CN105536834B - The precipitation method prepare ceria/two-dimensional layer carbonization titanium composite material method - Google Patents
The precipitation method prepare ceria/two-dimensional layer carbonization titanium composite material method Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/035—Precipitation on carriers
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- B82—NANOTECHNOLOGY
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention provides the precipitation method to prepare ceria/two-dimensional layer carbonization titanium composite material method, comprising: the ternary layered Ti of high-purity3AlC2The high-energy ball milling of powder refines crystal grain；Two-dimensional layer nano material MXene-Ti3C2Hydrofluoric acid corrode preparation；The precipitation method make MXene-Ti3C2Surface and interlayer form CeO2, it is made to load MXene-Ti3C2To get CeO2/MXene‑Ti3C2Nanocomposite；The present invention has preparation process simple, and technique is controllable, at low cost, has two-dimensional layer MXene-Ti3C2Lamella it is uniform, CeO2The features such as being evenly distributed, large specific surface area, electric conductivity is good, and photocatalytic is good, is conducive to the application in fields such as photocatalysis, lithium ion battery, supercapacitors.
Description
Technical field
The invention belongs to inorganic nano composite material technical field, in particular to the precipitation method prepare ceria/two-dimensional layer
The method of shape carbonization titanium composite material.
Background technique
Ternary layered ceramic material Ti3AlC2Belong to stratiform hexagonal crystallographic texture.In Ti3AlC2In crystal structure, Ti and C
Atom forms Ti6C is octahedra, is separated by Al layers, C atom is located at octahedral center, and C and Ti atom is combined into strongly covalent
Key, and between Ti-Ti and Ti and Al it is weak binding, it is combined similar to the Van der Waals force weak bond between graphite.
Ti3AlC2The performance of metal and ceramics is had both, at normal temperature, with heating conduction and electric conductivity and lower
Vickers microhardness and higher elasticity modulus, can be machined as metal, and at a higher temperature
With plasticity, while but also with higher yield strength, high-melting-point, the property of the ceramics such as high thermal stability and good inoxidizability
Energy.
Two-dimensional layer nano-carbide is the material of a type graphene-structured, due to its unique two-dimensional layered structure,
Biggish specific surface area, good electric conductivity and hydrophily, it is good magnetic and make it have superpower catalytic performance, photovoltaic
Can and chemical property, function ceramics, photocatalysis, lithium ion battery, solar battery, in terms of obtain
It is widely applied.
Nano ceric oxide is a kind of important rare-earth oxide.Nano-cerium oxide has good oxidationreduction
Performance and Oxygen storage capacity can be used as the three-way catalyst in vehicle maintenance service.Nano-cerium oxide has unique 4f electronics energy
Level structure can be used as ultraviolet absorbing agent.Nano-cerium oxide can be used as solid fuel cell electrolyte because of its stable crystal form.
Existing MXene-Ti3C2, performance is single, and surface area is smaller, and application range is relatively narrow, and is not suitable for mass production
The characteristics of.
Summary of the invention
In order to overcome the defects of the prior art described above, the purpose of the present invention is to provide the precipitation method to prepare ceria/bis-
The method for tieing up stratiform carbonization titanium composite material, the specific surface area of the composite material after having load is bigger, is suitble to a large amount of preparations, property
Can be high, the characteristics of being more widely applied.
To achieve the goals above, the technical solution adopted by the present invention is that:
The precipitation method prepare ceria/two-dimensional layer carbonization titanium composite material method, include the following steps:
Step 1 refines powder
It is greater than the ternary layered Ti of 97wt% using high-energy ball milling refinement purity3AlC2Ceramic powder, ball milling condition: ballstone,
The mass ratio of mixing and ball-milling medium is 10:1:1, rotational speed of ball-mill 350r/min, High Energy Ball Milling Time 2h, then by gained
Solid-liquid mixing is dried at 40 DEG C, obtains Ti3AlC2Ceramic powder；
Step 2, two-dimensional layer nano material MXene-Ti3C2Preparation
By gained Ti in step 13AlC2Ceramic powder is immersed in HF acid solution, wherein 5gTi3AlC2Powder is immersed in
80ml mass concentration is to react for 24 hours in 40wt%HF acid solution；Magnetic agitation, to Ti obtained by step 13AlC2Powder is corroded
After processing, it is 6 with deionized water eccentric cleaning to pH, by obtained solid sample drying at room temperature, obtains two-dimensional layer nano material
MXene-Ti3C2；
Step 3, precipitation method preparation
(1) cerous nitrate and MXene-Ti are controlled3C2Mass ratio be 2.2:1,4.4:1 or 8.8:1；Then configuration pH be 9~
11 ammonium hydroxide 10ml；
(2) by the MXene-Ti of 0.05g or 0.1g step (1)3C2It is dissolved separately in 50ml ultrapure water, is ultrasonically treated 2h,
Until being uniformly dispersed；
(3) cerous nitrate in step (1) is added in the solution of step (2), the concentration for controlling cerous nitrate solution is
0.02mol/l stirs 1h；
(4) take step (1) 10ml ammonium hydroxide that the magnetic agitation 2h in the solution of step (3) is added dropwise；By products therefrom centrifugation point
From taking lower layer's sediment fraction and cleaned respectively with dehydrated alcohol and deionized water；
(5) the resulting product of step (4) forced air drying in an oven is placed to handle, 40 DEG C hereinafter, heat preservation for 24 hours to get
CeO2/MXene-Ti3C2Nanocomposite.
The ball-milling medium is dehydrated alcohol.
Beneficial effects of the present invention:
Using precipitation method load C eO2To two-dimensional layer material MXene-Ti3C2On, carrying method is simple and effective, and is suitble to
A large amount of preparations.Composite material its specific surface area after load is bigger, and has CeO2Some characteristics, such as photocatalysis, shape
Looks multiplicity etc., therefore CeO2/MXene-Ti3C2The performance of nanocomposite is better than single MXene-Ti3C2, application will
More extensively.Due to graphene-supported CeO2 nano particle composite material capacitor with higher, preferable photocatalysis performance, and
MXene-Ti3C2 is class graphene-structured, for further in supercapacitor, lithium ion battery, photocatalysis, biosensor etc.
The preparation work of predecessor has been carried out in the application in field.
The present invention is by Ti3AlC2Chemical etching is carried out in HF acid, Al is etched away selectively, forms a kind of two-dimensional layer
Shape material MXene-Ti3C2, then using the precipitation method in two-dimensional layer material MXene-Ti3C2Upper load C eO2, make stratified material
Specific surface area increase, and make material have photocatalytic degradation, one's own physical property, the characteristics such as pattern multiplicity, therefore, CeO2/
MXene-Ti3C2The performance of nanocomposite is better than single MXene-Ti3C2, application will more extensively.
Detailed description of the invention
Fig. 1 is Ti3AlC2Before powder corrosion treatment, after corrosion treatment and load after product XRD spectrum.
Fig. 2 is Ti3AlC2The corrosion product MXene-Ti of powder3C2Sample after the 40 DEG C of air blast drying for 24 hours of baking oven low temperature
SEM figure.
Fig. 3 is to prepare CeO using the precipitation method2/MXene-Ti3C2Nano combined product is in the 40 DEG C of air blast drying of baking oven low temperature
Sample SEM figure after for 24 hours.
Specific embodiment
The present invention is described in further details below by embodiment.
From figure 3, it can be seen that CeO2It is evenly distributed in two-dimensional layer MXene-Ti3C2Surface and interlayer.
Embodiment 1
Step 1 refines powder
It is greater than the ternary layered Ti of 97wt% using high-energy ball milling refinement purity3AlC2Ceramic powder, ball milling condition: ballstone,
The mass ratio of mixing and dehydrated alcohol is 10:1:1, rotational speed of ball-mill 350r/min, High Energy Ball Milling Time 2h, then by gained
Solid-liquid mixing is dried at 40 DEG C, obtains Ti3AlC2Ceramic powder；
Step 2, two-dimensional layer nano material MXene-Ti3C2Preparation
By gained Ti in step 13AlC2Ceramic powder is immersed in HF acid solution, wherein 5gTi3AlC2Powder is immersed in
80ml mass concentration is to react for 24 hours in 40wt%HF acid solution；Magnetic agitation, to Ti obtained by step 13AlC2Powder is corroded
After processing, it is 6 with deionized water eccentric cleaning to pH, by obtained solid sample drying at room temperature, obtains two-dimensional layer nano material
MXene-Ti3C2；
Step 3, precipitation method preparation
(1) MXene-Ti is weighed3C20.05g, cerous nitrate 0.44g；Configure the ammonium hydroxide 10ml that pH is 9；
(2) by the MXene-Ti in step (1)3C2It is dissolved in 50ml ultrapure water, is ultrasonically treated 2h；
(3) cerous nitrate in step (1) is added in the solution of step (2), stirs 1h；
(4) ammonium hydroxide in step (1) is added dropwise in the solution of step (3), magnetic agitation 2h, it is heavy is then centrifuged for the portion of removing
Starch, and cleaned 5 times with dehydrated alcohol and deionized water respectively；
(5) step (4) products therefrom is placed in the 40 DEG C of forced air dryings of baking oven low temperature for 24 hours to get CeO2/MXene-Ti3C2
Nanocomposite.
Embodiment 2
Step 1 refines powder
It is greater than the ternary layered Ti of 97wt% using high-energy ball milling refinement purity3AlC2Ceramic powder, ball milling condition: ballstone,
The mass ratio of mixing and dehydrated alcohol is 10:1:1, rotational speed of ball-mill 350r/min, High Energy Ball Milling Time 2h, then by gained
Solid-liquid mixing is dried at 40 DEG C, obtains Ti3AlC2Ceramic powder；
Step 2, two-dimensional layer nano material MXene-Ti3C2Preparation
By gained Ti in step 13AlC2Ceramic powder is immersed in HF acid solution, wherein 5gTi3AlC2Powder is immersed in
80ml mass concentration is to react for 24 hours in 40wt%HF acid solution；Magnetic agitation, to Ti obtained by step 13AlC2Powder is corroded
After processing, it is 6 with deionized water eccentric cleaning to pH, by obtained solid sample drying at room temperature, obtains two-dimensional layer nano material
MXene-Ti3C2；
Step 3, precipitation method preparation
(1) MXene-Ti is weighed3C20.05g, cerous nitrate 0.44g；Configure the ammonium hydroxide 10ml that pH is 10；
(2) by the MXene-Ti in step (1)3C2It is dissolved in 50ml ultrapure water, is ultrasonically treated 2h；
(3) cerous nitrate in step (1) is added in the solution of step (2), stirs 1h；
(4) ammonium hydroxide in step (1) is added dropwise in the solution of step (3), magnetic agitation 2h is then centrifuged for sediment
Matter, and cleaned 5 times with dehydrated alcohol and deionized water respectively；
(5) step (4) products therefrom is placed in the 40 DEG C of forced air dryings of baking oven low temperature for 24 hours to get CeO2/MXene-Ti3C2
Nanocomposite.
Embodiment 3
Step 1 refines powder
It is greater than the ternary layered Ti of 97wt% using high-energy ball milling refinement purity3AlC2Ceramic powder, ball milling condition: ballstone,
The mass ratio of mixing and dehydrated alcohol is 10:1:1, rotational speed of ball-mill 350r/min, High Energy Ball Milling Time 2h, then by gained
Solid-liquid mixing is dried at 40 DEG C, obtains Ti3AlC2Ceramic powder；
Step 2, two-dimensional layer nano material MXene-Ti3C2Preparation
By gained Ti in step 13AlC2Ceramic powder is immersed in HF acid solution, wherein 5gTi3AlC2Powder is immersed in
80ml mass concentration is to react for 24 hours in 40wt%HF acid solution；Magnetic agitation, to Ti obtained by step 13AlC2Powder is corroded
After processing, it is 6 with deionized water eccentric cleaning to pH, by obtained solid sample drying at room temperature, obtains two-dimensional layer nano material
MXene-Ti3C2；
Step 3, precipitation method preparation
(1) MXene-Ti is weighed3C20.05g, cerous nitrate 0.44g；Configure the ammonium hydroxide 10ml that pH is 11；
(2) by the Mxene-Ti in step (1)3C2It is dissolved in 50ml ultrapure water, is ultrasonically treated 2h；
(3) cerous nitrate in step (1) is added in the solution of step (2), stirs 1h；
(4) ammonium hydroxide in step (1) is added dropwise in the solution of step (3), magnetic agitation 2h is then centrifuged for and uses respectively
Dehydrated alcohol and deionized water are cleaned 5 times；
(5) step (4) products therefrom is placed in the 40 DEG C of forced air dryings of baking oven low temperature for 24 hours to get CeO2/MXene-Ti3C2
Nanocomposite.
Embodiment 4
Step 1 refines powder
It is greater than the ternary layered Ti of 97wt% using high-energy ball milling refinement purity3AlC2Ceramic powder, ball milling condition: ballstone,
The mass ratio of mixing and dehydrated alcohol is 10:1:1, rotational speed of ball-mill 350r/min, High Energy Ball Milling Time 2h, then by gained
Solid-liquid mixing is dried at 40 DEG C, obtains Ti3AlC2Ceramic powder；
Step 2, two-dimensional layer nano material MXene-Ti3C2Preparation
By gained Ti in step 13AlC2Ceramic powder is immersed in HF acid solution, wherein 5gTi3AlC2Powder is immersed in
80ml mass concentration is to react for 24 hours in 40wt%HF acid solution；Magnetic agitation, to Ti obtained by step 13AlC2Powder is corroded
After processing, it is 6 with deionized water eccentric cleaning to pH, by obtained solid sample drying at room temperature, obtains two-dimensional layer nano material
MXene-Ti3C2；
Step 3, precipitation method preparation
(1) MXene-Ti is weighed3C20.1g, cerous nitrate 0.44g；Configure the ammonium hydroxide 10ml that pH is 9；
(2) by the MXene-Ti in step (1)3C2It is dissolved in 50ml ultrapure water, is ultrasonically treated 2h；
(3) cerous nitrate in step (1) is added in the solution of step (2), stirs 1h；
(4) ammonium hydroxide in step (1) is added dropwise in the solution of step (3), magnetic agitation 2h, is then centrifuged for taking lower layer heavy
Shallow lake part, and cleaned 5 times with dehydrated alcohol and deionized water respectively；
(5) step (4) products therefrom is placed in the 40 DEG C of forced air dryings of baking oven low temperature for 24 hours to get CeO2/MXene-Ti3C2
Nanocomposite.
Embodiment 5
Step 1 refines powder
It is greater than the ternary layered Ti of 97wt% using high-energy ball milling refinement purity3AlC2Ceramic powder, ball milling condition: ballstone,
The mass ratio of mixing and dehydrated alcohol is 10:1:1, rotational speed of ball-mill 350r/min, High Energy Ball Milling Time 2h, then by gained
Solid-liquid mixing is dried at 40 DEG C, obtains Ti3AlC2Ceramic powder；
Step 2, two-dimensional layer nano material MXene-Ti3C2Preparation
By gained Ti in step 13AlC2Ceramic powder is immersed in HF acid solution, wherein 5gTi3AlC2Powder is immersed in
80ml mass concentration is to react for 24 hours in 40wt%HF acid solution；Magnetic agitation, to Ti obtained by step 13AlC2Powder is corroded
After processing, it is 6 with deionized water eccentric cleaning to pH, by obtained solid sample drying at room temperature, obtains two-dimensional layer nano material
MXene-Ti3C2；
Step 3, precipitation method preparation
(1) MXene-Ti is weighed3C20.1g, cerous nitrate 0.44g；Configure the ammonium hydroxide 10ml that pH is 10；
(2) by the MXene-Ti in step (1)3C2It is dissolved in 50ml ultrapure water, is ultrasonically treated 2h；
(3) cerous nitrate in step (1) is added in the solution of step (2), stirs 1h；
(4) ammonium hydroxide in step (1) is added dropwise in the solution of step (3), magnetic agitation 2h, is then centrifuged for taking lower layer heavy
Shallow lake part, and cleaned 5 times with dehydrated alcohol and deionized water respectively；
(5) products therefrom is placed in the 40 DEG C of forced air dryings of baking oven low temperature for 24 hours to get CeO2/MXene-Ti3C2Nanometer is multiple
Condensation material.
Embodiment 6
Step 1 refines powder
It is greater than the ternary layered Ti of 97wt% using high-energy ball milling refinement purity3AlC2Ceramic powder, ball milling condition: ballstone,
The mass ratio of mixing and dehydrated alcohol is 10:1:1, rotational speed of ball-mill 350r/min, High Energy Ball Milling Time 2h, then by gained
Solid-liquid mixing is dried at 40 DEG C, obtains Ti3AlC2Ceramic powder；
Step 2, two-dimensional layer nano material MXene-Ti3C2Preparation
By gained Ti in step 13AlC2Ceramic powder is immersed in HF acid solution, wherein 5gTi3AlC2Powder is immersed in
80ml mass concentration is to react for 24 hours in 40wt%HF acid solution；Magnetic agitation, to Ti obtained by step 13AlC2Powder is corroded
After processing, it is 6 with deionized water eccentric cleaning to pH, by obtained solid sample drying at room temperature, obtains two-dimensional layer nano material
MXene-Ti3C2；
Step 3, precipitation method preparation
(1) MXene-Ti is weighed3C20.1g, cerous nitrate 0.22g；Configure the ammonium hydroxide 10ml that pH is 9；
(2) by the MXene-Ti in step (1)3C2It is dissolved in 50ml ultrapure water, is ultrasonically treated 2h；
(1) cerous nitrate in step (1) is added in the solution of step (2), stirs 1h；
(2) ammonium hydroxide in step (1) is added dropwise in the solution of step (3), magnetic agitation 2h, is then centrifuged for taking lower layer heavy
Shallow lake part, and cleaned 5 times with dehydrated alcohol and deionized water respectively；
(3) products therefrom is placed in the 40 DEG C of forced air dryings of baking oven low temperature for 24 hours to get CeO2/MXene-Ti3C2Nanometer is multiple
Condensation material.
Claims (1)
1. the precipitation method prepare ceria/two-dimensional layer carbonization titanium composite material method, include the following steps:
Step 1 refines powder
It is greater than the ternary layered Ti of 97wt% using high-energy ball milling refinement purity3AlC2Ceramic powder, ball milling condition: ballstone, mixing
And the mass ratio of ball-milling medium is 10:1:1, rotational speed of ball-mill 350r/min, High Energy Ball Milling Time 2h, then by gained solid-liquid
Mixing is dried at 40 DEG C, obtains Ti3AlC2Ceramic powder；
Step 2, two-dimensional layer nano material MXene-Ti3C2Preparation
By gained Ti in step 13AlC2Ceramic powder is immersed in HF acid solution, wherein 5gTi3AlC2Powder is immersed in 80ml matter
Amount concentration is to react for 24 hours in 40wt%HF acid solution；Magnetic agitation, to Ti obtained by step 13AlC2Powder carries out corrosion treatment
Afterwards, it is 6 with deionized water eccentric cleaning to pH, by obtained solid sample drying at room temperature, obtains two-dimensional layer nano material
MXene-Ti3C2；
Step 3, precipitation method preparation
(1) cerous nitrate and MXene-Ti are controlled3C2Mass ratio be 2.2:1,4.4:1 or 8.8:1；Then configuration pH is 9~11
Ammonium hydroxide 10ml；
(2) by the MXene-Ti of 0.05g or 0.1g step (1)3C2It is dissolved separately in 50ml ultrapure water, is ultrasonically treated 2h, until
It is uniformly dispersed；
(3) cerous nitrate in step (1) is added in the solution of step (2), the concentration for controlling cerous nitrate solution is 0.02mol/
L stirs 1h；
(4) take step (1) 10ml ammonium hydroxide that the magnetic agitation 2h in the solution of step (3) is added dropwise；Products therefrom is centrifugated,
It takes lower layer's sediment fraction and is cleaned respectively with dehydrated alcohol and deionized water；
(5) the resulting product of step (4) is placed forced air drying in an oven to handle, 40 DEG C hereinafter, keep the temperature for 24 hours to get CeO2/
MXene-Ti3C2Nanocomposite；
The ball-milling medium is dehydrated alcohol.
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