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一种AlN薄膜的制备方法 【EN】A kind of preparation method of AlN film

申请(专利)号:CN201610841499.8国省代码:江苏 32
申请(专利权)人:【中文】昆山运城塑业有限公司【EN】Yuncheng, Kunshan Su Ye Co., Ltd
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摘要:
【中文】本发明涉及宽禁带半导体的制备领域,特别涉及一种(100)择优取向的AlN薄膜的制备方法,包括以下步骤:(1)衬底预处理;(2)靶材预处理;(3)采用离子束辅助沉积技术,Ar+离子束溅射沉积Al膜,N+离子束轰击Al膜,在衬底上形成AlN缓冲层;(4)N2、Ar以及NH3混合气体下,采用磁控溅射沉积技术,在AlN缓冲层上形成AlN薄膜。该方法制得的薄膜(100)择优取向生长,且薄膜质量优良。 【EN】Paragraph:The present invention relates to the preparation field of wide bandgap semiconductor, in particular to a kind of preparation method of the AlN film of (100) preferred orientation, comprising the following steps: (1) substrate pre-treatment;(2) target pre-processes;(3) ion beam assisted deposition, Ar are used+Ion beam sputter depositing Al film, N+Ion beam bombardment Al film, is formed on the substrate AlN buffer layer;(4)N2, Ar and NH3Under mixed gas, using magnetron sputtered deposition technology, AlN film is formed on AlN buffer layer.The growth of (100) preferred orientation of film made from this method, and film quality is excellent.

主权项:
【中文】1.一种AlN薄膜的制备方法,其特征在于,包括以下步骤: (1)衬底预处理; (2)靶材预处理; (3)采用离子束辅助沉积技术,Ar离子束溅射沉积Al膜,N离子束轰击Al膜,在衬底上形成AlN缓冲层; (4)N、Ar以及NH混合气体下,采用磁控溅射沉积技术,在AlN缓冲层上形成AlN薄膜;其中,磁控溅射沉积AlN薄膜时NH含量占2%~5%,磁控溅射沉积AlN薄膜分次进行,NH含量依次逐渐增多;磁控溅射时Ar与N体积之比为1:1。 【EN】1. a kind of preparation method of AlN film, which comprises the following steps: (1) substrate pre-treatment; (2) target pre-processes; (3) ion beam assisted deposition, Ar are usedIon beam sputter depositing Al film, NIon beam bombardment Al film, on substrate Form AlN buffer layer; (4)N, Ar and NHUnder mixed gas, using magnetron sputtered deposition technology, AlN film is formed on AlN buffer layer;Its In, NH when magnetron sputtering depositing Al N thin filmContent accounts for 2%~5%, and magnetron sputtering depositing Al N thin film carries out by several times, NHContent Successively gradually increase;Ar and N when magnetron sputteringThe ratio between volume is 1:1.


说明书

【中文】

一种AlN薄膜的制备方法

技术领域

本发明涉及宽禁带半导体的制备领域,特别涉及一种(100)择优取向的AlN薄膜的制备方法。

背景技术

AlN薄膜材料作为一种重要的宽禁带直接带隙半导体材料,具有许多非常优异的物理化学性能,例如:优异的表声波速率、低热膨胀系数、高化学稳定性、高电阻率、高热导率、高硬度、高熔点、宽禁带、大击穿场强、低介电损耗等。

不同择优取向的AlN薄膜具有不同的性质,对于多晶AlN薄膜来说,薄膜在生长过程中容易形成(002)择优取向,其制备较容易。现有技术多对(002)择优取向的薄膜进行探索,而对(100)择优取向的AlN薄膜研究较少,本发明提供一种(100)择优取向的AlN薄膜的制备方法,为拓宽AlN薄膜的应用提供了条件。

发明内容

本发明的目的是提供一种AlN薄膜的制备方法,使得该方法制得的薄膜(100)择优取向生长,且薄膜质量优良。

为实现上述目的,本发明采用以下技术手段:

一种AlN薄膜的制备方法,包括以下步骤:

(1)衬底预处理;

(2)靶材预处理;

(3)采用离子束辅助沉积技术,Ar+离子束溅射沉积Al膜,N+离子束轰击Al膜,在衬底上形成AlN缓冲层;

(4)N2、Ar以及NH3混合气体下,采用磁控溅射沉积技术,在AlN缓冲层上形成AlN薄膜。

优选地,衬底预处理包括湿法清洗与干法刻蚀清洗。

可选地,干法刻蚀清洗为在磁控溅射系统内设置离子源,通过离子源轰击清洗衬底。

更优地,采用N+离子束和Ar+离子束共同对衬底干法刻蚀清洗。

优选地,靶材预处理包括通Ar靶材预溅射和通N2靶材预溅射。

优选地,磁控溅射系统内设置离子束辅助沉积装置,在磁控溅射系统内进行离子束辅助沉积。

优选地,磁控溅射沉积AlN薄膜时NH3含量占2%~5%。

优选地,磁控溅射沉积AlN薄膜分次进行,NH3含量依次逐渐增多。

优选地,磁控溅射溅射电源采用脉冲电源。

优选地,磁控溅射时Ar与N2体积之比为1:1。

与现有技术相比,本发明具有以下优点:本发明溅射时引入NH3,NH3在高压电场下电离出N和H的正离子和电子,N的正离子在电场作用下去辅助轰击靶材,H的正离子诱导AlN在(100)晶面择优生长,制备了(100)择优取向的AlN薄膜;并且离子束辅助沉积缓冲层的生长,使得形成Al-N键的同时,增强Al、N与衬底表面原子混合,使薄膜与衬底附着性强;并且缓冲层的存在使得之后AlN薄膜能够同质生长,薄膜结晶质量好、晶格缺陷少。

具体实施方式

为了更好的理解本发明,下面通过实施例对本发明进一步说明,实施例只用于解释本发明,不会对本发明构成任何的限定。

本发明实施例所用磁控溅射系统为复合镀膜系统,包括离子源清洗系统、离子束辅助沉积系统以及磁控溅射镀膜系统。通过离子源清洗系统对衬底进一步清洗;通过离子束辅助沉积系统形成AlN缓冲层;通过磁控溅射镀膜系统生长AlN薄膜。

本发明采用理学D/MAX-2200型X射线衍射仪(XRD)来表征AlN薄膜的结构;用中科院化学所本原纳米仪器公司生产的CSPM-3100型原子力显微镜(AFM)来观察薄膜表面的形貌、颗粒大小及表面粗糙度;薄膜附着性通过冷热循环法表征,在0°冰水混合物中保持5分钟,然后立即放入100°沸水中保持5分钟,如此冷热循环若干个周期。

对比例

一种AlN薄膜的制备方法,包括以下步骤:

(1)衬底预处理;

衬底预处理包括衬底预处理包括湿法清洗与离子源轰击清洗。

衬底选用精抛光的单晶Si(100);

湿法清洗:精将抛光的单晶Si(100)浸入丙酮溶液中进行超声波处理15分钟,然后在混合液1(去离子水:过氧化氢:氟水=5:2:l)中煮沸5分钟,再用混合液2(去离子水:过氧化氢:盐酸=7:2:1)煮沸5分钟,最后在去离子水中进行超声波处理20分钟,以除去硅片表面可能存在的有机物,取出后放入充入纯N2的烘干箱中加热至100℃烘干1小时。

离子源轰击清洗:将清洗过的单晶Si(100)衬底放置于磁控溅射复合系统的离子源清洗系统样品台上,关闭腔体;Ar+离子束对衬底干法刻蚀清洗15min。

(2)靶材预处理;

将Al靶安装在磁控溅射复合系统内,正常启动磁控溅射仪器,对腔体抽真空至1×10-5Pa,沉积前先将挡板挡上,充入Ar气,将Al靶材先预溅射15min,以除去靶面的Al2O3层。

(3)N2、Ar混合气体下,采用脉冲反应磁控溅射沉积技术,形成AlN薄膜。工艺参数设置:靶基距为4.5cm,溅射气压为0.5Pa,Ar与N2含量各占50%,溅射功率为150W,衬底温度为75℃,脉冲频率30kHz,占空比为50%,沉积时间为60min。

XRD结果显示,本实施例AlN薄膜只在36°附近出AlN(002)晶面衍射峰,说明薄膜在(002)面择优生长;AFM三维视图显示薄膜表面粗糙,其均方根粗糙度(RMS)为4.7nm;附着性通过冷热循环10周期之后开始脱落。

实施例1

一种AlN薄膜的制备方法,包括以下步骤:

(1)衬底预处理;

衬底预处理包括衬底预处理包括湿法清洗与离子源轰击清洗。

衬底选用精抛光的单晶Si(100);

湿法清洗:精将抛光的单晶Si(100)浸入丙酮溶液中进行超声波处理15分钟,然后在混合液1(去离子水:过氧化氢:氟水=5:2:l)中煮沸5分钟,再用混合液2(去离子水:过氧化氢:盐酸=7:2:1)煮沸5分钟,最后在去离子水中进行超声波处理20分钟,以除去硅片表面可能存在的有机物,取出后放入充入纯N2的烘干箱中加热至100℃烘干1小时。

离子源轰击清洗:将清洗过的单晶Si(100)衬底放置于磁控溅射复合系统的离子源清洗系统样品台上,关闭腔体;Ar+离子束对衬底干法刻蚀清洗15min。

(2)靶材预处理;

将Al靶安装在磁控溅射复合系统内,正常启动磁控溅射仪器,对腔体抽真空至1×10-5Pa,沉积前先将挡板挡上,充入Ar气,将Al靶材先预溅射15min,以除去靶面的Al2O3层。

(3)采用离子束辅助沉积技术,用2500V/50mA的Ar+离子束溅射沉积Al膜,2500V/10mA的N+离子束轰击Al膜,辅助沉积30min在衬底上形成AlN缓冲层;

(4)旋转样品台,使其从离子束辅助沉积镀膜位置旋转至磁控溅射镀膜位置,N2、Ar以及NH3混合气体下,采用脉冲反应磁控溅射沉积技术,在AlN缓冲层上形成AlN薄膜。工艺参数设置:靶基距为4.5cm,溅射气压为0.5Pa,NH3含量占4%,Ar与N2含量各占48%,溅射功率为150W,衬底温度为75℃,脉冲频率30kHz,占空比为50%,沉积时间为60min。

XRD结果显示,本实施例AlN薄膜只在33°附近出AlN(100)晶面衍射峰,说明薄膜在(100)面择优生长;AFM三维视图显示薄膜表面光滑平整、均匀一致,其均方根粗糙度(RMS)为3.7nm;附着性通过冷热循环13周期之后开始脱落。

实施例2

一种AlN薄膜的制备方法,包括以下步骤:

(1)衬底预处理;

衬底预处理包括衬底预处理包括湿法清洗与离子源轰击清洗。

衬底选用精抛光的单晶Si(100);

湿法清洗:精将抛光的单晶Si(100)浸入丙酮溶液中进行超声波处理15分钟,然后在混合液1(去离子水:过氧化氢:氟水=5:2:l)中煮沸5分钟,再用混合液2(去离子水:过氧化氢:盐酸=7:2:1)煮沸5分钟,最后在去离子水中进行超声波处理20分钟,以除去硅片表面可能存在的有机物,取出后放入充入纯N2的烘干箱中加热至100℃烘干1小时。

离子源轰击清洗:将清洗过的单晶Si(100)衬底放置于磁控溅射复合系统的离子源清洗系统样品台上,关闭腔体;N+离子束和Ar+离子束共同对衬底干法刻蚀清洗15min。

(2)靶材预处理;

将Al靶安装在磁控溅射复合系统内,正常启动磁控溅射仪器,对腔体抽真空至1×10-5Pa,沉积前先将挡板挡上,充入Ar气,将Al靶材先预溅射15min,以除去靶面的Al2O3层,再关闭Ar气,通入N2气,预溅射10min。

(3)采用离子束辅助沉积技术,用2500V/50mA的Ar+离子束溅射沉积Al膜,2500V/10mA的N+离子束轰击Al膜,辅助沉积30min在衬底上形成AlN缓冲层;

(4)旋转样品台,使其从离子束辅助沉积镀膜位置旋转至磁控溅射镀膜位置,N2、Ar以及NH3混合气体下,采用脉冲反应磁控溅射沉积技术,在AlN缓冲层上形成AlN薄膜。工艺参数设置:靶基距为4.5cm,溅射气压为0.5Pa,NH3含量占4%,Ar与N2含量各占48%,溅射功率为150W,衬底温度为75℃,脉冲频率30kHz,占空比为50%,沉积时间为60min。

XRD结果显示,本实施例AlN薄膜只在33°附近出AlN(100)晶面衍射峰,说明薄膜在(100)面择优生长;AFM三维视图显示薄膜表面光滑平整、均匀一致,其均方根粗糙度(RMS)为3.5nm;附着性通过冷热循环14周期之后开始脱落。

实施例3

一种AlN薄膜的制备方法,包括以下步骤:

(1)衬底预处理;

衬底预处理包括衬底预处理包括湿法清洗与离子源轰击清洗。

衬底选用精抛光的单晶Si(100);

湿法清洗:精将抛光的单晶Si(100)浸入丙酮溶液中进行超声波处理15分钟,然后在混合液1(去离子水:过氧化氢:氟水=5:2:l)中煮沸5分钟,再用混合液2(去离子水:过氧化氢:盐酸=7:2:1)煮沸5分钟,最后在去离子水中进行超声波处理20分钟,以除去硅片表面可能存在的有机物,取出后放入充入纯N2的烘干箱中加热至100℃烘干1小时。

离子源轰击清洗:将清洗过的单晶Si(100)衬底放置于磁控溅射复合系统的离子源清洗系统样品台上,关闭腔体;N+离子束和Ar+离子束共同对衬底干法刻蚀清洗15min。

(2)靶材预处理;

将Al靶安装在磁控溅射复合系统内,正常启动磁控溅射仪器,对腔体抽真空至1×10-5Pa,沉积前先将挡板挡上,充入Ar气,将Al靶材先预溅射15min,以除去靶面的Al2O3层,再关闭Ar气,通入N2气,预溅射10min。

(3)采用离子束辅助沉积技术,用2500V/50mA的Ar+离子束溅射沉积Al膜,2500V/10mA的N+离子束轰击Al膜,辅助沉积30min在衬底上形成AlN缓冲层;

(4)旋转样品台,使其从离子束辅助沉积镀膜位置旋转至磁控溅射镀膜位置,N2、Ar以及NH3混合气体下,采用脉冲反应磁控溅射沉积技术,在AlN缓冲层上形成AlN薄膜。工艺参数设置:靶基距为4.5cm,溅射气压为0.5Pa,NH3含量占5%,Ar与N2含量各占47.5%,溅射功率为150W,衬底温度为75℃,脉冲频率30kHz,占空比为50%,沉积时间为60min。

XRD结果显示,本实施例AlN薄膜只在33°附近出AlN(100)晶面衍射峰,说明薄膜在(100)面择优生长;AFM三维视图显示薄膜表面光滑平整、均匀一致,其均方根粗糙度(RMS)为3.3nm;附着性通过冷热循环15周期之后开始脱落。

实施例4

一种AlN薄膜的制备方法,包括以下步骤:

(1)衬底预处理;

衬底预处理包括衬底预处理包括湿法清洗与离子源轰击清洗。

衬底选用精抛光的单晶Si(100);

湿法清洗:精将抛光的单晶Si(100)浸入丙酮溶液中进行超声波处理15分钟,然后在混合液1(去离子水:过氧化氢:氟水=5:2:l)中煮沸5分钟,再用混合液2(去离子水:过氧化氢:盐酸=7:2:1)煮沸5分钟,最后在去离子水中进行超声波处理20分钟,以除去硅片表面可能存在的有机物,取出后放入充入纯N2的烘干箱中加热至100℃烘干1小时。

离子源轰击清洗:将清洗过的单晶Si(100)衬底放置于磁控溅射复合系统的离子源清洗系统样品台上,关闭腔体;N+离子束和Ar+离子束共同对衬底干法刻蚀清洗15min。

(2)靶材预处理;

将Al靶安装在磁控溅射复合系统内,正常启动磁控溅射仪器,对腔体抽真空至1×10-5Pa,沉积前先将挡板挡上,充入Ar气,将Al靶材先预溅射15min,以除去靶面的Al2O3层,再关闭Ar气,通入N2气,预溅射10min。

(3)采用离子束辅助沉积技术,用2500V/50mA的Ar+离子束溅射沉积Al膜,2500V/10mA的N+离子束轰击Al膜,辅助沉积30min在衬底上形成AlN缓冲层;

(4)旋转样品台,使其从离子束辅助沉积镀膜位置旋转至磁控溅射镀膜位置,N2、Ar以及NH3混合气体下,采用脉冲反应磁控溅射沉积技术,在AlN缓冲层上形成AlN薄膜。工艺参数设置:靶基距为4.5cm,溅射气压为0.5Pa,NH3含量占6%,Ar与N2含量各占47%,溅射功率为150W,衬底温度为75℃,脉冲频率30kHz,占空比为50%,沉积时间为60min。

XRD结果显示,本实施例AlN薄膜只在33°附近出AlN(100)晶面衍射峰,说明薄膜在(100)面择优生长;AFM三维视图显示薄膜表面光滑平整、均匀一致,其均方根粗糙度(RMS)为3.3nm;附着性通过冷热循环14周期之后开始脱落。

实施例5

一种AlN薄膜的制备方法,包括以下步骤:

(1)衬底预处理;

衬底预处理包括衬底预处理包括湿法清洗与离子源轰击清洗。

衬底选用精抛光的单晶Si(100);

湿法清洗:精将抛光的单晶Si(100)浸入丙酮溶液中进行超声波处理15分钟,然后在混合液1(去离子水:过氧化氢:氟水=5:2:l)中煮沸5分钟,再用混合液2(去离子水:过氧化氢:盐酸=7:2:1)煮沸5分钟,最后在去离子水中进行超声波处理20分钟,以除去硅片表面可能存在的有机物,取出后放入充入纯N2的烘干箱中加热至100℃烘干1小时。

离子源轰击清洗:将清洗过的单晶Si(100)衬底放置于磁控溅射复合系统的离子源清洗系统样品台上,关闭腔体;N+离子束和Ar+离子束共同对衬底干法刻蚀清洗15min。

(2)靶材预处理;

将Al靶安装在磁控溅射复合系统内,正常启动磁控溅射仪器,对腔体抽真空至1×10-5Pa,沉积前先将挡板挡上,充入Ar气,将Al靶材先预溅射15min,以除去靶面的Al2O3层,再关闭Ar气,通入N2气,预溅射10min。

(3)采用离子束辅助沉积技术,用2500V/50mA的Ar+离子束溅射沉积Al膜,2500V/10mA的N+离子束轰击Al膜,辅助沉积30min在衬底上形成AlN缓冲层;

(4)旋转样品台,使其从离子束辅助沉积镀膜位置旋转至磁控溅射镀膜位置,N2、Ar以及NH3混合气体下,采用脉冲反应磁控溅射沉积技术,在AlN缓冲层上形成AlN薄膜。工艺参数设置:靶基距为4.5cm,溅射气压为0.5Pa,溅射功率为150W,衬底温度为75℃,脉冲频率30kHz,占空比为50%。第一次NH3含量占3%,Ar与N2含量各占48.5%,沉积时间为10min;其他条件不变,调整NH3含量占4%,Ar与N2含量各占48%,第二次沉积时间为10min;其他条件不变,调整NH3含量占5%,Ar与N2含量各占47.5%,第三次沉积时间为40min。

XRD结果显示,本实施例AlN薄膜只在33°附近出AlN(100)晶面衍射峰,说明薄膜在(100)面择优生长;AFM三维视图显示薄膜表面光滑平整、均匀一致,其均方根粗糙度(RMS)为3.1nm;附着性通过冷热循环15周期之后开始脱落。

【EN】

A kind of preparation method of AlN film

Technical field

The present invention relates to the preparation field of wide bandgap semiconductor, in particular to a kind of AlN film of (100) preferred orientation

Preparation method.

Background technique

AlN thin-film material has many very excellent as a kind of important broad stopband direct band-gap semicondictor material

Physical and chemical performance, such as: it is excellent table acoustic wave velocity, low thermal coefficient of expansion, high chemical stability, high resistivity, highly thermally conductive

Rate, high rigidity, high-melting-point, broad stopband, big disruptive field intensity, low-dielectric loss etc..

The AlN film of different preferred orientations has different property, and for polymorph A lN film, film was being grown

(002) preferred orientation easy to form in journey, preparation are easier to.The film of multipair (002) preferred orientation of the prior art is visited

Rope, and it is less to the AlN thin film study of (100) preferred orientation, and the present invention provides a kind of AlN film of (100) preferred orientation

Preparation method provides condition to widen the application of AlN film.

Summary of the invention

The object of the present invention is to provide a kind of preparation methods of AlN film, so that film made from this method (100) is preferentially

Oriented growth, and film quality is excellent.

To achieve the above object, the present invention uses following technological means:

A kind of preparation method of AlN film, comprising the following steps:

(1) substrate pre-treatment;

(2) target pre-processes;

(3) ion beam assisted deposition, Ar are used+Ion beam sputter depositing Al film, N+Ion beam bombardment Al film, is serving as a contrast

AlN buffer layer is formed on bottom;

(4)N2, Ar and NH3Under mixed gas, using magnetron sputtered deposition technology, it is thin that AlN is formed on AlN buffer layer

Film.

Preferably, substrate pre-treatment includes that wet-cleaning and dry etching clean.

Optionally, dry etching cleaning is served as a contrast for ion source is arranged in magnetic control sputtering system by ion source Bombardment and cleaning

Bottom.

More preferably, using N+Ion beam and Ar+Ion beam jointly cleans substrate dry etching.

Preferably, target pretreatment includes logical Ar target pre-sputtering and logical N2Target pre-sputtering.

Preferably, ion beam assisted depositing device is set in magnetic control sputtering system, ion is carried out in magnetic control sputtering system

Beam assistant depositing.

Preferably, NH when magnetron sputtering depositing Al N thin film3Content accounts for 2%~5%.

Preferably, magnetron sputtering depositing Al N thin film carries out by several times, NH3Content successively gradually increases.

Preferably, magnetron sputtering shielding power supply uses the pulse power.

Preferably, Ar and N when magnetron sputtering2The ratio between volume is 1:1.

Compared with prior art, the invention has the following advantages that the present invention introduces NH when sputtering3,NH3Under high voltage electric field

The cation and electronics of N and H are ionized out, the cation of N goes down to assist bombardment target in electric field action, and the cation of H induces AlN

In (100) crystal face preferential growth, it is prepared for the AlN film of (100) preferred orientation;And the life of ion beam assisted depositing buffer layer

Long, while so that forming Al-N key, REINFORCED Al, N are mixed with substrate surface atom, keep film strong with substrate adhesion;And

AlN film homogenous growth after the presence of buffer layer enables, film crystalline quality is good, lattice defect is few.

Specific embodiment

In order to better understand the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving

The present invention is released, any restriction will not be constituted to the present invention.

Magnetic control sputtering system used in the embodiment of the present invention is composite film coating system, including ion source cleaning system, ion beam

Assisted deposition system and magnetron sputtering coating system.Substrate is further cleaned by ion source cleaning system;Pass through ion

Beam assisted deposition system forms AlN buffer layer;Pass through magnetron sputtering coating system growing AIN film.

The present invention characterizes the structure of AlN film using Neo-Confucianism D/MAX-2200 type X-ray diffractometer (XRD);With middle section

The CSPM-3100 type atomic force microscope (AFM) of basis nanometer instrument company, chemistry institute, institute production observes the shape of film surface

Looks, granular size and surface roughness;Film adhesion is characterized by cold cycling method, and 5 points are kept in 0 ° of mixture of ice and water

Clock is put into 100 ° of boiling water immediately after and is kept for 5 minutes, several periods of such cold cycling.

Comparative example

A kind of preparation method of AlN film, comprising the following steps:

(1) substrate pre-treatment;

Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.

The single crystalline Si (100) of substrate selection finishing polish;

Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonication 15 minutes by essence, then

It is boiled 5 minutes in mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l), then with the (deionized water: peroxide of mixed liquor 2

Change hydrogen: hydrochloric acid=7:2:1) it boils 5 minutes, it finally carries out ultrasonication 20 minutes in deionized water, to remove silicon wafer table

Face organic matter that may be present, is put into after taking-up and is filled with pure N2Drying box in be heated to 100 DEG C dry 1 hour.

Ion source Bombardment and cleaning: the single crystalline Si cleaned (100) substrate is placed in the ion of magnetron sputtering composite system

On the cleaning system sample stage of source, cavity is closed;Ar+Ion beam cleans 15min to substrate dry etching.

(2) target pre-processes;

Al target is mounted in magnetron sputtering composite system, magnetron sputtering apparatus is normally started, 1 is evacuated to cavity ×

10-5Pa, deposition is preceding first to block baffle, Ar gas is filled with, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer.

(3)N2, under Ar mixed gas, using pulse reaction magnetron sputtered deposition technology, form AlN film.Technological parameter

Setting: target-substrate distance 4.5cm, sputtering pressure 0.5Pa, Ar and N2Content respectively accounts for 50%, sputtering power 150W, underlayer temperature

It is 75 DEG C, pulse frequency 30kHz, duty ratio 50%, sedimentation time 60min.

XRD illustrates that film exists the results show that the present embodiment AlN film only nearby goes out AlN (002) crystallographic plane diffraction peak at 36 °

(002) face preferential growth;AFM 3-D view shows that film surface is coarse, and r.m.s. roughness (RMS) is 4.7nm;Adhesion

By being started shedding off after 10 period of cold cycling.

Embodiment 1

A kind of preparation method of AlN film, comprising the following steps:

(1) substrate pre-treatment;

Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.

The single crystalline Si (100) of substrate selection finishing polish;

Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonication 15 minutes by essence, then

It is boiled 5 minutes in mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l), then with the (deionized water: peroxide of mixed liquor 2

Change hydrogen: hydrochloric acid=7:2:1) it boils 5 minutes, it finally carries out ultrasonication 20 minutes in deionized water, to remove silicon wafer table

Face organic matter that may be present, is put into after taking-up and is filled with pure N2Drying box in be heated to 100 DEG C dry 1 hour.

Ion source Bombardment and cleaning: the single crystalline Si cleaned (100) substrate is placed in the ion of magnetron sputtering composite system

On the cleaning system sample stage of source, cavity is closed;Ar+Ion beam cleans 15min to substrate dry etching.

(2) target pre-processes;

Al target is mounted in magnetron sputtering composite system, magnetron sputtering apparatus is normally started, 1 is evacuated to cavity ×

10-5Pa, deposition is preceding first to block baffle, Ar gas is filled with, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer.

(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/

The N of 10mA+AlN buffer layer is formed on the substrate in ion beam bombardment Al film, assistant depositing 30min;

(4) specimen rotating holder rotates it to magnetron sputtering film location, N from ion beam assisted depositing plating film location2

Ar and NH3Under mixed gas, using pulse reaction magnetron sputtered deposition technology, AlN film is formed on AlN buffer layer.Work

Skill parameter setting: target-substrate distance 4.5cm, sputtering pressure 0.5Pa, NH3Content accounts for 4%, Ar and N2Content respectively accounts for 48%, sputtering

Power is 150W, and underlayer temperature is 75 DEG C, pulse frequency 30kHz, duty ratio 50%, sedimentation time 60min.

XRD illustrates that film exists the results show that the present embodiment AlN film only nearby goes out AlN (100) crystallographic plane diffraction peak at 33 °

(100) face preferential growth;AFM 3-D view shows that film surface is smooth, uniformity, r.m.s. roughness (RMS)

For 3.7nm;Adhesion after 13 period of cold cycling by starting shedding off.

Embodiment 2

A kind of preparation method of AlN film, comprising the following steps:

(1) substrate pre-treatment;

Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.

The single crystalline Si (100) of substrate selection finishing polish;

Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonication 15 minutes by essence, then

It is boiled 5 minutes in mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l), then with the (deionized water: peroxide of mixed liquor 2

Change hydrogen: hydrochloric acid=7:2:1) it boils 5 minutes, it finally carries out ultrasonication 20 minutes in deionized water, to remove silicon wafer table

Face organic matter that may be present, is put into after taking-up and is filled with pure N2Drying box in be heated to 100 DEG C dry 1 hour.

Ion source Bombardment and cleaning: the single crystalline Si cleaned (100) substrate is placed in the ion of magnetron sputtering composite system

On the cleaning system sample stage of source, cavity is closed;N+Ion beam and Ar+Ion beam cleans 15min to substrate dry etching jointly.

(2) target pre-processes;

Al target is mounted in magnetron sputtering composite system, magnetron sputtering apparatus is normally started, 1 is evacuated to cavity ×

10-5Pa, deposition is preceding first to block baffle, Ar gas is filled with, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer,

Ar gas is turned off, N is passed through2Gas, pre-sputtering 10min.

(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/

The N of 10mA+AlN buffer layer is formed on the substrate in ion beam bombardment Al film, assistant depositing 30min;

(4) specimen rotating holder rotates it to magnetron sputtering film location, N from ion beam assisted depositing plating film location2

Ar and NH3Under mixed gas, using pulse reaction magnetron sputtered deposition technology, AlN film is formed on AlN buffer layer.Work

Skill parameter setting: target-substrate distance 4.5cm, sputtering pressure 0.5Pa, NH3Content accounts for 4%, Ar and N2Content respectively accounts for 48%, sputtering

Power is 150W, and underlayer temperature is 75 DEG C, pulse frequency 30kHz, duty ratio 50%, sedimentation time 60min.

XRD illustrates that film exists the results show that the present embodiment AlN film only nearby goes out AlN (100) crystallographic plane diffraction peak at 33 °

(100) face preferential growth;AFM 3-D view shows that film surface is smooth, uniformity, r.m.s. roughness (RMS)

For 3.5nm;Adhesion after 14 period of cold cycling by starting shedding off.

Embodiment 3

A kind of preparation method of AlN film, comprising the following steps:

(1) substrate pre-treatment;

Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.

The single crystalline Si (100) of substrate selection finishing polish;

Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonication 15 minutes by essence, then

It is boiled 5 minutes in mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l), then with the (deionized water: peroxide of mixed liquor 2

Change hydrogen: hydrochloric acid=7:2:1) it boils 5 minutes, it finally carries out ultrasonication 20 minutes in deionized water, to remove silicon wafer table

Face organic matter that may be present, is put into after taking-up and is filled with pure N2Drying box in be heated to 100 DEG C dry 1 hour.

Ion source Bombardment and cleaning: the single crystalline Si cleaned (100) substrate is placed in the ion of magnetron sputtering composite system

On the cleaning system sample stage of source, cavity is closed;N+Ion beam and Ar+Ion beam cleans 15min to substrate dry etching jointly.

(2) target pre-processes;

Al target is mounted in magnetron sputtering composite system, magnetron sputtering apparatus is normally started, 1 is evacuated to cavity ×

10-5Pa, deposition is preceding first to block baffle, Ar gas is filled with, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer,

Ar gas is turned off, N is passed through2Gas, pre-sputtering 10min.

(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/

The N of 10mA+AlN buffer layer is formed on the substrate in ion beam bombardment Al film, assistant depositing 30min;

(4) specimen rotating holder rotates it to magnetron sputtering film location, N from ion beam assisted depositing plating film location2

Ar and NH3Under mixed gas, using pulse reaction magnetron sputtered deposition technology, AlN film is formed on AlN buffer layer.Work

Skill parameter setting: target-substrate distance 4.5cm, sputtering pressure 0.5Pa, NH3Content accounts for 5%, Ar and N2Content respectively accounts for 47.5%, splashes

Penetrating power is 150W, and underlayer temperature is 75 DEG C, pulse frequency 30kHz, duty ratio 50%, sedimentation time 60min.

XRD illustrates that film exists the results show that the present embodiment AlN film only nearby goes out AlN (100) crystallographic plane diffraction peak at 33 °

(100) face preferential growth;AFM 3-D view shows that film surface is smooth, uniformity, r.m.s. roughness (RMS)

For 3.3nm;Adhesion after 15 period of cold cycling by starting shedding off.

Embodiment 4

A kind of preparation method of AlN film, comprising the following steps:

(1) substrate pre-treatment;

Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.

The single crystalline Si (100) of substrate selection finishing polish;

Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonication 15 minutes by essence, then

It is boiled 5 minutes in mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l), then with the (deionized water: peroxide of mixed liquor 2

Change hydrogen: hydrochloric acid=7:2:1) it boils 5 minutes, it finally carries out ultrasonication 20 minutes in deionized water, to remove silicon wafer table

Face organic matter that may be present, is put into after taking-up and is filled with pure N2Drying box in be heated to 100 DEG C dry 1 hour.

Ion source Bombardment and cleaning: the single crystalline Si cleaned (100) substrate is placed in the ion of magnetron sputtering composite system

On the cleaning system sample stage of source, cavity is closed;N+Ion beam and Ar+Ion beam cleans 15min to substrate dry etching jointly.

(2) target pre-processes;

Al target is mounted in magnetron sputtering composite system, magnetron sputtering apparatus is normally started, 1 is evacuated to cavity ×

10-5Pa, deposition is preceding first to block baffle, Ar gas is filled with, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer,

Ar gas is turned off, N is passed through2Gas, pre-sputtering 10min.

(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/

The N of 10mA+AlN buffer layer is formed on the substrate in ion beam bombardment Al film, assistant depositing 30min;

(4) specimen rotating holder rotates it to magnetron sputtering film location, N from ion beam assisted depositing plating film location2

Ar and NH3Under mixed gas, using pulse reaction magnetron sputtered deposition technology, AlN film is formed on AlN buffer layer.Work

Skill parameter setting: target-substrate distance 4.5cm, sputtering pressure 0.5Pa, NH3Content accounts for 6%, Ar and N2Content respectively accounts for 47%, sputtering

Power is 150W, and underlayer temperature is 75 DEG C, pulse frequency 30kHz, duty ratio 50%, sedimentation time 60min.

XRD illustrates that film exists the results show that the present embodiment AlN film only nearby goes out AlN (100) crystallographic plane diffraction peak at 33 °

(100) face preferential growth;AFM 3-D view shows that film surface is smooth, uniformity, r.m.s. roughness (RMS)

For 3.3nm;Adhesion after 14 period of cold cycling by starting shedding off.

Embodiment 5

A kind of preparation method of AlN film, comprising the following steps:

(1) substrate pre-treatment;

Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.

The single crystalline Si (100) of substrate selection finishing polish;

Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonication 15 minutes by essence, then

It is boiled 5 minutes in mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l), then with the (deionized water: peroxide of mixed liquor 2

Change hydrogen: hydrochloric acid=7:2:1) it boils 5 minutes, it finally carries out ultrasonication 20 minutes in deionized water, to remove silicon wafer table

Face organic matter that may be present, is put into after taking-up and is filled with pure N2Drying box in be heated to 100 DEG C dry 1 hour.

Ion source Bombardment and cleaning: the single crystalline Si cleaned (100) substrate is placed in the ion of magnetron sputtering composite system

On the cleaning system sample stage of source, cavity is closed;N+Ion beam and Ar+Ion beam cleans 15min to substrate dry etching jointly.

(2) target pre-processes;

Al target is mounted in magnetron sputtering composite system, magnetron sputtering apparatus is normally started, 1 is evacuated to cavity ×

10-5Pa, deposition is preceding first to block baffle, Ar gas is filled with, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer,

Ar gas is turned off, N is passed through2Gas, pre-sputtering 10min.

(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/

The N of 10mA+AlN buffer layer is formed on the substrate in ion beam bombardment Al film, assistant depositing 30min;

(4) specimen rotating holder rotates it to magnetron sputtering film location, N from ion beam assisted depositing plating film location2

Ar and NH3Under mixed gas, using pulse reaction magnetron sputtered deposition technology, AlN film is formed on AlN buffer layer.Work

Skill parameter setting: target-substrate distance 4.5cm, sputtering pressure 0.5Pa, sputtering power 150W, underlayer temperature are 75 DEG C, pulse frequency

Rate 30kHz, duty ratio 50%.First time NH3Content accounts for 3%, Ar and N2Content respectively accounts for 48.5%, sedimentation time 10min;

Other conditions are constant, adjust NH3Content accounts for 4%, Ar and N2Content respectively accounts for 48%, and second of sedimentation time is 10min;Other

Part is constant, adjusts NH3Content accounts for 5%, Ar and N2Content respectively accounts for 47.5%, and third time sedimentation time is 40min.

XRD illustrates that film exists the results show that the present embodiment AlN film only nearby goes out AlN (100) crystallographic plane diffraction peak at 33 °

(100) face preferential growth;AFM 3-D view shows that film surface is smooth, uniformity, r.m.s. roughness (RMS)

For 3.1nm;Adhesion after 15 period of cold cycling by starting shedding off.

图1
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