CN112094103A - 一种大尺寸钕铝铟锌氧化物平面靶材及其制备方法 - Google Patents
一种大尺寸钕铝铟锌氧化物平面靶材及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种大尺寸钕铝铟锌氧化物平面靶材制备方法,其特征在于,包括如下步骤:S1、将氧化钕、氧化铝、氧化铟和氧化锌粉末混合研磨制浆得到混合浆料,用混合浆料进行喷雾造粒得到造粒粉;S2、将步骤S1所得的造粒粉依次进行模压和等静压成型得到靶材素坯;S3、将步骤S2得到的靶材素坯进行烧结得到烧结坯;其中,烧结包括:脱脂、烧成和降温三个阶段;S4、将步骤S3得到的烧结坯经机械加工和邦定得到大尺寸钕铝铟锌氧化物平面靶材;本发明还公开了一种大尺寸钕铝铟锌氧化物平面靶材。本发明采用模压和等静压成型工艺得到靶材素坯,采用脱脂、烧成和降温三个阶段烧结工艺,控制合理的烧结条件,提高了靶材均匀度,提高了大尺寸靶材的成品率。
Description
技术领域
本发明属于磁控溅射技术领域,尤其涉及一种大尺寸钕铝铟锌氧化物平面靶材及其制备方法。
背景技术
薄膜晶体管(Thin Film Transistor,简称TFT),是一种用途广泛的半导体器件,其最重要的用途是在显示器中用于驱动液晶排列变化、以及驱动OLED像素发光,从而实现图形的显示和快速响应。相对于目前主流的a-Si TFT(非晶硅)、LTPS TFT(低温多晶硅)工艺,近年来,金属氧化物TFT(简称,MOS TFT)具有迁移率高、均匀性好、透明度佳、工艺简单等优点,得到了广泛的研究和快速的发展,并已开始市场应用。目前,研究用于MOS TFT有源层的材料大多为基于氧化铟或氧化锌(In2O3、ZnO或IZO)掺杂的氧化物半导体材料。In2O3、ZnO或IZO都具有较高的载流子浓度,因而具备较强的电荷传输能力,可以有效驱动TFT器件工作,有利于以低温或室温工艺实现高性能的MOS TFT。但是,其过高的载流子浓度也会带来器件稳定性差和关态电流难以抑制的问题。针对此问题,行业中最主流的方式是通过稀土元素的掺杂实现对载流子浓度的抑制,目前应用较为广泛并已实现市场应用的是镓(Ga)元素掺杂工艺,即IGZO TFT。然而,Ga元素的掺入也使载流子的迁移率大幅降低,在仅采用低温或室温工艺的情况下难以制造出更高性能的MOS TFT,制约了在工艺温度有限的柔性显示器件方面的应用和发展。
发明内容
基于背景技术所述技术问题,本发明提供了一种大尺寸钕铝铟锌氧化物平面靶材制备方法,以氧化钕、氧化铝、氧化铟和氧化锌粉末为原料,采用模压和等静压成型工艺得到靶材素坯,采用脱脂、烧成和降温三个阶段烧结工艺,控制合理的烧结条件,提高了靶材均匀度,提高了大尺寸靶材的成品率。
本发明提出的一种大尺寸钕铝铟锌氧化物平面靶材制备方法,包括如下步骤:
S1、将氧化钕、氧化铝、氧化铟和氧化锌混合研磨制浆得到混合浆料,用混合浆料进行喷雾造粒得到造粒粉;
S2、将步骤S1所得的造粒粉依次进行模压和等静压成型得到靶材素坯;
S3、将步骤S2得到的靶材素坯进行烧结得到烧结坯;其中,烧结包括:脱脂、烧成和降温三个阶段;
S4、将步骤S3得到的烧结坯经机械加工和邦定得到大尺寸钕铝铟锌氧化物平面靶材。
优选地,步骤S1中,氧化钕、氧化铝、氧化铟和氧化锌的质量比0.1-5:0-5:50-95:5-50。
优选地,步骤S1中,氧化钕、氧化铝、氧化铟和氧化锌的纯度为99.99%及以上。
优选地,步骤S1中,混合浆料的粒径D50为0.1-1μm。
优选地,步骤S1中,造粒粉的粒径D50为5-60μm。
优选地,步骤S2中,模压的压力为20-60MPa,等静压的压力为100-500MPa。
优选地,步骤S2中,模压的时间为30-60s,等静压的时间为120-480s。
优选地,步骤S3中,脱脂阶段为:在空气气氛中,以0.2-0.8℃/min的升温速度升温至500℃,保温6-12小时。
优选地,步骤S3中,烧成阶段为:在氧气气氛中,以0.2-0.8℃/min的升温速度升温至1000℃,保温3-8小时;再以1.5-2.5℃/min的升温速度升温至1450-1550℃,保温5-12小时。
优选地,氧气纯度为99.5%。
优选地,步骤S3中,降温阶段为:在惰性气体气氛中,以1.0-1.5℃/min的降温速度降至500℃;停止通入惰性气体,以1.0-1.5℃/min的降温速度降至室温。
本发明还提供了一种大尺寸钕铝铟锌氧化物平面靶材,采用所述大尺寸钕铝铟锌氧化物平面靶材制备方法制得。
本发明中以氧化钕、氧化铝、氧化铟和氧化锌为原料,先以混合球磨制浆和喷雾造粒获得成分均匀的造粒粉,然后采用模压和等静压成型工艺得到大尺寸、低缺陷的靶材素坯,采用脱脂、烧成和降温三个阶段烧结工艺,控制合理的烧结条件,获得高密度的靶材,并提高了靶材均匀度,提高了大尺寸靶材的成品率。
附图说明
图1为本发明的工艺流程图。
具体实施方式
下面结合具体实例对本发明做出详细说明,应当了解,实施例只用于说明本发明,而不是用于对本发明进行限定,任何在本发明基础上所做的修改、等同替换等均在本发明的保护范围内。
实施例1
一种大尺寸钕铝铟锌氧化物平面靶材制备方法,包括如下步骤:
S1、将18.8g氧化钕、28.2g氧化铝、4183g氧化铟和470g氧化锌混合研磨制浆得到粒径D50为0.56μm的混合浆料,用混合浆料进行喷雾造粒得到粒径D50为21.3μm的造粒粉;其中,氧化钕、氧化铝、氧化铟和氧化锌的纯度均为99.99%,粒径D50分别为0.35μm、0.22μm、0.52μm、0.75μm;
S2、将步骤S1所得的造粒粉在30MPa压力下模压30s,然后在180MPa压力下等静压120s,成型得到靶材素坯;
S3、将步骤S2得到的靶材素坯进行烧结得到烧结坯;具体烧结过程包括:
脱脂阶段:在空气气氛中,以0.3℃/min的升温速度升温至500℃,保温6小时;
烧成阶段:在氧气气氛中,以0.5℃/min的升温速度升温至1000℃,保温6小时;再以2.0℃/min的升温速度升温至1480℃,保温8小时;
降温阶段:在惰性气体气氛中,以1.5℃/min的降温速度降至500℃,停止通入惰性气体,以1.5℃/min的降温速度降至室温;
S4、将步骤S3得到的烧结坯经机械加工至目标尺寸,经抛光和清洗后,与靶材背板邦定,获得尺寸为φ300*6mm的钕铝铟锌氧化物平面靶材。
实施例1所得钕铝铟锌氧化物平面靶材的相对密度为99.75%。
实施例2
一种大尺寸钕铝铟锌氧化物平面靶材制备方法,包括如下步骤:
S1、将118g氧化钕、177g氧化铝、26255g氧化铟和2950g氧化锌混合研磨制浆得到粒径D50为0.52μm的混合浆料,用混合浆料进行喷雾造粒得到粒径D50为25.8μm的造粒粉;其中,氧化钕、氧化铝、氧化铟和氧化锌的纯度均为99.996%,粒径D50分别为0.35μm、0.25μm、0.42μm、0.34μm;
S2、将步骤S1所得的造粒粉在45MPa压力下模压60s,然后在450MPa压力下等静压480s,成型得到靶材素坯;
S3、将步骤S2得到的靶材素坯进行烧结得到烧结坯;具体烧结过程包括:
脱脂阶段:在空气气氛中,以0.25℃/min的升温速度升温至500℃,保温8小时;
烧成阶段:在氧气气氛中,以0.4℃/min的升温速度升温至1000℃,保温8小时;再1.2℃/min的升温速度升温至1525℃,保温12小时;
降温阶段:在惰性气体气氛中,以1.0℃/min的降温速度降至500℃,停止通入惰性气体,以1.0℃/min的降温速度降至室温;
S4、将步骤S3得到的烧结坯经机械加工得到840*360*10mm尺寸,经抛光和清洗后,与靶材背板邦定,获得大尺寸钕铝铟锌氧化物平面靶材。
实施例2所得钕铝铟锌氧化物平面靶材的相对密度为99.85%,可满足G5.5TFT平面靶材要求。
实施例3
一种大尺寸钕铟锌氧化物平面靶材制备方法,包括如下步骤:
S1、将172g氧化钕、10750氧化铟和6278g氧化锌混合研磨制浆得到粒径D50为0.45μm的混合浆料,用混合浆料进行喷雾造粒得到粒径D50为18.3μm的造粒粉;其中,氧化钕、氧化铟和氧化锌的纯度均为99.998%,粒径D50分别为0.25μm、0.35μm、0.65μm;
S2、将步骤S1所得的造粒粉在40MPa压力下模压30s,然后在350MPa压力下等静压300s,成型得到靶材素坯;
S3、将步骤S2得到的靶材素坯进行烧结得到烧结坯;具体烧结过程包括:
脱脂阶段:在空气气氛中,以0.3℃/min的升温速度升温至500℃,保温10小时;
烧成阶段:在氧气气氛中,以0.5℃/min的升温速度升温至1000℃,保温8小时;再1.5℃/min的升温速度升温至1520℃,保温10小时;
降温阶段:在惰性气体气氛中,以1.2℃/min的降温速度降至500℃,停止通入惰性气体,以1.2℃/min的降温速度降至室温;
S4、将步骤S3得到的烧结坯经机械加工得到1002*212*8mm尺寸,经抛光和清洗后,与靶材背板邦定,获得大尺寸钕铟锌氧化物平面靶材。
实施例3所得大尺寸钕铟锌氧化物平面靶材的相对密度99.75%,可满足G8.5 TFT平面靶材要求。
对照例1
一种大尺寸钕铝铟锌氧化物平面靶材制备方法,包括如下步骤:
S1、将118g氧化钕、177g氧化铝、26255g氧化铟和2950g氧化锌混合研磨制浆得到粒径D50为0.35μm的混合浆料,用混合浆料进行喷雾造粒得到粒径D50为25.8μm的造粒粉;其中,氧化钕、氧化铝、氧化铟和氧化锌的纯度均为99.996%,粒径D50分别为0.35μm、0.25μm、0.42μm、0.34μm;
S2、将步骤S1所得的造粒粉在20MPa压力下模压60s,然后在160MPa压力下等静压480s,成型得到靶材素坯;
S3、将步骤S2得到的靶材素坯进行烧结得到烧结坯;具体烧结过程包括:
脱脂阶段:在空气气氛中,以0.25℃/min的升温速度升温至500℃,保温6小时;
烧成阶段:在氧气气氛中,以1.0℃/min的升温速度升温至1000℃,保温8小时;再0.8℃/min的升温速度升温至1525℃,保温12小时;
降温阶段:在惰性气体气氛中,以1.0℃/min的降温速度降至500℃,停止通入惰性气体,以1.0℃/min的降温速度降至室温;
S4、将步骤S3得到的烧结坯经机械加工得到840*360*10mm尺寸,并检测靶材指标。
对照例1所得钕铝铟锌氧化物平面靶材的相对密度为98.62%,不能满足TFT平面靶材要求。
对照例2
一种大尺寸钕铝铟锌氧化物平面靶材制备方法,包括如下步骤:
S1、将118g氧化钕、177g氧化铝、26255g氧化铟和2950g氧化锌混合研磨制浆得到粒径D50为0.35μm的混合浆料,用混合浆料进行喷雾造粒得到粒径D50为25.8μm的造粒粉;其中,氧化钕、氧化铝、氧化铟和氧化锌的纯度均为99.996%,粒径D50分别为0.35μm、0.25μm、0.42μm、0.34μm;
S2、将步骤S1所得的造粒粉在45MPa压力下模压60s,然后在450MPa压力下等静压480s,成型得到靶材素坯;
S3、将步骤S2得到的靶材素坯进行烧结得到烧结坯;具体烧结过程包括:
脱脂阶段:在空气气氛中,以0.25℃/min的升温速度升温至500℃,保温6小时;
烧成阶段:在氧气气氛中,以1.0℃/min的升温速度升温至1000℃,保温8小时;再0.8℃/min的升温速度升温至1525℃,保温12小时;
降温阶段:停止通气,以1.0℃/min的降温速度降至室温;
S4、将步骤S3得到的烧结坯经机械加工得到840*360*10mm尺寸,并检测靶材指标。
对照例2所得钕铝铟锌氧化物平面靶材的相对密度为98.86%,不能满足TFT平面靶材要求。
本发明具体实施例中,氧气气氛中氧气的纯度为99.5%。
本发明中相对密度的是指阿基米德排水法测算密度与其确定组分的理论密度之比的百分值。某确定组分的理论密度则是根据组分中四种氧化物的质量比以及其各自的理论密度计算得出。具体而言,In2O3的理论密度为7.18g/cm3、ZnO的理论密度为5.61g/cm3、Al2O3的单体密度为3.97g/cm3、Nd2O3的单体密度为7.24g/cm3,假若In2O3所占质量比为MIn2O3、ZnO所占质量比为MZnO、Al2O3所占质量比为MAl2O3、Nd2O3所占质量比为MNd2O3,则该特定组分的理论密度=(7.18*MIn2O3+5.61*MZnO+3.97*MAl2O3+7.24*MNd2O3)/100,单位为g/cm3。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之。
Claims (10)
1.一种大尺寸钕铝铟锌氧化物平面靶材制备方法,其特征在于,包括如下步骤:
S1、将氧化钕、氧化铝、氧化铟和氧化锌混合研磨制浆得到混合浆料,用混合浆料进行喷雾造粒得到造粒粉;
S2、将步骤S1所得的造粒粉依次进行模压和等静压成型得到靶材素坯;
S3、将步骤S2得到的靶材素坯进行烧结得到烧结坯;其中,烧结包括:脱脂、烧成和降温三个阶段;
S4、将步骤S3得到的烧结坯经机械加工和邦定得到大尺寸钕铝铟锌氧化物平面靶材。
2.根据权利要求1所述的大尺寸钕铝铟锌氧化物平面靶材制备方法,其特征在于,步骤S1中,氧化钕、氧化铝、氧化铟和氧化锌的质量比0.1-5:0-5:50-95:5-50。
3.根据权利要求1或2所述的大尺寸钕铝铟锌氧化物平面靶材制备方法,其特征在于,步骤S1中,混合浆料的粒径D50为0.1-1μm。
4.根据权利要求1-3中任一项所述的大尺寸钕铝铟锌氧化物平面靶材制备方法,优选地,步骤S1中,造粒粉的粒径D50为5-60μm。
5.根据权利要求1-4中任一项所述的大尺寸钕铝铟锌氧化物平面靶材制备方法,其特征在于,步骤S2中,模压的压力为25-60MPa,等静压的压力为180-450MPa。
6.根据权利要求1-5中任一项所述的大尺寸钕铝铟锌氧化物平面靶材制备方法,其特征在于,步骤S2中,模压的时间为30-60s,等静压的时间为120-480s。
7.根据权利要求1-6中任一项所述的大尺寸钕铝铟锌氧化物平面靶材制备方法,其特征在于,脱脂阶段为:在空气气氛中,以0.2-0.8℃/min的升温速度升温至500℃,保温6-12小时。
8.根据权利要求1-7中任一项所述的大尺寸钕铝铟锌氧化物平面靶材制备方法,其特征在于,烧成阶段为:在氧气气氛中,以0.2-0.8℃/min的升温速度升温至1000℃,保温3-8小时;再以1.5-2.5℃/min的升温速度升温至1450-1550℃,保温5-12小时。
9.根据权利要求1-8中任一项所述的大尺寸钕铝铟锌氧化物平面靶材制备方法,其特征在于,降温阶段为:在惰性气体气氛中,以1.0-1.5℃/min的降温速度降至500℃;停止通入惰性气体,以1.0-1.5℃/min的降温速度降至室温。
10.一种大尺寸钕铝铟锌氧化物平面靶材,其特征在于,采用权利要求1-9中任一项所述的大尺寸钕铝铟锌氧化物平面靶材制备方法制得。
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