CN116161661A - Method for preparing MXene two-dimensional material by gas phase etching MAX phase and application - Google Patents
Method for preparing MXene two-dimensional material by gas phase etching MAX phase and application Download PDFInfo
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- 238000005530 etching Methods 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 76
- 239000002243 precursor Substances 0.000 claims abstract description 38
- 239000003708 ampul Substances 0.000 claims abstract description 32
- 238000005520 cutting process Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 229910021589 Copper(I) bromide Inorganic materials 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 55
- 239000007789 gas Substances 0.000 description 49
- 239000000758 substrate Substances 0.000 description 8
- 125000000524 functional group Chemical group 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000001039 wet etching Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
The invention belongs to the technical field of novel two-dimensional materials, and particularly relates to a method for preparing an MXene two-dimensional material by vapor etching of MAX phase and application thereof. The invention discloses a method for preparing an MXene two-dimensional material by gas phase etching of MAX phase, which comprises the steps of placing MAX phase powder and etching gas precursor in a sealed ampoule according to a certain molar ratio; placing the vacuum sealed ampoule tube in a two-section temperature-control tube furnace, placing one end filled with MAX phase powder and etching gas precursor in a high temperature area, placing the other end in a low temperature area, and naturally cooling to room temperature after the reaction is finished; cutting the cooled ampoule tube, and collecting MXene powder obtained by gas etching MAX phase powder. The simple etching steps and wide application range make the method suitable for large-scale preparation, production and application of MXene.
Description
Technical Field
The invention belongs to the technical field of novel two-dimensional materials, and particularly relates to a method for preparing an MXene two-dimensional material by vapor etching of MAX phase and application thereof.
Background
MXene as an emerging secondThe dimensional material has very wide application prospect, such as being applied to battery electrodes, supercapacitor electrodes, magnetic shielding, catalytic materials and the like. The composite material is mainly prepared by etching a precursor MAX, and MX elements and A layer elements are alternately combined to form a layered structure, wherein M represents early transition metal elements (such as Ti, nb, V, mo and the like), A represents main group elements (such as Al, si, ga, sn and the like) and some transition elements (such as Zn, cd and the like), and X represents C, N. becausethe"M-A"metalbondisoftenweakerthanthe"M-X"covalentbond,theAlayerelementscanbeselectivelyetchedtogiveacompoundoftheformulaM n+1 X n T x (n=1, 2, 3), wherein Tx represents a surface functional group, the specific element depends on the etching environment. The traditional MXene is mainly prepared by wet etching MAX phase, such as HF acid aqueous solution etching with danger, HCl fluoridized salt aqueous solution etching, halogen etching dissolved in organic solvent, molten salt etching and the like. Wet etching usually requires placing MAX phase in a solution or molten salt, and after etching, performing multi-step procedures such as MXene and etchant separation, washing, drying, etc. In the etching and subsequent processing processes, the MXene can inevitably oxidize, so that the conductivity of the MXene is reduced, and the application of the MXene is not facilitated. Meanwhile, in the etching process, a strong etchant such as HF can inevitably etch the M element while etching the A layer element, and M vacancies are formed on the MXene, so that defects exist on the MXene structure, and the long-term stable existence of the MXene is not facilitated.
Disclosure of Invention
Aiming at the prior art, the invention provides a method for preparing the MXene two-dimensional material by vapor etching MAX phase, which has simple preparation process and no need of excessive subsequent processing steps and is not easy to oxidize and denature.
In order to solve the technical problems, the invention relates to a method for preparing an MXene two-dimensional material by vapor phase etching MAX phase, which comprises the following steps:
firstly, placing MAX phase powder and etching gas precursor in a sealed ampoule tube according to a certain molar ratio, wherein the etching gas precursor needs to be additionally placed in the lining ampoule tube to isolate the MAX phase powder and the etching gas precursor, and vacuum sealing the ampoule tube with the lining ampoule tube, wherein the vacuum degree is lower than 5Pa during tube sealing;
placing the ampoule tube sealed in the vacuum in the first step in a two-section temperature-control tube furnace, placing one end filled with MAX phase powder and etching gas precursor in a high temperature area, placing the other end in a low temperature area, heating at a speed of 10 ℃/min, etching for 12-24 hours, and naturally cooling to room temperature after the reaction is finished;
and thirdly, cutting the cooled ampoule tube obtained in the second step, and collecting MXene powder obtained by gas etching of MAX phase powder.
Another object of the present invention is to provide Ti 3 C 2 Br 2 The preparation method of the MXene powder comprises the following steps:
step one, ti3AlC 2 Powder and etching gas precursor CuBr 2 Placed in a sealed ampoule at a molar ratio (Al: br=1:10), wherein the etching gas precursor CuBr 2 The ampoule tube with the lining ampoule tube is required to be additionally placed in the lining ampoule tube to isolate MAX phase powder and etching gas precursor, and the ampoule tube with the lining ampoule tube is subjected to vacuum tube sealing, wherein the vacuum degree is lower than 5Pa during tube sealing;
step two, placing the ampoule tube subjected to vacuum sealing in the step one in a two-section temperature-control tube furnace, and filling MAX phase Ti3AlC2 powder and etching gas precursor CuBr 2 One end of the substrate is placed in a high temperature area (600 ℃), the other end of the substrate is placed in a low temperature area (200 ℃), the heating speed is 10 ℃/min, the etching time is 12 hours, and the substrate is naturally cooled to room temperature after the reaction is finished;
cutting the cooled ampoule pipe obtained in the step two, and collecting Br 2 Gas (from etching gas precursor CuBr 2 Release) etch MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 Br 2 MXene powder.
Another object of the present invention is to provide Ti 3 C 2 I x MXA process for the preparation of an ene powder, wherein,
in the first step, the etching gas precursor is I 2 ，I 2 Need not to place in lining ampoule, the mole ratio is Al: i=1: 5, a step of;
in the second step, MAX phase Ti is filled 3 AlC 2 Powder and etching gas precursor I 2 One end of the substrate is placed in a high temperature region (600 ℃) and the other end is placed in a low temperature region (300 ℃) and the etching time is 24 hours;
in step three, collect I 2 Gas etching MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 I x MXene powder.
Another object of the present invention is to provide Ti 3 C 2 Cl 2 A method for preparing MXene powder, wherein,
in the first step, the etching gas precursor is FeCl 3 The molar ratio is Al: cl=1: 15;
in the second step, MAX phase Ti is filled 3 AlC 2 Powder and etching gas precursor FeCl 3 Is placed at a high temperature region (650 ℃), and at a low temperature region (300 ℃);
in step three, cl is collected 2 Gas etching MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 Cl 2 MXene powder.
Another object of the present invention is to provide Ti 3 C 2 Br 2 A method for preparing MXene powder, wherein,
in the first step, the etching gas is HBr, and the molar ratio is Al: hbr=1: 5, a step of;
in the second step, MAX phase Ti is filled 3 AlC 2 One end of the powder was placed in a high temperature zone (600 ℃);
in the third step, collecting HBr gas to etch MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 Br 2 MXene powder.
Another object of the present invention is to provide Ti 3 C 2 I x A method for preparing MXene powder, wherein,
in the first step, the etching gas is HI, and the molar ratio is Al: hi=1: 5, a step of;
in the second step, MAX phase Ti is filled 3 AlC 2 One end of the powder was placed in a high temperature zone (600 ℃);
in the third step, HI gas is collected to etch MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 I x MXene powder.
It is a final object of the present invention to provide Ti 3 C 2 Cl 2 A method for preparing MXene powder, wherein,
in the first step, etching gas is HCl, and the molar ratio is Al: hcl=1: 5, a step of;
in the second step, MAX phase Ti is filled 3 AlC 2 One end of the powder was placed in a high temperature zone (600 ℃);
in the third step, the MAX phase Ti is etched by collecting HCl gas 3 AlC 2 Ti obtained from the powder 3 C 2 Cl 2 MXene powder.
Compared with the prior art, the invention has the beneficial effects that:
the method for preparing the MXene by gas-phase dry etching MAX phase can directly obtain solid MXene powder from solid MAX phase powder, greatly reduces the subsequent processing steps for preparing the MXene by wet etching, and can realize the separation of the MXene and the byproducts without subsequent further processing by vapor transport and deposition of the byproducts in a low-temperature area. And the stability of the MXene can be effectively increased by regulating the etching temperature, the M element is prevented from being etched by the etchant, and the structural integrity of the MXene is maintained. Meanwhile, different etchants can endow MXene with different surface functional groups, and the different surface functional groups can enable the MXene to have different properties, so that the application range is widened. The etching gases are different, the etching capability is also different, and the gas with stronger etching capability such as Cl 2 、Br 2 Different A elements in the MAX phase can be etched, and the method has universality for the etching of the MAX phase.
Drawings
FIG. 1 is a drawing of Ti prepared in example 1 of the present invention 3 C 2 Br 2 MXene (M Xene)Precursor MAX phase Ti 3 AlC 2 An XRD pattern of (b);
FIG. 2 is the Ti of FIG. 1 3 C 2 Br 2 MXene and its precursor MAX phase Ti 3 AlC 2 Is a visual image of the object;
FIG. 3 is the Ti of FIG. 2 3 C 2 Br 2 MXene and its precursor MAX phase Ti 3 AlC 2 Is a microscopic SEM image of (a).
Detailed Description
Example 1:
Br 2 vapor etching MAX phase Ti 3 AlC 2 Powder preparation of Ti 3 C 2 Br 2 MXene powder, the preparation steps of which are as follows:
step one, MAX phase Ti 3 AlC 2 Powder and etching gas precursor CuBr 2 According to Al: br=1: 10 in a sealed ampoule in which an etching gas precursor, cuBr, is placed 2 The ampoule tube with the lining ampoule tube is required to be additionally placed in the lining ampoule tube to isolate MAX phase powder and etching gas precursor, and the ampoule tube with the lining ampoule tube is subjected to vacuum tube sealing, wherein the vacuum degree is lower than 5Pa during tube sealing;
step two, placing the ampoule tube which is vacuum-sealed in the step one into a two-section temperature-control tube furnace, and filling MAX phase Ti 3 AlC 2 Powder and etching gas precursor CuBr 2 One end of the substrate is placed in a high temperature area (600 ℃), the other end of the substrate is placed in a low temperature area (200 ℃), the heating speed is 10 ℃/min, the etching time is 12 hours, and the substrate is naturally cooled to room temperature after the reaction is finished;
cutting the cooled ampoule pipe obtained in the step two, and collecting Br 2 Gas etching MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 Br 2 MXene powder.
Example 1 Ti 3 C 2 Br 2 MXene powder, FIG. 1 shows the Ti 3 C 2 Br 2 MXene powder and precursor MAX phase Ti thereof 3 AlC 2 XRD pattern of the powder. MAX phase Ti 3 AlC 2 The powder is etchedThe XRD characteristic peak disappeared, indicating that the Al element therein was completely etched, and Ti 3 C 2 Br 2 Peak of (004) relative to Ti of MXene powder 3 AlC 2 Offset to the left indicates that the presence of Br surface functional groups increases the interlayer spacing between mxenes. From the optical image of FIG. 2, MAX phase Ti 3 AlC 2 The powder appears grey, and the resulting MXene after etching turns black and becomes more fluffy, which is one of the macroscopic marks that MXene successfully prepares; in the microscopic SEM image of FIG. 3, MAX phase Ti 3 AlC 2 The compact layered structure of (c) is transformed after etching into a separate layered structure of the MXene classical "accordion" shape, which is also why the void-filled layered structure becomes fluffy under MXene macroscopically. The effectiveness of the etching method can be demonstrated by XRD, macroscopic optical images and SEM images.
Example 2:
the preparation process was essentially the same as in example 1, except that: in the first step, the etching gas precursor is I 2 ，I 2 Need not to place in lining ampoule, the mole ratio is Al: i=1: 5, a step of; in the second step, MAX phase Ti is filled 3 AlC 2 Powder and etching gas precursor I 2 One end of the substrate is placed in a high temperature region (600 ℃) and the other end is placed in a low temperature region (300 ℃) and the etching time is 24 hours; in step three, collect I 2 Gas etching MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 I x MXene powder.
Example 3:
the preparation process was essentially the same as in example 1, except that: in the first step, the etching gas precursor is FeCl 3 The molar ratio is Al: cl=1: 15; in the second step, MAX phase Ti is filled 3 AlC 2 Powder and etching gas precursor FeCl 3 Is placed at a high temperature region (650 ℃), and at a low temperature region (300 ℃); in step three, cl is collected 2 Gas etching MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 Cl 2 MXene powder.
Example 4:
the preparation process was essentially the same as in example 1, except that: in the first step, the etching gas is HBr, and the molar ratio is Al: hbr=1: 5, a step of; in the second step, MAX phase Ti is filled 3 AlC 2 One end of the powder was placed in a high temperature zone (600 ℃); in the third step, collecting HBr gas to etch MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 Br 2 MXene powder.
Example 5:
the preparation process was essentially the same as in example 1, except that: in the first step, the etching gas is HI, and the molar ratio is Al: hi=1: 5, a step of; in the second step, MAX phase Ti is filled 3 AlC 2 One end of the powder was placed in a high temperature zone (600 ℃); in the third step, HI gas is collected to etch MAX phase Ti 3 AlC 2 Ti obtained from the powder 3 C 2 I x MXene powder.
Example 6:
the preparation process was essentially the same as in example 1, except that: in the first step, etching gas is HCl, and the molar ratio is Al: hcl=1: 5, a step of; in the second step, MAX phase Ti is filled 3 AlC 2 One end of the powder was placed in a high temperature zone (600 ℃); in the third step, the MAX phase Ti is etched by collecting HCl gas 3 AlC 2 Ti obtained from the powder 3 C 2 Cl 2 MXene powder.
Example 7:
the preparation process was essentially the same as in example 1, except that: in the first step, the etching gas precursor is FeCl 3 The molar ratio is Al: cl=1: 15; in the second step, MAX phase Ti is filled 3 SiC 2 Powder and etching gas precursor FeCl 3 Is placed at a high temperature region (650 ℃), and at a low temperature region (300 ℃); in step three, cl is collected 2 Gas etching MAX phase Ti 3 SiC 2 Ti obtained from the powder 3 C 2 Cl 2 MXene powder.
From the above examples it can be concluded that when prepared according to the process shown in the claims, it can be prepared by different methodsAnd etching different MAX phases by gas to obtain corresponding MXene materials. The above embodiments mainly exemplify different etching gases, wherein the etching gases mainly comprise I 2 ，Br 2 ，Cl 2 HI, HBr, HCl, and etch target MAX phase including but not limited to Ti 3 AlC 2 ，Ti 3 SiC 2 Also comprises Ti 2 AlC，Ti 3 GeC 2 ，Ti 3 GaC 2 ，Ti 3 InC 2 ，Ti 3 SnC 2 And non-Ti based MAX are equal.
Although the foregoing embodiments have been described in some, but not all, embodiments of the invention, it should be understood that other embodiments may be devised in accordance with the present embodiments without departing from the spirit and scope of the invention.
Claims (8)
1. The method for preparing the MXene two-dimensional material by vapor etching MAX phase is characterized by comprising the following steps of:
firstly, placing MAX phase and etching gas or etching gas precursor in a sealed ampoule tube, and vacuum sealing the tube;
placing the ampoule tube sealed in the vacuum in the first step in a two-section temperature-control tube furnace, placing one end filled with MAX phase and etching gas precursor in a high-temperature area (600 ℃) and placing the other end in a low-temperature area (200 ℃), and naturally cooling to room temperature after the etching reaction is finished; the temperature of the high temperature area is 600-650 ℃, and the temperature of the low temperature area is 200-300 ℃;
and thirdly, cutting the cooled ampoule tube obtained in the second step, and collecting the powder of the MXene two-dimensional material.
2. The method of claim 1 wherein step one of said MAX phases comprises: ti (Ti) 3 AlC 2 Also comprises Ti 2 AlC，Ti 3 SiC 2 ，Ti 3 GeC 2 ，Ti 3 GaC 2 ，Ti 3 InC 2 ，Ti 3 SnC 2 And a non-Ti based MAX phase.
3. The method of claim 1, wherein step one the etching gas comprises: br (Br) 2 、I 2 、Cl 2 HBr, HI or HCl.
4. The method of claim 1, wherein the etching gas precursor of step one comprises CuBr 2 Or FeCl 3 。
5. The method of claim 1, wherein step one the etching gas precursor requires additional placement in the liner ampoule to isolate the MAX-phase powder from the etching gas precursor.
6. The method of claim 1, wherein when the MAX phase is Ti 3 AlC 2 Powder, etching gas precursor is CuBr 2 At the same time, the molar ratio Al: br=1: 10;
when MAX phase is Ti 3 AlC 2 Powder, etching gas precursor is I 2 ，I 2 Need not to place in lining ampoule, the mole ratio is Al: i=1: 5, a step of;
when MAX phase is Ti 3 AlC 2 Powder, etching gas precursor is FeCl 3 The molar ratio is Al: cl=1: 15;
when MAX phase is Ti 3 AlC 2 Powder, the etching gas is HBr, and the molar ratio is Al: hbr=1: 5, a step of;
when MAX phase is Ti 3 AlC 2 Powder, etching gas is HI, and the molar ratio is Al: hi=1: 5, a step of;
when MAX phase is Ti 3 AlC 2 Powder, etching gas is HCl, and the molar ratio is Al: hcl=1: 5.
7. an MXene two-dimensional material obtainable by the method of any one of claims 1 to 6.
8. Use of the MXene two-dimensional material of claim 7 as a battery electrode, supercapacitor electrode, magnetic shielding, catalytic material.
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| US20200399771A1 (en) * | 2019-06-24 | 2020-12-24 | The Hong Kong Polytechnic University | Method for hf-free facile and rapid synthesis of mxenes related compounds |
| CN114408873A (en) * | 2021-12-08 | 2022-04-29 | 中国科学院宁波材料技术与工程研究所 | Method for etching MXene material |
| CN114620728A (en) * | 2020-12-14 | 2022-06-14 | 北京航空航天大学 | Method and system for preparing two-dimensional material by gas phase method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20200399771A1 (en) * | 2019-06-24 | 2020-12-24 | The Hong Kong Polytechnic University | Method for hf-free facile and rapid synthesis of mxenes related compounds |
| CN111943207A (en) * | 2020-07-17 | 2020-11-17 | 郑州骋憬材料科技有限公司 | Method for preparing fluorine-free two-dimensional material MXene simply and in pollution-free manner |
| CN114620728A (en) * | 2020-12-14 | 2022-06-14 | 北京航空航天大学 | Method and system for preparing two-dimensional material by gas phase method |
| CN114408873A (en) * | 2021-12-08 | 2022-04-29 | 中国科学院宁波材料技术与工程研究所 | Method for etching MXene material |
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