CN114420883B - Sodium ion battery anode material PTA large Kong Cengzhuang carbon rod and preparation method thereof - Google Patents
Sodium ion battery anode material PTA large Kong Cengzhuang carbon rod and preparation method thereof Download PDFInfo
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- H01M4/00—Electrodes
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The invention discloses a sodium ion battery cathode material PTA large Kong Cengzhuang carbon rod and a preparation method thereof, wherein the preparation method comprises the following steps: mixing isopropanol or absolute ethyl alcohol with deionized water at room temperature, stirring for 4-8min, adding ammonia water, stirring for 50-80min, adding tannic acid, stirring for 25-35h, centrifuging, collecting solid, washing, and drying to obtain precursor PTA rod; and carrying out heat treatment on the precursor PTA rod to obtain the PTA macroporous layered carbon rod of the negative electrode material of the sodium ion battery. The negative electrode material PTA of the sodium ion battery prepared by the invention is a large Kong Cengzhuang carbon rod, has a regular material structure, a layered structure and pores, has good stability, and has higher specific capacity and good rate capability when being used as the negative electrode material of the sodium ion battery.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to a negative electrode material PTA large Kong Cengzhuang carbon rod of a sodium ion battery and a preparation method thereof.
Background
A number of non-carbonaceous materials with different sodium storage mechanisms have been developed as negative electrodes for sodium ion batteries, including metal oxides/sulfides (e.g., tiO 2 ，SnS 2 ，MoS 2 ) And metals/alloys (e.g. Sn, niSe 2 ) In general, these materials are being intercalated with Na + Serious volume changes still occur, resulting in reduced cycling stability. Therefore, the reasonable design and convenient synthesis of the non-noble metal material have high requirements on the sodium ion battery, and the carbon material with low price and simple manufacture has been widely studied as the negative electrode of the sodium ion battery, however, the defects of low theoretical specific capacity, non-ideal rate performance and the like prevent the carbon material with good structure from being in high-energy densityPractical application in sodium ion batteries is therefore still very desirable to develop carbon-based negative electrodes for high performance sodium ion batteries.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a carbon rod with a large PTA Kong Cengzhuang cathode material of a sodium ion battery and a preparation method thereof, so as to solve the problem that the theoretical specific capacity of the battery is too low when the existing carbon material is used as the cathode of the sodium ion battery.
The technical scheme for solving the technical problems is as follows: the preparation method of the large Kong Cengzhuang carbon rod of the negative electrode material PTA of the sodium ion battery comprises the following steps:
(1) Mixing isopropanol or absolute ethyl alcohol with deionized water at room temperature, stirring for 4-8min, adding ammonia water, stirring for 50-80min, adding tannic acid, stirring for 25-35h, centrifuging, collecting solid, washing, and drying to obtain precursor PTA rod;
(2) And carrying out heat treatment on the precursor PTA rod to obtain the PTA macroporous layered carbon rod of the negative electrode material of the sodium ion battery.
The beneficial effects of the invention are as follows: preparing a PTA (poly tannic acid) rod serving as a precursor into a PTA large Kong Cengzhuang carbon rod, wherein the PTA with a highly ordered layered structure induces two-step shrinkage with limited space, the first-step shrinkage occurs at a low carbonization temperature, and O-H groups are subjected to dehydration reaction, so that the distance between adjacent layers is reduced; the second step of shrinkage proceeds with increasing temperature, and in-plane shrinkage occurs. This shrinkage behavior results in large surface area, high porosity and rich defects in the macroporous carbon structure, whereas the porous layered structure can provide a large number of storage sites for sodium ions, contributing to the improvement of the capacity performance of the anode, and the presence of microporous and mesoporous structures indicates that the material has high capacity for storing sodium and low resistance during ion transport.
Based on the technical scheme, the invention can also be improved as follows:
further, in the step (1), the volume ratio of the isopropanol or absolute ethyl alcohol to the deionized water to the ammonia water is 40-60:90-110:0.75-1.
Further, the volume-mass ratio of the ammonia water and the tannic acid in the step (1) is (0.75-1:0.3-0.45) ml/g.
Further, the stirring speed in the step (1) is 80-120r/min.
Further, the rotational speed of the centrifugation in the step (1) is 9000-12000r/min.
Further, in the step (1), washing is sequentially performed by deionized water and absolute ethyl alcohol.
Further, the drying in the step (1) is drying at a temperature of 55-65 ℃ for 10-15 hours.
Further, the specific steps of the heat treatment in the step (2) are as follows: in Ar 2 Calcining the precursor PTA rod for 1.8-2.5h at 650-750 ℃ in the atmosphere.
The invention also provides the sodium ion battery negative electrode material PTA macroporous layered carbon rod prepared by the preparation method of the sodium ion battery negative electrode material PTA large Kong Cengzhuang carbon rod.
The invention also provides an application of the negative electrode material PTA large Kong Cengzhuang carbon rod of the sodium ion battery in preparing sodium ion batteries.
The invention has the following beneficial effects:
1. the negative electrode material PTA of the sodium ion battery prepared by the invention is a large Kong Cengzhuang carbon rod, and the raw materials are easy to obtain and environment-friendly.
2. The preparation method disclosed by the invention is simple in formula, easy to operate, good in repeatability and high in product purity.
3. The negative electrode material PTA of the sodium ion battery prepared by the invention is a large Kong Cengzhuang carbon rod, has a regular material structure, a layered structure and pores, has good stability, and has higher specific capacity and good rate capability when being used as the negative electrode material of the sodium ion battery.
Drawings
FIG. 1 is an SEM image of a large Kong Cengzhuang carbon rod of PTA prepared in example 1;
fig. 2 is a cycle stability test chart of a coin cell made of the PTA macroporous layered carbon rod prepared in example 1;
fig. 3 is a graph for testing the cycle stability of a coin cell made of the PTA macroporous layered carbon rod prepared in example 2;
fig. 4 is a cycle stability test chart of a coin cell made of the PTA macroporous layered carbon rod prepared in example 3;
fig. 5 is a graph showing the cycle stability test of a coin cell made of the PTA carbon rod prepared in comparative example 2.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1:
the preparation method of the sodium ion battery cathode material PTA large Kong Cengzhuang carbon rod comprises the following steps:
(1) Mixing 60ml of isopropanol and 90ml of deionized water at room temperature, stirring for 5min at a rotating speed of 100r/min, adding 1ml of ammonia water, stirring for 60min at a rotating speed of 100r/min, adding 0.45g of tannic acid, stirring for 30h at a rotating speed of 100r/min, centrifugally collecting solids at a rotating speed of 10000r/min by a high-speed centrifugal machine, washing with deionized water and absolute ethyl alcohol sequentially, placing in a constant-temperature vacuum oven, and drying at a temperature of 60 ℃ for 12h to obtain yellow powder, namely a precursor PTA rod;
(2) In Ar 2 Calcining the precursor PTA rod for 2 hours at 700 ℃ in the atmosphere at a heating rate of 5 ℃/min to obtain black powder, namely the PTA macroporous lamellar carbon rod of the negative electrode material of the sodium ion battery.
Example 2:
the preparation method of the sodium ion battery cathode material PTA large Kong Cengzhuang carbon rod comprises the following steps:
(1) Mixing 40ml of absolute ethyl alcohol and 110ml of deionized water at room temperature, stirring for 8min at the rotating speed of 80r/min, adding 0.8ml of ammonia water, stirring for 80min at the rotating speed of 80r/min, adding 0.4g of tannic acid, stirring for 35h at the rotating speed of 80r/min, centrifugally collecting solids at the rotating speed of 9000r/min by a high-speed centrifugal machine, washing with deionized water and absolute ethyl alcohol sequentially, placing in a constant-temperature vacuum oven, and drying for 15h at the temperature of 55 ℃ to obtain yellow powder, namely a precursor PTA rod;
(2) In Ar 2 Calcining the precursor PTA rod for 2.5 hours at 650 ℃ in the atmosphere at a heating rate of 5 ℃/min to obtain black powder, namely the PTA macroporous lamellar carbon rod of the negative electrode material of the sodium ion battery.
Example 3:
the preparation method of the sodium ion battery cathode material PTA large Kong Cengzhuang carbon rod comprises the following steps:
(1) Mixing 50ml of isopropanol and 100ml of deionized water at room temperature, stirring for 4min at a rotation speed of 120r/min, adding 1ml of ammonia water, stirring for 50min at a rotation speed of 120r/min, adding 0.45g of tannic acid, stirring for 25h at a rotation speed of 120r/min, centrifugally collecting solids at a rotation speed of 12000r/min by a high-speed centrifugal machine, washing with deionized water and absolute ethyl alcohol in sequence, placing in a constant-temperature vacuum oven, and drying at 65 ℃ for 10h to obtain yellow powder, namely a precursor PTA rod;
(2) In Ar 2 Calcining the precursor PTA rod for 1.8h at 750 ℃ in the atmosphere at a heating rate of 5 ℃/min to obtain black powder, namely the PTA macroporous lamellar carbon rod of the negative electrode material of the sodium ion battery.
Comparative example 1:
the preparation method of the PTA carbon rod for the negative electrode material of the sodium ion battery comprises the following steps:
180ml of isopropanol and 90ml of deionized water are mixed at room temperature, stirred for 5min at a rotation speed of 100r/min, then 1ml of ammonia water is added, stirred for 60min at a rotation speed of 100r/min, then 0.45g of tannic acid is added, and stirred for 30h at a rotation speed of 100r/min, and suspension is not generated, namely no precursor PTA rod is generated.
Comparative example 2:
the preparation method of the PTA carbon rod for the negative electrode material of the sodium ion battery comprises the following steps:
(1) Mixing 60ml of isopropanol and 90ml of deionized water at room temperature, stirring for 5min at a rotating speed of 100r/min, adding 1ml of ammonia water, stirring for 60min at a rotating speed of 100r/min, adding 0.45g of tannic acid, stirring for 30h at a rotating speed of 100r/min, centrifugally collecting solids at a rotating speed of 10000r/min by a high-speed centrifugal machine, washing with deionized water and absolute ethyl alcohol sequentially, placing in a constant-temperature vacuum oven, and drying at a temperature of 60 ℃ for 12h to obtain yellow powder, namely a precursor PTA rod;
(2) In Ar 2 And calcining the precursor PTA rod for 2 hours at 600 ℃ in the atmosphere at a heating rate of 5 ℃/min to obtain black powder, namely the sodium ion battery negative electrode material PTA carbon rod.
Test examples
1. Morphology of PTA large Kong Cengzhuang carbon rod
The morphology of the anode material PTA large Kong Cengzhuang carbon rod of the sodium ion battery prepared in the examples 1-3 is similar, therefore, SEM detection is carried out by taking the anode material PTA large Kong Cengzhuang carbon rod of the sodium ion battery prepared in the example 1, and the result is shown in figure 1. As can be seen from figure 1, the anode material PTA large Kong Cengzhuang carbon rod of the sodium ion battery prepared in the invention has a layered structure and pores, and the precursor PTA rod is contracted to generate the layered structure in the calcining and carbonizing process, and gas NH is generated in the PTA heating and calcining process 3 And CO 2 Thus forming pores.
2. Electrochemical performance of PTA big Kong Cengzhuang carbon rod
The button cell prepared by the sodium ion cell cathode material PTA big Kong Cengzhuang carbon rod prepared in the examples 1-3 and the PTA carbon rod prepared in the comparative example 2 are respectively subjected to electrochemical performance test, and the specific method for preparing the button cell comprises the following steps: the prepared PTA large Kong Cengzhuang carbon rod, acetylene black and polyvinylidene fluoride (PVDF) are mixed according to the mass ratio of 8:1:1, adding the copper foil into a mortar, adding N-methyl pyrrolidone, grinding until the mixture is uniform, coating the slurry on the copper foil, and moving the copper foil to a vacuum oven at 60 ℃ for 12 hours; ethylene carbonate and ethylene carbonate are mixed according to the volume ratio of 1:1, mixing, and then adding sodium perchlorate to prepare an electrolyte, wherein the concentration of the sodium perchlorate in the electrolyte is 1mol/L; then, button cells were fabricated in a glove box.
The sodium ion battery cathode material PTA macroporous layered carbon rod prepared in the example 1 is manufactured into a button battery, a constant current charge and discharge test is carried out on a NEWARE battery test system, the cut-off voltage of the sodium ion battery is set to be 0.01V to 3.0V, and the current density is set to be 100mAg -1 The number of cycles was 100. The test results are shown in FIG. 2, and it can be seen from FIG. 2 that the PTA macroporous layered carbon rod prepared by the invention is made into a button cell at 100mAg -1 After 100 cycles of current density, the specific capacity was maintained at 212mAhg -1 The initial coulombic efficiency was 43%, mainly because of electrolyte decomposition and SEI formation on the material surface, and the subsequent coulombic efficiency tended to stabilize.
The negative electrode material PTA macroporous layered carbon rod of the sodium ion battery prepared in the example 2 is manufactured into a button battery, a constant current charge and discharge test is carried out on a NEWARE battery test system, the cut-off voltage of the sodium ion battery is set to be 0.01V to 3.0V, and the current density is set to be 500mAg -1 The number of cycles was 100. The test result is shown in FIG. 3, and it can be seen from FIG. 3 that the PTA macroporous layered carbon rod prepared by the invention is made into a button cell at 500mAg -1 After 100 cycles, the specific capacity was maintained at 159mAhg -1 It can be seen that at relatively high current densities, the capacity fade is also very small and the reversibility is very good, in addition to the first-turn coulombic efficiency, which is then kept very stable.
The negative electrode material PTA macroporous layered carbon rod of the sodium ion battery prepared in the example 3 is manufactured into a button battery, a constant current charge and discharge test is carried out on a NEWARE battery test system, the cut-off voltage of the sodium ion battery is set to be 0.01V to 3.0V, and the current density is set to be 1Ag -1 The number of cycles was 300. The test results are shown in FIG. 4, and it can be seen from FIG. 4 that the PTA macroporous layered carbon rod prepared by the invention is made into button cell with 1Ag -1 After 300 cycles, the specific capacity was kept at 105mAhg -1 It can be seen that at high current densities, the capacity is substantially unattenuated and the reversibility is very good.
The sodium ion battery cathode material PTA carbon rod prepared in comparative example 2 is made into a button battery, constant current charge and discharge test is carried out on a NEWARE battery test system, and the sodium ion battery is arrangedHas a cutoff voltage of 0.01V to 3.0V and a current density of 100mAg -1 The number of cycles was 100. The test results are shown in FIG. 4, and it can be seen from FIG. 4 that the battery prepared in comparative example 2 has poor cycle stability and low capacity at 100mAg -1 After 100 cycles of current density, the specific capacity was maintained at 138mAhg -1 This is because the lower carbonization temperature results in incomplete shrinkage of the material structure, lower porosity and defects, lower specific surface area and pores are detrimental to electrolyte penetration and Na + The diffusion of ions greatly reduces the capacity.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (7)
1. The preparation method of the carbon rod with the size Kong Cengzhuang of the negative electrode material PTA of the sodium ion battery is characterized by comprising the following steps of:
(1) Mixing isopropanol or absolute ethyl alcohol with deionized water at room temperature, stirring for 4-8min, adding ammonia water, stirring for 50-80min, adding tannic acid, stirring for 25-35h, centrifuging, collecting solid, washing, and drying to obtain precursor PTA rod;
(2) Performing heat treatment on the precursor PTA rod to obtain a carbon rod of the negative electrode material PTA of the sodium ion battery, wherein the carbon rod is Kong Cengzhuang;
in the step (1), the volume ratio of the isopropanol or absolute ethyl alcohol to the deionized water to the ammonia water is 40-60:90-110:0.75-1;
the volume-mass ratio of the ammonia water to the tannic acid in the step (1) is (0.75-1:0.3-0.45) ml/g;
the specific steps of the heat treatment in the step (2) are as follows: in Ar 2 Calcining the precursor PTA rod for 1.8-2.5h at 650-750 ℃ in the atmosphere.
2. The method for preparing a carbon rod of a negative electrode material PTA large Kong Cengzhuang for sodium ion batteries according to claim 1, wherein the stirring speed in the step (1) is 80-120r/min.
3. The method for preparing a carbon rod of a negative electrode material PTA large Kong Cengzhuang for sodium ion batteries according to claim 1, wherein the rotational speed of centrifugation in the step (1) is 9000-12000r/min.
4. The method for preparing a carbon rod of a negative electrode material PTA large Kong Cengzhuang for sodium ion batteries according to claim 1, wherein the washing in the step (1) is sequentially carried out with deionized water and absolute ethyl alcohol.
5. The method for preparing a carbon rod of a negative electrode material PTA large Kong Cengzhuang for sodium ion battery according to claim 1, wherein the drying in the step (1) is performed at 55-65 ℃ for 10-15h.
6. A sodium ion battery anode material PTA macroporous layered carbon rod prepared by the method for preparing a sodium ion battery anode material PTA large Kong Cengzhuang carbon rod according to any one of claims 1-5.
7. The use of the negative electrode material PTA big Kong Cengzhuang carbon rod for sodium ion battery of claim 6 in preparing sodium ion battery.
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| CN105870425A (en) * | 2016-06-08 | 2016-08-17 | 中南大学 | Sodium-ion battery carbon negative electrode material and preparation method thereof |
| CN106910880A (en) * | 2017-03-28 | 2017-06-30 | 中南大学 | A kind of sodium-ion battery carbon ball negative material and preparation method thereof |
| CN113422051A (en) * | 2021-06-15 | 2021-09-21 | 杭州职业技术学院 | Carbon nanotube-string carbon hollow polyhedron nanosphere material and preparation and application thereof |
| CN113659143A (en) * | 2021-08-06 | 2021-11-16 | 东莞市创明电池技术有限公司 | Preparation method of negative electrode material of sodium ion battery, negative electrode material and sodium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105870425A (en) * | 2016-06-08 | 2016-08-17 | 中南大学 | Sodium-ion battery carbon negative electrode material and preparation method thereof |
| CN106910880A (en) * | 2017-03-28 | 2017-06-30 | 中南大学 | A kind of sodium-ion battery carbon ball negative material and preparation method thereof |
| CN113422051A (en) * | 2021-06-15 | 2021-09-21 | 杭州职业技术学院 | Carbon nanotube-string carbon hollow polyhedron nanosphere material and preparation and application thereof |
| CN113659143A (en) * | 2021-08-06 | 2021-11-16 | 东莞市创明电池技术有限公司 | Preparation method of negative electrode material of sodium ion battery, negative electrode material and sodium ion battery |
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