CN112582595A - C/SnO of lithium ion battery2Preparation method and application of/rGO composite anode material - Google Patents
C/SnO of lithium ion battery2Preparation method and application of/rGO composite anode material Download PDFInfo
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Abstract
The invention discloses a lithium ion battery C/SnO2A preparation method and application of/rGO composite cathode material relate to the technical field of lithium ion batteries, and the preparation method comprises the following steps: dissolving tin tetrachloride pentahydrate in ethylene glycol, and stirring and dispersing to obtain a solution A; adding sodium gluconate into the graphene oxide dispersion liquid, and stirring and dispersing to obtain a solution B; dripping the solution A into the solution B under stirring, and stirring to obtain a black mixed solution; transferring the black mixed solution into a reaction kettle, heating for reaction, and cooling to obtain a black suspension; the black suspension was centrifuged and,washing and centrifuging to obtain a precipitate; dissolving the precipitate in anhydrous ethanol, ultrasonically dispersing, drying, and grinding. The invention utilizes a solvothermal method to grow SnO on the surface of rGO in situ2Nanoparticles in SnO2The surface of the nano-particles is coated with a layer of amorphous carbon, and the obtained composite material can effectively inhibit SnO2The volume expansion of the lithium ion battery shortens a lithium ion diffusion path, and has good circulation stability and higher reversible capacity performance.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a C/SnO lithium ion battery2Preparation method and application of/rGO composite negative electrode material.
Background
With the development of socio-economic, the productivity is improved, the global demand for energy is continuously increased, and the main sources are three traditional non-renewable energy sources (natural gas, coal and petroleum). Due to the extensive and inefficient utilization of the former period, no reasonable planning is available, the consumption of fossil energy is large, and a series of severe environmental problems such as acid rain, global warming, haze and the like follow. The development of new efficient clean energy is urgently needed, which concerns the living environment of human society and the continuous development in the future, so that a great deal of research is focused on clean energy, wherein the most common daily use is batteries. In the electronic information era, along with the popularization of mobile phones, notebooks and even electric automobiles, the requirements on the energy storage devices of the products are higher and higher, and the lithium ion batteries with high energy density, light weight, cleanness and environmental protection are widely concerned. Lithium ion batteries have been widely used because of their safety, stability and high efficiency. The battery performance mainly depends on the properties of the positive and negative electrode materials, and therefore, an electrode material with higher capacity needs to be developed.
One of the important parts affecting the performance of the lithium ion battery is the negative electrode material, and although the graphite negative electrode material has been developed to date, a mature preparation process and relatively low cost, the requirements of high capacity and good cycle stability of the current negative electrode material of the lithium battery cannot be met, so that researchers still perform a great deal of research work. Among them, metal oxides such as Fe have received a wide attention3O4、Co3O4NiO and SnO2And the like. Among these, SnO2Has the advantages of low price, environmental protection, high specific capacity and the like, thereby being widely researched, SnO2The lithium ion battery anode material is very likely to become a next-generation lithium battery anode material.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides a lithium ion battery C/SnO2The preparation method and the application of the/rGO composite cathode material are characterized in that a solvothermal method is utilized to grow SnO on the surface of rGO in situ2Nanoparticles in SnO2The surface of the nano-particles is coated with a layer of amorphous carbon, thereby improving SnO2Volume expansion of the negative electrode material during cycling and poor electrical conductivity.
The invention provides a lithium ion battery C/SnO2The preparation method of the/rGO composite anode material comprises the following steps:
s1, dissolving tin tetrachloride pentahydrate in ethylene glycol, and stirring and dispersing to obtain a solution A; adding sodium gluconate into the graphene oxide dispersion liquid, and stirring and dispersing to obtain a solution B;
s2, dripping the solution A into the solution B under stirring, and stirring to obtain a black mixed solution;
s3, transferring the black mixed solution into a reaction kettle with a polytetrafluoroethylene lining, heating for reaction, and then cooling to room temperature to obtain black suspension;
s4, centrifuging the black suspension, removing supernatant, ultrasonically washing, and centrifuging to obtain a precipitate;
s5, dissolving the precipitate in absolute ethyl alcohol, performing ultrasonic dispersion and drying to obtain black powder, and grinding to obtain C/SnO2a/rGO nanocomposite.
Preferably, in S1, the weight ratio of tin tetrachloride pentahydrate to graphene oxide is 1: 0.06 to 0.1; preferably, the concentration of the graphene oxide dispersion liquid is 0.5-1 mg/mL.
In the present invention, the graphene oxide dispersion liquid uses water as a solvent.
Preferably, in S1, the molar ratio of stannic chloride pentahydrate to sodium gluconate is 1: 1 to 3.
Preferably, in S3, the temperature is raised to 170-200 ℃ and the reaction is kept for 4-7 h.
Preferably, in S4, the centrifugal speed is 8000-10000 rpm, and the centrifugal time is 8-10 min.
Preferably, in S4, the ultrasonic washing is performed 2-3 times by respectively using deionized water and absolute ethyl alcohol.
Preferably, in S5, the drying temperature is 60-70 ℃.
The invention also provides the lithium ion battery C/SnO prepared by the method2the/rGO composite anode material.
The invention also provides a lithium ion battery, which comprises a positive electrode, a negative electrode and an electrolyte, wherein the negative electrode contains the lithium ion battery C/SnO of claim 82the/rGO composite anode material.
Compared with the prior art, the beneficial effects of the invention are embodied in the following aspects:
1. the method utilizes a solvothermal method to grow SnO on the surface of reduced graphene oxide (rGO) in situ2The nano particles and the added sodium gluconate are used as a chelating agent and a carbon source to enable the prepared SnO2The particles are finer and finally in SnO2The surface of the nano-particles is coated with a layer of amorphous carbon. Prepared SnO2The particles are uniform in size and small in size, are about 7nm, are uniformly distributed on the surface of rGO, are not obviously aggregated, and have no other impurities; the rGO serving as a matrix material has higher conductivity, and also has the advantages of ultrahigh specific surface area, good mechanical property, stable chemical property and the like; nanoscale SnO2The material not only can shorten the diffusion path of lithium ions and improve the conductivity, but also can relieve the strain caused by volume expansion due to small absolute volume change, and the material is uniformly dispersed on the surface of rGO and SnO2The surface is coated with a layer of amorphous carbon, so that SnO can be effectively improved2Volume expansion and poor conductivity of the negative electrode material in the circulation process.
2. C/SnO prepared by the invention2the/rGO composite material has higher reversible capacity, good rate capability and cycle stability; the lithium ion battery prepared by adopting the composite material firstly passes through a reactor with the current density of 100mA g-1After five cycles of activation, 1A g-1The capacity reaches 700mA g after 100 cycles under the current density of (1)-1The above.
3. The raw materials used in the invention have low price, the preparation method is simple, and the prepared productThe composite material can simultaneously have SnO2High capacity and high conductivity of graphene, better stability compared to single material and SnO attached to the surface of graphene2Intermolecular forces among the graphene can be reduced after the particles are granulated, so that aggregation of the graphene is inhibited, and better structural stability and cycling stability are obtained.
Drawings
FIG. 1 is a schematic representation of C/SnO prepared in accordance with example 2 of the present invention2TEM image of/rGO composite anode material;
FIG. 2 is a schematic representation of C/SnO prepared in examples 1-3 of the present invention2XRD pattern of/rGO composite cathode material;
FIG. 3 is a schematic representation of C/SnO prepared in examples 1-3 of the present invention2Cycle performance diagram of/rGO composite anode material.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
C/SnO of lithium ion battery2The preparation method of the/rGO composite anode material comprises the following steps:
s1, adding 0.9mmol SnCl4·5H2Dissolving O (0.3155g) in 30ml of ethylene glycol, and magnetically stirring for 30min to obtain a solution A; ultrasonically dispersing the GO solution (30ml, 0.833mg/ml) for 30min, adding 0.9mmol of sodium gluconate, and magnetically stirring for 30min to obtain a solution B;
s2, quickly dropping the solution A into the solution B under stirring, and continuously stirring for 60min to obtain a black mixed solution;
s3, transferring the black mixed solution into a 100ml stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in a forced air drying oven, preserving the heat for 6 hours at 180 ℃, and naturally cooling to room temperature to obtain black suspension;
s4, centrifuging the black suspension liquid for 10min at the rotating speed of 9000rpm respectively, removing supernatant, adding 20ml of deionized water, ultrasonically washing for 10min at the power of 50W, centrifuging again, removing supernatant, washing for 3 times with deionized water under the condition, wherein the supernatant is colorless and transparent after centrifuging, then washing for 3 times with absolute ethyl alcohol, 20ml each time, and the supernatant is colorless and transparent for the last time;
s5, adding 10ml of absolute ethyl alcohol into the centrifugal precipitates respectively, carrying out ultrasonic treatment for 10min under the power of 50W, putting the centrifugal precipitates into a 60-DEG C forced air drying oven, keeping the temperature for 1h to remove the ethyl alcohol to obtain black powder, and grinding the black powder in an agate mortar for 15min to obtain a composite material, wherein the composite material is marked as C/SnO2/rGO-1。
Example 2
C/SnO of lithium ion battery2Compared with the preparation method of the/rGO composite anode material in the embodiment 1, the difference is only that the using amount of sodium gluconate in S1 is 1.8 mmol; the composite obtained is designated C/SnO2/rGO-2。
Example 3
C/SnO of lithium ion battery2Compared with the preparation method of the/rGO composite anode material in the embodiment 1, the difference is only that the using amount of sodium gluconate in S1 is 2.7 mmol; the composite obtained is designated C/SnO2/rGO-3。
Example 4
C/SnO of lithium ion battery2The preparation method of the/rGO composite anode material comprises the following steps:
s1, adding 0.9mmol SnCl4·5H2Dissolving O (0.3155g) in 30ml of ethylene glycol, and magnetically stirring for 30min to obtain a solution A; ultrasonically dispersing the GO solution (40ml, 0.5mg/ml) for 30min, adding 1.5mmol of sodium gluconate, and magnetically stirring for 30min to obtain a solution B;
s2, quickly dropping the solution A into the solution B under stirring, and continuously stirring for 60min to obtain a black mixed solution;
s3, transferring the black mixed solution into a 100ml stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in a forced air drying oven, preserving the heat for 7 hours at 170 ℃, and naturally cooling to room temperature to obtain black suspension;
s4, centrifuging the black suspension liquid for 10min at the rotating speed of 8000rpm respectively, removing supernatant, adding 20ml of deionized water, ultrasonically washing for 10min at the power of 50W, centrifuging again, removing supernatant, washing for 3 times by using the deionized water under the condition, wherein the supernatant is colorless and transparent after centrifuging, then washing for 3 times by using absolute ethyl alcohol, wherein each time is 20ml, and the supernatant is colorless and transparent for the last time;
s5, adding 10ml of absolute ethyl alcohol into the centrifugal precipitates respectively, carrying out ultrasonic treatment for 10min under the power of 50W, putting the centrifugal precipitates into a 60-DEG C forced air drying oven, keeping the temperature for 1h to remove the ethyl alcohol to obtain black powder, and grinding the black powder in an agate mortar for 15min to obtain the composite material C/SnO2/rGO。
Example 5
C/SnO of lithium ion battery2The preparation method of the/rGO composite anode material comprises the following steps:
s1, adding 0.9mmol SnCl4·5H2Dissolving O (0.3155g) in 30ml of ethylene glycol, and magnetically stirring for 30min to obtain a solution A; ultrasonically dispersing a GO solution (30ml, 1mg/ml) for 30min, adding 2.0mmol of sodium gluconate, and magnetically stirring for 30min to obtain a solution B;
s2, quickly dropping the solution A into the solution B under stirring, and continuously stirring for 60min to obtain a black mixed solution;
s3, transferring the black mixed solution into a 100ml stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in a forced air drying oven, preserving the heat for 4 hours at 200 ℃, and naturally cooling to room temperature to obtain black suspension;
s4, centrifuging the black suspension liquid for 8min at 10000rpm respectively, removing supernatant, adding 20ml of deionized water, ultrasonically washing for 10min at 50W power, centrifuging again, removing supernatant, washing for 3 times with deionized water under the condition, wherein the supernatant is colorless and transparent after centrifuging, then washing for 3 times with absolute ethyl alcohol, each time 20ml, and finally, the supernatant is colorless and transparent;
s5, adding 10ml of absolute ethyl alcohol into the centrifugal precipitates respectively, carrying out ultrasonic treatment for 10min under the power of 50W, putting the centrifugal precipitates into a 70 ℃ forced air drying oven for heat preservation for 1h to remove the ethyl alcohol to obtain black powder, and grinding the black powder in an agate mortar for 15min to obtain the composite material C/SnO2/rGO。
Comparative example
SnO of lithium ion battery2Preparation method of/rGO composite anode materialCompared with example 1, the difference is only that S1 is different:
s1, adding 0.9mmol SnCl4·5H2Dissolving O (0.3155g) in 30ml of ethylene glycol, and magnetically stirring for 30min to obtain a solution A; carrying out ultrasonic dispersion on the GO solution (30ml, 0.833mg/ml) for 30min to obtain a solution B;
the composite obtained is designated SnO2/rGO。
The composite materials prepared in the examples of the present invention and the comparative examples were subjected to characterization and performance test.
FIG. 1 is a C/SnO solution prepared in example 22TEM images of/rGO composite anode material, and images (a) - (f) are TEM images of the composite material at different positions and magnifications respectively. As can be seen from the figure, in SnO2Some amorphous carbon is present around the grains. Nano SnO2The change in absolute volume of the crystal particles during cycling is also relatively small. A large number of oxygen-containing functional groups on the surface of graphene oxide are used as nucleation sites in the initial reaction stage, and gluconic acid radicals are adsorbed on Sn due to electrostatic action4+Form C/SnO after carbonization under solvothermal conditions2Composite structure of/rGO. rGO is used as a matrix material and plays a role in relieving SnO2The effect of grain volume expansion and rGO has good electrical conductivity. SnO2Amorphous carbon around grain surface in SnO2Plays a role of buffering in the process of cyclic charge and discharge, and prevents the nano SnO2The aggregate grows up and the conductivity of the cathode material can be improved.
FIG. 2 shows composite SnO2/rGO、C/SnO2/rGO-1、C/SnO2rGO-2 and C/SnO2XRD diffractogram of/rGO-3. SnO of rutile structure2The standard diffraction peak patterns (JCPDS41-1445) are in one-to-one correspondence, and no other impurity peaks appear, which indicates that the solvothermal method is used for preparing a pure phase of SnO 2. The diffraction peak widths of these four samples are seen to be large, indicating that the grains of SnO2 are relatively fine.
FIG. 3 is composite SnO2/rGO、C/SnO2/rGO-1、C/SnO2rGO-2 and C/SnO2First pass current density of 100mAg for rGO-3-1After five cycles of activation, 1A is addedg-1At a current density of 600mAh g after 100 cycles-1、744mAh g-1、803mAh g-1And 716mAh g-1The capacity of (a); C/SnO in examples 1-32The capacity of the/rGO composite material is obviously higher than that of SnO in a comparative example2a/rGO composite material.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. C/SnO of lithium ion battery2The preparation method of the/rGO composite anode material is characterized by comprising the following steps:
s1, dissolving tin tetrachloride pentahydrate in ethylene glycol, and stirring and dispersing to obtain a solution A; adding sodium gluconate into the graphene oxide dispersion liquid, and stirring and dispersing to obtain a solution B;
s2, dripping the solution A into the solution B under stirring, and stirring to obtain a black mixed solution;
s3, transferring the black mixed solution into a reaction kettle with a polytetrafluoroethylene lining, heating for reaction, and then cooling to room temperature to obtain black suspension;
s4, centrifuging the black suspension, removing supernatant, washing and centrifuging to obtain a precipitate;
s5, dissolving the precipitate in absolute ethyl alcohol, performing ultrasonic dispersion and drying to obtain black powder, and grinding to obtain C/SnO2a/rGO nanocomposite.
2. The lithium ion battery C/SnO of claim 12The preparation method of the/rGO composite anode material is characterized in that in S1, the weight ratio of tin tetrachloride pentahydrate to graphene oxide is 1: 0.06 to 0.1; preferably, the concentration of the graphene oxide dispersion liquid is 0.5-1 mg/mL.
3. Root of herbaceous plantThe lithium ion battery C/SnO of claim 1 or 22The preparation method of the/rGO composite anode material is characterized in that in S1, the molar ratio of stannic chloride pentahydrate to sodium gluconate is 1: 1 to 3.
4. A lithium ion battery C/SnO according to any of claims 1 to 32The preparation method of the/rGO composite anode material is characterized in that in S3, the temperature is raised to 170-200 ℃ and the reaction is carried out for 4-7 hours in a heat preservation manner.
5. The lithium ion battery C/SnO according to any of claims 1-42The preparation method of the/rGO composite anode material is characterized in that in S4, the centrifugal rotating speed is 8000-10000 rpm, and the centrifugal time is 8-10 min.
6. The lithium ion battery C/SnO according to any of claims 1-52The preparation method of the/rGO composite anode material is characterized in that in S4, washing is carried out for 2-3 times by respectively adopting deionized water and absolute ethyl alcohol.
7. The lithium ion battery C/SnO of any of claims 1-62The preparation method of the/rGO composite anode material is characterized in that in S5, the drying temperature is 60-70 ℃.
8. A lithium ion battery C/SnO prepared by the method of any one of claims 1-72the/rGO composite anode material.
9. A lithium ion battery comprising a positive electrode, a negative electrode and an electrolyte, wherein the negative electrode comprises the lithium ion battery C/SnO of claim 82the/rGO composite anode material.
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| CN113991084A (en) * | 2021-10-27 | 2022-01-28 | 西安建筑科技大学 | SnS-SnO2-GO @ C heterostructure composite material and preparation method and application thereof |
| CN114094062A (en) * | 2021-10-09 | 2022-02-25 | 温州大学 | Preparation method and application of oxalic acid assisted synthesis of tin dioxide nanoparticle composite graphene high-performance lithium storage and sodium storage material |
| CN114639799A (en) * | 2022-03-28 | 2022-06-17 | 广东技术师范大学 | Composite electrode for all-solid-state metal lithium battery and preparation method thereof |
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| CN114639799A (en) * | 2022-03-28 | 2022-06-17 | 广东技术师范大学 | Composite electrode for all-solid-state metal lithium battery and preparation method thereof |
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