CN108455611A - A kind of preparation method of multi-slice two-dimensional layer transition metal carbide material MXene - Google Patents
A kind of preparation method of multi-slice two-dimensional layer transition metal carbide material MXene Download PDFInfo
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- CN108455611A CN108455611A CN201810196427.1A CN201810196427A CN108455611A CN 108455611 A CN108455611 A CN 108455611A CN 201810196427 A CN201810196427 A CN 201810196427A CN 108455611 A CN108455611 A CN 108455611A
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of preparation methods of multi-slice two-dimensional layer transition metal carbide material MXene, belong to carbide composite material field.Two-dimensional layer transition metal carbide material MXene is with Ti3AlC2, Ti2AlC, Ti3SiC2, Ti4SiC3In it is one or more be base material, the heating stirring under the reaction environment of ammonium fluoride and hydrochloric acid, it is neutral left and right to be centrifuged later to PH, is transferred in dimethyl sulfoxide solvent, is added in multifunction micro reactor after stirring and prepares two-dimensional layer transition metal carbide.The preparation process is simple, easy-to-operate, and pollution is small, prepares the two-dimensional layered structure with uniform composition and structure.This two-dimensional layer material interlamellar spacing is clear, and structural stability is good.
Description
Technical field
The invention belongs to carbide composite material fields, and in particular to a kind of multi-slice two-dimensional layer transition metal carbide
The preparation method of material MXene.
Background technology
Currently, two-dimensional material is more and more, it is extensively studied concern since its remarkable performance causes, is studied
Most two-dimensional materials is graphene, it has very high inherency mobility, good electric conductivity and excellent mechanical performance
Stability, to realize flexible extensive use.However New Two Dimensional stratiform transition metal carbide MXene has graphene high
It is the characteristics of specific surface area, high conductivity, flexibly adjustable but also with component, the advantages such as minimum nanometer thickness is controllable, in energy storage, inhale
The fields such as attached, sensor, conductive filler show huge potentiality.The preparation of two-dimensional layer transition metal carbide is mainly sharp
It is prepared with hf etching, the method operational hazards, environmental pollution is serious, and prepares the transition metal carbonization less than monolithic layer
Object, it is less efficient.
In order to avoid using the harm brought in hydrofluoric acid preparation process, ammonium fluoride and hydrochloric acid being selected to prepare two-dimensional layer
Transition metal carbide reduces the harm that hydrofluoric acid generates human body.Select multifunctional reactor as supplementary instrument, energy simultaneously
Enough prepare multi-slice, efficient two-dimensional layer transition metal carbide.And preparation process is easy to operate, can reduce to environment
Pollution.The domestic research to two-dimensional layer transition metal carbide MXene at present is mainly in ultracapacitor, sensor, urges
Agent etc., it is less in the application study of rubber, plastic applications.
Invention content
The purpose of the present invention is be directed to it is of the existing technology be unable to get single layer MXene nanometer sheets, a kind of two dimension is provided
The preparation method of stratiform transition metal carbide.Preparation process of the present invention is simple, while energy conservation and environmental protection, before having application well
Scape.
The present invention stirs transition metal carbide in dimethyl sulphoxide solution, is dissolved in deionized water after centrifugal drying
It is then added in microreactor and carries out hydro-thermal reaction, prepare monolithic layer two dimension transition metal carbide, be greatly improved
The preparation efficiency of multi-slice two dimension transition metal carbide.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of multi-slice two-dimensional layer transition metal carbide material MXene, includes the following steps：
(1) ammonium fluoride is dissolved in hydrochloric acid, is stirred in the three-necked flask of polytetrafluoroethylene (PTFE), obtains mixture；
(2) titanium carbide is added in the three-necked flask equipped with step (1) mixture, in 40-60 DEG C of constant temperature oil bath
It is stirred in pot, then centrifuges removing supernatant, be dried in vacuo, obtain two-dimentional transition metal carbide；
(3) the obtained two-dimentional transition metal carbide of step (2) is added in dimethyl sulfoxide solvent and is stirred, then centrifuged
It is separated off supernatant, is dried in vacuo；
(4) step (3) obtained product is mixed with water, is added in multifunction micro reactor and carries out water at high temperature
Thermal response is collected product, then is dried in vacuo to get multi-slice two-dimensional layer transition metal carbide material MXene.
Preferably, the titanium carbide, ammonium fluoride, hydrochloric acid, dimethyl sulfoxide (DMSO), water mass ratio be (2-4)：(1-3)：
(20-40)：(10-20)：(80-90), further preferably (2-4)：(1-3)：(20-40)：(10-20)：80.
Preferably, the time of step (1) described stirring is 4-6 minutes.
Preferably, step (2) described titanium carbide be titanium aluminum carbide, titanium carbon tin, silicon titanium-carbide it is one or more.
It is further preferred that the titanium carbide is Ti3AlC2、Ti2AlC、Ti3SiC2And Ti4SiC3In one kind or several
Kind.
Preferably, the time that titanium carbide is added in step (2) is 5-15 minutes.
Preferably, step (2) stirring is the speed high-speed stirred 12-24h with 200-400rpm.
Preferably, the vacuum drying of step (2), step (3) is dried in vacuo 8-12h under the conditions of being 40-60 DEG C.
Preferably, step (3) stirring is to stir 1-2h with the speed of 100-200rpm.
Preferably, the temperature of step (4) described hydro-thermal reaction is 150-200 DEG C.
Preferably, the time of step (4) described hydro-thermal reaction is 30-40 minutes.
Preferably, step (4) vacuum drying is dried in vacuo 4-6h under the conditions of being 40-60 DEG C.
Compared with prior art, the invention has the advantages that：
1, preparation method of the invention is not related to poisonous and hazardous HF solution, can be by the Al in metal carbides, Si yet
Layer erodes completely, obtain between lamella will not stick to each other MXene.
2, present invention gained MXene has uniform composition and structure, and interlamellar spacing is clear, and structural stability is good.
3, the preparation method is that it is a kind of simple, efficiently, the method for obtaining two-dimensional nano lamella of safety non-pollution.
4, two-dimensional layer transition metal carbide material MXene prepared by the present invention can be in aqueous solution with form of single sheet
It is evenly dispersed.
Description of the drawings
Fig. 1 is the Ti that embodiment 1 obtains3C2The electron scanning micrograph of nanometer sheet.
Fig. 2 is the Ti that embodiment 2 obtains2The electron scanning micrograph of C nano piece.
Fig. 3 is the Ti that embodiment 3 obtains4C3The electron scanning micrograph of nanometer sheet.
Fig. 4 is the Ti that embodiment 1 obtains3C2Nanometer sheet and Ti3AlC2X-ray diffractogram.
Specific implementation mode
The specific implementation of the present invention is further described below in conjunction with example and attached drawing, but embodiments of the present invention
It is without being limited thereto.
Embodiment 1
(1) ammonium fluoride for weighing 2g is dissolved in 30ml concentrated hydrochloric acids (a concentration of 35wt%), in three mouthfuls of burnings of polytetrafluoroethylene (PTFE)
It is stirred 5 minutes in bottle.
(2) by 3gTi3AlC2In being slowly added into the three-necked flask of step (1) in 10 minutes, in 50 DEG C of constant temperature oil bath
Pot is centrifuged with the speed high-speed stirred 18h of 300rpm and removes supernatant, 10h is dried in vacuo at 50 DEG C.
(3) by the obtained two-dimentional transition metal carbide Ti of step (2)3C2It is added in the dimethyl sulfoxide solvent of 15ml
1.5h is stirred, centrifuges and removes supernatant, 50 DEG C of vacuum drying 10h.
(4) by step (3) obtained Ti3C2It mixes, is added in multifunction micro reactor with 80ml deionized waters
Hydro-thermal reaction 35 minutes under 175 DEG C of high temperature, collect reactor in product to get two-dimensional layer transition metal carbide Ti3C2。
(5) by the obtained two-dimensional layer transition metal carbide Ti of step (4)3C2It is dried in vacuo 5h at 50 DEG C.
MXene (Ti obtained by the present embodiment3C2) nanometer sheet electron scanning micrograph as shown in Figure 1, as seen from the figure
The Ti arrived3C2Nanometer sheet is laminar structured.MXene (Ti obtained by the present embodiment3C2) nanometer sheet and Ti3AlC2X-ray diffraction
Figure is as shown in figure 4, the Ti obtained as seen from the figure3C2It is that strong peak disappears at 39 ° in the angle of diffraction, illustrates that Al elements are etched away,
It is MXene (Ti to obtain product3C2) nanometer sheet.
Embodiment 2
(1) ammonium fluoride for weighing 2g is dissolved in 30ml concentrated hydrochloric acids (a concentration of 35wt%), in three mouthfuls of burnings of polytetrafluoroethylene (PTFE)
It is stirred 10 minutes in bottle.
(2) by 3gTi2AlC in 10 minutes in being slowly added into the three-necked flask of step (1), in 50 DEG C of constant temperature oil bath
Pot is centrifuged with the speed high-speed stirred 18h of 300rpm and removes supernatant, 10h is dried in vacuo at 50 DEG C.
(3) by the obtained two-dimentional transition metal carbide Ti of step (2)2C is added in the dimethyl sulfoxide solvent of 15ml
1.5h is stirred, centrifuges and removes supernatant, 50 DEG C of vacuum drying 10h.
(4) by step (3) obtained Ti2C is mixed with 80ml deionized waters, is added in multifunction micro reactor
Hydro-thermal reaction 35 minutes under 175 DEG C of high temperature, collect reactor in product to get two-dimensional layer transition metal carbide Ti2C。
(5) by the obtained two-dimensional layer transition metal carbide Ti of step (4)2C is dried in vacuo 5h at 50 DEG C.
MXene (Ti obtained by the present embodiment2C) electron scanning micrograph of nanometer sheet as shown in Fig. 2, obtain as seen from the figure
The Ti arrived2C nano piece interlamellar spacing is clear, and stable structure is good.
Embodiment 3
(1) ammonium fluoride for weighing 2g is dissolved in 30ml concentrated hydrochloric acids (a concentration of 35wt%), in three mouthfuls of burnings of polytetrafluoroethylene (PTFE)
It is stirred 10 minutes in bottle.
(2) by 3gTi4SiC3In being slowly added into the three-necked flask of step (1) in 10 minutes, in 50 DEG C of constant temperature oil bath
Pot is centrifuged with the speed high-speed stirred 18h of 300rpm and removes supernatant, 10h is dried in vacuo at 50 DEG C.
(3) by the obtained two-dimentional transition metal carbide Ti of step (2)4C3It is added in the dimethyl sulfoxide solvent of 15ml
1.5h is stirred, centrifuges and removes supernatant, 50 DEG C of vacuum drying 10h.
(4) by step (3) obtained Ti4C3It mixes, is added in multifunction micro reactor with 80ml deionized waters
Hydro-thermal reaction 35 minutes under 175 DEG C of high temperature, collect reactor in product to get two-dimensional layer transition metal carbide Ti4C3。
(5) by the obtained metal carbides Ti of step (4)4C3It is dried in vacuo 5h at 50 DEG C.
MXene (Ti obtained by the present embodiment4C3) nanometer sheet electron scanning micrograph as shown in figure 3, as seen from the figure
The Ti arrived4C3Nanometer sheet forms uniform, stable structure, and interlamellar spacing is clear.
Claims (10)
1. a kind of preparation method of multi-slice two-dimensional layer transition metal carbide material MXene, which is characterized in that including following
Step：
(1) ammonium fluoride is dissolved in hydrochloric acid, is stirred in the three-necked flask of polytetrafluoroethylene (PTFE), obtains mixture；
(2) titanium carbide is added in the three-necked flask equipped with step (1) mixture, in 40-60 DEG C of thermostatical oil bath
Stirring, then removing supernatant is centrifuged, it is dried in vacuo, obtains two-dimentional transition metal carbide；
(3) the obtained two-dimentional transition metal carbide of step (2) is added in dimethyl sulfoxide solvent and is stirred, then centrifuged
Remove supernatant, vacuum drying；
(4) step (3) obtained product is mixed with water, it is anti-to carry out hydro-thermal at high temperature in addition multifunction micro reactor
It answers, collects product, then be dried in vacuo to get multi-slice two-dimensional layer transition metal carbide material MXene.
2. preparation method according to claim 1, which is characterized in that the titanium carbide, ammonium fluoride, hydrochloric acid, dimethyl
Sulfoxide, water mass ratio be (2-4)：(1-3)：(20-40)：(10-20)：(80-90).
3. preparation method according to claim 1, it is characterised in that：Step (2) described titanium carbide is Ti3AlC2、
Ti2AlC、Ti3SiC2And Ti4SiC3One or more of.
4. preparation method according to claim 1, which is characterized in that the time that titanium carbide is added in step (2) is 5-
15 minutes.
5. preparation method according to claim 1, which is characterized in that step (2) stirring is with 200-400rpm
Speed high-speed stirred 12-24h.
6. preparation method according to claim 1, which is characterized in that the vacuum drying of step (2), step (3) is 40-
It is dried in vacuo 8-12h under the conditions of 60 DEG C.
7. preparation method according to claim 1, which is characterized in that step (3) stirring is with 100-200rpm
Speed stirs 1-2h.
8. preparation method according to claim 1, which is characterized in that the temperature of step (4) described hydro-thermal reaction is 150-
200℃。
9. preparation method according to claim 1, which is characterized in that the time of step (4) described hydro-thermal reaction is 30-40
Minute.
10. preparation method according to claim 1, which is characterized in that step (4) vacuum drying is 40-60 DEG C of item
It is dried in vacuo 4-6h under part.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109607603A (en) * | 2018-12-04 | 2019-04-12 | 北京航空航天大学 | A method of control MXene two-dimensional material degradation |
| CN109896524A (en) * | 2019-01-30 | 2019-06-18 | 合肥国轩高科动力能源有限公司 | A kind of preparation method and applications of two dimensional crystal MXene nano material |
| CN110510613A (en) * | 2019-08-29 | 2019-11-29 | 东北大学 | A kind of preparation method of two-dimensional metallic carbonitride MXene |
| CN113651327A (en) * | 2021-07-19 | 2021-11-16 | 西安电子科技大学芜湖研究院 | Method for synthesizing and collecting MXene material under assistance of organic solvent |
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| CN103771402A (en) * | 2013-12-30 | 2014-05-07 | 华南农业大学 | Graphene preparation method |
| CN105197992A (en) * | 2015-09-10 | 2015-12-30 | 同济大学 | Preparation method of lamellar stacking titanium dioxide nanoparticles |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607603A (en) * | 2018-12-04 | 2019-04-12 | 北京航空航天大学 | A method of control MXene two-dimensional material degradation |
| CN109607603B (en) * | 2018-12-04 | 2020-01-10 | 北京航空航天大学 | Method for controlling degradation of MXene two-dimensional material |
| CN109896524A (en) * | 2019-01-30 | 2019-06-18 | 合肥国轩高科动力能源有限公司 | A kind of preparation method and applications of two dimensional crystal MXene nano material |
| CN110510613A (en) * | 2019-08-29 | 2019-11-29 | 东北大学 | A kind of preparation method of two-dimensional metallic carbonitride MXene |
| CN113651327A (en) * | 2021-07-19 | 2021-11-16 | 西安电子科技大学芜湖研究院 | Method for synthesizing and collecting MXene material under assistance of organic solvent |
| CN113651327B (en) * | 2021-07-19 | 2023-02-28 | 西安电子科技大学芜湖研究院 | Method for synthesizing and collecting MXene material under assistance of organic solvent |
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Application publication date: 20180828 |