CN116282027A

CN116282027A - Method for preparing porous titanium carbide by rapid sintering

Info

Publication number: CN116282027A
Application number: CN202310327076.4A
Authority: CN
Inventors: 徐英; 赵智益; 李涛; 郑换琴; 郑权
Original assignee: Lanzhou University
Current assignee: Lanzhou University
Priority date: 2023-03-30
Filing date: 2023-03-30
Publication date: 2023-06-23

Abstract

The invention discloses a method for preparing porous titanium carbide by rapid sintering. The method comprises the following specific processes: firstly preparing titanium oxide or titanium metal dispersion, immersing a carbon substrate in the dispersion, fully soaking, drying, then connecting a power supply, then introducing instant high current of 60-200A at two ends of the dried carbon substrate, quickly heating to 1600-2700K, and keeping heating for 30-200 seconds to enable the titanium oxide or titanium metal to react with the carbon substrate to generate porous titanium carbide. The method for preparing the porous titanium carbide by utilizing the instantaneous high-current rapid heating sintering method has the advantages of extremely short preparation time, simple preparation and low cost, and the prepared porous titanium carbide has a stable structure and wide application prospect in the fields of lithium/sodium ion batteries, catalysis, sensing and the like.

Description

Method for preparing porous titanium carbide by rapid sintering

Technical Field

The invention belongs to the field of material preparation, and particularly relates to a method for obtaining porous titanium carbide through rapid sintering.

Background

Titanium carbide is a typical ceramic material, and has high hardness and excellent conductivity. Such materials are often used in the fields of lithium/sodium ion batteries, catalysis and sensing. In recent years, porous titanium carbide has been attracting attention because of its abundant pore structure, high specific surface area, and many adsorption sites. In the charge and discharge process of the lithium-sulfur battery, a plurality of side reactions can occur to influence the performance of the battery, and the shuttle effect can be effectively weakened by embedding sulfur into the porous structure, so that the performance of the lithium-sulfur battery can be effectively improved by using porous carbonization as a substrate. Meanwhile, the porous titanium carbide not only maintains the excellent conductivity of the titanium carbide, but also provides a large number of active adsorption sites for metal ions in the abundant pore structure, and has wide application prospects in the fields of catalysts and adsorbents.

Titanium carbide can be prepared by carbothermic, direct carbonization, chemical vapor deposition, etc., but there are fewer methods for preparing porous titanium carbide. The carbothermal reduction method uses carbon black and titanium oxide to mix, and the reaction time is long at 1700K or more, the particle size of titanium carbide is large, and the product is difficult to form a porous state. The direct carbonization method is to directly react titanium powder and carbon powder to generate titanium carbide, and the titanium carbide material with certain porosity can be generated, but the reaction is difficult to control, and the preparation cost is high. The chemical vapor deposition method synthesizes the coating or the nano material by reacting chemical gas or steam on the surface of the substrate, and the method can successfully prepare the porous titanium carbide, but the operation process is complex, and the raw material titanium chloride is corrosive. Therefore, we need to explore a method for preparing porous titanium carbide with short preparation time, simple operation, mass production and low cost, so as to promote the practical application in the fields of lithium/sodium ion batteries, catalysis, sensing and the like.

Disclosure of Invention

In view of the above-mentioned shortcomings in the prior art, it is an object of the present invention to provide a method for preparing porous titanium carbide by rapid sintering.

In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:

a method for preparing porous titanium carbide by rapid sintering comprises the following steps:

(1) Dispersing titanium oxide or metallic titanium in a solvent, adding a small amount of oleylamine, carrying out ultrasonic treatment to uniformly disperse the oleylamine, immersing a carbon substrate, and drying the carbon substrate loaded with the titanium oxide or metallic titanium for later use after the carbon substrate is fully immersed;

(2) And (3) connecting the two ends of the carbon substrate obtained in the step (1) to a direct current power supply, introducing an instantaneous heavy current of 60-200A under the protection of vacuum or inert atmosphere, rapidly heating to 1600-2700K, keeping heating for 30-200 seconds, and finally taking down the sample.

Further, the titanium oxide in the step (1) is one or more of titanium oxide, titanium dioxide, titanium trioxide and titanium pentoxide.

Further, the solvent in the step (1) is one or more of deionized water, absolute ethyl alcohol, n-hexane, methanol, isopropanol and cyclohexane.

Further, the carbon substrate in the step (1) is one or more of carbon cloth, carbon felt, carbon paper, carbon fiber, graphene and carbon nanotube.

Further, the mixing ratio of the titanium oxide or the metallic titanium and the solvent in the step (1) is 1 mmol/20 mL to 1 mmol/2 mL.

Further, the ratio of the oleylamine to the solvent in the step (1) is 50. Mu.L:10 mL to 300. Mu.L:10 mL.

Further, in the rapid temperature rising process in the step (2), the inert atmosphere is one or more of nitrogen, argon and helium.

The method for preparing the porous titanium carbide by rapid sintering provided by the invention has the following advantages:

(1) The preparation time of the material is short, no new impurity is introduced, and the obtained product is pure;

(2) The prepared porous titanium carbide has stable structure;

(3) The preparation method is simple, low in cost and capable of large-scale preparation.

Drawings

FIG. 1 is an X-ray diffraction pattern of porous titanium carbide prepared in example 1 of the present invention;

FIG. 2 is a scanning electron micrograph of porous titanium carbide prepared according to example 1 of the present invention;

FIG. 3 is a scanning electron micrograph of porous titanium carbide prepared according to example 2 of the present invention;

FIG. 4 is a scanning electron micrograph of porous titanium carbide prepared according to example 4 of the present invention.

Detailed Description

The following description of the embodiments of the present invention is provided to facilitate understanding of the present invention by those skilled in the art, but it should be understood that the present invention is not limited to the scope of the embodiments, and all the inventions which make use of the inventive concept are protected by the spirit and scope of the present invention as defined and defined in the appended claims to those skilled in the art.

Example 1

(1) Preparing uniformly dispersed titanium dioxide solution and loading the solution on carbon cloth, wherein the preparation method comprises the following specific steps:

(a) 79mg of titanium dioxide is added into 10mL of absolute ethyl alcohol, 150 mu L of oleylamine is dripped into the absolute ethyl alcohol, and stirring and dissolving are carried out;

(b) Dispersing (a) by ultrasonic for 30 minutes until the solution is uniformly dispersed;

(c) Soaking the carbon cloth in the solution (b) for 30 minutes, taking out, airing and putting into an oven for drying.

(2) Carrying out rapid high-temperature treatment on the carbon cloth loaded with the titanium dioxide obtained in the step (1), wherein the specific steps are as follows:

(a) Connecting two ends of carbon cloth loaded with titanium dioxide into a direct current power supply;

(b) Under the protection of argon, 70A current is introduced into two ends of the carbon cloth, the carbon cloth loaded with titanium dioxide rapidly reaches 2700K in 8 seconds, and the carbon cloth is kept at the temperature for 100 seconds.

Example 2

(1) The preparation method comprises the following specific steps of:

(a) 63mg of titanium oxide is added into 10mL of normal hexane, 75 mu L of oleylamine is dripped into the mixture, and the mixture is stirred and dissolved;

(c) Soaking carbon cloth in the solution (b) for 40 minutes, and putting the carbon cloth into an oven for drying.

(2) Carrying out rapid high-temperature treatment on the titanium oxide-loaded carbon cloth obtained in the step (1), wherein the specific steps are as follows:

(a) Connecting two ends of the carbon cloth loaded with titanium oxide into a direct current power supply;

(b) Under the vacuum condition, 65A current is introduced into two ends of the carbon cloth, the carbon cloth loaded with titanium oxide rapidly reaches 2600K in 8 seconds, and the carbon cloth is kept at the temperature for 150 seconds.

Example 3

(1) Preparing a uniformly dispersed titanium dioxide solution and loading the solution on a carbon nano tube, wherein the preparation method comprises the following specific steps of:

(a) 79mg of titanium dioxide is added into 20mL of methanol, 100 mu L of oleylamine is dripped into the mixture, and the mixture is stirred and dissolved;

(b) Ultrasonically dispersing (a) for 25 minutes;

(c) Soaking the carbon nano tube into the solution (b) for 50 minutes, and putting the carbon nano tube into an oven for drying.

(a) Connecting two ends of the carbon nano tube loaded with titanium dioxide into a direct current power supply;

(b) Under the protection of argon, 80A current is introduced into two ends of the carbon nano tube, the carbon nano tube loaded with titanium dioxide rapidly reaches 2650K in 7 seconds, and the temperature is kept for 120 seconds.

Example 4

(1) The preparation method comprises the following specific steps of:

(a) 79mg of titanium dioxide is added into 20mL of normal hexane, and the mixture is stirred and dissolved;

(b) Ultrasonically dispersing (a) for 45 minutes;

(c) Soaking the carbon fiber in the solution (b) for 50 minutes, and putting the carbon fiber into an oven for drying.

(2) Carrying out rapid high-temperature treatment on the carbon fiber loaded with titanium dioxide obtained in the step (1), wherein the specific steps are as follows:

(a) Connecting two ends of carbon fiber loaded with titanium dioxide into a direct current power supply;

(b) Under the protection of argon, 75A current is introduced into two ends of the carbon fiber, the carbon fiber loaded with titanium dioxide rapidly reaches 2600K in 5 seconds, and the carbon fiber is kept at the temperature for 150 seconds.

Claims

1. A method for preparing porous titanium carbide by rapid sintering, which is characterized by comprising the following steps:

step one: dispersing titanium oxide or metallic titanium in a solvent, adding a small amount of oleylamine, carrying out ultrasonic treatment to uniformly disperse the titanium oxide or metallic titanium, immersing a carbon-containing substrate, and drying the carbon substrate loaded with the titanium oxide or metallic titanium for later use after the carbon-containing substrate is fully immersed;

step two: and D, connecting direct current power supplies to two ends of the carbon substrate obtained in the step I, introducing instantaneous heavy current of 60-200A under the protection of vacuum or inert atmosphere, rapidly heating to 1600-2700K, keeping heating for 30-200 seconds, and finally taking down the sample.

2. The method of rapid sintering for producing porous titanium carbide according to claim 1 wherein the titanium oxide is one or more of titanium oxide, titanium dioxide, titanium trioxide, titanium pentoxide.

3. The method of claim 1, wherein the solvent is one or more of deionized water, absolute ethanol, n-hexane, methanol, isopropanol, and cyclohexane.

4. The method for preparing porous titanium carbide by rapid sintering according to claim 1, wherein the mixing ratio of titanium oxide or metallic titanium and solvent is 1 mmol/20 ml to 1 mmol/2 ml.

5. The method of rapid sintering for producing porous titanium carbide according to claim 1 wherein the ratio of oleylamine to solvent is described as 50 μl:10mL to 300 μl:10mL.

6. The method for preparing porous titanium carbide by rapid sintering according to claim 1, wherein the carbon substrate is one or more of carbon cloth, carbon felt, carbon paper, carbon fiber, graphene and carbon nanotube.

7. The method for preparing porous titanium carbide by rapid sintering according to claim 1, wherein the inert atmosphere is one or more of nitrogen, argon and helium.