CN1133900A - 改善含碳和氧的氮化钛层质量的方法 - Google Patents

改善含碳和氧的氮化钛层质量的方法 Download PDF

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CN1133900A
CN1133900A CN96101302A CN96101302A CN1133900A CN 1133900 A CN1133900 A CN 1133900A CN 96101302 A CN96101302 A CN 96101302A CN 96101302 A CN96101302 A CN 96101302A CN 1133900 A CN1133900 A CN 1133900A
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tin layer
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金鼎泰
黄成辅
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SK Hynix Inc
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • 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
    • C23C16/22—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 inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
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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
    • C23C16/56—After-treatment

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Abstract

一种制备氮化钛(TiN)层的方法，包括的步骤为：用原材料形成TiN层；将TiN层置于氢气和氮气的等离子体中。本发明通过消除TiN层中的杂质和减少TiN层中的气孔率，降低了TiN层的电阻率，从而提高了TiN层的电学稳定性。

Description

改善含碳和氧的氮化 钛层质量的方法
本发明涉及一种改善氮化钛(TiN)层质量的方法，TiN层通常用作钨的粘结层和敷铝过程中的扩散阻挡层，特别是涉及一种去除存在于TiN层中的碳和氧原子的方法。
通常，在半导体制造工艺中，TiN层广泛地用作扩散阻挡层和粘结层。制备TiN层的方法一般有两种，一种是物理气相沉积技术(以下简称PVD法)，另一种是化学气相沉积技术(以下简称CVD法)。然而，人们通常采用CVD法来形成TiN层，因为该方法具有优良的台阶覆盖效果。
TiN层是通过热解诸如四二甲胺基钛(TDMAT)和四二乙胺基钛(TDEAT)等原材料得到的，所沉积的TiN层为多孔结构。
但是，由于采用热解方法得到的TiN层含有碳化物和氧化物，因此TiN层具有104μohm-cm或者更大的电阻率。同时，由于其多孔性，当TiN层暴露于空气中时，TiN层会吸收水份和氧气。在暴露约24小时的条件下，TiN层的电阻率是未经暴露的TiN层电阻率的3.5倍。TiN层的质量因此而恶化。
本发明的目的是提供一种采用等离子气体消除暴露于空气中的TiN层中的杂质，从而降低其电阻率的方法。
根据本发明的一个方面，提供一种制备TiN层的方法，其包括的步骤为：以原材料形成TiN层；将TiN层暴露于氢和氮等离子气体中。
根据本发明的另一个方面，提供一种制备TiN层的方法，其包括的步骤为：以原材料形成TiN层；将TiN层暴露于氢等离子气体中。
下文将描述本发明的一个实施例。
首先，采用CVD方法，通过热解TDMAT和TDEAT沉积TiN层。然后，利用氮气和氢气对TiN层进行初次等离子处理。也就是说，TiN层暴露于氮气和氢气中。
在优选实施例中，初次等离子处理的条件如下：
1)氮气量：100-500标准立方厘米
2)氢气量：100-500标准立方厘米
3)温度：200-500℃
4)压力：0.5-5乇
5)射频(RF)功率：200-700瓦
6)处理时间：10-60秒
对于TiN层的初次等离子处理是在合成TiN层的工作室中或者紧随TiN层暴露于空气中而放入另一工作室中完成的，没有时间上的延迟。
对TiN层进行初次处理后，采用氮气进行第二次等离子处理。
在优选实施例中，第二次等离子处理的条件如下：
1)氮气量：100-500标准立方厘米
3)温度：200-500℃
4)压力：0.5-5乇
5)射频(RF)功率：200-700瓦
6)处理时间：10-60秒
在初次等离子处理中，激活的氢离子渗透进入TiN层，使TiN层中的-C≡N，＝C＝N-和＝C＝O根的键断裂，从而与分裂出来的碳和氧原子发生化合。另一方面，由化合形成的副产物包括CH4和H2O，这些副产物将逸出TiN层。
此外，被激发的氮离子阻止了TiN层对存在于工作室中的氧离子的吸收，并占据逸出的CH4和H2O所形成的空位。
在进行了初次等离子处理的TiN层上再进行第二次等离子处理，使氮原子最大限度地占据TiN层。
等离子处理的结果使钛和氮相结合。因此，经过等离子处理的TiN层的密度要高于未经过等离处理的TiN层，并且能够获得具有较低的电阻率的TiN层。
表1描述了TiN层的电阻率随其形成后暴露于空气的时间的变化。
表(1)TiN层的电阻率
暴露于空气的时间            电阻率(μohm-cm)
   未经等离子处理 经过等离子处理
   0小时     19706     2714
   22小时     70044     3922
   47小时     93376     4249
   73小时     112009     4444
初次等离子处理：           第二次等离子处理：
1)温度：450℃               1)温度：450℃
2)压力：2乇                 2)压力：2乇
3)射频功率：350瓦           3)射频功率：350瓦
4)氢气：200标准立方厘米     4)氮气：300标准立方厘米
5)氮气：300标准立方厘米     5)时间：30秒
6)时间：30秒
在表1中，第二次等离子处理除了只采用300标准立方厘米的氮气等离子体外，与初次等离子处理的条件相同。
从表1中可以看出TiN层的电阻率有相当显著的下降。
此外，表2列出了TiN层的应力变化，表3列出了TiN层中氧原子和碳原子的减少情况。
表(2)TiN层的应力情况
    未经等离子处理     经过等离子处理
延迟时间   0小时         24小时   0小时            24小时
应力(达因/平方厘米) -9.00E+08     -1.30E+09 -6.70E+09        -7.70E+09
应力变化比率(％)           44％             15％
表(3)TiN层的成份
 未经等离子处理(原子百分数)   经过等离子处理(原子百分数)
 Ti       37       45
 C       29       18
 N       21       27
 O       13       10
下文将描述本发明的另一实施例。
对通过热解TDMAT和TDEAT沉积而成的TiN层进行只包含氮气和氢气中的一种等离子气体的等离子处理。在此，所有处理条件与上文所述实施例相同。
当然，根据TiN层的特点，可以只采用两步等离子处理中的一步。
如上所述，本发明通过消除TiN层中的杂质和减少TiN层中的孔隙，获得了降低TiN层的电阻率的效果。因此，本发明可以提高TiN层的电学稳定性。
虽然为了说明的目的公开了本发明的优选实施例，但是，本专业技术领域的人员应当理解，在不偏离本发明权利要求书的范围和精神的前提下，可以作出各种改进、添加和替代。

Claims (16)

1、一种制备氮化钛(TiN)层的方法，包括以下步骤：
用原材料形成TiN层；
将该TiN层暴露于氢气和氮气的等离子体中。
2、根据权利要求1所述的方法，其中，TiN层的暴露步骤是在温度为200～500℃，压力为0.5～5乇，射频功率为200～700瓦的工作室中进行的。
3、根据权利要求2所述的方法，其中，氢和氮等离子气体的量分别为100-500标准立方厘米。
4、根据权利要求2所述的方法，其中，TiN层的暴露步骤持续10～60秒。
5、根据权利要求1所述的方法，其中，TiN层的暴露步骤还包括将其再暴露于氮等离子气体中的步骤。
6、根据权利要求5所述的方法，其中，将TiN层再暴露于氮等离子气体中的步骤是在温度为200～500℃，压力为0.5～5乇，射频功率为200～700瓦的工作室中进行的。
7、根据权利要求5所述的方法，其中，再暴露步骤中的氮等离子气体的量为100-500标准立方厘米。
8、根据权利要求5所述的方法，其中，再暴露TiN层的步骤持续10～60秒。
9、一种制备TiN层的方法，包括以下步骤：
用原材料形成TiN层；
将TiN层暴露于氢气等离子体中。
10、根据权利要求9所述的方法，其中，将TiN层暴露的步骤是在温度为200～500℃，压力为0.5～5乇，射频功率为200～700瓦的工作室中进行的。
11、根据权利要求10所述的方法，其中，氢气等离子体的量为100-500标准立方厘米。
12、根据权利要求10所述的方法，其中，暴露TiN层的步骤持续10～60秒。
13、根据权利要求9所述的方法，其中，暴露TiN层的步骤还包括将该TiN层再暴露于氮气等离子体中的步骤。
14、根据权利要求13所述的方法，其中，将TiN层再暴露于氮气等离子体中的步骤是在温度为200～500℃，压力为0.5～5乇，射频功率为200～700瓦的工作室中进行的。
15、根据权利要求13所述的方法，其中，再暴露步骤中的氮气等离子体的量为100-500标准立方厘米。
16、根据权利要求13所述的方法，其中，再暴露TiN层的步骤持续10～60秒。
CN96101302A 1995-03-28 1996-01-19 制备氮化钛层的方法 Expired - Fee Related CN1057799C (zh)

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CN101734920B (zh) * 2009-12-04 2012-07-04 西安交通大学 一种氮化钛多孔陶瓷及其制备方法
CN102719691A (zh) * 2012-02-21 2012-10-10 山东科技大学 一种具有TiN涂层的多孔膜及其制备方法
CN107615888A (zh) * 2014-12-05 2018-01-19 北美Agc平板玻璃公司 利用宏粒子减少涂层的等离子体源和将等离子体源用于沉积薄膜涂层和表面改性的方法
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CN107615888B (zh) * 2014-12-05 2022-01-04 北美Agc平板玻璃公司 利用宏粒子减少涂层的等离子体源和将等离子体源用于沉积薄膜涂层和表面改性的方法
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US6086960A (en) 2000-07-11
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