CN110980698B - H1.07Ti1.73O4Preparation method of/rGO compound sodium ion battery anode material - Google Patents
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Abstract
The invention provides a method for preparing a hydrogen storage battery1.07Ti1.73O4Firstly, preparing micron-sized K by a simple high-temperature solid-phase reaction method0.81Li0.27Ti1.73O4Granules, K0.81Li0.27Ti1.73O4The surface of the graphene oxide GO is coated with a layer of polymer material with positive charges, and after the polymer material is mixed with graphene oxide GO solution with negative charges, the polymer material is attracted by the positive charges and the negative charges, and K is simultaneously added0.81Li0.27Ti1.73O4Reacting with acid in acidic environment to prepare H1.07Ti1.73O4Composite structure of @ GO, then by hydrothermal, H is prepared1.07Ti1.73O4@ rGO composite. H1.07Ti1.73O4The @ rGO nano composite material is used for a sodium ion battery cathode and shows excellent rate performance and cycling stability.
Description
Technical Field
The invention relates to the field of electrochemical power supply preparation, in particular to H1.07Ti1.73O4A preparation method of a/rGO compound sodium ion battery cathode material.
Background
With the development of power batteries, sodium ion power batteries have energy density and power density comparable to those of lithium ion batteries, and almost all the advantages of lithium ion batteries, such as fast charge and discharge speed, long cycle life, good load performance, high operating voltage, and the like. Meanwhile, the manufacturing cost of the sodium ion battery is lower than that of the lithium ion battery, and the sodium abundance is far higher than that of the lithium ion batteryThe abundance of lithium. Sodium ion batteries have received much attention for large scale applications and future electrochemical energy storage devices. Sodium ion battery negative electrode materials have been studied extensively as important factors for improving battery energy and cycle life. Similar to lithium ion batteries, the negative electrode material of sodium ion batteries mainly includes carbon-based materials, transition metal oxygen/sulfide materials, alloy materials such as Sn, and composite materials thereof. In order to develop a safer, high-rate and long-cycle stable sodium ion battery, the intercalation-type negative electrode material is now beginning to be widely noticed by people. HxTiyOzThe material is called HTO for short, is a novel intercalation cathode material, and the research is in the initial stage, and the rate capability and the cycling stability of the material need to be further improved. Graphene is a highly conductive two-dimensional material and has high mechanical properties. The HTO has low conductivity, and the graphene is used as a conductive layer, so that the conductivity of the electrode can be greatly improved, the three-dimensional net-shaped supporting effect can be achieved, the surface dynamics behavior of the whole material is improved, and the multiplying power and the cycle performance of the electrode are further improved.
Disclosure of Invention
The invention provides a H1.07Ti1.73O4A preparation method of a @ rGO (HTO @ rGO) compound sodium ion battery negative electrode material comprises the steps of firstly preparing micron-sized K through a simple high-temperature solid-phase reaction method0.81Li0.27Ti1.73O4(KLTO) particles are prepared by coating a layer of polymer material with positive charges on the surface of KLTO, mixing the polymer material with Graphene Oxide (GO) solution with negative charges, preparing a composite material with HTO loaded on the surface of GO by a positive and negative charge attraction method and simultaneously reacting KLTO with acid in an acid environment, and then hydrothermally converting GO into reduced graphene oxide (rGO) and forming a stable chemical bond between HTO and rGO to prepare the HTO @ rGO composite material, thereby increasing the multiplying power and the cycle performance of the composite material.
The technical scheme for realizing the invention is as follows:
h1.07Ti1.73O4Negative electrode of/rGO compound sodium ion batteryThe preparation method of the material comprises the following steps:
(1) preparation K0.81Li0.27Ti1.73O4(KLTO) powder;
(2) adding NaCl powder and poly (diallyldimethylammonium chloride), PDDA for short, into deionized water, and stirring to obtain ionized water solution;
(3) mixing the K prepared in the step (1)0.81Li0.27Ti1.73O4Adding the powder into the ionized water solution obtained in the step (2), and intensively stirring for 60min to obtain a KLTO suspension;
(4) preparing a graphene oxide solution, dropwise adding the KLTO turbid liquid obtained in the step (3) into the graphene oxide solution, and strongly stirring at room temperature for 24 hours to obtain a precipitate;
(5) and (4) washing the precipitate obtained in the step (4), placing the washed product in a reaction kettle for hydrothermal reaction, and freeze-drying the product after the reaction to obtain the HTO @ rGO cathode material, namely HTO/rGO, wherein the material is used for the cathode material of the sodium-ion battery.
K in the step (1)0.81Li0.27Ti1.73O4The preparation method of the powder comprises the following steps: fully mixing lithium carbonate, potassium carbonate and titanium oxide, and then heating the mixture to 1200 ℃ to sinter for 12 h; after sintering, taking out pure white powder after the furnace is cooled; the obtained sample is annealed for 4h in the air atmosphere at 500 ℃ to obtain pure white K0.81Li0.27Ti1.73O4And (3) powder.
The mass ratio of the lithium carbonate to the potassium carbonate to the titanium oxide is (0.64-0.69): (1.8-2.2): (1.32-1.40).
The mass ratio of the NaCl powder, the poly (diallyldimethylammonium chloride) (PDDA) and the deionized water in the step (2) is 1: 5: 100.
k in the step (3)0.81Li0.27Ti1.73O4The mass ratio of the powder to the ionized water solution is (1-10): 100.
the concentration of the graphene oxide solution in the step (4) is 0.05-0.1mg/ml, and the pH value is 4-6.
The hydrothermal reaction temperature in the step (5) is 120-180 ℃, the time is 6-18h, the freeze-drying temperature is-30 +/-10 ℃, and the time is 48-72 h.
The HTO @ rGO negative electrode material is H1.07Ti1.73O4The microparticles are supported on the surface of the rGO and are mutually connected to form a composite structure of a net structure.
The invention has the beneficial effects that:
(1) preparing KLTO micron particles by a high-temperature solid phase method and regulating and controlling the surface properties of the KLTO micron particles;
(2) the HTO/rGO composite structure is prepared by adopting a simple electrostatic adsorption self-assembly method, and the method is simple and easy to implement and is suitable for large-scale production;
(3) the composite structure of loading HTO/rGO to the rGO micro-sheet effectively improves the whole conductivity, improves the surface dynamic performance of HTO, and improves the multiplying power and the cycle performance of the battery.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a scanning electron micrograph of HTO microparticles (a, b) and HTO @ rGO composites (c, d) prepared in example 1 at different magnifications.
Fig. 2 is an XRD pattern of pure HTO and HTO @ rGO composites prepared in example 1.
Fig. 3 is a charge and discharge curve of the HTO @ rGO composite electrode finally obtained in example 1.
FIG. 4 shows pure HTO and HTO @ rGO composite electrodes obtained in example 1 at 0.1A g-1And (4) testing the cycling stability under the current density.
Fig. 5 is a performance test of pure HTO and HTO @ rGO composite electrodes obtained in example 1 at different current densities.
FIG. 6 shows pure HTO and HTO @ rGO composite electrodes obtained in example 1 at 2A g-1The cycle stability test at high current density.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
Preparation of an HTO/rGO composite sodium-ion battery anode material:
(1) KLTO micron particles
KLTO microparticles were synthesized by a high temperature solid phase reaction preparation method.
The preparation steps are as follows: lithium carbonate (Li)2CO30.640 g), potassium carbonate (K)2CO31.8 g) and titanium oxide (TiO)21.32 g) was thoroughly mixed and the mixture was then heated to 1200 deg.foAnd C, sintering for 12 hours. And after sintering, taking out pure white powder after the furnace is cooled. The obtained sample was then annealed at 500 ℃ for 4h in an air atmosphere to obtain pure white KLTO powder.
(2) Synthesis of rGO supported HTO microparticle composite material
First, Graphene Oxide (GO) was synthesized by using a modified Hummers method.
Next, 1g NaCl and 5g PDDA (20%) were added to 100ml of deionized water and stirred for half an hour to give an ionized positively charged aqueous solution. 10 mg of the pure white KLTO powder obtained in step (1) was added to 100mg of a positively charged aqueous solution, and after vigorously stirring for 60min, the KLTO powder was positively charged.
Preparing 200 ml of 0.1mg/ml graphene oxide solution, and dropwise adding a certain amount of HCl to adjust the pH value to 5. The KLTO suspension was then added drop by drop to GO solution, with whisker precipitation occurring during the addition, and kept under vigorous stirring at room temperature 23 ℃ for 24 hours to acidify the KLTO to HTO. The precipitate was then washed repeatedly and collected by centrifugation. Then the obtained reactant is put into a 50 ml reaction kettle and undergoes hydrothermal reaction at 120 ℃ for 18 hours, and then the obtained product is freeze-dried at-40 ℃ for 48 hours. And then annealing the product at 450 ℃ for 2 hours under the protective atmosphere of argon to obtain black HTO @ rGO powder.
Assembling and testing electrochemical performance of the button cell:
electrochemical performance testing was performed by CR2032 button cell at room temperature. The working electrode is prepared as follows: firstly, mixing a sample material, acetylene black and carboxymethyl cellulose (CMC) according to a weight ratio of 80:10:10, dripping a proper amount of water into the mixed sample, and violently stirring for 10 minutes to form uniform slurry; secondly, uniformly scraping the obtained slurry on a copper foil by using a scraper, keeping the copper foil at 120 ℃, performing vacuum drying for 12 hours, and removing the solvent; finally, the copper foil coated with the sample was pressed into small wafers with a die press.
The HTO/rGO obtained in the example is used as a positive electrode, a sodium sheet is used as a negative electrode material, a Whatman glass fiber diaphragm, and 1M NaPF dissolved in ethyl carbonate and diethyl carbonate (volume ratio is 1: 1)6The charging and discharging test is completed under a Xinwei battery test system for the electrolyte, the test voltage range is 0.01-3.0V, the test temperature is room temperature, and the test current density is 100 mAh g-1. The first discharge capacity is about 242 mAh g-1All higher than the existing HTO-based composites, and the HTO/rGO after about 10 cycles of activation, the capacity begins to increase gradually, stabilizes at 110 weeks, and at 250 weeks the capacity is about 190 mAh g-1Electrochemical performance test results are shown in fig. 3 and 4. The rate capability is shown in fig. 5. At 0.1, 0.2, 0.5, 1.0, 2.0, 5.0 and 10.0A g−1The discharge capacities of HTO/rGO were 142.8, 131.1, 117.7, 108.6, 96.8, 80.7, and 66.7 mA h g, respectively−1. At the same timeThe discharge capacities of HTO were 125.4, 92.7, 60.6, 37.7, 15.6, 2.8, and 2.7 mA hr g, respectively, at the flow density−1. And our HTO/rGO at high current densities, such as 2A g-1In the case of (1), after 1000 weeks of the cycle, 104 mAh g of the electric charge can still be discharged-1. These data demonstrate that HTO/rGO prepared with a simple process has excellent rate performance and cycle stability.
Example 2
Preparation of a layered HTO/rGO composite sodium-ion battery anode material:
(1) HTO microparticle synthesis
Lithium carbonate (Li)2CO30.690 g), potassium carbonate (K)2CO32.2 g) and titanium oxide (TiO)21.40 g) was thoroughly mixed and the mixture was then heated to 1200 deg.foAnd C, sintering for 12 hours. After sintering, the furnace was cooled and pure white KLTO powder was taken out. The obtained sample was then annealed at 500 ℃ for 4 hours in an air atmosphere to obtain pure white KLTO powder.
(2) Synthesis of rGO supported HTO microparticle composite material
First, Graphene Oxide (GO) was synthesized by using a modified Hummers method. Next, 1mg NaCl and 5g PDDA (20%) were added to 100ml deionized water and stirred for half an hour to give an ionized positively charged aqueous solution.
10 mg of the pure white KLTO powder obtained in step (1) was added to 1000mg of a positively charged aqueous solution, and after vigorously stirring for 60 minutes, the KLTO powder was aligned. Preparing 400 ml of graphene oxide solution with the concentration of 0.05 mg/ml, and dropwise adding a certain amount of HCl to adjust the pH value to 5. The KLTO suspension was then added drop by drop to the GO solution, with whisker precipitation occurring during the addition. And maintained at room temperature 23oStirring vigorously for 48 hours under C. KLTO was acidified to HTO. The precipitate was then washed repeatedly and collected by centrifugation. Then the obtained reactant is put into a 50 ml reaction kettle and is put into a 180 ml reaction kettleoC, carrying out hydrothermal reaction for 6 hours, and then carrying out freeze drying on the obtained product at-40 ℃ for 72 hours to obtain black HTO @ rGO powder, wherein a sample can be obtainedThe material is used for the negative electrode material of the sodium-ion battery.
Example 3
Preparation of a layered HTO/rGO composite sodium-ion battery anode material:
(1) HTO microparticle synthesis
Lithium carbonate (Li)2CO30.670 g), potassium carbonate (K)2CO32.0 g) and titanium oxide (TiO)21.35 g) was thoroughly mixed and the mixture was then heated to 1200 deg.foAnd C, sintering for 12 hours. After sintering, the furnace was cooled and pure white KLTO powder was taken out. The obtained sample was then annealed at 500 ℃ for 4 hours in an air atmosphere to obtain pure white KLTO powder.
(2) Synthesis of rGO supported HTO microparticle composite material
First, Graphene Oxide (GO) was synthesized by using a modified Hummers method. Next, 1mg NaCl and 5g PDDA (20%) were added to 100ml deionized water and stirred for half an hour to give an ionized positively charged aqueous solution.
10 mg of the pure white KLTO powder obtained in step (1) was added to 200mg of a positively charged aqueous solution, and after vigorously stirring for 60 minutes, the KLTO powder was aligned. Preparing 200 ml of 0.1mg/ml graphene oxide solution, and dropwise adding a certain amount of HCl to adjust the pH value to 5. The KLTO suspension was then added drop by drop to the GO solution, with whisker precipitation occurring during the addition. And maintained at room temperature 23oStirring vigorously for 48 hours under C. KLTO was acidified to HTO. The precipitate was then washed repeatedly and collected by centrifugation. Then the obtained reactant is put into a 50 ml reaction kettle and is put into a reactor with the volume of 150oC, carrying out hydrothermal reaction for 6 hours, and then carrying out freeze drying on the obtained product at-40 ℃ for 48 hours to obtain black HTO @ rGO powder. The sample can be used as a negative electrode material of a sodium-ion battery.
Example 4
Preparation of a layered HTO/rGO composite sodium-ion battery anode material:
(1) HTO microparticle synthesis
Lithium carbonate (Li)2CO30.650 g), potassium carbonate (K)2CO32.1 g) and titanium oxide (TiO)21.35 g) was thoroughly mixed and the mixture was then heated to 1200 deg.foAnd C, sintering for 12 hours. After sintering, the furnace was cooled and pure white KLTO powder was taken out. The obtained sample was then annealed at 500 ℃ for 4 hours in an air atmosphere to obtain pure white KLTO powder.
(2) Synthesis of rGO supported HTO microparticle composite material
First, Graphene Oxide (GO) was synthesized by using a modified Hummers method. Next, 1mg NaCl and 5g PDDA (20%) were added to 100ml deionized water and stirred for half an hour to give an ionized positively charged aqueous solution.
10 mg of the pure white KLTO powder obtained in step (1) was added to 200mg of a positively charged aqueous solution, and after vigorously stirring for 60 minutes, the KLTO powder was aligned. Preparing 200 ml of 0.08 mg/ml graphene oxide solution, and dropwise adding a certain amount of HCl to adjust the pH value to 6. The KLTO suspension was then added drop by drop to the GO solution, with whisker precipitation occurring during the addition. And maintained at room temperature 23oStirring vigorously for 48 hours under C. KLTO was acidified to HTO. The precipitate was then washed repeatedly and collected by centrifugation. Then the obtained reactant is put into a 50 ml reaction kettle, and 160 ml of the reaction kettle is usedoC, carrying out a hydrothermal reaction for 10 hours, and then carrying out freeze drying on the obtained product at-20 ℃ for 60 hours to obtain black HTO @ rGO powder. The sample can be used as a negative electrode material of a sodium-ion battery.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. H1.07Ti1.73O4The preparation method of the/rGO compound sodium ion battery anode material is characterized by comprising the following steps:
(1) preparation K0.81Li0.27Ti1.73O4Powder;
(2) adding NaCl powder and a poly (diallyldimethylammonium chloride) solution into deionized water, and stirring to obtain an ionized aqueous solution;
(3) mixing the K prepared in the step (1)0.81Li0.27Ti1.73O4Adding the powder into the ionized water solution obtained in the step (2), and intensively stirring for 60min to obtain K0.81Li0.27Ti1.73O4Suspending liquid;
(4) preparing a graphene oxide solution, and mixing the K obtained in the step (3)0.81Li0.27Ti1.73O4Dropwise adding the turbid liquid into a graphene oxide solution, wherein the pH value of the graphene oxide solution is 4-6, and strongly stirring at room temperature for 24 hours to obtain a precipitate;
(5) washing the precipitate obtained in the step (4), putting the washed product into a reaction kettle for hydrothermal reaction, and freeze-drying the product after the reaction to obtain H1.07Ti1.73O4a/rGO composite material.
2. H according to claim 11.07Ti1.73O4The preparation method of the/rGO compound sodium-ion battery anode material is characterized in that K in the step (1)0.81Li0.27Ti1.73O4The preparation method of the powder comprises the following steps: fully mixing lithium carbonate, potassium carbonate and titanium oxide, and then heating the mixture to 1200 ℃ to sinter for 12 h; after sintering, taking out pure white powder after the furnace is cooled; the obtained sample is annealed for 4h in the air atmosphere at 500 ℃ to obtain pure white K0.81Li0.27Ti1.73O4And (3) powder.
3. H according to claim 21.07Ti1.73O4The preparation method of the/rGO compound sodium ion battery cathode material is characterized by comprising the following steps: the mass ratio of the lithium carbonate to the potassium carbonate to the titanium oxide is (0.64-0.69): (1.8-2.2): (1.32-1.40).
4. H according to claim 11.07Ti1.73O4The preparation method of the/rGO compound sodium ion battery cathode material is characterized in that in the step (2), the mass ratio of the NaCl powder to the poly (diallyldimethylammonium chloride) to the deionized water is 1: 5: 100.
5. h according to claim 11.07Ti1.73O4The preparation method of the/rGO compound sodium ion battery cathode material is characterized in that K in the step (3)0.81Li0.27Ti1.73O4The mass ratio of the powder to the ionized water solution is (1-10): 100.
6. h according to claim 11.07Ti1.73O4The preparation method of the/rGO compound sodium-ion battery anode material is characterized in that the concentration of the graphene oxide solution in the step (4) is 0.05-0.1 mg/ml.
7. H according to claim 11.07Ti1.73O4The preparation method of the/rGO compound sodium ion battery cathode material is characterized in that the hydrothermal reaction temperature in the step (5) is 120-180 ℃, the time is 6-18h, the freeze-drying temperature is-30 +/-10 ℃, and the time is 48-72 h.
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