CN1072735C - 沉积铝薄膜的方法 - Google Patents

沉积铝薄膜的方法 Download PDF

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CN1072735C
CN1072735C CN94193375A CN94193375A CN1072735C CN 1072735 C CN1072735 C CN 1072735C CN 94193375 A CN94193375 A CN 94193375A CN 94193375 A CN94193375 A CN 94193375A CN 1072735 C CN1072735 C CN 1072735C
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A·C·琼斯
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    • 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
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material
    • C23C18/10—Deposition of aluminium only
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C21/00—Alloys based on aluminium
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    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
    • C23C16/20—Deposition of aluminium only
    • 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
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material

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Abstract

一种将高纯度第ⅢA族金属层沉积在基材上的方法，它包括基材与第ⅢA族金属的叔丁基化合物接触，然后使该化合物裂解，在基材上留下沉积的第ⅢA族金属。本发明的方法可用于任何适合的基材，如硅和聚酰亚胺。本发明的方法可用于第ⅢA族金属/硅合金的生长，以及用于使半导体Ⅲ-Ⅴ合金沉积，如AlGaAs、AlInAs和AlSb合金的沉积。

Description

沉积铝薄膜的方法
本发明涉及一种沉积金属薄膜，特别是铝薄膜的方法。
铝薄膜的沉积对于许多应用来说是重要的，如在VLSI技术中硅制设备的金属化、半导体Ⅲ-Ⅴ合金的生长如AlGaAs、AlInAs和AlSb以及介电质的生长如AlN。另外，基于数字纪录介质的混合传感器目前正在开发，它需要铝以微米级沉积在硅上或穿孔刻蚀到硅上。
金属有机化学蒸汽沉积法(MOCVD)是一种有吸引力的薄膜生长技术，其优点是有大面积生长的能力、可准确控制层厚以及良好的保形复盖。所以，已作出了许多努力，旨在研制适合于铝化学蒸汽沉积的前体。
已广泛地研究了挥发性有机铝化合物作为化学蒸汽沉积(CVD)前体，其中包括三甲基铝、二甲基氢化铝以及式AlR3的高碳烷基铝，其中R为正丙基、正丁基和异丁基。但是，常常表明用这些前体生长的铝膜其形态差和纯度低。特别是，在金属有机化合物热解过程中，有机基团的分解产生碳杂质。促使人们研究氢化铝为基础的双三甲基胺铝烷加合物和二甲基乙基胺铝烷加合物，由它们已生长出不含碳的铝和低碳含量的AlGaAs。但是，这些铝烷加合物由于不可预见的气相化学，它在室温贮存过程中可能产生过早的分解，还倾向于释放出氢气，因此有关它们大规模的应用仍值得怀疑。
迄今最成功和最广泛研究的CVD前体是三异丁基铝(TIBA)。详细的表面科学研究表明，在温度低于327℃下，容易的异丁烯的β-氢化物消除产生不含碳的铝膜。但是，在较高的温度下，异丁基可消除β-甲基，产生表面甲基，从而使沉积的铝膜的碳含量显著增加。这就限制了由TIBA的铝沉积的温度范围，从而防碍了它在技术上重要的Al/Si合金生长中的应用，Al/Si合金的生长需要高的基材温度(一般高于400℃)，来使硅前体(一般为SiH4)裂解。
所以，仍需要这样一种铝前体，它可把三烷基铝化合物的稳定性优点与沉积高纯度铝膜的可能性结合起来。类似的第ⅢA族金属化合物也可用于沉积。
现在令人吃惊的发现，三叔丁基铝可用作铝沉积的前体。
因此，本发明提供一种将第ⅢA族金属膜沉积在基材上的方法，它包括使基材与第ⅢA族金属前体接触，然后处理前体使之分解，在基材上留下沉积的第ⅢA族金属，其中前体为第ⅢA族金属的三叔丁基化合物。
本发明还提供一种有第ⅢA族金属层沉积在上的基材，金属层由前体在基材上分解得到，其中前体是第ⅢA族金属的三叔丁基化合物。
对于本发明的方法来说，重要的第ⅢA族金属是铝、镓、铟，其中铝是最重要的。
在本发明一优选方法中，将前体作为蒸汽相送到基材上，并在基材上裂解，在基材上留下金属膜。本发明的方法也可在液相中完成，例如将前体涂在基材上或将基材浸入前体中，然后加热使前体裂解，在基材上留下金属。
在本发明一优选方法中，将基材加热到适当的温度，使前体裂解。150-400℃的温度可能为适合的，显然也可使用比这一范围或高或低的温度。
本发明的方法可用于任何一种适合的基材，如硅或聚酰亚胺。本发明的方法可用于第ⅢA族金属/硅合金的生长，特别是铝硅合金，它需要很高的温度使硅前体特别是SiH4裂解。
本发明的方法可用于使半导体Ⅲ-Ⅴ合金沉积，如AlGaAs、AlInAs和AlSb沉积以及用于介电质生长，如AlN生长。
三叔丁基铝(TTBA)对于用减压MOVPE法或化学束取向生长(Chemical beam epitaxy)((CBE))的低碳AlGaAs的生长也是适合的前体，已表明其中无甲基金属有机前体是必不可少的。
三叔丁基铝可使沉积高纯度铝的温度范围扩大。TTBA可用于用LPCVD法的铝导电薄膜生长的各种应用中。
现在用以下实施例进一步说明本发明。
实施例
用Ann.Chem.719(1968)40中描述的方法合成三叔丁铝，并用质子核磁共振谱(1HNMR)和感应耦合等离子体发射谱(ICP-ES)表征生成的无色液体。
1HNMR(C6D6)ppm:1.3(S,Al-C(CH3)3)
ICP-ES:Al含量(％)测量值13.1，计算值13.6
铝膜在一简单的用辐射基材加热的冷壁水平石英反应器(Electrogas Ltd)中沉积。所用的基材是Si(Ⅲ)单晶片，使用前它经丙酮脱气、在20％HNO3/D1水中洗涤并干燥。不用进一步预处理。TTBA保持在30℃下。在这一温度下它有适合于LPCVD的蒸汽压力(大于1乇)。在基材温度为400℃下其生长速率达1.2米/小时。用tallystep法测量层厚。生长条件的全部数据列入下表1。
          表1用于由TTBA沉积铝的生长条件
池压                              4.56乇
基材                            单晶硅(Ⅲ)
TTBA温度                           30℃
N2载气流速                   1.0-3.0标毫升/分钟
生长温度                             300-400℃
最高生长速率                     1.5米/小时(在400℃下)
最初用在盐酸中溶解的方法表征铝膜，用感应耦合质谱(ICP-MS)分析金属，表明按金属计铝的纯度大于99％。
铝膜在300-400℃范围内由TTBA沉积，为无泽灰色，只有很低的反射率(一般在633纳米处为30％)。这一点可归因于粗糙的表面形态，它常常在用TIBA沉积的薄膜中观察到，除非用TiCl4预处理。
已发现由TTBA制成的铝膜是导电的。
在400℃下在Si(Ⅲ)上生长的薄膜的粘附性也是极好的，在“粘贴带”试验中，当粘贴带从铝膜上剥离开时，铝膜仍保持完好。
三烷基铝前体用于铝沉积使我们关心碳是否进入到沉积的薄膜中，特别是在这一实施例中使用的相当高的基材温度下。但是，俄歇电子能谱分析的结果(如下表2所示)表明，在400℃下用TTBA生长的铝膜中仅有微量的碳和氧存在。
为了进行比较，在上表1所示的相同的条件下，用传统的前体TIBA沉积铝膜。在下表2中列出该层的俄歇分析结果，结果表明其纯度比由TTBA得到的铝层低，含有更多的碳和氧。
用二次离子质谱进一步分析分开的铝膜证实，与用TIBA生长的铝膜相比，用TTBA生长的铝膜的碳含量至少低3倍。
     表2在400℃下用TTBA和TIBA在Si(Ⅲ)
         上生长的铝膜的俄歇电子能谱分析
                  原子组成％
膜前体    Al      C      O
TTBA     98.2    0.7    1.1
TIBA     84.5    3.1    12.4
*用AES和顺序离子轰击结合得到的亚表面数据(2000埃或2000埃以下)
发现用TTBA生长的铝膜中氧的含量低于用TIBA生长的铝膜。这一点可反映出氧被夹带在空间整体和刚性的TTBA分子中的倾向降低。在TTBA生长的膜中氧的存在可归因于简单的CVD反应器的应用，不可能从这种反应器中严格排除所有微量氧。

Claims (9)

1．一种用化学蒸汽沉积在基材上沉积铝薄膜的方法，它包括以下步骤：基材与铝前体接触，以及处理前体使之分解，留下沉积在基材上的铝，其中前体是三叔丁基铝。
2．根据权利要求1的方法，其中基材被加热到150-400℃范围的温度。
3．根据权利要求1的方法，其中基材是硅或聚酰亚胺。
4．根据权利要求1的方法，其中用也沉积在基材上的硅前体处理铝前体形成铝/硅合金。
5．根据权利要求4的方法，其中硅前体是SiH4。
6．根据权利要求1的方法，其中通过用也沉积在基材上的第Ⅴ族前体和第Ⅲ族前体处理铝前体制得铝/第ⅢA族/第Ⅴ族合金。
7．根据权利要求6的方法，其中制得的合金选自AlGaAs、和AlInAs。
8．根据权利要求6的方法，其中铝/第Ⅴ族合金被制备。
9．根据权利要求8的方法，其中铝/第Ⅴ族合金是AlSb。
CN94193375A 1993-07-30 1994-07-29 沉积铝薄膜的方法 Expired - Fee Related CN1072735C (zh)

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JPH09501985A (ja) 1997-02-25
DE69431443D1 (de) 2002-10-31
EP0804631A1 (en) 1997-11-05
KR960704085A (ko) 1996-08-31
CA2168214A1 (en) 1995-02-09
WO1995004168A1 (en) 1995-02-09
CN1130924A (zh) 1996-09-11
DE69431443T2 (de) 2003-05-22
ATE224964T1 (de) 2002-10-15
AU7267494A (en) 1995-02-28
KR100352726B1 (ko) 2002-11-07
AU686207B2 (en) 1998-02-05
US5863836A (en) 1999-01-26
GB9315771D0 (en) 1993-09-15
DE804631T1 (de) 1998-03-05

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