CN108499588A - A kind of g-C3N4The preparation method of/MXene composite materials - Google Patents
A kind of g-C3N4The preparation method of/MXene composite materials Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 15
- 239000004202 carbamide Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- 229910009819 Ti3C2 Inorganic materials 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000003570 air Substances 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- WTHDKMILWLGDKL-UHFFFAOYSA-N urea;hydrate Chemical compound O.NC(N)=O WTHDKMILWLGDKL-UHFFFAOYSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 238000007146 photocatalysis Methods 0.000 abstract description 12
- 238000004065 wastewater treatment Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 230000036314 physical performance Effects 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 16
- 239000000843 powder Substances 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000004108 freeze drying Methods 0.000 description 4
- 230000002687 intercalation Effects 0.000 description 4
- 238000009830 intercalation Methods 0.000 description 4
- -1 titanium carbide compound Chemical class 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 150000007974 melamines Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical class OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J37/08—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
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Abstract
The present invention relates to a kind of g C3N4The preparation method of/MXene composite materials, including：MXene material preparations, MXene and g C3N4Prepared by the mixture of precursor species, g C3N4It is prepared by/MXene composite materials.The present invention is simple, and technological parameter is easy to control, of low cost, is easy to large-scale production；The g C being prepared3N4/ MXene composite material good crystallinities, particle is tiny and is evenly distributed, and large specific surface area, electric conductivity is good, has preferable photocatalysis performance, one's own physical performance is good, has application value in fields such as photocatalysis, wastewater treatment, biosensors.
Description
Technical field
The invention belongs to nano-functional material preparation field, more particularly to a kind of g-C3N4The preparation of/MXene composite materials
Method.
Background technology
Conductor photocatalysis shows huge potentiality in solution energy shortage and environmental pollution etc., by each international politics
The great attention at mansion.Therefore, developing novel, efficient photochemical catalyst becomes the necessity of photocatalysis technology development.
In recent years, a kind of novel, nonmetallic materials g-C for being responded under visible light3N4, due to energy gap (about 2.7eV)
Relatively narrow, the advantages that chemical stability is good, preparation method is easy, is widely paid close attention to.So far, it is not found in nature
Naturally occurring g-C3N4Crystal, g-C3N4Experiment synthesis is depended on, g-C is synthesized3N4Presoma generally select nitrogen content
Abundant compound such as urea, thiocarbamide, cyanamide, melamine etc..But the g-C of synthesis3N4Specific surface area is usually less than 10m2/ g,
And light induced electron is easily compound with hole, leading to its, light-catalysed the effect is unsatisfactory.In order to inhibit photo-generate electron-hole pair
It is compound, it can be by g-C3N4It is compound with other materials, improve its photocatalytic activity using the synergistic effect of the two.
MXene is a kind of novel two-dimensional layer nano material, can be prepared by corroding corresponding MAX phases.
Ti3AlC2And Ti2AlC is typical MAX phases.MAX phases are the general designations of a kind of ternary layered compound, and this kind of compound has system
One chemical formula Mn+1AXn, wherein M is transition metal, and A is III, IV major element, and X is C or N, n=1,2,3 etc..MAX phases
Be structurally characterized in that M atoms and A atomic layers are alternately arranged, form six side's layer structure of nearly closs packing, X atoms are filled in octahedron
Gap, wherein M-A keys have the characteristic of metallic bond, weaker relative to M-X key active forces.Therefore, in a solution of hydrofluoric acid, MAX
The A atomic layers of phase are easy to be etched, and remaining M forms two-dimentional M with X atomic layersn+1XnAtomic crystal, in order to emphasize that they are by MAX
It mutually removes, and there is the two-dimensional structure similar with graphene (Graphene), be MXene by their Uniform Names.For example,
By corroding MAX phases Ti with hydrofluoric acid3AlC2It can obtain Mxene-Ti3C2。
Research finds that the organic molecules such as urea can increase MXene interlamellar spacings with intercalation MXene.Intercalation is modified clay
One of important method, from structure and performance, MXene is a kind of " conductive hydrophilic clay ", therefore, prepares organic intercalation
MXene compounds are the emphasis of future studies.Two-dimensional layer nano-carbide (Ti3C2And Ti2C) it is a type graphene-structured
Material, unique pattern and good electric conductivity, magnetism and thermoelectricity capability etc., make its be expected to be applied to air-sensitive, catalysis, answer
The fields such as condensation material, energy stores, environmental pollution improvement, surface plasma body technique, photocell and liquid crystal display.
Therefore, g-C3N4/ MXene composite materials, are expected in photocatalysis, wastewater treatment, ultracapacitor and biosensor
There is good application in equal fields.In addition, related g-C3N4With MXene is compound has not been reported.
Invention content
Technical problem to be solved by the invention is to provide a kind of g-C3N4The preparation method of/MXene composite materials, the party
Method is simple, and technological parameter is easy to control, and is easy to large-scale production, obtained g-C3N4/ MXene composite materials have preferable
Photocatalysis performance, good one's own physical property and the characteristics such as pattern is various, in fields such as photocatalysis, wastewater treatment, biosensors
There is application value.
A kind of g-C of the present invention3N4The preparation method of/MXene composite materials, is as follows：
(1) MAX phases are added with the matched proportion density of 0.01~0.3g/ml in HF solution, are stirred, cleaned, it is dry, it is placed in urine
In plain aqueous solution, continue to stir, then clean, re-dry, obtain MXene materials, the wherein mass ratio of MAX phases and urea is 1:1-
3；
(2) by g-C3N4Precursor species are added in solvent, and stirring is added MXene materials in step (1), continues to stir,
It is dry, obtain MXene and g-C3N4The mixture of precursor species, calcining, obtains g-C3N4/ MXene composite materials, wherein g-
C3N4A concentration of 0.1~the 0.5g/ml of precursor species in a solvent, MXene materials and g-C3N4The mass ratio of precursor species
It is 0.01~0.3:1.
MAX phases are Ti in the step (1)3AlC2Or Ti2AlC, MXene material correspond to have two-dimensional layered structure
Ti3C2Or Ti2C。
Whipping temp is 20~80 DEG C in the step (1), and mixing time is 10~30h；Cleaning is clear with deionized water
It is 6~7 to be washed till pH.
Dry, re-dry is dried in vacuo at 20~80 DEG C in the step (1).
It is 20~80 DEG C to continue whipping temp in the step (1), continue mixing time be 12~for 24 hours；Clean again is to use
Deionized water is cleaned 2~3 times.
G-C in the step (2)3N4Precursor species are thiocarbamide or melamine；Solvent is water.
Whipping temp is 20~80 DEG C in the step (2), and mixing time is 1~2h；Continue mixing time be 10~
24h。
The technological parameter of calcining is in the step (2)：Calcination temperature is 500~600 DEG C, and calcination time is 1~10h,
Heating rate is 1~10 DEG C/min, and calcination atmosphere is air, nitrogen or argon gas.
The method fabricated in situ g-C that the present invention passes through calcining3N4/ MXene composite materials, g-C3N4It is carbonized with two-dimensional layer
Preferable contact can be formed between titanium, is conducive to light induced electron and is quickly shifted to titanium carbide, be conducive to point for improving electron hole
From efficiency, its photocatalysis performance is promoted.
Advantageous effect
(1) present invention is simple, and technological parameter is easy to control, of low cost, is easy to large-scale production；
(2) g-C that the present invention is prepared3N4/ MXene composite material good crystallinities, particle is tiny and is evenly distributed, than
Surface area is big, and electric conductivity is good, has preferable photocatalysis performance, one's own physical performance is good, in photocatalysis, wastewater treatment, life
There is application value in the fields such as object sensor.
Description of the drawings
Fig. 1 is the MXene materials (Ti that embodiment 1 is prepared3C2) scanning electron microscope diagram；
Fig. 2 is the g-C that embodiment 1 is prepared3N4/ two-dimensional layer titanium carbide compound (g-C3N4/ MXene composite woods
Material) X-ray diffractogram；
Fig. 3 is the g-C that embodiment 1 is prepared3N4/ two-dimensional layer titanium carbide compound (g-C3N4/ MXene composite woods
Material) and pure g-C3N4 Photocatalyzed Hydrogen Production performance comparison figure；
Fig. 4 is titanium carbide material MXene after the urea intercalation processing that is prepared of comparative example 1 and the g- that is prepared
C3N4/ two-dimensional layer titanium carbide compound (g-C3N4/ MXene composite materials) X-ray diffractogram.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) purity is more than to 98% Ti3AlC240% HF solution is added with the matched proportion density of 0.06g/ml for ceramic powder
In, it is stirred for 24 hours at 60 DEG C；Then it is 6~7 to be cleaned to pH with deionized water, and by obtained solid sample, vacuum is done at 60 DEG C
It is dry；Powder after drying is placed in 0.05g/ml aqueous solution of urea (Ti3AlC2Mass ratio with urea is 1:1) in, at 60 DEG C
Stirring is for 24 hours；It is cleaned 2~3 times with deionized water again, obtained solid sample is dried in vacuo at 60 DEG C to get to two dimension
The Ti of layer structure3C2(MXene materials).
(2) 2g thiocarbamides are added in 20ml water, the MXene materials in 0.1g steps (1) are added after 2h is stirred at 60 DEG C,
Continue to stir 10h；Then it is dried to get MXene and g-C by freeze-drying3N4The mixture of precursor species, sets
Carry out calcination processing under an argon atmosphere in tube furnace, calcination temperature is 600 DEG C, calcination time 1h, heating rate 1
DEG C/min is to get to g-C3N4/ MXene composite materials.By the g-C3N4/ MXene composite materials and pure g-C3N4 carry out photocatalysis
Hydrogen is produced, the condition of Photocatalyzed Hydrogen Production is：50mg catalyst is placed in the aqueous solution containing 10vol% triethanolamines, with Dai You≤
The 300W xenon lamps of 420nm visible filters are visible light source, are sampled within each hour under the Continuous irradiation of visible light source
It is primary and with the yield of gas chromatographic detection hydrogen.
Fig. 1 shows：The MXene materials that the present embodiment obtains are completely open two-dimensional slice structure, and lamellar spacing is several
Ten nanometers, therefore there is larger specific surface area.
Fig. 2 shows：For composite material in 2 θ=13 °, 27.5 ° there is g-C3N4Characteristic peak, illustrate that the present embodiment is finally made
Standby substance is g-C3N4With two-dimensional layer titanium carbide compound.
Fig. 3 shows：The g-C that the present embodiment obtains3N4/ MXene composite materials have preferable photocatalysis production under visible light
Hydrogen performance, performance are pure g-C3N46 times or so.
Embodiment 2
(1) purity is more than to 98% Ti240% HF solution is added with the matched proportion density of 0.01g/ml for AlC ceramic powders
In, stir 30h at 20 DEG C；Then it is 6~7 to be cleaned to pH with deionized water, and by obtained solid sample, vacuum is done at 20 DEG C
It is dry；Powder after drying is placed in 0.05g/ml aqueous solution of urea (Ti2The mass ratio of AlC and urea is 1:1) in, at 20 DEG C
Stirring is for 24 hours；It is cleaned 2~3 times with deionized water again, obtained solid sample is dried in vacuo at 20 DEG C to get to two dimension
The Ti of layer structure2C (MXene materials).
(2) 2g melamines are added in 20ml water, the MXene in 20mg steps (1) is added after 2h is stirred at 20 DEG C
Material continues stirring for 24 hours；Then it is dried to get MXene and g-C by freeze-drying3N4The mixing of precursor species
Object is placed in tube furnace and carries out calcination processing under an argon atmosphere, and calcination temperature is 500 DEG C, calcination time 10h, heating speed
Rate is 10 DEG C/min to get to g-C3N4/ MXene composite materials.
The g-C that the present embodiment is prepared3N4/ MXene composite materials are pale yellow powder, are had to visible light preferable
It absorbs.
Embodiment 3
(1) purity is more than to 98% Ti240% HF solution is added with the matched proportion density of 0.01g/ml for AlC ceramic powders
In, stir 30h at 20 DEG C；Then it is 6~7 to be cleaned to pH with deionized water, and by obtained solid sample, vacuum is done at 20 DEG C
It is dry；Powder after drying is placed in 0.05g/ml aqueous solution of urea (Ti2The mass ratio of AlC and urea is 1:1) in, at 20 DEG C
Stirring is for 24 hours；It is cleaned 2~3 times with deionized water again, obtained solid sample is dried in vacuo at 20 DEG C to get to two dimension
The Ti of layer structure2C (MXene materials).
(2) 10g melamines are added in 20ml water, the MXene in 3g steps (1) is added after 1.5h is stirred at 50 DEG C
Material continues to stir 10h；Then it is dried to get MXene and g-C by freeze-drying3N4The mixing of precursor species
Object is placed in tube furnace and carries out calcination processing in air atmosphere, and calcination temperature is 550 DEG C, calcination time 2h, heating rate
It is 10 DEG C/min to get to g-C3N4/ MXene composite materials.
Comparative example 1
(1) purity is more than to 98% Ti3AlC240% HF solution is added with the matched proportion density of 0.3g/ml for ceramic powder
In, stir 10h at 80 DEG C；Then it is 6~7 to be cleaned to pH with deionized water, and by obtained solid sample, vacuum is done at 80 DEG C
It is dry；Powder after drying is placed in 0.05g/ml aqueous solution of urea (Ti3AlC2Mass ratio with urea is 1:1) in, at 80 DEG C
Stir 12h；It is cleaned 2~3 times with deionized water again, obtained solid sample is dried in vacuo at 80 DEG C to get to two dimension
The Ti of layer structure3C2(MXene materials).
(2) 2g urea is added in 20ml, the MXene materials in 0.1g steps (1) is added after 1h is stirred at 80 DEG C, after
Continuous stirring 10h；Then it is dried to get MXene and g-C by freeze-drying3N4The mixture of precursor species, is placed in
Carrying out calcination processing in tube furnace under an argon atmosphere, calcination temperature is 600 DEG C, calcination time 1h, heating rate is 1 DEG C/
Min is to get to g-C3N4/ MXene composite materials.
Fig. 4 shows：Compared with Example 1, apparent g-C is not found3N4Diffraction maximum, it can be seen that using urea
As g-C3N4Presoma the effect is unsatisfactory；But after caning be found that 600 DEG C of calcinings by comparison, two-dimensional layer nanometer
Material Ti3C2It is significantly moved to left in 8 ° or so of diffraction maximum generations, this shows that the method by high-temperature calcination under an inert atmosphere can
The effective interlamellar spacing for expanding MXene.
Claims (8)
1. a kind of g-C3N4The preparation method of/MXene composite materials, is as follows：
(1) MAX phases are added with the matched proportion density of 0.01~0.3g/ml in HF solution, are stirred, cleaned, it is dry, it is placed in urea water
In solution, continue to stir, then clean, re-dry, obtain MXene materials, the wherein mass ratio of MAX phases and urea is 1:1-3；
(2) by g-C3N4Precursor species are added in solvent, and stirring is added MXene materials in step (1), continues to stir, dry,
Obtain MXene and g-C3N4The mixture of precursor species, calcining, obtains g-C3N4/ MXene composite materials, wherein g-C3N4Before
Drive a concentration of 0.1~0.5g/ml of body substance in a solvent, MXene materials and g-C3N4The mass ratio of precursor species is 0.01
~0.3:1.
2. a kind of g-C described in accordance with the claim 13N4The preparation method of/MXene composite materials, which is characterized in that the step
Suddenly MAX phases are Ti in (1)3AlC2Or Ti2AlC, MXene material correspond to Ti3C2Or Ti2C。
3. a kind of g-C described in accordance with the claim 13N4The preparation method of/MXene composite materials, which is characterized in that the step
Suddenly whipping temp is 20~80 DEG C in (1), and mixing time is 10~30h；Cleaning be with deionized water clean to pH be 6~7.
4. a kind of g-C described in accordance with the claim 13N4The preparation method of/MXene composite materials, which is characterized in that the step
Suddenly dry, re-dry is dried in vacuo at 20~80 DEG C in (1).
5. a kind of g-C described in accordance with the claim 13N4The preparation method of/MXene composite materials, which is characterized in that the step
Suddenly it is 20~80 DEG C to continue whipping temp in (1), continue mixing time be 12~for 24 hours；Clean again be clean 2 with deionized water~
3 times.
6. a kind of g-C described in accordance with the claim 13N4The preparation method of/MXene composite materials, which is characterized in that the step
Suddenly g-C in (2)3N4Precursor species are thiocarbamide or melamine；Solvent is water.
7. a kind of g-C described in accordance with the claim 13N4The preparation method of/MXene composite materials, which is characterized in that the step
Suddenly whipping temp is 20~80 DEG C in (2), and mixing time is 1~2h；Continue mixing time be 10~for 24 hours.
8. a kind of g-C described in accordance with the claim 13N4The preparation method of/MXene composite materials, which is characterized in that the step
Suddenly the technological parameter of calcining is in (2)：Calcination temperature is 500~600 DEG C, and calcination time is 1~10h, and heating rate is 1~10
DEG C/min, calcination atmosphere is air, nitrogen or argon gas.
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