CN112079626A - 一种铝钕铟锌氧化物旋转靶及其制备方法 - Google Patents

一种铝钕铟锌氧化物旋转靶及其制备方法 Download PDF

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CN112079626A
CN112079626A CN202010971405.5A CN202010971405A CN112079626A CN 112079626 A CN112079626 A CN 112079626A CN 202010971405 A CN202010971405 A CN 202010971405A CN 112079626 A CN112079626 A CN 112079626A
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文宏福
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Shaoguan Oulai Hi Tech Material Co ltd
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Abstract

本发明公开了一种铝钕铟锌氧化物旋转靶的制备方法，包括如下步骤：S1、将氧化铝、氧化钕、氧化铟、氧化锌加入水、粘结剂搅拌均匀、砂磨得到浆料；S2、将步骤S1所得浆料喷雾干燥得到造粒粉；S3、将步骤S2所得造粒粉冷等静压成型，得到旋转靶素坯；S4、将旋转靶素坯精修后脱脂烧结得到烧结坯；S5、将烧结坯与金属背管邦定得到铝钕铟锌氧化物旋转靶；本发明公开了一种铝钕铟锌氧化物旋转靶。本发明制得的旋转靶具有纯度高，密度高，晶粒小的优点，用于G2.5‑G11代线金属氧化物TFT‑LCD及TFT‑OLED。

Description

一种铝钕铟锌氧化物旋转靶及其制备方法
技术领域
本发明属于磁控溅射技术领域，尤其涉及一种铝钕铟锌氧化物旋转靶及其制备方法。
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，其目前主要应用在液晶显示(LCD)中以驱动液晶排列变化、以及驱动有机发光显示(OLED)像素发光。现在的TFT材料主要有非晶硅、多晶硅以及金属氧化物三类。其中非晶硅TFT具有对光敏感、迁移率低和稳定性差的缺点；多晶硅TFT虽然有较高的迁移率，但是由于晶界导致其电学均匀性差，另外多晶硅制备温度高以及生产成本较高，限制了其在平面显示中的应用，金属氧化物TFT具有迁移率高、均匀性好、透明度佳、工艺简单等优点，在近年得到了广泛的研究和快速的发展。
目前，用于制作金属氧化物TFT有源层的材料大多为基于氧化铟、氧化锌及两者混合(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，有利于在低温或室温工艺实现高性能金属氧化物TFT。然而过高的载流子浓度也会带来器件稳定性差和闭态电流难以抑制的问题。为了解决这个问题，行业中主流的方式是通过掺杂其他元素来对载流子浓度进行一定的抑制，其中以日本东京工业大学细野秀雄先生提出的镓(Ga)掺杂技术，即铟镓锌氧化物(IGZO)，的研究和应用最为广泛。然而，Ga元素的掺入使得载流子的迁移率降低幅度过高，在低温或室温工艺的情况下很难实现更高性能的金属氧化物TFT，这不利于工艺温度有限的柔性显示器件实现更高性能的发展。
为了克服IGZO上述缺陷，同时也为发展中国自主知识产权、保护国家平面显示超级市场，国内很多院校、企业和研究机构都将研究重点放在新一代金属氧化物TFT的研究上来。其中华南理工大学的彭俊彪先生等(CN 102110718 A)公布了一种铝钕铟锌氧化物TFT的制备技术，按此技术制备的铝钕铟锌氧化物TFT具有工艺简单、制备温度低、迁移率高、电学稳定性好等优点，是一种非常有潜力的金属氧化物TFT技术。
要实现大规模量产制作铝钕铟锌氧化物有源层TFT，需要用到关键性材料---大尺寸、高质量铝钕铟锌氧化物靶材。根据镀膜厂商使用的镀膜机组不同，磁控溅射靶材又分为平面靶材和旋转靶材两种。相比传统的平面靶材，旋转靶材具有利用率高，镀膜连续性好，镀膜成分均匀等优势。目前国内在铝钕铟锌氧化物靶材还处在实验室研究阶段，未见有可大规模量产、大尺寸、高质量旋转靶材的报导。
发明内容
基于背景技术所述技术问题，本发明提供了一种铝钕铟锌氧化物旋转靶的制备方法，制得的旋转靶具有纯度高，密度高，晶粒小的优点，用于G2.5-G11代线金属氧化物TFT-LCD及TFT-OLED。
本发明中一种铝钕铟锌氧化物旋转靶的制备方法，包括如下步骤：
S1、将氧化铝、氧化钕、氧化铟、氧化锌加入水、粘结剂搅拌均匀、砂磨得到浆料；
S2、将步骤S1所得浆料喷雾干燥得到造粒粉；
S3、将步骤S2所得造粒粉冷等静压成型，冷等静压的升压速率为10-30Mpa/min，最大压力为200-450Mpa，保压时间为10-30min，降压速率为30-60Mpa/min，得到旋转靶素坯；
S4、将旋转靶素坯精修后脱脂烧结得到烧结坯；
S5、将烧结坯与金属背管邦定得到铝钕铟锌氧化物旋转靶。
优选地，步骤S1中，氧化铝、氧化钕、氧化铟、氧化锌总量中，氧化铝所占的质量分数为x％,氧化钕所占的质量分数为y％,氧化铟所占的质量分数为z％，氧化锌所占的质量分数为(100-x-y-z)％,其中，0≤x＜10，0＜x＜10，0＜z<100。
优选地，步骤S1中，氧化铝、氧化钕、氧化铟、氧化锌均为4N粉末，粒径D50为0.1-1.0μm，比表面积BET为5-30m2/g。
优选地，步骤S1中，浆料的粒径D50小于0.5μm。
优选地，步骤S2中，造粒粉的粒径D50为20-50μm。
优选地，步骤S3中，旋转靶素坯的相对密度为55-65％。
优选地，步骤S4中，脱脂烧结的脱脂温度为500-600℃，升温速率为0.5-1.0℃/min，保温时间为4-8h，烧结气氛为空气，烧成温度为1400-1600℃，升温速率为1.0-2.0℃/min，保温时间为12-24h，烧结气氛为氧气。
优选地，步骤S4中，烧结坯的相对密度为99.0-99.7％。
优选地，烧结坯在邦定前还进行了内外圆研磨和端面加工。
本发明工艺还包括对铝钕铟锌氧化物旋转靶进行检测和包装。
本发明中靶材的相对密度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的理论密度为3.97g/cm3、Nd2O3的理论密度为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。
本发明制得铝钕铟锌氧化物旋转靶材纯度>99.99％,相对密度>99.0％，靶材的平均晶粒尺寸<10μm，具有纯度高，密度高，晶粒小的优点，单节管状靶材尺寸可达OD153*ID135*L400mm及以上，可用于G2.5-G11代线金属氧化物TFT-LCD及TFT-OLED。
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
一种铝钕铟锌氧化物旋转靶的制备方法，包括如下步骤：
S1、将0.05kg氧化铝粉末、0.45kg氧化钕粉末、31.25kg氧化铟粉末、18.25kg氧化锌粉末加入50kg纯水及3Kg聚乙烯醇类粘结剂搅拌均匀、砂磨，当检测浆料的粒度D50为0.47μm时停止砂磨得到浆料；
S2、将步骤S1所得浆料喷雾干燥得到造粒粉，检测造粒粉的粒度D50为32.6μm；
S3、将步骤S2所得造粒粉冷等静压成型，冷等静压的升压速率为24Mpa/min，最大压力为350Mpa，保压时间为15min，降压速率为58Mpa/min，得到旋转靶素坯；旋转靶素坯的相对密度为62.1％；
S4、将旋转靶素坯精修后脱脂烧结得到烧结坯；脱脂烧结的脱脂温度为500℃，升温速率为0.5℃/min，保温时间为6h，烧结气氛为空气，烧成温度为1450℃，升温速率为1.6℃/min，保温时间为15h，烧结气氛为氧气；烧结坯的相对密度为99.17％；
S5、将烧结坯做内外圆研磨及端面加工，制得尺寸为OD153*ID135*L400mm的单节管状靶材，与金属背管邦定，并做检测包装得到铝钕铟锌氧化物旋转靶。
实施例1制取的烧结坯样品的杂质分析结果如下表：
元素 Fe Si Na Ni Cu Pb Sn Cr
含量(ppm) 9 7 5 2 2 3 5 2
实施例1制取的靶材样品扫描电子显微镜(SEM)检测发现其平均晶粒尺寸为7.3μm。
实施例2
一种铝钕铟锌氧化物旋转靶的制备方法，包括如下步骤：
S1、将0.05kg氧化铝粉末、0.45kg氧化钕粉末、31.25kg氧化铟粉末、18.25kg氧化锌粉末加入50kg纯水及3Kg聚乙烯醇类粘结剂搅拌均匀、砂磨，当检测浆料的粒度D50为0.47μm时停止砂磨得到浆料；
S2、将步骤S1所得浆料喷雾干燥得到造粒粉，检测造粒粉的粒度D50为32.6μm；
S3、将步骤S2所得造粒粉冷等静压成型，冷等静压的升压速率为24Mpa/min，最大压力为420Mpa，保压时间为15min，降压速率为58Mpa/min，得到旋转靶素坯；旋转靶素坯的相对密度为62.5％；
S4、将旋转靶素坯精修后脱脂烧结得到烧结坯；脱脂烧结的脱脂温度为500℃，升温速率为0.5℃/min，保温时间为6h，烧结气氛为空气，烧成温度为1500℃，升温速率为1.6℃/min，保温时间为15h，烧结气氛为氧气。；烧结坯的相对密度为99.29％；
S5、将烧结坯做内外圆研磨及端面加工，制得尺寸为OD153*ID135*L400mm的单节管状靶材，与金属背管邦定，并做检测包装得到铝钕铟锌氧化物旋转靶。
实施例2制取的烧结坯样品的杂质分析结果如下表：
元素 Fe Si Na Ni Cu Pb Sn Cr
含量(ppm) 11 6 4 2 1 3 4 2
实施例2制取的靶材样品SEM检测结果显示其平均晶粒尺寸为7.1μm。
实施例3
一种铝钕铟锌氧化物旋转靶的制备方法，包括如下步骤：
S1、将0.55kg氧化铝粉末、0.35kg氧化钕粉末、30.95kg氧化铟粉末、18.15kg氧化锌粉末加入50kg纯水及3Kg聚乙烯醇类粘结剂搅拌均匀、砂磨，当检测浆料的粒度D50为0.43μm时停止砂磨得到浆料；
S2、将步骤S1所得浆料喷雾干燥得到造粒粉，检测造粒粉的粒度D50为31.7μm；
S3、将步骤S2所得造粒粉冷等静压成型，冷等静压的升压速率为24Mpa/min，最大压力为420Mpa，保压时间为15min，降压速率为58Mpa/min，得到旋转靶素坯；旋转靶素坯的相对密度为62.3％；
S4、将旋转靶素坯精修后脱脂烧结得到烧结坯；脱脂烧结的脱脂温度为500℃，升温速率为0.5℃/min，保温时间为6h，烧结气氛为空气，烧成温度为1500℃，升温速率为1.6℃/min，保温时间为15h，烧结气氛为氧气；烧结坯的相对密度为99.31％；
S5、将烧结坯做内外圆研磨及端面加工，制得尺寸为OD153*ID135*L400mm的单节管状靶材，与金属背管邦定，并做检测包装得到铝钕铟锌氧化物旋转靶。
实施例3制取的烧结坯样品的杂质分析结果如下表：
元素 Fe Si Na Ni Cu Pb Sn Cr
含量(ppm) 10 6 3 2 2 4 4 1
实施例3制取的靶材样品SEM检测结果显示其平均晶粒尺寸为7.2μm。
实施例4
一种铝钕铟锌氧化物旋转靶的制备方法，包括如下步骤：
S1、将0.55kg氧化铝粉末、0.35kg氧化钕粉末、30.95 kg氧化铟粉末、18.15kg氧化锌粉末加入50kg纯水及3Kg聚乙烯醇类粘结剂搅拌均匀、砂磨，当检测浆料的粒度D50为0.43μm时停止砂磨得到浆料；
S2、将步骤S1所得浆料喷雾干燥得到造粒粉，检测造粒粉的粒度D50为31.7μm；
S3、将步骤S2所得造粒粉冷等静压成型，冷等静压的升压速率为24Mpa/min，最大压力为420Mpa，保压时间为15min，降压速率为58Mpa/min，得到旋转靶素坯；旋转靶素坯的相对密度为62.3％；
S4、将旋转靶素坯精修后脱脂烧结得到烧结坯；脱脂烧结的脱脂温度为500℃，升温速率为0.5℃/min，保温时间为6h，烧结气氛为空气，烧成温度为1550℃，升温速率为1.6℃/min，保温时间为15h，烧结气氛为氧气；烧结坯的相对密度为99.32％；
S5、将烧结坯做内外圆研磨及端面加工，制得尺寸为OD153*ID135*L400mm的单节管状靶材，与金属背管邦定，并做检测包装得到铝钕铟锌氧化物旋转靶。
实施例4制取的烧结坯样品的杂质分析结果如下表：
元素 Fe Si Na Ni Cu Pb Sn Cr
含量(ppm) 8 7 4 2 2 3 3 2
实施例4制取的靶材样品SEM检测结果显示其平均晶粒尺寸为7.4μm。
实施例5
一种铝钕铟锌氧化物旋转靶的制备方法，包括如下步骤：
S1、将0.32kg氧化铝粉末、0.2kg氧化钕粉末、44.46kg氧化铟粉末、5.02kg氧化锌粉末加入50kg纯水及3Kg聚乙烯醇类粘结剂搅拌均匀、砂磨，当检测浆料的粒度D50为0.46μm时停止砂磨得到浆料；
S2、将步骤S1所得浆料喷雾干燥得到造粒粉，检测造粒粉的粒度D50为34.1μm；
S3、将步骤S2所得造粒粉冷等静压成型，冷等静压的升压速率为24Mpa/min，最大压力为420Mpa，保压时间为15min，降压速率为58Mpa/min，得到旋转靶素坯；旋转靶素坯的相对密度为62.4％；
S4、将旋转靶素坯精修后脱脂烧结得到烧结坯；脱脂烧结的脱脂温度为500℃，升温速率为0.5℃/min，保温时间为6h，烧结气氛为空气，烧成温度为1500℃，升温速率为1.6℃/min，保温时间为15h，烧结气氛为氧气；烧结坯的相对密度为99.43％；
S5、将烧结坯做内外圆研磨及端面加工，制得尺寸为OD153*ID135*L400mm的单节管状靶材，与金属背管邦定，并做检测包装得到铝钕铟锌氧化物旋转靶。
实施例5制取的烧结坯样品的杂质分析结果如下表：
元素 Fe Si Na Ni Cu Pb Sn Cr
含量(ppm) 10 6 4 2 2 2 4 1
实施例5制取的靶材样品SEM检测结果显示其平均晶粒尺寸为7.1μm。
实施例6
一种铝钕铟锌氧化物旋转靶的制备方法，包括如下步骤：
S1、将0.32kg氧化铝粉末、0.2kg氧化钕粉末、44.46kg氧化铟粉末、5.02kg氧化锌粉末加入50kg纯水及3Kg聚乙烯醇类粘结剂搅拌均匀、砂磨，当检测浆料的粒度D50为0.46μm时停止砂磨得到浆料；
S2、将步骤S1所得浆料喷雾干燥得到造粒粉，检测造粒粉的粒度D50为34.1μm；
S3、将步骤S2所得造粒粉冷等静压成型，冷等静压的升压速率为24Mpa/min，最大压力为420Mpa，保压时间为15min，降压速率为58Mpa/min，得到旋转靶素坯；旋转靶素坯的相对密度为62.4％；
S4、将旋转靶素坯精修后脱脂烧结得到烧结坯；脱脂烧结的脱脂温度为500℃，升温速率为0.5℃/min，保温时间为6h，烧结气氛为空气，烧成温度为1600℃，升温速率为1.6℃/min，保温时间为15h，烧结气氛为氧气；烧结坯的相对密度为99.61％；
S5、将烧结坯做内外圆研磨及端面加工，制得尺寸为OD153*ID135*L400mm的单节管状靶材，与金属背管邦定，并做检测包装得到铝钕铟锌氧化物旋转靶。
实施例6制取的烧结坯样品的杂质分析结果如下表：
元素 Fe Si Na Ni Cu Pb Sn Cr
含量(ppm) 9 6 5 1 1 3 3 1
实施例6制取的靶材样品SEM检测结果显示其平均晶粒尺寸为7.7μm。
本发明具体实施例中使用的是氧化铝粉末、氧化钕粉末、氧化铟粉末、氧化锌粉末均为4N的高纯度粉末。
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内。

Claims (9)

1.一种铝钕铟锌氧化物旋转靶的制备方法，其特征在于，包括如下步骤：
S1、将氧化铝、氧化钕、氧化铟、氧化锌加入水、粘结剂搅拌均匀、砂磨得到浆料；
S2、将步骤S1所得浆料喷雾干燥得到造粒粉；
S3、将步骤S2所得造粒粉冷等静压成型，冷等静压的升压速率为10-30Mpa/min，最大压力为200-450Mpa，保压时间为10-30min，降压速率为30-60Mpa/min，得到旋转靶素坯；
S4、将旋转靶素坯精修后脱脂烧结得到烧结坯；
S5、将烧结坯与金属背管邦定得到铝钕铟锌氧化物旋转靶。
2.根据权利要求1所述的铝钕铟锌氧化物旋转靶的制备方法，其特征在于，步骤S1中，氧化铝、氧化钕、氧化铟、氧化锌总量中，氧化铝所占的质量分数为x％,氧化钕所占的质量分数为y％,氧化铟所占的质量分数为z％，氧化锌所占的质量分数为(100-x-y-z)％,其中，0≤x＜10，0＜x＜10，0＜z<100。
3.根据权利要求1或2所述的铝钕铟锌氧化物旋转靶的制备方法，其特征在于，步骤S1中，氧化铝、氧化钕、氧化铟、氧化锌均为4N粉末，粒径D50为0.1-1.0μm，比表面积BET为5-30m2/g。
4.根据权利要求1-3中任一项所述的铝钕铟锌氧化物旋转靶的制备方法，其特征在于，步骤S1中，浆料的粒径D50小于0.5μm。
5.根据权利要求1-4中任一项所述的铝钕铟锌氧化物旋转靶的制备方法，其特征在于，步骤S2中，造粒粉的粒径D50为20-50μm。
6.根据权利要求1-5中任一项所述的铝钕铟锌氧化物旋转靶的制备方法，其特征在于，步骤S3中，旋转靶素坯的相对密度为55-65％。
7.根据权利要求1-6中任一项所述的铝钕铟锌氧化物旋转靶的制备方法，其特征在于，步骤S4中，脱脂烧结的脱脂温度为500-600℃，升温速率为0.5-1.0℃/min，保温时间为4-8h，烧结气氛为空气，烧成温度为1400-1600℃，升温速率为1.0-2.0℃/min，保温时间为12-24h，烧结气氛为氧气。
8.根据权利要求1-7中任一项所述的铝钕铟锌氧化物旋转靶的制备方法，其特征在于，步骤S4中，烧结坯的相对密度为99.0-99.7％。
9.一种铝钕铟锌氧化物旋转靶，其特征在于，采用权利要求1-8中任一项所述的铝钕铟锌氧化物旋转靶的制备方法制得。
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112723863A (zh) * 2021-02-01 2021-04-30 韶关市欧莱高纯材料技术有限公司 一种高世代tft级细晶粒ito靶材的制造方法
CN113735567A (zh) * 2021-09-15 2021-12-03 先导薄膜材料（广东）有限公司 一种氧化物平面靶及其制备方法
CN113831141A (zh) * 2021-09-15 2021-12-24 先导薄膜材料（广东）有限公司 一种氧化物旋转靶材及其制备方法
CN116253560A (zh) * 2022-12-15 2023-06-13 先导薄膜材料（广东）有限公司 一种氧化铝靶材及其制备方法

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090139862A1 (en) * 2006-06-02 2009-06-04 Bekaert Advanced Coatings Rotatable sputter target
CN102110718A (zh) * 2010-10-20 2011-06-29 华南理工大学 用于薄膜晶体管的氧化物半导体薄膜及其制备方法
US20120152728A1 (en) * 2010-12-17 2012-06-21 Semiconductor Energy Laboratory Co., Ltd. Sputtering target, method for manufacturing the same, and method for manufacturing semiconductor device
US20140102892A1 (en) * 2011-05-10 2014-04-17 Idemitsu Kosan Co., Ltd. In2o3-zno sputtering target
CN105906338A (zh) * 2016-04-19 2016-08-31 北京冶科纳米科技有限公司 一种高密度igzo旋转靶材的制造方法
CN108336135A (zh) * 2018-03-15 2018-07-27 华南理工大学 一种钕铟锌氧化物薄膜晶体管及其制备方法
CN109071356A (zh) * 2016-04-13 2018-12-21 株式会社钢臂功科研 氧化物烧结体和溅射靶及它们的制造方法
CN111018515A (zh) * 2019-12-26 2020-04-17 广州市尤特新材料有限公司 靶材的制造方法和靶材

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090139862A1 (en) * 2006-06-02 2009-06-04 Bekaert Advanced Coatings Rotatable sputter target
CN101484605A (zh) * 2006-06-02 2009-07-15 贝卡尔特先进涂层公司 可旋转溅射靶
CN102110718A (zh) * 2010-10-20 2011-06-29 华南理工大学 用于薄膜晶体管的氧化物半导体薄膜及其制备方法
US20120152728A1 (en) * 2010-12-17 2012-06-21 Semiconductor Energy Laboratory Co., Ltd. Sputtering target, method for manufacturing the same, and method for manufacturing semiconductor device
US20140102892A1 (en) * 2011-05-10 2014-04-17 Idemitsu Kosan Co., Ltd. In2o3-zno sputtering target
CN109071356A (zh) * 2016-04-13 2018-12-21 株式会社钢臂功科研 氧化物烧结体和溅射靶及它们的制造方法
CN105906338A (zh) * 2016-04-19 2016-08-31 北京冶科纳米科技有限公司 一种高密度igzo旋转靶材的制造方法
CN108336135A (zh) * 2018-03-15 2018-07-27 华南理工大学 一种钕铟锌氧化物薄膜晶体管及其制备方法
CN111018515A (zh) * 2019-12-26 2020-04-17 广州市尤特新材料有限公司 靶材的制造方法和靶材

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张力等: "磁控溅射法制备IGZO薄膜材料技术的研究进展", 《热加工工艺》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112723863A (zh) * 2021-02-01 2021-04-30 韶关市欧莱高纯材料技术有限公司 一种高世代tft级细晶粒ito靶材的制造方法
CN113735567A (zh) * 2021-09-15 2021-12-03 先导薄膜材料（广东）有限公司 一种氧化物平面靶及其制备方法
CN113831141A (zh) * 2021-09-15 2021-12-24 先导薄膜材料（广东）有限公司 一种氧化物旋转靶材及其制备方法
CN116253560A (zh) * 2022-12-15 2023-06-13 先导薄膜材料（广东）有限公司 一种氧化铝靶材及其制备方法
CN116253560B (zh) * 2022-12-15 2024-06-07 先导薄膜材料（广东）有限公司 一种氧化铝靶材及其制备方法

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