CN115974033A - Nitrogen-doped mesoporous carbon-coated iron sodium phosphate pyrophosphate composite material and preparation method thereof - Google Patents
Nitrogen-doped mesoporous carbon-coated iron sodium phosphate pyrophosphate composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of battery anode materials, and discloses a preparation method of a nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material, which comprises the following steps of S1, preparing a template organic solution; s2, adding a compound containing pyrophosphate, phosphate, a sodium source, a nitrogen source and a carbon source into the template organic solution; s3, preparing an iron source solution; s4, adding the iron source solution into the mixed solution to obtain a suspension; s5, heating, stirring and evaporating the suspension to dryness, and drying to obtain a nano positive electrode precursor; s6, performing solid-phase sintering on the nano anode precursor to obtain the nitrogen-doped mesoporous carbon-coated iron sodium phosphate pyrophosphate composite material; the invention simultaneously utilizes the soft template agent to play a role in the generation of the anode material and the nitrogen-doped carbon material to obtain the nitrogen-doped mesoporous carbon coated spherical ferric sodium pyrophosphate composite material with uniform and nanocrystallized particle size, and the composite material shows excellent performance in the high-rate discharge of the sodium ion battery.
Description
Technical Field
The invention relates to the technical field of battery anode materials, in particular to a nitrogen-doped mesoporous carbon-coated iron sodium phosphate pyrophosphate composite material, and further comprises a preparation method of the nitrogen-doped mesoporous carbon-coated iron sodium phosphate pyrophosphate composite material.
Background
With the continuous development of economy, the demand for energy is increasing continuously, and as a clean and efficient energy storage and conversion medium, the ion battery is paid more and more attention and attention by people. Among them, lithium ion batteries are widely used in portable mobile devices such as mobile phones, notebook computers, cameras, electric vehicles, and energy storage power stations. However, the manufacturing cost of lithium batteries is increasing due to the shortage of lithium resources, limiting the application of lithium ion batteries. The sodium element has similar properties with the lithium element, and the electrochemical performance of the sodium-ion battery is also similar to that of the lithium-ion battery; and the reserve of sodium is richer, the source is richer, and the cost is lower, so that the sodium-ion battery becomes an energy storage medium which has the most potential to replace a lithium-ion battery. However, the ion radius of sodium ions is larger than that of lithium ions, and sodium ions are more difficult to be inserted and extracted, so that the high-rate performance of the sodium ion battery is poorer than that of the lithium ion battery.
The ferric sodium pyrophosphate phosphate has the advantages of low cost, good structural stability and excellent cycle performance, and is one of ideal choices of battery anode materials with sodium ions having industrial application prospects. However, because of the low intrinsic electronic conductivity of ferric pyrophosphate phosphate, modification by means of carbon coating is required; the mesoporous carbon material has the characteristics of easy surface functionalization, unique physiochemical properties and biocompatibility. Therefore, the composite cathode material is obtained by efficiently doping the carbon-coated iron sodium pyrophosphate phosphate with nitrogen, and has wide application prospects.
Chinese patent discloses a method for synthesizing sodium ferric phosphate pyrophosphate sodium/carbon serving as a sodium ion battery anode material and a sodium ion battery (publication number: CN 115148976A) thereof, wherein the composite anode material is prepared by a ball milling method, but noise pollution is easily caused in the ball milling process, and the prepared sodium ferric phosphate pyrophosphate sodium has large particle size and is not beneficial to the application of the sodium ion battery anode material under high magnification; the mesoporous carbon composite material is also prepared by a grinding method, and not only is noise pollution easily caused in the ball milling process, but also fluorine element which pollutes the environment is generated in the preparation process. Therefore, a composite cathode material which is not easy to generate noise pollution in the preparation process, does not pollute the environment, has the advantages of uniform particle size and high purity, and shows excellent performance in high-rate discharge of the sodium-ion battery and a preparation method thereof are needed.
Disclosure of Invention
The invention aims to provide a nitrogen-doped mesoporous carbon-coated phosphoric acid ferric sodium pyrophosphate composite material and a preparation method thereof, and simultaneously, a soft template agent is utilized to play a role in the generation of a positive electrode material and a nitrogen-doped carbon material to obtain a nano nitrogen-doped mesoporous carbon-coated spherical phosphoric acid ferric sodium pyrophosphate composite material with uniform particle size.
In order to achieve the above purpose, the invention provides the following technical scheme:
the preparation method of the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material comprises the following steps:
s1, adding a template organic matter into water, and stirring and dissolving to obtain a template organic solution;
s2, adding a compound containing pyrophosphate, phosphate, a sodium source, a nitrogen source and a carbon source into the template organic solution obtained in the S1 to obtain a mixed solution;
s3, adding an iron source into water to obtain an iron source solution;
s4, dropwise adding the iron source solution obtained in the step S3 into the mixed solution of the step S2 to obtain a suspension;
s5, heating, stirring and evaporating the suspension obtained in the S4 to dryness, and drying to obtain a nano positive electrode precursor;
and S6, presintering the nano anode precursor obtained in the S5 under the protection of inert gas, naturally cooling, taking out, grinding, and sintering and cooling again under the protection of inert gas to obtain the nitrogen-doped mesoporous carbon coated iron sodium pyrophosphate composite material.
Further, in S1, the template organic substance is one or more of polyoxyethylene polyoxypropylene ether, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, and polyoxyethylene ether compound; the temperature in the stirring and dissolving process is room temperature, the stirring speed is 100-900 r/min, and the time is 1.0-3.0 h; the concentration of the obtained template organic matter solution is 1-100 g/L.
Further, in S2, the pyrophosphate is one or more of trisodium monohydrogen pyrophosphate, disodium dihydrogen pyrophosphate, sodium trishydrogen pyrophosphate and hydrates thereof; the phosphate is one or more of ammonium phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate and hydrates thereof; the nitrogen source is one or more of urea, polyvinylpyrrolidone and glycine; the carbon source is one or more of glucose, fructose, galactose, lactose, sucrose, maltose and the nitrogen source.
Further, in S3, the iron source is one or more of ferric nitrate, ferric acetate, ferric ammonium oxalate, ferric citrate, ferric ammonium citrate, and hydrates thereof.
Further, in S4, the mixed solution of S2 is added to the iron source solution of S3 to obtain a suspension containing sodium: iron: a phosphoric acid group: the molar mass ratio of pyrophosphate groups is 4.
Further, in S5, the obtained nano positive electrode precursor is an iron salt precursor, and the mass ratio of the template organic matter to the precursor is 0.01-1: 1.
further, in S6, the sintering of the nano positive electrode precursor is solid phase sintering, and the specific steps are as follows: presintering for 3-12 h at 250-400 ℃ under inert gas, taking out the material, grinding, and calcining for 9-15 h at 450-600 ℃; the inert gas is one or more of nitrogen or argon; the nitrogen element in the obtained nitrogen-doped mesoporous carbon-coated phosphoric acid ferric sodium pyrophosphate composite material is as follows: the molar mass ratio of the phosphoric acid ferric sodium pyrophosphate is 0.01-0.5; carbon element (C): the molar mass ratio of the ferric sodium pyrophosphate phosphate is 0.01-0.5.
The composite material prepared by the preparation method of the nitrogen-doped mesoporous carbon-coated ferric sodium pyrophosphate composite material.
The composite material prepared by the preparation method of the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material is applied to a positive electrode material of a sodium ion battery.
The composite material prepared by the preparation method of the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material is applied to a sodium ion battery anode material, and a template organic matter of the composite anode material is used as a template agent generated by iron sodium pyrophosphate phosphate and also used as a template agent of a nitrogen-doped mesoporous carbon coating layer.
The technical scheme has the beneficial effects that:
1. the preparation method of the nitrogen-doped mesoporous carbon-coated ferric sodium pyrophosphate phosphate composite material provided by the invention is characterized in that the high-magnification sodium ion battery nitrogen-doped mesoporous carbon-coated ferric sodium pyrophosphate phosphate composite cathode material is prepared by using the soft template in an auxiliary manner, and the aggregation of ferric salt precursors is avoided due to the existence of template organic matters in the synthesis process, so that the synthesis of nano ferric salt precursors is facilitated; meanwhile, the template organic matter also plays a role of a template in the formation process of the nitrogen-doped mesoporous carbon;
2. the prepared carbon film coated on the surface of the composite anode material can greatly improve the conductivity of the material, the coated carbon layer enhances the structural rigidity of the material, the structural collapse and damage of the electrode material in the charging and discharging process can be inhibited, nitrogen doping provides more active sites for sodium ion deintercalation, and the mesoporous carbon material not only has the characteristics of large specific surface area, large pore volume and adjustable pore diameter, so that the reversible capacity of the battery is improved, and the rate capability is optimized;
3. according to the invention, the soft template is used as the template to synthesize a nano ferric salt precursor, and then the nano ferric salt precursor is sintered at high temperature to synthesize the high-rate sodium ion battery nitrogen-doped mesoporous carbon-coated phosphoric acid ferric sodium pyrophosphate composite anode material, so that the prepared anode material is nano particles with uniform particle size, the nitrogen-doped mesoporous carbon is more uniformly coated, and the performance is excellent under the high-rate discharge condition;
4. the invention is not easy to generate noise pollution and environment pollution in the preparation process; the material prepared by the invention is used as the anode of a sodium ion battery for experiment, and under the voltage window of 1.5-4.2V and the multiplying power of 0.1C, the first discharge specific capacity is 118.7mAh/g, under the multiplying power of 1C, the first discharge specific capacity is 108.2mAh/g, and under the multiplying power of 10C, the capacity retention rate of the material is 95.5 percent after 500 weeks of cyclic charge and discharge. Namely, the nitrogen-doped carbon-coated iron sodium pyrophosphate phosphate composite material as a positive electrode material has good rate capability and long cycle life.
Drawings
FIG. 1 is an SEM image of a material prepared by the method for preparing the nitrogen-doped mesoporous carbon coated iron sodium pyrophosphate phosphate composite material of example 1;
FIG. 2 is an XRD pattern of a material prepared by the method for preparing a nitrogen-doped mesoporous carbon coated iron sodium pyrophosphate composite material of example 1;
fig. 3 is a first charge-discharge curve at a magnification of 0.1C when the material prepared by the method for preparing a nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate composite material of the invention is used as a positive electrode of a sodium ion battery in example 1;
fig. 4 is a first charge-discharge curve at a 1C rate when a material prepared by the method for preparing a nitrogen-doped mesoporous carbon coated iron sodium pyrophosphate composite material of the present invention is used as a sodium ion battery positive electrode in example 1;
fig. 5 shows the cycle performance at a rate of 10C when the material prepared by the method for preparing the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material of the invention is used as a positive electrode of a sodium ion battery in example 1.
Detailed Description
The invention is described in further detail below with reference to the following figures and embodiments:
example 1
The preparation method of the nitrogen-doped mesoporous carbon-coated ferric sodium pyrophosphate phosphate composite material comprises the following steps:
s1, stirring 0.2g of polyoxyethylene polyoxypropylene ether at room temperature and at a stirring speed of 200r/min for 1 hour to dissolve the polyoxyethylene polyoxypropylene ether to obtain 40mL of template organic solution;
s2, adding 0.004molNH into 40mL of template organic solution obtained in S1 4 H 2 PO 4 、0.002molNa 4 P 2 O 7 0.1247g of glucose and 0.1247g of polyvinylpyrrolidone are dissolved in the solution to obtain a mixed solution;
s3, taking 0.006molFe (NO) 3 ) 3 ·9H 2 Stirring O at room temperature and stirring speed of 200r/min for 0.5h to dissolve;
s4, dropwise adding the solution prepared in the S3 into the mixed solution of the S2 to obtain a suspension;
s5, stirring and evaporating the suspension of the S4 at the temperature of 80 ℃ at the speed of 400r/min, and drying to obtain a nano positive electrode precursor;
and S6, sintering the nano anode precursor obtained in the step S5 at 300 ℃ for 12h in a nitrogen atmosphere, cooling the nano anode precursor to room temperature along with a furnace, grinding the nano anode precursor in a mortar for 0.5h, and then performing solid-phase sintering at 500 ℃ for 10h to obtain the nitrogen-doped carbon-coated iron sodium pyrophosphate composite material.
As shown in fig. 1, is an SEM image of the nitrogen-doped carbon-coated iron sodium pyrophosphate phosphate composite prepared by the above method;
as shown in fig. 2, the XRD pattern of the nitrogen-doped carbon-coated ferric sodium pyrophosphate composite material prepared by the above method;
the composite material obtained in the embodiment, conductive agent acetylene black, binder and N-methyl pyrrolidone are weighed according to the weight ratio of 8 4 EC: DEC (volume ratio 1)/5.0% fec as electrolyte, assembled into button cells, and tested for electrochemical performance.
As shown in fig. 3 to 5, the first discharge specific capacity is 118.7mAh/g under the voltage window of 1.5 to 4.2v and the multiplying power of 0.1c; the first discharge specific capacity under 1C multiplying power is 108.2mAh/g; the capacity retention rate of the material is 95.5 percent after 500 weeks of cyclic charge and discharge under the multiplying power of 10C, namely the nitrogen-doped carbon-coated ferric sodium pyrophosphate phosphate composite material as the anode material has good multiplying power performance and long cycle life.
Example 2
The preparation method of the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material comprises the following steps:
s1, stirring 0.2g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer for 1h to dissolve at room temperature under the condition that the stirring speed is 300r/min, thus obtaining 40mL of template solution;
s2, adding 0.002mol (NH) into 40mL of template organic solution obtained in S1 4 ) 2 HPO 4 、0.004molNa 4 P 2 O 7 ·10H 2 O, 0.2493g fructose and 0.2493g glycine are dissolved in the solution;
s3, taking 0.012molFe (NO) 3 ) 3 ·9H 2 Stirring O at room temperature at a stirring speed of 200r/min for 0.5h to dissolve;
s4, dropwise adding the solution prepared in the S3 into the mixed solution of the S2 to obtain a suspension;
s5, stirring and evaporating the suspension of the S4 at the temperature of 80 ℃ at the speed of 500r/min, and drying to obtain a nano positive electrode precursor;
and S6, sintering the nano anode precursor obtained in the step S5 at 300 ℃ for 12h in a nitrogen atmosphere, cooling the nano anode precursor to room temperature along with a furnace, grinding the nano anode precursor in a mortar for 0.5h, and then performing solid-phase sintering at 500 ℃ for 10h to obtain the nitrogen-doped carbon-coated iron sodium pyrophosphate composite material.
The composite material prepared in the embodiment is prepared into a positive pole piece by the same method as the embodiment 1, and the positive pole piece is used for testing a positive pole material of a sodium-ion battery; the obtained nitrogen-doped carbon-coated ferric sodium pyrophosphate phosphate composite material as a positive electrode material has high specific capacity, good cycle stability and excellent electrochemical performance.
Example 3
The preparation method of the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material comprises the following steps:
s1, stirring 0.4g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer for 1h to dissolve at room temperature under the condition that the stirring speed is 300r/min, thus obtaining 40mL of template solution;
s2, adding 0.002mol Na into 40mL of template organic solution obtained in S1 2 HPO 4 、0.004mol Na 2 H 2 P 2 O 7 0.2493g of sucrose and 0.2493g of urea are dissolved in the solution;
s3, taking 0.012mol Fe (CH) 3 COO) 2 Stirring 4H2O at room temperature and at a stirring speed of 200r/min for 0.5H to dissolve;
s4, dropwise adding the solution prepared in the S3 into the mixed solution of the S2 to obtain a suspension;
s5, stirring and evaporating the suspension of the S4 at the temperature of 80 ℃ at the speed of 400r/min, and drying to obtain a nano positive electrode precursor;
and S6, sintering the nano anode precursor obtained in the S5 at 300 ℃ for 12 hours in a nitrogen atmosphere, cooling the nano anode precursor to room temperature along with a furnace, grinding the nano anode precursor in a mortar for 0.5 hour, and then performing solid-phase sintering at 500 ℃ for 10 hours to obtain the nitrogen-doped carbon-coated ferric sodium pyrophosphate phosphate composite material.
The composite material prepared in the embodiment is prepared into a positive pole piece by the same method as the embodiment 1, and the positive pole piece is used for testing the positive pole material of the sodium-ion battery; the obtained nitrogen-doped carbon-coated ferric sodium pyrophosphate phosphate composite material as a positive electrode material has high specific capacity and good cycle stability, and particularly shows excellent electrochemical performance under the condition of high-rate discharge.
The above description is only an example of the present invention, and the common general knowledge of the technical solutions or characteristics known in the solutions is not described herein too much. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (10)
1. The preparation method of the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material is characterized by comprising the following steps of:
s1, adding a template organic matter into water, and stirring and dissolving to obtain a template organic solution;
s2, adding a compound containing pyrophosphate, phosphate, a sodium source, a nitrogen source and a carbon source into the template organic solution obtained in the S1 to obtain a mixed solution;
s3, adding an iron source into water to obtain an iron source solution;
s4, dropwise adding the iron source solution obtained in the step S3 into the mixed solution of the step S2 to obtain a suspension;
s5, heating, stirring and evaporating the suspension obtained in the S4 to dryness, and drying to obtain a nano positive electrode precursor;
and S6, presintering the nano anode precursor obtained in the S5 under the protection of inert gas, naturally cooling, taking out, grinding, and sintering and cooling again under the protection of inert gas to obtain the nitrogen-doped mesoporous carbon coated iron sodium pyrophosphate composite material.
2. The method for preparing the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material according to claim 1, wherein the method comprises the following steps: in S1, the template organic matter is one or more of polyoxyethylene polyoxypropylene ether, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer and polyoxyethylene ether compound; the temperature of the stirring and dissolving process is room temperature, the stirring speed is 100-900 r/min, and the time is 1.0-3.0 h; the concentration of the obtained template organic matter solution is 1-100 g/L.
3. The method for preparing the nitrogen-doped mesoporous carbon-coated ferric sodium pyrophosphate composite material according to claim 1, wherein the method comprises the following steps: in S2, the pyrophosphate is one or more of trisodium monohydrogen pyrophosphate, disodium dihydrogen pyrophosphate, sodium trisodium pyrophosphate and hydrates thereof; the phosphate is one or more of ammonium phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate and hydrates thereof; the nitrogen source is one or more of urea, polyvinylpyrrolidone and glycine; the carbon source is one or more of glucose, fructose, galactose, lactose, sucrose, maltose and the nitrogen source.
4. The method for preparing the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material according to claim 1, wherein the method comprises the following steps: in S3, the iron source is one or more of ferric nitrate, ferric acetate, ferric ammonium oxalate, ferric citrate, ferric ammonium citrate, and hydrates thereof.
5. The method for preparing the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material according to claim 1, wherein the method comprises the following steps: in S4, adding the mixed solution of S2 into the iron source solution of S3 to obtain sodium in a suspension: iron: a phosphoric acid group: the molar mass ratio of the pyrophosphate groups is 4.
6. The method for preparing the nitrogen-doped mesoporous carbon-coated ferric sodium pyrophosphate composite material according to claim 1, wherein the method comprises the following steps: in S5, the obtained nano anode precursor is an iron salt precursor, and the mass ratio of the template organic matter to the precursor is 0.01-1: 1.
7. the method for preparing the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate phosphate composite material according to claim 1, wherein the method comprises the following steps: in S6, sintering of the nano anode precursor is solid-phase sintering, and the method comprises the following specific steps: presintering for 3-12 h at 250-400 ℃ under inert gas, taking out the material, grinding, and calcining for 9-15 h at 450-600 ℃; the inert gas is one or more of nitrogen or argon; the nitrogen element in the obtained nitrogen-doped mesoporous carbon-coated phosphoric acid ferric sodium pyrophosphate composite material is as follows: the molar mass ratio of the phosphoric acid ferric sodium pyrophosphate is 0.01-0.5; carbon element (C): the molar mass ratio of the ferric sodium pyrophosphate phosphate is 0.01-0.5.
8. The composite material prepared by the method for preparing the nitrogen-doped mesoporous carbon-coated iron sodium phosphate pyrophosphate composite material according to any one of claims 1 to 7.
9. The application of the composite material prepared by the preparation method of the nitrogen-doped mesoporous carbon coated iron sodium pyrophosphate composite material as defined in any one of claims 1 to 7 in a positive electrode material of a sodium ion battery.
10. The application of the composite material prepared by the preparation method of the nitrogen-doped mesoporous carbon-coated iron sodium pyrophosphate composite material as claimed in claim 9 in the positive electrode material of a sodium-ion battery is characterized in that: the template organic matter of the composite anode material is used as a template agent for generating the phosphoric acid ferric sodium pyrophosphate and is also used as a template agent of the nitrogen-doped mesoporous carbon coating layer.
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