WO2011071098A1 - Materiau en silicium pour element d'emission infrarouge, et element d'emission infrarouge - Google Patents

Materiau en silicium pour element d'emission infrarouge, et element d'emission infrarouge Download PDF

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Publication number
WO2011071098A1
WO2011071098A1 PCT/JP2010/072083 JP2010072083W WO2011071098A1 WO 2011071098 A1 WO2011071098 A1 WO 2011071098A1 JP 2010072083 W JP2010072083 W JP 2010072083W WO 2011071098 A1 WO2011071098 A1 WO 2011071098A1
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Prior art keywords
transmitting member
infrared transmitting
silicon
infrared
polycrystalline silicon
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PCT/JP2010/072083
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English (en)
Japanese (ja)
Inventor
浩司 続橋
洋 池田
昌弘 金井
三郎 脇田
哲也 東条
Original Assignee
三菱マテリアル株式会社
三菱マテリアル電子化成株式会社
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Publication of WO2011071098A1 publication Critical patent/WO2011071098A1/fr

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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/02Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of crystals, e.g. rock-salt, semi-conductors
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/037Purification
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B28/00Production of homogeneous polycrystalline material with defined structure
    • C30B28/04Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/06Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B13/00Optical objectives specially designed for the purposes specified below
    • G02B13/14Optical objectives specially designed for the purposes specified below for use with infrared or ultraviolet radiation

Definitions

  • the present invention relates to a silicon material for an infrared transmitting member used as a material for an infrared transmitting member such as a lens member or a prism member that transmits infrared in an infrared laser device and the like, and an infrared transmitting member made of the silicon material for the infrared transmitting member.
  • an infrared transmitting member such as a lens member or a prism member that transmits infrared laser light is provided using a semiconductor crystal material such as germanium or silicon as shown in Patent Document 1, for example.
  • a semiconductor crystal material such as germanium or silicon
  • compound crystal materials such as calcium fluoride (CaF 2 ) and zinc selenium (ZnSe) are also used. These materials are appropriately selected and used according to the application in consideration of the refractive index and transmittance.
  • germanium is a material that transmits infrared rays having a wavelength of 2 to 20 ⁇ m, has a relatively large refractive index of about 4 and has a small change in refractive index depending on the wavelength, and is suitable as a lens member.
  • germanium has a problem that it cannot be widely used as an infrared transmitting member such as a lens member or a prism member because it is a relatively expensive material with a small reserve.
  • the transmittance decreases when the temperature exceeds about 100 ° C., and cannot be used in an environment where the temperature increases.
  • silicon is widely used as a solar cell and a semiconductor substrate, and is a material that can be obtained at a lower cost than germanium.
  • the refractive index is relatively large as about 3.5 and the change in the refractive index due to the wavelength is small, so that it is suitable for constituting a lens member.
  • the silicon described above has a large absorption peak at a wavelength of about 9 ⁇ m although it has a high transmittance for infrared rays having a wavelength of 1.2 to 6 ⁇ m. For this reason, silicon has been used only as a material for an infrared transmitting member for infrared rays having a narrow wavelength range of 1.2 to 6 ⁇ m.
  • Patent Document 1 discloses that the absorption of infrared rays having a wavelength of 8 to 12 ⁇ m is suppressed by reducing the thickness of the lens member. However, most of infrared rays having a wavelength of about 9 ⁇ m are absorbed. It will be done. Further, the shape of the lens member is also limited to a Fresnel lens or the like. Therefore, silicon cannot be widely used as an infrared transmitting member for infrared rays having a wavelength of 8 to 12 ⁇ m.
  • the present invention has been made in view of the above-described situation, and can provide a transmittance for infrared rays having a wavelength of around 9 ⁇ m (8 to 12 ⁇ m) and can be used in a wide wavelength range. It is an object to provide a silicon material for an infrared transmitting member used as an infrared transmitting member and an infrared transmitting member made of the silicon material for an infrared transmitting member.
  • the silicon material for an infrared transmitting member is a silicon material for an infrared transmitting member used as a material for an infrared transmitting member such as a lens or prism that transmits infrared rays, and is polycrystalline.
  • the polycrystalline silicon is characterized by having a resistivity of 1 ⁇ cm or more and an oxygen concentration of less than 1.0 ⁇ 10 18 atoms / cc (atoms / cm 3 ).
  • the silicon material for an infrared transmitting member having this configuration has a resistivity of 1 ⁇ cm or more and an oxygen concentration of less than 1.0 ⁇ 10 18 atoms / cc.
  • the absorption of infrared rays having a wavelength of around 9 ⁇ m (8 to 12 ⁇ m) is caused by oxygen contained in the silicon crystal. Therefore, by setting the oxygen concentration to less than 1.0 ⁇ 10 18 atoms / cc, it is possible to suppress the absorption of infrared rays having a wavelength of about 9 ⁇ m (8 to 12 ⁇ m), and the infrared transmitting member usable in a wide wavelength range. It can be used as a material.
  • the oxygen concentration is preferably less than 5.0 ⁇ 10 17 atoms / cc, and more preferably less than 1.0 ⁇ 10 16 atoms / cc.
  • the oxygen concentration can be reduced relatively easily as compared with single crystal silicon, and infrared absorption can be suppressed as described above.
  • this silicon material for an infrared transmitting member there are crystal grain boundaries inside.
  • the infrared laser has a relatively low output, it is not necessary to consider the influence of scattering at the crystal grain boundaries. .
  • the average crystal grain size of the polycrystalline silicon is 3 mm or more and 20 mm or less.
  • the average crystal grain size of polycrystalline silicon is 3 mm or more, when an infrared transmitting member is formed using this silicon material for infrared transmitting member, the grain boundary existing inside the infrared transmitting member The number is reduced, and scattering of infrared rays can be suppressed. Therefore, even when the infrared laser has a high output, it is possible to use the silicon material for the infrared transmitting member. Further, since the average crystal grain size of polycrystalline silicon is 20 mm or less, this polycrystalline silicon can be produced relatively easily.
  • the polycrystalline silicon is produced by a unidirectional solidification method.
  • polycrystalline silicon is produced by the unidirectional solidification method, impurities are discharged from the solid side to the liquid side at the solid-liquid interface, and high-purity polycrystalline silicon can be obtained. . Therefore, the oxygen concentration in the silicon material for an infrared transmitting member can be reliably reduced, and infrared absorption can be suppressed.
  • it since it is unidirectionally solidified, columnar crystals grow in the direction of solidification, and the crystal grain size can be made relatively large.
  • the polycrystalline silicon may be doped with B or Al.
  • the resistivity can be adjusted by doping silicon with B or Al, and the resistivity of the polycrystalline silicon can be reliably set to 1 ⁇ cm or more.
  • the infrared transmitting member according to the present invention is manufactured using the aforementioned silicon material for infrared transmitting member. Since the infrared transmitting member having this configuration is made of polycrystalline silicon having a resistivity of 1 ⁇ cm or more and an oxygen concentration of less than 1.0 ⁇ 10 18 atoms / cc, it absorbs infrared rays having a wavelength of about 9 ⁇ m. Can be suppressed, and infrared rays having a wide range of wavelengths can be transmitted.
  • lens member which consists of a silicon material for infrared transmission members which is an embodiment of the present invention. It is explanatory drawing which shows the measuring method of the average crystal grain diameter of a polycrystalline silicon. It is a schematic explanatory drawing of the manufacturing apparatus of the polycrystalline silicon which is the silicon material for infrared rays transmissive members which is embodiment of this invention.
  • the silicon material for an infrared transmitting member according to the present embodiment is composed of polycrystalline silicon formed by a unidirectional solidification method. That is, it has a structure in which a plurality of columnar crystals extend upward from the lower part.
  • the resistivity of this polycrystalline silicon is 1 ⁇ cm or more.
  • the resistivity of the polycrystalline silicon was measured by a four-probe method (JIS H 0602: a resistivity measurement method by a four-probe method of a silicon single crystal and a silicon wafer).
  • the oxygen concentration is less than 1.0 ⁇ 10 18 atoms / cc.
  • This oxygen concentration is measured by the FT-IR method (JEIDA-61: standard measurement of interstitial oxygen atom concentration in silicon by infrared absorption, JEITA EM-3503 (former JEIDA-56): in silicon crystals by infrared absorption. (Standard measurement of substitutional carbon atom concentration).
  • the oxygen concentration is preferably less than 5.0 ⁇ 10 17 atoms / cc, and more preferably less than 1.0 ⁇ 10 16 atoms / cc.
  • the average crystal grain size of this polycrystalline silicon is set to 3 mm or more and 20 mm or less.
  • the crystal grain size is measured by the following method. As shown in FIG. 2, measurement samples 2, 3, and 4 are collected by slicing the lower portion, the central portion, and the upper portion in the height direction (one-direction solidification direction) of the polycrystalline silicon ingot 1. The surface texture of each measurement sample is observed, and the number of crystal grain boundaries 6 intersecting the reference straight line S is counted. By dividing the length of the reference line S by the number of crystal grain boundaries 6 intersecting the reference line S, the average crystal grain size of each measurement sample is obtained. Then, the average crystal grain size of the polycrystalline silicon ingot 1 is calculated from the measurement results of these measurement samples.
  • the polycrystalline silicon manufacturing apparatus 20 includes a crucible 21 in which the silicon melt L is stored, a chill plate 22 on which the crucible 22 is placed, an underfloor heater 23 that supports the chill plate 22 from below, and a crucible 21. And a ceiling heater 24 disposed above. A heat insulating material 25 is provided around the crucible 21.
  • the crucible 21 is made of silica whose horizontal cross-sectional shape is square (square) or round (circular).
  • the chill plate 22 has a hollow structure, and Ar gas is supplied to the inside through a supply pipe 26.
  • a silicon raw material is charged into the crucible 21.
  • This silicon raw material is melted by energizing and heating the ceiling heater 24 and the underfloor heater 23.
  • the silicon melt L is stored in the crucible 21.
  • the oxygen concentration is less than 1.0 ⁇ 10 18 atoms / cc.
  • the crystal grain size can be increased, and the average crystal grain size of polycrystalline silicon can be set to 3 mm or more and 20 mm or less.
  • the silicon material for the infrared transmitting member and the lens member 10 made of this silicon material for the infrared transmitting member according to the present embodiment having such a configuration is made of polycrystalline silicon and has an oxygen concentration of 1.0 ⁇ . Since it is less than 10 18 atoms / cc, preferably less than 5.0 ⁇ 10 17 atoms / cc, more preferably less than 1.0 ⁇ 10 16 atoms / cc, the wavelength is about 9 ⁇ m due to oxygen in the silicon crystal. It becomes possible to suppress absorption of infrared rays (8 to 12 ⁇ m).
  • the silicon material for the infrared transmitting member according to the present embodiment is made of polycrystalline silicon, the oxygen concentration can be reduced relatively easily as compared with single crystal silicon, and the absorption of infrared rays can be suppressed. It becomes possible.
  • polycrystalline silicon is produced by the unidirectional solidification method, impurities are discharged from the solid side to the liquid side at the solid-liquid interface. Obtainable. Therefore, the oxygen concentration in the silicon material for an infrared transmitting member can be reliably reduced, and infrared absorption can be suppressed.
  • it is unidirectionally solidified columnar crystals grow in the direction of solidification, and the crystal grain size can be made relatively large.
  • the average crystal grain size of the polycrystalline silicon is 3 mm or more and 20 mm or less, the number of crystal grain boundaries existing inside the lens member 10 made of this silicon material for infrared transmitting member is reduced, and infrared rays are reduced. Can be suppressed. Therefore, even when the output of the infrared laser is high, it is possible to use an infrared transmitting member such as the lens member 10 made of the silicon material for the infrared transmitting member.
  • the lens member 10 (convex lens) as shown in FIG. 1 has been described as an example of the infrared transmitting member, but the present invention is not limited to this, and other lens members such as a concave lens, a Fresnel lens, and a meniscus lens. It may be a prism member that transmits infrared rays and controls the traveling direction of infrared rays.
  • silicone material for infrared rays transmissive members which consists of polycrystalline silicon using the polycrystalline silicon manufacturing apparatus shown in FIG. 3, it is not limited to this, Other polycrystalline silicon manufacturing apparatuses May be used.
  • a silicon material for an infrared transmitting member can be used as a material for an infrared transmitting member that can secure transmittance even for infrared rays having a wavelength of around 9 ⁇ m (8 to 12 ⁇ m), And the infrared rays transmission member which consists of this silicon material for infrared rays transmission members can be provided.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Optics & Photonics (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Silicon Compounds (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

L'invention concerne un matériau en silicium pour élément d'émission infrarouge, qui peut émettre des rayons infrarouges dont la longueur d'onde est approximativement de 9µm et qui est utilisé comme matière pour matériau d'émission infrarouge qui peut servir dans une large zone de longueur d'onde. L'invention concerne également un élément d'émission infrarouge formé à partir dudit matériau en silicium pour élément d'émission infrarouge. Le matériau en silicium pour élément d'émission infrarouge, qui est utilisé comme matière pour matériaux d'émission infrarouge tels que lentilles ou prismes, qui émettent respectivement des rayons infrarouges, est formé à partir de silicium polycristallin, et se caractérise en ce que la résistivité dudit silicium polycristallin est d'au moins 1Ωcm, et la teneur en oxygène est inférieure à 1.0×1018atoms/cc.
PCT/JP2010/072083 2009-12-09 2010-12-09 Materiau en silicium pour element d'emission infrarouge, et element d'emission infrarouge WO2011071098A1 (fr)

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JP2009-279522 2009-12-09
JP2009279522A JP5437039B2 (ja) 2009-12-09 2009-12-09 赤外線透過部材及び赤外線透過部材用シリコン材料

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Cited By (1)

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WO2018151140A1 (fr) * 2017-02-20 2018-08-23 株式会社トクヤマ Fil de noyau destiné à être utilisé dans le dépôt de silicium, méthode de production dudit fil de noyau et méthode de production de silicium polycristallin

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US9496330B2 (en) * 2013-08-02 2016-11-15 Semiconductor Energy Laboratory Co., Ltd. Oxide semiconductor film and semiconductor device
TWI541396B (zh) * 2013-12-20 2016-07-11 中美矽晶製品股份有限公司 用於晶碇鑄造爐的冷卻裝置及鑄造晶碇之方法
WO2016174947A1 (fr) * 2015-04-28 2016-11-03 カーリットホールディングス株式会社 Élément optique formé de matériau au silicium et dispositif optique le comprenant
WO2017115797A1 (fr) * 2015-12-28 2017-07-06 カーリットホールディングス株式会社 Matériau de silicium, élément optique comprenant celui-ci, et dispositif optique
WO2017126394A1 (fr) * 2016-01-18 2017-07-27 住友電気工業株式会社 Composant optique
JP2017128491A (ja) * 2016-01-18 2017-07-27 住友電気工業株式会社 光学部品

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JP2005303045A (ja) * 2004-04-13 2005-10-27 Mitsubishi Materials Corp シリコン部材およびその製造方法
JP2009084149A (ja) * 2008-10-31 2009-04-23 Sharp Corp 板状シリコン製造用直線加工部材、下地板製造方法ならびに下地板、板状シリコンならびに太陽電池
JP2009203499A (ja) * 2008-02-26 2009-09-10 Mitsubishi Materials Corp ターゲット材およびその製造方法

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JP5489614B2 (ja) * 2008-12-19 2014-05-14 株式会社トクヤマ 光学部材の製造方法
WO2010074074A1 (fr) * 2008-12-24 2010-07-01 株式会社 村田製作所 Élément optique de transmission de rayonnement de lumière infrarouge et son procédé de fabrication ainsi que dispositif optique et équipement optique
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JPH11310496A (ja) * 1998-02-25 1999-11-09 Mitsubishi Materials Corp 一方向凝固組織を有するシリコンインゴットの製造方法およびその製造装置
JP2005303045A (ja) * 2004-04-13 2005-10-27 Mitsubishi Materials Corp シリコン部材およびその製造方法
JP2009203499A (ja) * 2008-02-26 2009-09-10 Mitsubishi Materials Corp ターゲット材およびその製造方法
JP2009084149A (ja) * 2008-10-31 2009-04-23 Sharp Corp 板状シリコン製造用直線加工部材、下地板製造方法ならびに下地板、板状シリコンならびに太陽電池

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018151140A1 (fr) * 2017-02-20 2018-08-23 株式会社トクヤマ Fil de noyau destiné à être utilisé dans le dépôt de silicium, méthode de production dudit fil de noyau et méthode de production de silicium polycristallin
JPWO2018151140A1 (ja) * 2017-02-20 2019-12-12 株式会社トクヤマ シリコン析出用芯線、該芯線の製造方法、および多結晶シリコンの製造方法
US11254579B2 (en) 2017-02-20 2022-02-22 Tokuyama Corporation Core wire for use in silicon deposition, method for producing said core wire, and method for producing polycrystalline silicon

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JP2011123185A (ja) 2011-06-23

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