CN101135416A - 高流动性GaCl3的输送 - Google Patents

高流动性GaCl3的输送 Download PDF

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CN101135416A
CN101135416A CNA2007101379744A CN200710137974A CN101135416A CN 101135416 A CN101135416 A CN 101135416A CN A2007101379744 A CNA2007101379744 A CN A2007101379744A CN 200710137974 A CN200710137974 A CN 200710137974A CN 101135416 A CN101135416 A CN 101135416A
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carrier gas
gallium trichloride
gallium
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hastelloy
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T·A·斯泰德尔
C·M·伯特彻
R·D·克拉克
L·A·塞尼卡尔
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Air Products and Chemicals Inc
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Abstract

本发明是用于将高纯度气相三氯化镓输送到氮化镓反应器的装置，其包括：在升高的压力下的载气源；能从载气除去水分的净化器；能将载气加热到至少80℃温度的加热器；容器，具有三氯化镓供应，用于载气的阀门控制的进口，其具有浸渍管，该浸渍管具有低于三氯化镓水平面的出口，用于除去载气和夹带的三氯化镓的阀门控制的出口；能加热容器足以使三氯化镓熔融的加热器；与阀门控制的出口相连接的输送管线，从而输送夹带的三氯化镓至氮化镓的反应区。也描述了用于上述装置的方法。

Description

高流动性GaCl3的输送
相关申请的交叉参考
本发明申请要求享受于2006年6月9日申请的US临时专利申请系列号60/812560的权益。
发明背景
电子制造业对诸如含镓膜的化合物半导体具有强烈的兴趣。以前，含镓化合物已通过使用三甲基镓而得到合成。那种合成昂贵且慢。
合成含镓化合物的一个缺点是用于镓源例如室温下固态的三氯化镓(GaCl3)的输送系统。由于GaCl3在其固态时的低蒸气压，用于固态前体的传统蒸气输送系统不能提供GaCl3的高流量和高纯度输送。
由于它们的低温度容量，以及在更高的温度下加速的氯的化学性质——高腐蚀性，可输送如此高流动速率的现有的液态蒸气输送系统不适合熔融的(大于80℃)GaCl3。
由于大多数固态前体的低蒸气压，现有的固态化学气相输送系统仅为较低的流动速率而存在。Air Products and Chemicals Inc.，Allentown，PA，USA已研发出在美国专利申请公开No.2005-0039794A1，10/902778中说明的Schumacher牌产品一固体源蒸发器。
另一种相关的液相气相输送系统是由Air Products and Chemicals Inc.，Allentown，PA，USA提供的Gasguard BSGS三氯硅烷起泡器模式(大约1999年3月)。
通过可使得用于电子应用的含镓化合物得以经济且高纯度的合成的本发明的三氯化镓容器和输送系统，现有技术中容器和输送系统的缺陷被克服。
发明概述
本发明是用于将气相的高纯三氯化镓传输到用于生产含镓化合物的反应器的装置，其包括：在高于大气压的升高的压力下的惰性载气源；能从载气除去水分下降至不超过10份/十亿(“ppb”)、优选为5ppb的净化器；能将载气加热到至少80℃、优选为110℃温度的加热器；具有耐腐蚀内表面的容器，其具有三氯化镓供应，用于载气的阀门控制的入口，其形成了具有低于三氯化镓水平面的出口的浸渍管，阀门控制的出口，用于除去载气和在载气中夹带的三氯化镓；能加热容器足以使三氯化镓熔融的加热器；与阀门控制出口相连接的输送管线，以运送载气和夹带的三氯化镓至用于将三氯化镓转变为含镓化合物的反应区。
本发明也是将气相三氯化镓输送至反应区从而合成含镓化合物的方法，包括：在高于大气压的压力下提供选自氢气、氮气、氦气、氩气及它们的混合物的载气；使载气流过可选择性除去水分到不大于10ppb、优选5ppb的净化介质，以净化载气；将载气加热到至少80℃、优选地110℃的温度；将载气注入熔融三氯化镓浴中，从而在载气中夹带三氯化镓；从容器中除去载气和夹带的三氯化镓，在至少80℃、优选110℃的温度下运送载气和夹带的三氯化镓至反应区，从而合成含镓膜。
附图的简要说明
图1是本发明的一个实施方案为了合成含镓氮化物而以高纯度和高流动速率输送GaCl3的示意图；
图2是各种金属合金暴露于三氯化镓以及随后用水冲洗的侵蚀副产物总量的曲线图。
发明详述
本发明的装置和方法在外延反应器中、使用高蒸气压外延(HVPE)、通过将高流量和高纯度GaCl3蒸气输送到上述反应器中，确保进行镓膜沉积的化学气相沉积(CVD)。
由于固态GaCl3的低蒸气压，用于固态前体的传统气相输送系统不被提供用于高流量和高纯度GaCl3的输送。
由于它们的低温度容量，以及在更高的温度下加速的氯的化学性质——高腐蚀性，可输送如此高流动速率的现有的液相气相输送系统不适合熔融的(大于80℃)GaCl3。
如下描述本发明。GaCl3固态前体被放置在316LSS起泡容器中，在其中它被加热高于它的78℃熔点。在此温度以及以上，它是液态的并可被以低流动速率起泡。
从其熔点(78℃)到130℃的额外加热，增加了液态GaCl3的蒸气压(130℃下GaCl3的蒸气压为90Torr)，足以通过起泡以高流动速率(300至400gr/小时)输送。在那些更高的温度下，5至15升/分钟的载气流动速率将得到所需的高质量流动速率，但是所述的流动速率也要低至足以避免液体的湍流，液体的湍流可引发液体以大滴气溶胶的形式从容器出口喷出。当起泡时，只接受饱和蒸气以维持一致的质量传递并且避免通常由气溶胶滴引起的颗粒问题。
本发明方法使用经净化的载气(H2、Ar、He或N2)来使GaCl3起泡。超高纯度(UHP)净化器除去水分至低于十份/十亿(ppb)、优选为五份/十亿，从而防止水分与氯(在GaCl3中)反应生成HCl。
从载气中的除去水分可控制HCl侵蚀金属起泡器的湿润表面，这可提供金属杂质到GaCl3前体中而引起侵蚀缺陷。金属杂质会干扰含镓膜的外延晶体生长。
HCl在高温下增长的侵蚀速率已导致本发明的另一可选特征的加入。含氟聚合物、氟化乙烯-丙烯(“FEP”)、聚四氟乙烯(“ETFE”)或PFA(聚四氟乙烯的共聚物或衍生物，在下文中共同地为聚四氟乙烯)的保护涂层可被模塑到上述金属或合金即不锈钢(SS)起泡器内侧的湿润表面上，从而更好防止由SS湿润表面产生的金属杂质。假如意外地引入了水分，上述涂层也可阻止对于金属或合金容器的腐蚀。
容器、阀、管道系统和零件优选地为电解抛光的316L不锈钢(“SS”)。316L不锈钢SS阀优选使用特殊的PFA座，从而支持高温操作并抵抗氯侵蚀。这些元件还可以是Hastelloy，例如Hastelloy B-2合金、Hastelloy B-3合金、例如Hastelloy C-22合金、Nickel(镍)或Monel(蒙乃尔高强度耐蚀镍铜合金)。HastelloyB-3合金具有的组成以重量％计为：Ni-65％、Mo-28.5％、Cr-1.5％、Fe-1.5％、Co-3％、W-3％、Mn-3％、Al-0.5％、Ti-0.2％、Si-0.1％和C-0.01％。Hastelloy C-22合金具有的组成以重量％计为：Ni-56％、Mo-13％、Cr-22％、Fe-3％、Co-2.5％、W-3％、Mn-0.5％、V-0.35％、Si-0.08％和C-0.01％。可选地，涂覆有氧化硅(“硅石”)的金属可被用于减小侵蚀。硅石可以是无定形硅石，例如得自于Restek ofBellefonte，PA，USA的Siltek。无定形硅石涂层优选被施涂到316L电解抛光的不锈钢Hastelloy B-2、Hastelloy B-3或Hastelloy C-22。另一硅耐蚀涂层是熔融硅石，被再施涂到诸如316L SS的金属上。表1显示了相关的耐腐蚀合金的组成。
表1
  元素 Elgiloy 316LSS Nicke1200 HastelloyC-22 HastelloyB-2 HastelloyB-3
  ％   ％   ％   ％   ％   ％
  Cr   19-21   16-18   22   最大1   1.5
  Co   39-41   -   最大2.5   最大1   最大3
  Cu   -   -   最大0.25   最大0.5   最大0.5   最大0.2
  Fe   16   bal(～66％)   最大0.40   3   最大2   1.5
  Mn   1.5-2.5   最大2.0   最大0.35   最大0.5   最大1   最大3
  Mo   6-8   2.0～3.0   13   28   28.5
  Ni   14-16   10.0～14.0   最小99.0   56   69   65
  Si   -   最大0.75   最大0.35   最大0.08   最大0.1   最大0.1
  V   -   -   最大0.35
  W   -   -   3   最大3
  碳   最大0.15   最大0.03   最大0.15   最大0.01   最大0.01   最 大0.01
  Be   最大0.1
  Nb
  Ti   最大0.2
  Al   最大0.5
  S   最大0.01
  P
对构成容器、进口、出口、阀和输送管线的材料的各种合金进行了试验：将所述合金暴露于三氯化镓。所得结果列于下面的表2中，其显示Hastelloy C-22表现为最低的可测量的侵蚀。如下方式收集数据：比较与三氯化镓接触前后的合金样片(样品)重量，不但分析暴露于样片的三氯化镓、而且分析在暴露于三氯化镓之后与样片相接触的清洗水。而HastelloyB-2和HastelloyB-3合金产生最少的挥发性侵蚀副产物，因此被预期可制造具有较少金属性杂质的镓膜。所有副产品的比较示于图2中，其为下述副产品的组合：在与一定合金样片接触后在气相三氯化镓中发现的侵蚀副产物，以及在所述样片暴露于三氯化镓后、在与一定合金样片相接触的清洗水中发现的侵蚀副产物。
表2
通过重量和金属分析的合金侵蚀速率对比
  评估基于：   样片重量变化   提取的金属**
  分级   说明   avg mil/yr   avg mil/yr
  1   C-22   0.028   .026**
  2   B-2   0.044   0.028*
  3   Inc-686   0.054   0.033*
  4   Inc-600   0.074   0.050*
  5   316SS   0.065   .060**
  6   镍   0.106   .086**
  7   Elgiloy   0.217   .183**
表3
相关金属氯化物挥发物
  金属   金属氯化物   BP-℃
  铬   CrCl2CrCl3CrO2Cl2   947(s)1300117
  钴   CoCl2   1087
  铜   CuClCuCl2   1212d>300
  铁   FeCl2FeCl3   1024315
  钼   MoCl2MoCl3MoCl4MoCl5MoCl6   d530(mp 1037)407264254(s)
  镍   NiCl2   970(s)
  钨   WCl2WCl4WCl5WCl6WCl4OWCl2O2   d 589d 498288341220260(s)
  锌   ZnCl2   732
起泡器被提供有可选的模塑的PFA内衬，用于可能需要更多的保护以防止金属污染的应用。在这种情况下，所有的阀应当由316LSS转换成全部的全氟聚合物的阀，诸如Telflon PFA(本体和座)阀。
将参考附图进一步描述本发明。在高于大气压的升高的压力下，在载气供应10中提供包括氩气、氦气、氢气、氮气或它们的混合物的高纯度惰性气体。载气以5至15升/分钟的流动速率经过阀12、净化器14和过滤器16被分配，净化器14除去任何水分至低于10ppb、优选5ppb，过滤器16除去颗粒、特别是可能在净化器14中无意中产生的颗粒。载气如果足够纯则可流经任何净化器或过滤器，可选地可通过流量控制器18来测量和计量载气流量。
载气通过管线20被输送到包含三氯化镓容器26的绝热壳24中。载气管线被构造通过一个或多个正弦弯曲22，从而形成可分开加热或如附图所示的热交换表面，从用于容器26的加热器40带走热量。
被加热的载气经过阀36被输送，然后经过作为容器26的装阀门的进口的浸渍管32进入容器26中。浸渍管的出口在熔融三氯化镓28的表面下，通过可环绕容器26的加热器40加热另外的室温固体至高于三氯化镓的78℃熔点，三氯化镓被保持为液态。
容器26也可称为“起泡器”，因为从浸渍管出口32分配的载气鼓泡上升通过熔融液态三氯化镓从而在气相中夹带三氯化镓，以通过由阀38控制的装阀门的出口34除去。加热器40受传统的加热控制42控制。
经三氯化镓饱和的载气从容器26中被除去至输送管线44中，输送管线44是共轴管线，具有运送三氯化镓的内管线46，外管线44与内管线46一起形成环状空间48，环状空间48允许受热的气氛(优选为惰性的氮气)占据所述环形空间并维持升高温度的载气和三氯化镓，其从容器26通过阀50分配到含镓化合物反应器52以在靶54上形成含镓化合物产品。
所述的装置和方法使得三氯化镓可在110℃至140℃下、以300至400克/小时的流动速率被输送到在反应器52中的含镓化合物反应区，这是经济的生产高纯度含镓化合物所希望的。
已结合数个示例性的实施方案描述了本发明，但本发明的全部范围将由下述的权利要求所确定。

Claims (23)

1.一种装置，用于将高纯度气相三氯化镓输送到用于生产含镓产品的反应器，其包括：
在高于大气压的升高的压力下的惰性载气源；
能将载气加热到至少80℃温度的加热器；
具有耐腐蚀内表面的容器，其具有三氯化镓供应，用于载气的阀门控制的进口，其形成具有低于三氯化镓水平面的出口的浸渍管，和用于除去所述载气和在载气中夹带的三氯化镓的阀门控制的出口；
能加热所述容器足以使三氯化镓熔融的加热器；
与阀门控制的出口相连接的输送管线，用于运送所述载气和夹带的三氯化镓至反应区，所述反应区用于将三氯化镓转变为含镓产品。
2.如权利要求1所述的装置，其包括能从所述载气中除去水分下降至不多于10份/十亿的净化器。
3.如权利要求1所述的装置，其中能加热所述载气的所述加热器与能加热所述容器的所述加热器是一个加热器。
4.如权利要求1所述的装置，其中所述载气源包括质量流量控制器。
5.如权利要求2所述的装置，其中所述载气源具有在所述净化器下游的过滤器。
6.如权利要求1所述的装置，其中所述容器位于绝热外壳内。
7.如权利要求1所述的装置，其中所述载气源包括载气管线，其被构造成正弦弯曲，从而提供足够的热交换表面，以加热紧邻能加热所述载气的所述加热器的所述载气。
8.如权利要求1所述的装置，其中所述输送管线是共轴管线，具有运送所述载气和夹带的三氯化镓的内部管线，和外部共轴管线，以提供含有加热介质的环形空间。
9.如权利要求1所述的装置，其中所述容器由选自不锈钢、Hastelloy、Hastelloy B-2、Hastelloy B-3、Hastelloy C-22、镍、Monel、Inconel 686或它们的混合物的金属构成。
10.如权利要求1所述的装置，其中所述输送管线由选自不锈钢、Hastelloy、Hastelloy B-2、Hastelloy B-3、Hastelloy C-22、镍、Monel、Inconel 686和它们的混合物的金属构成。
11.如权利要求1所述的装置，其中所述装阀门的进口、装阀门的出口和该进口和出口中的阀由选自不锈钢、Hastelloy、Hastelloy B-2、Hastelloy B-3、Hastelloy C-22、镍、Monel、Inconel 686和它们的混合物的金属构成。
12.如权利要求11所述的装置，其中所述阀具有含氟聚合物底座。
13.如权利要求1所述的装置，其中所述容器具有含氟聚合物的内衬。
14.如权利要求1所述的装置，其中所述容器和所述输送管线具有与三氯化镓相接触的内表面，那些表面具有金属氯化物的钝化层。
15.如权利要求11所述的装置，其中所述装阀门的进口、装阀门的出口和在所述进口和出口中的所述阀具有与三氯化镓相接触的内表面，那些表面具有金属氯化物的钝化层。
16.如权利要求1所述的装置，其中所述容器和所述输送管线具有与三氯化镓相接触的内表面，那些表面具有含硅化合物的钝化层。
17.如权利要求11所述的装置，其中所述装阀门的进口、装阀门的出口和在所述进口和出口中的所述阀具有与三氯化镓相接触的内表面，那些表面具有含硅化合物的钝化层。
18.一种将气相三氯化镓输送至用于合成含镓产品的反应区的方法，其包括：
在高于大气压的压力下提供选自氢气、氮气、氦气、氩气及它们的混合物的载气；
将所述载气加热到至少80℃的温度；
将所述载气注入在容器中的熔融三氯化镓浴中，从而在载气中夹带三氯化镓；
从容器中除去载气和夹带的三氯化镓，在至少80℃的温度下通过输送管线输送所述载气和夹带的三氯化镓至合成含镓产品的反应区。
19.如权利要求18所述的方法，其包括使所述载气通过选择性除去水分到不大于10份/十亿的净化介质从而净化所述载气的步骤。
20.如权利要求18所述的方法，其中所述载气以5-15升/分钟的速率流动。
21.如权利要求18所述的方法，其中三氯化镓以300-400克/小时的速率被输送至反应区。
22.如权利要求18所述的方法，其中在容器中的三氯化镓被加热至110℃至140℃的温度。
23.如权利要求18所述的方法，其中所述容器和所述输送管线具有与三氯化镓相接触的内表面，在输送夹带的三氯化镓之前通过将氯化气体流经所述容器和输送管线将那些表面钝化。
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EP1865091A2 (en) 2007-12-12
TW200804617A (en) 2008-01-16
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