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    • 1. 发明专利
    • Method of filling container with high-purity monosilane
    • 用高纯度单体填充容器的方法
    • JPS6162699A
    • 1986-03-31
    • JP18277384
    • 1984-09-03
    • Mitsui Toatsu Chem Inc
    • HIAI ATSUHIKOWAKIMURA KAZUOTANAKA MASAOFUKUDA NOBUHIRO
    • F17C5/00F17C6/00
    • F17C6/00F17C2221/012F17C2221/037F17C2223/0153F17C2227/0135F17C2227/0157Y02E60/321
    • PURPOSE:To fill a container with high-purity monosilane gas by retaining monosilane under reflux in a storing tank for a liquid monosilane, and then filling the container with the monosilane from the storing tank. CONSTITUTION:Monosilane is formed by reducing chlorosilane group by a reducing agent and reacting alloys such as Mg2Si and the like upon hydrochloric acid or ammonium chloride, and is accompanied by refined hydrogen. The monosilane is condensated and stored in a storing tank. In the storing tank, after the monosilane is retained under reflux, preferably, in the state of boiling to the vicinity of boiling point temperature of the monosilane, the monosilane is drawn out by a pump from the lower portion of the storing tank, and heated by a vaporizer to be filled in a container. The monosilane may be drawn out from the vapor phase portion of the storing tank retained under reflux by a compressor to be filled in the container.
    • 目的:通过将甲硅烷回流保存在用于液体单硅烷的储存罐中,然后用储存罐中的甲硅烷填充容器,来填充高纯度甲硅烷气体的容器。 构成:通过还原剂还原氯硅烷,并将合金如Mg2Si等与盐酸或氯化铵反应形成甲硅烷,伴随精炼氢气。 将甲硅烷冷凝并储存在储存罐中。 在储存罐中,在甲硅烷保持回流之后,优选在沸点至甲硅烷的沸点温度附近的状态下,通过泵从存储罐的下部引出单甲硅烷,并加热 通过蒸发器填充在容器中。 甲硅烷可以从保存在回流下的储存罐的气相部分中被压缩机引出以填充到容器中。
    • 2. 发明专利
    • Manufacture of polychloro silane
    • 聚氯硅烷的制造
    • JPS59184720A
    • 1984-10-20
    • JP5798683
    • 1983-04-04
    • Mitsui Toatsu Chem Inc
    • TOYODA YOSHIAKIWAKIMURA KAZUOHASE TADAHARUKIDO OSAMUKITANO NOBUHIRO
    • C01B33/107
    • PURPOSE: To increase the reaction yield, and to prevent the loss caused by scattering the particles of staring materials and the product by specifying the introducing condition of a chlorine-contg. gas into the particle-fixed layer of a reactor when an alloy of metal and Si, and Si particles are chlorinated at a high temp.
      CONSTITUTION: An alloy of a metal such as calcium silicon, magnesium silicon, ferrosilicon and Si or Si particles are charged into a reactor having a stirrer for mixing powder to form a fixed layer. The thicknesss of the layer can be chosen at will if the layer has a certain degree of thickness so as to be easily mixed by the stirrer. A chlorine-contg. gas is introduced in such a condition that the fixed layer is not fluidized and particles are not accompanied. The fixed layer is mixed continuously or intermittently by above-mentioned stirrer to carry out chlorination by a solid-gas reaction.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:提高反应产率,并通过指定氯气的引入条件来防止由于起泡物质和产物的散射而引起的损失。 当金属和Si和Si颗粒的合金在高温下氯化时,气体进入反应器的颗粒固定层。 构成:将金属如硅钙,镁硅,硅铁和Si或Si颗粒的合金装入具有用于混合粉末以形成固定层的搅拌器的反应器中。 如果该层具有一定的厚度以便通过搅拌器容易地混合,则可以随意选择该层的厚度。 氯气 在固定层不流化并且不伴随颗粒的条件下引入气体。 固定层通过上述搅拌器连续或间歇地混合,通过固体气体反应进行氯化。
    • 3. 发明专利
    • Treatment of synthetic liquid for chlorination containing polychlorosilane
    • 用于含有聚氯乙烯的氯化合成液的处理
    • JPS59116119A
    • 1984-07-04
    • JP22389882
    • 1982-12-22
    • Mitsui Toatsu Chem Inc
    • TOYODA YOSHIAKIWAKIMURA KAZUOHASE TADAHARUKIDO OSAMUKITANO NOBUHIRO
    • C01B33/107
    • PURPOSE: To inactivate smoothly a solid substance ignitable under a shock produced as a by-product when a synthetic liq. for chlorination contg. polychlorosilanes is treated, by bringing the solid substance into contact with HF.
      CONSTITUTION: When an alloy consisting of a metal and Si such as Ca-Si, Mg- Si or ferrosilicon or Si itself is chlorinated at a high temp., a synthetic liq. for chlorination contg. various polychlorosilanes is obtd. The synthetic liq. is liq. at ordinary temp. When part of the synthetic liq. contacts with water or wet air, a white solid substance ignitable under a shock is inevitably produced as a by-product in a manufacturing apparatus or on the surface of the apparatus. The solid substance is brought into contact with gaseous HF or an aqueous HF soln. The solid substance is inactivated, and the danger of ignition can be avoided.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:使合成物质在产生副产物的冲击下平稳地灭活固体物质。 用于氯化 通过使固体物质与HF接触来处理聚氯代硅烷。 构成:当由金属和Si组成的合金如Ca-Si,Mg-Si或硅铁或Si本身在高温下氯化时,合成液体。 用于氯化 各种聚氯代硅烷是有效的。 合成液体 是liq。 在普通的温度 当部分合成液体。 与水或湿空气接触,在冲击下可点燃的白色固体物质不可避免地作为制造设备中或设备表面上的副产物产生。 使固体物质与气态HF或HF水溶液接触。 固体物质灭活,可以避免点燃的危险。
    • 4. 发明专利
    • Novel manufacture of silicon hydride
    • 硅胶的新制造
    • JPS59116117A
    • 1984-07-04
    • JP22300882
    • 1982-12-21
    • Mitsui Toatsu Chem Inc
    • IWAO TETSUYATOYODA YOSHIAKIWAKIMURA KAZUOKITANO NOBUHIROTANAKA MASAO
    • C01B33/04
    • C01B33/04C01B33/043
    • PURPOSE: To obtain silicon hydride with an inexpensive reducing agent in a high yield while reducing the production of by-products when silicon halide is reduced with alkyl aluminum hydride to manufacture silicon hydride, by using a mixture of said alkyl aluminum hydride with a restricted amount of trialkyl aluminum.
      CONSTITUTION: An industrially inexpensive and easily available mixture of alkyl aluminum hydride (expressed as a compound A hereunder) with trialkyl aluminum (expressed as a compound B hereunder) contains a relatively large amount of the compound B. Part of the compound B is removed from the mixture by a conventional method such as distillation or recrystallization so as to regulate the amount of the compound B to ≤10mol% of the amount of the compound A. By using the resulting mixture as a reducing agent for silicon halide, the production of by-products such as hydrosilicon halide and ethane is considerably reduced without deteriorating the action of the compound A, and silicon hydride is obtd. in a high yield.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:为了以高产率以廉价的还原剂获得氢化硅,同时通过使用烷基氢化铝还原卤化硅制造氢化硅,同时减少副产物的产生,通过使用所述烷基氢化铝与限制量的混合物 的三烷基铝。 构成:将烷基氢化铝(以下表示为化合物A)与三烷基铝(以下表示为化合物B)的工业上便宜且易于获得的混合物含有相对大量的化合物B.将化合物B的一部分从 该混合物通过常规方法如蒸馏或重结晶,以便将化合物B的量调节至化合物A的量的<10mol%。通过使用所得混合物作为卤化硅的还原剂,生产 副产物如氢化硅卤化物和乙烷显着降低,而不会降低化合物A的作用,并且可以获得氢化硅。 以高收益。
    • 5. 发明专利
    • High-purity monosilane
    • 高纯度单体
    • JPS6163518A
    • 1986-04-01
    • JP18277884
    • 1984-09-03
    • Mitsui Toatsu Chem Inc
    • HIAI ATSUHIKOWAKIMURA KAZUOTANAKA MASAOFUKUDA NOBUHIRO
    • C01B33/04
    • PURPOSE: A high-purity monosilane useful as an amorphous silicon solar cell, by making the monosilane having ≤ specific contents of nitrogen and oxygen.
      CONSTITUTION: A chlorosilane (e.g., silicon tetrachloride, etc.) and a reducing agent (alkyl aluminum hydride) are bubbled sufficiently with a hydrogen gas, so that a nitrogen content is ≤1ppm, and an oxygen content is ≤0.5ppm. Then, the reduction reaction is carried out to give a crude monosilane gas, the greater part of contained unreduced substance and hydrocarbon are condensed and separated. Substantially the whole amount of a condensable gas in the prepared uncondensed gas is condensed, the condensed solution is partially evaporated to give the monosilane containing a very small amount of impurities, which is treated with an adsorbent, and purified. The purified monosilane is liquefied, stored in a holder with a reflux condenser, and stored under reflux. The monosilane is evaporated, and packed into a container, to give a high-purity monosilane having ≤1ppm nitrogen and ≤0.5ppm oxygen.
      COPYRIGHT: (C)1986,JPO&Japio
    • 目的:用作非晶硅太阳能电池的高纯度硅烷,通过使具有<=氮和氧的特定含量的甲硅烷。 构成:将氯硅烷(例如四氯化硅等)和还原剂(烷基铝氢化物)用氢气充分鼓泡,使得氮含量<= 1ppm,氧含量<0.5ppm。 然后,进行还原反应,得到粗制的甲硅烷气体,大部分含有未还原物质和烃的物质被冷凝和分离。 基本上将制备的未冷凝气体中的可冷凝气体的总量冷凝,冷凝的溶液被部分蒸发,得到含有非常少量杂质的甲硅烷,其用吸附剂处理并纯化。 将纯化的甲硅烷液化,储存在具有回流冷凝器的保持器中,并回流储存。 将甲硅烷蒸发并装入容器中,得到具有<= 1ppm氮和<= 0.5ppm氧的高纯度甲硅烷。
    • 6. 发明专利
    • Method of filling container with monosilane
    • 用单体填充容器的方法
    • JPS6162700A
    • 1986-03-31
    • JP18277684
    • 1984-09-03
    • Mitsui Toatsu Chem Inc
    • HIAI ATSUHIKOWAKIMURA KAZUOTANAKA MASAO
    • F17C5/00F17C6/00
    • F17C6/00F17C2221/012F17C2221/014F17C2223/0161F17C2227/0135F17C2227/04F17C2260/037Y02E60/321
    • PURPOSE:To safely conduct a work by disposing three or more layers of packings on a pressure-up rotary device for filling a container layer packing side space and inert gas in an outer layer packing side space. CONSTITUTION:Liquid monosilane in a product holder 2 is filled from a line 3 through a line 5 and carburetor 6 in a container 7 by a pressure-up rotary device 4. Three or more layers of packings 9, 10, 11 are inserted in the ground seal portion 8 of the device 4, thereby to form plural space portions 12, 13. Hydrogen gas is poured in the inner layer space portion 12 from a line 14, and inert gas such as nitrogen gas and the like is poured in the outer layer space portion 13. In this arrangement, monosilane which leaks from the device will be accompanied by hydrogen gas to be collected, and further diluted to be discharged to the outside of a system to avoid the danger or ignition.
    • 目的:通过在压层旋转装置上放置三层或更多层的填料来安全地进行工作,以在外层填料侧空间填充容器层填料侧空间和惰性气体。 构成:产品保持架2中的液体单硅烷通过加压旋转装置4从管线3通过管线5和容器7中的化油器6填充。将三层或更多层填料9,10,11插入 从而形成多个空间部分12,13,从管线14将氢气注入内层空间部分12中,将惰性气体如氮气等倒入外层空间部分12中。 在这种布置中,从装置泄漏的甲硅烷将伴随着要收集的氢气,并进一步稀释以排放到系统的外部,以避免危险或点燃。
    • 7. 发明专利
    • Method of purifying monosilane
    • 净化单体的方法
    • JPS6163517A
    • 1986-04-01
    • JP18277584
    • 1984-09-03
    • Mitsui Toatsu Chem Inc
    • HIAI ATSUHIKOWAKIMURA KAZUOTANAKA MASAOFUKUDA NOBUHIRO
    • C01B33/04
    • PURPOSE: To provide a high-purity monosilane, by storing a liquid monosilane in a storage tank, and keeping the monosilane under reflux.
      CONSTITUTION: A hydrogen-containing monosilane which is produced and puri fied by a conventional procedure is condensed and stored in a storage tank. The storage tank is equipped with a back-flow condenser, the monosilane is kept approximately at -112°C, the boiling point of the monosilane, and refluxed by the back-flow condenser. Consequently, gases such as oxygen, nitrogen, hydrogen, argon, etc. having lower boiling points than the monosilane has are removed, and the high-purity monosilane having low content of low-boiling impurities is obtained. The monosilane thus prepared is taken out from the bottom of the storage tank, heated by an evaporater, packed into a container, and shipped.
      COPYRIGHT: (C)1986,JPO&Japio
    • 目的:提供高纯度甲硅烷,通过将液体单硅烷储存在储罐中,并保持甲硅烷回流。 构成:通过常规方法制备和纯化的含氢单硅烷冷凝并储存在储罐中。 储罐配有回流冷凝器,甲硅烷保持在约-112℃,即甲硅烷的沸点,并由回流冷凝器回流。 因此,除去沸点低于甲硅烷的氧,氮,氢,氩等气体,得到低沸点杂质含量低的高纯度甲硅烷。 如此制备的单硅烷从储罐的底部取出,由蒸发器加热,装入容器中并运输。
    • 8. 发明专利
    • Production of monosilane
    • 生产单体
    • JPS6163515A
    • 1986-04-01
    • JP18277284
    • 1984-09-03
    • Mitsui Toatsu Chem Inc
    • HIAI ATSUHIKOWAKIMURA KAZUOTANAKA MASAOFUKUDA NOBUHIRO
    • C01B33/04
    • PURPOSE: In producing a monosilane by reducing a chlorosilane shown by a specific formula, a monosilane having an extremely high purity, can be produced by using a chlorosilane containing substantially neither nitrogen nor oxygen as a reducing agent.
      CONSTITUTION: In producing a monosilane by reducing one or more chlorosilanes shown by the formula SiH
      n Cl
      4-n (n is 0, 1, 2, or 3), raw materials of reaction system such as the chlorosilane, a reducing agent, etc. are degassed under re duced pressure, or purged with hydrogen, so that the raw materials are treated in such a way that they contain 2 G at about 10W150°C, to form a monosilane. The monosilane is stripped with hydro gen, purified with an adsorbent, condensed, a hydrogen gas is separated by a gas-liquid separator, to give the monosilane having extremely high purity.
      COPYRIGHT: (C)1986,JPO&Japio
    • 目的:通过还原特定配方所示的氯代硅烷来制造甲硅烷,可以通过使用基本上不含氮或氧的氯硅烷作为还原剂来制造纯度非常高的单硅烷。 构成:通过还原一种或多种式SiHnCl4-n(n为0,1,2或3)所示的氯硅烷生产甲硅烷,将反应体系如氯硅烷,还原剂等的原料脱气 在压力下或用氢气吹扫,使得原料以这样的方式被处理,使得它们含有约0.5ppm的氧气。 基本上完全除去氮气和氧气并进料到反应器中的氯硅烷,还原剂等,并在约10-150℃下以约0-10kg / cm 2 G还原,形成 甲硅烷 用氢化物除去甲硅烷,用吸附剂纯化,冷凝,用气 - 液分离器分离氢气,得到具有极高纯度的单甲硅烷。
    • 9. 发明专利
    • Production of silane
    • 生产硅烷
    • JPS59128393A
    • 1984-07-24
    • JP5883
    • 1983-01-05
    • Mitsui Toatsu Chem Inc
    • TOYODA YOSHIAKIIWAO TETSUYAWAKIMURA KAZUOHASE TADAHARUKIDO OSAMUKITANO NOBUHIRO
    • C01B33/04C07F7/12
    • PURPOSE: To obtain the titled compound useful as a synthetic raw material, etc., in high yield, without producing by-products, by adding a specific amount of an alkyl-Al halide to a composition composed of an alkyl-Al hydride, trialkyl-Al and fine Al powder, and reducing polyhalosilane using said mixture.
      CONSTITUTION: A composition composed mainly of (A) an alkylaluminum hydride and containing (B) a trialkylaluminum and (C) fine aluminum powder is added with (D) an alkylaluminum halide of formula AlR
      n X
      3-n (R is 1W10C alkyl; n is 0, 1 or 1.5; X is halogen). The amount of the component (D) is less than 1.8 times the amount necessary to convert the whole component (B) in the composition to dialkylaluminum monohalide but sufficient to decrease the residual amount of the component (B) in the composition to ≤10mol% of the component (A). The objective compound can be obtained by reducing a polyhalosilane with the above mixture.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:通过向由烷基铝氢化物组成的组合物中添加特定量的烷基铝卤化物,以高产率获得用作合成原料等的标题化合物,而不产生副产物 -Al和细Al粉末,并使用所述混合物还原多卤硅烷。 组成:主要由(A)烷基铝氢化物和含(B)三烷基铝和(C)细铝粉末组成的组合物中加入(D)式AlRnX3-n(R为1-10C烷基; n为 为0,1或1.5; X为卤素)。 组分(D)的量小于将组合物中的全部组分(B)转化为一卤化二烷基铝所需的量的1.8倍,但足以将组合物中组分(B)的残留量降低至<= 10mol 组分(A)的%。 可以通过用上述混合物还原多卤硅烷来获得目标化合物。
    • 10. 发明专利
    • Manufacture of amorphous solar battery
    • 非晶太阳能电池的制造
    • JPS6161474A
    • 1986-03-29
    • JP18277784
    • 1984-09-03
    • Mitsui Toatsu Chem Inc
    • HIAI ATSUHIKOWAKIMURA KAZUOTANAKA MASAOFUKUDA NOBUHIRO
    • H01L31/04H01L31/20
    • H01L31/202Y02E10/50Y02P70/521
    • PURPOSE:To improve secular deterioration by forming a photoactive layer by glow discharge decomposition of a high purity silicon hydride. CONSTITUTION:A transparent substrate having transparent electrodes is mounted in a reaction chamber, and heated at 100-400 deg.C under reduced pressure. High purity silicon hydride and doping gas for imparting the first conductivity are mixed to be fed to the chamber, decomposed by glow discharge or light emission to form the first conductive layer on the electrodes. Then, high purity silicon hydride is decomposed by glow discharge to form a photoactive layer on the first conductive layer. Then, doping gas for imparting the second conductivity and the silicon hydride are fed to the chamber, decomposed by glow discharge or light emission to form the second conductive layer on the photoactive layer. Then, the second electrode is formed to complete a solar battery. The nitrogen and oxygen contents of the silicon are preferably less than 1ppm and less than 0.5ppm.
    • 目的:通过高纯硅氢化物的辉光放电分解形成光活性层来改善长期恶化。 构成:将具有透明电极的透明基板安装在反应室中,并在减压下在100-400℃下加热。 将用于赋予第一导电性的高纯度硅氢化合物和掺杂气体混合进入室,通过辉光放电或发光分解,以在电极上形成第一导电层。 然后,通过辉光放电分解高纯度氢化硅,以在第一导电层上形成光活性层。 然后,将用于赋予第二导电性的掺杂气体和氢化硅供给到室中,通过辉光放电或发光分解,以在光敏层上形成第二导电层。 然后,形成第二电极以完成太阳能电池。 硅的氮和氧含量优选小于1ppm且小于0.5ppm。