阅读说明：本技术 一种Ti3C2粉体的制备方法 (Ti3C2Method for preparing powder ) 是由 胡春峰 索尔沃托瑞·格拉索 朱德贵 范龙凤 于 2018-10-10 设计创作，主要内容包括：本发明公开了一种Ti_3C_2粉体的制备方法,包括以下步骤：(1)以Ti_3AlC_2陶瓷粉为原料,在水浴中对其进行刻蚀；(2)调整上述溶液PH值,使得溶液为中性；(3)将上述溶液进行离心分散、超声剥离得到Ti_3C_2纳米悬浮液；(4)将上述Ti_3C_2纳米悬浮液通过喷雾干燥机进行快速干燥,进风口温度为180℃,出风口温度为80℃,进料速度为300ml/h。(The invention discloses a Ti 3 C 2 The preparation method of the powder comprises the following steps: (1) with Ti 3 AlC 2 Etching ceramic powder serving as a raw material in water bath; (2) adjusting the pH value of the solution to make the solution neutral; (3) the solution is centrifugally dispersed and ultrasonically stripped to obtain Ti 3 C 2 A nanosuspension; (4) mixing the above Ti 3 C 2 The nanometer suspension is rapidly dried by a spray dryer, the temperature of an air inlet is 180 ℃, the temperature of an air outlet is 80 ℃, and the feeding speed is 300 ml/h.)

1. Ti₃C₂The preparation method of the powder is characterized by comprising the following steps:

(1) with Ti₃AlC₂Etching ceramic powder serving as a raw material in water bath;

(2) adjusting the pH value of the solution to make the solution neutral;

(3) the solution is centrifugally dispersed and ultrasonically stripped to obtain Ti₃C₂A nanosuspension;

(4) mixing the above Ti₃C₂The nanometer suspension is rapidly dried by a spray dryer, the temperature of an air inlet is 180 ℃, the temperature of an air outlet is 80 ℃, and the feeding speed is 300 ml/h.

2. A Ti according to claim 1₃C₂The preparation method of the powder is characterized in that few-layer or single-layer Ti is obtained by centrifugal dispersion and ultrasonic stripping for a plurality of times in the step (3)₃C₂And (4) nano suspension.

3. The method of claim 1Seed of Ti₃C₂The powder preparation method is characterized in that the powder is prepared from 400-mesh Ti₃AlC₂Ceramic powder is used as raw material.

4. A Ti according to claim 1₃C₂The preparation method of the powder is characterized in that the etching agent is hydrochloric acid with 36 percent of concentration and LiF; hydrochloric acid and LiF and Ti₃AlC₂The ratio of the ceramics is 30: 1.89: 1.5.

5. A Ti according to claim 1₃C₂The preparation method of the powder is characterized in that the water bath etching temperature is 40 ℃ and the time is 24 h.

6. A Ti according to claim 1₃C₂The preparation method of the powder is characterized in that deionized water is used for cleaning in the step (2) until the supernatant is neutral.

Technical Field

The invention relates to the field of self-supporting materials, in particular to Ti₃C₂A method for preparing powder.

Background

Ti₃C₂The two-dimensional layered structure of graphene has very high elastic modulus, excellent electrical property, optical property, mechanical property and magnetic property, so that Ti₃C₂The material has good application prospect as a self-supporting material in the fields of electric energy storage and conversion such as lithium ion battery electrode materials, electronic devices, sodium ion batteries, super capacitors, novel sensors and the like. At the same time, Ti₃C₂The excellent performance and the unique structure of the composite material lead the composite material to have potential application value in the fields of friction lubrication and composite material reinforcement,are increasingly concerned by researchers at home and abroad. In general, Ti₃C₂The suspension is oxidized in about one week and its stability is poor by adding Ti₃C₂The suspension is prepared into Ti₃C₂Powder, can obviously improve Ti₃C₂Stability of (2).

Chinese patent document 201710251110.9 discloses transition metal oxide nanoparticle doped two-dimensional layered Ti₃C₂A film nanocomposite and a method of making the same, which first produces two-dimensional single or multi-layered Ti₃C₂And (3) nano materials. In a single or multiple layers of Ti₃C₂The nano-sheet is taken as a substrate, is dissolved and dissolved with manganese nitrate solution by utilizing electrostatic adsorption, is filtered to form a film, and is thermally treated to synthesize the two-dimensional layered manganese oxide doped Ti₃C₂The preparation efficiency of the preparation method is slow.

Chinese patent document 201310131520.1 discloses a method for rapidly preparing graphene powder by freeze filtration, which prepares graphene into a suspension and then rapidly prepares the powder in a dry form, but since graphene and Ti₃C₂Ceramics belong to two different materials with different physical properties (i.e. dispersibility, interaction between solids, hydrodynamic state, rheological behavior) necessitating different drying processes, different pairs of drying processes, different process properties of the powder, and drying processes not disclosed in this document.

Disclosure of Invention

The invention provides a method for efficiently preparing stable Ti in short time₃C₂Powder method is favorable for promoting Ti₃C₂Rapid development in future research.

The technical scheme adopted by the invention is as follows:

ti₃C₂The preparation method of the powder comprises the following steps:

(1) with Ti₃AlC₂Etching ceramic powder serving as a raw material in water bath;

(2) adjusting the pH value of the solution to make the solution neutral;

(3) the solution is centrifugally dispersed and ultrasonically stripped to obtain Ti₃C₂A nanosuspension;

(4) mixing the above Ti₃C₂The nanometer suspension is rapidly dried by a spray dryer, the temperature of an air inlet is 180 ℃, the temperature of an air outlet is 80 ℃, and the feeding speed is 300 ml/h.

As a preferred technical scheme, few layers or single-layer Ti is obtained by centrifugal dispersion and ultrasonic stripping for a plurality of times in the step (3)₃C₂And (4) nano suspension.

As a preferable technical proposal, 400-mesh Ti is used₃AlC₂Ceramic powder is used as raw material.

As a preferred technical scheme, the etching agent is hydrochloric acid with the concentration of 36 percent and LiF; hydrochloric acid and LiF and Ti₃AlC₂The ratio of the ceramics is 30: 1.89: 0.1-2.

As a preferred technical scheme, the etching agent is hydrochloric acid with the concentration of 36 percent and LiF; hydrochloric acid and LiF and Ti₃AlC₂The ratio of the ceramics is 30: 1.89: 1.5.

As a preferred technical scheme, the water bath etching temperature is 40 ℃, and the time is 24 h.

As a preferable technical scheme, deionized water is used for washing in the step (2) until the supernatant is neutral. The invention has the beneficial effects that:

simple process, low cost and high safety. The invention uses Ti₃AlC₂The ceramic powder is used as raw material, and HF is extremely toxic, so that HCl and LiF are used for replacing HF to etch Ti₃AlC₂The safety in the experimental process is improved. Then Ti can be obtained by simple processes such as centrifugal dispersion, ultrasonic oscillation and the like₃C₂And (3) suspension.

The powder has high preparation yield and time-saving preparation process. Prepared Ti₃C₂The suspension is quickly dried by a small spray dryer, and Ti with uniform granularity can be prepared due to uniform liquid and good fluidity₃C₂High powder yield and high output.

The etching agent is acid solution and fluorine salt. HF is a strong corrosive acid, which is harmful to human bodies and the environment and can not ensure the safety of the experimental process; secondly, the nano-sheets prepared by HF contain a certain amount of defects, such as holes; the mixed etching of LiF and HCl can avoid the defects, and meanwhile, the Ti3C2 has good layering effect and is easy to strip.

The etchant was 30ml of 36% hydrochloric acid and 1.89g of LiF. The HCl and LiF react to generate HF, hydrofluoric acid is used as weak electrolyte and cannot be completely ionized, and the HCl added into the HF solution can improve the hydrogen ion concentration and the anion electrolysis efficiency of the solution. The concentration of hydrochloric acid also has a large influence, and if the concentration is too low, part of Ti is still remained₃AlC₂No corrosion, small space between the layers and large thickness of the layers; too high a concentration increases the acidity of the entire solution, resulting in a smaller specific surface area of the corrosion product lamellae and a smaller interlayer spacing of the obtained corrosion products.

Drawings

FIG. 1 shows Ti prepared in example 1₃C₂X-ray diffraction pattern of the powder.

FIG. 2 shows Ti prepared in example 1₃C₂Scanning electron microscope images of (a).

Detailed Description

The invention is further described below by means of specific embodiments, which may be varied otherwise without departing from the invention

The description is given for the details of the features, and all changes which come within the meaning and range of equivalency of the invention are therefore intended to be embraced therein.