CN1044010C - 使用涂敷热解氮化硼的石墨舟的金属电阻加热法 - Google Patents

使用涂敷热解氮化硼的石墨舟的金属电阻加热法 Download PDF

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CN1044010C
CN1044010C CN93107926A CN93107926A CN1044010C CN 1044010 C CN1044010 C CN 1044010C CN 93107926 A CN93107926 A CN 93107926A CN 93107926 A CN93107926 A CN 93107926A CN 1044010 C CN1044010 C CN 1044010C
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metal
boron nitride
graphite boat
graphite
resistance heating
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CN1097222A (zh
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J·M·莫里斯
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General Electric Co
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Advanced Ceramics Corp
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Priority to EP93303212A priority patent/EP0621351B1/en
Priority to JP5119228A priority patent/JP2665873B2/ja
Priority to DE69325571T priority patent/DE69325571T2/de
Application filed by Advanced Ceramics Corp filed Critical Advanced Ceramics Corp
Priority to CN93107926A priority patent/CN1044010C/zh
Publication of CN1097222A publication Critical patent/CN1097222A/zh
Priority to HK98115251A priority patent/HK1014036A1/xx
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/0011—Heating features
    • B01D1/0017—Use of electrical or wave energy
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
    • C04B41/5062—Borides, Nitrides or Silicides
    • C04B41/5064—Boron nitride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/87—Ceramics
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/246—Replenishment of source material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/26—Vacuum evaporation by resistance or inductive heating of the source

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

使用具有石墨体和热解氮化硼镀膜的石墨容器的电阻加热法，其中预定重量的金属装入料被存放在镀膜上面而容器则通过使用可变电功率源来加热以使金属装入料在小于两分钟的短时间间隔内充分蒸发，同时控制热循环以提供在施加功率的每一循环中的冷却阶段，同时根据以半连续方式完成的每一加热周期放进新的金属装入料。

Description

使用涂敷热解氮化硼的石墨舟的金属电阻加热法
本发明涉及金属蒸发，更具体地说，涉及使用具热解氮化硼镀膜的石墨容器的金属电阻加热的改进方法。
例如铝、铜、铬、锌和锡等许多金属通过真空淀积法被涂到各种衬底，例如金属、玻璃和塑料上，在该淀积过程中借助于电阻加热使容器发热，以便使送入的与容器接触的金属蒸发。这种容器(通常称为“舟”)以串联电路的方式被接到电路中，使得电流直接流过该舟，此舟又加热与它接触的金属直到该金属蒸发。该金属是在供产品上涂料的真空环境中被蒸发，该产品可以个别地导入真空室或连续不断地送入和通过该室。离散性产品可包括电视显像管、汽车前灯、玩具或诸如此类。
目前，大多数电阻加热容器是由二硼化钛和单独的或与氮化铝结合的氮化硼的金属间陶瓷复合物组成。该复合物的使用寿命很短并需要连续调整的电源。此外，在使用期间上述加热器的电阻特性是不稳定的，因为陶瓷复合物的金属元件是导电体，它构成电路的组成部分。结果金属蒸发是不均匀的，导致不均匀的金属淀积。
现已提出将涂有热解氮化硼的石墨容器用作由金属间陶瓷复合物组成的电阻加热器的替换物。热解氮化硼镀膜是用作容器中的已熔金属与通过石墨体的电流通道的电气绝缘体并把更多的均匀热供给该金属。而且已发现，已熔金属在仅仅短时间间隔之后将穿过热解氮化硼镀膜的镀层表面并直接渗入有孔的石墨体。热循环的变化使氮化硼镀膜在很短的使用时间间隔之内破裂。这破坏了石墨用作金属蒸发器的实用性。增加热解氮化硼镀膜的厚度能延迟，但不会有效地防止穿过氮化硼镀膜的泄漏。
按照本发明已发现，涂有氮化硼的石墨容器可在以下情况下借助热传导用于蒸发与它接触的金属并将提供延长的使用期限：即，被蒸发的金属是以半连续方式加以淀积，而与此同时，改变输入到容器的功率以提供受控的加热循环，在该循环中，输入功率是在足以使金属装入料充分蒸发的一定时间周期内(最好在少于两分钟以内才被施加，并且在重新放进新的金属装入料之前提供冷却阶段。
电阻加热法是按照本发明使用含石墨体和热解氮化硼镀膜的石墨容器来实现的，该方法包括以下步骤：把预定重量的金属装入料放进所述容器遍及所述氮化硼镀膜；把电功率如此施加于所述容器使电流直接流过石墨体从而使金属装入料在少于两分钟的有限时间间隔之内充分蒸发；改变加到所述容器的电功率以控制横过所述氮化硼镀膜的热循环和在施加功率的每一周期中设置冷却阶段并根据每一热循环的完成以半连续方式把新的金属装入料放进所述容器中。
当结合附图阅读时，本发明的其他优点从以下详细描述中变得明白易懂，其中：
图1是按照本发明使用的具有热解氮化硼镀膜的石墨金属蒸发器的透视图；
图2是沿图1的直线2-2取得的断面图；及
图3是在实践本发明期间通过图1的蒸发器的电流流动型式曲线图；
如图1所示，电阻加热器10包括带有热解氮化硼镀膜14的石墨体12，镀膜14覆盖石墨体12的某一给定面积，凹部15就是在该面积内形成。石墨体12是一个高强度石墨的机械体。凹部15可以是任何所需形状或几何尺寸，最好像图2所示使成圆面形以及像图1所示使成半球形侧面，以便接收和保存被电阻加热器10所蒸发的金属装入料(图中未示)。金属装入料可由任何从铝、铜、锌和锡组成的那类中选出的金属组成并且可呈一块或多块状态，其总重量最好在6毫克到200毫克之间。
石墨体12最好是属于具有预定横截面积的矩形结构以提供确定的电阻通道，对给定的输入电压来说，该通道将在其内产生最佳热值以便像在下文所讨论的那样在受控的热循环条件下保证金属装入料的完全蒸发。石墨体12必须依适当尺寸制造以便使它能在所需时间间隔之内引起金属装入料蒸发。石墨体12的输入电压、横截面积以及长度将决定热循环时间。为了在少于两分钟之内施加从4到25伏的电压获得金属装入料的充分蒸发，对石墨体12来说，有必要具有大约15mm2和72mm2之间的最大横截面积以及203.2mm(尽管最好小于127mm)的最大长度。具有15mm2横截面和200mm长度的蒸发器大概需要25伏的输入电压而72mm2横截面和75mm长度只需要4伏的输入电压。
通过使氨和卤化硼，例如三氯化硼作为反应剂的气体蒸气通入加热反应器(图中未示)能在石墨体12上形成热解氮化硼涂层。该反应器的温度在低于6664Pa的压力下被提升到高达2300℃的温度以通过化学汽相淀积形成氮化硼镀膜，(如美国专利3152226中所教导的那样，该专利的说明书编入本文中供参考)。热解氮化硼镀膜14必须足够薄以最大限度将热传递到金属装入料使得有可能在所需的少于两分钟的一定时间间隔内完全蒸发同时还必须足够厚以便在延长的使用寿命期间随着恒定的热循环变化保持其结构上的完整性。对热解氮化硼镀膜来说，较好的厚度范围应当在0.254mm和0.508mm之间。
现已证明加热器10的使用寿命比一般的电阻加热器长几个数量级。加热器10是以半连续方式在周期不足两分钟的每一加热循环期间金属装入料充分蒸发的情况下工作的。在每一工作循环中，在与充分蒸发金属装入料所需时间一致的短时间间隔内施加功率，并且在重新加上功率之前包括一个冷却周期。这导致像图3所示的电流流动型式，其中在使金属装入料充分蒸发所需时间周期内电流几乎是恒定的，接着是冷却周期，在该周期中先放置新的金属装入料再重新加上功率。在没有金属穿过氮化硼镀膜14渗入石墨体12的情况下通过这种半连续方式操纵加热器10，热解氮化硼镀膜14只起绝缘阻挡层的作用。

Claims (2)

1．一种使用涂敷热解氮化硼的石墨舟的金属电阻加热方法，该石墨舟装有石墨体，该石墨体具有在15mm2和72mm2之间的最大横截面积、203.2mm的最大长度和厚度在0.254mm和0.508mm之间的热解氮化硼镀膜，其特征在于，所述方法包括以下步骤：把从铝、铜、锌和锡组成的那类金属选出的具有在6毫克和200毫克之间的预定重量的金属装入料存放在所述石墨舟中，用氮化硼镀膜把石墨体和金属装入料分开；把具有恒定电流和4到25伏之间可变电压的电功率施加于所述石墨舟达一个受控短时间间隔之久，在该时间间隔内足以使金属装入料充分蒸发，使电流直接流过所述石墨体；改变施加于所述石墨舟的电功率以控制横过所述镀膜的加热循环，而所述电功率则重复地被中断以提供同时在每次施加输入功率之间基本上没有电流流通的最短的冷却周期，在所述冷却周期内把新的金属装入料放进所述石墨舟中。
2．如权利要求1所定义的电阻加热法，其特征在于，所述受控短时间间隔小于两分钟。
CN93107926A 1991-12-20 1993-07-03 使用涂敷热解氮化硼的石墨舟的金属电阻加热法 Expired - Fee Related CN1044010C (zh)

Priority Applications (6)

Application Number Priority Date Filing Date Title
US07/810,910 US5239612A (en) 1991-12-20 1991-12-20 Method for resistance heating of metal using a pyrolytic boron nitride coated graphite boat
EP93303212A EP0621351B1 (en) 1991-12-20 1993-04-23 Method for evaporating metal using a resistance heated, pyrolytic boron nitrided coated graphite boat
JP5119228A JP2665873B2 (ja) 1991-12-20 1993-04-23 熱分解窒化硼素被覆ボートを使用する金属の抵抗加熱方法
DE69325571T DE69325571T2 (de) 1991-12-20 1993-04-23 Verfahren zur Verdampfung von Metall mittels eines mit pytolytischem Bornitrid überzogenen Graphit-Schiffchens mit Widerstandsheizung
CN93107926A CN1044010C (zh) 1991-12-20 1993-07-03 使用涂敷热解氮化硼的石墨舟的金属电阻加热法
HK98115251A HK1014036A1 (en) 1991-12-20 1998-12-23 Method for evaporating metal using a resistance heated pyrolytic boron nitrided coated graphite boat

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US07/810,910 US5239612A (en) 1991-12-20 1991-12-20 Method for resistance heating of metal using a pyrolytic boron nitride coated graphite boat
EP93303212A EP0621351B1 (en) 1991-12-20 1993-04-23 Method for evaporating metal using a resistance heated, pyrolytic boron nitrided coated graphite boat
JP5119228A JP2665873B2 (ja) 1991-12-20 1993-04-23 熱分解窒化硼素被覆ボートを使用する金属の抵抗加熱方法
CN93107926A CN1044010C (zh) 1991-12-20 1993-07-03 使用涂敷热解氮化硼的石墨舟的金属电阻加热法

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CN1044010C true CN1044010C (zh) 1999-07-07

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US (1) US5239612A (zh)
EP (1) EP0621351B1 (zh)
JP (1) JP2665873B2 (zh)
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DE (1) DE69325571T2 (zh)
HK (1) HK1014036A1 (zh)

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US5239612A (en) 1993-08-24
JP2665873B2 (ja) 1997-10-22
DE69325571T2 (de) 1999-11-18
JPH06306585A (ja) 1994-11-01
HK1014036A1 (en) 1999-09-17
EP0621351A1 (en) 1994-10-26
DE69325571D1 (de) 1999-08-12
CN1097222A (zh) 1995-01-11

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