Preparing method for two-dimensional crystal MXene nanometer material

A technology of two-dimensional crystals and nanomaterials, which is applied in the field of preparing two-dimensional crystal MXene by etching MAX phase ceramics with HF acid salt, which can solve the problems of high risk of concentrated HF, high requirements for storage conditions, and great human hazards. The method is simple and easy to implement, easy to store, and easy to promote large-scale industrialization.

Inactive Publication Date: 2016-12-14
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, two-dimensional crystal MXene materials are mainly obtained by etching ternary layered compound MAX phase ceramics with concentrated HF acid, but concentrated HF is highly dangerous and harmful to humans, and requires high storage conditions.

Method used

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  • Preparing method for two-dimensional crystal MXene nanometer material
  • Preparing method for two-dimensional crystal MXene nanometer material
  • Preparing method for two-dimensional crystal MXene nanometer material

Examples

Experimental program
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Effect test

Embodiment 1

[0034] TiH 2 , TiC, and Al powders were weighed at a molar ratio of 1:2:1.1, and ball milled for 12 hours to make them evenly mixed. Using a vacuum tube furnace, using high-purity argon as a protective gas, sintering at 1400 ° C for 2 hours to prepare high-purity Ti 3 AlC 2 The bulk material is finally ground into a 325 mesh powder, and its XRD pattern is shown in figure 1 , microstructure see figure 2 . From figure 1 and figure 2 It can be seen that this embodiment has prepared high-purity Ti with layered structure 3 AlC 2 material (or Ti 3 AlC 2 ceramics).

[0035] Weigh 2g Ti 3 AlC 2 Powder, 7.5g NaHF 2 Add 100ml of deionized water, stir magnetically, and react at 60°C for 24 hours. The reaction product is fully washed with deionized water and absolute ethanol until the supernatant is nearly neutral, and dried in vacuum at 80°C to obtain a two-dimensional crystal titanium carbide nanomaterial Ti 3 C 2 T x , whose microstructure see image 3 . From imag...

Embodiment 2

[0037] TiH 2 , TiC, and Al powders were weighed at a molar ratio of 1:2:1.1, and ball milled for 12 hours to make them evenly mixed. Using a vacuum tube furnace, using high-purity argon as a protective gas, sintering at 1400 ° C for 2 hours to prepare high-purity Ti 3 AlC 2 The bulk material is finally ground into a 325 mesh powder. Weigh 2g Ti 3 AlC 2 Powder, 10g KHF 2 Add 200ml of deionized water, stir magnetically, and react at 60°C for 24 hours. The reaction product is fully washed with deionized water and absolute ethanol until the supernatant is nearly neutral, and dried in vacuum at 80°C to obtain a two-dimensional crystal titanium carbide nanomaterial Ti 3 C 2 T x , whose microstructure see Figure 4 . From Figure 4 It can be seen that the two-dimensional crystal titanium carbide nanomaterial Ti prepared in this embodiment 3 C 2 T x It has a distinct graphene-like two-dimensional layered structure.

Embodiment 3

[0039] TiH 2 , TiC, and Al powders were weighed at a molar ratio of 1:2:1.1, and ball milled for 12 hours to make them evenly mixed. Using a vacuum tube furnace, using high-purity argon as a protective gas, sintering at 1400 ° C for 2 hours to prepare high-purity Ti 3 AlC 2 The bulk material is finally ground into a 325 mesh powder. Weigh 2g Ti 3 AlC 2 Powder, 10g NH 4 HF 2 Add 200ml of deionized water, stir magnetically, react at 60°C for 18h, wash the reaction product thoroughly with deionized water and absolute ethanol until the supernatant is nearly neutral, and dry it in vacuum at 80°C to obtain a two-dimensional crystal titanium carbide nanomaterial Ti 3 C 2 T x , whose microstructure see Figure 5 . From Figure 5 It can be seen that the two-dimensional crystal titanium carbide nanomaterial Ti prepared in this embodiment 3 C 2 T x It has a distinct graphene-like two-dimensional layered structure.

[0040] The present invention utilizes NaHF 2 、KHF 2 Etc...

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Abstract

The invention relates to a preparing method for a two-dimensional crystal MXene nanometer material. The preparing method comprises the steps that a high-purity ternary lamellar MAX-phase ceramic block material is ground and then screened, and MAX-phase ceramic powder is obtained; the MAX-phase ceramic powder and HF acid salt crystals are weighed in the mass ratio of 2:(5-15) and then added into deionized water, an etching reaction is carried out at 30-85 DEG C, washing and drying are carried out, and the two-dimensional crystal MXene nanometer material is obtained. The MXene nanometer material prepared through the method has an obvious graphene-like two-dimensional lamellar structure and is expected to be applied to the fields such as supercapacitors, lithium ion batteries and adsorption; the MAX phase is subjected to etching treatment with acid salt, the method is simple and easy to implement, safe and reliable, and large-scale industrialized popularization is easy.

Description

technical field [0001] The invention belongs to the field of preparation of two-dimensional crystal MXene nanomaterials, in particular to a method for preparing two-dimensional crystal MXene by etching MAX phase ceramics with HF acid salt. Background technique [0002] MXene material is a new type of two-dimensional transition metal carbide or carbonitride with a graphene-like structure and its chemical formula is M n+1 x n T x , wherein M represents a transition metal, X represents carbon or nitrogen, Tx is -OH / =O, -F, n=1, 2, 3. MXene has good conductivity, hydrophilicity, light transmission, and magnetism, and can be used in supercapacitors, lithium-ion batteries, hydrogen storage, sensors and other fields. [0003] At present, two-dimensional crystal MXene materials are mainly obtained by etching ternary layered compound MAX phase ceramics with concentrated HF acid, but concentrated HF is highly dangerous, harmful to humans, and requires high storage conditions. Con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/56C04B35/626
CPCC04B35/5618C04B35/626C04B2235/78
Inventor 于云冯爱虎王勇江峰于洋米乐宋力昕
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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