公开(公告)号：WO2016110385A1

公开(公告)日：2016-07-14

申请号：PCT/EP2015/079938

申请日：2015-12-16

Applicant: FORSCHUNGSVERBUND BERLIN E.V.

Inventor： GALAZKA, Zbigniew ,  UECKER, Reinhard ,  KLIMM, Detlef ,  BICKERMANN, Matthias

IPC: C30B29/16 ,  C30B15/20 ,  C30B17/00 ,  C30B11/00

CPC classification number: C30B29/16 ,  C30B11/005 ,  C30B11/006 ,  C30B15/08 ,  C30B15/20 ,  C30B15/34 ,  C30B17/00

Abstract: A method for growing beta phase of gallium oxide (β-Ga 2 O 3 ) single crystals from the melt contained within a metal crucible surrounded by a thermal insulation and heated by a heater. A growth atmosphere provided into a growth furnace has a variable oxygen concentration or partial pressure in such a way that the oxygen concentration reaches a growth oxygen concentration value (C2, C2', C2") in the concentration range (SC) of 5 - 100 vol. % below the melting temperature (MT) of Ga 2 O 3 or at the melting temperature (MT) or after complete melting of the Ga 2 O 3 starting material adapted to minimize creation of metallic gallium amount and thus eutectic formation with the metal crucible. During the crystal growth step of the β-Ga 2 O 3 single crystal from the melt at the growth temperature (GT) the growth oxygen concentration value (C2, C2', C2") is maintained within the oxygen concentration range (SC).

Abstract translation: 从包含在由绝热体包围并被加热器加热的金属坩埚内的熔体中生长氧化镓（β-Ga 2 O 3）单晶的β相的方法。 提供到生长炉中的生长气氛具有可变的氧浓度或分压，使得氧浓度达到浓度范围（SC）为5-100的生长氧浓度值（C2，C2'，C2“） 体积％低于Ga 2 O 3的熔融温度（MT），在熔融温度（MT）下或完全熔化之后，适于最小化金属镓的量的产生，并因此与金属坩埚形成共晶，在晶体生长步骤期间 在生长温度（GT）下，熔体中的β-Ga2O3单晶的生长氧浓度值（C2，C2'，C2“）保持在氧浓度范围（SC）内。

公开(公告)号：WO2013159808A1

公开(公告)日：2013-10-31

申请号：PCT/EP2012/057447

申请日：2012-04-24

Applicant: FORSCHUNGSVERBUND BERLIN E.V. ,  GALAZKA, Zbigniew ,  UECKER, Reinhard ,  FORNARI, Roberto

Inventor： GALAZKA, Zbigniew ,  UECKER, Reinhard ,  FORNARI, Roberto

IPC: C30B11/00 ,  C30B11/14 ,  C30B29/16

CPC classification number: C30B30/04 ,  C30B11/00 ,  C30B11/002 ,  C30B11/003 ,  C30B11/007 ,  C30B11/14 ,  C30B29/16 ,  H01F1/01 ,  Y10T117/1004

Abstract: A method and apparatus for growing truly bulk ln 2 O 3 single crystals from the melt, as well as melt-grown bulk ln 2 O 3 single crystals are disclosed. The growth method comprises a controlled decomposition of initially non-conducting ln 2 O 3 starting material (23) during heating-up of a noble metal crucible (4) containing the ln 2 O 3 starting material (23) and thus increasing electrical conductivity of the ln 2 O 3 starting material with rising temperature, which is sufficient to couple with an electromagnetic field of an induction coil (6) through the crucible wall (24) around melting point of ln 2 O 3 . Such coupling leads to an electromagnetic levitation of at least a portion (23.1) of the liquid ln203 starting material with a neck (26) formation acting as crystallization seed. During cooling down of the noble metal crucible (4) with the liquid ln 2 O 3 starting material at least one bulk ln 2 O 3 single crystal (28.1, 28.2) is formed. We named this novel crystal growth method the "Levitation-Assisted Self-Seeding Crystal Growth Method". The apparatus for growing bulk ln 2 O 3 single crystals from the melt comprises an inductively heated thermal system with a noble metal crucible (4) and evacuation passages (22, 22.1) for gaseous decomposition products of ln 2 O 3 , while keeping very low temperature gradients. Various configurations of the induction coil (6), the noble metal crucible (4) and a lid (12) covering the crucible can be utilized to obtain very low temperature gradients, sufficient evacuation passages and a high levitation force. The electrical properties of the melt grown ln 2 O 3 single crystals can be modified in a wide range by at least one heat treatment in suitable atmospheres and appropriate temperatures.

Abstract translation: 公开了一种用于从熔体中生长真正体积的ln 2 O 3单晶以及熔融生长的体积ln 2 O 3单晶的方法和装置。 生长方法包括在包含ln 2 O 3起始材料（23）的贵金属坩埚（4）的加热期间初始不导电的In2O3起始材料（23）的受控分解，从而增加ln 2 O 3起始材料的电导率随着上升 温度，其足以与感应线圈（6）的电磁场通过坩埚壁（24）在ln 2 O 3的熔点附近耦合。 这种耦合导致至少一部分（23.1）的液体ln203起始材料与用作结晶种子的颈部（26）形成的电磁悬浮。 在用液体ln 2 O 3起始材料冷却贵金属坩埚（4）时，形成至少一个体积ln 2 O 3单晶（28.1,28.2）。 我们将这种新型晶体生长方法命名为“悬浮辅助自种晶体生长法”。 用于从熔体生长大量ln 2 O 3单晶的装置包括具有贵金属坩埚（4）的感应加热的热系统和用于ln 2 O 3的气体分解产物的排气通道（22,22.1），同时保持非常低的温度梯度。 可以利用感应线圈（6），贵金属坩埚（4）和覆盖坩埚的盖（12）的各种构造来获得非常低的温度梯度，足够的排气通道和高悬浮力。 通过在合适的气氛和合适的温度下进行至少一次热处理，熔体生长的ln2O3单晶的电性能可以在很宽的范围内进行修饰。

公开(公告)号：EP3242965A1

公开(公告)日：2017-11-15

申请号：EP15810626.0

申请日：2015-12-16

Applicant: Forschungsverbund Berlin E.V.

Inventor： GALAZKA, Zbigniew ,  UECKER, Reinhard ,  KLIMM, Detlef ,  BICKERMANN, Matthias

IPC: C30B29/16 ,  C30B15/20 ,  C30B17/00 ,  C30B11/00

CPC classification number: C30B29/16 ,  C30B11/005 ,  C30B11/006 ,  C30B15/08 ,  C30B15/20 ,  C30B15/34 ,  C30B17/00

Abstract: A method for growing beta phase of gallium oxide (²-Ga 2 O 3 ) single crystals from the melt contained within a metal crucible surrounded by a thermal insulation and heated by a heater. A growth atmosphere provided into a growth furnace has a variable oxygen concentration or partial pressure in such a way that the oxygen concentration reaches a growth oxygen concentration value (C2, C2', C2") in the concentration range (SC) of 5 - 100 vol. % below the melting temperature (MT) of Ga 2 O 3 or at the melting temperature (MT) or after complete melting of the Ga 2 O 3 starting material adapted to minimize creation of metallic gallium amount and thus eutectic formation with the metal crucible. During the crystal growth step of the ²-Ga 2 O 3 single crystal from the melt at the growth temperature (GT) the growth oxygen concentration value (C2, C2', C2") is maintained within the oxygen concentration range (SC).

公开(公告)号：EP2841630B1

公开(公告)日：2017-04-12

申请号：EP12717273.2

申请日：2012-04-24

Applicant: Forschungsverbund Berlin E.V.

Inventor： GALAZKA, Zbigniew ,  UECKER, Reinhard ,  FORNARI, Roberto

IPC: C30B11/00 ,  C30B11/14 ,  C30B29/16 ,  C30B30/04 ,  H01F1/01

CPC classification number: C30B30/04 ,  C30B11/00 ,  C30B11/002 ,  C30B11/003 ,  C30B11/007 ,  C30B11/14 ,  C30B29/16 ,  H01F1/01 ,  Y10T117/1004

公开(公告)号：EP2841630A1

公开(公告)日：2015-03-04

申请号：EP12717273.2

申请日：2012-04-24

Applicant: Forschungsverbund Berlin E.V.

Inventor： GALAZKA, Zbigniew ,  UECKER, Reinhard ,  FORNARI, Roberto

IPC: C30B11/00 ,  C30B11/14 ,  C30B29/16

CPC classification number: C30B30/04 ,  C30B11/00 ,  C30B11/002 ,  C30B11/003 ,  C30B11/007 ,  C30B11/14 ,  C30B29/16 ,  H01F1/01 ,  Y10T117/1004

Abstract: A method and apparatus for growing truly bulk ln
2 O
3 single crystals from the melt, as well as melt-grown bulk ln
2 O
3 single crystals are disclosed. The growth method comprises a controlled decomposition of initially non-conducting ln
2 O
3 starting material (23) during heating-up of a noble metal crucible (4) containing the ln
2 O
3 starting material (23) and thus increasing electrical conductivity of the ln
2 O
3 starting material with rising temperature, which is sufficient to couple with an electromagnetic field of an induction coil (6) through the crucible wall (24) around melting point of ln
2 O
3 . Such coupling leads to an electromagnetic levitation of at least a portion (23.1) of the liquid ln203 starting material with a neck (26) formation acting as crystallization seed. During cooling down of the noble metal crucible (4) with the liquid ln
2 O
3 starting material at least one bulk ln
2 O
3 single crystal (28.1, 28.2) is formed. We named this novel crystal growth method the "Levitation-Assisted Self-Seeding Crystal Growth Method". The apparatus for growing bulk ln
2 O
3 single crystals from the melt comprises an inductively heated thermal system with a noble metal crucible (4) and evacuation passages (22, 22.1) for gaseous decomposition products of ln
2 O
3 , while keeping very low temperature gradients. Various configurations of the induction coil (6), the noble metal crucible (4) and a lid (12) covering the crucible can be utilized to obtain very low temperature gradients, sufficient evacuation passages and a high levitation force. The electrical properties of the melt grown ln
2 O
3 single crystals can be modified in a wide range by at least one heat treatment in suitable atmospheres and appropriate temperatures.

Abstract translation: 一种用于从熔体生长真正散装氧化铟单晶的方法和设备，以及熔融生长的本体氧化铟单晶是游离缺失盘。 的生长方法，包括的期间（4），其含有氧化铟原料（23）的贵金属坩埚升温INITIALLY非导电氧化铟原料（23）和因此增加了氧化铟的导电性起始材料与上升的受控分解 温度，在所有这足以夫妇与在通过坩埚壁（24）周围的氧化铟熔点的感应线圈（6）的电磁场。 搜索耦合导致具有一个颈部（26）的形成作为结晶晶种的液态氧化铟原料的至少部分（23.1）的电磁悬浮的。 在冷却过程中，贵金属坩埚（4）与所述液体氧化铟原料至少一个本体氧化铟单晶（28.1，28.2）的向下形成。 我们命名这个新的晶体生长方法的“悬浮辅助自种晶体生长方法”。 为与贵金属坩埚（4）和排气通路（22，22.1），用于氧化铟的气态分解产物从感应加热热系统的熔融包括生长块状氧化铟单晶，同时保持非常低的温度梯度的装置。 感应线圈（6）的各种配置中，所述贵金属坩埚（4）和盖（12）覆盖所述坩埚可以用于获得非常低的温度梯度，充排气通路和高的悬浮力。 熔体生长单晶氧化铟可以在宽的范围内由至少一个热处理在合适的气氛和合适的温度被修改的电性能。

公开(公告)号：EP3242965B1

公开(公告)日：2019-06-26

申请号：EP15810626.0

申请日：2015-12-16

Applicant: Forschungsverbund Berlin E.V.

Inventor： GALAZKA, Zbigniew ,  UECKER, Reinhard ,  KLIMM, Detlef ,  BICKERMANN, Matthias

IPC: C30B29/16 ,  C30B15/20 ,  C30B17/00 ,  C30B11/00

公开(公告)号：EP1264012A1

公开(公告)日：2002-12-11

申请号：EP01919157.6

申请日：2001-03-02

Applicant: Forschungsverbund Berlin e.V.

Inventor： SPEIT, Burkhard ,  REICHE, Peter ,  KLIMM, Detlef ,  DONECKER, Jörg ,  GANSCHOW, Steffen ,  UECKER, Reinhard ,  MÜLLER, Bernd

IPC: C30B29/12 ,  C30B11/00 ,  C30B33/02 ,  G02B1/02 ,  C01F11/22

CPC classification number: C30B33/00 ,  C30B29/12 ,  Y10T117/10

Abstract: The invention relates to a method for producing crystals and/or crystal materials. According to said method, unwanted impurities are removed from the crystal and/or the material by means of a purification agent or a getter. Substances containing elementary fluorine and/or reactive fluorine are used as the purification agent or getter. Preferred getters are XeF2 and/or carbon fluoride. Crystals obtained in this way are suitable for use as optical components.