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KR-102961656-B1 - Method of manufacturing MAX having high purity

KR102961656B1KR 102961656 B1KR102961656 B1KR 102961656B1KR-102961656-B1

Abstract

The present invention relates to a method for manufacturing Max with high purity, comprising: a step of preparing a raw material mixture comprising (i) a first component including a transition metal, (ii) a second component including aluminum, and (iii) a third component including either carbon or nitrogen; and a step of obtaining Max by heating the raw material mixture in an inert gas atmosphere under reduced pressure, wherein the heating comprises: a first heating step of raising the raw material mixture to a first temperature of -10°C to +20°C, the melting point of aluminum; a first holding step of maintaining the raw material mixture at the first temperature for 1 minute to 60 minutes; a second heating step of raising the raw material mixture to a second temperature higher than the first temperature after the first holding step; and a second holding step of maintaining the raw material mixture at the second temperature for 1 hour to 10 hours.

Inventors

  • 오정민
  • 김문성
  • 서창열
  • 박상운
  • 채지광

Assignees

  • 주식회사 이노맥신

Dates

Publication Date
20260508
Application Date
20231012

Claims (8)

  1. In the method of manufacturing Max, (i) a step of preparing a raw material mixture comprising titanium powder, (ii) aluminum powder and (iii) carbon powder; and The method includes the step of heating the above raw material mixture in an inert gas atmosphere under reduced pressure to obtain Max, The above heating is, A first heating step of raising the above raw material mixture to a first temperature of 665℃ to 675℃; A first holding step of maintaining the raw material mixture at the first temperature for 1 to 60 minutes; A second heating step of raising the raw material mixture to a second temperature of 1300℃ to 1500℃ after the first holding step; and It includes a second holding step of maintaining the raw material mixture at the second temperature for 1 to 10 hours, and The above raw material mixture is in a compacted state, and The above first heating step is a manufacturing method in which the heating speed is faster than the above second heating step.
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  4. In paragraph 1, A manufacturing method in which the first maintenance step is performed for 5 to 20 minutes.
  5. In paragraph 1, A manufacturing method in which the above reduced pressure state is 150 tor to 250 tor.
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Description

Method of manufacturing MAX having high purity The present invention relates to a method for manufacturing Max that obtains high-purity Max. MXene, one of the 2-D materials, has excellent properties in many applications. MXene is obtained from MAX, and in the manufacture of MAX, it is important to obtain MAX of high purity. FIG. 1 is a flowchart of a method for manufacturing Max according to an embodiment of the present invention, and FIG. 2 illustrates a heating method in a method for manufacturing Max according to an embodiment of the present invention, and Figure 3 shows the max obtained in Comparative Example 1, and Figure 4 is an XRD graph of Max obtained in Comparative Example 1, and Figure 5 shows the max obtained in Comparative Example 2, and Figure 6 is the XRD graph of Max obtained in Comparative Example 2, and FIG. 7 shows the max obtained in Example 1, and Figure 8 is an XRD graph of Max obtained in Example 1, and Figure 9 shows the max obtained in Comparative Example 3, and Figure 10 is the XRD graph of Max obtained in Comparative Example 3. Generally, MXenes consist of transition metal carbides and nitrides or carbonitrides having the chemical formula M n+1 X n, where M is a transition metal (e.g., Ti, Sc, Zr, Hf, V, Nb, Mo, Ta, Cr, etc.), X is carbon or nitrogen, and n is selected from 1 to 3. With reference to FIGS. 1 and FIGS. 2, a method for manufacturing Max according to the present invention will be described. First, a raw material mixture is prepared comprising (i) a first component including a transition metal, (ii) a second component including aluminum, and (iii) a third component including either carbon or nitrogen (S100). The molar ratio between the first component, the second component, and the third component in the raw material mixture may be 3:1:2. Or, for every 1 mole of the second component, the first component may be 2.5 to 3.5 moles or 2.7 to 3.3 moles and the third component may be 1.5 to 2.5 moles or 1.7 to 2.3 moles. Transition metals such as Ti, Sc, Zr, Hf, V, Nb, Mo, Ta, and Cr can be used, but titanium can be used in particular. Carbon can be used as the third component in particular. Each component may be in powder form, and the raw material mixture is obtained by mixing each component. The mixing method may use a ball mill, although it is not limited to this. Next, the raw material mixture is prepared in the form of a compact (S200). A compacted body can be obtained by applying pressure to a mixture of raw materials using a hydraulic press. The compact may be disc-shaped with a diameter of 30 mm to 70 mm and a thickness of 10 mm to 50 mm. The shape and size of the compact may be varied. Then, a max is obtained from the raw material mixture through heating (S300 to S700). Heating can be performed in an inert gas atmosphere under reduced pressure (vacuum). The pressure in the reduced pressure state may be 120 to 280 tor, 150 to 250 tor, or 180 tor to 220 tor. The inert gas may be argon, but is not limited thereto. When heated, the compacted body may be contained in a container (crucible). The container may be made of the same material as the first component. Additionally, when heated, the container may not be directly exposed to the heat source, but is not limited thereto, the container may be heated while loaded inside a carbon box. In addition, but not limited to this, heating may be performed with one compacted body loaded into each container. The heating step will be explained in detail below with reference to FIG. 2. First, the temperature is raised to the first temperature (S300). The first temperature may be a first temperature of -10°C to the melting point of aluminum +20°C. Specifically, the first temperature may be 660°C to 680°C, 665°C to 675°C, or 668°C to 672°C. The heating rate to the first temperature can be 10℃/min. Next, the first temperature is maintained (S400). The maintenance time of the first temperature may be 1 minute to 60 minutes, 5 minutes to 20 minutes, or 8 minutes to 12 minutes. By maintaining the first temperature, aluminum changes into a liquid state. During the holding time, some of the aluminum volatilizes and evaporates, while the rest dissolves with titanium and carbon to form an alloy, which can suppress the formation of TiC. If a holding time is not provided at the first temperature, the aluminum cannot be dissolved and does not have time to volatilize and evaporate, causing it to melt and flow down in a liquid state, which leads to the formation of TiC. Then, the temperature is raised to the second temperature (S500). The second temperature may be 1300°C to 1500°C or 1350°C to 1450°C. The heating rate to the second temperature is slower than the heating rate to the first temperature and may be 0.3 to 0.7 times the heating rate to the first temperature. Specifically, the heating rate to the second temperature may be 5℃/min. Next, maintain the second temperature (S600). The holding time at the second temperature may be 1 to 10 hours