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
  • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
  • C30B11/002—Crucibles or containers for supporting the melt
• • 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
  • C30B29/16—Oxides
  • C30B29/20—Aluminium oxides
• • 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
  • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
  • C30B35/002—Crucibles or containers
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
  • Y10T117/10—Apparatus
  • Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
  • Y10T117/1032—Seed pulling
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
  • Y10T117/10—Apparatus
  • Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
  • Y10T117/1092—Shape defined by a solid member other than seed or product [e.g., Bridgman-Stockbarger]

Definitions

• the present invention relates to a crucible for crystal growth, in particular a sapphire single crystal, a method for sapphire crystal growing with such a crucible and a use of such a crucible for sapphire Einkristallzucht.
• the single crystal growth of sapphire single crystals has been intensively pursued for several years, since monocrystalline sapphire substrates are used in particular for the epitaxial deposition of gallium nitride (GaN), which is used for the production of, inter alia, LEDs (light emitting diodes) and certain semiconductor lasers is widely used.
• GaN gallium nitride
• Various methods of growing single crystals of sapphire single crystals are known.
• Metal wherein the metal has a melting point of at least 1800 ° C.
• the crucible has a base crucible of W, Mo, Re or an alloy of these materials and an inner lining of W, Mo, Re or an alloy of these materials.
• the basic crucible is essentially pot-shaped
• the inner lining comprises at least a cup-shaped first section which covers a bottom region of the base crucible and a jacket-shaped second section which at least partially covers a wall region of the base crucible.
• the first section and the second section are formed by separate components.
• a W-Mo alloy, a W-Re alloy, a Mo-Re alloy or a W-Mo-Re alloy understood. Since the base crucible is provided with the inner liner, repeated use of the Basalt crucible for sapphire crystal growth allows in which for the production of a further single crystal only the inner lining needs to be renewed.
• the inner lining can with a much lower
• Wall thickness be executed as the base crucible, whereby a significant material savings is achieved.
• a corrosion of the base crucible caused by the A 2 O melt is at least largely avoided, so that a significantly increased service life of the base crucible is achieved. Since the inner lining has the pot-shaped first portion and the jacket-shaped second portion, which are formed by separate components, is a particularly efficient and
• Inner lining is tight with respect to Al 2 O 3 melt. Due to the
• the cup-shaped first portion can be made particularly efficient and inexpensive by forming from a film.
• the preparation may e.g. by deep drawing, pressing or pressing with appropriate shapes.
• the jacket-shaped second section can be produced in a particularly efficient and cost-effective manner by winding from a film.
• the first section and the second section are preferably made of the same material. Compared with a production of an inner lining of a component, a more cost-effective production is achieved, in which in particular the first portion can be efficiently cup-shaped.
• the first portion and the second portion may be fixedly connected to each other.
• the two sections may in particular be so firmly connected to each other that the inner lining with respect to the Al 2 0 3 melt is tight and this does not come into contact with the material of the base crucible.
• the fixed connection can in particular by a material connection, for example by welding, together
• first portion and the second portion may be e.g. also only lie sealingly against each other.
• a second section formed by a wound film may also be placed with its lower end in the first section and there through its
• Residual stress i. his coasting force, and if necessary, the by
• the base crucible and the inner lining are preferably matched to one another in such a way that the inner lining can be detached from the base crucible together with the single crystal of sapphire after the single crystal growth.
• This can in particular by a suitable choice of material for the base crucible and the inner lining, by a suitable adjustment of the dimensions of the base crucible and the
• Inner lining and be achieved by structuring the contact areas between the base crucible and the inner lining.
• cup-shaped first portion is formed by forming from a film, a particularly cost-effective production is made possible with a dense configuration of the inner lining in the bottom region of the crucible is achieved.
• the forming may be e.g. be done by deep drawing or by pressing or pressing in an appropriate form.
• the second section is formed from a wound film, a particularly efficient and cost-effective production of the second section is made possible.
• the second section may be formed by a film that belongs to a substantially hollow cylindrical shape is wound, wherein the connection point is formed such that these with respect to
• the first section and the second section are materially connected to one another. In this case, it is reliably ensured that the inner lining is dense with respect to Al 2 O 3 melt and that it does not come into contact with the base crucible.
• material-locking connection can e.g. be realized by welding or Vereedem.
• the first portion and the second portion are connected to each other via mutually engaging portions of the first portion and the second portion.
• the first portion and the second portion can be an area of the first
• this type of connection can be made with a material connection, e.g. by welding or sintering.
• a material connection e.g. by welding or sintering.
• a particularly reliable and resilient connection is provided.
• a structure is provided for facilitating the separability of the inner liner from the base crucible after formation of a sapphire single crystal.
• At least the outer side of the inner lining may be provided with a surface structuring.
• Surface structuring may e.g. by embossing in the material of the
• the surface structuring may be formed so as to facilitate the separability of the inner liner and the base crucible after the formation of a sapphire single crystal.
• the surface structuring may be designed such that the inner lining only touches the base crucible in regions.
• the crucible has a base crucible of W, Mo, Re or an alloy of these materials and an inner lining of W, Mo, Re or an alloy of these materials.
• the base crucible is substantially pot-shaped and the inner lining has a smaller wall thickness than the base crucible.
• the structure may e.g. from the material of
• Inner lining and / or base crucible It is e.g. However, also possible to design the structure as a separate element that at least partially between the base crucible and the inner lining
• the structure is characterized by a
• the structure is characterized by a separate
• Intermediate element is formed, which is arranged between the inner lining and the base crucible. It is e.g. possible to provide the intermediate element anywhere between the inner liner and the base crucible, but e.g. Also, the intermediate element only partially between the
• inner lining and the base crucible Provide inner lining and the base crucible.
• Form intermediate element in the form of a profiled, in particular corrugated, film which is arranged as a spacer at least partially between the inner lining and the base crucible.
• the melting of the Al 2 O 3 powder and the formation of the sapphire single crystal can ensure the distancing of the base crucible and the inner lining.
• the intermediate element can be destroyed, for example, in particular by breaking due to high brittleness of the intermediate element.
• the intermediate element may preferably also be made of W, Mo, Re or a
• Intermediate layer makes it possible to reduce the stresses acting on the single crystal formed, since stresses caused by different thermal expansions (in particular of the monocrystal and the crucible formed) can be absorbed by the intermediate layer, so that lower-tension crystals can be achieved. In this way, an increased quality of the crystals formed is made possible.
• the outside of the inner lining may be provided with ahexstruktuntation.
• the surface texture may be e.g. be introduced by embossing in the material of the inner lining and / or the base crucible.
• the heatnstruktuntation can be designed such that the inner lining touches the base crucible only partially.
• Thethermstruktuntation can in particular be designed such that the inner lining due to the heatstruktun réelle in large areas of the
• Inner wall of the base crucible is kept at a distance. In this way, good separability of the single crystal (including the inner lining) from the base crucible can be ensured.
• Inner lining can be easily and efficiently separated from the base crucible. Since the basic crucible is provided with the inner lining, a
• the inner lining can be designed with a significantly lower wall thickness than that
• the inner lining has a
• Wall thickness ⁇ 1 mm preferably ⁇ 0.5 mm, more preferably between 0.05 mm and 0.5 mm, on.
• the inner lining can be efficiently removed by deformation from e.g. produce a corresponding film.
• a high degree of material savings is realized with such a thin-walled design.
• at least the inner lining has a degree of purity of> 99%, preferably> 99.9%, so that contamination of the
• the degree of purity refers to how large the proportion of other constituents in addition to the
• Base material or the elements of the base alloy may be maximum.
• the base crucible also has a corresponding degree of purity.
• At least the inner lining of pure Mo is formed with a purity of> 99%, preferably> 99.9%.
• the inner lining can be provided at a high degree of purity in a satisfactory cost frame.
• the material of the inner lining is different from the material of the base crucible.
• the inner liner may be made of pure Mo or a high Mo alloy
• the base crucible may be made of W or a high-W alloy.
• the base crucible on the one hand a low thermal expansion and thus in particular a low shrinkage in a cooling after the formation of the single crystal, which has a favorable effect on the removability of the single crystal, and on the other hand, the
• Inner lining are provided relatively inexpensive and the risk of sticking between the inner liner and the base crucible can be minimized.
• other combinations of materials are possible, with which both a reliable bonding of inner liner and base crucible can be prevented, as well a good removability of the single crystal is ensured.
• various of the materials Mo, W, Re can be used for the inner lining and the base crucible or different alloys of these elements.
• the object is also achieved by a method for sapphire single crystal growth with such a crucible, in which a sapphire monocrystal is formed by solidification from the melt, starting from a bottom region of the crucible.
• the single crystal formation can be carried out starting from a seed crystal, which is arranged in the bottom region of the crucible.
• the object is also achieved by use of such a crucible in a method for sapphire single crystal growth in which a sapphire single crystal is formed by solidification from the melt, starting from a bottom region of the crucible.
• FIG. 1 shows a schematic representation of a crucible for crystal growth according to an embodiment
• FIG. 2 shows a schematic representation of a structure for facilitating the
• FIG. 3 shows a schematic illustration of a possible connection of a first section and a second section of an inner lining
• Fig. 4 is a schematic representation of a modification in which a
• Structure is formed to facilitate the separability of the inner lining of the base crucible by a separate intermediate element
• FIG. 5 shows a schematic representation of a crucible for crystal growth according to a modification of the embodiment.
• Fig. 1 is a schematic representation of crucible -1- for crystal growth according to an embodiment.
• the crucible -1- is specially designed for crystal growth of sapphire single crystals.
• the crucible -1- has a pot-shaped base crucible -2-, the off
• W tungsten
• Mo mobdenum
• Re rhenium
• an alloy formed from at least two of these elements can be made.
• cup-shaped base pot -2- is made in one piece from the described material, wherein the material preferably has a purity> 99%, preferably
• the outer crucible is e.g. made of high purity W.
• the base crucible -2- has a bottom area -2a and a peripheral wall area -2b-.
• the base crucible -2- can in particular be designed substantially rotationally symmetrical about an axis -A-.
• the base crucible -2- may e.g. be produced by powder metallurgy production by pressing, sintering and, if necessary, subsequent mechanical processing.
• the crucible may e.g. in the wall area -2b- one
• Wall thickness between about 5 mm and 25 mm, preferably between 10 mm and 20 mm and in the bottom region -2a of up to 40 mm.
• the base crucible -2 from a sheet by deep drawing, pressing or pressing.
• the starting sheet for example, a thickness between 1 and 12 mm, preferably between 2 and 6 mm exhibit.
• a base crucible -2- is shown with a substantially uniform wall thickness in FIG. 1, the wall thickness can vary both in the base region 2a and in the wall region 2b -b.
• the base crucible -2- can in particular be manufactured by powder metallurgy from the desired material or the desired alloy.
• the crucible -1- further comprises an inner lining -3-, with the
• the inner lining -3- may also be made of W (tungsten), Mo (molybdenum), Re (rhenium) or an alloy formed from at least two of these elements.
• the material of the inner lining preferably has a purity of> 99%, preferably> 99.9%.
• the inner lining -3- is e.g. made of high purity Mo
• the inner lining -3- has a cup-shaped first portion -4-, which covers the bottom portion -2a of the base crucible -2-, and a jacket-shaped second portion -5-, the wall portion -2b- of the base crucible -2- at least partially covered , on.
• the cup-shaped first section -4- is made by forming from a film and has substantially a rotational symmetry about the
• the first section -4- may e.g. be made by deep drawing from a film.
• the first section -4- has a the
• Wall portion -2b- of the base crucible -2- substantially parallel to the wall portion -2b- extends, so that a bottom and side closed pot or tub shape is formed.
• the circumferential side wall -4b- has a height in the range between 10 mm and 25 mm, preferably between 10 mm and 15 mm.
• the cup-shaped first section -4- has both in the region of the bottom -4a and in the region of the side wall -4b- a wall thickness between 0.05 mm and 1 mm, preferably between 0.05 mm and 0.75 mm, more preferably between 0.05 mm and 0.5 mm.
• the second section -5- of the inner lining -3- is also made of a film.
• the second section -5- is formed as a separate component.
• the second section -5- is made of the same material as the first section -4-.
• the second section -5- is formed by winding a sheet-like film into a substantially hollow cylindrical shape. The film is wound up in such a way that the two end edges are arranged overlappingly and firmly connected to one another, e.g. by a fold and / or by welding or sintering. However, it is e.g. also possible that the end edges are only tightly against each other.
• the first section -4- and the second section -5- are arranged such that the two sections overlap in a circumferential area.
• the overlapping area may be e.g. be about 10 mm wide.
• Section -4- and the second section -5- are firmly interconnected in the overlapping area, e.g. by a fold and / or by
• first section -4- and the second section -5- can also be connected to each other alternatively or additionally by interengaging areas, as shown schematically in Fig. 3. In the illustration of Fig. 3, both the side wall -4b- of the first portion -4- and the second portion -5- in the
• the two previously described interconnected end edges of the second section -5- be interconnected by interengaging areas.
• the second portion -5- is disposed in the overlapping area outside the first portion -4-.
• the inner lining -3- and the base crucible -2- are made of different materials or different alloys.
• the materials or alloys are chosen such that in a sapphire crystal growth in the crucible -1- (ie at the high temperatures required here) no sticking between the inner lining -3- and the base crucible -2- occurs. If the inner lining -3- and the base crucible -2- are made of different materials, the tendency is to one
• the materials are chosen such that both the base crucible -2- and the inner lining -3- have sufficient mechanical strength.
• the material combination is further selected in relation to the respective thermal expansion of the materials such that the single crystal formed together with the inner lining -3- can be removed from the base crucible -2-.
• a structure for facilitating the separability of the inner lining -3- from the base crucible -2- may also be provided after formation of a sapphire single crystal.
• At least one outer side of the inner lining -3- and / or at least one inner side of the Grundtiegels -2- be provided with a surface structuring, which facilitates the removability of the single crystal formed from the crucible -1-.
• a surface structuring which facilitates the removability of the single crystal formed from the crucible -1-.
• a surface structuring which causes the inner lining -3- is not applied over a large area of the material of the base crucible -2-, but to a certain distance from the inside of the inner lining -3- of the
• Inner diameter of the base crucible -2- leads In addition to generating the surface structuring by embossing, other methods can be used, in particular the
• Inner lining -3- to be provided with a surface structuring, which causes the inner lining -3- does not lie over large areas flat against the material of the basic crucible -2-.
• a surface structuring which causes the inner lining -3- does not lie over large areas flat against the material of the basic crucible -2-.
• Base pot -2- is arranged. It should be noted that the figures are only schematic representations, the wall thicknesses of the individual components not necessarily in the right proportion
• the intermediate element -6- may e.g. be formed by a profiled film, which is provided as a spacer between the base crucible -2- and the inner lining -3-.
• the intermediate element -6- is formed from W, Mo, Re or an alloy of these materials.
• Base pot -2- is provided in the form of a surface structuring or in the form of a separate intermediate element -6-.
• sapphire-Einkristallzucht is a single-crystalline
• Sapphire seed crystal with a given crystallographic orientation in the bottom region of the crucible -1- arranged inside the inner lining -3- and the crucible -1- is filled up to a predetermined filling level with Al 2 O 3 starting material.
• the Al 2 O 3 starting material is converted by a controlled increase in temperature in a liquid melt and the seed crystal countercooled so that this melts on its surface, but is not completely melted.
• a sapphire single crystal is slowly deposited from the melt, starting from the seed crystal.
• the formed sapphire single crystal, together with the inner lining -3- is removed from the base crucible -2.
• the base crucible -2- is then again provided with an inner lining -3- and can be used again for sapphire crystal growth.
• the seed crystal is placed in the bottom region of the crucible -1-, it is also possible, for example, to use the crucible in a process in which the seed crystal is immersed from above in Al 2 O 3 melt, the Formation of the sapphire single crystal starting from this
• Seed crystal takes place and the forming sapphire single crystal in the

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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)
• Crystals, And After-Treatments Of Crystals (AREA)

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• 2011
  • 2011-08-05 AT ATGM445/2011U patent/AT12783U1/de not_active IP Right Cessation
• 2012
  • 2012-08-03 JP JP2014523142A patent/JP5964963B2/ja not_active Expired - Fee Related
  • 2012-08-03 WO PCT/AT2012/000206 patent/WO2013020153A1/de not_active Ceased
  • 2012-08-03 US US14/237,267 patent/US20140174341A1/en not_active Abandoned
  • 2012-08-03 KR KR1020147002892A patent/KR20140048231A/ko not_active Withdrawn

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