CN106185937A - A kind of preparation method of carbon nano-particle/two-dimensional layer titanium carbide composite - Google Patents
A kind of preparation method of carbon nano-particle/two-dimensional layer titanium carbide composite Download PDFInfo
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- CN106185937A CN106185937A CN201610551496.0A CN201610551496A CN106185937A CN 106185937 A CN106185937 A CN 106185937A CN 201610551496 A CN201610551496 A CN 201610551496A CN 106185937 A CN106185937 A CN 106185937A
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- particle
- mxene
- carbon nano
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- titanium carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The present invention relates to the preparation method of a kind of carbon nano-particle/two-dimensional layer titanium carbide composite, including: two-dimensional layer titanium carbide nano material MXene (Ti3C2/Ti2C) Fluohydric acid. corrosion preparation；Through step process raw material MXene (Ti such as ultrasonic, vacuum impregnation, hydro-thermals3C2/Ti2C) and monosaccharide, make carbon nano-particle at MXene (Ti3C2/Ti2C) material interlayer and Surface Creation, i.e. obtains carbon nano-particle/two-dimensional layer titanium carbide composite.The present invention uses the nontoxic raw material that is easy to get, and preparation process is simple, and technique is controlled, low cost, reproducible, the two-dimensional layer MXene (Ti prepared3C2/Ti2C) lamellar structure is uniformly complete, and carbon nano-particle is at MXene (Ti3C2/Ti2C) material interlayer is uniform with surface distributed, and it is big that the composite prepared has specific surface area, the features such as conduction property is good, and hydrophilic physical property is good；Can apply in fields such as function ceramics, absorbing material, ultracapacitor, ion batteries.
Description
Technical field
The invention belongs to nano-functional material preparing technical field, be specifically related to a kind of carbon nano-particle/two-dimensional layer carbon
Change the preparation method of titanium composite material.
Background technology
MXene in reported first in 2011, mainly passes through oxygen fluoric acid selective as a class New Two Dimensional nano material
The A composition that corrosion removes in raw material MAX phase prepares.MXene is a kind of novel transition metal carbide two-dimensional material, has
Class graphene-structured, due to the two-dimensional layered structure of its uniqueness, bigger specific surface area, good capacitive character and hydrophilic, makes
It has had Preliminary Applications in function ceramics, absorbing material, ultracapacitor, the field such as ion battery.Carbon nanomaterial has low
Density, high intensity, high-specific surface area, excellent thermally and chemically stability and good electrochemical properties, become related personnel
Study hotspot.Due to special shape and size, carbon nano-particle is introduced in other materials as the modified material that strengthens,
It is widely used in inhaling the fields such as ripple, absorption, catalysis, electrochemistry.
MXene material itself has obtained relatively broad research, but MXene material behavior is single, surface defect is more, layer
The shortcomings such as spacing is little limit the further application of this material.Carbon nanomaterial is incorporated into MXene material interlayer and surface energy
Enough greatly increase its specific surface area, improve the utilization rate of MXene lamella further；Gained composite has carbon nanomaterial concurrently
Characteristic, can strengthen MXene materials conductive character and dielectric property, expands the application space of MXene material.
Although present stage develops swift and violent about the related work of MXene, but the most few about its work assembled, by carbon
Nano material is incorporated in Mxene material not yet patent report.
Summary of the invention
Solve the technical problem that
In place of the deficiencies in the prior art, it is multiple that the present invention proposes a kind of carbon nano-particle/two-dimensional layer titanium carbide
The preparation method of condensation material, for MXene (Ti3C2/Ti2C) material behavior is single, surface defect is more, interlamellar spacing is little etc. lacks
Point.
Technical scheme
The preparation method of a kind of carbon nano-particle/two-dimensional layer titanium carbide composite, it is characterised in that step is as follows:
Step 1: being immersed in by MAX ceramic powder in the HF solution that mass fraction is 10～40wt%, MAX concentration is 0.05
～0.1g/ml；Then magnetic agitation reaction 10～120h under temperature 20～65 DEG C；
Using deionized water centrifuge washing is 7 to solution ph, and 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: be placed in monosaccharide solutions by MXene, ultrasonic disperse 0.5～24h, dipping 2～10h obtains under vacuum
To mixed solution；
Described monosaccharide solutions be concentration be the monosaccharide solutions of 0.1～1mol/L；Described MXene and monosaccharide mass ratio are 0.1
～2；
Step 3: imported by mixed solution in hydrothermal reaction kettle inner bag, is warming up to 150～220 DEG C, is incubated 2～20h, reaction
Naturally cool to room temperature after end and be precipitated product；Described reactor inner bag compactedness is 60～80%；
Step 4: be 7 to solution ph by gained precipitated product deionized water centrifuge washing, vacuum filtration obtains solid-state
Sample, is vacuum dried 8～40h at 40～100 DEG C, i.e. obtains carbon nano-particle and is distributed in interlayer and the surface of MXene material
Carbon nano-particle/two-dimensional layer titanium carbide composite.
Described monosaccharide solutions uses ultrasonic disperse to obtain uniform monosaccharide solutions.
Described monosaccharide can be fructose or glucose.
MAX ceramic powder particle diameter used is 0.1～30 μm, purity >=98%.
When MAX ceramic powder is Ti3AlC2Or Ti2During AlC, the binary stratified nano materials Mxene obtained is Ti3C2Or
Ti2C。
Beneficial effect
The preparation method of a kind of carbon nano-particle/two-dimensional layer titanium carbide composite that the present invention proposes, uses hydro-thermal
Method by carbon nano-particle at MXene (Ti3C2/Ti2C) material interlayer and Surface Creation, including: two-dimensional layer titanium carbide nanometer material
Material MXene (Ti3C2/Ti2C) Fluohydric acid. corrosion preparation；Through step process raw material MXene such as ultrasonic, vacuum impregnation, hydro-thermals
(Ti3C2/Ti2C) and monosaccharide, make carbon nano-particle at MXene (Ti3C2/Ti2C) material interlayer and Surface Creation, i.e. obtains carbon and receives
Rice grain/two-dimensional layer titanium carbide composite.Its method is the most efficiently suitable for a large amount of preparation.The composite obtained enhances
Single MXene (Ti3C2/Ti2C) mechanical property of material, improves its structural stability；Composite effectively increases MXene
(Ti3C2/Ti2C) specific surface area of material, and make it have the special nature of carbon nanomaterial concurrently, there is more excellent Jie
Electricity and electrochemical properties.Therefore the performance of carbon nano-particle/two-dimensional layer titanium carbide nano composite material is better than single MXene
(Ti3C2/Ti2C) material, its application will be more extensive.
The composite prepared by the method compensate for single MXene (Ti3C2/Ti2C) shortcoming of material, has two dimension concurrently
Nano titanium carbide material and the characteristic of carbon nanomaterial.The method has that advantages of nontoxic raw materials is pollution-free, with low cost, preparation technology is simple
Single, react the advantage such as controlled.
Accompanying drawing explanation
Fig. 1 is the process chart of the inventive method
Fig. 2 (a) is the SEM collection of illustrative plates of MXene；Fig. 2 (b) is the SEM collection of illustrative plates of MXene load carbon nano-particle
Detailed description of the invention
In conjunction with embodiment, accompanying drawing, the invention will be further described:
Embodiment one
The present embodiment comprises the following steps:
(1) 10g Ti is weighed3AlC2Ceramic powder, being immersed in 200ml concentration is that in 40wt%HF solution, under room temperature, magnetic force stirs
Mix reaction 80h；Being washed with deionized by gained solution and be about 7 to pH, sucking filtration becomes solid powder, 80 DEG C of vacuum drying 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 water, ultrasonic disperse 5h, it is thus achieved that monosaccharide solutions；By 0.63g
The two-dimensional layer material MXene (Ti that step 2 is obtained3C2) join among the glucose solution prepared, ultrasonic disperse
24h, vacuum impregnation 10h；
(3) solution impregnated is placed in hydrothermal reaction kettle at 180 DEG C reaction 6h, described reactor inner bag compactedness
It is 60～80%；
(4) to solution ph, products therefrom deionized water centrifuge washing being about 7, vacuum filtration obtains solid sample,
It is vacuum dried 40h at 100 DEG C, i.e. obtains carbon nano-particle/two-dimensional layer titanium carbide composite.Its pattern such as Fig. 2 (b) institute
Show.
Embodiment two
The present embodiment comprises the following steps:
(1) 1g Ti is weighed2AlC ceramic powder, being immersed in 10ml concentration is magnetic agitation at 40 DEG C in 10wt%HF solution
Reaction 10h；Being washed with deionized by gained solution and be about 7 to pH, sucking filtration becomes solid powder, 40 DEG C of vacuum drying 8h, to obtain final product
To MXene (Ti2C) nano material.
(2) taking 5g glucose to be dissolved in 30ml deionized water, ultrasonic disperse 0.5h, it is thus achieved that glucose solution, by 0.5g
The two-dimensional layer material MXene (Ti that step 2 is obtained2C) join among the glucose solution prepared, ultrasonic disperse
0.5h, vacuum impregnation 4h；
(3) solution impregnated is placed in hydrothermal reaction kettle at 150 DEG C reaction 10h；Described reactor inner bag is filled
Degree is 60～80%；
(4) to solution ph, products therefrom deionized water centrifuge washing being about 7, vacuum filtration obtains solid sample,
It is vacuum dried 8h at 80 DEG C, i.e. obtains carbon nano-particle/two-dimensional layer titanium carbide composite.
Embodiment three
The present embodiment comprises the following steps:
(1) 20g Ti is weighed3AlC2Ceramic powder, being immersed in 400ml concentration is that in 30wt%HF solution, at 65 DEG C, magnetic force stirs
Mix reaction 120h；Being washed with deionized by gained solution and be about 7 to pH, sucking filtration becomes solid powder, 60 DEG C of vacuum drying 24h,
I.e. obtain MXene (Ti3C2) nano material.
(2) take 4g fructose to be dissolved in 30ml deionized water, ultrasonic disperse 2h, it is thus achieved that fructose soln, by 1g step 2 institute
The two-dimensional layer material MXene (Ti obtained3C2) join among the fructose soln prepared, ultrasonic disperse 10h, vacuum impregnation
2h；
(3) solution impregnated is placed in hydrothermal reaction kettle at 220 DEG C reaction 20h；Described reactor inner bag is filled
Degree is 60～80%；
(4) to solution ph, products therefrom deionized water centrifuge washing being about 7, vacuum filtration obtains solid sample,
It is vacuum dried 20h at 100 DEG C, i.e. obtains carbon nano-particle/two-dimensional layer titanium carbide composite.
Embodiment four
The present embodiment comprises the following steps:
(1) 10g Ti is weighed2AlC ceramic powder, being immersed in 200ml concentration is that in 20wt%HF solution, at 20 DEG C, magnetic force stirs
Mix reaction 20h；Being washed with deionized by gained solution and be about 7 to pH, sucking filtration becomes solid powder, 50 DEG C of vacuum drying 30h, i.e.
Obtain MXene (Ti2C) nano material.
(2) take 4g fructose to be dissolved in 60ml deionized water, ultrasonic disperse 2h, it is thus achieved that fructose soln；By 2g step 2 institute
The two-dimensional layer material MXene (Ti obtained2C) join among the fructose soln prepared, ultrasonic disperse 10h, vacuum impregnation
5h；
(3) solution impregnated is placed in hydrothermal reaction kettle at 200 DEG C reaction 20h；Described reactor inner bag is filled
Degree is 60～80%；
(4) to solution ph, products therefrom deionized water centrifuge washing being about 7, vacuum filtration obtains solid sample,
It is vacuum dried 20h at 70 DEG C, i.e. obtains carbon nano-particle/two-dimensional layer titanium carbide composite.
Claims (5)
1. the preparation method of carbon nano-particle/two-dimensional layer titanium carbide composite, it is characterised in that step is as follows:
Step 1: MAX ceramic powder is immersed in the HF solution that mass fraction is 10～40wt%, MAX concentration be 0.05～
0.1g/ml；Then magnetic agitation reaction 10～120h under temperature 20～65 DEG C；
Using deionized water centrifuge washing is 7 to solution ph, and vacuum filtration obtains solid matter, 40～80 DEG C of vacuum drying 8
～40h, obtain binary stratified nano materials MXene；
Step 2: be placed in monosaccharide solutions by MXene, ultrasonic disperse 0.5～24h, dipping 2～10h is mixed under vacuum
Close solution；
Described monosaccharide solutions be concentration be the monosaccharide solutions of 0.1～1mol/L；Described MXene and monosaccharide mass ratio are 0.1～2；
Step 3: imported by mixed solution in hydrothermal reaction kettle inner bag, is warming up to 150～220 DEG C, is incubated 2～20h, and reaction terminates
After naturally cool to room temperature and be precipitated product；Described reactor inner bag compactedness is 60～80%；
Step 4: be 7 to solution ph by gained precipitated product deionized water centrifuge washing, vacuum filtration obtains solid sample,
It is vacuum dried 8～40h at 40～100 DEG C, i.e. obtains carbon nano-particle and be distributed in the interlayer of MXene material and the carbon nanometer on surface
Granule/two-dimensional layer titanium carbide composite.
The most according to claim 1, the preparation method of carbon nano-particle/two-dimensional layer titanium carbide composite, its feature exists
In: described monosaccharide solutions uses ultrasonic disperse to obtain uniform monosaccharide solutions.
The most according to claim 1, the preparation method of carbon nano-particle/two-dimensional layer titanium carbide composite, its feature exists
In: described monosaccharide can be fructose or glucose.
The preparation method of carbon nano-particle the most according to claim 1/two-dimensional layer titanium carbide composite, its feature exists
In: MAX ceramic powder particle diameter used is 0.1～30 μm, purity >=98%.
5., according to the preparation method of the carbon nano-particle described in claim 1 or 4/two-dimensional layer titanium carbide composite, it is special
Levy and be: when MAX ceramic powder is Ti3AlC2Or Ti2During AlC, the binary stratified nano materials Mxene obtained is Ti3C2Or
Ti2C。
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