CN106206684B - 氧化物半导体膜及其制备方法 - Google Patents

氧化物半导体膜及其制备方法 Download PDF

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CN106206684B
CN106206684B CN201510219946.1A CN201510219946A CN106206684B CN 106206684 B CN106206684 B CN 106206684B CN 201510219946 A CN201510219946 A CN 201510219946A CN 106206684 B CN106206684 B CN 106206684B
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oxide semiconductor
semiconductor film
sputtering
film according
oxide
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CN106206684A (zh
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庄大明
赵明
曹明杰
郭力
高泽栋
魏要伟
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Tsinghua University
Hongfujin Precision Industry Shenzhen Co Ltd
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Tsinghua University
Hongfujin Precision Industry Shenzhen Co Ltd
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Priority to TW104115812A priority patent/TWI593630B/zh
Priority to US14/749,340 priority patent/US9530640B2/en
Priority to US15/338,529 priority patent/US9945022B2/en
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Abstract

本发明涉及一种氧化物半导体膜，含有铟元素(In)、铈元素(Ce)、锌元素(Zn)及氧元素(O)，该In:Ce:Zn的摩尔比为2:(0.5~2):1，氧化物半导体膜为n型半导体，载流子浓度为1012cm‑3~1020cm‑3，载流子迁移率为5.0 cm2V‑1s‑1~45.0 cm2V‑1s‑1。本发明还涉及一种氧化物半导体膜的制备方法。

Description

氧化物半导体膜及其制备方法
技术领域
本发明涉及一种氧化物半导体膜及其制备方法。
背景技术
随着信息技术的飞速发展，平板显示技术正向着更高分辨率、更快响应速度、更低能耗、全透明器件以及柔性显示等目标发展，这也对有源驱动显示（如AMLCD，ActiveMatrix Liquid Crystal Display）中TFT（thin film transistor）器件的性能提出更高要求。传统的非晶硅TFT由于其迁移率较低（~ 0.5cm2 V-1 s-1）的特性不能满足高分辨率、大尺寸LCD的显示要求，更限制其在AMOLED（Active Matrix Organic Light Emitting Diode）显示中的应用。而低温多晶硅TFT虽然迁移率较高，但是其生产成本过高，大面积均匀性较难保证，不适合应用于大面积、高分辨显示器。相较于非晶硅TFT和低温多晶硅TFT，基于非晶氧化物半导体InGaZnO4的薄膜晶体管（IGZO-TFT）以其透过率高、制备温度低、工艺兼容性好等诸多优点，能够替代非晶硅TFT，并且有望用于透明显示以及OLED显示。
然而，IGZO-TFT器件迁移率在非晶硅TFT和低温多晶硅TFT之间，若能进一步提高IGZO-TFT的器件迁移率，其优势将更明显。研究发现，二元氧化物氧化铟锌（IZO）的迁移率远大于三元氧化物IGZO，但由于其载流子浓度过高，且在使用中易受光照及栅压等影响导致性能参数发生变化，即稳定性差，因此不适合制备TFT器件。
发明内容
有鉴于此，确有必要提供一迁移率较高且稳定性较好的氧化物半导体膜及其制备方法。
一种氧化物半导体膜，含有铟元素(In)、铈元素(Ce)、锌元素(Zn)及氧元素(O)，该In:Ce:Zn的摩尔比为2:(0.5~2):1，氧化物半导体膜为n型半导体，载流子浓度为1012cm-3~1020cm-3，载流子迁移率为5.0 cm2V-1s-1~45.0 cm2V-1s-1。
与现有技术相比，三元氧化物ICZO中铈（Ce）元素的加入不仅能降低载流子浓度，同时还能保证高迁移率，从而具有较好的半导体性能，适合用于制备薄膜晶体管，用于平板显示器或其它电子设备中。另外，由于In、Ce及Zn均可在室温进行溅射，该溅射形成半导体膜的过程可以在室温进行，从而简化了生产工艺。
附图说明
图1为本发明实施例薄膜晶体管的结构示意图。
图2为本发明实施例2-1氧化物半导体薄膜的XRD图谱。
图3为本发明实施例2-1氧化物半导体薄膜的电学性能随溅射氧气流量的变化数据图。
图4为本发明实施例2-1氧化物半导体薄膜的扫描电镜照片。
图5为本发明实施例2-2氧化物半导体薄膜的电学性能随溅射氧气流量的变化数据图。
图6为本发明实施例2-2氧化物半导体薄膜的扫描电镜照片。
图7为本发明实施例2-3氧化物半导体薄膜的电学性能随溅射氧气流量的变化数据图。
图8为本发明实施例2-3氧化物半导体薄膜的扫描电镜照片。
主要元件符号说明
薄膜晶体管 10
绝缘基底 110
栅极 120
绝缘层 130
半导体层 140
源极 151
漏极 152
如下具体实施方式将结合上述附图进一步说明本发明。
具体实施方式
下面将结合附图及具体实施例对本发明提供的氧化物半导体膜及其制备方法作进一步的详细说明。
本发明实施例提供一种溅射靶，由氧化铟(In2O3)、氧化铈(CeO2)及氧化锌(ZnO)混合后烧结形成，该溅射靶中含有化合物In2CexZnO4+2x，其中x=0.5~2。
优选地，该化合物In2CexZnO4+2x为晶态。该溅射靶中可以含有非晶态的In、Ce及Zn的氧化物，优选地，晶态In2CexZnO4+2x在该溅射靶中的含量为80%以上。
在一实施例中，该溅射靶仅含有由In2O3、CeO2及ZnO氧化物混合后烧结形成的物质及微量杂质，该杂质的含量优选为小于10ppm。
在另一实施例中，该溅射靶仅含有晶态In2CexZnO4+2x及微量杂质，该杂质的含量优选为小于10ppm。
在一实施例中，该溅射靶由In2O3、CeO2及ZnO混合后烧结形成的烧结物经过机械加工成型得到。
该溅射靶的相对密度优选大于或等于90%，该相对密度=溅射靶实际密度:In2CexZnO4+2x理论密度×100%。
该溅射靶的体电阻优选为10-2Ωcm ~10Ωcm。
该溅射靶表面的粗糙度优选小于或等于2微米，更优选为小于或等于0.5微米。
该溅射靶的平均抗弯强度优选为大于或等于50MPa，更优选为大于或等于55MPa。
本发明实施例提供一种溅射靶的制备方法，包括：
将In2O3粉末、CeO2粉末及ZnO粉末均匀混合形成一混合体，该混合体中In:Ce:Zn的摩尔比为2:(0.5~2):1；以及
将该混合体在1250°C~1650°C进行烧结。
在该混合体中，该In2O3粉末、CeO2粉末及ZnO粉末的粒径优选为小于或等于10微米，更优选为0.5微米~2微米。
该In2O3粉末、CeO2粉末及ZnO粉末的纯度优选为3N(质量百分比99.9%)~5N(质量百分比99.999%)。
该In2O3粉末、CeO2粉末及ZnO粉末摩尔比例为In2O3: CeO2: ZnO =2: (1 ~4): 2。
该In2O3粉末、CeO2粉末及ZnO粉末可以在空气或保护气体（如Ar气或N2气）中进行混合，该混合步骤可进一步包括：
将该In2O3粉末、CeO2粉末及ZnO粉末在液态介质中进行球磨；及
将球磨后的混合物烘干去除该液态介质。
该液态介质为不与原料In2O3粉末、CeO2粉末及ZnO粉末发生反应，且通过之后的烘干步骤可以去除，不向混合物中引入其它杂质。该液态介质例如可以是水、乙醇及丙酮中的至少一种。
该球磨是在球磨机中进行，该液态介质与该原料In2O3粉末、CeO2粉末及ZnO粉末置入该球磨机中。该球磨机的转速优选为100 rpm~600rpm。在球磨的过程中，一方面可以将该In2O3粉末、CeO2粉末及ZnO粉末充分混合均匀，另一方面可以将粉末的粒径细化，得到所需粒径的原料粉末。该球磨时间以混合均匀并且原料粒度达到要求为准。
该烘干的温度优选为30°C~60°C，该烘干步骤可以在空气或保护气体（如Ar气或N2气）中进行，优选为在高纯(3N~5N)保护气体中进行烘干。
该烧结的步骤可以是将该混合体进行热压烧结（非等静压）、常压烧结或热等静压烧结。该热压烧结的压力可以为30MPa~100MPa，烧结时间可以为1小时~24小时。该热等静压烧结的压力可以为100MPa~300MPa，烧结时间可以为1小时~40小时。该常压烧结的烧结时间可以为1小时~40小时。
该烧结过程在保护气体中进行，该保护气体可以为Ar气或N2气，优选为纯度为3N~5N的Ar气或N2气。
当烧结过程中同时施加压力时，该混合体可以在烧结过程中成型，以形成预定形状的溅射靶，适于后续溅射使用。具体可以是将该烧结体放入具有预定形状的模具中进行热压烧结或等静压烧结。
当该烧结为常压烧结时，该混合体可以在烧结前先进行成型，以形成预定形状的溅射靶，适于后续溅射使用。具体可以是将该烧结体放入具有预定形状的模具中进行压制。该压制所用的压力可以为30MPa~300MPa。
另外，当采用任何烧结方式进行烧结前，均可对混合体进行预成型步骤，例如可以采用模具、浇铸或注射等方式使混合体预成型，在预成型过程中可以在混合体中加入粘结剂和/或溶剂。该粘结剂和/或溶剂在后续的烧结步骤中可以被完全去除。
在烧结后得到具有预定形状的烧结体后可以直接作为该溅射靶使用，也可以进一步进行加工成型、打磨等步骤。
在烧结过程中，原料In2O3粉末、CeO2粉末及ZnO粉末反应生成晶态In2CexZnO4+2x。
本发明实施例进一步提供一种氧化物半导体膜，包括体铟元素(In)、铈元素(Ce)、锌元素(Zn)及氧元素(O)，该In:Ce:Zn的摩尔比为2:(0.5~2):1，氧化物半导体膜为n型半导体，载流子浓度为1012cm-3~1020cm-3，载流子迁移率为5.0 cm2V-1s-1~45.0 cm2V-1s-1。
该氧化物半导体膜优选为非晶质氧化物。在另一实施例中，该氧化物半导体膜中也可含有晶态In2CexZnO4+2x。
在一实施例中，该氧化物半导体膜除该In、Ce、Zn及O元素外，仅含有微量杂质，该杂质的含量优选为小于10ppm。
该氧化物半导体膜的禁带宽度优选为3.0 eV ~3.5 eV。
该氧化物半导体膜的可见光透过率优选为60%~90%。
该氧化物半导体膜的厚度优选为50nm~1000nm。
该氧化物半导体膜的载流子浓度优选为1013cm-3~1015cm-3。
该氧化物半导体膜的载流子迁移率优选为12.3 cm2V-1s-1~45.0 cm2V-1s-1。
该氧化物半导体膜可以通过使用上述溅射靶，通过溅射法获得。
本发明实施例进一步提供一种氧化物半导体膜的制备方法，包括使用上述溅射靶，通过溅射法在基底上溅射形成氧化物膜。
该溅射法可以为磁控溅射法，例如直流溅射法或交流溅射法（如中频磁控溅射法或射频磁控溅射法），优选为中频磁控溅射法或射频磁控溅射法。该溅射的电流优选为0.1A~2.0A。该溅射的时间优选为1分钟~120分钟。
该溅射的温度可以为常温或高温，优选小于或等于400°C。当采用高温时，该制备方法可进一步包括在溅射前将该基底在真空中预热的步骤，该预热温度例如可以为50°C~400°C。
该溅射法中使用的载气可以为稀有气体、稀有气体与氧气的混合气或稀有气体与氢气的混合气，该稀有气体优选为Ar气。该载气优选为Ar气与氧气的混合气。该氧气的流量优选小于3sccm。载气中各气体的纯度优选为3N~5N。
该溅射时溅射室内的压力优选为0.1Pa~2.0Pa。
该基板的材料为绝缘材料且能够耐受该氧化物半导体膜制备过程中的加热温度。当该氧化物半导体膜制备过程所用温度较低，如采用常温溅射，该基板的材料选择范围较宽。该基板的材料可以列举为玻璃、硅或聚合物（如PI、PE、PET等）。
在进行溅射前，该制备方法可进一步包括对基底进行清洁的步骤，以去除基底表面的杂质。
在进行溅射前，该基底材料可以安装在夹具上进行固定，该基底与该溅射靶可以相互平行，也可以呈一夹角，该夹角可以为20º~85º之间。该基底与该溅射靶之间的距离优选小于或等于8cm。
在进行溅射在该基底上形成氧化物膜后，该氧化物膜可直接作为氧化物半导体膜。在另一实施例中，该制备方法还可进一步包括将该氧化物膜退火的步骤。具体地，是在真空、氮气或保护气体（如Ar气）中进行退火。该退火过程的本底真空优选为10-3Pa~10Pa。该退火温度优选为100°C~400°C，升温速率优选为1°C/min~20°C/min，退火时间优选为1小时~10小时。该退火过程可在一定程度上提高该氧化物膜的结晶度，从而对氧化物半导体膜产品的性能进行调整。
本发明实施例提供的氧化物半导体膜及其制备方法中，采用原位掺杂Ce的氧化铟锌得到In2CexZnO4+2x溅射靶，其中x=0.5~2。利用该溅射靶溅射得到n型氧化物半导体膜，In:Ce:Zn的摩尔比例为2:(0.5~2):1。该n型氧化物半导体膜的载流子霍尔迁移率在5.0 cm2V- 1s-1~45.0 cm2V-1s-1，载流子浓度在1012cm-3~1020cm-3，可以用于制备n型薄膜晶体管，用于平板显示器或其它电子设备中。该Ce元素在该氧化物半导体膜中的含量不能太小或太大，当x<0.5，半导体氧化物膜的性质偏向IZO，容易导致膜的稳定性降低，应用到半导体元件在使用中易受光照及栅压等影响使该半导体氧化物膜的参数发生变化；当x>2时，该半导体氧化物膜的迁移率下降，影响半导体元件性能。
本发明实施例还提供一种半导体元件，该半导体元件包括所述氧化物半导体膜。
请参阅图1，本发明实施例还提供一种薄膜晶体管10，该薄膜晶体管包括绝缘基底110、半导体层140、源极151、漏极152、栅极120及绝缘层130。该源极151与漏极152间隔设置，该半导体层140与该源极151和漏极152电连接，该栅极120通过该绝缘层130与该半导体层140、源极151及漏极152绝缘设置。该半导体层140为所述氧化物半导体膜。该薄膜晶体管10中除该氧化物半导体膜外的其它元件可根据现有技术设置及制备。图1中的薄膜晶体管10为一顶栅结构，可以理解，该薄膜晶体管10也可以为底栅结构或其它薄膜晶体管结构。
实施例1：溅射靶及其制备方法
实施例1-1
称量纯度为4N的209g In2O3粉末、260g CeO2粉末和61g ZnO粉末（三种氧化物摩尔比例为In2O3: CeO2: ZnO =1:2:1），将三种粉末放入球磨罐中混合。球磨介质选为无水乙醇，球磨转速200 rpm，球磨时间10 h。球磨结束后在压力为1 atm、纯度为5N的Ar气保护下烘干1 h。烘干后将粉末放入热压烧结炉中，在高纯Ar气氛围中进行热压烧结，烧结压力为50 MPa，烧结温度为1350℃，升温速率为15 ºC /min，烧结时间为5 h。烧结结束后随炉冷却至室温取样。靶材相对密度>87%，体电阻0.75Ωcm。将靶材用于中频交流磁控溅射，起弧容易，溅射稳定。
实施例1-2
称量纯度为4N的249g In2O3粉末、231g CeO2粉末和73g ZnO粉末（三种氧化物摩尔比例为In2O3: CeO2: ZnO =2:3:2），将三种粉末放入球磨罐中混合。球磨介质选为无水乙醇，球磨转速为400 rpm，球磨时间为20 h。球磨结束后在压力为1 atm、纯度为5N的Ar气保护下烘干1 h。采用常压烧结制备靶材，将粉末放入普通压机中，压力为75MPa，保压时间为60 min。脱模后放入烧结炉，在高纯N2气氛围中进行烧结，烧结温度为1450℃，升温速率为10 ºC /min，烧结时间为8h。烧结结束后随炉冷却至室温取样。靶材相对密度>85%，体电阻0.12Ωcm。将靶材用于中频交流磁控溅射，起弧容易，溅射稳定。
实施例1-3
称量纯度为4N的209g In2O3粉末、260g CeO2粉末和61g ZnO粉末（三种氧化物摩尔比例为In2O3: CeO2: ZnO =1:2:1），放入球磨罐中混合。球磨介质选为无水乙醇，球磨转速500 rpm，球磨时间为10 h。球磨结束后在压力为1 atm、纯度为5N的N2气保护下烘干1 h。将粉末进行包裹后，放入等静压机中，在高纯Ar气氛围中进行烧结。烧结压力为100 MPa，烧结温度为1450℃，升温速率为10 ºC /min，烧结时间为20 h。烧结结束后随炉冷却至室温取样。靶材相对密度>86%，体电阻0.62Ωcm。将靶材用于中频交流磁控溅射，起弧容易，溅射稳定。
实施例2：氧化物半导体膜
实施例2-1
选用市售普通钠钙玻璃作为基底，将基底洗净并用N2吹干后置入磁控溅射仪中。基底与靶材表面平行，距离8 cm。靶材为实施例1-1掺铈氧化铟锌靶材In2CexZnO4+2x，三种氧化物摩尔比例为In2O3: CeO2: ZnO =1:2:1。采用40 sccm的Ar和0 ~ 2sccm的O2作为工作气体，工作电流为1.0 A，工作气压为0.7 Pa，在室温进行磁控溅射，溅射时间为28 min，制得250 nm厚的ICZO薄膜，经过Hall测试测得该ICZO薄膜霍尔迁移率达14 cm2V-1s-1~25.6cm2V-1s-1，载流子浓度在1013 cm-3~1020 cm-3。请参阅图2，从XRD谱图可以看到该ICZO薄膜为无定形结构。请参阅图3，ICZO薄膜载流子浓度及霍尔迁移率随溅射使用的O2流量的变化数据如图3所示。请参阅图4，ICZO薄膜扫描电镜表面形貌如图4所示。
实施例2-2
选用市售普通钠钙玻璃作为衬底，将基片洗净并用N2吹干后置入磁控溅射仪中。基底与靶材表面平行，距离8 cm。靶材为实施例1-2掺铈氧化铟锌靶材In2CexZnO4+2x，制备该靶材所用的三种氧化物摩尔比例为In2O3: CeO2: ZnO =2:3:2，用40 sccm的Ar和0 ~ 3sccm的O2作为工作气体，基底预热温度为250℃，工作电流为1.0 A，工作气压为0.7 Pa，溅射时间为28 min，制得250 nm厚的ICZO薄膜。经过Hall测试测得该ICZO薄膜霍尔迁移率达17.8cm2V-1s-1~ 45.0 cm2V-1s-1，载流子浓度在1015 cm-3~1020 cm-3。请参阅图5，ICZO薄膜载流子浓度及霍尔迁移率随溅射使用的O2流量的变化数据如图5所示。请参阅图6，ICZO薄膜扫描电镜表面形貌如图6所示。
实施例2-3
选用市售普通钠钙玻璃作为基底，将基片洗净并用N2吹干后置入磁控溅射仪中。基底与靶材表面平行，距离8 cm。靶材为实施例1-3掺铈氧化铟锌靶材In2CexZnO4+2x，制备该靶材所用的三种氧化物摩尔比例为In2O3: CeO2: ZnO =1:2:1。采用40 sccm的纯Ar作为工作气体，工作电流为1.0 A，工作气压为0.7 Pa，在室温进行磁控溅射，溅射时间为28 min，制得250 nm厚的ICZO薄膜，经过Hall测试测得该ICZO薄膜霍尔迁移率达15.6 cm2V-1s-1，载流子浓度为1020 cm-3。将溅射态薄膜放入石英管式炉内退火，在1 Pa真空下退火1 h，退火温度为150ºC到350 ºC，可得载流子浓度在1014 cm-3~1020 cm-3，霍尔迁移率在17.1 cm2V-1s-1~20.6 cm2V-1s-1之间的ICZO薄膜，适合制备TFT器件。请参阅图7，ICZO薄膜载流子浓度及霍尔迁移率随退火温度的变化数据如图7所示。请参阅图8，ICZO薄膜扫描电镜表面形貌如图8所示。
另外，本领域技术人员还可在本发明精神内做其他变化，当然，这些依据本发明精神所做的变化，都应包含在本发明所要求保护的范围之内。

Claims (17)

1.一种氧化物半导体膜，其特征在于，含有铟元素(In)、铈元素(Ce)、锌元素(Zn)及氧元素(O)，该铟元素、铈元素和锌元素的摩尔比为2:(0.5～1.5):1，氧化物半导体膜为n型半导体，载流子浓度为1012cm-3～1020cm-3，载流子迁移率为5.0cm2V-1s-1～45.0cm2V-1s-1。
2.如权利要求1所述的氧化物半导体膜，其特征在于，该氧化物半导体膜的材料为非晶态氧化物。
3.如权利要求1所述的氧化物半导体膜，其特征在于，该氧化物半导体膜的禁带宽度为3.0eV～3.5eV。
4.如权利要求1所述的氧化物半导体膜，其特征在于，该氧化物半导体膜的载流子浓度为1013cm-3～1015cm-3。
5.如权利要求1所述的氧化物半导体膜，其特征在于，该氧化物半导体膜的透过率为60％～90％。
6.如权利要求1所述的氧化物半导体膜，其特征在于，该氧化物半导体膜的厚度50nm为1000nm。
7.一种氧化物半导体膜的制备方法，其特征在于，包括使用一溅射靶，通过溅射法在基底上溅射形成氧化物膜的步骤，该溅射靶含有化合物In2CexZnO4+2x，其中x＝0.5～1.5。
8.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，该溅射靶由氧化铟(In2O3)、氧化铈(CeO2)及氧化锌(ZnO)混合后烧结形成。
9.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，该溅射法为直流溅射法或交流溅射法，该交流溅射法为中频磁控溅射法或射频磁控溅射法。
10.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，该溅射的温度为常温溅射。
11.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，进一步包括在溅射前将该基底在真空中预热的步骤，预热温度为50℃～400℃。
12.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，该溅射法中使用的载气为稀有气体、稀有气体与氧气的混合气或稀有气体与氢气的混合气。
13.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，该溅射时溅射室内的压力为0.1Pa～2.0Pa。
14.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，该基底的材料为玻璃、硅或聚合物。
15.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，在进行溅射前，进一步包括对基底进行清洁的步骤，以去除基底表面的杂质。
16.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，该基底与该溅射靶相互平行或呈一夹角，该夹角为20°～85°之间，该基底与该溅射靶之间的距离小于或等于8cm。
17.如权利要求7所述的氧化物半导体膜的制备方法，其特征在于，进一步包括将该氧化物膜在真空、氮气或Ar气中退火的步骤，退火温度为100℃～400℃，升温速率为1℃/min～20℃/min，退火时间为1小时～10小时。
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