CN109574013A - A kind of Nb4C3TxThe preparation method of-MXene film - Google Patents
A kind of Nb4C3TxThe preparation method of-MXene film Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 33
- 229910019762 Nb4C3 Inorganic materials 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 239000007790 solid phase Substances 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 238000001272 pressureless sintering Methods 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 230000002349 favourable effect Effects 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 7
- 239000012071 phase Substances 0.000 abstract description 3
- 230000001376 precipitating effect Effects 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 abstract description 2
- 230000009514 concussion Effects 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 abstract description 2
- 229910021641 deionized water Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000967 suction filtration Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- -1 Isopropyl amine Chemical class 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910009819 Ti3C2 Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000012769 display material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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Abstract
A kind of Nb4C3TxThe preparation method of-MXene film belongs to the preparation technical field of two-dimensional material MXene, includes the following steps: firstly, preparing pure ternary layered ceramic powder Nb using solid-phase sintering method4AlC3；Secondly, the MAX phase powder in step 1 is slowly added into HF acid solution, selective etch falls Al atom, obtains MXene material, and resulting product is added deionized water, is centrifuged, and obtains solid precipitating；Finally, organic solvent is added into solid precipitating, Nb is can be obtained in centrifugation concussion separation, suction filtration after stirring4C3Tx- MXene film.Nb provided by the invention4C3TxPreparation method is simple for film, and yield is high, and the organic solvent used is cheap, is conducive to carry out industrialized production.
Description
Technical field
The invention belongs to the preparation technical fields of two-dimensional material MXene, are related to a kind of Nb4C3TxDelamination is at flexible membrane
Preparation method.
Technical background
Start within 2011, new two-dimensional material transition metal carbide/nitride (MXene) progresses into the view of people
Open country, this New Two Dimensional material have been applied in many fields, for example, hydrogen stores, photocatalysis, sewage purification etc..And when it
When using electrode for energy storage material, the performance for the excellent benefit that it is shown causes the concern of countries in the world researcher.
In the MXene material of huge number (such as Ti3C2、V2C、Nb2C、Ti2C etc.), Nb4C3TxIt is reported conduction
One of highest MXene material of rate is the candidate of most desired negative electrode material.
In the preparation method of traditional electrode material, needs to use copper foil as collector, PVDF, conductive auxiliary agent is added
Deng process is not only cumbersome, but also needs to increase corresponding cost.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of Nb4C3TxThe preparation method of-MXene film.It should
Nb4C3TxThe preparation of-MXene flexible membrane not only increases ductility, the plasticity of material, it might even be possible to directly as electrode material,
Reduce material cost, labour cost etc., more conducively industrialization development.
To achieve the goals above, technical scheme is as follows:
A kind of Nb4C3TxThe preparation method of-MXene film, includes the following steps:
Step 1: pure ternary layered ceramic powder Nb is prepared using solid-phase sintering method4AlC3
Nb powder, Al powder, graphite are subjected to ball milling by the atomic ratio of 4:1.5:2.7, obtain dry mixed-powder；In argon
It under gas shielded, is placed on carrying out pressureless sintering in high temperature process furnances, it is small to rise to heat preservation 4-6 at 1500-1650 DEG C from room temperature
When, solid phase material Nb is obtained after dropping to room temperature4AlC3。
Step 2: the Nb that step 1 is obtained4AlC3Powder is slowly added in HF solution, at room temperature magnetic agitation 130-150
Hour, selective etch falls Al atom, and after reaction, product is added deionized water and is centrifuged, solid precipitating is obtained,
That is MXene powder Nb4C3Tx；The Nb4C3TxIn TxIndicate material surface functional group, such as O2-、OH-、F-。
Step 3: Nb obtained in step 24C3TxIt is added in organic solvent in powder, wherein Nb4C3TxConcentration is 28-
30mg/mL；Stirring is centrifugated after 10-20 hours, obtains the Nb of favorable dispersibility4C3TxAqueous solution takes out layering solution
Filter, can obtain MXene flexible membrane after drying.The organic solvent include dimethyl sulfoxide DMSO, isopropylamine, concentration be 25%
Tetramethylammonium hydroxide (TMAOH).
In step 1, the purity of described Nb, Al and C are respectively mass fraction not less than 99.95%, 99.8% and
99%.
In step 1, the heating rate in the high temperature process furnances is 5 DEG C/min.
In step 2, the mass fraction of the HF is 40-50%, centrifugation rate 3500r/min.
The beneficial effects of the present invention are: the present invention is proposed using organic solvent TMAOH to Nb4C3TxCarry out intercalation separation.It should
Organic solvent is able to enter interlayer, by concussion, effectively increase interlamellar spacing, enable most of molecules with monolithic layer or
The form of few layer exists, and flexible good film can be obtained by simply filtering later.Manufacture craft is simple, and yield is high,
Nb4C3TxThe successful preparation of film will be a quantum jump of energy storage field, and more promotion and application are worth.
Detailed description of the invention
Fig. 1 is the Nb obtained using the embodiment of the present invention 44C3TxThe XRD effect picture of-MXene film.
Fig. 2 is the Nb obtained using the embodiment of the present invention 44C3TxThe TEM of-MXene film schemes.
Fig. 3 is the Nb obtained using the embodiment of the present invention 44C3TxThe SEM of-MXene film schemes.
Specific embodiment
The present invention is further detailed by example below with reference to attached drawing.
Embodiment 1
Nb powder, Al powder, graphite are subjected to ball milling according to atomic ratio 4:1.5:2.7, after obtaining dry mixed-powder,
Argon gas protection is lower in high temperature process furnances carries out pressureless sintering, keeps the temperature 6 hours at 1500 DEG C, obtains solid phase material after dropping to room temperature
Nb4AlC3。
By Nb4AlC3Powder is slowly added in the HF solution that mass fraction is 40%, and it is small to carry out magnetic agitation 130 at room temperature
When, it is centrifuged after reaction, obtains MXene powder Nb4C3Tx。
In Nb4C3TxIt is added in dimethyl sulfoxide (DMSO) solution in powder, wherein Nb4C3TxConcentration is 28mg/mL；Room temperature
Lower magnetic agitation 10 hours after centrifuge separation, filters obtained aqueous solution, Nb is obtained after drying4C3TxPowder.
Embodiment 2
Nb powder, Al powder, graphite are subjected to ball milling according to atomic ratio 4:1.5:2.7, after obtaining dry mixed-powder,
Argon gas protection is lower in high temperature process furnances carries out pressureless sintering, keeps the temperature 5 hours at 1600 DEG C, obtains solid phase material after dropping to room temperature
Nb4AlC3。
By Nb4AlC3Powder is slowly added in the HF solution that mass fraction is 50%, and it is small to carry out magnetic agitation 150 at room temperature
When, it is centrifuged after reaction, obtains MXene powder Nb4C3Tx。
In Nb4C3TxIt is added in isopropyl amine aqueous solution in powder, wherein Nb4C3TxConcentration is 29mg/mL；Magnetic agitation at room temperature
20 hours, after centrifuge separation, obtained aqueous solution is filtered, Nb is obtained after drying4C3TxPowder.
Embodiment 3
Nb powder, Al powder, graphite are subjected to ball milling according to atomic ratio 4:1.5:2.7, after obtaining dry mixed-powder,
Argon gas protection is lower in high temperature process furnances carries out pressureless sintering, keeps the temperature 4 hours at 1650 DEG C, obtains solid phase material after dropping to room temperature
Nb4AlC3。
By Nb4AlC3It is that it is small to carry out magnetic agitation 140 at room temperature in 50%HF acid solution that powder, which is slowly added to mass fraction,
When, it is centrifuged after reaction, obtains MXene powder Nb4C3Tx。
In Nb4C3TxIsopropyl amine aqueous solution is added in powder, wherein Nb4C3Tx concentration is 30mg/mL, at room temperature magnetic agitation
15 hours, after centrifuge separation, obtained aqueous solution is filtered, Nb is obtained after drying4C3TxPowder.
Embodiment 4
Nb powder, Al powder, graphite are subjected to ball milling according to atomic ratio 4:1.5:2.7, after obtaining dry mixed-powder,
Argon gas protection is lower in high temperature process furnances carries out pressureless sintering, keeps the temperature 4 hours at 1650 DEG C, obtains solid phase material after dropping to room temperature
Nb4AlC3。
By Nb4AlC3Powder is slowly added in HF solution, is carried out magnetic agitation 140 hours, is carried out at room temperature after reaction
Centrifuge separation, obtains MXene powder Nb4C3Tx。
In Nb4C3TxTetramethyl ammonium hydroxide solution is added in powder, wherein Nb4C3Tx concentration is 30mg/mL, at room temperature
Stirring 10 hours, centrifuge separation, obtains the Nb of favorable dispersibility4C3TxAqueous solution filters layering solution, after drying
To flexible good Nb4C3TxFilm.Nb4C3Tx film obtained in the present invention is pure phase, does not contain any miscellaneous phase.
To Nb4C3TxFilm carries out XRD test, and test results are shown in figure 1, and material stratiform attribute is excellent as the result is shown.TEM
Shown in test result Fig. 2, display material exists in the form of single layer or few layer.Meanwhile film has preferable flexibility.
Embodiment described above only expresses embodiments of the present invention, and but it cannot be understood as to the invention patent
Range limitation, it is noted that for those skilled in the art, without departing from the inventive concept of the premise, also
Several modifications and improvements can be made, these are all belonged to the scope of protection of the present invention.
Claims (10)
1. a kind of Nb4C3TxThe preparation method of-MXene film, it is characterised in that following steps:
Step 1: Nb powder, Al powder, graphite are subjected to ball milling by the atomic ratio of 4:1.5:2.7, obtain dry mixed-powder；
Under protection of argon gas, it is placed on carrying out pressureless sintering in high temperature process furnances, is risen at 1500-1650 DEG C from room temperature and keep the temperature 4-
6 hours, solid phase material Nb was obtained after dropping to room temperature4AlC3；
Step 2: the Nb that step 1 is obtained4AlC3Powder is slowly added in HF solution, and magnetic agitation 130-150 is small at room temperature
When, it is centrifuged after reaction, obtains MXene powder Nb4C3Tx, Nb4C3TxIn TxIndicate material surface functional group；
Step 3: Nb obtained in step 24C3TxIt is added in organic solvent in powder, wherein Nb4C3TxConcentration is 28-30mg/
mL；Stirring is centrifugated after 10-20 hours, obtains the Nb of favorable dispersibility4C3TxAqueous solution filters layering solution, dries
MXene flexible membrane can be obtained after dry.
2. a kind of Nb according to claim 14C3TxThe preparation method of-MXene film, which is characterized in that described in step 2
Surface functional group includes O2-、OH-、F-。
3. a kind of Nb according to claim 1 or 24C3TxThe preparation method of-MXene film, which is characterized in that step 3 institute
The organic solvent stated includes dimethyl sulfoxide DMSO, isopropylamine, the tetramethylammonium hydroxide (TMAOH) that concentration is 25%.
4. a kind of Nb according to claim 1 or 24C3TxThe preparation method of-MXene film, which is characterized in that step 1 institute
The purity of Nb, Al and C for stating are respectively mass fraction not less than 99.95%, 99.8% and 99%.
5. a kind of Nb according to claim 34C3TxThe preparation method of-MXene film, which is characterized in that described in step 1
The purity of Nb, Al and C are respectively mass fraction not less than 99.95%, 99.8% and 99%.
6. a kind of Nb described according to claim 1 or 2 or 54C3TxThe preparation method of-MXene film, which is characterized in that step 2
The mass fraction of the HF is 40-50%, centrifugation rate 3500r/min.
7. a kind of Nb according to claim 34C3TxThe preparation method of-MXene film, which is characterized in that described in step 2
The mass fraction of HF is 40-50%, centrifugation rate 3500r/min.
8. a kind of Nb according to claim 44C3TxThe preparation method of-MXene film, which is characterized in that described in step 2
The mass fraction of HF is 40-50%, centrifugation rate 3500r/min.
9. a kind of Nb described according to claim 1 or 2 or 5 or 7 or 84C3TxThe preparation method of-MXene film, which is characterized in that
Heating rate in high temperature process furnances described in step 1 is 5 DEG C/min.
10. a kind of Nb according to claim 64C3TxThe preparation method of-MXene film, which is characterized in that described in step 1
High temperature process furnances in heating rate be 5 DEG C/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112226644A (en) * | 2020-09-25 | 2021-01-15 | 河海大学 | MXene reinforced copper-based composite material and preparation method thereof |
| CN112938978A (en) * | 2021-03-03 | 2021-06-11 | 盐城工学院 | Preparation method of vanadium carbide nanosheet |
| CN116425160A (en) * | 2023-04-21 | 2023-07-14 | 四川金时新能科技有限公司 | Nb (Nb) alloy 4 C 3 T x MXene material and rapid preparation method thereof |
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| CN112938978A (en) * | 2021-03-03 | 2021-06-11 | 盐城工学院 | Preparation method of vanadium carbide nanosheet |
| CN116425160A (en) * | 2023-04-21 | 2023-07-14 | 四川金时新能科技有限公司 | Nb (Nb) alloy 4 C 3 T x MXene material and rapid preparation method thereof |
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Application publication date: 20190405 |
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