CN113247903B - Porous Ti 3 C 2 SnO nano material and preparation method and application thereof - Google Patents
Porous Ti 3 C 2 SnO nano material and preparation method and application thereof Download PDFInfo
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- CN113247903B CN113247903B CN202110672976.3A CN202110672976A CN113247903B CN 113247903 B CN113247903 B CN 113247903B CN 202110672976 A CN202110672976 A CN 202110672976A CN 113247903 B CN113247903 B CN 113247903B
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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Abstract
The present invention relates to porous Ti 3 C 2 The SnO nano material can be used as the negative electrode of potassium ion battery. First Ti is reacted with a weak acid 3 C 2 Oxidizing; then Ti is etched away by strong acid 3 C 2 Surface oxidation of produced TiO 2 Obtaining porous Ti 3 C 2 (ii) a Then mixing the porous Ti 3 C 2 With SnCl 2 ·2H 2 O is mixed and then prepared into porous Ti by hydrothermal synthesis reaction 3 C 2 SnO, wherein Ti 3 C 2 The aperture of the surface is 20 nm-50nm, and the diameter of the SnO nano-particles is 30nm-80nm. The invention has the beneficial effects that: porous Ti 3 C 2 the/SnO shows ideal rate performance and cycling stability.
Description
Technical Field
The invention belongs to the technical field of electrode materials and electrochemistry of potassium ion batteries, and particularly relates to porous Ti 3 C 2 SnO nano material and a preparation method thereof, wherein the material can be used as a negative electrode active material of a potassium ion battery.
Background
With the development requirements of large-scale energy storage application fields such as electric vehicles and smart power grids, the further development of lithium ion batteries is inevitably restricted by the rare lithium resource uneven distribution. The potassium ion battery is distinguished by unique advantages (such as rich potassium resource, uniform distribution and low price) and becomes a powerful competitor of the lithium ion battery. However, although the existing potassium ion electrode material has good potassium storage capacity, the potassium storage capacity is greatly reduced due to the larger radius of potassium ions and the like. Therefore, finding suitable potassium storage materials and modifying and optimizing the performance of the existing electrode materials become one of the important challenges in developing potassium ion batteries. Greater K + The radius (0.138 nm) causes the electrode reaction kinetics to slow down and leads to pulverization of the electrode active material during cycling. KIBs are still in the beginning stage, and electrode materials with high capacity and good cycle stability are yet to be developed. Graphite is the most commonly used material with excellent conductivity, large interlayer spacing (3.4 nm) and 279mAh g -1 The capacity of (c). However, practical application of graphite cathode materials remains challenging due to their low capacity and capacity retention. Alloy baseComposite materials are an effective alternative to this problem. Sn-based negative electrode materials are considered to be the most promising materials in potassium ion battery electrodes, with higher theoretical capacity. However, low electronic conductivity and volume expansion lead to slow reaction kinetics and poor cycling stability.
Therefore, the development of high-performance potassium ion battery materials has very important scientific guiding significance for the development and application of new energy storage devices
Disclosure of Invention
Aiming at the defects of the existing SnO electrode material, the invention provides porous Ti 3 C 2 SnO nano material and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
porous Ti 3 C 2 SnO nano material and its preparation method, characterized in that, ti is first treated with weak acid 3 C 2 Oxidizing; then Ti is etched away by strong acid 3 C 2 Surface oxidation of the resulting TiO 2 Obtaining porous Ti 3 C 2 (ii) a Then porous Ti 3 C 2 With SnCl 2 ·2H 2 O is mixed and then prepared into porous Ti by hydrothermal synthesis reaction 3 C 2 SnO, wherein Ti 3 C 2 The surface aperture is 20 nm-50nm, and the diameter of SnO nano-particles is 30nm-80nm.
The method specifically comprises the following steps:
1) Taking Ti 3 C 2 Dispersing 50mg of powder in 50ml of deionized water, and performing ultrasonic dispersion for half an hour;
2) Adding hydrogen peroxide (10ml) and (3000r min) into the step (1) -1 Magnetically stirring for 15 minutes;
3) Adding concentrated hydrochloric acid 3ml.3000r min into the step (2) -1 Stirring for 25 minutes and then carrying out suction filtration;
4) Dispersing the sample obtained in the step (3) in 30ml of deionized water, and freezing at the ultralow temperature of-60 ℃; transferring the completely frozen sample to a vacuum freeze drier for vacuum drying for 48 hours to obtain porous Ti 3 C 2
5) Weighing the porous Ti in the step (4) according to the proportion 3 C 2 Powder 30mg and 80mg SnCl 2 ·2H 2 O, dispersing in 60ml deionized water, transferring to a polytetrafluoroethylene reaction kettle for hydrothermal reaction after magnetic stirring, wherein the reaction temperature is 180 ℃, the reaction time is 12 hours, centrifugally washing a product obtained after the reaction is finished, filtering and drying to obtain porous Ti 3 C 2 SnO nano-materials.
According to the scheme, the Ti in the step 1) 3 C 2 The number of powder layers is 2-20, ti 3 C 2 The thickness of the lamella is 0.2-2 microns, and the mass is 20-100 mg; the deionized water is 30-80 ml; the concentration of the hydrogen peroxide in the step 2) is 9.0-9.7mol/L, and the dosage is 2-10ml; 1-5ml of concentrated hydrochloric acid in the step 3); snCl described in step 5) 2 ·2H 2 O is 60-200mg;
according to the scheme, the hydrothermal reaction temperature in the step 5) is 120-220 ℃, and the reaction time is 8-12 hours;
according to the scheme, the porous Ti 3 C 2 The SnO nano material and the preparation method thereof are characterized in that: ti in the nano material 3 C 2 The aperture of the surface is 20 nm-50nm, and the diameter of the SnO nano-particles is 30nm-80nm.
The porous Ti 3 C 2 The application of the/SnO nanometer material as a potassium ion battery cathode material.
The beneficial effects of the invention are: by acidic oxidation-in-situ etching method on Ti 3 C 2 Pore-forming preparation of 3D porous interpenetrating Ti on lamellar surface 3 C 2 A substrate and further preparing porous Ti through hydrothermal synthesis 3 C 2 SnO nano-materials. The result shows that the nano composite material prepared by the method has uniform particles and uniform appearance. Ti having good conductivity 3 C 2 Can provide a very good electron transmission channel, and the porous structure can provide a smooth and continuous transfer channel for the diffusion of electrolyte ions. While nano SnO 2 The nano particles are loaded on the Ti sheet layer 3 C 2 Surface, can act as a pillar to prevent Ti 3 C 2 Stacking between the sheets. Thus porous Ti 3 C 2 The synergistic enhancement effect between the nano-particles and SnO can greatly improve the active specific surface area of the material and the specific capacity of the material. The porous Ti provided by the invention 3 C 2 The preparation method of the SnO nano material can effectively improve the charge and discharge performance of the potassium ion battery, enhance the rate capability of the electrode and solve the problems of poor SnO conductivity and Ti 3 C 2 The self-accumulation and the like, and has good prospect in the application field of the potassium ion battery cathode.
Drawings
FIG. 1 shows porous Ti prepared in example 1 of the present invention 3 C 2 SnO nanometer scanning electron microscope;
FIG. 2 is a graph showing the rate capability test in example 1 of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, but the contents of the present invention are not limited to the following embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1:
porous Ti 3 C 2 The preparation method of the SnO nano material comprises the following steps:
1) Taking 40mg of Ti 3 C 2 Dispersing the powder in 60ml of deionized water, and performing ultrasonic dispersion for half an hour;
2) Adding 5ml of hydrogen peroxide into the step (1), and magnetically stirring for 20 minutes;
3) Adding 2ml of concentrated hydrochloric acid into the step (2), stirring for 10 minutes, and then carrying out suction filtration;
4) Dispersing the sample obtained in the step (3) in 40ml of deionized water, and freezing for 48 hours at the ultralow temperature of-60 ℃; transferring the completely frozen sample to a vacuum freeze drier for vacuum drying for 48 hours to obtain porous Ti 3 C 2 ；
5) Weighing the porous Ti in the step (4) 3 C 2 Powder 30mg and 80mg SnCl 2 ·2H 2 Dispersing O in 80ml of deionized water, magnetically stirring, transferring to a 100ml of polytetrafluoroethylene reaction kettle for hydrothermal reaction at 180 ℃ for 8 hours, centrifugally washing a product obtained after the reaction is finished, and drying in vacuum to obtain porous Ti 3 C 2 SnO nanomaterial, porous Ti 3 C 2 The grain diameter of SnO is 20-100 um.
Example 2:
porous Ti 3 C 2 The preparation method of the SnO nano material comprises the following steps:
1) 80mg of Ti was taken 3 C 2 Dispersing the powder in 80ml of deionized water, and performing ultrasonic dispersion for half an hour;
2) Adding 10ml of hydrogen peroxide into the step (1), and magnetically stirring for 20 minutes;
3) Adding 3ml of concentrated hydrochloric acid into the step (2), stirring for 20 minutes, and then carrying out suction filtration;
4) Dispersing the sample obtained in the step (3) in 40ml of deionized water, and freezing for 48 hours at the ultralow temperature of-60 ℃; transferring the completely frozen sample to a vacuum freeze drier for vacuum drying for 56 hours to obtain porous Ti 3 C 2
5) Weighing the porous Ti in the step (4) 3 C 2 60mg and 150mg of SnCl powder 2 ·2H 2 Dispersing O in 90ml of deionized water, magnetically stirring, transferring to a 100ml of polytetrafluoroethylene reaction kettle for hydrothermal reaction at 220 ℃ for 6 hours, centrifugally washing a product obtained after the reaction is finished, and drying in vacuum to obtain porous Ti 3 C 2 SnO nanomaterial, porous Ti 3 C 2 The grain diameter of SnO is 50-120 um.
Example 3:
porous Ti 3 C 2 The preparation method of the SnO nano material comprises the following steps:
1) Taking 100mg of Ti 3 C 2 Dispersing the powder in 100ml of deionized water, and performing ultrasonic dispersion for half an hour;
2) Adding 15ml of hydrogen peroxide into the step (1), and magnetically stirring for 30 minutes;
3) Adding 5ml of concentrated hydrochloric acid into the step (2), stirring for 20 minutes, and then carrying out suction filtration;
4) Dispersing the sample obtained in the step (3) in 60ml of deionized water, and freezing for 56 hours at the ultralow temperature of-60 ℃; transferring the completely frozen sample to a vacuum freeze drier for vacuum drying for 72 hours to obtain porous Ti 3 C 2 ；
5) Weighing the porous Ti in the step (4) 3 C 2 Powder 80mg and 200mg SnCl 2 ·2H 2 Dispersing O in 120ml of deionized water, transferring the mixture to a 200ml polytetrafluoroethylene reaction kettle after magnetic stirring for hydrothermal reaction at 220 ℃ for 8 hours, centrifugally washing the product obtained after the reaction is finished, and drying the product in vacuum to obtain the porous Ti 3 C 2 SnO nanomaterial, porous Ti 3 C 2 The grain diameter of SnO is 60-120 um.
And (4) performance testing:
porous Ti 3 C 2 Testing of electrochemical properties of SnO:
160mg of Ti is weighed according to the mass ratio of 8 3 C 2 Fully grinding 20mg of conductive carbon black or Ketjen black and 20mg of PVDF (polyvinylidene fluoride) binder in an agate mortar for 50min, adding 10ml of NMP (N-methyl pyrrolidone) solvent, continuously grinding to prepare slurry, uniformly coating the slurry on a copper foil current collector by using a scraper, drying the pole pieces in a vacuum drying oven at 70 ℃ for 24 hours, taking out the pole pieces, cutting the pole pieces into round pieces with the diameter of 12 mm by using a punching machine, and preparing to obtain a negative electrode, wherein the loading capacity of active substances of each pole piece is about 0.8-1mg; and in an inert atmosphere glove box, a potassium sheet with the diameter of 8mm is taken as a counter electrode to be packaged in a CR2032 button cell, and a constant current charge-discharge performance test is carried out. The cycle stability performance test parameters were as follows: the charging and discharging voltage interval is 0.01-2V, and the current is 500mA g -1 The number of cycles is 300. The multiplying power test current density is 0.0 5A g respectively -1 、0.1A g -1 、0.2A g -1 、0.5A g -1 、 1A g -1 、2A g -1 、0.1A g -1 、0.05A g -1 。
While the preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including the preferred embodiment and all changes and modifications that fall within the scope of the present application.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present application without departing from the spirit and scope of the application. Thus, if such modifications and variations of the present application fall within the scope of the claims of the present application and their equivalents, the present application is intended to include such modifications and variations as well.
In addition to the technical features described in the specification, the technology is known to those skilled in the art.
Claims (5)
1. Porous Ti 3 C 2 The preparation method of SnO nanometer material is characterized in that firstly Ti is mixed with weak acid 3 C 2 Oxidizing; then Ti is etched away by strong acid 3 C 2 Surface oxidation of the resulting TiO 2 Obtaining porous Ti 3 C 2 (ii) a Then porous Ti 3 C 2 With SnCl 2 ·2H 2 O is mixed and then prepared into porous Ti by hydrothermal synthesis reaction 3 C 2 SnO, wherein Ti 3 C 2 The aperture of the surface is 20nm to 50nm, and the diameter of the SnO nano-particles is 30nm to 80nm;
the method specifically comprises the following steps:
1) Taking Ti 3 C 2 Dispersing the powder in deionized water, and performing ultrasonic dispersion for half an hour;
2) Adding hydrogen peroxide into the mixture obtained in the step (1) according to a certain proportion, and magnetically stirring for 10-30 minutes;
3) Adding concentrated hydrochloric acid into the step (2), stirring for 10-20 minutes, and then performing suction filtration;
4) Dispersing the sample obtained in the step (3) in deionized water, and freezing at ultralow temperature; transferring the completely frozen sample to a vacuum freeze dryer for vacuum drying for 24-56 hours to obtain porous Ti 3 C 2 ；
5) Weighing the porous Ti in the step (4) according to the proportion 3 C 2 Powder and SnCl 2 ·2H 2 Dispersing O in deionized water, magnetically stirring, transferring to a polytetrafluoroethylene reaction kettle for hydrothermal reaction, centrifugally washing a product obtained after the reaction is finished, filtering and drying to obtain porous Ti 3 C 2 SnO nano-materials.
2. The porous Ti of claim 1 3 C 2 The preparation method of the SnO nano material is characterized by comprising the following steps: ti described in step 1) 3 C 2 The number of powder layers is 2-20, ti 3 C 2 The thickness of the lamella is 0.2-2 microns, and the mass is 20-100 mg; 30-80 ml of deionized water; the concentration of the hydrogen peroxide in the step 2) is 9.0-9.7mol/L, and the dosage is 2-10ml; 1-5ml of concentrated hydrochloric acid in the step 3); snCl described in step 5) 2 ·2H 2 O is 60-200mg.
3. The porous Ti of claim 1 3 C 2 The preparation method of the SnO nanometer material is characterized in that the hydrothermal reaction temperature in the step 5) is 120-220 ℃, and the reaction time is 8-12 hours.
4. Porous Ti prepared by the preparation method of any one of claims 1 to 3 3 C 2 SnO nano-materials.
5. The porous Ti of claim 4 3 C 2 SnO nano material, characterized in that: ti in the nano material 3 C 2 The surface aperture is 20nm to 50nm, and the diameter of the SnO nano-particles is 30nm to 80nm.
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