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Preparation method of granular tin dioxide/two-dimensional nano titanium carbide composite material

A two-dimensional nanometer, tin dioxide technology, applied in the direction of hybrid capacitor electrodes, electrical components, battery electrodes, etc., can solve the problems of pulverization, low specific capacity lithium intercalation potential, agglomeration, etc., to achieve improved capacitance, excellent electrochemical performance effect

Active Publication Date: 2016-04-06
SHAANXI UNIV OF SCI & TECH
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Problems solved by technology

[0004] Tin oxide has attracted much attention because of its high specific capacity and low lithium intercalation potential. It was once considered to be the most promising substitute for carbon anode materials, but it also has some disadvantages, such as volume expansion of up to 50% during the first charge and discharge process. % or more, the phenomenon of "powdering" and "agglomeration" is prone to occur during the repeated intercalation and extraction of lithium ions during the cycle, which lead to a rapid decline in the electrochemical performance of tin oxide, thus limiting its wide application in lithium-ion batteries. application
[0005] Marwick and others prepared graphene-based tin dioxide nanocomposites and studied their electrochemical properties. The experimental results showed that the charge-discharge capacity of graphene-based tin dioxide as a negative electrode material for lithium-ion batteries was significantly improved (Marwick. SnO 2 / Study on the electrochemical performance of graphene composite materials [D]. Yanshan: Yanshan University, 2011.); Zhu et al prepared SnO by hydrothermal method 2 / graphite nanocomposite materials and show that its performance in lithium-ion batteries, photocatalysis, etc. 2 / GrapheneNanocompositesforLithiumStorageApplication, [J].ElectrochimicaActa.154(2015)338–344.). 2 Supported on graphene, graphene cannot effectively relieve SnO 2 The volume effect, and in Li + Easily damaged during de-embedding

Method used

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  • Preparation method of granular tin dioxide/two-dimensional nano titanium carbide composite material
  • Preparation method of granular tin dioxide/two-dimensional nano titanium carbide composite material

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Embodiment 1

[0018] This embodiment includes the following steps:

[0019] (1) High-purity ternary layered Ti was prepared by vacuum sintering 3 AlC 2 The ceramic powder is then high-energy ball milled for 4 hours, the speed is 400r / min, the ball-to-material ratio is 10:1, and the powder is refined and dried at 60°C. From figure 2 The SEM image in (a) shows the Ti 3 AlC 2 From the microscopic morphology of the crystal, it can be seen that the grain size is about 8 μm, and its obvious layered structure;

[0020](2) Submerge 2 g of the powder obtained in step (1) at 60°C in 100 mL of 40% hydrofluoric acid solution for 48 hours, stir, and centrifuge the corrosion product with deionized water until the pH of the centrifuged supernatant = 5; then washed 3 times with absolute ethanol; the resulting solid sample was dried at room temperature to obtain a two-dimensional layered nanomaterial MXene-Ti 3 C 2 ,See figure 2 (b), where the SEM image shows the MXene-Ti 3 C 2 It can be seen th...

Embodiment 2

[0023] The present embodiment comprises the following steps:

[0024] (1) High-purity ternary layered Ti was prepared by vacuum sintering 3 AlC 2 Ceramic powder, then high-energy ball milling powder for 1h, rotating speed 400r / min, ball-to-material ratio 10:1, drying at 40°C after refining the powder, to obtain Ti 3 AlC 2 ceramic powder;

[0025] (2) Submerge 2 g of the powder obtained in step (1) at 60°C in 50 mL of 35% hydrofluoric acid solution to react for 6 hours, stir, wash with deionized water until the pH is about 5-6, and wash with absolute ethanol 2 times, centrifuged, and the resulting solid sample was dried to obtain a two-dimensional layered MXene-Ti 3 C 2 nanomaterials;

[0026] (3) SnCl 4 ·5H 2 O, glucose and the two-dimensional nanometer MXene-Ti obtained in step (2) 3 C 2 Mixed, Sn 4+ The molar ratio with glucose is 3:1, SnCl 4 ·5H 2 O and two-dimensional nanometer MXene-Ti 3 C 2 The mass ratio is 2:1, with ethanol as solvent and NH 3 ·H 2 O a...

Embodiment 3

[0028] This embodiment includes the following steps:

[0029] (1) High-purity ternary layered Ti was prepared by vacuum sintering 3 AlC 2 Ceramic powder, then high-energy ball milling powder for 3 hours, rotating speed 400r / min, ball-to-material ratio 10:1, drying at 50°C after refining the powder;

[0030] (2) Submerge 3 g of the powder obtained in step (1) in 70 mL of 35% hydrofluoric acid solution at 60°C for 24 hours, stir, and centrifuge the corrosion products with deionized water until the pH of the centrifuged supernatant is between 5 and 6; then wash with absolute ethanol for 3 times; dry the resulting solid sample to obtain a two-dimensional layered nanomaterial MXene-Ti 3 C 2 ;

[0031] (3) SnCl 4 ·5H 2 O, glucose and the two-dimensional nanometer MXene-Ti obtained in step (2) 3 C 2 Mixed, Sn 4+ The molar ratio with glucose is 3:1, SnCl 4 ·5H 2 O and two-dimensional nanometer MXene-Ti 3 C 2 The mass ratio is 2:1, with ethanol as solvent and NH 3 ·H 2 O...

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Abstract

The invention provides a preparation method of a tin dioxide / two-dimensional nano titanium carbide composite material. The preparation method comprises: carrying out ball milling on ternary layered Ti3AlC2 ceramic powder; immersing the obtained product in hydrofluoric acid solution to perform the reaction for 6h to 120h; stirring, centrifugally cleaning a corrosion product by using deionized water, and drying an obtained solid sample to obtain a two-dimensional layered nano material MXene-Ti3C2; and mixing SnCl4.5H2O, glucose and the two-dimensional nano MXene-Ti3C2, using ethanol as a solvent, adjusting PH to 12 to 14, stirring with a magnetic force for 2h, performing the reaction at 120 DEG C for 6h, and after naturally cooling to a room temperature, carrying out centrifuging and drying to obtain a SnO2 / MXene-Ti3C2 composite material. The material obtained by the preparation method can effectively alleviate a volume effect of SnO2 nano particles, and the SnO2 / MXene-Ti3C2 nano composite material has an excellent application prospect in the field of an anode material field of a high storage germanium lithium ion battery.

Description

technical field [0001] The invention belongs to the technical field of nano functional material preparation and application thereof, and in particular relates to a preparation method of granular tin dioxide / two-dimensional nano titanium carbide composite material. Background technique [0002] Two-dimensional layered nanocarbide MXene-Ti 3 C 2 It is a material with a graphene-like structure. Ultrathin two-dimensional nanosheets have super catalytic properties due to their unique morphology, small particle size, large surface-to-volume ratio, and atomic-level layer thickness. Photovoltaic performance and electrochemical performance have been widely used in functional ceramics, photocatalysis, lithium-ion batteries, solar cells, gas sensors, etc., but the two-dimensional layered nanocarbide MXene-Ti 3 C 2 It is not easy to synthesize directly, but by Ti 3 AlC 2 It is a simple and easy method to prepare ceramic powder as a precursor. [0003] Ternary layered Ti 3 AlC 2 ...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/48H01M4/58H01G11/46H01G11/36
CPCH01G11/36H01G11/46H01M4/362H01M4/48H01M4/58Y02E60/10
Inventor 王芬王子婧曹敏娟朱建锋杨海波
Owner SHAANXI UNIV OF SCI & TECH
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