CN113735125B - Carbide derived carbon material and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a carbide derived carbon material, a preparation method and application thereof, and a two-dimensional carbide crystal V is prepared by a high-temperature solid phase method 2 AlC, two-dimensional carbide crystal V 2 AlC and Lewis acid molten salt CuCl 2 The carbide derivative carbon material is obtained by mixing and reacting at high temperature, the preparation method has the advantages of simple process steps, mild reaction, easy control, no use of chlorine with strong corrosion and severe toxicity, environmental protection and no pollution, and the prepared carbide derivative carbon material has excellent performance and is suitable for hydrogen storage, catalyst carriers, lithium ion battery electrodes and supercapacitor electrode materials.
Description
Technical Field
The invention relates to the field of nano materials, in particular to a carbide derived carbon material, a preparation method and application thereof.
Background
Carbide-Derived Carbon (CDC) is a novel Carbon material obtained by taking Carbide as a precursor and removing non-Carbon atoms in a crystal lattice to leave a framework Carbon structure. CDC can generally be obtained by selectively etching a metal element using high-temperature chlorine gas. CDC has the characteristics of high specific surface area, adjustable pore size distribution, controllable microstructure and the like, so that the CDC has important application value in a plurality of fields. In recent years, carbide precursors used to prepare CDC mainly include binary carbide, ternary carbide, and polymeric carbon precursors. The ternary carbide used to prepare the CDC is typically the MAX phase.
MAX is a C or N-containing metal carbide or metal nitride having the formula M n+1 AX n Wherein M represents a transition metal element (Ti, nb, V, ta, etc.), A is mainly a third and fourth main group element (Al, si, etc.), and X is a carbon or nitrogen element. n=1, 2 or 3. Depending on the value of n, the MAX phase may be divided into 211, 312 and 413 phases. Chemical method is used for selectively coating element A in precursor MAX phaseCorrosion can result in a new type of two-dimensional nanomaterial called two-dimensional transition metal carbide or nitride (MXene). In 2003, gogotsi was prepared by high temperature chlorination of Ti 3 SiC 2 Preparing Ti 3 SiC 2 -CDC. This CDC has a larger pore volume and a more precisely tuned pore size. In addition, hoffman et al have systematically studied ternary carbides Ti 3 AIC 2 、Ti 2 A1C、Ti 2 A1C 0.5 N 0.5 、Ta 2 a1C and the like are CDC preparation processes of the precursor, and respectively characterize structural characteristics of the obtained CDC.
However, CDC synthesis is often accompanied by high temperatures, and hazardous chlorine is required to participate in the reaction, limiting its further application. Meanwhile, most of MAX precursors adopted are Ti-based, and CDC research on preparing V-based MAX precursors is less.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a carbide derived carbon material, a preparation method and application thereof, and a two-dimensional carbide crystal V is prepared by a high-temperature solid phase method 2 AlC, two-dimensional carbide crystal V 2 AlC and Lewis acid molten salt CuCl 2 The carbide derivative carbon material is obtained by mixing and reacting at high temperature, the preparation method has the advantages of simple process steps, mild reaction, easy control, no use of chlorine with strong corrosion and severe toxicity, environmental protection and no pollution, and the prepared carbide derivative carbon material has excellent performance and is suitable for hydrogen storage, catalyst carriers, lithium ion battery electrodes and supercapacitor electrode materials.
In order to achieve the above object, the present invention provides a method for preparing a carbide-derived carbon material, comprising the steps of:
1) Mixing and grinding vanadium powder, aluminum powder and graphite powder according to the mass ratio of 2 (1-1.5) to 1 to prepare a precursor mixed material;
2) The precursor mixture is treated for 2 to 5 hours at the constant temperature of 1300 to 1600 ℃ under the inert atmosphere to prepare the two-dimensional carbide crystal V 2 AlC；
3) The mass ratio of the substances is 1: (3-5): 1: v of 1 2 AlC、CuCl 2 KCl and NaClMixing and grinding, and then processing the mixture for 4-10 hours at the constant temperature of 650-1000 ℃ under the inert atmosphere to obtain a mixture;
4) Adding deionized water into the mixture for centrifugal separation, adding the obtained precipitate into a sodium persulfate solution for stirring, adding deionized water for cleaning, and carrying out vacuum drying to obtain the carbide-derived carbon material.
Further, alcohol is added during grinding in the step 1), and after grinding, the precursor mixture is obtained by drying.
Further, transferring the precursor mixture in the step 2) into a tube furnace, introducing inert gas, heating the tube furnace to 1600 ℃ at a speed of 4 ℃/min, and performing constant temperature treatment for 2 hours.
Further, the mixture in the step 3) is transferred to a tube furnace, inert gas is introduced, the tube furnace is heated to 750 ℃ at 10 ℃/min, and the temperature is kept for 5 hours.
Further, the mass ratio of the vanadium powder, the aluminum powder and the graphite powder in the step 1) is 2:1.3:1.
Further, V in the step 3) 2 AlC、CuCl 2 The mass ratio of KCl to NaCl was 1:5:1:1.
further, the purities of the vanadium powder, the aluminum powder and the graphite powder are all analytically pure, and the graphite powder is artificial graphite powder.
Further, the concentration of the sodium persulfate solution was 1M.
The invention also provides a carbide derived carbon material, which is prepared by adopting the preparation method of the carbide derived carbon material.
The invention also provides application of the carbide derived carbon material as hydrogen storage, a catalyst carrier, a lithium ion battery electrode and a supercapacitor electrode material.
Compared with the prior art, the method firstly prepares the two-dimensional carbide crystal V by a high-temperature solid phase method 2 AlC, V prepared by high temperature solid phase method 2 AlC is a ternary lamellar compound, in its crystal phase, V atomic layers and Al atomic layers are alternately arranged to form a nearly close-packed hexagonal lamellar structure, and C atoms are filled inOctahedral voids; then adopting Lewis acid to melt salt CuCl 2 Etching V 2 AlC, cu in ionic state in molten salt 2+ Al and V atoms can be oxidized to form a two-dimensional carbide crystal V 2 The Al and V atomic layers in AlC are etched away, and only C atoms are finally left, so that the carbide derived carbon CDC material is obtained, the preparation method is simple in process steps, mild in reaction, easy to control, environment-friendly and pollution-free, the use of chlorine with strong corrosion and severe toxicity is avoided, the hydrogen evolution overpotential of the prepared carbide derived carbon material is 513mV, meanwhile, the mass specific capacitance of the carbide derived carbon material reaches 9.7F/g at the sweeping speed of 2mV/s, the performance is excellent, and the carbide derived carbon material is suitable for hydrogen storage, catalyst carriers, lithium ion battery electrodes and supercapacitor electrode materials and has important application prospects in various fields.
Drawings
FIG. 1 is a V produced in example 1 of the present invention 2 XRD patterns of AlC and CDC materials;
FIG. 2 is an SEM image of a CDC material prepared in example 1 of the present invention;
FIG. 3 is a graph of electrochemical test results of the CDC material prepared in example 1 of the present invention;
FIG. 4 is a graph II of electrochemical test results of CDC material prepared in example 1 of the present invention.
Detailed Description
The present invention will be further illustrated by the following description, taken in conjunction with the accompanying drawings and specific embodiments, and it will be apparent that the embodiments described are some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
The invention provides a preparation method of carbide derived carbon CDC material, which comprises the steps of preparing a two-dimensional carbide crystal V by a high-temperature solid phase method 2 AlC, then adopt Lewis acid molten salt CuCl 2 Etching V 2 AlC, two-dimensional carbide crystal V 2 And etching away the Al and V atomic layers in AlC to obtain the CDC material. The method specifically comprises the following steps:
1) Adding vanadium powder, aluminum powder and graphite powder into a mortar together according to the mass ratio of (1-1.5) 1, adding alcohol for grinding, and drying at 35 ℃ for 12 hours to obtain a precursor mixed material; preferably, the mass ratio of the vanadium powder to the aluminum powder to the graphite powder is 1:1.3:1; preferably, the purities of the vanadium powder, the aluminum powder and the graphite powder are all analytically pure, and the graphite powder is artificial graphite powder;
2) Transferring the precursor mixture into a tube furnace, introducing inert gas, heating the tube furnace to 1300-1600 ℃ at a speed of 4-10 ℃/min, and performing constant temperature treatment for 2-5 h to obtain the two-dimensional carbide crystal V 2 AlC; preferably, the tube furnace is heated to 1600 ℃ at a speed of 4 ℃/min and is treated at a constant temperature for 2 hours; the inert gas is flowing argon atmosphere;
3) The mass ratio of the substances is 1: (3-5): 1: v of 1 2 AlC、CuCl 2 Grinding KCl and NaCl in a mortar for 2min, transferring the mixed material into a tube furnace, introducing inert gas, heating the tube furnace to 650-1000 ℃ at 10 ℃/min, and performing constant temperature treatment for 4-10 h; preferably, the tube furnace is heated to 750 ℃ at 10 ℃/min and is treated at constant temperature for 5 hours; preferably V 2 AlC、CuCl 2 The mass ratio of KCl to NaCl was 1:5:1:1, a step of;
4) And (3) placing the obtained mixture into a 50ml centrifuge tube, adding deionized water for centrifugation, wherein the centrifugal speed is 3500rpm/min, the time is 3min, discarding supernatant, repeating for 3 times, adding the precipitate into a 1M sodium persulfate solution, stirring for 4h, adding deionized water for cleaning, and finally, carrying out vacuum drying at 60 ℃ for 12h to obtain the CDC material.
The invention also provides a carbide derived carbon material prepared by the method, and the CDC material is applied to hydrogen storage, catalyst carriers, lithium ion battery electrodes and super capacitor electrode materials, and has important application prospects in various fields.
The present invention will be described in detail with reference to the following examples.
Example 1:
1) Mixing and grinding vanadium powder, aluminum powder and graphite powder with granularity of 200 meshes for 10min, wherein the molar ratio of vanadium element to aluminum element to carbon element is 2:1.3:1, placing in a crucible, then placing in a tube flowing argon gasThe temperature rising rate of 4 ℃/min is increased to 1500 ℃ in the furnace for sintering, the heat preservation time is 2h, and the parameters of the tubular furnace for flowing argon are as follows: argon pressure is 0.07MPa, argon flow is 40cc/min, and the furnace is cooled to room temperature to obtain a bulk precursor MAX phase compound V 2 AlC. The bulk powder was ground and sieved to a sieve size of 40 microns.
2)V 2 AlC、CuCl 2 The mass ratio of NaCl to KCl is 1:5:1:1 in a mortar for 2min, placing the ground mixture in a crucible, then placing in a tubular furnace flowing argon gas, heating to 750 ℃ at a heating rate of 10 ℃/min for sintering, and cooling the furnace to room temperature for 5h to obtain a mixture of CDC and molten salt.
3) The resulting mixture was placed in a 50ml centrifuge tube, centrifuged with deionized water at 3500rpm/min for 3min, and the supernatant discarded and repeated 3 times. Adding the precipitate into 1M sodium persulfate solution, stirring for 4 hours, adding deionized water for cleaning, and finally drying in vacuum at 60 ℃ for 12 hours to obtain the CDC material.
For V prepared in example 1 2 XRD analysis of AlC and CDC materials, see FIG. 1, from which the original V can be seen 2 AlC is completely etched, leaving only the carbon layer, i.e., CDC.
SEM analysis was performed on the CDC material prepared in example 1, see fig. 2, and it can be seen from fig. 2 that CDC exhibits a distinct layered structure.
Electrochemical test analysis of the CDC Material obtained in example 1 referring to FIG. 3, it can be seen from FIG. 3 that CDC has significant electrocatalytic Hydrogen evolution activity at 0.5MH 2 SO 4 The solution reaches 10mA cm -2 The current density only needs 513mV overpotential.
Electrochemical analysis of the CDC Material obtained in example 1, see FIG. 4, it can be seen from FIG. 4 that CDC can be used as a cathode material in 3MH 2 SO 4 In the solution, the mass specific capacitance reaches 9.7F/g at the scanning speed of 2mV/s, and reaches 6.6F/g at the scanning speed of 10 mV/s.
Example 2:
1) Vanadium powder, aluminum powder and stone with granularity of 200 meshesMixing and grinding the toner for 10min, wherein the molar ratio of vanadium element to aluminum element to carbon element is 2:1.3:1, placing in a crucible. Then placing the mixture into a tubular furnace flowing argon, heating to 1500 ℃ at a heating rate of 4 ℃/min for sintering, wherein the heat preservation time is 2h, and the parameters of the tubular furnace flowing argon are as follows: argon pressure is 0.07MPa, argon flow is 40cc/min, and the furnace is cooled to room temperature to obtain a bulk precursor MAX phase compound V 2 AlC. The bulk powder was ground and sieved to a sieve size of 40 microns.
2)V 2 AlC、CuCl 2 The mass ratio of NaCl to KCl is 1:3:1:1 in a mortar for 2min, placing the ground mixture in a crucible, then placing in a tubular furnace flowing argon gas, heating to 750 ℃ at a heating rate of 10 ℃/min for sintering, and cooling the furnace to room temperature for 5h to obtain a mixture of CDC and molten salt.
3) The resulting mixture was placed in a 50ml centrifuge tube, centrifuged with deionized water at 3500rpm/min for 3min, and the supernatant discarded and repeated 3 times. Adding the precipitate into 1M sodium persulfate solution, stirring for 4 hours, adding deionized water for cleaning, and finally drying in vacuum at 60 ℃ for 12 hours to obtain the CDC material.
Example 3:
1) Mixing and grinding vanadium powder, aluminum powder and graphite powder with granularity of 200 meshes for 10min, wherein the molar ratio of vanadium element to aluminum element to carbon element is 2:1.3:1, placing in a crucible. Then placing the mixture into a tubular furnace flowing argon, heating to 1500 ℃ at a heating rate of 4 ℃/min for sintering, wherein the heat preservation time is 2h, and the parameters of the tubular furnace flowing argon are as follows: argon pressure is 0.07MPa, argon flow is 40cc/min, and the furnace is cooled to room temperature to obtain a bulk precursor MAX phase compound V 2 AlC. The bulk powder was ground and sieved to a sieve size of 40 microns.
2)V 2 AlC、CuCl 2 The mass ratio of NaCl to KCl is 1:5:1:1 grinding in a mortar for 2min, placing the ground mixture in a crucible, then placing in a tubular furnace flowing argon gas, heating to 650 ℃ at a heating rate of 10 ℃/min for sintering, keeping the temperature for 5h, and cooling the furnace to room temperature to obtain CDC and meltingSalt mixture.
3) The resulting mixture was placed in a 50ml centrifuge tube, centrifuged with deionized water at 3500rpm/min for 3min, and the supernatant discarded and repeated 3 times. Adding the precipitate into 1M sodium persulfate solution, stirring for 4 hours, adding deionized water for cleaning, and finally drying in vacuum at 60 ℃ for 12 hours to obtain the CDC material.
Example 4:
1) Adding vanadium powder, aluminum powder and graphite powder into a mortar together according to the mass ratio of 2:1:1, adding alcohol for grinding, and drying at 35 ℃ for 12 hours to obtain a precursor mixture;
2) Transferring the precursor mixture into a tube furnace, introducing inert gas, heating the tube furnace to 1300 ℃ at a speed of 4 ℃/min, and performing constant temperature treatment for 5 hours to obtain a two-dimensional carbide crystal V 2 AlC；
3) The mass ratio of the substances is 1:3:1: v of 1 2 AlC、CuCl 2 Grinding KCl and NaCl in a mortar for 2min, transferring the mixed material into a tube furnace, introducing inert gas, heating the tube furnace to 650 ℃ at 10 ℃/min, and performing constant temperature treatment for 10h;
4) And (3) placing the obtained mixture into a 50ml centrifuge tube, adding deionized water for centrifugation, wherein the centrifugal speed is 3500rpm/min, the time is 3min, discarding supernatant, repeating for 3 times, adding the precipitate into a 1M sodium persulfate solution, stirring for 4h, adding deionized water for cleaning, and finally, carrying out vacuum drying at 60 ℃ for 12h to obtain the CDC material.
Example 5:
1) Adding vanadium powder, aluminum powder and graphite powder into a mortar together according to the mass ratio of 2:1.5:1, adding alcohol for grinding, and drying at 35 ℃ for 12 hours to obtain a precursor mixture;
2) Transferring the precursor mixture into a tube furnace, introducing inert gas, heating the tube furnace to 1600 ℃ at a speed of 10 ℃/min, and performing constant temperature treatment for 2 hours to obtain a two-dimensional carbide crystal V 2 AlC；
3) The mass ratio of the substances is 1:5:1: v of 1 2 AlC、CuCl 2 Grinding KCl and NaCl in a mortar for 2min, transferring the mixture into a tube furnace, introducing inert gas, and heating the tube furnace at 10deg.C/minHeating to 1000 ℃, and performing constant temperature treatment for 4 hours;
4) And (3) placing the obtained mixture into a 50ml centrifuge tube, adding deionized water for centrifugation, wherein the centrifugal speed is 3500rpm/min, the time is 3min, discarding supernatant, repeating for 3 times, adding the precipitate into a 1M sodium persulfate solution, stirring for 4h, adding deionized water for cleaning, and finally, carrying out vacuum drying at 60 ℃ for 12h to obtain the CDC material.
Example 6:
1) Adding vanadium powder, aluminum powder and graphite powder into a mortar together according to the mass ratio of 2:1.2:1, adding alcohol for grinding, and drying at 35 ℃ for 12 hours to obtain a precursor mixture;
2) Transferring the precursor mixture into a tube furnace, introducing inert gas, heating the tube furnace to 1400 ℃ at a speed of 6 ℃/min, and performing constant temperature treatment for 3 hours to obtain a two-dimensional carbide crystal V 2 AlC；
3) The mass ratio of the substances is 1:4:1: v of 1 2 AlC、CuCl 2 Grinding KCl and NaCl in a mortar for 2min, transferring the mixed material into a tube furnace, introducing inert gas, heating the tube furnace to 850 ℃ at 10 ℃/min, and performing constant temperature treatment for 6h;
4) And (3) placing the obtained mixture into a 50ml centrifuge tube, adding deionized water for centrifugation, wherein the centrifugal speed is 3500rpm/min, the time is 3min, discarding supernatant, repeating for 3 times, adding the precipitate into a 1M sodium persulfate solution, stirring for 4h, adding deionized water for cleaning, and finally, carrying out vacuum drying at 60 ℃ for 12h to obtain the CDC material.
The invention combines lamellar vanadium-based MAX phase compound V 2 AlC and Lewis acid molten salt CuCl 2 Uniformly mixing, placing in a tube furnace, performing high-temperature reaction under flowing argon atmosphere, then cleaning with deionized water and sodium persulfate solution, and drying the washed sample in a vacuum environment at a certain temperature for a certain time to obtain the carbide derived carbon material. The method for preparing the carbide derived carbon CDC of the invention does not relate to toxic and harmful Cl 2 Using CuCl only 2 Will V 2 The Al and V layers in AlC phase are completely corroded to obtain CDC, so that the use of chlorine with strong corrosion and severe toxicity is avoided, and the method is environment-friendly, pollution-free, mild in reaction and easy to controlThe preparation method has simple operation steps and is suitable for expanded production. Therefore, the catalyst has important application prospects in various fields, such as hydrogen storage, catalyst carriers, lithium ion battery electrodes and supercapacitor electrode materials.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced with equivalents; such modifications and substitutions do not depart from the spirit of the technical solutions according to the embodiments of the present invention.
Claims (10)
1. A method for preparing a carbide-derived carbon material, comprising the steps of:
1) Mixing and grinding vanadium powder, aluminum powder and graphite powder according to the mass ratio of 2 (1-1.5) to 1 to prepare a precursor mixed material;
2) The precursor mixture is treated for 2 to 5 hours at the constant temperature of 1300 to 1600 ℃ under the inert atmosphere to prepare the two-dimensional carbide crystal V 2 AlC；
3) The mass ratio of the substances is 1: (3-5): 1: v of 1 2 AlC、CuCl 2 Mixing and grinding KCl and NaCl, and then processing the mixture at the constant temperature of 650-1000 ℃ for 4-10 hours under inert atmosphere to obtain a mixture;
4) Adding deionized water into the mixture for centrifugal separation, adding the obtained precipitate into a sodium persulfate solution for stirring, adding deionized water for cleaning, and carrying out vacuum drying to obtain the carbide-derived carbon material.
2. The method for preparing a carbide derived carbon material as claimed in claim 1, wherein alcohol is added during the grinding in step 1), and the precursor mixture is prepared by drying after grinding.
3. The method for preparing a carbide derived carbon material according to claim 1, wherein the precursor mixture in the step 2) is transferred to a tube furnace, inert gas is introduced, the tube furnace is heated to 1600 ℃ at 4 ℃/min, and the tube furnace is subjected to constant temperature treatment for 2 hours.
4. The method for preparing a carbide derived carbon material according to claim 1, wherein the mixture in the step 3) is transferred to a tube furnace, inert gas is introduced, the tube furnace is heated to 750 ℃ at 10 ℃/min, and the tube furnace is subjected to constant temperature treatment for 5 hours.
5. The method for preparing a carbide-derived carbon material according to claim 1, wherein the mass ratio of the vanadium powder, the aluminum powder and the graphite powder in the step 1) is 2:1.3:1.
6. The method for producing a carbide derived carbon material as claimed in claim 1, wherein V in step 3) 2 AlC、CuCl 2 The mass ratio of KCl to NaCl was 1:5:1:1.
7. the method for preparing a carbide derived carbon material according to claim 1, wherein the purities of the vanadium powder, the aluminum powder and the graphite powder are all analytically pure, and the graphite powder is artificial graphite powder.
8. A method of preparing a carbide derived carbon material according to claim 1, wherein the concentration of the sodium persulfate solution is 1M.
9. A carbide derived carbon material prepared by the method of any one of claims 1 to 8.
10. Use of the carbide derived carbon material of claim 9 as hydrogen storage, catalyst support, lithium ion battery electrode, and supercapacitor electrode material.
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