CN112103479B - Preparation and application of polymer-coated carbon nanotube/ferrous fluoride composite material - Google Patents
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Abstract
The invention relates to a preparation method of a polymer-coated carbon nano tube/ferrous fluoride composite material, which comprises the following steps: (1) and (2) dropwise adding a ferrous hexafluorosilicate aqueous solution on the carbon nano tube modified by Triton X-100, drying, and annealing under argon flow in a tube furnace to obtain the carbon nano tube/ferrous fluoride material. (2) Preparing a lithiated perfluorosulfonic acid polymer solution, soaking a perfluorosulfonic acid polymer in a lithium hydroxide solution, replacing hydrogen atoms in a sulfonate group with lithium atoms to obtain the lithiated perfluorosulfonic acid polymer, dissolving the lithiated perfluorosulfonic acid polymer in dimethyl sulfoxide, and stirring and heating to dissolve the lithiated perfluorosulfonic acid polymer. (3) And dropwise adding the lithiated perfluorosulfonic acid polymer solution on the carbon nano tube/ferrous fluoride material to prepare the lithiated perfluorosulfonic acid polymer coated carbon nano tube/ferrous fluoride composite material. The invention also provides the application of the lithium ion battery positive electrode material.
Description
Technical Field
The invention belongs to the technical field of metal fluoride materials, and particularly relates to a method for preparing a polymer coated carbon nano tube/ferrous fluoride for a lithium metal battery anode material, and specifically the method for improving the cycling stability of the electrode material by utilizing a lithiated perfluorinated sulfonic acid polymer coated carbon nano tube/ferrous fluoride.
Background
In order to meet the requirements of electronic products and electric vehicles for energy storage, the energy storage capacity of the battery needs to be further improved. The conversion-type-based positive electrode material is capable of performing multiple electron transfer reactions, and can release more capacitance than the intercalation-type positive electrode material (0.5-1 electron reaction). The metal fluoride in the electrode material of the conversion type has a higher discharge platform due to the stronger electronegativity of fluorine ions. However, the high electronegativity also results in the electrical insulation of the metal fluoride and the slight solubility of the metal-fluorine ionic bond in a certain voltage range. These lead to the continuous loss of active materials of metal fluorides during the charging and discharging processes and the continuous decrease of the cycle performance of the electrode material.
In order to solve the problems of poor conductivity, trace dissolution and the like of the metal fluoride, the invention provides a method for protecting the loss of metal ions by using a carbon nano tube as a conductive network and coating a lithiated perfluorosulfonic acid polymer on the surface of ferrous fluoride so as to play a role in improving the cycle stability of the metal fluoride.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a method for preparing a polymer-coated carbon nanotube/ferrous fluoride composite material for a lithium metal battery anode material aiming at the problems of poor conductivity, metal ion dissolution and the like of ferrous fluoride in the prior art, wherein the carbon nanotube is favorable for electron transmission of the ferrous fluoride and improves the electrochemical reaction activity of the ferrous fluoride, and the lithiated perfluorosulfonic acid polymer plays a role in inhibiting the loss of metal ions of the ferrous fluoride in the charging and discharging processes. The technical purpose of the invention is realized by the following technical scheme:
a preparation method of a polymer-coated carbon nanotube/ferrous fluoride composite material comprises the following steps:
(1) and (2) dropwise adding a ferrous hexafluorosilicate aqueous solution on the carbon nano tube modified by Triton X-100, drying, and annealing under argon flow in a tube furnace to obtain the carbon nano tube/ferrous fluoride material.
(2) Preparing a lithiated perfluorosulfonic acid polymer solution, soaking a perfluorosulfonic acid polymer in a lithium hydroxide solution, replacing hydrogen atoms in a sulfonate group with lithium atoms to obtain the lithiated perfluorosulfonic acid polymer, dissolving the lithiated perfluorosulfonic acid polymer in dimethyl sulfoxide, and stirring and heating to dissolve the lithiated perfluorosulfonic acid polymer.
(3) And dropwise adding the lithiated perfluorosulfonic acid polymer solution on the carbon nano tube/ferrous fluoride material to prepare the lithiated perfluorosulfonic acid polymer coated carbon nano tube/ferrous fluoride composite material.
Preferably, in the step (1), the aqueous solution of ferrous hexafluorosilicate is 10 to 30% by weight. The annealing temperature of the tube furnace is 200-300 ℃, and the annealing time is 2-4 h.
In the step (2), the perfluorinated sulfonic acid polymer is soaked in 1mol/L lithium hydroxide solution for 12-18 hours. The lithiated perfluorosulfonic acid polymer is dissolved in dimethyl sulfoxide solution to form a 10-20wt% solution.
The prepared lithiated perfluorosulfonic acid polymer coated carbon nanotube/ferrous fluoride composite material is applied to a lithium metal battery anode material, and the carbon nanotube/ferrous fluoride composite material is prepared by the following steps in percentage by mass: carbon black: binder (PVDF) ═ 8: 1: 1, uniformly coating the ground slurry on a carbon-attached aluminum foil, placing the carbon-attached aluminum foil in a blast oven for 2-8h for drying, placing the dried material in a vacuum drying oven for vacuum drying for 8-24h, and cutting and weighing according to needs to obtain the corresponding anode material.
The technical scheme of the invention is convenient and easy to implement, and the loading capacity of the ferrous fluoride on the carbon nano tube can be controlled by the adding amount of the ferrous hexafluorosilicate aqueous solution. The amount of polymer coating can also be controlled by controlling the amount of lithiated perfluorosulfonic acid polymer solution added. The electrochemical performance of the whole composite material is improved by controlling the proportion of the carbon nano tube and the ferrous fluoride and the coating amount of the polymer. Scanning electron micrographs and transmission electron micrographs of the lithiated perfluorosulfonic acid polymer coated carbon nanotube/ferrous fluoride composite material are shown in the attached figures 1-4, and XRD characterization shows that the ferrous fluoride and carbon nanotube composite material is successfully prepared.
Drawings
FIG. 1 is a scanning electron micrograph of the carbon nanotube/ferrous fluoride composite material of the present invention.
Fig. 2 is a scanning electron micrograph of the lithiated perfluorosulfonic acid polymer-coated carbon nanotube/ferrous fluoride composite material according to the present invention.
FIG. 3 is a transmission electron microscope image of the carbon nanotube/ferrous fluoride composite prepared in the present invention.
Fig. 4 is a transmission electron microscope picture of the lithiated perfluorosulfonic acid polymer-coated carbon nanotube/ferrous fluoride composite material prepared in the present invention.
FIG. 5 is an XRD pattern of the carbon nanotube/ferrous fluoride composite material prepared in the present invention
Fig. 6 is a constant current charge-discharge curve diagram of the lithiated perfluorosulfonic acid polymer-coated carbon nanotube/ferrous fluoride composite material prepared in the present invention.
Fig. 7 is a graph of the cycle stability of the lithiated perfluorosulfonic acid polymer-coated carbon nanotube/ferrous fluoride composite prepared in the present invention.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples. The carbon nano tube is purchased from Nanjing Xiancheng nanometer material science and technology Limited with the tube diameter of 20-30 nm.
Example 1
(1) 1.2g of iron powder and 10g of fluorosilicic acid solution (23 wt%) were stirred at room temperature for 24 hours, and the solution was centrifuged to remove excess solids, to obtain a ferrous hexafluorosilicate solution and diluted to 45 ml.
(2) Soaking the carbon nano tube in a Triton X-100 aqueous solution to modify the surface of the carbon tube, and then putting the carbon nano tube into an oven for drying.
(3) 6ml of ferrous hexafluorosilicate solution was added dropwise to the modified 0.2g of carbon nanotubes, which were then dried in an oven.
(4) And (3) putting the product obtained in the last step into a tube furnace, and annealing at the temperature of 200-300 ℃ for 2-4h to obtain the ferrous fluoride/carbon nano tube composite material.
(5) Soaking a certain mass of perfluorosulfonic acid polymer in 1mol/L lithium hydroxide solution for 12-18 hours.
(6) The lithiated perfluorosulfonic acid polymer is dissolved in dimethyl sulfoxide solution to form a 10-20wt% solution.
(7) 0.5ml of polymer solution was dropped onto 0.1g of carbon nanotube/ferrous fluoride, and dried in an oven.
(8) Grinding the lithiated perfluorosulfonic acid polymer-coated ferrous fluoride/carbon nano tube at a ratio of 200mg, carbon black at a ratio of 25mg and a binder (PVDF) at a ratio of 25mg, uniformly coating the ground slurry on a carbon-attached aluminum foil, and placing the carbon-attached aluminum foil in a forced air oven for 3h for drying. And (5) placing the dried material in a vacuum drying oven, and performing vacuum drying for 12 hours. The cut positive electrode materials were weighed to 5.2mg, 5.5mg, and 6.0mg, respectively.
Example 2
(1) 1.2g of iron powder and 10g of fluorosilicic acid solution (23 wt%) were stirred at room temperature for 24 hours, and the solution was centrifuged to remove excess solids, to obtain a ferrous hexafluorosilicate solution and diluted to 45 ml.
(2) Soaking the carbon nano tube in a Triton X-100 aqueous solution to modify the surface of the carbon tube, and then putting the carbon nano tube into an oven for drying.
(3) 6ml of ferrous hexafluorosilicate solution was added dropwise to the modified 0.2g of carbon nanotubes, which were then dried in an oven.
(4) And (3) putting the product obtained in the last step into a tube furnace, and annealing at the temperature of 200-300 ℃ for 2-4h to obtain the ferrous fluoride/carbon nano tube composite material.
(5) Soaking a certain mass of perfluorosulfonic acid polymer in 1mol/L lithium hydroxide solution for 12-18 hours.
(6) The lithiated perfluorosulfonic acid polymer is dissolved in dimethyl sulfoxide solution to form a 10-20wt% solution.
(7) Dropping 1ml polymer solution on 0.1g carbon nanotube/ferrous fluoride, and drying in an oven.
(8) Grinding the lithiated perfluorosulfonic acid polymer-coated ferrous fluoride/carbon nano tube at a ratio of 200mg, carbon black at a ratio of 25mg and a binder (PVDF) at a ratio of 25mg, uniformly coating the ground slurry on a carbon-attached aluminum foil, and placing the carbon-attached aluminum foil in a forced air oven for 3h for drying. And (5) placing the dried material in a vacuum drying oven, and performing vacuum drying for 12 hours. The cut positive electrode materials were weighed to 5.3mg, 5.8mg, and 6.1mg, respectively.
Example 3
(1) 1.2g of iron powder and 10g of fluorosilicic acid solution (23 wt%) were stirred at room temperature for 24 hours, and the solution was centrifuged to remove excess solids, to obtain a ferrous hexafluorosilicate solution and diluted to 45 ml.
(2) Soaking the carbon nano tube in a Triton X-100 aqueous solution to modify the surface of the carbon tube, and then putting the carbon nano tube into an oven for drying.
(3) 6ml of ferrous hexafluorosilicate solution was added dropwise to the modified 0.2g of carbon nanotubes, which were then dried in an oven.
(4) And (3) putting the product obtained in the last step into a tube furnace, and annealing at the temperature of 200-300 ℃ for 2-4h to obtain the ferrous fluoride/carbon nano tube composite material.
(5) Soaking a certain mass of perfluorosulfonic acid polymer in 1mol/L lithium hydroxide solution for 12-18 hours.
(6) The lithiated perfluorosulfonic acid polymer is dissolved in dimethyl sulfoxide solution to form a 10-20wt% solution.
(7) 2ml of polymer solution was dropped onto 0.1g of carbon nanotube/ferrous fluoride and dried in an oven.
(8) Grinding the lithiated perfluorosulfonic acid polymer-coated ferrous fluoride/carbon nano tube at a ratio of 200mg, carbon black at a ratio of 25mg and a binder (PVDF) at a ratio of 25mg, uniformly coating the ground slurry on a carbon-attached aluminum foil, and placing the carbon-attached aluminum foil in a forced air oven for 3h for drying. And (5) placing the dried material in a vacuum drying oven, and performing vacuum drying for 12 hours. The cut positive electrode materials were weighed to 5.9mg, 5.1mg, and 5.6mg, respectively.
Example 4
(1) 1.2g of iron powder and 10g of fluorosilicic acid solution (23 wt%) were stirred at room temperature for 24 hours, and the solution was centrifuged to remove excess solids, to obtain a ferrous hexafluorosilicate solution and diluted to 45 ml.
(2) Soaking the carbon nano tube in a Triton X-100 aqueous solution to modify the surface of the carbon tube, and then putting the carbon nano tube into an oven for drying.
(3) 6ml of ferrous hexafluorosilicate solution was added dropwise to the modified 0.2g of carbon nanotubes, which were then dried in an oven.
(4) And (3) putting the product obtained in the last step into a tube furnace, and annealing at the temperature of 200-300 ℃ for 2-4h to obtain the ferrous fluoride/carbon nano tube composite material.
(5) Soaking a certain mass of perfluorosulfonic acid polymer in 1mol/L lithium hydroxide solution for 12-18 hours.
(6) The lithiated perfluorosulfonic acid polymer is dissolved in dimethyl sulfoxide solution to form a 10-20wt% solution.
(7) 4ml of polymer solution was added dropwise onto 0.1g of carbon nanotubes/ferrous fluoride and dried in an oven.
(8) Grinding the lithiated perfluorosulfonic acid polymer-coated ferrous fluoride/carbon nano tube at a ratio of 200mg, carbon black at a ratio of 25mg and a binder (PVDF) at a ratio of 25mg, uniformly coating the ground slurry on a carbon-attached aluminum foil, and placing the carbon-attached aluminum foil in a forced air oven for 3h for drying. And (5) placing the dried material in a vacuum drying oven, and performing vacuum drying for 12 hours. The cut positive electrode materials were weighed to 5.8mg, 5.1mg, and 5.8mg, respectively.
Example 5
(1) 1.2g of iron powder and 10g of fluorosilicic acid solution (23 wt%) were stirred at room temperature for 24 hours, and the solution was centrifuged to remove excess solids, to obtain a ferrous hexafluorosilicate solution and diluted to 45 ml.
(2) Soaking the carbon nano tube in a Triton X-100 aqueous solution to modify the surface of the carbon tube, and then putting the carbon nano tube into an oven for drying.
(3) 6ml of ferrous hexafluorosilicate solution was added dropwise to the modified 0.2g of carbon nanotubes, which were then dried in an oven.
(4) And (3) putting the product obtained in the last step into a tube furnace, and annealing at the temperature of 200-300 ℃ for 2-4h to obtain the ferrous fluoride/carbon nano tube composite material.
(5) Soaking a certain mass of perfluorosulfonic acid polymer in 1mol/L lithium hydroxide solution for 12-18 hours.
(6) The lithiated perfluorosulfonic acid polymer is dissolved in dimethyl sulfoxide solution to form a 10-20wt% solution.
(7) 5ml of polymer solution was dropped onto 0.1g of carbon nanotube/ferrous fluoride and dried in an oven.
(8) Grinding the lithiated perfluorosulfonic acid polymer-coated ferrous fluoride/carbon nano tube at a ratio of 200mg, carbon black at a ratio of 25mg and a binder (PVDF) at a ratio of 25mg, uniformly coating the ground slurry on a carbon-attached aluminum foil, and placing the carbon-attached aluminum foil in a forced air oven for 3h for drying. And (5) placing the dried material in a vacuum drying oven, and performing vacuum drying for 12 hours. The cut positive electrode materials were weighed to 5.7mg, 5.3mg, and 6.3mg, respectively.
Connecting the battery to a LAND battery test system, standing for 10min, and testing constant current discharge performance with discharge current of 100mA g-1The discharge termination voltage is 1.2V, the test adopts button cell to directly measure and obtain data, as can be seen in the attached figures 1 and 3, the small particles with the diameter of about 10nm are compounded on the surface of the carbon nano tube with the diameter of 20-40 nm. The successful preparation of ferrous fluoride can be demonstrated as shown in figure 5. As shown in figures 2 and 4It can be seen that the carbon nanotube/ferrous fluoride surface is covered with a thin layer of polymer. Fig. 6 and 7 show stable electrical properties and good specific capacity.
The preparation of the ferrous fluoride/carbon nano tube composite material can be realized by adjusting the process parameters according to the content of the invention, and the test shows that the performance is basically consistent with the invention, namely the polymer coated carbon nano tube/ferrous fluoride is used for the anode material of the lithium metal battery, the discharge medium voltage is 1.7-1.8V, and the specific capacity is 430-450mAh g--1. The capacity is maintained at 110-130mAh g after 100 cycles of circulation-1. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (6)
1. A preparation method of a polymer-coated carbon nanotube/ferrous fluoride composite material comprises the following steps:
(1) dripping a ferrous hexafluorosilicate aqueous solution on the carbon nano tube modified by Triton X-100, drying, and annealing under argon flow in a tube furnace to obtain a carbon nano tube/ferrous fluoride material;
(2) preparing a lithiation perfluorosulfonic acid polymer solution, soaking a perfluorosulfonic acid polymer in a lithium hydroxide solution to enable lithium atoms to replace hydrogen atoms in a sulfonate group to obtain a lithiation perfluorosulfonic acid polymer, dissolving the lithiation perfluorosulfonic acid polymer in dimethyl sulfoxide, and stirring, heating and dissolving the lithiation perfluorosulfonic acid polymer;
(3) and dropwise adding the lithiated perfluorosulfonic acid polymer solution on the carbon nano tube/ferrous fluoride material to prepare the lithiated perfluorosulfonic acid polymer coated carbon nano tube/ferrous fluoride composite material.
2. The production method according to claim 1, wherein in the step (1), the mass concentration of the ferrous hexafluorosilicate aqueous solution is 10 to 30 wt%.
3. The method as claimed in claim 1, wherein in the step (1), the annealing temperature of the tube furnace is 200-300 ℃, and the annealing time is 2-4 h.
4. The method according to claim 1, wherein in the step (2), the perfluorosulfonic acid polymer is immersed in a 1mol/L lithium hydroxide solution for 12 to 18 hours.
5. The method of claim 1, wherein in step (2), the lithiated perfluorosulfonic acid polymer is dissolved in a dimethylsulfoxide solution to form a 10 to 20wt% solution.
6. The application of the lithiated perfluorosulfonic acid polymer-coated carbon nanotube/ferrous fluoride composite material prepared by the preparation method of claim 1 in the positive electrode material of a lithium metal battery is characterized in that the lithiated perfluorosulfonic acid polymer-coated carbon nanotube/ferrous fluoride composite material is prepared by the following steps in percentage by mass: carbon black: binder PVDF = 8: 1: 1, uniformly coating the ground slurry on a carbon-attached aluminum foil, placing the carbon-attached aluminum foil in a blast oven for 2-8h for drying, placing the dried material in a vacuum drying oven for vacuum drying for 8-24h, and cutting and weighing according to needs to obtain the corresponding anode material.
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| CN105977448A (en) * | 2016-07-13 | 2016-09-28 | 广东工业大学 | Ferric fluoride/conducting polymer composite material, preparation method thereof and lithium secondary battery |
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