CN106185937B - A kind of preparation method of carbon nano-particle/two-dimensional layer carbonization titanium composite material - Google Patents

A kind of preparation method of carbon nano-particle/two-dimensional layer carbonization titanium composite material Download PDF

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CN106185937B
CN106185937B CN201610551496.0A CN201610551496A CN106185937B CN 106185937 B CN106185937 B CN 106185937B CN 201610551496 A CN201610551496 A CN 201610551496A CN 106185937 B CN106185937 B CN 106185937B
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particle
mxene
carbon nano
dimensional layer
composite material
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CN106185937A (en
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殷小玮
李新亮
韩美康
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases

Abstract

The present invention relates to a kind of preparation method of carbon nano-particle/two-dimensional layer carbonization titanium composite material, including:Two-dimensional layer titanium carbide nano material MXene (Ti3C2/Ti2It is prepared by hydrofluoric acid corrosion C);Through the step process raw material MXene such as ultrasound, vacuum impregnation, hydro-thermal (Ti3C2/Ti2C) and monose, carbon nano-particle is made in MXene (Ti3C2/Ti2C) material interlayer and Surface Creation, that is, carbon nano-particle/two-dimensional layer carbonization titanium composite material is obtained.The present invention uses the nontoxic raw material that is easy to get, and preparation process is simple, and technique is controllable, and cost is low, reproducible, the two-dimensional layer MXene (Ti being prepared3C2/Ti2C lamellar structure) is uniformly complete, and carbon nano-particle is in MXene (Ti3C2/Ti2C) material interlayer is uniform with surface distributed, and the composite being prepared has the features such as specific surface area is big, and conduction property is good, and hydrophilic physical property is good;It can apply in fields such as function ceramics, absorbing material, ultracapacitor, ion batteries.

Description

A kind of preparation method of carbon nano-particle/two-dimensional layer carbonization titanium composite material
Technical field
The invention belongs to nano-functional material preparing technical field, more particularly to a kind of carbon nano-particle/two-dimensional layer carbon Change the preparation method of titanium composite material.
Background technology
MXene was reported first as a kind of New Two Dimensional nano material in 2011, mainly passed through oxygen fluoric acid selectivity The A compositions that corrosion is removed in raw material MAX phases are prepared.MXene is a kind of novel transition metal carbide two-dimensional material, is had Class graphene-structured, due to its unique two-dimensional layered structure, larger specific surface area, good capacitive character and hydrophily, make It has Preliminary Applications in fields such as function ceramics, absorbing material, ultracapacitor, ion batteries.Carbon nanomaterial has low Density, high intensity, high-specific surface area, excellent thermally and chemically stability and good electrochemical properties, turn into related personnel Study hotspot.Due to special shape and size, carbon nano-particle is introduced in other materials as enhancing material is modified, It is widely used in inhaling ripple, adsorbs, is catalyzed, the field such as electrochemistry.
MXene materials have obtained relatively broad research in itself, but MXene material properties are single, surface defect is more, layer The shortcomings of spacing is small limits further applying for the material.Carbon nanomaterial is incorporated into MXene materials interlayer and surface energy Its specific surface area is enough greatly increased, further improves the utilization rate of MXene lamellas;Gained composite has carbon nanomaterial concurrently Characteristic, MXene materials conductives property and dielectric property can be strengthened, expand the application space of MXene materials.
Although the related work development at this stage on MXene is swift and violent, the work assembled on it is simultaneously few, by carbon Nano material is incorporated into Mxene materials that there has been no patent report.
The content of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes that a kind of carbon nano-particle/two-dimensional layer titanium carbide is answered The preparation method of condensation material, for MXene (Ti3C2/Ti2C) material property is single, surface defect is more, interlamellar spacing is small etc. lacks Point.
Technical scheme
The preparation method of a kind of carbon nano-particle/two-dimensional layer carbonization titanium composite material, it is characterised in that step is as follows:
Step 1:MAX ceramic powders are immersed in the HF solution that mass fraction is 10~40wt%, MAX concentration is 0.05 ~0.1g/ml;Then magnetic agitation reacts 10~120h under 20~65 DEG C of temperature;
Use deionized water centrifuge washing to solution ph for 7, vacuum filtration obtains solid matter, and 40~80 DEG C of vacuum are done Dry 8~40h, obtain binary stratified nano materials MXene;
Step 2:MXene is placed in monosaccharide solutions, 0.5~24h of ultrasonic disperse, impregnates 2~10h under vacuum and obtain To mixed solution;
The monosaccharide solutions are the monosaccharide solutions that concentration is 0.1~1mol/L;The MXene is 0.1 with monose mass ratio ~2;
Step 3:Mixed solution is imported in hydrothermal reaction kettle inner bag, is warming up to 150~220 DEG C, is incubated 2~20h, reaction Room temperature is naturally cooled to after end and obtains precipitated product;The reactor inner bag compactedness is 60~80%;
Step 4:It is 7 by gained precipitated product deionized water centrifuge washing to solution ph, vacuum filtration obtains solid-state Sample, 8~40h are dried in vacuo at 40~100 DEG C, that is, obtain interlayer and surface that carbon nano-particle is distributed in MXene materials Carbon nano-particle/two-dimensional layer carbonization titanium composite material.
The monosaccharide solutions obtain uniform monosaccharide solutions using ultrasonic disperse.
The monose can be fructose or glucose.
MAX ceramic powders particle diameter used is 0.1~30 μm, purity >=98%.
When MAX ceramic powders are Ti3AlC2Or Ti2During AlC, obtained binary stratified nano materials Mxene is Ti3C2Or Ti2C。
Beneficial effect
The preparation method of a kind of carbon nano-particle proposed by the present invention/two-dimensional layer carbonization titanium composite material, using hydro-thermal Method is by carbon nano-particle in MXene (Ti3C2/Ti2C) material interlayer and Surface Creation, including:Two-dimensional layer titanium carbide nanometer material Expect MXene (Ti3C2/Ti2It is prepared by hydrofluoric acid corrosion C);Through the step process raw material such as ultrasound, vacuum impregnation, hydro-thermal MXene (Ti3C2/Ti2C) and monose, carbon nano-particle is made in MXene (Ti3C2/Ti2C) material interlayer and Surface Creation, that is, obtain carbon and receive Rice grain/two-dimensional layer carbonization titanium composite material.Its method is simply efficiently adapted to a large amount of prepare.The composite of acquisition enhances Single MXene (Ti3C2/Ti2C) the mechanical property of material, its structural stability is improved;Composite effectively increases MXene (Ti3C2/Ti2C) the specific surface area of material, and it is had the special nature of carbon nanomaterial concurrently, with more excellent Jie Electricity and electrochemical properties.Therefore the performance of carbon nano-particle/two-dimensional layer carbonization titanium nanometer composite material is better than single MXene (Ti3C2/Ti2C) material, its application will be more extensive.
The composite prepared by this method compensate for single MXene (Ti3C2/Ti2C) the shortcomings that material, two dimension is had concurrently The characteristic of nano titanium carbide material and carbon nanomaterial.This method has that advantages of nontoxic raw materials is pollution-free, cost is cheap, preparation technology is simple The advantages that list, controllable reaction.
Brief description of the drawings
Fig. 1 is the process chart of the inventive method
Fig. 2 (a) is MXene SEM spectrum;Fig. 2 (b) is the SEM spectrum that MXene loads carbon nano-particle
Embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described:
Embodiment one
The present embodiment comprises the following steps:
(1) 10g Ti are weighed3AlC2Ceramic powder, it is immersed in 200ml concentration and is stirred for magnetic force under normal temperature in 40wt%HF solution Mix reaction 80h;It is about 7 that resulting solution, which is washed with deionized to pH, filters into solid powder, and 80 DEG C are dried in vacuo 40h, i.e., Obtain MXene (Ti3C2) nano material.Shown in its pattern such as Fig. 2 (a).
(2) take 1.26g glucose to be dissolved in 70ml deionized waters, ultrasonic disperse 5h, obtain monosaccharide solutions;By 0.63g The two-dimensional layer material MXene (Ti that step 2 is obtained3C2) be added among the glucose solution prepared, ultrasonic disperse 24h, vacuum impregnation 10h;
(3) solution impregnated is placed in hydrothermal reaction kettle at 180 DEG C and reacts 6h, the reactor inner bag compactedness For 60~80%;
(4) it is about 7 with deionized water centrifuge washing to solution ph by products therefrom, vacuum filtration obtains solid sample, 40h is dried in vacuo at 100 DEG C, that is, obtains carbon nano-particle/two-dimensional layer carbonization titanium composite material.Its pattern such as Fig. 2 (b) institutes Show.
Embodiment two
The present embodiment comprises the following steps:
(1) 1g Ti are weighed2AlC ceramic powders, 10ml concentration is immersed in as magnetic agitation at 40 DEG C in 10wt%HF solution React 10h;It is about 7 that resulting solution, which is washed with deionized to pH, filters into solid powder, 40 DEG C of vacuum drying 8h, produces To MXene (Ti2C) nano material.
(2) take 5g glucose to be dissolved in 30ml deionized waters, ultrasonic disperse 0.5h, glucose solution is obtained, by 0.5g The two-dimensional layer material MXene (Ti that step 2 is obtained2C) it is added among the glucose solution prepared, ultrasonic disperse 0.5h, vacuum impregnation 4h;
(3) solution impregnated is placed in hydrothermal reaction kettle and reacts 10h at 150 DEG C;The reactor inner bag filling Spend for 60~80%;
(4) it is about 7 with deionized water centrifuge washing to solution ph by products therefrom, vacuum filtration obtains solid sample, 8h is dried in vacuo at 80 DEG C, that is, obtains carbon nano-particle/two-dimensional layer carbonization titanium composite material.
Embodiment three
The present embodiment comprises the following steps:
(1) 20g Ti are weighed3AlC2Ceramic powder, it is that magnetic force stirs at 65 DEG C in 30wt%HF solution to be immersed in 400ml concentration Mix reaction 120h;It is about 7 that resulting solution, which is washed with deionized to pH, filters into solid powder, and 60 DEG C are dried in vacuo 24h, Obtain MXene (Ti3C2) nano material.
(2) take 4g fructose to be dissolved in 30ml deionized waters, ultrasonic disperse 2h, fructose soln is obtained, by 1g step 2 institute The two-dimensional layer material MXene (Ti of acquisition3C2) be added among the fructose soln prepared, ultrasonic disperse 10h, vacuum impregnation 2h;
(3) solution impregnated is placed in hydrothermal reaction kettle and reacts 20h at 220 DEG C;The reactor inner bag filling Spend for 60~80%;
(4) it is about 7 with deionized water centrifuge washing to solution ph by products therefrom, vacuum filtration obtains solid sample, 20h is dried in vacuo at 100 DEG C, that is, obtains carbon nano-particle/two-dimensional layer carbonization titanium composite material.
Embodiment four
The present embodiment comprises the following steps:
(1) 10g Ti are weighed2AlC ceramic powders, it is that magnetic force stirs at 20 DEG C in 20wt%HF solution to be immersed in 200ml concentration Mix reaction 20h;It is about 7 that resulting solution, which is washed with deionized to pH, filters into solid powder, and 50 DEG C are dried in vacuo 30h, i.e., Obtain MXene (Ti2C) nano material.
(2) take 4g fructose to be dissolved in 60ml deionized waters, ultrasonic disperse 2h, obtain fructose soln;By 2g step 2 institute The two-dimensional layer material MXene (Ti of acquisition2C) it is added among the fructose soln prepared, ultrasonic disperse 10h, vacuum impregnation 5h;
(3) solution impregnated is placed in hydrothermal reaction kettle and reacts 20h at 200 DEG C;The reactor inner bag filling Spend for 60~80%;
(4) it is about 7 with deionized water centrifuge washing to solution ph by products therefrom, vacuum filtration obtains solid sample, 20h is dried in vacuo at 70 DEG C, that is, obtains carbon nano-particle/two-dimensional layer carbonization titanium composite material.

Claims (5)

1. the preparation method of a kind of carbon nano-particle/two-dimensional layer carbonization titanium composite material, it is characterised in that step is as follows:
Step 1:MAX ceramic powders are immersed in the HF solution that mass fraction is 10~40wt%, the concentration of MAX ceramic powders For 0.05~0.1g/ml;Then magnetic agitation reacts 10~120h under 20~65 DEG C of temperature;
Use deionized water centrifuge washing to solution ph for 7, vacuum filtration obtains solid matter, 40~80 DEG C of vacuum drying 8 ~40h, obtain binary stratified nano materials MXene;
Step 2:MXene is placed in monosaccharide solutions, 0.5~24h of ultrasonic disperse, impregnates 2~10h under vacuum and mixed Close solution;
The monosaccharide solutions are the monosaccharide solutions that concentration is 0.1~1mol/L;The MXene is 0.1~2 with monose mass ratio;
Step 3:Mixed solution is imported in hydrothermal reaction kettle inner bag, is warming up to 150~220 DEG C, is incubated 2~20h, reaction terminates After naturally cool to room temperature and obtain precipitated product;The reactor inner bag compactedness is 60~80%;
Step 4:It is 7 by gained precipitated product deionized water centrifuge washing to solution ph, vacuum filtration obtains solid sample, 8~40h is dried in vacuo at 40~100 DEG C, that is, obtains carbon nano-particle and is distributed in the interlayer of MXene materials and the carbon nanometer on surface Particle/two-dimensional layer carbonization titanium composite material.
2. the preparation method of carbon nano-particle/two-dimensional layer carbonization titanium composite material, its feature exist according to claim 1 In:The monosaccharide solutions obtain uniform monosaccharide solutions using ultrasonic disperse.
3. the preparation method of carbon nano-particle/two-dimensional layer carbonization titanium composite material, its feature exist according to claim 1 In:The monose is fructose or glucose.
4. the preparation method of carbon nano-particle according to claim 1/two-dimensional layer carbonization titanium composite material, its feature exist In:MAX ceramic powders particle diameter used is 0.1~30 μm, purity >=98%.
5. the preparation method of carbon nano-particle/two-dimensional layer carbonization titanium composite material according to claim 1 or 4, it is special Sign is:When MAX ceramic powders are Ti3AlC2Or Ti2During AlC, obtained binary stratified nano materials Mxene is Ti3C2Or Ti2C。
CN201610551496.0A 2016-07-13 2016-07-13 A kind of preparation method of carbon nano-particle/two-dimensional layer carbonization titanium composite material Expired - Fee Related CN106185937B (en)

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