CN111675221B - Preparation method of titanium carbide hollow sphere - Google Patents
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- CN111675221B CN111675221B CN202010559796.XA CN202010559796A CN111675221B CN 111675221 B CN111675221 B CN 111675221B CN 202010559796 A CN202010559796 A CN 202010559796A CN 111675221 B CN111675221 B CN 111675221B
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Abstract
The invention belongs to the technical field of preparation of nano functional materials, and particularly relates to a preparation method of a titanium carbide hollow sphere 3 AlC 2 Immersing the powder in a lithium fluoride/hydrochloric acid solution, heating and stirring for a certain time, and then centrifugally cleaning precipitates by using deionized water; then, carrying out intercalation on the precipitate by using absolute ethyl alcohol ultrasound, and then centrifuging by using deionized water to obtain a few-layer titanium carbide nanosheet dispersion liquid; and directly freezing the few-layer titanium carbide nanosheet dispersion liquid by using liquid nitrogen, and then performing freeze-drying to obtain the titanium carbide hollow sphere. The invention uses Ti 3 AlC 2 The method is characterized in that the powder is used as a precursor to prepare a few-layer titanium carbide nanosheet dispersion liquid, then titanium carbide with different concentrations is quickly frozen in liquid nitrogen, and a freeze-drying method is utilized to prepare the titanium carbide hollow sphere, so that the method is used for preparing the titanium carbide hollow sphere through freeze-drying.
Description
Technical Field
The invention belongs to the technical field of preparation of nanometer functional materials, and particularly relates to a preparation method of a titanium carbide hollow sphere.
Background
Transition metal carbides or carbon/nitride MXenes are a new two-dimensional material with a structure similar to graphene. MXenes is prepared by etching an A atomic layer in MAX crystals by a liquid phase chemical method, so that the element of the A layer in the MAX phase is removed, the structure of MX can be kept unchanged, and the MXenes has excellent catalytic and electrochemical properties. MXenes has metalloid conductivity, and simultaneously has abundant functional groups such as-F, -OH and the like on the surface compared with the traditional two-dimensional material, so that the MXenes has excellent chemical reaction activity and has great prospect as a substrate material.
For the novel two-dimensional MXene nano material, the prepared two-dimensional MXenes are stacked bodies of multilayer nanosheets in the process of etching an A atomic layer from MAX crystals by a liquid phase chemical method. The stacking of these MX layers prevents the full utilization of the two-dimensional material surface area and the full contact between the electrolyte/current collector and the electrode sheet. But the interaction force among the multiple MXene layers is strong, only a small amount of single-layer nanosheets can be obtained by a simple mechanical stripping method, and the preparation efficiency is extremely low. It is a feasible method to weaken interlayer acting force by selecting proper ions or molecules to intercalate between MXene layers and delaminate by ultrasonic or vibration.
MXenes, being a two-dimensional material, like other two-dimensional materials, tend to stack together and affect their performance. The flaky shape of the MXenes material is converted into a hollow sphere, and the conductivity of the MXenes material can be well exerted due to good independence between the spheres. Meanwhile, the shape of the hollow sphere can be used for loading other particles, or storing ions, reducing electromagnetism and the like. Therefore, the preparation of the MXenes hollow spheres has a great effect on the practical application of the MXenes hollow spheres. The literature "Mengqiang ZHao, Yury Gogotsi; advanced Materials, 2017, 29 and 1702410 report that flaky MXenes are converted into hollow spheres by using PMMA as a template and are applied to a sodium-ion battery cathode material, and the PMMA template is introduced into the preparation process of the titanium carbide hollow spheres in the method, so that the preparation process is complex.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a method for preparing titanium carbide hollow spheres by freeze drying, wherein the titanium carbide hollow spheres are ternary layered Ti 3 AlC 2 The powder is used as a precursor to prepare a few-layer titanium carbide nanosheet dispersion liquid, then titanium carbide with different concentrations is rapidly frozen in liquid nitrogen, and a freeze-drying method is utilized to prepare the titanium carbide hollow sphere, so that the method is a simple method for preparing the titanium carbide hollow sphere.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing titanium carbide hollow spheres by freeze drying comprises the following steps:
(1) pouring lithium fluoride into a hydrochloric acid solution and stirring to obtain a solution;
(2) mixing Ti 3 AlC 2 Immersing the powder in the solution in the step (1), heating and stirring, washing with deionized water, and centrifuging to obtain a precipitate;
(3) performing intercalation on the precipitate in the step (2) by using absolute ethyl alcohol ultrasound, centrifuging to obtain a precipitate, adding ionic water for ultrasound, and centrifuging to obtain a few-layer titanium carbide nanosheet dispersion liquid;
(4) diluting the few-layer titanium carbide nanosheet dispersion prepared in the step (3), freezing with liquid nitrogen, and then freeze-drying to obtain the titanium carbide hollow sphere.
Preferably, the concentration of the hydrochloric acid solution in the step (1) is 9-12M; the mass of the lithium fluoride in the step (1) is 1-2 g; the adding amount of the hydrochloric acid in the step (1) is 20-60 mL; the stirring in the step (1) is carried out for 30-60 minutes at room temperature.
Preferably, Ti described in step (2) 3 AlC 2 The mass ratio of the powder mass to the lithium fluoride in the step (1) is 1-2: 2; the heating and stirring in the step (2) are carried out for 24 hours at the temperature of 35 ℃; and (3) centrifugally cleaning the precipitate obtained in the step (2) by using deionized water until the pH value is 6.
Preferably, the absolute ethyl alcohol ultrasonic treatment time in the step (3) is 1-3 hours; the specific preparation method of the few-layer titanium carbide nanosheet dispersion liquid in the step (3) comprises the following steps: and adding deionized water into the precipitate, performing ultrasonic dispersion uniformly, centrifuging at the rotating speed of 4000 r/min to obtain a few-layer titanium carbide nanosheet suspension, repeating the step, and taking 5-8 times.
Preferably, the diluting to different concentrations in the step (4) is to add deionized water into the few-layer titanium carbide nanosheet dispersion liquid to obtain the few-layer titanium carbide nanosheet dispersion liquid with the concentration of 0.02-0.1 mg/mL; the step (4) of freezing is to place the solution in a centrifuge tube and freeze the solution in liquid nitrogen for 5-30 minutes; and (4) performing freeze drying at-80 ℃ for 24-96 hours in vacuum.
The preparation method comprises the following specific operation steps:
(1) pouring 20-60 mL of a hydrochloric acid solution with the concentration of 9-12M into a polytetrafluoroethylene beaker, starting stirring, adding 1-2 g of lithium fluoride into the solution, and continuously stirring at room temperature for 30-60 minutes;
(2) 2 g of Ti 3 AlC 2 Adding the powder into the solution, continuously stirring at 35 ℃ for reacting for 24 hours, then carrying out centrifugal separation on the product, pouring out the supernatant, and then carrying out centrifugal cleaning by using deionized water until the pH value of the supernatant is 6;
(3) and (4) carrying out ultrasonic treatment on the centrifuged precipitate for 1-2 hours by using absolute ethyl alcohol for intercalation, and centrifuging to pour out the absolute ethyl alcohol. Adding deionized water into the centrifuged precipitate, performing ultrasonic treatment, centrifuging at the rotating speed of 4000 r/min, taking the suspension, repeating the step for 5-8 times, and thus obtaining the few-layer titanium carbide nanosheet dispersion liquid;
(4) diluting the few-layer titanium carbide nanosheet dispersion liquid to be 0.02-0.1 mg/mL, directly freezing the dispersion liquid with liquid nitrogen for 5-30 minutes, and then freeze-drying the dispersion liquid at-80 ℃ for 24-96 hours to obtain the titanium carbide hollow sphere.
A titanium carbide hollow sphere prepared by the method.
The application of the titanium carbide hollow sphere is characterized in that the titanium carbide hollow sphere can be applied to electrochemical energy storage materials.
The titanium carbide hollow sphere of the invention is made of Ti 3 AlC 2 Preparing a few-layer titanium carbide nanosheet dispersion liquid by taking the powder as a precursor, then quickly freezing titanium carbide with different concentrations in liquid nitrogen, and preparing the titanium carbide hollow sphere by using a freeze-drying method. The hollow sphere is used for providing a space for loading particles, and meanwhile, the few-layer titanium carbide has a certain electric conduction capability.
Has the advantages that:
(1) the titanium carbide hollow sphere is prepared by a simple liquid nitrogen freeze-drying method, and the method can realize simple and convenient synthesis of the titanium carbide hollow sphere by reducing the concentration of the few-layer titanium carbide nanosheet dispersion liquid.
(2) According to the invention, liquid nitrogen freezing is used as a freezing mode, so that the effect of rapid freezing is achieved, the titanium carbide nanosheets can have curling power, and meanwhile, the low concentration of the few-layer titanium carbide nanosheet dispersion liquid provides a forming space for the titanium carbide hollow spheres.
Drawings
FIG. 1 is SEM images (a), (b) and (c) of hollow titanium carbide spheres prepared in example 1.
FIG. 2 is SEM images of hollow titanium carbide spheres prepared from different concentrations of the few-layer titanium carbide nanosheet dispersion of example 4, wherein (a) is 0.04 mg/mL, (b) is 0.06 mg/mL, (c) is 0.08 mg/mL, and (d) is 0.1 mg/mL.
FIG. 3 is SEM images (a) and (b) of the sample obtained in comparative example 1 taken at different magnifications. FIG. 4 is SEM images (a) and (b) of the sample obtained in comparative example 2 taken at different magnifications.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and examples.
Example 1
Pouring 40 mL of a 9M hydrochloric acid solution into a polytetrafluoroethylene beaker, starting stirring, adding 2 g of lithium fluoride, and continuously stirring at room temperature for 30 minutes; 2 g of Ti 3 AlC 2 The powder was slowly added to the above solution, and then the reaction was continued with stirring at 35 ℃ for 24 hours. The corrosion product is then centrifuged and the supernatant is decanted off. Centrifugally cleaning with deionized water for 6 times until the pH value of the supernatant is 6; and (3) carrying out ultrasonic treatment on the centrifuged precipitate for 2 hours by using absolute ethyl alcohol for intercalation, and then centrifuging to remove the ethyl alcohol. And then adding deionized water into the precipitate after the first centrifugation, centrifuging again after ultrasonic stripping, taking the suspension, adding deionized water, ultrasonically stripping, centrifuging again, taking the suspension, and taking 5 times to obtain the few-layer titanium carbide nanosheet dispersion liquid. And (3) diluting the few-layer titanium carbide nanosheet dispersion liquid to 0.02 mg/mL by adding deionized water, putting the diluted few-layer titanium carbide nanosheet dispersion liquid into a centrifugal tube, directly freezing the diluted few-layer titanium carbide nanosheet dispersion liquid for 10 minutes by using liquid nitrogen, and then freezing and drying the diluted few-layer titanium carbide nanosheet dispersion liquid for 48 hours at the temperature of-80 ℃ to obtain the titanium carbide hollow sphere.
Compared with titanium carbide with the shape of a nano sheet, the titanium carbide hollow sphere applied to the electrochemical energy storage material has the specific discharge capacity of 400 mAh g of the titanium carbide nano sheet -1 Increased to 1000 mAh g -1 And the good energy storage performance is shown.
Example 2
Pouring 20 mL of a 9M hydrochloric acid solution into a polytetrafluoroethylene beaker, starting stirring, adding 2 g of lithium fluoride, and continuously stirring at room temperature for 30 minutes; 2 g of Ti 3 AlC 2 The powder was slowly added to the above solution, and then the reaction was continued with stirring at 35 ℃ for 24 hours. The corrosion product is then centrifuged and the supernatant is decanted off. Centrifugally cleaning with deionized water for 5 times until the pH value of the supernatant is 6; and (3) carrying out ultrasonic treatment on the centrifuged precipitate for 1 hour by using absolute ethyl alcohol for intercalation, and then centrifuging to remove the ethyl alcohol. Adding deionized water into the precipitate after the first centrifugation, ultrasonically stripping, centrifuging again, and taking the suspensionAnd adding deionized water for ultrasonic stripping, then centrifuging to obtain a suspension, and taking for 5 times to obtain the few-layer titanium carbide nanosheet dispersion liquid. And (3) diluting the few-layer titanium carbide nanosheet dispersion liquid to 0.1 mg/mL by adding deionized water, putting the diluted few-layer titanium carbide nanosheet dispersion liquid into a centrifugal tube, directly freezing the diluted few-layer titanium carbide nanosheet dispersion liquid for 5 minutes by using liquid nitrogen, and then freezing and drying the diluted few-layer titanium carbide nanosheet dispersion liquid for 24 hours at the temperature of-80 ℃ to obtain the titanium carbide hollow sphere.
Compared with titanium carbide with the shape of a nano sheet, the titanium carbide hollow sphere applied to the electrochemical energy storage material has the specific discharge capacity of 400 mAh g of the titanium carbide nano sheet -1 Increasing to 900 mAh g -1 And the good energy storage performance is shown.
Example 3
Pouring 60 mL of 12M hydrochloric acid solution into a polytetrafluoroethylene beaker, starting stirring, adding 1 g of lithium fluoride, and continuously stirring at room temperature for 60 minutes; 0.5 g of Ti 3 AlC 2 The powder was slowly added to the above solution, and then the reaction was continued with stirring at 35 ℃ for 24 hours. The corrosion product is then centrifuged and the supernatant is decanted off. Centrifugally cleaning with deionized water for 5 times until the pH value of the supernatant is 6; and (4) carrying out ultrasonic treatment on the centrifuged precipitate for 1.5 hours by using absolute ethyl alcohol for intercalation, and centrifuging to remove the ethyl alcohol. And then adding deionized water into the precipitate after the first centrifugation, centrifuging again after ultrasonic stripping, taking the suspension, adding deionized water, ultrasonically stripping, centrifuging again, taking the suspension, and taking 8 times to obtain the few-layer titanium carbide nanosheet dispersion liquid. And (3) diluting the few-layer titanium carbide nanosheet dispersion liquid to 0.06 mg/mL by adding deionized water, putting the diluted few-layer titanium carbide nanosheet dispersion liquid into a centrifugal tube, directly freezing the diluted few-layer titanium carbide nanosheet dispersion liquid for 30 minutes by using liquid nitrogen, and then freeze-drying the diluted few-layer titanium carbide nanosheet dispersion liquid for 96 hours at the temperature of-80 ℃ to obtain the titanium carbide hollow sphere.
Compared with titanium carbide with the shape of a nano sheet, the titanium carbide hollow sphere applied to the electrochemical energy storage material has the specific discharge capacity of 400 mAh g of the titanium carbide nano sheet -1 Increased to 950 mAh g -1 And the good energy storage performance is shown.
Example 4
The conditions of the dispersion liquid of the few-layer titanium carbide nano-sheets are controlled to be diluted to 0.04 mg/mL, 0.06 mg/mL, 0.08 mg/mL and 0.1 mg/mL by adding deionized water, and the other conditions are the same as those of the example 1. The result proves that the concentration of the frozen few-layer titanium carbide nanosheet dispersion liquid is controlled, the fact that within the concentration range of 0.02-0.1 mg/mL, the few-layer titanium carbide nanosheet dispersion liquid forms titanium carbide hollow spheres after being rapidly frozen by liquid nitrogen and freeze-dried is found, and the size of the titanium carbide hollow spheres is gradually increased along with the increase of the concentration. Fig. 2 is an SEM image of titanium carbide hollow spheres prepared from different concentrations of the few-layer titanium carbide nanosheet dispersion in this example.
Comparative example 1
Pouring 40 mL of a 9M hydrochloric acid solution into a polytetrafluoroethylene beaker, starting stirring, adding 2 g of lithium fluoride, and continuously stirring at room temperature for 30 minutes; 2 g of Ti 3 AlC 2 The powder was slowly added to the above solution, and then the reaction was continued with stirring at 35 ℃ for 24 hours. The corrosion product is then centrifuged and the supernatant is decanted off. Centrifugally cleaning with deionized water for 8 times until the pH value of the supernatant is 6; and (4) carrying out ultrasonic treatment on the centrifuged precipitate for 0.5 hour by using absolute ethyl alcohol for intercalation, and centrifuging to remove the ethyl alcohol. And then adding deionized water into the precipitate after the first centrifugation, centrifuging again after ultrasonic stripping, taking the suspension, adding deionized water, ultrasonically stripping, centrifuging again, taking the suspension, and taking 8 times to obtain the few-layer titanium carbide nanosheet dispersion liquid. And putting the few-layer titanium carbide nanosheet dispersion liquid into a centrifugal tube without dilution, directly freezing the dispersion liquid with liquid nitrogen for 10 minutes, and then freezing and drying the dispersion liquid at the temperature of minus 80 ℃ for 48 hours to obtain a sample. The result proves that the titanium carbide hollow sphere cannot be prepared in the same way after the concentration of the titanium carbide dispersion liquid exceeds 0.1 mg/mL, and the titanium carbide nanocolloid can be formed at higher concentration.
The titanium carbide hollow sphere is applied to an electrochemical energy storage material, and compared with titanium carbide with a nano-roll shape, the titanium carbide hollow sphere has the specific discharge capacity of 380 mAh g -1 。
Comparative example 2
Pouring 40 mL of a 9M hydrochloric acid solution into a polytetrafluoroethylene beaker, starting stirring, adding 2 g of lithium fluoride, and continuously stirring at room temperature for 30 minutes; 2 g of ternary layered Ti 3 AlC 2 The powder was slowly added to the above solution, and then the reaction was continued with stirring at 35 ℃ for 24 hours. Then the corrosion products are separatedThe heart was separated and the supernatant was decanted. Centrifugally cleaning with deionized water for 8 times until the pH value of the supernatant is 6; and (4) carrying out ultrasonic treatment on the centrifuged precipitate for 0.5 hour by using absolute ethyl alcohol for intercalation, and centrifuging to remove the ethyl alcohol. And then adding deionized water into the precipitate after the first centrifugation, centrifuging again after ultrasonic stripping, taking the suspension, adding deionized water, ultrasonically stripping, centrifuging again, taking the suspension, and taking 8 times to obtain the few-layer titanium carbide nanosheet dispersion liquid. Diluting the few-layer titanium carbide nanosheet dispersion to 0.1 mg/mL, putting the diluted few-layer titanium carbide nanosheet dispersion into a centrifuge tube, freezing the centrifuge tube in a refrigerator at the temperature of-18 ℃ for 6 hours, and then freezing and drying the centrifuge tube at the temperature of-80 ℃ for 48 hours to obtain a sample. The result proves that the titanium carbide hollow sphere can not be prepared in the same way under the condition of slow freezing in a refrigerator instead of liquid nitrogen quick freezing, and the titanium carbide hollow sphere still has the shape of a titanium carbide nano sheet during slow freezing.
The titanium carbide hollow sphere is applied to an electrochemical energy storage material, and compared with titanium carbide with a nano-roll shape, the titanium carbide hollow sphere has the specific discharge capacity of 420 mAh g -1 。
The one-dimensional titanium carbide nanobelt of the invention is ternary layered Ti 3 AlC 2 Preparing a few-layer titanium carbide nanosheet dispersion liquid by taking the powder as a precursor, then quickly freezing titanium carbide with different concentrations in liquid nitrogen, and preparing the titanium carbide hollow sphere by using a freeze-drying method. The titanium carbide hollow sphere is prepared by a simple liquid nitrogen freeze-drying method, and the method can be used for quickly and conveniently synthesizing the titanium carbide hollow sphere at low cost by changing the concentration of the few-layer titanium carbide nanosheet dispersion liquid. The hollow ball is used for providing a space for loading particles, and meanwhile, the few-layer titanium carbide has certain conductivity. The titanium carbide hollow sphere prepared by the method has important use value in the aspects of material transportation, catalyst loading and the like. Searching the literature, and finding that no one has adopted such a simple and effective method to prepare the titanium carbide hollow sphere so far.
Claims (4)
1. The preparation method of the titanium carbide hollow sphere is characterized by comprising the following steps of:
(1) adding lithium fluoride into a hydrochloric acid solution and stirring to obtain a solution; the mass of the lithium fluoride is 1-2 g; the addition amount of the hydrochloric acid solution is 20-60 mL; the concentration of the hydrochloric acid solution is 9-12M;
(2) mixing Ti 3 AlC 2 Immersing the powder in the solution obtained in the step (1), heating and stirring, washing with deionized water, and centrifuging to obtain a precipitate; the Ti 3 AlC 2 The mass ratio of the powder mass to the lithium fluoride in the step (1) is 1-2: 2;
(3) performing intercalation on the precipitate in the step (2) by using absolute ethyl alcohol ultrasound, centrifuging to obtain a precipitate, adding ionic water for ultrasound, and centrifuging to obtain a few-layer titanium carbide nanosheet dispersion liquid; the ultrasonic time of the absolute ethyl alcohol is 1-2 hours; the specific preparation method of the few-layer titanium carbide nanosheet dispersion liquid comprises the following steps: adding deionized water into the precipitate, performing ultrasonic dispersion uniformly, centrifuging at the rotating speed of 4000 r/min to obtain a few-layer titanium carbide nanosheet suspension, repeating the step, and taking 5-8 times;
(4) ultrasonically diluting the few-layer titanium carbide nanosheet dispersion prepared in the step (3), freezing the dispersion by using liquid nitrogen, and then freeze-drying the dispersion by cooling to obtain a titanium carbide hollow sphere; the ultrasonic dilution is to obtain a few-layer titanium carbide nanosheet dispersion solution with the concentration of 0.02-0.1 mg/mL after adding deionized water into the few-layer titanium carbide nanosheet dispersion solution; the freezing step is that the solution is placed in a centrifuge tube and is frozen in liquid nitrogen for 5-30 minutes; the freeze drying is vacuum treatment at-80 ℃ for 24-96 hours.
2. The method according to claim 1, wherein the stirring in step (1) is performed at room temperature for 30 to 60 minutes.
3. The method according to claim 1, wherein the heating and stirring in the step (2) is carried out at 35 ℃ for 24 hours; and (3) centrifugally cleaning the precipitate obtained in the step (2) by using deionized water until the pH value is 6.
4. The preparation method according to any one of claims 1 to 3, characterized by comprising the following specific operating steps:
(1) pouring 20-60 mL of a hydrochloric acid solution with the concentration of 9-12M into a polytetrafluoroethylene beaker, starting stirring, adding 1-2 g of lithium fluoride into the solution, and continuously stirring at room temperature for 30-60 minutes;
(2) 2 g of Ti 3 AlC 2 Adding the powder into the solution obtained in the step 1, continuously stirring at 35 ℃ for reacting for 24 hours, then performing centrifugal separation on the product, pouring out the supernatant, and centrifugally cleaning with deionized water until the pH value of the supernatant is 6;
(3) performing ultrasonic treatment on the centrifuged precipitate for 1-2 hours by using absolute ethyl alcohol to perform intercalation, centrifuging again to pour out the absolute ethyl alcohol, adding deionized water into the centrifuged precipitate, performing ultrasonic treatment, centrifuging at the rotating speed of 4000 r/min, taking the suspension, repeating the step, and taking 5-8 times to obtain a few-layer titanium carbide nanosheet dispersion liquid;
(4) diluting the few-layer titanium carbide nanosheet dispersion liquid prepared in the step (3) to 0.02-0.1 mg/mL, directly freezing the dispersion liquid with liquid nitrogen for 5-30 minutes, and then freeze-drying the dispersion liquid at-80 ℃ for 24-96 hours to obtain the titanium carbide hollow sphere.
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