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    • 8. 发明授权
      US3160476A Process of producing compact boron, particularly in monocrystalline form 失效
    • Process of producing compact boron, particularly in monocrystalline form
    • 生产紧密硼，特别是单晶形式的方法
    • US3160476A
    • 1964-12-08
    • US17749662
    • 1962-03-05
    • SIEMENS AG
    • ERHARD SIRTL
    • C01B35/02 , C23C16/28 , C30B25/00 , C30B25/02
    • C30B25/00 , C01B35/023 , C23C16/28 , C30B25/02 , C30B29/02
    • Monocrystalline boron is prepared by passing a stream of reaction gas containing a halogen-containing boron compound and purified hydrogen over a heated carrier element, whereby boron is deposited on said carrier, and adding initially to the reaction gas a hydrogen halide which displaces the teaction equilibrium in favour of combined boron, in such a proportion that the temperature T0 at which boron removal from the carrier by reverse reaction commences, is disposed at most 200 DEG C. below the temperature T at which the boron liberation reaction is carried out and the boron liberation is completely stopped below the temperature T0. The hydrogen halide added is preferably the one formed during the reaction, e.g. HCl or HBr and the boron compounds may be BCl3, BClBr2 or BBr2Cl. The carrier is rod shaped or filamentary and may be of moulded boron, e.g. presintered boron powder or monocrystalline boron and is crystallographically oriented so that the rod axis lies in a crystal alignment which corresponds to a determined preferential growth alignment. The carrier is heated electrically to a temperature not below 1200 DEG K, a low temperature modification of boron being formed at 1300 DEG K and a high temperature form at 1700 DEG K. The surface may be cleaned by etching and purifying in a high vacuum, or by heating in a current of pure H2 and the vessel flushed out with a H2 flow containing at least 10 mol. % of hydrogen halide. Alternatively the oxide film is a multiple of the layer thickness of the oxide film is removed by heating in a gas mixture containing a hydrogen halide in such quantity that neither B nor Si (impurity) are deposited and thereafter reducing the supply of halide so that boron only is deposited. The temperature of the carrier and the mol. ratios of the reaction gases are adjusted so that the temperature lies below the minimum separation temperature of silicon but above that of boron. If required, the quantity of silicon deposited may be controlled by varying the hydrogen halide concentration. The atomic ratio of B : H is preferably at least 2%, e.g. the mol. ratio of BCl3 : H2 may be 1 : 10 and the maximum Si : B ratio is 0.1%. The reaction gas may be prepared by passing pure hydrogen through an evaporation vessel containing a liquid halogen containing boron compound, e.g BCl3, some of which is converted to hydrogen halide by water and using the hydrogen leaving the vessel as reaction gas. Waste gas after passage over the carrier may be reused for a second carrier element. Doped boron may be prepared using elements of Group II and IV in the form of their gaseous compounds, e.g. beryllium halides and compounds of carbon and silicon. The reaction chamber may be lined with corundum and the remaining parts made of glasses using aluminium borate in combination with quartz-like AlPO4, BPO4.
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