Simple and pollution-free method for preparing fluoride-free two-dimensional material MXene

A two-dimensional material, non-polluting technology, applied in the field of nanomaterials, can solve the problems of unfavorable MXene industrialization, serious environmental pollution, shallow etching depth, etc., and achieve the effects of low cost, high purity, and reduced reaction time.

Active Publication Date: 2020-11-17
XUZHOU LANOXENE INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above method of using fluoride to prepare is relatively efficient, the preparation process is serious for environmental pollution and the large number of F-group terminal functional groups on the prepared MXene two-dimensional material greatly limits its application in the field of energy storage.
[0004] In order to solve the above problems, a method for preparing MXene two-dimensional materials by fluorine-free etching of layer A elements in the MAX phase has also appeared on the market, such as CN110540236A, using high-temperature molten salt Two-dimensional MXene materials were prepared by the method (using transition metal bromide / transition metal iodide and MAX phase reaction to prepare MXene two-dimensional materials with Br / I as the surface group), but the preparation method was carried out under normal pressure. The etching depth is shallow; and the product needs to be pickled and dried to remove impurities, and the conditions are more complicated, which is not conducive to the industrialization of MXene production

Method used

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  • Simple and pollution-free method for preparing fluoride-free two-dimensional material MXene
  • Simple and pollution-free method for preparing fluoride-free two-dimensional material MXene
  • Simple and pollution-free method for preparing fluoride-free two-dimensional material MXene

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Such as figure 1 As shown, weigh 10g of iodine element and 0.1g of Ti 3 After the AlC is mixed evenly, it is transferred to a tube furnace, 10Mpa, and treated in an Ar atmosphere at 500°C for 6h. After the reaction is complete, 300°C is passed into an Ar cycle gas for 2h to remove AlI. 3 and iodine vapor, and then cooled naturally. Ready-made MXene two-dimensional material nanosheets.

[0047] figure 1 is Ti in Example 1 3 AlC (a) and the prepared MXene two-dimensional material (b) scanning electron microscope (SEM) morphology and size characteristics. Such as figure 1 As shown in (a), MAX presents a thick bulk structure with a thickness of about 1 μm. Selective Redox Etching of Ti by High Temperature Iodine Vapor 3 The interphase Al layer of AlC makes its layered structure get peeled off. Such as figure 1 As shown in (b), the as-prepared MXene presents an ultrathin lamellar structure with a single-layer lamellar thickness of about 10 nm.

[0048] figure 2 i...

Embodiment 2

[0051] Weigh 5g of iodine element and 0.1g of V 2 After the AlC is mixed evenly, it is transferred to a tube furnace, and treated at 200°C for 24h in a 2Mpa He atmosphere. After the reaction is complete, a He cycle gas is introduced at 200°C for 2h to remove AlI. 3 and iodine vapor, and then cooled naturally. Ready-made MXene two-dimensional material nanosheets. Figure 4 It is the scanning electron microscope (SEM) shape size feature of the prepared MXene two-dimensional material in example 2. The as-prepared MXene exhibits an ultrathin lamellar structure.

Embodiment 3

[0053] Weigh 17g of BI 3 and 0.1 g of Ti 2 After the AlN is mixed evenly, transfer it to a tube furnace, 5Mpa, and treat it in a vacuum atmosphere at 800°C for 4h. After the reaction is complete, continue vacuuming at 900°C for 2h to remove AlI 3 and iodine vapor, and then cooled naturally. Ready-made MXene two-dimensional material nanosheets. Figure 5 It is the scanning electron microscope (SEM) shape size feature of the prepared MXene two-dimensional material in example 3. The as-prepared MXene exhibits an ultrathin lamellar structure.

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Abstract

The invention creatively provides a simple and pollution-free method for preparing a fluoride-free two-dimensional material MXene, which comprises the following steps: uniformly mixing an iodine cosolvent and an MAX phase, transferring the mixture into a sealed reaction bin, heating the mixture in an inert environment for reaction to obtain the MXene two-dimensional material. According to the method for preparing the two-dimensional material MXene, the principle is that the two-dimensional material MXene is prepared by etching MAX through iodine cosolvent steam, iodine steam is generated afterthe iodine cosolvent is heated, the iodine steam and A-layer elements are subjected to redox reaction etching at the high temperature, and the MXene is obtained. The method has the advantages of easily available raw materials, low cost, mild reaction conditions, simple operation, no fluorine, no solvation, no waste liquid generation, low toxicity, environmental protection, and realization of large-scale production.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and in particular relates to a simple and pollution-free method for preparing fluorine-free two-dimensional material MXene. Background technique [0002] The two-dimensional material MXene is a new type of carbon / nitride prepared by using the weak bonding force between the A sheet and the MX sheet in the MAX phase, and selecting a suitable etchant to etch the A atomic layer in the MAX phase. The two-dimensional nano-layered material has both good conductivity and hydrophilicity. Compared with the single-atom structure of graphene, the MX structure contains more stable M and X double atoms or polyatoms. In addition, the bond between C and C atoms in graphene is single, while the bond between M-X is a mixed valence bond of covalent bond-ionic bond-metal bond, which also indicates that this type of M-X two-dimensional material MXene will have a higher ratio than graphite. Graphene has richer ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/914C01B32/921C01B21/06C01B21/076B82Y40/00
CPCC01B32/914C01B32/921C01B21/076C01B21/0617C01B21/062C01B21/0627B82Y40/00C01P2004/20C01P2004/03C01P2002/72C01P2002/85
Inventor 曲婕孙闯苏忠
Owner XUZHOU LANOXENE INST CO LTD
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