EP3697941A1 - Méthode de synthèse d'un matériau bidimensionnel bn - Google Patents
Méthode de synthèse d'un matériau bidimensionnel bnInfo
- Publication number
- EP3697941A1 EP3697941A1 EP18786363.4A EP18786363A EP3697941A1 EP 3697941 A1 EP3697941 A1 EP 3697941A1 EP 18786363 A EP18786363 A EP 18786363A EP 3697941 A1 EP3697941 A1 EP 3697941A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- substrate
- implanted
- layer
- atoms
- annealing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000000463 material Substances 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 73
- 239000000758 substrate Substances 0.000 claims abstract description 124
- 238000000137 annealing Methods 0.000 claims abstract description 72
- 229910052796 boron Inorganic materials 0.000 claims abstract description 50
- 239000002356 single layer Substances 0.000 claims abstract description 43
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 42
- 238000005468 ion implantation Methods 0.000 claims abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000010410 layer Substances 0.000 claims description 132
- 238000002513 implantation Methods 0.000 claims description 40
- 238000009792 diffusion process Methods 0.000 claims description 35
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 230000008569 process Effects 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 11
- 238000005530 etching Methods 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 8
- 238000005538 encapsulation Methods 0.000 claims description 5
- 238000000407 epitaxy Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 125000004429 atom Chemical group 0.000 description 77
- 150000002500 ions Chemical class 0.000 description 21
- 125000004433 nitrogen atom Chemical group N* 0.000 description 16
- 230000015572 biosynthetic process Effects 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 238000001451 molecular beam epitaxy Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 5
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- 239000004926 polymethyl methacrylate Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000002156 adsorbate Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 229910052752 metalloid Inorganic materials 0.000 description 4
- 150000002738 metalloids Chemical class 0.000 description 4
- 230000035515 penetration Effects 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000000231 atomic layer deposition Methods 0.000 description 3
- 239000007943 implant Substances 0.000 description 3
- 239000012212 insulator Substances 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 229910003271 Ni-Fe Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000002800 charge carrier Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- -1 MoSe2 Chemical compound 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 229910003090 WSe2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005280 amorphization Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- BGECDVWSWDRFSP-UHFFFAOYSA-N borazine Chemical compound B1NBNBN1 BGECDVWSWDRFSP-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- ZOCHARZZJNPSEU-UHFFFAOYSA-N diboron Chemical compound B#B ZOCHARZZJNPSEU-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000012705 liquid precursor Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/48—Ion implantation
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- C—CHEMISTRY; METALLURGY
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/0242—Crystalline insulating materials
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/0254—Nitrides
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/76—Making of isolation regions between components
- H01L21/762—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers
- H01L21/7624—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers using semiconductor on insulator [SOI] technology
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0005—Separation of the coating from the substrate
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
- C23C14/5813—Thermal treatment using lasers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/20—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only AIIIBV compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/66977—Quantum effect devices, e.g. using quantum reflection, diffraction or interference effects, i.e. Bragg- or Aharonov-Bohm effects
Definitions
- the invention relates to the field of the synthesis of homogeneous layers and large areas of two-dimensional materials, called 2D materials, consisting of at least two different atoms, and more particularly the synthesis of hexagonal boron nitride h-BN.
- Two-dimensional Mat2D materials have been developed recently. They have a planar structure and are composed of one to a few tens or even a hundred L monolayers, each monolayer comprising a few atomic planes (typically 1 to 5), the number of planes being a function of the atomic structure.
- the chemical bonds within a monolayer are of the covalent type.
- FIG. 1A illustrates a stack of two layers of the hexagonal variety of h-BN seen in perspective
- FIG. 1B a monolayer seen from above
- FIG. 1C the stack of two monolayers L seen from above.
- 2D materials are different from conventional solid 3D materials for which, on the surface, the atoms have unsatisfied chemical bonds, called pendent bonds.
- pendent bonds the properties of the surface of the 2D materials are different from the surface properties of the bulk materials.
- the electronic properties of DCMTs depend on their chemical formula and the number of layers, they can be metallic or semiconductors.
- the h-BN material is insulating whatever the number of layers.
- h-BN can be used as a tunnel barrier.
- the electronic and optical properties of the 2D layers (graphene and DCMT) are much better when these layers are based on an h-BN multilayer and / or are covered with multilayers of h-BN.
- the electronic properties of a MoS 2 layer are significantly improved by encapsulation between two layers of h-BN, hBN (Top) and hBN (Bot) as described in the publication.
- the device is produced on an oxidized SiO 2 silicon substrate on Si.
- the use of h-BN in an electronic device typically requires the production, over a large area, of a 2D material consisting of from 20 to 100 monolayers of BN.
- the B and N atoms can also come from a single liquid precursor: borazine: B 3 H 6 N 3 .
- borazine B 3 H 6 N 3 .
- it remains difficult to obtain uniform multilayers of controlled thickness see Sun et al., Chem Soc Rev., 2018, 47, 4242-4257, for the CVD method.
- Very recently Uchida et al. (ACS Nano 12, 6236 (2018)) demonstrated the growth of several layers of h-BN with a thickness of 2-5 nm. They had to use a bimetallic Ni-Fe catalyst which has a stable fcc structure and which has a balanced solubility ratio for the B and N atoms (unlike a pure Fe film). They were able to segregate a multilayer h-BN.
- This method does not allow to obtain thick layers (10-30 nm) and are further synthesized on a NiFe layer obtained by sputtering. As such a layer is polyc stalline, the segregation inside the grains is different from that which occurs at the grain boundaries. The growth of the h-BN multilayer is then non-uniform on the grain size scale.
- An object of the present invention is to overcome the aforementioned drawbacks by proposing a method for synthesizing BN type 2D materials at a time. fast and allowing to obtain homogeneous and thick layers (10-30 nm) on large surfaces.
- a temperature and an annealing time are determined so that a diffusion length of the atoms of the implanted element or elements is between 5 and 10 nm.
- a single element delivery step is carried out by ion implantation, said implanted element being nitrogen N, the element B introducing step consisting of a deposition of a monocrystalline layer of said element. B on a first chemically inert support, the layer being called deposited layer and the element B being called deposited element, the deposited layer constituting said substrate.
- the first support is monocrystalline and the deposited layer is epitaxially grown on said first support.
- a part of the deposited layer that has not been transformed into a two-dimensional material after annealing is called a residual substrate, and the method comprises, after the annealing step, a step of separation of the at least one monolayer of two-dimensional material from said residual substrate and a step of transferring said at least one monolayer of two-dimensional material onto a destination substrate.
- the separation step comprises a sub-step of detaching the residual substrate from the first support using a laser, and a selective etching step of said residual substrate.
- the two delivery steps are carried out by ion implantation in the substrate.
- the substrate is insulating and monocrystalline.
- the substrate consists of a monocrystalline metal layer deposited on a second monocrystalline support, the element N and the element B being implanted in said metal layer.
- part of the substrate that is not transformed into a two-dimensional material after annealing is called a residual substrate
- the method comprises, after the annealing step, a step of separating the at least one monolayer of two-dimensional material from said residual substrate. and a step of transferring said at least one monolayer of two-dimensional material to a destination substrate.
- the separation step comprises a sub-step of detaching said residual substrate from the second support with the aid of a laser, and a selective etching step of said residual substrate.
- FIG. 3 illustrates a typical concentration profile of the atoms introduced by ion implantation in a given substrate at a given implantation energy E, measured in keV.
- Figure 6 shows the growth of BN layers according to the invention, in the example where both B and N elements are implanted.
- Figure 6a illustrates the implanted substrate and
- Figure 6b illustrates the 2D material layer obtained in the substrate after annealing.
- FIG. 7 illustrates a first variant of the process according to the invention in which the step of introducing the element B is carried out by depositing a thin layer of boron on a first chemically inert support.
- FIG. 8 illustrates an example of the first variant in which an element N implanted in a layer of material B.
- FIG. 10 illustrates an exemplary implementation of the method described in FIG. 9.
- FIG. 11 illustrates another example of implementation of the process described in FIG. 9, with a separation step comprising a laser separation sub-step and a selective etching step of the residual substrate.
- FIG. 12 illustrates a second variant of the process according to the invention for which the step of adding the N element and the step of introducing the element B each consist of an ion implantation in a chemically inert substrate.
- FIG. 13 illustrates a first option for performing double implantation, in which the implantation energies of elements B and N are determined so as to present their maximum concentration Rp N and Rp B at the same depth.
- FIG. 12 illustrates a second variant of the process according to the invention for which the step of adding the N element and the step of introducing the element B each consist of an ion implantation in a chemically inert substrate.
- FIG. 13 illustrates a first option for performing double implantation, in which the implantation energies of elements B and N are determined so as to present their maximum concentration Rp N and Rp B at the same depth.
- FIG. 14 illustrates the position of the Gaussian maximum of implantation of boron Rp B and nitrogen Rp N in a substrate of Si0 2 (silica) as a function respectively of the implantation energy E B of ions B and E N N ions, for the realization of h-BN.
- FIG. 15 shows different ways, in the case of a double implantation, to take account of the ex-diffusion of N.
- FIG. 16 illustrates the different steps of the second variant of the method according to a first embodiment in which the substrate, chemically inert with respect to N and B, is preferably monocrystalline and insulating.
- FIG. 18 illustrates another option of the method according to the invention, which comprises a step of separating the two-dimensional mat2D material from the residual substrate, and a step of recovering mat2D on a destination substrate.
- FIG. 19 illustrates the different steps of the second variant of the method according to the invention and according to a second embodiment, in which the elements N and B are implanted in a chemically inert substrate which is a thin layer of metal.
- Ion implantation is a material engineering process. As its name suggests, it is used to implant the ions of a chemical element in a solid material (target) thereby changing some of the physicochemical properties of this solid, especially at the surface. Ion implantation is used in the manufacture of semiconductor devices, for the surface treatment of metals, as well as for research in materials science.
- the ions allow both to change the physico-chemical properties of the target, but also the structural properties because the crystal structure of the target can be modified, damaged or even destroyed (amorphization).
- a source of ion production containing the atom to be implanted (gaseous, solid or liquid). Typically a plasma is created, and an electric field applied to the output of this source allows the extraction of ions. This beam Ionic then passes through a magnetic field where the ion to be implanted is selected according to its atomic mass and its charge,
- Ion acceleration typically reaches energies ranging from 1 to 500 keV or more.
- the depth of penetration is called the average depth of implantation of the atoms.
- the depth of penetration corresponds to Rp.
- the inventors have noted that the atomic densities of the monolayers of 2D materials, depending on the size of the elementary mesh and the number of atoms of each element in these, are very well adapted to the use of ion implantation. These densities are typically a few 10 15 atoms / cm 2 per monolayer
- monolayer L is understood to mean an elementary sheet as defined above.
- the material obtained by the method according to the invention and consisting of a monolayer or a stack of a plurality of monolayers L is called mat2D or material h-BN.
- the stack is also called a layer.
- the use of a layer of h-BN material in a device typically involves making a material consisting of at least twenty monolayers (up to about one hundred).
- the method 10 comprises a step 100 of adding the element B and a step 200 of adding the element N so as to form, in a substrate, a zone Z [M + X] comprising atoms of element B and atoms of the element N.
- at least one addition step is carried out by ion implantation.
- annealing step 300 makes it possible to form the at least one monolayer L of two-dimensional material mat2D by diffusion of said atoms in the substrate.
- a single delivery step is performed by ion implantation, and it is the element N which is implanted.
- the B feed step consists of a deposition of a boron layer on a chemically inert support (substrate).
- a boron layer can be likened to a metal layer.
- the boron layer is monocrystalline, obtained by epitaxy on a suitable substrate.
- the deposited element is denominated B, and L B the deposited layer.
- the element N is thus incorporated into a thin layer of the element B in a uniform manner by ion implantation.
- the deposition step of B is therefore carried out before the N implantation step.
- the Sub "substrate" in which the implanted element is implanted here consists essentially of the L B layer (atoms of the N element).
- zone Z [B + N] consists of the part of the layer L B which comprises implanted atoms, and according to a second variant, the two input stages are performed by ion implantation in the same substrate Sub chemically inert and stable at high temperature
- the order of implantation, first N or first B, is indifferent Zone Z [B + N] consists of the part of this Sub substrate which comprises N atoms and implanted B atoms.
- chemically inert substrate is meant a substrate whose constituent elements do not form parasitic compounds with the elements B or N of the 2D material during annealing.
- the substrate in which the implantation takes place is monocrystalline.
- Formation of the 2D material after ion implantation of the element (s) into the substrate (which may be a thin layer) requires high temperature annealing to activate diffusion of the implanted species (or species).
- well-defined diffusion coefficients for the implanted species
- the h-BN layer thus formed consisting of one or more monolayers of two-dimensional material according to the implanted dose, is homogeneous and crystalline.
- the annealing is carried out under appropriate conditions, mainly corresponding to a temperature, an atmosphere and a suitable duration.
- the annealing is carried out at "high" temperature, typically between 600 ° C. and 1200 ° C.
- an excimer laser for example XeCI for a wavelength of 308 nm
- a solid state laser for example a frequency-doubled or tripled Nd: YAG laser
- the fluence used is 0.1 to 1 Joule per cm 2 with the use of 1 to 10 pulses.
- the annealing time is generally much greater (1 to qq ⁇ ) than the duration of the laser pulse, the annealing times are much shorter than the annealing times in a furnace (minimum 1 minute for a furnace). fast annealing). This type of annealing can also be carried out under partial pressure of nitrogen.
- the annealing step of the method 10 according to the invention is preceded by a step encapsulating the substrate comprising zone Z with a high temperature stable material which is either a chemically inert dielectric such as SiO 2 , Al 2 O 3, HfCl 2, Si 3 N 4, or a metal such as Mo, W, Or.
- a high temperature stable material which is either a chemically inert dielectric such as SiO 2 , Al 2 O 3, HfCl 2, Si 3 N 4, or a metal such as Mo, W, Or.
- FIG. 5 shows the nucleation of a second monolayer L2 of BN over the first monolayer L1, and also the presence of zones without any monolayer.
- the atoms implanted in zone Z [B + N] are present in this zone in a very homogeneous manner over a large area.
- they are not located on the surface but in the substrate and do not need to travel over great distances to precipitate in the h-BN form as shown in FIG. 6a.
- the diffusion length of the implanted atoms during annealing must be greater than or equal to the distance between the position of the implanted atom and the position of the atom in the crystallized monolayer (s). This distance is at most equal to the distance traveled by an implanted atom located at the end of the Gaussian to reach the place where the crystallization starts (typically the peak implantation).
- a diffusion length much greater than this distance is undesirable, and therefore it is preferable to obtain a diffusion length substantially equal to this maximum path distance, which typically corresponds to a few Gaussian widths at half height FWHM. For example, 99.7% of the implanted atoms are at a distance of 2.55xFWHM. The maximum distance that must traverse the implanted atoms to integrate the crystalline zone BN is therefore of the order of 3xFWHM.
- the atoms implanted during the annealing typically of the order of a few nm to 10 nm, (obtained by controlling the annealing parameters such as temperature, atmosphere and duration), the atoms perform a slight displacement compared to the lengths. diffusion observed for the growth methods of those skilled in the art (up to several tens of microns). This avoids local stacks and holes in the hBN layer.
- the use of ion implantation and suitable annealing therefore favor the crystallization of homogeneous hBN layers.
- the ion implantation allows to control with a great precision the dose of implanted atoms (typically 1 .5% with the rule of 3 ⁇ ).
- N has a tendency to exo-diffuse.
- DN To compensate for this exo-diffusion one typically implements DN such that:
- the dose of B to be implanted is close to the final number B atoms in the mat2D material.
- the atomic density per unit area D 0 N of the element N in a monolayer of the two-dimensional material is equal to:
- the annealing parameters are determined, mainly temperature T and time t, so that the diffusion takes place under good conditions.
- D T be the diffusion coefficient of atoms at a temperature T.
- the diffusion length Ld of the atoms during annealing is approximately given by the formula:
- T and t are determined so that during annealing (see above):
- T and t are determined so that Ld N and Ld B are weak while respecting:
- the Sub r is the residual substrate, that is to say the portion of the uncrystallized substrate made of hBN material.
- the method according to the invention comprises, after the annealing step, a step of separating mat2D from the residual substrate Sub r and a step of transferring mat2D onto a Subd destination substrate. Examples are given below.
- the method according to the invention further comprises, after the annealing step, a step 370 of selective dissolution of the upper part of the residual substrate so as to expose the two-dimensional mat2D material.
- a step 370 of selective dissolution of the upper part of the residual substrate so as to expose the two-dimensional mat2D material.
- the interest is then that one can deposit directly on the h-BN a layer of a 2D semiconductor material such as MoS2, MoSe2, WS2, WSe2 etc.
- the step of supplying the deposited element B consists of a deposition of a preferably monocrystalline thin layer L B of B on a first support (substrate) Subse chemically inert.
- the layer L B is produced by epitaxy on the first Subi substrate ("MBE” for Molecular beam Epitaxy or “CVD” for Chemical Vapor Deposition) which is then necessarily monocrystalline. Subi then serves as growth germ.
- MBE Molecular beam Epitaxy
- CVD Chemical Vapor Deposition
- the monocrystalline arrangement of the L B layer favors the organized synthesis of mat2D, that is, monocrystalline growth (see above).
- the deposition of the layer L B is carried out by evaporation or sputtering.
- the deposition step of the layer L B is carried out by an atomic layer deposition method called ALD for "Atomic Layer deposition" in English.
- ALD atomic layer deposition method
- the implantation energy E (N) of the implanted element N is determined so that the location of the implanted element N is carried out in the deposited layer L B.
- FIG. 8 illustrates the example of an element N implanted in L M.
- the implanted element N has, in the zone in which it is located, a concentration C N (p) as a function of the penetration depth p.
- This curve conventionally has the shape of a Gaussian, whose maximum Rp N and the width at half height FWHM N is a function of E N , as explained above.
- FIG. 9 illustrates an embodiment of the method according to the first variant comprising, after the annealing step, a step 310 for separating the two-dimensional mat2D material from the residual layer L B r and a step 320 for transferring the mat2D material to a Subd destination substrate.
- selective etching is carried out of the unreacted residual material with the element N.
- the h-BN mat2D layer then floats by capillarity on the surface of the etching bath of the Boron, and is transferred to the Subd destination substrate according to one of the methods known to those skilled in the art, identical to the graphene transfer method, as illustrated in FIG.
- the separation step 310 comprises a sub-step of detachment of the residual substrate L r B (integrating the hBN layer) of the first substrate Subi using a laser and a sub-step selective etching of the residual substrate to isolate the hBN layer, as illustrated in FIG.
- 1 1 -1 is represented the initial stack consisting here of a layer of hBN encapsulated in a PMMA layer which will serve as intermediate support and localized on the residual layer L r B , itself deposited on Subi.
- En1 1-2 is shown the sub-step of detachment using a laser beam 50 ("laser lift off" in English).
- Laser lift-off This laser lift-off process is based on the difference in optical absorption between the (transparent) substrate and the L r B layer; Excimer lasers (near-UV wavelength) are typically used for a few ns of pulse duration. The energy of the laser is absorbed by the layer L r B , which produces a significant local elevation of the temperature, leading to the detachment of this layer.
- the laser can be incident "from above” and thus be directly focused on the top of the h-BN layer (without cross the substrate), so as to directly take off.
- the h-BN / PMMA stack is transferred to the Subd destination substrate consisting of oxidized silicon (Si0 2 on Si) and in 1 1 -6 the PMMA layer is removed and a layer is obtained. of h-BN material on the oxidized silicon substrate.
- the layer of 2D material matrix2D
- the residual layer L B r is found above mat2D very close to the upper surface and can then be etched chemically.
- the mat2D layer is then obtained directly (without transfer) on its substrate of insulating origin.
- the step 100 of adding the element N and the step 200 of introducing the element B consist of an ion implantation in a substrate Sub chemically inert, that is to say not chemically reacting with N or B.
- the energy E B of implantation of the element B and the energy E N of implantation of the element N are determined so as to present respectively a maximum R pB and R P N concentration C B (p) and C N (p) substantially equal to the depth p 0, as shown in Figure 13.
- FIG. 14 illustrates the position of the maximum of the Gaussian for the implantation of boron Rp B and nitrogen Rp N in an Si substrate of Si0 2 (silica) insulating as a function respectively of the energy of implantation E B of the ions B and E N of the ions N, for the realization of h-BN.
- E B of the ions B and E N of the ions N for the realization of h-BN.
- the element N is implanted at a depth greater than the implementation depth of the element B in the Sub substrate (see FIG. 15c).
- the depth is a function of the implantation energy.
- Zone Z [B + N] here consists of spatially separated N and B atoms before annealing.
- Figure 15 shows different ways, in the case of a double implantation, to take into account the exo-diffusion of N.
- the black corresponds to the element N and the dark gray to the element B.
- Figure 15a illustrates annealing under N 2 atmosphere
- figure 15b illustrates the increase of N dose
- figure 19c illustrates implantation at a different depth of N and B (deeper N)
- figure 15d illustrates encapsulation ( before annealing) with a thin layer of insulator (SiO 2 , Al 2 O 3 , Si 3 N 4 ...) or even metal, (Mo, W, Ni );
- Figure 15e encapsulation with a "top substrate”.
- FIG. 16 illustrates the different steps of the second variant of the method 10 according to a first embodiment according to which the substrate Sub (substrate in the sense of implantation), chemically inert and preferentially monocrystalline, is insulating.
- Sub substrate is typically selected from Al 2 0 3 , MgO, .Quartz, ...
- the substrate Sub is a layer epitaxied on a SubO substrate.
- DN is greater than nD 0 N, n being the number of monolayers desired.
- DB a dose of B ions to be implanted, slightly greater than or equal to nD 0 B.
- the DB dose to be implanted is preferably equal to very slightly higher than nD 0 N (see above).
- the respective doses of B DB ions and N DN ions are determined in such a way as to respect the stoichiometry of the elementary mesh of mat2D material and the desired number of layers n.
- the order of implantation between N and B is indifferent.
- a Z [B + N] region having N atoms and implanted B atoms is created in the vicinity of the depth p 0 in the Sub substrate.
- the implantation energy is determined with the help of FIG. 14 as a function of the desired depth for each element.
- FIG. 19 illustrates the different steps of the second variant of the method according to a second embodiment in which the elements N and B are implanted in a chemically inert Sub substrate which is a thin layer of metal L, which is preferentially monocrystalline.
- the metal is chosen from those in which the boron is very slightly soluble: gold, copper, platinum, but the implantation can also be carried out in a layer of Ni, Fe, ... or in an alloy of these materials (eg Ni-Fe).
- a metal layer therefore constitutes a chemically inert substrate as defined above.
- B atoms are implanted in the thin metal layer L met at a depth p0 included in the thickness of the metal layer.
- L met has a thickness of between a few nm and a few tens of nanometers.
- the layer L met is itself deposited on a second support / Sub2 substrate chemically inert, and preferably insulating and monocrystalline.
- the layer L sets is formed by epitaxy on Sub2.
- X atoms are implanted in the metal layer L starts at substantially the same depth p 0.
- a layer of mat2D is formed either at the interface with the air, at the surface of the metal layer, or inside the layer or at the interface with Sub2 .
- a portion L r is formed of the metal layer located between the mat2D layer and the substrate Sub2.
- this step is not easy to achieve by etching because the entry point of the liquid of the attack is only the slice of L r met .
- a separation as illustrated in Figure 1 1 comprising a sub-step of laser separation to make accessible L r met and a selective etching step of L r met (by dissolution of the metal), solves this problem.
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FR1701097A FR3072687A1 (fr) | 2017-10-20 | 2017-10-20 | Procede de realisation d'au moins une monocouche d'un materiau bidimensionnel et dispositif associe |
PCT/EP2018/078840 WO2019077158A1 (fr) | 2017-10-20 | 2018-10-22 | Méthode de synthèse d'un matériau bidimensionnel bn |
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