WO2019221583A1 - Aln lamellaire, procédé pour la fabrication de celui-ci et nanofeuille d'aln exfoliée à partir de celui-ci - Google Patents

Aln lamellaire, procédé pour la fabrication de celui-ci et nanofeuille d'aln exfoliée à partir de celui-ci Download PDF

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WO2019221583A1
WO2019221583A1 PCT/KR2019/006947 KR2019006947W WO2019221583A1 WO 2019221583 A1 WO2019221583 A1 WO 2019221583A1 KR 2019006947 W KR2019006947 W KR 2019006947W WO 2019221583 A1 WO2019221583 A1 WO 2019221583A1
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aln
layered
crystal structure
powder
precursor
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PCT/KR2019/006947
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English (en)
Korean (ko)
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심우영
김혜수
원종범
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연세대학교 산학협력단
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/68—Crystals with laminate structure, e.g. "superlattices"
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/12—Mountings, e.g. non-detachable insulating substrates
    • H01L23/14—Mountings, e.g. non-detachable insulating substrates characterised by the material or its electrical properties
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/12—Mountings, e.g. non-detachable insulating substrates
    • H01L23/14—Mountings, e.g. non-detachable insulating substrates characterised by the material or its electrical properties
    • H01L23/142—Metallic substrates having insulating layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/704—Piezoelectric or electrostrictive devices based on piezoelectric or electrostrictive films or coatings
    • H10N30/706—Piezoelectric or electrostrictive devices based on piezoelectric or electrostrictive films or coatings characterised by the underlying bases, e.g. substrates

Definitions

  • the present invention relates to a layered AlN, a method for producing the same and an AlN nanosheet peeled from the same, more specifically, unlike a conventional bulk AlN has a two-dimensional crystal structure, and excellent peelability in the form of nanosheets
  • the present invention relates to a layered AlN, a method for preparing the same, and an AlN nanosheet peeled therefrom, which is easy to do, and has excellent thermal conductivity and piezoelectric properties.
  • the research on existing 2D materials is based on the top-down method for separating van der Waals bonds with weak interlayer bondability by physical and chemical methods, and the bottom-up method for growing large-area thin films based on vapor deposition. It is becoming.
  • the top-down method since the pristine of the material to be exfoliated must have a two-dimensional layered crystal structure, graphene without band gap, layered metal oxide / nitride with low charge mobility, electron mobility / Research subjects such as transition metal chalcogenides with low electrical conductivity have very limited problems.
  • 2D materials Due to the limitations of previous research methods, 2D materials have been very limitedly studied for materials such as graphene and transition metal chalcogenides. It is limited in that it is not suitable for the development of low-dimensional future materials of a myriad of 3D bulk materials that are not layered.
  • AlN aluminum nitride
  • the AlN is manufactured from a two-dimensional material, the above-described characteristics may be improved, and thus, the AlN may be applied to a semiconductor substrate or a component of high thermal conductivity ceramics.
  • the present invention has a two-dimensional crystal structure, has excellent peelability and is easy to peel in the form of a nanosheet, and has a layered AlN and an AlN nanosheet peeled therefrom having excellent thermal conductivity and piezoelectric properties.
  • the purpose is to provide.
  • the present invention is (1) heat treatment and cooling the mixture containing Ca precursor or Ca powder, Al precursor or Al powder, and N precursor, the space group (C2 / 2 or P2) obtaining a layered compound represented by the formula Ca 3 Al 2 N 4 having a monoclinic crystal structure of / c and (2) Ca included in the layered compound without changing the crystal structure of the layered compound
  • It provides a method for producing a layered AlN comprising the step of treating the layered compound with a mixed solution comprising a salt capable of selectively removing ions and a solvent capable of dissolving the salt.
  • the salt may be represented by the following formula (1).
  • M is any one selected from Al, Mg, and Mn
  • X is any one selected from Cl, F, and I.
  • the solvent may be at least one selected from deionized water, tetrahydrofuran and dichloromethane.
  • the heat treatment of step (1) may be performed for 80 to 200 hours at 1000 ⁇ 1200 °C.
  • the cooling of the step (1) may be performed at a temperature reduction rate of 0.5 ⁇ 3 °C / hour or 10 ⁇ 15 °C / hour.
  • the present invention also provides a layered AlN having a monoclinic crystal structure in which the space group is C2 / 2 or P2 / c.
  • the layered AlN having a monoclinic crystal structure having a space group of C2 / 2 is 1354 in an X-ray diffractogram obtained by a powder X-ray diffraction method using Cu-K ⁇ rays. Peaks at 2 ⁇ values of ⁇ 02, 1668 ⁇ 02, 2079 ⁇ 02, 2125 ⁇ 02, 2685 ⁇ 02, 2743 ⁇ 02, 3146 ⁇ 02, and 3233 ⁇ 02, 3304 ⁇ 02, 3577 ⁇ 02, 377 ⁇ 02, It may not have peaks at 2 ⁇ values of 4948 ⁇ 02, 5902 ⁇ 02, 6554 ⁇ 02 and 7095 ⁇ 02.
  • the layered AlN having a monoclinic crystal structure in which the space group is P2 / c has an X-ray diffraction diagram obtained by a powder X-ray diffraction method using Cu-K ⁇ rays. It has peaks at 2 ⁇ values of 994 ⁇ 02, 1824 ⁇ 02, 1873 ⁇ 02, 1895 ⁇ 02, 1996 ⁇ 02, 2424 ⁇ 02, 2521 ⁇ 02 and 3011 ⁇ 02, and 3304 ⁇ 02, 3577 ⁇ 02, 377 ⁇ 02 , 4948 ⁇ 02, 5902 ⁇ 02, 6554 ⁇ 02 and 7095 ⁇ 02 may not have peaks at 2 ⁇ values.
  • the present invention also provides an AlN nanosheet peeled from the layered AlN according to the present invention and having an amorphous crystal structure.
  • the thickness of the AlN nanosheets may be 300 nm or less.
  • the layered AlN according to the present invention has a two-dimensional crystal structure, has excellent peelability and is easily peeled off in the form of a nanosheet, and has a high thermal conductivity and piezoelectric semiconductor substrate. It can be widely used for the substrate of a thyristor and a piezoelectric element.
  • FIG. 1 is a schematic diagram of a layered AlN manufacturing method according to an embodiment of the present invention.
  • FIG. 2 is a graph showing XRD analysis results of 3D bulk AlN of Comparative Example 1, layered Ca 3 Al 2 N 4 of Preparation Example 1, and layered AlN of Example 1.
  • FIG. 2 is a graph showing XRD analysis results of 3D bulk AlN of Comparative Example 1, layered Ca 3 Al 2 N 4 of Preparation Example 1, and layered AlN of Example 1.
  • FIG. 3A is an SEM image of the layered Ca 3 Al 2 N 4 of Preparation Example 1.
  • FIG. 3B is an SEM image of the layered Ca 3 Al 2 N 4 of Preparation Example 1.
  • 3C is an SEM image of the layered AlN of Example 1.
  • FIG. 4 is a photograph of layered Ca 3 Al 2 N 4 of Preparation Example 1.
  • the method of manufacturing a layered AlN according to the present invention can produce a bulk AlN of a conventional 3D structure in a two-dimensional structure, and unlike the existing bulk AlN can be easily peeled, and can produce a layered AlN having excellent thermal conductivity properties. .
  • step (1) the mixture comprising Ca precursor or Ca powder, Al precursor or Al powder, and N precursor is heat-treated and then cooled to give a monoclinic system having a space group of C2 / 2 or P2 / c. monoclinic) to obtain a layered compound having a crystal structure represented by the formula Ca 3 Al 2 N 4 .
  • the Ca precursor or Ca powder, Al precursor or Al powder, and N precursor may be mixed independently of each other, the N precursor may be included in the mixture with the same material as the Ca precursor or Al precursor.
  • the N precursor may be a compound including N ions
  • the Ca precursor may be a compound including Ca ions
  • the N precursor and the Ca precursor may be the same material as the compound including Ca and N elements.
  • it may be Ca 3 N 2 but is not limited thereto.
  • the Al precursor may be a compound including Al ions, for example, may be AlN, but is not limited thereto.
  • the mixture may be heat treated after being encapsulated in a reaction vessel, and the inside of the reaction vessel may be maintained in an inert gas atmosphere or a vacuum atmosphere.
  • the material of the reaction vessel may be, for example, alumina, molybdenum, tungsten or quartz, but any material that does not react with the sample and does not break at a high temperature may be used without limitation in the material.
  • the Ca 3 Al 2 N 4 is (2) has an AlN different 2D crystal structure of the 3D crystal structure, which will be described later stage be prepared through the step (1) As shown in Figure 1 of the Ca 3 Al 2 N 4 By selectively removing Ca ions, a layered AlN may be prepared without changing the crystal structure of Ca 3 Al 2 N 4 .
  • the heat treatment may be performed at 1000 to 1200 ° C. for 80 to 200 hours.
  • the heat treatment is performed at less than 1000 ° C., the sintering reaction of the mixture may not be completed, and thus unreacted raw materials may remain, resulting in a decrease in yield of the layered compound prepared. have.
  • the heat treatment is performed in excess of 1200 °C, there may be a problem such as the reaction vessel used in the sintering reaction by the vaporization of Ca ions, or the yield of the layered compound produced is lowered.
  • the heat treatment is performed for less than 80 hours, the sintering reaction of the mixture may not be completed, so that unreacted raw materials may remain, and thus the yield of the layered compound prepared may be deteriorated. have.
  • the heat treatment is performed for more than 200 hours, there is a fear that the manufacturing process time unnecessarily increases.
  • the cooling process after the heat treatment in step (1) is necessary for crystallization of the layered compound, and the single crystal size of the crystal may change according to the cooling rate.
  • the cooling may be performed at a temperature reduction rate of 10 to 15 ° C./hour or 0.5 to 3 ° C./hour, and when the temperature reduction rate is 10 to 15 ° C./hour, the layered Ca 3 Al 2 N 4 may be polycrystalline. have.
  • the heat-sensing and speed can be purified unity to 0.5 ⁇ 3 °C / hour day when the layered Ca 3 Al 2 N 4, a single crystal size of the layered AlN after Ca ion scavenging included in the layered Ca 3 Al 2 N 4 is Can be maintained.
  • grain boundaries of the particles may decrease, and the aspect ratio of the InAs nanosheets peeled off when the layered InAs is peeled off may increase.
  • the temperature reduction rate is less than 0.5 °C / hour, a change in the composition of the material produced due to the vaporization of Ca ions may occur, and if the temperature reduction rate exceeds 3 °C / hour, the layered compound prepared is polycrystalline Can be.
  • the layered compound prepared in step (1) includes a salt including a salt capable of selectively removing Ca ions contained in the layered compound and a solvent capable of dissolving the salt. Treated with solution to prepare a layered AlN without changing the crystal structure of the layered compound.
  • the salt may include an anion having a high electronegativity and a cation having an electronegativity value between the alkali metal ion and the Al ion in order to easily react with the alkali metal ion contained in the layered compound.
  • the salt may be represented by the following Chemical Formula 1, wherein the salt is a cation having an electronegativity value between the alkali metal ion and the Al ion, and is composed of M and Cl ions having a high electronegativity.
  • M may be any one selected from Al, Mg, and Mn, and X may be any one selected from Cl, F, and I.
  • the solvent may include at least one selected from deionized water, tetrahydrofuran and dichloromethane.
  • the salt may be included in the mixed solution at a high concentration that can be dissolved in the solvent in order to increase the Ca ion removal efficiency of the layered Ca 3 Al 2 N 4 and prevent the removal of Al ions.
  • the salt may be used in an amount sufficient to remove Ca ions of the layered Ca 3 Al 2 N 4 , but preferably the layered Ca 3 Al 2 N 4 and the salt in the mixed solution are 1: 1 to 1: It may be included in a molar ratio of three. If the molar ratio of the layered Ca 3 Al 2 N 4 and salt is less than 1: 1, Ca ions of the layered Ca 3 Al 2 N 4 may not be removed to the desired level, if the molar ratio is 1 If it exceeds 3, the salt may not be dissolved in the mixed solution, resulting in a precipitate.
  • the step (2) may be carried out at a temperature at which the Ca ion removal reaction may occur smoothly, the temperature may vary depending on the composition of the mixed solution, preferably at least 20 °C, more preferably Preferably it may be carried out at a temperature of 20 ⁇ 60 °C. If carried out below 20 ° C., Ca ions may not be removed to the desired level, and if carried out at temperatures above 60 ° C., the layered structure of the layered Ca 3 Al 2 N 4 produced may collapse. have.
  • the alkali metal ion removal rate may be excellent while maintaining the layered structure of the layered Ca 3 Al 2 N 4 prepared when performed at a temperature of 20 ⁇ 60 °C.
  • the step (2) may be performed a plurality of times depending on the composition of the mixed solution, the removal rate of Ca ions, but is preferably performed once to maintain the layered structure of the layered AlN.
  • a reactant produced by reacting Ca ions with the salt in addition to the layered AlN may be present, for example, calcium chloride, and the powder obtained through step (2) may be removed to remove it. It can be washed with a solvent.
  • the solvent for removing the reactant may be used without limitation as long as it is a solvent having solubility in calcium chloride and may be at least one selected from water, deionized water and ethanol.
  • Layered AlN according to the present invention has a monoclinic (monoclinic) crystal structure of the space group (space group) of C2 / 2 or P2 / c, which is different from the existing 3D bulk AlN as a nanocrystalline sheet with excellent peelability It is easy to peel off in the form of, and may have excellent thermal conductivity characteristics.
  • the layered AlN having a monoclinic crystal structure in which the space group is C2 / 2 is 1354 ⁇ 02, 1668 ⁇ 02, 2079 ⁇ . 02, 2125 ⁇ 02, 2685 ⁇ 02, 2743 ⁇ 02, 3146 ⁇ 02 and 3233 ⁇ 02 with peaks at 2 ⁇ values, 3304 ⁇ 02, 3577 ⁇ 02, 377 ⁇ 02, 4948 ⁇ 02, 5902 ⁇ 02, 6554 It may not have peaks at 2 ⁇ values of ⁇ 02 and 7095 ⁇ 02.
  • the layered AlN having a monoclinic crystal structure in which the space group is P2 / c is 994 ⁇ 02, 1824 ⁇ 02, 1873 ⁇ 02, 1895 ⁇ 02, 1996 ⁇ 02, 2424 ⁇ 02, 2521 ⁇ 02, and 3011 ⁇ . It may have a peak at a 2 ⁇ value of 02 and may not have a peak at a 2 ⁇ value of 3304 ⁇ 02, 3577 ⁇ 02, 377 ⁇ 02, 4948 ⁇ 02, 5902 ⁇ 02, 6554 ⁇ 02 and 7095 ⁇ 02.
  • the AlN nanosheets according to the present invention can be obtained by peeling from the layered AlN according to the present invention and have an amorphous crystal structure.
  • the AlN nanosheets may have a thickness of 300 nm or less, and if the thickness exceeds 300 nm, the surface area of the AlN nanosheets may be lowered to lower thermal conductivity and piezoelectric properties, or the AlN nanosheets. Lamination of sheets can be difficult.
  • a peeling method of the layered AlN a peeling method of a layered material known in the art may be used, and for example, a peeling method using energy by ultrasonic waves, a peeling method by invasion of a solvent, a peeling method using a tape, and adhesion Any of the stripping methods using a substance having a surface may be used.
  • the layered AlN and AlN nanosheets according to the present invention have excellent thermal conductivity and piezoelectric properties, they may be used for semiconductor substrates of high thermal conductivity ceramics, substrates of thyristors, or piezoelectric elements.
  • the layered AlN and AlN nanosheets according to the present invention may be included as piezoelectric elements included in the piezoelectric elements, thereby providing excellent piezoelectric properties.
  • the configuration other than the piezoelectric element included in the piezoelectric element may adopt a configuration known in the art, and thus the detailed description thereof will be omitted.
  • the layered AlN and AlN nanosheets according to the present invention have excellent thermal conductivity, when used in a semiconductor substrate or a substrate of a high thermal conductivity ceramic, the thermal conductivity may be excellent.
  • Configurations other than the substrate may employ a configuration known in the art, so the detailed description thereof will be omitted.
  • the layered Ca 3 Al 2 N 4 prepared in Preparation Example 1 was mixed with deionized water, tetrahydrofuran and AlCl 3 to remove Ca ions from the Ca 3 Al 2 N 4 , through which a layered AlN was prepared.
  • Example 2 The layered AlN prepared in Example 1 was peeled off with a tape to prepare an AlN nanosheet.
  • the layered Ca 3 Al 2 N 4 (preparation example 1) has a monoclinic crystal structure of space groups C2 / 2 and P2 / c.
  • the layered AlN (Example 1) having Ca ions removed from the layered Ca 3 Al 2 N 4 has a monoclinic crystal structure of C2 / 2 and P2 / c, which is a bulk of 3D structure. It is a crystal structure different from AlN.
  • AlN prepared after removing Ca ions of the layered Ca 3 Al 2 N 4 has a layered structure.

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Abstract

La présente invention concerne de l'AlN lamellaire, un procédé pour la fabrication de celui-ci et une nanofeuille d'AlN exfoliée à partir de celui-ci et, plus précisément : de l'AlN lamellaire qui a une structure cristalline bidimensionnelle, contrairement à de l'AlN massif classique, une facilité d'exfoliation permettant une exfoliation facile sous la forme d'une nanofeuille et une excellente conductivité thermique; un procédé pour la fabrication de celui-ci; et une nanofeuille d'AlN exfoliée à partir de celui-ci.
PCT/KR2019/006947 2018-05-18 2019-06-10 Aln lamellaire, procédé pour la fabrication de celui-ci et nanofeuille d'aln exfoliée à partir de celui-ci WO2019221583A1 (fr)

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KR1020180057454A KR102271060B1 (ko) 2018-05-18 2018-05-18 층상형 AlN, 이의 제조 방법 및 이로부터 박리된 AlN 나노시트
KR10-2018-0057454 2018-05-18

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KR102425892B1 (ko) 2020-09-09 2022-07-26 연세대학교 산학협력단 인듐과 인을 포함하는 층상구조 화합물, 나노시트 및 이를 이용한 전기 소자
US11597651B2 (en) 2020-09-09 2023-03-07 Industry-Academic Cooperation Foundation, Yonsei University Layered group III-V compound and nanosheet containing phosphorus, and electrical device using the same
KR102425893B1 (ko) * 2020-09-14 2022-07-26 연세대학교 산학협력단 칼륨, 인듐과 비소를 포함하는 층상구조 화합물, 나노시트 및 이를 이용한 전기 소자
US11634340B2 (en) 2020-09-09 2023-04-25 Industry-Academic Cooperation Foundation, Yonsei University Layered group III-V compound and nanosheet containing arsenic, and electrical device using the same
KR102425890B1 (ko) * 2020-09-14 2022-07-26 연세대학교 산학협력단 알루미늄과 안티몬을 포함하는 층상구조 화합물, 나노시트 및 이를 이용한 전기 소자
KR102425889B1 (ko) * 2020-09-14 2022-07-26 연세대학교 산학협력단 인듐과 비소를 포함하는 층상구조 화합물, 나노시트 및 이를 이용한 전기 소자
KR102425894B1 (ko) * 2020-09-14 2022-07-26 연세대학교 산학협력단 인듐과 안티몬을 포함하는 층상구조 화합물, 나노시트 및 이를 이용한 전기 소자
US11643753B2 (en) 2020-09-14 2023-05-09 Industry-Academic Cooperation Foundation, Yonsei University Layered group III-V compound and nanosheet containing antimony, and electrical device using the same
KR102425891B1 (ko) * 2020-09-14 2022-07-26 연세대학교 산학협력단 갈륨과 안티몬을 포함하는 층상구조 화합물, 나노시트 및 이를 이용한 전기 소자
KR102514681B1 (ko) 2020-11-10 2023-03-27 연세대학교 산학협력단 층상구조를 가지고 강유전 유사 특성을 가지는 3-5족 화합물

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