CN104498895A - 一种超薄氮氧化硅膜材料及其制备方法和用途 - Google Patents

一种超薄氮氧化硅膜材料及其制备方法和用途 Download PDF

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CN104498895A
CN104498895A CN201410811923.5A CN201410811923A CN104498895A CN 104498895 A CN104498895 A CN 104498895A CN 201410811923 A CN201410811923 A CN 201410811923A CN 104498895 A CN104498895 A CN 104498895A
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宋志伟
褚卫国
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National Center for Nanosccience and Technology China
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Abstract

一种超薄氮氧化硅膜材料及其制备方法：将衬底置于化学气相沉积设备腔体中，通入NH3、O2气体和含有SiH4的气体作为反应气体，通入载体和保护气体，进行气相沉积，获得氮氧化硅膜材料，其中，所述化学气相沉积设备腔体的工作温度为100-260℃，工作压力为1-4Pa，功率为200-450W；其中，所述气相沉积的时间为15-40s；所述SiH4气体与O2气体的体积比为9-110，所述含有SiH4的气体与NH3气体的体积比为3-11，所述含有SiH4的气体与载体和保护气体的体积比为0.1-1。本发明在四英寸硅基体上制备得到的氮氧化硅膜材料的厚度为6-9nm，薄膜不均匀性低于0.7％。

Description

一种超薄氮氧化硅膜材料及其制备方法和用途
技术领域
本发明属于光学、半导体和微电子器件技术领域，具体涉及一种氮氧化硅膜材料及其制备方法和用途。
背景技术
薄膜是一种特殊的物质形态，由于其在厚度这一特定方向上尺寸很小，只是微观可测的量，而且在厚度方向上由于表面、界面的存在，使物质连续性发生中断，由此使得薄膜材料产生了与块状材料不同的独特性能。光学薄膜是由薄的分层介质构成的，通过界面传播光束的一类光学介质材料，广泛用于光学和光电子技术领域，制造各种光学仪器。光学薄膜技术在理论、设计、计算和工艺方面已形成了完整的体系，一些新型微观结构的功能薄膜被不断开发出来，这些功能薄膜的相继出现，使得光学薄膜技术广泛地渗透到各个新兴的科学研究领域中。
氮氧化硅薄膜是一种良好的耐高温陶瓷材料，具有优异的力学性能、热力学性能、化学稳定性及耐原子氧特性；由于氮氧化硅是二氧化硅和氮化硅的中间相，其光学和电学性能介于两者之间，因而可通过改变化学组成，在一定范围内调控其折光指数(1.46(SiO2)～2.3(SiN1.3))及介电常数(3.9(SiO2)和7.8(SiN1.3))；另外氮氧化硅还可有效地抑制硼、氧、钠等杂质元素扩散。这一系列优良特性吸引研究者们围绕氮氧化硅材料的制备及其在微电子器件、光波导、梯度光学材料等方面的应用开展了大量工作，其中又以氮氧化硅薄膜材料的制备及应用研究最引人关注。
当前在微电子器件、光波导材料等方面主要采用二氧化硅作为介质薄膜。二氧化硅薄膜虽具有低的介电常数、缺陷密度和残余应力，但在阻止氧、钠、硼等杂质元素的扩散方面不如氮化硅；然而氮化硅中Si悬空键的存在及其随氮含量增加而增加的特点会导致薄膜在一定条件下表现出很高的介电常数和拉应力，并且富氮SiNX膜含有很高的正电荷和负电荷缺陷，成为电荷俘获的中心。而氮氧化硅薄膜材料由于兼有氮化硅和二氧化硅的优良特性，很有潜力替代二氧化硅薄膜材料在微电子和光学等方面得到应用。
随着薄膜的应用越来越广泛，薄膜的制备技术也逐渐成为高科技产品加工技术中的重要手段。薄膜的制备方法很多，如气相生长法、液相生长法(或气、液相外延法)、氧化法、扩散与涂布法、电镀法等等，而每一种制膜方法中又可分为若干种方法。等离子体化学气相沉积(PECVD)法由于其灵活性、沉积温度低，重复性好的特点，提供了在不同基体上制备各种薄膜的可能性，成为制备氮氧化硅薄膜最常用的方法之一。
薄膜的均匀性是薄膜制备过程中首先需要解决的关键问题和挑战。薄膜厚度的不均匀性，反映了待镀基片上所沉积的薄膜厚度依基片在真空室里所处位置的变化而变化的情况。膜厚不均匀性包括两个方面：①在同一组镀制过程中处于不同基片位置沉积的薄膜有近似的膜厚分布；②获得的每片薄膜只存在一定范围内的膜厚误差分布。膜厚不均匀性的方面①保证了产业化的镀膜效率，方面②保证了每个成品的性能。因此，膜厚不均匀性是衡量镀膜装置性能和薄膜质量的一项重要指标，直接影响到镀膜器件的可靠性、稳定性，以及产品的一致性。对光学、光电等器件生产的成品率影响很大。
而目前研究薄膜均匀性的较少，尤其是运用在器件中的光学/介质薄膜，对于采用高密度等离子体增强化学气相沉积设备制备氮氧化硅膜材料的方法，操作条件较多，包括温度、压力、功率、时间、通入气体比例等，且相互之间有着密切的相互关系，不是独立的单一变量，因此在本领域探究一种均匀性良好的氮氧化硅制备方法是非常重要的。
发明内容
为了克服现有技术中氮氧化硅薄膜不均匀性较大的缺陷，本发明的目的之一在于提供了一种氮氧化硅膜材料，本发明提供的膜材料具有良好的均匀性，厚度约为8nm，其具有良好的绝缘性、稳定性和机械特性，可以作为绝缘层、保护膜或光学膜，广泛应用于半导体、微波、光电子以及光学器件等领域。
为达上述目的，本发明采用如下技术手段：
一种超薄氮氧化硅膜材料，所述氮氧化硅膜材料的厚度为6-9nm；且在四英寸基底范围内，薄膜不均匀性低于0.7％；
其中，所述不均匀性的计算方法为：薄膜不均匀性＝(最大值-最小值)/(平均值×2)×100％，四英寸基底范围内，所测不同点数不少于10个，优选不少于17个。
其中，所述最大值为氮化硅膜材料测试点厚度的最大值；最小值为氮化硅膜材料测试点厚度的最小值；平均值为氮化硅膜材料测试点厚度的平均值，计算公式为：平均值＝测试点厚度之和/测试点个数。
作为优选，所述超薄氮氧化硅膜材料的组分为SiOxNY，其中0<x<2，0<Y<2。
本发明的目的之二在于提供一种本发明所述的超薄氮氧化硅膜材料的制备方法，包括如下步骤：
将衬底置于化学气相沉积设备腔体中，通入NH3、O2和含有SiH4的气体作为反应气体，通入载体和保护气体，进行气相沉积，获得氮氧化硅膜材料；
其中，所述化学气相沉积设备腔体的工作温度为100-260℃，工作压力为1-4Pa，功率为200-450W；
其中，所述气相沉积的时间为15-40s；所述含有SiH4的气体与O2气体的体积比为9-110，所述含有SiH4的气体与NH3气体的体积比为3-11，所述含有SiH4的气体与载体和保护气体的体积比为0.1-1。其中载气和保护气体为同一种气体。
对于采用化学气相沉积设备制备氮氧化硅膜材料的方法，操作条件较多，包括温度、压力、功率、时间、通入气体比例等，且相互之间有着密切的相互关系，不是独立的单一变量，因此如何寻找一个合适的操作条件，对于本领域技术人员来讲是具有很大难度的。
采用化学气相沉积设备制备氮氧化硅膜材料的操作条件中，通过将化学气相沉积设备腔体的工作温度设置在100-260℃，工作压力设置在1-4Pa，功率设置为200-450W；且控制气相沉积的时间为15-40s；控制通入的含有SiH4的气体与O2气体的体积比为9-110，控制通入的含有SiH4的气体与NH3气体的体积比为3-11，控制通入的含有SiH4的气体与载体和保护气体的体积比为0.1-1，实现了控制厚度为8nm左右的氮氧化硅膜材料薄膜不均匀性低于0.7％的目的。
本发明采用的化学气相沉积设备制备氮氧化硅膜材料的操作条件中，所限定的数值包括任何在所述范围内的数值，例如，化学气相沉积设备腔体的工作温度可以为110℃、157℃、218℃、260℃等，工作压力可以为1.2Pa、1.8Pa、2.2Pa、2.8Pa、3.2Pa、3.9Pa等，功率可以为220W、295W、362W、375W、387W、423W、450W等，气相沉积的时间可以为18s、22s、28s、33s、35s、38s等，通入的含有SiH4的气体与O2气体的体积比可以为10、30、80、102等，通入的含有SiH4的气体与NH3气体的体积比可以为3.5、4.8、9.3、10.5等。
作为优选，所述化学气相沉积设备为高密度等离子体增强化学气相沉积设备；优选抽真空至1×10-4-1×10-6Pa。
作为优选，所述载气和保护气为惰性气体，优选为氖气、氪气、氮气、氩气中的1种或两种的混合。
作为优选，所述气体的纯度大于99％，优选为大于99.99％。
优选地，所述含有SiH4的气体中SiH4占1-10％，氩气占90-99％，优选为SiH4占5％，氩气占95％。但是所述含有SiH4的气体的总体纯度仍应大于99％。
作为优选，所述衬底为P型掺杂单晶硅、N型掺杂单晶硅或金属中的任意1种；任选地在上述衬底上制备一层均匀的金属或非金属薄膜作为实验的衬底。
优选地，所述P型掺杂单晶硅或N型掺杂单晶硅衬底进行如下预处理：用HF酸浸泡后用去离子水清洗，然后干燥。
优选地，所述HF酸的质量浓度为2-10％，例如3％、5％、7％、8.3％、9％等，进一步优选为5％。
优选地，所述用HF酸浸泡的时间为0.5-10min，例如1min、1.4min、3min、5min、7min、8.4min、9min等，进一步优选为3min。
优选地，所述金属衬底进行如下预处理：用丙酮和异丙醇酸分别超声清洗，然后干燥。
优选地，所述超声的时间为2min以上，优选为5min。
作为优选，气相沉积设备腔体的工作温度为230℃，工作压力为2Pa，功率为362W；所述气相沉积的时间为22s；所述含有SiH4的气体与O2气体的体积比为100，所述含有SiH4的气体与NH3气体的体积比为4.7，所述含有SiH4的气体与氩气的体积比为0.33。
作为优选技术方案，本发明所述制备方法包括如下步骤：
(1)将衬底置于高密度等离子体增强化学气相沉积设备腔体中，抽真空使背底真空度为1×10-4-1×10-6Pa，加热衬底到100-260℃；
(2)按1:(9-110)的体积比通入O2气体和含有SiH4的气体作为反应气体，按1:(3-11)的体积比通入含有NH3的气体和SiH4作为反应气体，通入氩气作为载气和保护气体，调整工作气压为1-4Pa，功率为200-450W，进行化学气相沉积15-40s；
(3)在保护性气体的气氛下，降至室温，得到所述的超薄氮氧化硅膜材料。
作为优选，步骤(3)所述的保护性气体为惰性气体；优选为氩气。
本发明的目的之三在于提供本发明所述的超薄氮氧化硅膜材料的用途，所述氮氧化硅膜材料作为绝缘层、保护膜或光学膜，可应用于半导体、微波、光电子以及光学器件等领域。
与现有技术相比，本发明具有如下有益效果：
(1)本发明提供的氮氧化硅膜材料的厚度在8nm左右，且具有良好的均匀性，在四英寸基底范围内，薄膜不均匀性低于0.7％；其较现有磁控溅射法和电子束蒸镀法得到的氮氧化硅膜材料的均匀性有明显提高；
(2)本发明使用的衬底采用P(或N)型掺杂单晶硅、金属或上述衬底上制备一层金属或非金属薄膜，可以在不同材料界面制备具有良好均匀性的，厚度为8nm左右的氮氧化硅膜材料；
(3)本发明提供的具有良好均匀性超薄的硅化合物薄膜材料制备工艺简单易行，具有极大的应用潜力。
附图说明
图1为本发明实施例1性能表征测试点厚度的分布图。
具体实施方式
为便于理解本发明，本发明列举实施例如下。本领域技术人员应该明了，所述实施例仅仅是帮助理解本发明，不应视为对本发明的具体限制。
实施例1
一种氮氧化硅膜材料，通过如下方法制备得到：
(1)以抛光的P型(100)掺杂单晶硅做衬底，并进行如下预处理：首先将所述衬底用5wt％的HF酸浸泡3min，再用去离子水清洗，最后干燥其表面；
(2)将步骤(1)获得的预处理后的衬底放入高密度等离子体增强化学气相沉积设备腔体中，并将沉积室抽真空，使背底真空度在1×10-5Pa左右，并加热衬底到230℃；
(3)以纯度均大于99.99％的含有SiH4的气、NH3气、O2气和Ar2气为气源；其中，含有SiH4的气、O2气、NH3气为反应气体，Ar2气为载气和保护气，供给的Ar2气、O2气、NH3气和含有SiH4的气体气流量分别为：400sccm、1.2sccm、26.8sccm、130.5sccm；控制沉积室的工作气压为2Pa，功率为362W，进行化学气相沉积22s；
(4)在Ar2气气氛下，降温至室温，获得均匀性良好的，厚度为8nm左右的氮氧化硅膜材料；
性能表征：
将获得的SiON膜材料进行光谱椭偏仪(设备型号为SE 850)测试，测试条件为：室温，200～930nm波长范围扫描，选取17个测试点，所述17个测试点的分布为1个中心点，8个半径为r的圆周点，8个半径为2r的圆周点，所述圆周点均匀分布于所在圆周上，其中，r的取值小于基片的最短边长的1/4(图1为测试点的示意图)；测试结果如图1所示；通过计算其不均匀性为0.7％。
实施例2
一种氮氧化硅膜材料，通过如下方法制备得到：
(1)在抛光的P型(100)掺杂单晶硅片上制备200nm厚的Ti膜，并以此做为衬底，并进行如下预处理：首先用丙酮和异丙醇各超声5min，再用去离子水清洗，最后干燥其表面；
(2)将步骤(1)获得的预处理后的衬底放入高密度等离子体增强化学气相沉积设备腔体中，并将沉积室抽真空，使背底真空度在1×10-5Pa左右，并加热衬底到150℃；
(3)以纯度均大于99.99％的含有SiH4的气、NH3气、O2气和Ar2气为气源；其中，含有SiH4的气、O2气、NH3气为反应气体，Ar2气为载气和保护气，供给的Ar2气、O2气、NH3气和含有SiH4的气体气流量分别为：385sccm、4sccm、24sccm、130.5sccm；控制沉积室的工作气压为3Pa，功率为328W，进行化学气相沉积25s；
(4)在Ar2气气氛下，降温至室温，获得均匀性良好的，厚度约为9nm的氮氧化硅膜材料；
将获得的SiON膜材料进行光谱椭偏仪(设备型号为SE 850)测试，测试方法与实施例1的性能表征方法相同；过计算其不均匀性为0.68％。
实施例3
一种氮氧化硅膜材料，通过如下方法制备得到：
(1)以抛光的蓝宝石做衬底，并进行如下预处理：首先将所述衬底用丙酮和异丙醇各超声5min，再用去离子水清洗，最后干燥其表面；
(2)将步骤(1)获得的预处理后的衬底放入高密度等离子体增强化学气相沉积设备腔体中，并将沉积室抽真空，使背底真空度在1×10-6Pa左右，并加热衬底到260℃；
(3)以纯度均大于99.99％的含有SiH4的气、NH3气、O2气和Ar2气为气源；其中，含有SiH4的气、O2气、NH3气为反应气体，Ar2气为载气和保护气，供给的Ar2气、O2气、NH3气和含有SiH4的气体气流量分别为：450sccm、10.5sccm、17.5sccm、130.5sccm；控制沉积室的工作气压为2.5Pa，功率为280W，进行化学气相沉积30s，获得一层厚度为10nm左右的的氮氧化硅薄膜；
(4)在Ar2气气氛下，降温至室温，获得均匀性良好的，厚度为8.5nm左右的氮氧化硅膜材料；
将获得的氮氧化硅膜材料进行光谱椭偏仪(设备型号为SE 850)测试，测试方法与实施例1的性能表征方法相同；通过计算其不均匀性为0.65％。
实施例4
一种氮氧化硅膜材料，通过如下方法制备得到：
(1)以抛光的蓝宝石做衬底，并进行如下预处理：首先将所述衬底用丙酮和异丙醇各超声2min，再用去离子水清洗，最后干燥其表面；
(2)将步骤(1)获得的预处理后的衬底放入高密度等离子体增强化学气相沉积设备腔体中，并将沉积室抽真空，使背底真空度在1×10-6Pa左右，并加热衬底到100℃；
(3)以纯度均大于99.99％的含有SiH4的气、NH3气、O2气和Ar2气为气源；其中，含有SiH4的气、O2气、NH3气为反应气体，Ar2气为载气和保护气，供给的Ar2气、O2气、NH3气和含有SiH4的气体气流量分别为：145sccm、14.5sccm、43.5sccm、130.5sccm；控制沉积室的工作气压为4Pa，功率为200W，进行化学气相沉积15s，获得一层厚度为8nm左右的的氮氧化硅薄膜；
(4)在Ar2气气氛下，降温至室温，获得均匀性良好的，厚度为8nm左右的氮氧化硅膜材料；
将获得的氮氧化硅膜材料进行光谱椭偏仪(设备型号为SE 850)测试，测试方法与实施例1的性能表征方法相同；通过计算其不均匀性为0.62％。
实施例5
一种氮氧化硅膜材料，通过如下方法制备得到：
(1)以抛光的P型(100)掺杂单晶硅做衬底，并进行如下预处理：首先将所述衬底用2wt％的HF酸浸泡10min，再用去离子水清洗，最后干燥其表面；
(2)将步骤(1)获得的预处理后的衬底放入高密度等离子体增强化学气相沉积设备腔体中，并将沉积室抽真空，使背底真空度在1×10-4Pa左右，并加热衬底到150℃；
(3)以纯度均大于99.99％的含有SiH4的气、NH3气、O2气和Ar2气为气源；其中，含有SiH4的气、O2气、NH3气为反应气体，Ar2气为载气和保护气，供给的Ar2气、O2气、NH3气和含有SiH4的气体气流量分别为：1305sccm、2.6sccm、13.1sccm、130.5sccm；控制沉积室的工作气压为1Pa，功率为450W，进行化学气相沉积40s；
(4)在Ar2气气氛下，降温至室温，获得均匀性良好的，厚度为8nm左右的氮氧化硅膜材料；
将获得的氮氧化硅膜材料进行光谱椭偏仪(设备型号为SE 850)测试，测试方法与实施例1的性能表征方法相同；通过计算其不均匀性为0.66％。
申请人声明，本发明通过上述实施例来说明本发明的详细方法，但本发明并不局限于上述详细方法，即不意味着本发明必须依赖上述详细方法才能实施。所属技术领域的技术人员应该明了，对本发明的任何改进，对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等，均落在本发明的保护范围和公开范围之内。

Claims (10)

1.一种超薄氮氧化硅膜材料，其特征在于，所述氮氧化硅膜材料的厚度为6-9nm；且在四英寸基底范围内，薄膜不均匀性低于0.7％；
其中，所述不均匀性的计算方法为：薄膜不均匀性＝(最大值-最小值)/(平均值×2)×100％，四英寸基底范围内，所测不同点数不少于10个，优选不少于17个。
2.根据权利要求1所述的超薄氮氧化硅膜材料，其特征在于，所述超薄氮氧化硅膜材料的组分为SiOxNY，其中0<x<2，0<Y<2。
3.一种权利要求1或2所述的超薄氮氧化硅膜材料的制备方法，包括如下步骤：
将衬底置于化学气相沉积设备腔体中，通入NH3、O2和含有SiH4的气体作为反应气体，通入载体和保护气体，进行气相沉积，获得氮氧化硅膜材料；
其中，所述化学气相沉积设备腔体的工作温度为100-260℃，工作压力为1-4Pa，功率为200-450W；
其中，所述气相沉积的时间为15-40s；所述含有SiH4的气体与O2气体的体积比为9-110，所述含有SiH4的气体与NH3气体的体积比为3-11，所述含有SiH4的气体与载体和保护气体的体积比为0.1-1。
4.根据权利要求3所述的制备方法，其特征在于，所述化学气相沉积设备为高密度等离子体增强化学气相沉积设备；优选抽真空至1×10-4-1×10-6Pa；
优选地，所述载气和保护气为惰性气体，优选为氖气、氪气、氮气、氩气中的1种或两种的混合；
优选地，所述气体的纯度大于99％，优选为大于99.99％；
优选地，所述含有SiH4的气体中SiH4占1-10％，氩气占90-99％，优选为SiH4占5％，氩气占95％。
5.根据权利要求3或4所述的制备方法，其特征在于，所述衬底为P型掺杂单晶硅、N型掺杂单晶硅或金属中的任意1种；任选地在上述衬底上制备金属或非金属薄膜作为实验的衬底。
6.根据权利要求5所述的制备方法，其特征在于，所述P型掺杂单晶硅或N型掺杂单晶硅衬底进行如下预处理：用HF酸浸泡后用去离子水清洗，然后干燥；
优选地，所述HF酸的质量浓度为2-10％，优选为5％。
优选地，所述用HF酸浸泡的时间为0.5-10min，优选为3min。
7.根据权利要求5所述的制备方法，其特征在于，所述金属衬底进行如下预处理：用丙酮和异丙醇酸分别超声清洗，然后干燥；
优选地，所述超声的时间为2min以上，优选为5min。
8.根据权利要求3-7任一项所述的制备方法，其特征在于，化学气相沉积设备腔体的工作温度为230℃，工作压力为2Pa，功率为362W；所述气相沉积的时间为22s；所述含有SiH4的气体与O2气体的体积比为100，所述含有SiH4的气体与NH3气体的体积比为4.7，所述含有SiH4的气体与氩气的体积比为0.33。
9.根据权利要求3所述的制备方法，其特征在于，包括如下步骤：
(1)将衬底置于高密度等离子体增强化学气相沉积设备腔体中，抽真空使背底真空度为1×10-4-1×10-6Pa，加热衬底到100-260℃；
(2)按1:(9-110)的体积比通入O2气体和含有SiH4的作为反应气体，按1:(3-11)的体积比通入NH3气体和含有SiH4的作为反应气体，通入氩气作为载气和保护气体，调整工作气压为1-4Pa，功率为200-450W，进行化学气相沉积15-40s；
(3)在保护性气体的气氛下，降至室温，得到所述的超薄氮氧化硅膜材料；
优选地，步骤(3)所述的保护性气体为惰性气体；优选为氩气。
10.一种权利要求1或2所述的超薄氮氧化硅膜材料的用途，其特征在于，所述氮氧化硅膜材料作为绝缘层、保护膜或光学膜，应用于半导体、微波、光电子或光学器件领域。
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