CN110649258B - Preparation method of three-dimensional porous tin oxide graphene composite electrode material - Google Patents

Preparation method of three-dimensional porous tin oxide graphene composite electrode material Download PDF

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CN110649258B
CN110649258B CN201910949893.7A CN201910949893A CN110649258B CN 110649258 B CN110649258 B CN 110649258B CN 201910949893 A CN201910949893 A CN 201910949893A CN 110649258 B CN110649258 B CN 110649258B
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郭林
赵赫威
曾小龙
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Abstract

The preparation method of the three-dimensional porous tin oxide graphene composite electrode material is simple and convenient, and the three-dimensional porous tin oxide graphene composite electrode material can be prepared. The method comprises the following specific steps: (1) preparing a buffer solution with a target pH value at room temperature, adding a proper amount of tin tetrachloride pentahydrate and graphene oxide, and violently stirring until the mixture is uniformly dispersed to form a yellow transparent solution; (2) heating the mixed solution to 60-80 ℃, reacting for 2-6h under the condition of stirring, naturally cooling, and centrifugally washing to obtain brown yellow/black precipitate; (3) transferring 20-40mg of the obtained brown yellow/black precipitate into a 5-20mL polytetrafluoroethylene reaction kettle, adding pure water, stirring, performing ultrasonic treatment, reacting at 180 ℃ for 24-48h to obtain a black gel sample, transferring the black gel sample into a freeze dryer, and drying for 24-48h to obtain a dry black block; (3) and transferring the dried black blocks into a tubular furnace, and calcining for 4-6h at 650 ℃ in an argon protection environment to obtain the three-dimensional porous tin oxide graphene composite electrode material.

Description

Preparation method of three-dimensional porous tin oxide graphene composite electrode material
Technical Field
The invention relates to the technical field of new energy, and particularly relates to a preparation method of a three-dimensional porous tin oxide graphene composite electrode material.
Background
With the rapid development of economy and technology, people must also face the global energy crisis and serious environmental pollution problems caused by their rapid development while enjoying the convenience they bring. The search for new clean, efficient and sustainable energy is one of the most important challenges facing people today. Rechargeable secondary batteries have recently attracted considerable attention as a "carrier" for bringing energy to practical use in human life.
At present, the rechargeable lithium ion battery has the advantages of high voltage, large specific energy, good safety performance, long cycle life, rapid charge and discharge and the like, and is widely researched. The rechargeable lithium ion battery has high working voltage and energy density, and long service life, and is widely applied to daily life and scientific research. The electrochemical performance of rechargeable lithium ion batteries depends on their electrode materials. Although graphite has been used as an electrode material for commercial rechargeable lithium ion batteries, its theoretical specific capacity (392 mAh g)-1) Low, hinder high energyThe development of mass density rechargeable lithium ion batteries. In order to realize high-performance rechargeable lithium ion batteries, new electrode materials need to be explored and new electrode structures need to be designed.
Tin dioxide (SnO)2) Due to the theoretical specific capacity (about 782mA h)-1) High, low lithium insertion potential, low cost, has proven to be a promising anode for rechargeable lithium ion batteries. However, SnO with slow lithium ion transport and severe volume expansion (over 300%) during lithium intercalation and deintercalation2The stability and rate performance of the rechargeable lithium ion battery may be greatly reduced. Synthesis of nano-SnO in various types of carbon matrices2Is a method for improving the cycle performance, because the carbon matrix can ensure the active material SnO in the cycle process2Confined within a closed volume so that capacity loss due to crushing can be minimized and there is good electrical contact with the battery; morphological design is another approach to improve cycling stability, where complex nanostructures have been synthesized, such as hollow spheres, nanowires, polyhedra and layered structures, which can better sustain volume expansion during charge and discharge. However, when SnO is used2Achieving high rate performance of rechargeable lithium ion batteries at their excellent cycling performance remains a significant challenge when used as anodes.
Disclosure of Invention
The invention aims to provide a preparation method of a green and environment-friendly three-dimensional porous tin oxide graphene composite electrode material, which is simple to operate and aims to overcome the defects in the prior art by using a simple liquid phase reaction method and using metal salts, buffer solutions and the like which are conveniently obtained as raw materials. Which comprises the following steps:
firstly, preparing 50mL of glycine/hydrochloric acid standard buffer solution with the pH value of 2.0-2.6, adding 5-10mg of graphene oxide and 0.25-0.5mmol of stannic chloride pentahydrate, stirring at room temperature for 10-30min, and performing ultrasonic treatment for 10-30min to obtain a brown yellow transparent solution;
secondly, heating the brown yellow transparent solution obtained in the first step to 60-80 ℃, continuously stirring for 2-6h, cooling the solution to room temperature, and centrifugally washing to obtain brown yellow/black precipitate, namely the two-dimensional tin oxide/graphene oxide composite nanosheet;
step three, transferring 20-40mg of the brown yellow/black precipitate obtained in the step two into a 5-20mL reaction kettle containing polytetrafluoroethylene, adding 3-18mL pure water, and stirring at room temperature for 10-30min to obtain a dark yellow liquid;
fourthly, transferring the polytetrafluoroethylene reaction kettle filled with the sample in the third step into an ultrasonic machine, and carrying out ultrasonic treatment for 30-60min to fully disperse the polytetrafluoroethylene reaction kettle, wherein the temperature is controlled not to exceed 50 ℃ in the ultrasonic treatment process;
fifthly, transferring the reaction kettle in the fourth step into an oven, and reacting for 24-48h at 180 ℃ to obtain a black gel sample;
sixthly, transferring the black gel-like sample obtained in the fifth step into a freeze dryer, and drying for 24-48h to obtain a dry black block;
and seventhly, transferring the dried black block obtained in the sixth step into a tube furnace, and calcining for 4-6 hours at 650 ℃ in an argon protection environment to obtain the three-dimensional porous tin oxide graphene composite electrode material.
In the present invention, the solutions used are prepared under conventional conditions, such as by dissolving the substances in an aqueous solution at room temperature, unless otherwise specified.
In the present invention, if not specifically stated, the employed apparatuses, instruments, devices, materials, processes, methods, steps, preparation conditions, etc. are those conventionally employed in the art or can be easily obtained by those of ordinary skill in the art according to the techniques conventionally employed in the art.
In the present invention, the buffer solution is an alcohol/water system, preferably a glycine-hydrochloric acid system, wherein the alcohol/water system is a glycol and water system, and the volume ratio of the glycol to the water is 7:1 to 9:1, preferably 8.4:1.6, but not limited thereto.
In the present invention, the graphene oxide is mainly synthesized by Hummers method, and the preparation method can be referred to j.am.chem.soc.,1958,80,1339, and the thickness of the graphene oxide is 1nm or less, but not limited thereto.
The room temperature means a temperature range of 20 ℃ to 35 ℃.
Furthermore, the size of the prepared two-dimensional tin oxide/graphene nanosheet is 1-20 microns, and the thickness is 3-7 nm.
Furthermore, the prepared three-dimensional porous tin oxide graphene composite electrode material has a good porous structure, and the size of the material can be regulated.
Further, the pH of the glycine-hydrochloric acid buffer solution (alcohol-water system) is in the range of 1.6 to 3.2, preferably 2.0 to 2.6.
Further, the stirring time in the first step, the second step and the third step is 10-30 min; the ultrasonic time in the first step is 10-30 min; the ultrasonic time in the fourth step is 30-60 min; the heating temperature in the second step is preferably 60-80 ℃, and the stirring time is 2-6 h.
Further, the ultrasonic temperature in the fourth step cannot exceed 50 ℃.
Further, the mass concentration range of the graphene oxide in the solution in the first step is preferably 0.1-1.5g/L, and the molar concentration range of the stannic chloride pentahydrate in the solution in the first step is preferably 5-10 mmol/L. If the molar concentration of the metal salt is lower than 5mmol/L, oxide particles adsorbed on the surface of the graphene oxide can be generated; if the molar concentration of the metal salt is higher than 10mmol/L, oxide particles existing alone may be generated, which may affect the preparation of the ultra-thin material.
Furthermore, the three-dimensional porous tin oxide graphene composite electrode material prepared by the method has good electrochemical performance, and the capacity of the battery after the battery is circulated for 5000 circles and has the capacity of 450-600mAh g under the current density of 10A/g by taking the three-dimensional porous tin oxide graphene composite electrode material as the anode of the lithium ion battery-1。
Compared with the existing preparation of the ultrathin two-dimensional nano material, the preparation method has the following advantages:
the raw materials adopted in the preparation process are simple and easy to obtain, the cost is lower, no pollution is caused to the environment, the process is simple, and the operation is simple and convenient;
2, the three-dimensional porous tin oxide graphene composite electrode material prepared by the method has the characteristics of controllable tin oxide loading amount, uniform appearance, excellent electrochemical performance and the like;
drawings
FIG. 1 is a scanning electron microscope photograph and a transmission electron microscope photograph of the ultra-thin tin oxide two-dimensional nanomaterial obtained in example 1 of the present invention;
FIG. 2 is a schematic view of a polytetrafluoroethylene reactor used in the present invention;
fig. 3 is a scanning electron microscope photograph of the three-dimensional porous tin oxide graphene composite electrode material obtained in example 1 of the present invention;
fig. 4 is an electrochemical test result of the three-dimensional porous tin oxide graphene composite electrode material obtained in example 1 of the present invention.
Detailed Description
The following describes the preparation method of the ultra-thin two-dimensional nanomaterial in detail with reference to the accompanying drawings and examples. It should be understood that these examples are only illustrative of the present invention and do not limit the scope of the present invention in any way.
Example 1
Preparation method of low-tin dioxide load three-dimensional porous tin oxide graphene composite electrode material
Firstly, 0.188g of glycine and 183uL of concentrated HCl are taken and added into a mixed solution of 8ml of deionized water and 42ml of ethylene glycol at room temperature to prepare a glycine-ammonium hydrochloride standard buffer solution (alcohol-water system) with the pH value of 2.2, and the mixture is stirred for 15min and subjected to ultrasonic treatment for 10min to obtain 50ml of uniformly mixed colorless transparent solution;
secondly, adding 5mg of graphene oxide into the solution obtained in the first step, and stirring for 15min at room temperature to obtain a brown yellow transparent solution;
thirdly, 0.25mmol of stannic chloride pentahydrate is added into the brown yellow transparent solution obtained in the second step, and the mixture is stirred for 15min at room temperature to obtain a brown yellow transparent solution;
fourthly, heating the brown yellow transparent solution obtained in the third step to 70 ℃, continuously stirring for 4 hours, cooling the solution to room temperature, and centrifugally washing to obtain brown yellow precipitate, namely the two-dimensional tin oxide/graphene oxide composite nanosheet (shown in figure 1);
fifthly, transferring 30mg of the brown yellow precipitate obtained in the fourth step into a 8mL polytetrafluoroethylene reaction kettle (shown in figure 2), performing ultrasonic treatment at room temperature for 1h, and reacting in an oven at 180 ℃ for 24h to obtain a black gel sample;
sixthly, transferring the black gelatinous sample obtained in the fifth step into a freeze dryer, and drying for 24 hours to obtain a dry black block;
seventhly, transferring the dried black block obtained in the sixth step into a tube furnace, calcining for 6 hours at 650 ℃ in an argon environment to obtain a black three-dimensional porous tin oxide graphene composite electrode material (figure 3), wherein the three-dimensional porous tin oxide graphene composite electrode material prepared by the method has good electrochemical performance, is used as an anode of a lithium ion battery, and has the capacity of 600mAh g and 450-doped mAh g after the battery is cycled for 5000 circles under the current density of 10A/g-1(FIG. 4).
Example 2
Preparation method of medium-tin dioxide-loaded three-dimensional porous tin oxide graphene composite electrode material
Firstly, 0.188g of glycine and 183uL of concentrated HCl are taken and added into a mixed solution of 8ml of deionized water and 42ml of ethylene glycol at room temperature to prepare a glycine-ammonium hydrochloride standard buffer solution (alcohol-water system) with the pH value of 2.2, and the mixture is stirred for 15min and subjected to ultrasonic treatment for 10min to obtain 50ml of uniformly mixed colorless transparent solution;
secondly, adding 5mg of graphene oxide into the solution obtained in the first step, and stirring for 15min at room temperature to obtain a brown yellow transparent solution;
thirdly, 0.375mmol of stannic chloride pentahydrate is added into the brown yellow transparent solution obtained in the second step, and stirred for 15min at room temperature to obtain a brown yellow transparent solution;
fourthly, heating the brown yellow transparent solution obtained in the third step to 70 ℃, continuously stirring for 4 hours, cooling the solution to room temperature, and centrifugally washing to obtain brown yellow precipitate, namely the two-dimensional tin oxide/graphene oxide composite nanosheet;
fifthly, transferring 30mg of the brown yellow precipitate obtained in the fourth step into a 8mL polytetrafluoroethylene reaction kettle, performing ultrasonic treatment for 1h at room temperature, and reacting in an oven at 180 ℃ for 24h to obtain a black gel sample;
sixthly, transferring the black gelatinous sample obtained in the fifth step into a freeze dryer, and drying for 24 hours to obtain a dry black block;
and seventhly, transferring the dried black block obtained in the sixth step into a tube furnace, and calcining for 6 hours at 650 ℃ in an argon environment to obtain the black three-dimensional porous tin oxide graphene composite electrode material.
Example 3
Preparation method of high-tin dioxide-loading-capacity three-dimensional porous tin oxide graphene composite electrode material
Firstly, 0.188g of glycine and 183uL of concentrated HCl are taken and added into a mixed solution of 8ml of deionized water and 42ml of ethylene glycol at room temperature to prepare a glycine-ammonium hydrochloride standard buffer solution (alcohol-water system) with the pH value of 2.2, and the mixture is stirred for 15min and subjected to ultrasonic treatment for 10min to obtain 50ml of uniformly mixed colorless transparent solution;
secondly, adding 5mg of graphene oxide into the solution obtained in the first step, and stirring for 15min at room temperature to obtain a brown yellow transparent solution;
thirdly, 0.5mmol of stannic chloride pentahydrate is added into the brown yellow transparent solution obtained in the second step, and the mixture is stirred for 15min at room temperature to obtain a brown yellow transparent solution;
fourthly, heating the brown yellow transparent solution obtained in the third step to 70 ℃, continuously stirring for 6 hours, cooling the solution to room temperature, and centrifugally washing to obtain brown yellow precipitate, namely the two-dimensional tin oxide/graphene oxide composite nanosheet;
fifthly, transferring 30mg of the brown yellow precipitate obtained in the fourth step into a 8mL polytetrafluoroethylene reaction kettle, performing ultrasonic treatment for 1h at room temperature, and reacting in an oven at 180 ℃ for 48h to obtain a black gel sample;
sixthly, transferring the black gelatinous sample obtained in the fifth step into a freeze dryer, and drying for 48 hours to obtain a dry black block;
and seventhly, transferring the dried black block obtained in the sixth step into a tube furnace, and calcining for 6 hours at 650 ℃ in an argon environment to obtain the black three-dimensional porous tin oxide graphene composite electrode material.

Claims (7)

1. A preparation method of a three-dimensional porous tin oxide graphene composite electrode material is characterized by comprising the following steps:
firstly, preparing 50mL of glycine/hydrochloric acid standard buffer solution with the pH value of 2.0-2.6, adding 5-10mg of graphene oxide and 0.25-0.5mmol of stannic chloride pentahydrate, stirring at room temperature for 10-30min, and performing ultrasonic treatment for 10-30min to obtain a brown yellow transparent solution; the standard buffer solution is an alcohol/water system; the molar concentration range of the stannic chloride pentahydrate in the solution is 5-10 mmol/L;
secondly, heating the brown yellow transparent solution obtained in the first step to 60-80 ℃, continuously stirring for 2-6h, cooling the solution to room temperature, and centrifugally washing to obtain brown yellow/black precipitate, namely the two-dimensional tin oxide/graphene oxide composite nanosheet;
step three, transferring 20-40mg of the brown yellow/black precipitate obtained in the step two into a 5-20mL reaction kettle containing polytetrafluoroethylene, adding 3-18mL pure water, and stirring at room temperature for 10-30min to obtain a dark yellow liquid;
fourthly, transferring the polytetrafluoroethylene reaction kettle filled with the sample in the third step into an ultrasonic machine, and carrying out ultrasonic treatment for 30-60min to fully disperse the polytetrafluoroethylene reaction kettle, wherein the temperature is controlled not to exceed 50 ℃ in the ultrasonic treatment process;
fifthly, transferring the reaction kettle in the fourth step into an oven, and reacting for 24-48h at 180 ℃ to obtain a black gel sample;
sixthly, transferring the black gel-like sample obtained in the fifth step into a freeze dryer, and drying for 24-48h to obtain a dry black block;
and seventhly, transferring the dried black block obtained in the sixth step into a tube furnace, and calcining for 4-6 hours at 650 ℃ in an argon protection environment to obtain the three-dimensional porous tin oxide graphene composite electrode material.
2. The preparation method of the three-dimensional porous tin oxide graphene composite electrode material according to claim 1, characterized in that: in the alcohol/water system, the alcohol is ethylene glycol.
3. The preparation method of the three-dimensional porous tin oxide graphene composite electrode material according to claim 1, characterized in that: the pH of the alcohol/water system was 2.2.
4. The preparation method of the three-dimensional porous tin oxide graphene composite electrode material according to claim 1, characterized in that: the thickness of the graphene oxide is less than 1 nm.
5. The preparation method of the three-dimensional porous tin oxide graphene composite electrode material according to claim 1, characterized in that: the size of the prepared two-dimensional tin oxide/graphene oxide nanosheet is 1-20 microns, and the thickness is 3-7 nm.
6. The preparation method of the three-dimensional porous tin oxide graphene composite electrode material according to claim 1, characterized in that: the mass concentration range of the graphene oxide in the solution is 0.1-1.5 g/L.
7. The method for preparing the three-dimensional porous tin oxide graphene composite electrode material as claimed in claim 1, wherein the three-dimensional porous tin oxide graphene composite electrode material is used as an anode of a lithium ion battery, and the battery capacity after 5000 cycles of circulation has 450-600mAh g under the current density of 10A/g-1。
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