WO2020053102A1 - Procédé de préparation de films minces monocristallins - Google Patents

Procédé de préparation de films minces monocristallins Download PDF

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Publication number
WO2020053102A1
WO2020053102A1 PCT/EP2019/073877 EP2019073877W WO2020053102A1 WO 2020053102 A1 WO2020053102 A1 WO 2020053102A1 EP 2019073877 W EP2019073877 W EP 2019073877W WO 2020053102 A1 WO2020053102 A1 WO 2020053102A1
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Prior art keywords
plane
process according
sapphire
miscut
crystal thin
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PCT/EP2019/073877
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English (en)
Inventor
Dominique CHATAIN
Igor OZEROV
Blandine COURTOIS
Alain RANGUIS
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Centre National De La Recherche Scientifique
Universite D'aix-Marseille
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Publication of WO2020053102A1 publication Critical patent/WO2020053102A1/fr

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Classifications

    • 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
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C30B23/025—Epitaxial-layer growth characterised by the substrate
    • 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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate
    • 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
    • C30B29/02—Elements
    • 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
    • C30B29/52—Alloys

Definitions

  • the invention relates to a process for preparing single-crystal thin films of pure metals or alloys, by deposition and growth of grains on a (0001) sapphire having a miscut comprised between 0.2° and 5°, and oriented towards a specific plane. It also relates to a single-crystal thin film obtainable by such a process and uses thereof
  • Sapphire which is a crystalline alumina of the mineral corundum with a trigonal (or rhombohedral) structure, is widely used as substrate for the growth of semiconductor or metallic thin films. Due to its mechanical and chemical robustness and its high melting point (ca. 2050°C), sapphire allows treatments under harsh conditions, in particular high-temperature treatments.
  • this step might be beneficial for the formation of a Cu 2 0 ultrathin layer on sapphire substrate after copper deposition.
  • This initial sapphire annealing step is crucial in the process.
  • a similar process is also described in CN 107354506 and CN 107190315.
  • EP 2 540 862 relates to a carbon film laminate which includes a (0001) sapphire as a substrate, a (111) copper thin film formed by epitaxial growth on the substrate, and graphene deposited on the copper film.
  • the (0001) sapphire has a surface composed of terrace surfaces which are flat at the atomic level and atomic-layer steps.
  • the sapphire substrate has a tolerance of 0.3° or less with respect to the plane direction. As evidenced by Figure 1 , the miscut of said substrate is random and steps are not straight. Contrary to what is stated in the document, the film formed in the process is not strictly a single-crystal.
  • the film can rather be described as a polycrystalline material, composed of grains having a (111) plane parallel to the substrate but different in-plane orientations (rotations about the ⁇ 111> out-of-plane axis).
  • a particular sapphire substrate i.e. a (0001) sapphire substrate having a miscut comprised between 0.2° and 5°, said miscut being oriented towards a specific plane, allows access to high quality single-crystal thin films, without necessarily“pre-annealing” the substrate.
  • Such a configuration of the substrate implies terraces with step edges running in majority along a specific direction on the surface of the sapphire substrate.
  • subjecting the film-substrate system to a heating stage enables the coalescence of the grains into a single grain, in one preferred orientation, without twinning and/or grain boundaries.
  • Single-crystal films between 100 nm and 1 pm thickness can be obtained by such a process, and can find applications in electronics and plasmonics.
  • the use of a traditional (0001) sapphire with a random miscut in such a process would lead to a polycrystalline film composed of several grains with different orientations relative to the substrate.
  • the invention relates to a process for preparing a single-crystal thin film comprising the following successive steps:
  • a single-crystal thin film as defined above, as a substrate for manufacturing a film of a two-dimensional material or as a material for electronic or plasmonic devices.
  • Figure 1 shows AFM (Atomic Force Microscopy) scan of an as-deposited copper film showing grains of size ranging from 30 to 50 nm.
  • Figure 2 shows AFM scan of the copper single crystal film after annealing of the deposit.
  • Figure 3 shows EBSD (Electron Backscatter Diffraction) data on a typical area of 250x200 microns of 300 nm thick copper film annealed for 6 h at 980 °C under Ar+40%H 2 flow at 10 cc/min.
  • EBSD Electro Backscatter Diffraction
  • Sapphire is a single-crystal alumina (a-A1 2 0 3 ) organized in a trigonal crystal structure (3m).
  • Sapphire planes can be defined by their Miller indices: h, k, i and 1, wherein h, k, i and 1, identical or different, are each a positive integer, a negative integer, or zero.
  • a plane of sapphire may also be referred by a letter:
  • x is the negative of x and may also be written -x, with x being any integer.
  • the substrate is a sapphire. Said substrate may have any shape. In the process of the invention, the substrate is preferably a wafer of sapphire.
  • Said substrate may be typically composed of a plurality of surfaces or facets.
  • Each surface or facet of a sapphire may be in a (h k i 1) plane.
  • each surface or facet of a sapphire may be in a plane independently selected from (0001), (P02), (1120), (llOO), (1123) and (1101 ) .
  • (h k i 1) refers to a plane having h, k, i, and 1 as Miller indices or to any plane of the corresponding family.
  • A“(h k i 1) surface” refers to a surface which is in a (h k i 1) plane.
  • A“(h k i 1) sapphire” refers to a sapphire substrate the“deposition surface” of which is in a (h k i 1) plane.
  • A“(0001) sapphire” refers to a sapphire substrate the“deposition surface” of which is in a (0001) plane, i.e. a (c)-plane.
  • The“deposition surface” refers to the surface onto which a layer or a film is deposited in the process of the invention.
  • A“(h k i 1) sapphire having a miscut of q°” refers to a sapphire substrate the deposition surface of which is not in a (h k i 1) plane but is the surface revealed by a miscut of 0° with respect to the (h k i 1) plane, 0° being an angle comprised between 0° and 180°.
  • cut refers either to the action consisting in revealing a surface which is at a given angle with respect to a given plane, and/or to the result of said action.
  • the miscut of a sapphire may be carried out by polishing a surface of said sapphire.
  • a“(h k i 1) sapphire having a miscut of 0°” may be obtained by polishing a surface which is in a (h k i 1) plane, with an angle of 0° off the said plane.
  • the surface of a sapphire revealed by a miscut typically comprises terraces with steps.
  • the orientation of a miscut refers to the orientation of the terraces and straight steps of the surface revealed by the miscut.
  • the miscut may be oriented towards one plane, such as (a)-plane, (m)- plane, (r)-plane, (p)-plane or (s)-plane, preferably (a)-plane or (p)-plane.
  • Said plane is the plane towards which the ledges connecting the terraces of the surface revealed by the miscut are oriented.
  • the angle and the orientation of a miscut are typically two independent parameters, and may thus be independently controlled when the miscut of the sapphire is carried out. For one given angle, several orientations may be selected. For one given orientation, several angles may be selected.
  • the sapphire substrate has a (0001) sapphire plane.
  • Said sapphire may have a miscut comprised between 0.2° and 5°, preferably between 0.25° and 3°, more preferably between 0.25° and 2°.
  • Said sapphire substrate may be obtained by polishing a (0001) surface of sapphire, tilted by an angle as defined above, with respect to the (0001) plane.
  • Said miscut may be oriented towards one plane.
  • said miscut is oriented towards a plane selected from (a)-plane or (p)-plane.
  • said miscut is oriented towards (a)-plane.
  • a sapphire in particular a (0001) sapphire
  • said substrate Before step (a), which consists in depositing a layer of inorganic material on a sapphire substrate, said substrate may be subjected to one or more treatments, said treatments being each independent.
  • Such treatments may be chemical and/or thermal treatments and may be implemented with the aim of obtaining a clean substrate, and in particular clean surface(s).
  • such treatments may be implemented for removing the sapphire dust produced by miscutting the sapphire substrate, and/or for removing potential organic contaminants. More broadly, such treatments may be implemented for improving the quality of deposition of the layer of inorganic material in step (a).
  • said substrate may be subjected to a cleaning under ultrasonic conditions, in one or more organic solvents for an appropriate period of time.
  • organic solvents include, but are not limited to, acetone, dichloromethane, chloroform, ethyl acetate, alcohols such as ethanol or isopropanol, dimethylsulfoxide, ethers such as diethyl ether or tetrahydrofuran, acetonitrile, dimethylformamide, and a mixture thereof.
  • said substrate may be ultrasonically cleaned in acetone for 5 minutes and then in isopropanol for 5 minutes.
  • Said substrate may be exposed to an oxygen plasma at a temperature of 100 °C to 350 °C, preferably 180 °C to 250 °C, in a reactor, such as a barrel reactor.
  • said substrate may be annealed at a temperature comprised between 1000 °C and 1200 °C under an oxygen atmosphere, before depositing the layer of inorganic material.
  • Said annealing step may be carried out for 2 to 15 hours.
  • Said annealing step is optional and may be carried out with the aim of further improving the surface of said substrate, and accordingly, further improving the features of the single-crystal thin film obtained according to the process of the invention.
  • Step (a) of the process according the invention consists in depositing a layer of inorganic material on a sapphire.
  • Said layer of inorganic material is advantageously deposited on a (0001) sapphire substrate having a miscut comprised between 0.2° and 5°, preferably between 0.25° and 3°, more preferably between 0.25° and 2°, and oriented towards (a)-plane or (p)-plane, preferably (a)-plane.
  • said layer of inorganic material may be deposited on a surface revealed by a miscut comprised between 0.20° and 5°, preferably between 0.25° and 3°, more preferably between 0.25° and 2°, and oriented towards (a)-plane or (p)-plane, said miscut being carried out on a (0001) surface of a (0001) sapphire substrate.
  • Said layer of inorganic material may be deposited on all or part of a surface of a sapphire.
  • Said layer of inorganic material may be deposited by any deposition techniques known to the skilled artisan.
  • said layer is deposited by physical vapor deposition (PVD).
  • PVD physical vapor deposition
  • Examples of physical vapor deposition include, but are not limited to, evaporation under vacuum, sputtering deposition and molecular beam epitaxy.
  • said layer is deposited by evaporation under vacuum.
  • the speed of deposition of said layer may typically be comprised between 0.05 nm/sec and 2 nm/sec, preferably between 0.2 nm/sec and 0.5 nm/sec.
  • the deposition may typically be carried out under a vacuum comprised between 1.10 5 Pa and 5.10 4 Pa, preferably between 8.10 5 Pa and 2.10 4 Pa. This step may be carried out in order to avoid oxidation of the films and their contamination by gas residues.
  • Said layer of inorganic material may be deposited at a temperature comprised between 0 °C and 160 °C, preferably between 15 °C and 35 °C.
  • the thickness of the layer of inorganic material may be monitored with a quartz microbalance during deposition.
  • a laminate may be obtained, said laminate being composed of a (0001) sapphire substrate onto which a layer of inorganic material is deposited.
  • the thickness of the layer of inorganic material may be comprised between 100 nm and 1 pm, preferably between 250 nm and 800 nm, as measured by a contact profilometer or by any other techniques known to the skilled artisan.
  • Said layer of inorganic material obtained in step (a) is typically polycrystalline.
  • the grains constituting said polycrystalline layer may have a size comprised between 20 and 60 nm, and may have any orientation.
  • the purity of said layer of inorganic material deposited in step (a) is advantageously higher than or equal to 99 %, preferably higher than or equal to 99.9 %, more preferably higher than or equal to 99.99 %.
  • said inorganic material deposited in step (a) may be a pure metal or an alloy.
  • said inorganic material deposited in step (a) is a pure metal or an alloy whose crystalline structure is face-centered cubic (FCC) under standard temperature and pressure (also called“STP conditions”).
  • Standard temperature is 0 °C and standard pressure is 100 000 Pa.
  • Pure metal refers to a material composed of only one metal element.
  • Alloy refers to a material composed of at least two elements of the periodic table, at least one of which is a metal element.
  • Metal element refers to transition metal element, post-transition metal element, or metalloid element.
  • transition metal elements include, but are not limited to, nickel, copper, silver, gold, palladium, rhodium, iridium, platinum and lanthanides such as ytterbium or cerium.
  • post-transition metal elements include, but are not limited to, aluminum and lead.
  • metalloid elements include, but are not limited to, silicon and germanium.
  • FCC Fe-centered cubic
  • a material whose unit cell is a cube and whose atoms are located at each of the comers and each of the centers of all the cubic faces of the unit cell.
  • each atom of the crystalline structure is the element composing the pure metal.
  • each atom of the crystalline structure is independently one of the at least two elements composing the alloy.
  • Examples of pure metals whose crystalline structure is FCC under STP conditions include, but are not limited to copper, nickel, silver, gold, aluminum, platinum, palladium, rhodium, iridium, ytterbium, cerium and lead, preferably copper.
  • alloys whose crystalline structure is FCC under STP conditions include, but are not limited to, CuNi, CuNiAu and FeCoNi.
  • Step (b) of the process according to the invention consists in heating the laminate obtained in step (a) to a temperature comprised between 75 % and 95 %, preferably between 80 % and 95 % of the melting point of said inorganic material.
  • the temperature in step (b) may be comprised between 810 °C and 1030 °C, preferably between 868 °C and 1030 °C, when said inorganic material is copper (melting point of copper is 1085 °C).
  • heating in step (b) is carried out for 30 minutes to 30 hours, preferably for 1 hour to 20 hours, more preferably for 2 hours to 10 hours.
  • the time of heating in step (b) may be dependent on the characteristics of the miscut, in particular the plane towards which the miscut is oriented, the nature of the inorganic material and the purity and the thickness of the layer of the inorganic material deposited in step (a).
  • the time of heating in step (b) can thus been adjusted by the skilled artisan according to these factors.
  • Step (b) may be carried out under an atmosphere composed of inert gas such as argon, and dihydrogen.
  • inert gas such as argon, and dihydrogen.
  • the thickness of said single-crystal thin film may be comprised between 100 nm and 1 pm, preferably between 250 nm and 800 nm, as measured by a contact profilometer or by any other techniques known to the skilled artisan.
  • said single-crystal thin film has a highly flat surface and has no defects, in particular grain boundaries and twin boundaries.
  • RMS (Root Mean Square) roughness of said single-crystal thin film is typically in the range of 1 to 2.5 nm.
  • said single-crystal thin film is a single crystal of a pure metal or an alloy whose crystalline structure is FCC under NTP conditions, and having a (111) orientation, i.e. the surface of said single-crystal thin film is in a (111) plane of the FCC structure.
  • (111) plane refers to a (h k 1) plane of a FCC structure, wherein h, k, and 1 are Miller indices.
  • the process of the invention is advantageously carried out in a clean room, in order to prevent possible contamination of surfaces, in particular by air-suspended dust particles.
  • Said process may be applied on a large scale, such as the scale of a sapphire wafer, for instance on an area of about 20 cm 2 , which can correspond to a round wafer with a diameter of 2 inches.
  • the invention also relates to a single-crystal thin film obtainable by a process as defined above.
  • the single-crystal thin film according to the invention may be used as a substrate for manufacturing a film of a two-dimensional material.
  • “Two-dimensional material” is typically a crystalline material consisting of a single layer of atoms or ions.
  • Typical examples of two- dimensional material include, but are not limited to, graphene, graphyne, molybdenum disulfide, borophene, germanene, silicene, phosphorene.
  • said two-dimensional material is graphene or molybdenum disulfide.
  • a process for manufacturing a film of a two-dimensional material may comprise a step of depositing a film of a two-dimensional material onto a single-crystal thin film of the invention. Accordingly, a process for manufacturing a film of a two-dimensional material may comprise the steps of :
  • step (c) depositing a film of a two-dimensional material onto the single-crystal thin film obtained in step (b).
  • Depositing a film of a two-dimensional material onto a single-crystal thin film of the invention may be carried out by any deposition techniques, and in particular by chemical vapor deposition.
  • said deposition may be carried out at a temperature of about 1000 °C.
  • the carbon source may be methane gas.
  • the single-crystal thin film according to the invention may also be used in electronics or plasmonics, in particular as a material for electronic or plasmonic devices.
  • the single-crystal thin film according to the invention may be used in plasmonic biosensors.
  • Example 1 Preparation of a single-crystal film of copper
  • a wafer of a (0001) sapphire was epi-polished to give a miscut towards the (a) plane, with an angle between 0.25° and 2°.
  • the miscut of the wafer was controlled by tilting the sample, mounted on a goniometer, from a nominal orientation using X-ray. Once the tilt has been fixed, the miscut surface is obtained by using mechano-chemical polishing.
  • Deposited thickness from 300 to 800 nm.
  • the sample was transferred through air to a furnace.
  • the furnace was sealed and 1 atm of gas (Argon + H 2 ) flowed at a rate of lOcc/min.
  • the temperature was increased to 980°C and the sample was annealed for times comprised between 1 h and 20 h.
  • the purest film tilted towards A grew into a single crystal within 6 h.
  • Typical slip bands running at 120° merge at the copper surface in the shape of steps were observed by AFM ( Figure 2). This is the signature of the single-crystal nature of the copper film with a (111) surface orientation. The steps appear during cooling, where the film is under compression on the sapphire substrate because of the different dilatation coefficients (higher in copper than in sapphire). No grain boundary or twin exist in the film.
  • EBSD Electro Backscatter Diffraction
  • the film crystallinity was controlled by an EBSD (Electron BackScatter Diffraction) mapping of several sample regions of about 250x200 microns.
  • the step average direction and the width of terraces of the sapphire substrate was controlled by AFM (Atomic Force Microscopy).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

L'invention concerne un procédé de préparation de films minces monocristallins de métaux ou d'alliages purs, par dépôt et croissance de grains sur un saphir (0001) présentant une mauvaise découpe comprise entre 0,2° et 5°, et orientés vers un plan spécifique. L'invention concerne également un film mince monocristallin pouvant être obtenu par un tel procédé et ses utilisations.
PCT/EP2019/073877 2018-09-10 2019-09-06 Procédé de préparation de films minces monocristallins WO2020053102A1 (fr)

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EP18306183.7 2018-09-10
EP18306183 2018-09-10

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WO2020053102A1 true WO2020053102A1 (fr) 2020-03-19

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112522669A (zh) * 2020-11-30 2021-03-19 天津大学 一种晶圆级单层硼烯的制备方法及晶圆级单层硼烯

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EP2540862A1 (fr) 2010-02-26 2013-01-02 National Institute of Advanced Industrial Science And Technology Stratifié de film de carbone
CN107190315A (zh) 2017-06-30 2017-09-22 北京大学 一种制备超平整无褶皱石墨烯单晶的方法
CN107354506A (zh) 2017-06-30 2017-11-17 北京大学 一种制备超平整铜单晶薄膜的方法

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EP2540862A1 (fr) 2010-02-26 2013-01-02 National Institute of Advanced Industrial Science And Technology Stratifié de film de carbone
CN107190315A (zh) 2017-06-30 2017-09-22 北京大学 一种制备超平整无褶皱石墨烯单晶的方法
CN107354506A (zh) 2017-06-30 2017-11-17 北京大学 一种制备超平整铜单晶薄膜的方法

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SIAH F ET AL: "In-plane anisotropic strain of ZnO closely packed microcrystallites grown on tilted (0001) sapphire", JOURNAL OF APPLIED PHYSICS, AMERICAN INSTITUTE OF PHYSICS, US, vol. 88, no. 5, 1 September 2000 (2000-09-01), pages 2480 - 2483, XP012051448, ISSN: 0021-8979, DOI: 10.1063/1.1287527 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112522669A (zh) * 2020-11-30 2021-03-19 天津大学 一种晶圆级单层硼烯的制备方法及晶圆级单层硼烯

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