CN109449379B - Nitrogen-doped carbon composite SnFe2O4Lithium ion battery cathode material and preparation method and application thereof - Google Patents
Nitrogen-doped carbon composite SnFe2O4Lithium ion battery cathode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nitrogen-doped carbon composite SnFe2O4The preparation method of the lithium ion battery negative electrode material comprises the following steps: 1) the iron source and the tin source are coprecipitated to generate SnFe under the action of a surfactant Tween-202O4A nanoparticle; 2) SnFe2O4Reacting the nanoparticles with dopamine hydrochloride in a Tris-HCl buffer solution to prepare a precursor; 3) and calcining the precursor under an inert atmosphere. The invention relates to a lithium ion battery cathode material which is nitrogen-doped carbon composite SnFe2O4The nano-particles have the advantages of stable structure, high charge-discharge efficiency, excellent cycle performance, good electrochemical reversibility and the like, and the preparation method is simple in preparation process, low in cost, environment-friendly, suitable for practical application of lithium ion batteries and capable of realizing industrial large-scale production.
Description
Technical Field
The invention relates to nitrogen-doped carbon composite SnFe2O4A lithium ion battery cathode material and a preparation method and application thereof belong to the technical field of lithium ion batteries.
Background
Theoretical capacity of current, commercial graphite negative electrode materials (372mAh g)-1) The lithium ion battery has low diffusion rate and can not meet the development trend of high energy density and high multiplying power charge and discharge capacity of the lithium ion battery. Therefore, finding a new negative electrode material capable of replacing graphite has become a great hot spot in the research field of lithium ion batteries in recent years.
Among the numerous negative electrode materials, Sn-based negative electrode materials have a high theoretical specific capacity, such as SnO2(1494mAh·g-1)、SnO (1138mAh·g-1)、Sn(991mAh·g-1) And the production cost is low, so that the method is considered to have the best application prospect. However, tin-based negative electrode materials suffer from two major drawbacks: 1) SnOxAnd Li+The conversion reaction of (a) is irreversible, resulting in a loss of charge-discharge capacity in the first cycleSevere, coulombic efficiency is only about 50%; 2) metallic Sn and Li+The alloying/dealloying reaction can cause the metal Sn to generate huge volume expansion (up to 300 percent), so that the Sn-based material is deformed, cracked, dropped and the like, the electrical contact performance is deteriorated, and finally the specific capacity of the material is rapidly reduced.
In order to solve the above problems, researchers at home and abroad have reduced the absolute volume expansion in the lithium intercalation/deintercalation process by nano-structuring or specially structuring the material, or have effectively relieved the volume expansion generated in the charge and discharge process by doping or coating other substances by utilizing the synergistic effect in recent years. For example: preparation of binary metal oxide transition metal acid salt AFe with spinel structure2O4(A is Zn, Co, Ni, Cu or Mn), by increasing Li+The de-intercalation in the spinel structure and the structural stability during charge and discharge are maintained to improve the problems of volume over-expansion and stability of the single metal oxide.
Tin ferrite (SnFe)2O4) Is a material with inverse spinel structure, has three-dimensional diffusion channel in the inverse spinel structure, and is beneficial to Li+The migration diffusion of (2) is also beneficial to high-rate charge and discharge, the charge and discharge platform (about 1.05V) is lower than other transition metal oxides, and the theoretical specific capacity (about 1130mAh g)-1) Higher than pure metal oxide and inactive ferrite (such as CuFe)2O4). However, tin ferrite has low conductivity and excessive volume expansion rate in the charging and discharging processes of the lithium ion battery, which can cause the structural damage of the material, and further cause the rapid decrease of the specific capacity, the cycling stability and other performances. Therefore, cheap and environment-friendly SnFe is prepared by improving the material structure or doping the carbon material with good conductivity2O4The lithium ion negative electrode material compounded with carbon improves the specific capacity, the coulombic efficiency, the rate capability and the cycling stability of the first discharge of the lithium battery, and has important significance for the field of the lithium ion battery.
Disclosure of Invention
The invention aims to provide nitrogen-doped carbon composite SnFe2O4A lithium ion battery cathode material, a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
nitrogen-doped carbon composite SnFe2O4The preparation method of the lithium ion battery negative electrode material comprises the following steps:
1) adding an iron source and a tin source into a Tween-20 aqueous solution at the same time, fully and uniformly stirring, adding an alkali solution, fully reacting, separating and collecting precipitates to obtain SnFe2O4A nanoparticle;
2) SnFe2O4Adding the nano-particles and dopamine hydrochloride into a Tris-HCl buffer solution, fully reacting, and centrifuging to collect a solid product to obtain a precursor;
3) calcining the precursor in inert atmosphere to obtain the nitrogen-doped carbon composite SnFe2O4A lithium ion battery cathode material.
The molar ratio of Fe to Sn in the step 1) is 1: 0.5.
The iron source in the step 1) is at least one of ferrous chloride tetrahydrate, ferric trichloride, ferric nitrate nonahydrate, ferrous oxalate, ferrous sulfate and ferric sulfate.
The tin source in the step 1) is at least one of stannous chloride dihydrate and stannous sulfate.
The tween-20 aqueous solution in the step 1) is prepared from tween-20 and water according to the volume ratio of 1: (10-50) mixing.
The alkali solution in the step 1) is one of NaOH solution and ammonia water.
The reaction in the step 1) is carried out at the temperature of 20-80 ℃, and the reaction time is 2-4 h.
Step 2) said SnFe2O4The mass ratio of the nano particles to the dopamine hydrochloride is 1: (0.1-0.5).
The reaction in the step 2) is carried out at the temperature of 20-80 ℃, and the reaction time is 2-4 h.
The calcination in the step 3) is specifically as follows: heating to 600-800 ℃ at a rate of 1-5 ℃/min and keeping for 1-2 h.
The invention has the beneficial effects that: the invention relates to a lithium ion battery cathode material which is nitrogen-doped carbon composite SnFe2O4Nanoparticles (SnFe)2O4@ NC), has the advantages of stable structure, high charge-discharge efficiency, excellent cycle performance, good electrochemical reversibility and the like, has simple preparation process, low cost and environmental friendliness, is suitable for the practical application of lithium ion batteries, and can realize industrialized large-scale production.
1) SnFe in the invention2O4The mechanism of lithium storage of (A) involves Li+De-intercalation and Li in inverse spinel three-dimensional channels+With SnO and Fe2O3Conversion reaction of (1), Li+Three alloying reactions with Sn, its charge-discharge platform is lower than that of transition metal oxide, and its theoretical specific capacity is 1130 mAh.g-1Higher than SnO and Fe2O3And the like;
2) the nitrogen-doped carbon layer has good conductivity and can improve SnFe2O4The conductivity of @ NC, so that the material shows better rate performance in the charge-discharge process;
3) the nitrogen-doped carbon layer can be used as a buffer layer, so that the volume change of the material in the charge-discharge process can be effectively relieved, and the stable structure of the material is ensured, thereby improving the cycle performance and the rate performance of the material;
4) SnFe in the invention2O4The synthesis method of the nano particles and the polymerization method of the nano particles and dopamine hydrochloride are very simple, low in production cost, low in energy consumption and environment-friendly, are suitable for practical application of lithium ion batteries, and can realize industrial large-scale production.
Drawings
FIG. 1 is SnFe of example 12O4And SnFe of examples 1 to 32O4X-ray powder diffractogram (XRD) of @ NC.
FIG. 2 is SnFe of example 12O4Scanning Electron Microscopy (SEM) for @ NC.
FIG. 3 is SnFe of example 12O4CV plot of the first 3 cycles of half-cell cycle of @ NC assembly.
FIG. 4 is SnFe of example 12O4Assembled half-cell at current densityDegree of 0.2 A.g-1Cycle performance graph below.
FIG. 5 shows SnFe of example 12O4Current density of 0.2A g of half-cell assembled at @ NC-1Cycle performance graph below.
FIG. 6 is SnFe of example 12O4Rate performance plot for the @ NC assembled half-cell.
Detailed Description
Nitrogen-doped carbon composite SnFe2O4The preparation method of the lithium ion battery negative electrode material comprises the following steps:
1) adding an iron source and a tin source into a Tween-20 aqueous solution at the same time, fully and uniformly stirring, adding an alkali solution, fully reacting, separating and collecting precipitates to obtain SnFe2O4A nanoparticle;
2) SnFe2O4Adding the nano-particles and dopamine hydrochloride into a Tris-HCl buffer solution, fully reacting, and centrifuging to collect a solid product to obtain a precursor;
3) calcining the precursor in inert atmosphere to obtain the nitrogen-doped carbon composite SnFe2O4Lithium ion battery cathode material (SnFe)2O4@NC)。
Preferably, the molar ratio of Fe to Sn in step 1) is 1: 0.5.
Preferably, the concentration of the iron source in the tween-20 aqueous solution in the step 1) is 0.02-0.5 mol/L.
Preferably, the concentration of the tin source in the tween-20 aqueous solution in the step 1) is 0.01-0.1 mol/L.
Preferably, the iron source in step 1) is at least one of ferrous chloride tetrahydrate, ferric chloride, ferric nitrate nonahydrate, ferrous oxalate, ferrous sulfate and ferric sulfate.
Further preferably, the iron source in step 1) is at least one of ferrous chloride tetrahydrate and ferric nitrate nonahydrate.
Preferably, the tin source in step 1) is at least one of stannous chloride dihydrate and stannous sulfate.
Preferably, the tween-20 aqueous solution in the step 1) is prepared from tween-20 and water according to a volume ratio of 1: (10-50) mixing.
Preferably, the alkali solution in step 1) is one of a NaOH solution and an ammonia water, and is used for adjusting the pH value of the reaction solution to be greater than 10.
Preferably, the reaction in the step 1) is carried out at 20-80 ℃, and the reaction time is 2-4 h.
Preferably, the SnFe in the step 2)2O4The mass ratio of the nano particles to the dopamine hydrochloride is 1: (0.1-0.5).
Preferably, the reaction in the step 2) is carried out at 20-80 ℃, and the reaction time is 2-4 h.
Preferably, the inert atmosphere in step 3) is a nitrogen atmosphere or an argon atmosphere.
Preferably, the calcination in step 3) is specifically: heating to 600-800 ℃ at the speed of 1-5 ℃/min and keeping for 1-2 h.
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
nitrogen-doped carbon composite SnFe2O4Lithium ion battery cathode material (SnFe)2O4@ NC), comprising the following steps:
1) 12mmol of FeCl2·4H2O and 6mmol of SnCl2·2H2Adding O into 150mL of Tween-20 aqueous solution (prepared from Tween-20 and distilled water according to the volume ratio of 1: 10), stirring thoroughly, adding 4mol/L NaOH solution until the pH value of the reaction solution>Stirring at 10 deg.C and 80 deg.C for 3h, separating and collecting precipitate, washing precipitate with distilled water for multiple times, and drying at 60 deg.C for 10h to obtain SnFe2O4Nanoparticles (XRD pattern shown in figure 1);
2) SnFe with the mass ratio of 1:0.32O4Adding the nanoparticles and dopamine hydrochloride into a Tris-HCl buffer solution (pH 8.5) with the concentration of 10mmol/L, stirring for 4h at 80 ℃, centrifuging again, collecting a solid product, washing the solid product with distilled water for multiple times, and drying for 10h at 60 ℃ to obtain a precursor;
3) will be provided withThe precursor is put in nitrogen atmosphere, and is heated to 700 ℃ at the speed of 5 ℃/min and kept for 1h to obtain the nitrogen-doped carbon composite SnFe2O4The lithium ion battery cathode material (XRD pattern is shown in figure 1; SEM pattern is shown in figure 2).
Respectively with SnFe2O4Nanoparticles and SnFe2O4And @ NC is a negative electrode active material, and the negative electrode active material and the metal lithium are assembled into a lithium ion button half-cell for electrochemical performance test.
Assembling the lithium ion button half cell: mixing a negative electrode active material, Super P Li conductive carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, uniformly mixing with N-methyl pyrrolidone, stirring into a viscous state, coating the viscous state on copper foil, drying at 120 ℃ in vacuum for 10 hours, and cutting into a pole piece with the diameter of about 12mm as a working electrode, wherein a Li piece is a counter electrode. The diaphragm is Celgard polyethylene microporous film, and the electrolyte is LiPF with the concentration of 1mol/L6The mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC) and Ethyl Methyl Carbonate (EMC) is prepared (the volume ratio of EC, DMC and EMC in the mixed electrolyte is 1:1: 1).
Half-cells were assembled in an argon-filled glove box using CR2032 button cells.
And (3) electrochemical performance testing: the test was carried out with a Newware CT-3008 battery test system (Shenzhen New Wille electronics, Inc.).
SnFe of example 12O4The CV curve plot of 3 cycles before the half cell cycle of @ NC assembly is shown in FIG. 3 (test conditions: 0.01-3.0V, sweep rate 0.1 mV/s).
SnFe of example 12O4The assembled half-cell was operated at a current density of 0.2 A.g-1The cycle performance chart below is shown in fig. 4.
SnFe of example 12O4Current density of 0.2A g of half-cell assembled at @ NC-1The cycle performance of the following is shown in fig. 5.
SnFe of example 12O4The rate performance plot of the @ NC assembled half cell is shown in figure 6.
Example 2:
nitrogen-doped carbon composite SnFe2O4Lithium ionAnode material of sub-battery (SnFe)2O4@ NC), comprising the following steps:
1) 15mmol of Fe (NO)3)3·9H2O and 7.5mmol of SnCl2·2H2Adding O into 150mL of Tween-20 aqueous solution (prepared from Tween-20 and distilled water according to the volume ratio of 1: 25), stirring thoroughly, adding 4mol/L NaOH solution until the pH value of the reaction solution>Stirring at 10 and 25 deg.C for 4h, separating and collecting precipitate, washing precipitate with distilled water for multiple times, and drying at 80 deg.C for 6h to obtain SnFe2O4A nanoparticle;
2) SnFe with the mass ratio of 1:0.12O4Adding the nanoparticles and dopamine hydrochloride into a Tris-HCl buffer solution (pH 8.5) with the concentration of 10mmol/L, stirring for 6h at 25 ℃, centrifuging again, collecting a solid product, washing the solid product with distilled water for multiple times, and drying for 10h at 80 ℃ to obtain a precursor;
3) placing the precursor in argon atmosphere, raising the temperature to 600 ℃ at the speed of 2 ℃/min and keeping the temperature for 2h to obtain the nitrogen-doped carbon composite SnFe2O4The lithium ion battery cathode material (XRD pattern is shown in figure 1; the product morphology is consistent with that of example 1).
Example 3:
nitrogen-doped carbon composite SnFe2O4Lithium ion battery cathode material (SnFe)2O4@ NC), comprising the following steps:
1) 15mmol of Fe (NO)3)3·9H2O and 7.5mmol of SnCl2·2H2Adding O into 150mL of Tween-20 aqueous solution (prepared from Tween-20 and distilled water according to the volume ratio of 1: 10), stirring thoroughly, mixing well, adding ammonia water with the mass fraction of 25% until the pH value of the reaction solution>Stirring at 10 deg.C and 80 deg.C for 2h, separating and collecting precipitate, washing precipitate with distilled water for multiple times, and drying at 60 deg.C for 10h to obtain SnFe2O4A nanoparticle;
2) SnFe with the mass ratio of 1:0.52O4The nanoparticles and dopamine hydrochloride were added to a Tris-HCl buffer (pH 10 mmol/L)8.5), stirring for 4h at 50 ℃, centrifuging again to collect a solid product, washing the solid product with distilled water for multiple times, and drying for 10h at 60 ℃ to obtain a precursor;
3) placing the precursor in nitrogen atmosphere, raising the temperature to 700 ℃ at the speed of 5 ℃/min and keeping the temperature for 1h to obtain the nitrogen-doped carbon composite SnFe2O4The lithium ion battery cathode material (XRD pattern is shown in figure 1; the product morphology is consistent with that of example 1).
And (3) analyzing a test result:
as can be seen from fig. 1: SnFe of example 12O4And SnFe of examples 1 to 32O4The crystal diffraction peaks of @ NC are all equal to the standard JCPDS #11-0614SnFe2O4The diffraction peaks of the crystals (A) correspond to one another.
As can be seen from fig. 2: SnFe prepared in example 12O4The @ NC is granular, and the particle size of the granules is 50-100 nm.
As can be seen from fig. 3: the first turn of the graph shows a distinct redox peak, in which the discharge branches correspond to Li, respectively+Embedding inverse spinel structure (1.3-1.5V weak peak) and Li+And Sn2+And Fe3+Oxidation-reduction reaction of (1), accompanied by the formation of SEI film (0.5V), Sn and Li+Alloying reaction (0.05V); the charging branches correspond to Li respectivelyxSn dealloying reaction (0.15V), Sn and Fe with Li2Oxidation-reduction reaction of O (1.65V). The latter two and three rings except Li+And Sn2+And Fe3+The redox reaction of (2) is shifted to the right beyond 0.77V, and other peak positions are basically coincided with the first circle, which indicates that the reversibility of the reaction is good.
As can be seen from fig. 4: SnFe of example 12O4Has good cycle performance and self-growth performance.
As can be seen from fig. 5: SnFe of example 12O4@ NC has good cycling stability.
As can be seen from fig. 6: SnFe of example 12O4@ NC has good rate capability.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. Nitrogen-doped carbon composite SnFe2O4The preparation method of the lithium ion battery cathode material is characterized by comprising the following steps: the method comprises the following steps:
1) adding an iron source and a tin source into a Tween-20 aqueous solution at the same time, fully and uniformly stirring, adding an alkali solution, fully reacting, separating and collecting precipitates to obtain SnFe2O4A nanoparticle;
2) SnFe2O4Adding the nano-particles and dopamine hydrochloride into a Tris-HCl buffer solution, fully reacting, and centrifuging to collect a solid product to obtain a precursor;
3) calcining the precursor in inert atmosphere to obtain the nitrogen-doped carbon composite SnFe2O4A lithium ion battery negative electrode material;
the iron source in the step 1) is at least one of ferrous chloride tetrahydrate, ferric trichloride, ferric nitrate nonahydrate, ferrous oxalate, ferrous sulfate and ferric sulfate;
the tin source in the step 1) is at least one of stannous chloride dihydrate and stannous sulfate;
step 2) said SnFe2O4The mass ratio of the nano particles to the dopamine hydrochloride is 1: (0.1 to 0.5);
the calcination in the step 3) is specifically as follows: heating to 600-800 ℃ at a rate of 1-5 ℃/min and keeping for 1-2 h.
2. The method of claim 1, wherein: the molar ratio of Fe to Sn in the step 1) is 1: 0.5.
3. The method of claim 1, wherein: the tween-20 aqueous solution in the step 1) is prepared from tween-20 and water according to the volume ratio of 1: (10-50) mixing; the alkali solution in the step 1) is one of NaOH solution and ammonia water.
4. The production method according to claim 1 or 3, characterized in that: the reaction in the step 1) is carried out at the temperature of 20-80 ℃, and the reaction time is 2-4 h.
5. The method of claim 1, wherein: the reaction in the step 2) is carried out at the temperature of 20-80 ℃, and the reaction time is 2-4 h.
6. Nitrogen-doped carbon composite SnFe2O4The lithium ion battery cathode material is characterized in that: prepared by the method of any one of claims 1 to 5.
7. The nitrogen-doped carbon composite SnFe of claim 62O4The application of the lithium ion battery negative electrode material in the preparation of the lithium ion battery.
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| CN111029563B (en) * | 2019-12-10 | 2022-11-29 | 河南创力新能源科技股份有限公司 | Preparation method of alkaline secondary battery iron negative electrode material |
| CN114628669B (en) * | 2020-12-10 | 2023-11-07 | 中国科学院大连化学物理研究所 | Carbon carrier nitrogen doped Fe 2 O 3 @ NC, preparation and application thereof |
| CN112928273B (en) * | 2021-01-29 | 2022-07-26 | 华南师范大学 | Lithium ion battery cathode material and preparation method and application thereof |
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