed of 1500 r/min-3500 r/min by using revolution of 15 r/min-35 r/min and rotation of 1500 r/min-3500 r/min for 3 h-6 h, preparing a conductive colloid after the dispersion is completed, and taking out the conductive colloid from the planetary dispersing machine;
step five: adding the lithium iron phosphate anode material into the prepared conductive colloid, wherein the adding mass ratio is 30-70%, putting the conductive colloid into another planetary dispersing machine, and dispersing for 1-4 h by using the revolution rotating speed of 15-35 r/min and the rotation rotating speed of 1000-3500 r/min; and adding 10% of N-methyl pyrrolidone into the dispersed conductive colloid, and performing vacuum dispersion for 0.5 h-3 h by using a revolution rotating speed of 15 r/min-35 r/min and a rotation rotating speed of 1000 r/min-3500 r/min to prepare the lithium iron phosphate anode slurry with required solid content and viscosity.
2. The dispersion process of the lithium iron phosphate positive electrode material according to claim 1, characterized in that: the polyvinylidene fluoride used above is us Solef 5130; the graphene is prepared by a graphite oxide reduction method; the dispersant used was British grass big Hypermer KD-1.
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Effective date of registration: 20221013 Address after: No.8, Huancheng Road, Fengcheng Town, Tianzhu County, Qiandongnan Miao and Dong Autonomous Prefecture, Guizhou 556600 Patentee after: Wu Weiyue Address before: 100176 Aerospace Science Park, No. 6, Jinxiu Street, Beijing Economic and Technological Development Zone, Daxing District, Beijing Patentee before: BEIJING WANYUAN INDUSTRY Co.,Ltd. |