CN105536834A - Method for preparing cerium dioxide/two-dimensional layered titanium carbide composite material through precipitation process - Google Patents

Method for preparing cerium dioxide/two-dimensional layered titanium carbide composite material through precipitation process Download PDF

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CN105536834A
CN105536834A CN201510908276.4A CN201510908276A CN105536834A CN 105536834 A CN105536834 A CN 105536834A CN 201510908276 A CN201510908276 A CN 201510908276A CN 105536834 A CN105536834 A CN 105536834A
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mxene
alc
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ti3c2
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CN105536834B (en
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朱建锋
周文静
汤祎
曹敏娟
吕文静
任莹莹
鹿萧
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Shaanxi University of Science and Technology
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    • 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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    • 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
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

The invention provides a method for preparing a cerium dioxide/two-dimensional layered titanium carbide composite material through a precipitation process. The method comprises the following steps: high-energy ball milling and crystal grain refinement so as to obtain high-purity three-component layered Ti3AlC2 powder; preparation of two-dimensional layered nano-material MXene-Ti3C2 through hydrofluoric acid corrosion; and formation of CeO2 on the surface and interlayers of MXene-Ti3C2 through the precipitation process so as to allow CeO2 to be loaded with MXene-Ti3C2, thereby obtaining the CeO2/MXene-Ti3C2 nanocomposite material. The method has the advantages of simple process, controllable technology and low cost; and the prepared nanocomposite material has the characteristics of uniform lamellas of the two-dimensional layered MXene-Ti3C2, uniform distribution of CeO2 and the like and the advantages of a large specific surface area, good conductivity and good photocatalysis performance, which facilitates application of the nanocomposite material in fields like photocatalysis, lithium ion batteries and supercapacitors.

Description

The precipitation method prepare the method for ceria/two-dimensional layer titanium carbide composite
Technical field
The invention belongs to inorganic nano composite material technical field, particularly the precipitation method prepare the method for ceria/two-dimensional layer titanium carbide composite.
Background technology
Ternary layered ceramic material Ti 3alC 2belong to stratiform hexagonal crystallographic texture.At Ti 3alC 2in crystal structure, Ti and C atom forms Ti 6c is octahedra, separate by Al layer, C atom is positioned at octahedral center, and C and Ti atom is combined into strong covalent bond, and Ti-Ti, and is weak binding between Ti and Al, is similar to the Van der Waals force weak bond combination between graphite.
Ti 3alC 2have metal and ceramic performance concurrently, at normal temperatures, it has heat conductivility and electric conductivity, and lower vickers microhardness and higher elastic modelling quantity, can machining be carried out as metal, and at a higher temperature there is plasticity, possess again higher yield strength simultaneously, high-melting-point, the performance of the pottery such as high thermal stability and good non-oxidizability.
Two-dimensional layer nano-carbide is the material of a kind graphene-structured, due to the two-dimensional layered structure of its uniqueness, larger specific area, good electric conductivity and hydrophily, good magnetic and make it have superpower catalytic performance, photovoltaic performance and chemical property, is widely used in function ceramics, photocatalysis, lithium ion battery, solar cell, biology sensor etc.
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 electronic energy level structure, can be used as ultra-violet absorber.Nano-cerium oxide, because of its stable crystal formation, can be used as solid fuel cell electrolyte.
Existing MXene-Ti 3c 2, performance is single, and surface area is less, and range of application is narrower, and is not suitable for mass-produced feature.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, the object of the present invention is to provide the precipitation method to prepare the method for ceria/two-dimensional layer titanium carbide composite, the specific area with the composite after load is larger, is applicable to a large amount of preparation, performance is high, application feature more widely.
To achieve these goals, the technical solution used in the present invention is:
The precipitation method prepare the method for ceria/two-dimensional layer titanium carbide composite, comprise the steps:
Step one, refinement powder
High-energy ball milling refinement purity is utilized to be greater than the ternary layered Ti of 97wt% 3alC 2ceramic powder, ball milling condition: the mass ratio of ballstone, batch mixing and ball-milling medium is 10:1:1, and rotational speed of ball-mill is 350r/min, and High Energy Ball Milling Time is 2h, is then dried at 40 DEG C by gained solid-liquid batch mixing, obtains Ti 3alC 2ceramic powder;
Step 2, two-dimensional layer nano material MXene-Ti 3c 2preparation
By gained Ti in step one 3alC 2ceramic powder is immersed in HF acid solution, wherein 5gTi 3alC 2it is react 24h in 40wt%HF acid solution that powder is immersed in 80ml mass concentration; Magnetic agitation, to step one gained Ti 3alC 2after powder carries out corrosion treatmentCorrosion Science, be 6 by deionized water eccentric cleaning to pH, by gained solid sample drying at room temperature, obtain two-dimensional layer nano material MXene-Ti 3c 2;
Step 3, prepared by the precipitation method
(1) cerous nitrate and MXene-Ti is controlled 3c 2mass ratio be 2.2:1,4.4:1 or 8.8:1; Then the ammoniacal liquor 10ml that pH is 9 ~ 11 is configured;
(2) by the MXene-Ti of 0.05g or 0.1g step (1) 3c 2be dissolved in 50ml ultra-pure water respectively, ultrasonic process 2h, until be uniformly dispersed;
(3) add in the solution of step (2) by the cerous nitrate in step (1), the concentration controlling cerous nitrate solution is 0.02mol/l, stirs 1h;
(4) get step (1) 10ml ammoniacal liquor to drip in the solution of step (3), magnetic agitation 2h; By products therefrom centrifugation, take off layer sediment fraction and use absolute ethyl alcohol and washed with de-ionized water respectively;
(5) product of step (4) gained is placed forced air drying process in an oven, less than 40 DEG C, insulation 24h, obtains CeO 2/ MXene-Ti 3c 2nano composite material.
Described ball-milling medium is absolute ethyl alcohol.
Beneficial effect of the present invention:
Adopt precipitation method load C eO 2to two-dimensional layer material MXene-Ti 3c 2on, carrying method is simply effective, and is applicable to a large amount of preparation.Its specific area of composite after load is larger, and has CeO 2some characteristics, such as photocatalysis, pattern are various etc., therefore CeO 2/ MXene-Ti 3c 2the performance of nano composite material is more better than single MXene-Ti 3c 2, its application will be more extensive.Because graphene-supported CeO2 nano particle composite material has higher electric capacity, good photocatalysis performance, and MXene-Ti3C2 is class graphene-structured, for further at ultracapacitor, lithium ion battery, the application in the field such as photocatalysis, biology sensor, has carried out the preparation work of predecessor.
The present invention is by Ti 3alC 2in HF acid, carry out chemical etching, Al is etched away by selective, form a kind of two-dimensional layer material MXene-Ti 3c 2, then adopt the precipitation method at two-dimensional layer material MXene-Ti 3c 2upper load C eO 2, the specific area of stratified material is increased, and makes material have photocatalytic degradation, one's own physical property, the characteristics such as pattern is various, therefore, CeO 2/ MXene-Ti 3c 2the performance of nano composite material is more better than single MXene-Ti 3c 2, its application will be more extensive.
Accompanying drawing explanation
Fig. 1 is Ti 3alC 2before powder corrosion treatmentCorrosion Science, after corrosion treatmentCorrosion Science and the XRD collection of illustrative plates of load afterproduct.
Fig. 2 is Ti 3alC 2the corrosion product MXene-Ti of powder 3c 2sample SEM after 24h is dried in the 40 DEG C of air blast of baking oven low temperature schemes.
Fig. 3 prepares CeO for adopting the precipitation method 2/ MXene-Ti 3c 2the sample SEM of nano combined product after 24h is dried in the 40 DEG C of air blast of baking oven low temperature schemes.
Detailed description of the invention
Below by embodiment, the present invention is described in further details.
As can be seen from Figure 3, CeO 2be evenly distributed in two-dimensional layer MXene-Ti 3c 2surface and interlayer.
Embodiment 1
Step one, refinement powder
High-energy ball milling refinement purity is utilized to be greater than the ternary layered Ti of 97wt% 3alC 2ceramic powder, ball milling condition: the mass ratio of ballstone, batch mixing and absolute ethyl alcohol is 10:1:1, and rotational speed of ball-mill is 350r/min, and High Energy Ball Milling Time is 2h, is then dried at 40 DEG C by gained solid-liquid batch mixing, obtains Ti 3alC 2ceramic powder;
Step 2, two-dimensional layer nano material MXene-Ti 3c 2preparation
By gained Ti in step one 3alC 2ceramic powder is immersed in HF acid solution, wherein 5gTi 3alC 2it is react 24h in 40wt%HF acid solution that powder is immersed in 80ml mass concentration; Magnetic agitation, to step one gained Ti 3alC 2after powder carries out corrosion treatmentCorrosion Science, be 6 by deionized water eccentric cleaning to pH, by gained solid sample drying at room temperature, obtain two-dimensional layer nano material MXene-Ti 3c 2;
Step 3, prepared by the precipitation method
(1) MXene-Ti is taken 3c 20.05g, cerous nitrate 0.44g; Configuration pH is the ammoniacal liquor 10ml of 9;
(2) by the MXene-Ti in step (1) 3c 2be dissolved in 50ml ultra-pure water, ultrasonic process 2h;
(3) cerous nitrate in step (1) is added in the solution of step (2), stir 1h;
(4) ammoniacal liquor in step (1) is dripped in the solution of step (3), magnetic agitation 2h, then centrifuging and taking bottom sediment, and use absolute ethyl alcohol and washed with de-ionized water 5 times respectively;
(5) step (4) products therefrom is positioned over baking oven low temperature 40 DEG C of forced air drying 24h, obtains CeO 2/ MXene-Ti 3c 2nano composite material.
Embodiment 2
Step one, refinement powder
High-energy ball milling refinement purity is utilized to be greater than the ternary layered Ti of 97wt% 3alC 2ceramic powder, ball milling condition: the mass ratio of ballstone, batch mixing and absolute ethyl alcohol is 10:1:1, and rotational speed of ball-mill is 350r/min, and High Energy Ball Milling Time is 2h, is then dried at 40 DEG C by gained solid-liquid batch mixing, obtains Ti 3alC 2ceramic powder;
Step 2, two-dimensional layer nano material MXene-Ti 3c 2preparation
By gained Ti in step one 3alC 2ceramic powder is immersed in HF acid solution, wherein 5gTi 3alC 2it is react 24h in 40wt%HF acid solution that powder is immersed in 80ml mass concentration; Magnetic agitation, to step one gained Ti 3alC 2after powder carries out corrosion treatmentCorrosion Science, be 6 by deionized water eccentric cleaning to pH, by gained solid sample drying at room temperature, obtain two-dimensional layer nano material MXene-Ti 3c 2;
Step 3, prepared by the precipitation method
(1) MXene-Ti is taken 3c 20.05g, cerous nitrate 0.44g; Configuration pH is the ammoniacal liquor 10ml of 10;
(2) by the MXene-Ti in step (1) 3c 2be dissolved in 50ml ultra-pure water, ultrasonic process 2h;
(3) cerous nitrate in step (1) is added in the solution of step (2), stir 1h;
(4) ammoniacal liquor in step (1) is dripped in the solution of step (3), magnetic agitation 2h, then centrifugally remove deposit, and use absolute ethyl alcohol and washed with de-ionized water 5 times respectively;
(5) step (4) products therefrom is positioned over baking oven low temperature 40 DEG C of forced air drying 24h, obtains CeO 2/ MXene-Ti 3c 2nano composite material.
Embodiment 3
Step one, refinement powder
High-energy ball milling refinement purity is utilized to be greater than the ternary layered Ti of 97wt% 3alC 2ceramic powder, ball milling condition: the mass ratio of ballstone, batch mixing and absolute ethyl alcohol is 10:1:1, and rotational speed of ball-mill is 350r/min, and High Energy Ball Milling Time is 2h, is then dried at 40 DEG C by gained solid-liquid batch mixing, obtains Ti 3alC 2ceramic powder;
Step 2, two-dimensional layer nano material MXene-Ti 3c 2preparation
By gained Ti in step one 3alC 2ceramic powder is immersed in HF acid solution, wherein 5gTi 3alC 2it is react 24h in 40wt%HF acid solution that powder is immersed in 80ml mass concentration; Magnetic agitation, to step one gained Ti 3alC 2after powder carries out corrosion treatmentCorrosion Science, be 6 by deionized water eccentric cleaning to pH, by gained solid sample drying at room temperature, obtain two-dimensional layer nano material MXene-Ti 3c 2;
Step 3, prepared by the precipitation method
(1) MXene-Ti is taken 3c 20.05g, cerous nitrate 0.44g; Configuration pH is the ammoniacal liquor 10ml of 11;
(2) by the Mxene-Ti in step (1) 3c 2be dissolved in 50ml ultra-pure water, ultrasonic process 2h;
(3) cerous nitrate in step (1) is added in the solution of step (2), stir 1h;
(4) ammoniacal liquor in step (1) is dripped in the solution of step (3), magnetic agitation 2h, then centrifugal and use absolute ethyl alcohol and washed with de-ionized water 5 times respectively;
(5) step (4) products therefrom is positioned over baking oven low temperature 40 DEG C of forced air drying 24h, obtains CeO 2/ MXene-Ti 3c 2nano composite material.
Embodiment 4
Step one, refinement powder
High-energy ball milling refinement purity is utilized to be greater than the ternary layered Ti of 97wt% 3alC 2ceramic powder, ball milling condition: the mass ratio of ballstone, batch mixing and absolute ethyl alcohol is 10:1:1, and rotational speed of ball-mill is 350r/min, and High Energy Ball Milling Time is 2h, is then dried at 40 DEG C by gained solid-liquid batch mixing, obtains Ti 3alC 2ceramic powder;
Step 2, two-dimensional layer nano material MXene-Ti 3c 2preparation
By gained Ti in step one 3alC 2ceramic powder is immersed in HF acid solution, wherein 5gTi 3alC 2it is react 24h in 40wt%HF acid solution that powder is immersed in 80ml mass concentration; Magnetic agitation, to step one gained Ti 3alC 2after powder carries out corrosion treatmentCorrosion Science, be 6 by deionized water eccentric cleaning to pH, by gained solid sample drying at room temperature, obtain two-dimensional layer nano material MXene-Ti 3c 2;
Step 3, prepared by the precipitation method
(1) MXene-Ti is taken 3c 20.1g, cerous nitrate 0.44g; Configuration pH is the ammoniacal liquor 10ml of 9;
(2) by the MXene-Ti in step (1) 3c 2be dissolved in 50ml ultra-pure water, ultrasonic process 2h;
(3) cerous nitrate in step (1) is added in the solution of step (2), stir 1h;
(4) ammoniacal liquor in step (1) is dripped in the solution of step (3), magnetic agitation 2h, then centrifuging and taking lower sediment part, and use absolute ethyl alcohol and washed with de-ionized water 5 times respectively;
(5) step (4) products therefrom is positioned over baking oven low temperature 40 DEG C of forced air drying 24h, obtains CeO 2/ MXene-Ti 3c 2nano composite material.
Embodiment 5
Step one, refinement powder
High-energy ball milling refinement purity is utilized to be greater than the ternary layered Ti of 97wt% 3alC 2ceramic powder, ball milling condition: the mass ratio of ballstone, batch mixing and absolute ethyl alcohol is 10:1:1, and rotational speed of ball-mill is 350r/min, and High Energy Ball Milling Time is 2h, is then dried at 40 DEG C by gained solid-liquid batch mixing, obtains Ti 3alC 2ceramic powder;
Step 2, two-dimensional layer nano material MXene-Ti 3c 2preparation
By gained Ti in step one 3alC 2ceramic powder is immersed in HF acid solution, wherein 5gTi 3alC 2it is react 24h in 40wt%HF acid solution that powder is immersed in 80ml mass concentration; Magnetic agitation, to step one gained Ti 3alC 2after powder carries out corrosion treatmentCorrosion Science, be 6 by deionized water eccentric cleaning to pH, by gained solid sample drying at room temperature, obtain two-dimensional layer nano material MXene-Ti 3c 2;
Step 3, prepared by the precipitation method
(1) MXene-Ti is taken 3c 20.1g, cerous nitrate 0.44g; Configuration pH is the ammoniacal liquor 10ml of 10;
(2) by the MXene-Ti in step (1) 3c 2be dissolved in 50ml ultra-pure water, ultrasonic process 2h;
(3) cerous nitrate in step (1) is added in the solution of step (2), stir 1h;
(4) ammoniacal liquor in step (1) is dripped in the solution of step (3), magnetic agitation 2h, then centrifuging and taking lower sediment part, and use absolute ethyl alcohol and washed with de-ionized water 5 times respectively;
(5) products therefrom is positioned over baking oven low temperature 40 DEG C of forced air drying 24h, obtains CeO 2/ MXene-Ti 3c 2nano composite material.
Embodiment 6
Step one, refinement powder
High-energy ball milling refinement purity is utilized to be greater than the ternary layered Ti of 97wt% 3alC 2ceramic powder, ball milling condition: the mass ratio of ballstone, batch mixing and absolute ethyl alcohol is 10:1:1, and rotational speed of ball-mill is 350r/min, and High Energy Ball Milling Time is 2h, is then dried at 40 DEG C by gained solid-liquid batch mixing, obtains Ti 3alC 2ceramic powder;
Step 2, two-dimensional layer nano material MXene-Ti 3c 2preparation
By gained Ti in step one 3alC 2ceramic powder is immersed in HF acid solution, wherein 5gTi 3alC 2it is react 24h in 40wt%HF acid solution that powder is immersed in 80ml mass concentration; Magnetic agitation, to step one gained Ti 3alC 2after powder carries out corrosion treatmentCorrosion Science, be 6 by deionized water eccentric cleaning to pH, by gained solid sample drying at room temperature, obtain two-dimensional layer nano material MXene-Ti 3c 2;
Step 3, prepared by the precipitation method
(1) MXene-Ti is taken 3c 20.1g, cerous nitrate 0.22g; Configuration pH is the ammoniacal liquor 10ml of 9;
(2) by the MXene-Ti in step (1) 3c 2be dissolved in 50ml ultra-pure water, ultrasonic process 2h;
(1) cerous nitrate in step (1) is added in the solution of step (2), stir 1h;
(2) ammoniacal liquor in step (1) is dripped in the solution of step (3), magnetic agitation 2h, then centrifuging and taking lower sediment part, and use absolute ethyl alcohol and washed with de-ionized water 5 times respectively;
(3) products therefrom is positioned over baking oven low temperature 40 DEG C of forced air drying 24h, obtains CeO 2/ MXene-Ti 3c 2nano composite material.

Claims (2)

1. the precipitation method prepare the method for ceria/two-dimensional layer titanium carbide composite, comprise the steps:
Step one, refinement powder
High-energy ball milling refinement purity is utilized to be greater than the ternary layered Ti of 97wt% 3alC 2ceramic powder, ball milling condition: the mass ratio of ballstone, batch mixing and ball-milling medium is 10:1:1, and rotational speed of ball-mill is 350r/min, and High Energy Ball Milling Time is 2h, is then dried at 40 DEG C by gained solid-liquid batch mixing, obtains Ti 3alC 2ceramic powder;
Step 2, two-dimensional layer nano material MXene-Ti 3c 2preparation
By gained Ti in step one 3alC 2ceramic powder is immersed in HF acid solution, wherein 5gTi 3alC 2it is react 24h in 40wt%HF acid solution that powder is immersed in 80ml mass concentration; Magnetic agitation, to step one gained Ti 3alC 2after powder carries out corrosion treatmentCorrosion Science, be 6 by deionized water eccentric cleaning to pH, by gained solid sample drying at room temperature, obtain two-dimensional layer nano material MXene-Ti 3c 2;
Step 3, prepared by the precipitation method
(1) cerous nitrate and MXene-Ti is controlled 3c 2mass ratio be 2.2:1,4.4:1 or 8.8:1; Then the ammoniacal liquor 10ml that pH is 9 ~ 11 is configured;
(2) by the MXene-Ti of 0.05g or 0.1g step (1) 3c 2be dissolved in 50ml ultra-pure water respectively, ultrasonic process 2h, until be uniformly dispersed;
(3) add in the solution of step (2) by the cerous nitrate in step (1), the concentration controlling cerous nitrate solution is 0.02mol/l, stirs 1h;
(4) get step (1) 10ml ammoniacal liquor to drip in the solution of step (3), magnetic agitation 2h; By products therefrom centrifugation, take off layer sediment fraction and use absolute ethyl alcohol and washed with de-ionized water respectively;
(5) product of step (4) gained is placed forced air drying process in an oven, less than 40 DEG C, insulation 24h, obtains CeO 2/ MXene-Ti 3c 2nano composite material.
2. a kind of precipitation method according to claim 1 prepare the method for ceria/two-dimensional layer titanium carbide composite, it is characterized in that, described ball-milling medium is absolute ethyl alcohol.
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CN106589362A (en) * 2016-12-22 2017-04-26 陕西科技大学 Polyaniline nano particle/two-dimensional layered titanium carbide composite material and low-temperature preparation method of polyaniline nano particle/two-dimensional layered titanium carbide composite material
CN106589362B (en) * 2016-12-22 2019-05-28 陕西科技大学 A kind of polyaniline nanoparticles/two-dimensional layer carbonization titanium composite material and its low temperature preparation method
CN106976917A (en) * 2017-03-03 2017-07-25 陕西科技大学 Sheet cobalt black two-dimensional layer carbonization titanium composite material and its two-step preparation
CN108704637A (en) * 2018-06-07 2018-10-26 南京理工大学 MXene/CeO2The preparation method of composite material
CN109692698A (en) * 2018-12-29 2019-04-30 陕西师范大学 A kind of Bi/Ti of catalytic reduction of NOx3C2Nano-sheet photochemical catalyst and preparation method thereof
CN112704736A (en) * 2021-01-08 2021-04-27 深圳万物创新集团有限公司 CeO (CeO)2/MXene composite two-dimensional material and preparation method and application thereof
CN114763265A (en) * 2021-01-13 2022-07-19 中国科学院过程工程研究所 Rare earth doped MXene microsphere and preparation method thereof
CN114763265B (en) * 2021-01-13 2024-01-26 中国科学院过程工程研究所 Rare earth doped MXene microsphere and preparation method thereof
CN115259874A (en) * 2021-04-29 2022-11-01 中国科学院福建物质结构研究所 Toughened and conductive MXene-zirconia composite ceramic and preparation method thereof
CN115259874B (en) * 2021-04-29 2023-11-17 中国科学院福建物质结构研究所 Toughened and conductive MXene-zirconia composite ceramic and preparation method thereof
CN114160089A (en) * 2021-11-05 2022-03-11 上海船舶工艺研究所(中国船舶工业集团公司第十一研究所) VOCs adsorbing material of titanium tricarboxide composite titanium dioxide and preparation method thereof
CN114160089B (en) * 2021-11-05 2024-04-05 上海船舶工艺研究所(中国船舶集团有限公司第十一研究所) VOCs adsorption material of titanium carbide composite titanium dioxide and preparation method thereof
CN115283666A (en) * 2022-06-23 2022-11-04 江苏岐铭新材料科技发展有限公司 Aluminum alloy powder spheroidizing process
CN115779940A (en) * 2022-12-08 2023-03-14 安徽师范大学 CeO2-x/MXene composite material with double simulated enzyme properties and preparation method and application thereof

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