CN107706404B - Preparation and application of selenium-coated tin dioxide/graphene nanocomposite - Google Patents
Preparation and application of selenium-coated tin dioxide/graphene nanocomposite Download PDFInfo
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- CN107706404B CN107706404B CN201711178146.5A CN201711178146A CN107706404B CN 107706404 B CN107706404 B CN 107706404B CN 201711178146 A CN201711178146 A CN 201711178146A CN 107706404 B CN107706404 B CN 107706404B
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- H—ELECTRICITY
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Abstract
The invention discloses a selenium-coated tin dioxide/graphene nano composite material and application thereof in a sodium ion battery cathode material. The selenium-coated tin dioxide/graphene nano composite material is characterized in that: 1) SnO with two different crystal phases2(i.e., tetragonal SnO2And orthorhombic SnO2) Growing closely together to form nano-scale particles; 2) the formed nano-particles are uniformly combined on the surface of the three-dimensional conductive graphene; 3) disordered selenium is uniformly coated on the surface of the stannic oxide/graphene nano structure. The selenium-coated tin dioxide/graphene nano composite material provided by the invention is simple in preparation method, cheap in raw materials, uniform in appearance, and capable of being prepared in a large scale, and shows excellent sodium storage performance when being used as a sodium ion battery cathode material.
Description
Technical Field
The invention belongs to the technical field of nano materials and sodium ion secondary batteries, and particularly relates to a selenium-coated tin dioxide/graphene nano composite material and application thereof.
Background
Energy and environment have been the focus of attention all over the world. In recent years, along with the increasing consumption of non-renewable energy and the gradual increase of environmental pollution problems, the demand for clean energy is also increasing. Because the storage capacity of lithium resources in the world is very largeLimited, lithium ion batteries alone are difficult to meet the stringent requirements for future energy storage. Therefore, the development of next-generation high-performance energy storage power sources capable of replacing lithium ion batteries is not slow. Sodium is an active metal element in the same main group as lithium and has similar physical and chemical properties, and as such, sodium ion batteries have similar energy storage mechanisms as lithium ion batteries. Meanwhile, the sodium element is very abundant in the earth crust, and thus has received much attention. However, the radius of sodium ions is larger than that of lithium ions, so that the commercialized high-performance lithium battery negative electrode cannot be directly used for a sodium ion battery, and a sodium ion battery negative electrode material which can be mass-produced and commercialized does not exist at present, so that it is urgent to develop a cheap and commercialized sodium ion battery negative electrode material. Transition metal oxides, e.g. tin dioxide (SnO)2) Has received much attention due to its high theoretical specific capacity and its low cost. But it faces the problem of more serious capacity attenuation, mainly because the structure of the material expands and contracts correspondingly with the intercalation and deintercalation of sodium ions in the circulation process, thereby leading to the pulverization of electrodes and the loss of electric contact, and causing the serious attenuation of the material circulation performance. Here, we prepared a new class of selenium-coated tin dioxide/graphene nanocomposite through a simple scheme, which shows excellent rate and cycle performance as a sodium ion battery anode material. This is the material with the best cycling performance among the reported tin dioxide based sodium ion battery anode materials.
Disclosure of Invention
The invention aims to solve the problem of SnO2The selenium-coated tin dioxide/graphene nano composite material has the advantages of high specific capacity and good cycling stability.
The selenium-coated stannic oxide/graphene nano composite material is prepared from selenium and two types of stannic oxide (tetragonal system SnO)2And orthorhombic SnO2) And graphene. The method is characterized in that: 1) SnO with two different crystal phases2(i.e., tetragonal SnO2And orthorhombic SnO2) Tighten upGrowing closely together to form nano-scale particles; 2) the formed nano-particles are uniformly combined on the surface of the three-dimensional conductive graphene; 3) disordered selenium is uniformly coated on the surface of the stannic oxide/graphene nano structure.
The preparation method of the selenium-coated tin dioxide/graphene nano composite material comprises the following steps:
1) adding 2.48 gL-tartaric acid into 50mL of deionized water, then adding 295 mu L of anhydrous stannic chloride into the solution, adding 150mg of graphene oxide aqueous solution under strong stirring, and diluting to 300 mL;
2) dropping 50mL of 0.1-0.8mg mL of the suspension into the suspension under continuous stirring-1Performing ultrasonic treatment on the sodium borohydride solution for 3-7h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn;
3) uniformly mixing the selenium powder and the intermediate product of Sn, heating to the temperature of 300 ℃ and 700 ℃, and calcining for 3-8 h; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
The concentration of the graphene oxide aqueous solution in the step 1) is 2-5mg mL-1(ii) a Preferably, the concentration of the graphene oxide aqueous solution is 3.5mg mL-1；
The concentration of the sodium borohydride solution in the step 2) is 0.1-0.8mg mL-1(ii) a Preferably, the concentration of the sodium borohydride solution is 0.3-0.5mg mL-1The ultrasonic time is 4-6 h.
The mass ratio in the step 3) is 1-4: 1; preferably, the mass ratio is 2 to 31.
The calcination temperature in the step 3) is 300-700 ℃, and the calcination time is 3-8 h; preferably, the calcination temperature is 400-600 ℃; calcining for 4-5 h;
the selenium-coated tin dioxide/graphene nano composite material is applied to the preparation of a sodium ion battery electrode material.
The invention provides a selenium-coated tin dioxide/graphene nano composite material, which consists of coated selenium, two types of tin dioxide and graphene. The method is characterized in that: the two different crystalline phases of stannic oxide are grown together tightly to form nano-scale particles, the particles are uniformly combined on the surface of the three-dimensional conductive graphene, and disordered selenium is uniformly coated on the surface of the integral structure. The selenium-coated tin dioxide/graphene nanocomposite material provided by the invention is simple in preparation method, cheap in raw materials, uniform in appearance and capable of being prepared in a large scale; the composite material has excellent sodium storage performance when being used as a sodium ion battery cathode material, and is a sodium ion battery cathode material with very promising application due to the synergistic effect of two tin dioxide heterostructures in the composite material and a graphene three-dimensional conductive network, which is benefited by the selenium coating layer.
Drawings
FIG. 1 powder pattern X-ray diffraction test pattern of selenium-coated tin dioxide/graphene nanocomposite material of example 2;
fig. 2 raman plot of selenium-coated tin dioxide/graphene nanocomposite in example 2;
FIG. 3 scanning electron micrograph of selenium-coated tin dioxide/graphene nanocomposite of example 2;
fig. 4 a transmission electron microscope photograph, (b) a high resolution transmission electron microscope photograph and (c) a transmission electron microscope elemental distribution photograph of the selenium-coated tin dioxide/graphene nanocomposite material of example 2;
fig. 5 is a comparison of the rate capability of the selenium-coated tin dioxide/graphene nanocomposite material and the tin dioxide/graphene nanocomposite material when used as the negative electrode material of a sodium ion battery in example 2;
fig. 6 shows the cycling performance of the selenium-coated tin dioxide/graphene nanocomposite material of example 2 as a sodium ion battery negative electrode material at different current densities.
Detailed Description
Example 1 preparation of selenium-coated tin dioxide/graphene nanocomposite
2.48g L-tartaric acid was added to 50mL of deionized water, and then 295 μ L of anhydrous tin tetrachloride was added to the solution, and 150mg of an aqueous graphene oxide solution (3.5mg mL) was added under vigorous stirring-1) Diluting to 300 mL; 50mL of 0.1m are added dropwise to the suspension under continuous stirringg mL-1 sodium borohydride solution, performing ultrasonic treatment for 3-6h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn; uniformly mixing selenium powder and an intermediate product of Sn according to a mass ratio of 2.5:1, heating to 400 ℃, and calcining for 4 hours; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
Example 2 preparation of selenium-coated tin dioxide/graphene nanocomposite
2.48g L-tartaric acid was added to 50mL of deionized water, and then 295 μ L of anhydrous tin tetrachloride was added to the solution, and 150mg of an aqueous graphene oxide solution (3.5mg mL) was added under vigorous stirring-1) Diluting to 300 mL; while stirring, 50mL of 0.3mg mL was added dropwise to the suspension-1Performing ultrasonic treatment on the sodium borohydride solution for 3-6h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn; uniformly mixing selenium powder and an intermediate product of Sn according to a mass ratio of 2.5:1, heating to 400 ℃, and calcining for 4 hours; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
Example 3 preparation of selenium-coated tin dioxide/graphene nanocomposite
2.48g L-tartaric acid was added to 50mL of deionized water, and then 295 μ L of anhydrous tin tetrachloride was added to the solution, and 150mg of an aqueous graphene oxide solution (2mg mL) was added under vigorous stirring-1) Diluting to 300 mL; while stirring, 50mL of 0.2mg mL was added dropwise to the suspension-1Performing ultrasonic treatment on the sodium borohydride solution for 3-6h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn; and (2) preparing an intermediate product of selenium powder and Sn according to a mass ratio of 2.5:1, uniformly mixing, heating to 400 ℃, and calcining for 4 hours; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
Example 4 preparation of selenium-coated tin dioxide/graphene nanocomposite
2.48g L-tartaric acid was added to 50mL of deionized water, and then 295 μ L of anhydrous tin tetrachloride was added to the solution, and 150mg of an aqueous graphene oxide solution (3.5mg mL) was added under vigorous stirring-1) Diluted to 30 deg.C0 mL; while stirring, 50mL of 0.3mg mL was added dropwise to the suspension-1Performing ultrasonic treatment on the sodium borohydride solution for 3-6h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn; and (2) preparing an intermediate product of selenium powder and Sn according to a mass ratio of 1:
1, uniformly mixing, heating to 500 ℃, and calcining for 5 hours; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
Example 5 preparation of selenium-coated tin dioxide/graphene nanocomposite
2.48g L-tartaric acid was added to 50mL of deionized water, and then 295 μ L of anhydrous tin tetrachloride was added to the solution, and 150mg of an aqueous graphene oxide solution (3.5mg mL) was added under vigorous stirring-1) Diluting to 300 mL; while stirring, 50mL of 0.8mg mL was added dropwise to the suspension-1Performing ultrasonic treatment on the sodium borohydride solution for 3-6h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn; and (2) preparing an intermediate product of selenium powder and Sn according to a mass ratio of 4:
1, uniformly mixing, heating to 700 ℃, and calcining for 8 hours; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
Example 6 preparation of selenium-coated tin dioxide/graphene nanocomposite
2.48g L-tartaric acid was added to 50mL of deionized water, and then 295 μ L of anhydrous tin tetrachloride was added to the solution, and 150mg of an aqueous graphene oxide solution (5mg mL) was added under vigorous stirring-1) Diluting to 300 mL; 50mL of 0.3mgmL was added dropwise to the suspension with constant stirring-1Performing ultrasonic treatment on the sodium borohydride solution for 3-6h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn; and (2) preparing an intermediate product of selenium powder and Sn according to a mass ratio of 1: 1, uniformly mixing, heating to 300 ℃, and calcining for 3 hours; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
Example 7 preparation of selenium-coated tin dioxide/graphene nanocomposite
2.48g L-tartaric acid was added to 50ml of deionized water, and then295 mu L of anhydrous tin tetrachloride is added into the solution, and 150mg of graphene oxide aqueous solution (3.5mg mL) is added under strong stirring-1Diluting to 300 mL; while stirring, 50mL of 0.45mg mL was added dropwise to the suspension-1Performing ultrasonic treatment on the sodium borohydride solution for 3-6h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn; and (2) preparing an intermediate product of selenium powder and Sn according to a mass ratio of 2.5:1, uniformly mixing, heating to 400 ℃, and calcining for 4 hours; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
Example 8 preparation of selenium-coated tin dioxide/graphene nanocomposite
2.48g L-tartaric acid was added to 50ml of deionized water, and then 295 μ L of anhydrous tetrachloro acid was added to the solution
Tin, 150mg of an aqueous graphene oxide solution (3.5mg mL) was added with vigorous stirring-1) Diluting to 300 mL; while stirring, 50mL of 0.2mg mL was added dropwise to the suspension-1Performing ultrasonic treatment on the sodium borohydride solution for 3-6h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn; uniformly mixing selenium powder and an intermediate product of Sn according to a mass ratio of 2.5:1, heating to 400 ℃, and calcining for 4 hours; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
TABLE 1 Performance test results for selenium-coated tin dioxide/graphene nanocomposites
Powder X-ray diffraction (Rigaku DmaxrB, CuK α radiation) test was performed on the selenium-coated tin dioxide/graphene nanocomposite obtained in example 2, and as shown in FIG. 1, the selenium-coated tin dioxide/graphene nanocomposite prepared had two types of tin dioxide (i.e., tetragonal system: t-SnO)2And orthorhombic system o-SnO2) The characteristic peak of selenium is not shown. This suggests that selenium may be present in a disordered form. Further, example 2 raman test detected at 2 via figure 262cm-1The presence of selenium indicates the presence of selenium on the surface of the selenium-coated tin dioxide/graphene nanocomposite. Fig. 3 is a scanning electron microscope picture of the selenium-coated tin dioxide/graphene nanocomposite material of example 2. FIG. 4 is a TEM photograph and TEM element distribution photograph of the Se-coated Sn dioxide/graphene nanocomposite material of example 2, illustrating two SnO types2:(t-SnO2And o-SnO2) Are closely connected to form a heterostructure, while the element Mapping indicates the presence and uniform distribution of the elements tin, selenium, carbon, oxygen. In example 2, the rate and cycle performance of the selenium-coated tin dioxide/graphene nanocomposite material as a sodium ion battery negative electrode material are shown in fig. 5 and 6 (obtained by constant current charge and discharge test), and are 0.05Ag-1The specific capacity of the selenium-coated tin dioxide/graphene nano composite material reaches 660mAh g under the current density of the selenium-coated tin dioxide/graphene nano composite material-1The specific capacity of the tin dioxide/graphene nano composite material is about 4 times of that of the same current density, and the specific capacity is greatly improved. Further, in 5Ag-1After 5000 constant current charge-discharge cycles at the current density, the specific capacity retention rate of the selenium-coated tin dioxide/graphene nanocomposite material is 70%. This is the so far reported SnO-containing2The material with the best cycle performance in the cathode material of the sodium-ion battery. The selenium-coated tin dioxide/graphene nano composite material as the cathode of the sodium ion battery shows excellent multiplying power and cycle performance, and benefits from the synergistic effect of two tin dioxide heterostructures in the composite material and the graphene three-dimensional conductive network. The selenium-coated tin dioxide/graphene nano composite material is a sodium ion battery negative electrode material with very promising application.
Claims (7)
1. A selenium-coated stannic oxide/graphene nano composite material is composed of selenium, two stannic oxides and graphene, wherein the two stannic oxides are tetragonal SnO2And orthorhombic SnO2The method is characterized in that: 1) SnO with two different crystal phases2Grow closely together to form a nano-structureA grade of particles; 2) the formed nano-particles are uniformly combined on the surface of the three-dimensional conductive graphene; 3) disordered selenium is uniformly coated on the surface of the stannic oxide/graphene nano structure.
2. The preparation method of the selenium-coated tin dioxide/graphene nano composite material comprises the following steps:
1) adding 2.48g L-tartaric acid into 50mL of deionized water, then adding 295 mu L of anhydrous stannic chloride into the solution, adding 150mg of graphene oxide aqueous solution under strong stirring, and diluting to 300 mL;
2) under the condition of continuous stirring, 50mL of 0.1-0.8mg mL is added dropwise-1Performing ultrasonic treatment on the sodium borohydride solution for 3-7h, centrifuging, washing with deionized water and absolute ethyl alcohol, and performing vacuum drying at 80 ℃; obtaining an intermediate product of Sn;
3) uniformly mixing the selenium powder and the intermediate product of Sn, heating to the temperature of 300 ℃ and 700 ℃, and calcining for 3-8 h; and obtaining the selenium-coated stannic oxide/graphene nano composite material.
3. The method of preparing the selenium-coated tin dioxide/graphene nanocomposite material of claim 2, wherein: the concentration of the graphene oxide aqueous solution in the step 1) is 2-5mg mL-1。
4. The method of preparing the selenium-coated tin dioxide/graphene nanocomposite material of claim 2, wherein: the concentration of the sodium borohydride solution in the step 2) is 0.3-0.5mg mL-1The ultrasonic time is 4-6 h.
5. The method of preparing the selenium-coated tin dioxide/graphene nanocomposite material of claim 2, wherein: the mass ratio of the selenium powder to the Sn intermediate product in the step 3) is 2-3: 1.
6. The method of preparing the selenium-coated tin dioxide/graphene nanocomposite material of claim 2, wherein: the temperature rise in the step 3) is 400-600 ℃; the calcination time is 4-5 h.
7. The use of the selenium-coated tin dioxide/graphene nanocomposite material of claim 1 in the preparation of a sodium ion battery electrode material.
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| CN110668509B (en) * | 2019-09-30 | 2020-10-23 | 南昌大学 | Selenium-coated high-nickel ternary layered positive electrode material and preparation method thereof |
| CN114678510A (en) * | 2022-04-18 | 2022-06-28 | 合肥工业大学 | Selenium-coated disordered lithium-rich material and preparation method thereof |
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