CN112390622A - 一种eigzo靶材的制备方法 - Google Patents

一种eigzo靶材的制备方法 Download PDF

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CN112390622A
CN112390622A CN202011326595.1A CN202011326595A CN112390622A CN 112390622 A CN112390622 A CN 112390622A CN 202011326595 A CN202011326595 A CN 202011326595A CN 112390622 A CN112390622 A CN 112390622A
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oxide powder
sintering
eigzo
mixed slurry
zinc oxide
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刘文杰
钟小华
童培云
朱刘
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Vital Thin Film Materials Guangdong Co Ltd
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Abstract

本发明提供了一种EIGZO靶材的制备方法，属于靶材领域。本发明以氧化铟粉末作为基体材料，通过添加氧化铒对半导体内的载流子浓度进行调控，不仅提高了氧化物半导体的稳定性，而且铒离子的掺杂量较低，可保证In的5s电子轨道完整性，确保高迁移率的优势；同时将氧化铟、氧化铒、氧化镓和氧化锌复配，进一步提高氧化物半导体的光稳定性；另外，采用先不通入氧气烧结，再通入氧气烧结的方式，提高了所得EIGZO靶材的相对密度，进一步确保氧化物半导体具有更好的迁移率。

Description

一种EIGZO靶材的制备方法
技术领域
本发明属于靶材领域，具体涉及一种EIGZO靶材的制备方法。
背景技术
磁控溅射技术是制备高性能薄膜材料的重要技术，应用于各种高端电子行业。磁控溅射制备的氧化物薄膜晶体管(TFT)有源层，具有良好的迁移率和稳定性，可满足高分辨LCD、AMOLED、电子纸等高端显示的需求，并且相比于LTPS有源层，具有工艺简单、成本低、均匀性好等优势。但是，目前商用的氧化物半导体的迁移率仍低于LTPS技术，而且靶材依赖进口，核心专利掌握在外国企业手中，原材料自主可控程度低。
氧化物半导体的迁移率与其靶材性能密切相关，如何提高靶材性能成为当今攻克的难题。
发明内容
本发明的目的在于克服现有技术存在的不足之处而提供一种EIGZO靶材的制备方法，所得EIGZO靶材相对密度高，平均晶粒尺寸小，抗弯强度大，由其制得的氧化物半导体的迁移率能达到LTPS技术水平。
为实现上述目的，本发明提供了一种EIGZO靶材的制备方法，包括以下制备步骤：
(1)将氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末、分散剂和水混合，球磨，得到第一混合浆料；
(2)在所述第一混合浆料中加入粘结剂，混匀，得到第二混合浆料；
(3)将所述第二混合浆料进行喷雾干燥，得到EIGZO粉粒；
(4)将所述EIGZO粉粒置于模具中进行压制，得到素坯，再将素坯进行冷等静压；
(5)将经冷等静压处理后的素坯以0.1～0.5℃/min的速率升温至150～400℃进行脱脂烧结；
(6)继续以0.1～0.5℃/min的速率升温至500～1300℃进行烧结；
(7)通入氧气，并继续以0.1～0.5℃/min的速率升温至1300～1580℃进行烧结，冷却，即得所述EIGZO靶材。
上述制备方法以高迁移率氧化物半导体——In203作为基体材料，通过掺杂入少量铒元素对半导体内的载流子浓度进行调控。铒元素和氧的断键能高达700kJ/mol以上，可与氧形成更强的化学键，有助于抑制半导体薄膜中氧空位的产生，控制载流子浓度，提高氧化物半导体的稳定性。同时，较强的氧断键能，可以大大降低铒离子的掺杂量，可保证In的5s电子轨道完整性；在保证稳定性的同时，也确保了高迁移率的优势。另外，通过在能隙中引入光生载流子复合中心(即氧化铟、氧化镓、氧化铒和氧化锌的复合)的设计，进一步提高器件的光稳定性。
同时，上述制备方法采用先不通入氧气烧结，再通入氧气烧结的方式，提高了所得EIGZO靶材的相对密度，进一步确保由EIGZO靶材制得的氧化物半导体具有更好的迁移率。
上述制备方法所得EIGZO靶材，不仅相对密度在99％以上，平均晶粒尺寸为10μm，抗弯强度≥80MPa，而且迁移率和稳定性能达到LTPS技术水平，由其进行镀膜后的器件迁移率>30cm2/(Vs)，分辨率>300PPI，亮度未>700cd/m2，色域>100％。
优选地，以所述氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末的总重量为基准进行计算，所述氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末的质量比为氧化铟：氧化镓：氧化铒：氧化锌＝60～65％:15～20％:3～5％:15～17％。
优选地，所述步骤(6)和步骤(7)中的烧结都为分阶段烧结。烧结过程中，在几个温度下进行保温烧结，就分为几个阶段。分阶段烧结是指两阶段以上的烧结。相比单一阶段的烧结，采用分阶段烧结，有利于提高EIGZO靶材的密度，进而有利于进一步提高氧化物半导体的迁移率。
优选地，所述步骤(6)中的烧结分为4个阶段，相邻两阶段烧结温度相差50～300℃，每阶段保温时间为1～4h。某阶段的烧结温度指的是该阶段的保温烧结温度。
进一步优选地，所述步骤(6)中，第一阶段和第二阶段的烧结温度为600～900℃，第三阶段的烧结温度为1050～1150℃，第四阶段的烧结温度为1250～1300℃。
优选地，所述步骤(7)中的烧结分为4个阶段，相邻两阶段烧结温度相差50～150℃，每阶段保温时间为2～8h。
进一步优选地，所述步骤(7)中，第一至第三阶段的烧结温度为1300～1520℃，第四阶段的烧结温度为1550～1580℃。
优选地，所述步骤(7)中，氧气流量为50～100L/min。
脱脂烧结的时间可以根据脱脂情况进行调整，通常该过程中的保温烧结时间为2～4h。
优选地，所述经冷等静压处理后的素坯的相对密度为50～60％。
优选地，所述步骤(4)中，冷等静压的压力为300～400MPa。
优选地，所述步骤(3)中，喷雾干燥的温度为240-260℃，进料速度600-1000mL/min，EIGZO粉粒粒度小于200微米。
优选地，所述步骤(2)中，粘结剂的重量为第一混合浆料重量的2～3％，第二混合浆料的pH值为9～10。
优选地，所述步骤(2)中，采用搅拌的方式进行混匀。
优选地，所述步骤(2)中，搅拌时间为2～5h。
优选地，所述粘结剂为醇类粘结剂。
优选地，所述步骤(1)中，分散剂的重量为所述氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末的总重量的1-2％，球磨时间为3～10h，第一混合浆料的固含量为60～70％。
相比现有技术，本发明的有益效果在于：本发明以高迁移率氧化物半导体——In203作为基体材料，通过掺杂铒元素对半导体内的载流子浓度进行调控，不仅提高了氧化物半导体的稳定性，而且铒离子的掺杂量较低，可保证In的5s电子轨道完整性，确保高迁移率的优势；同时将氧化铟、氧化铒、氧化镓和氧化锌复配，进一步提高了氧化物半导体的光稳定性；另外，采用先不通入氧气烧结，再通入氧气烧结的方式，提高了所得EIGZO靶材的相对密度，进一步确保氧化物半导体具有更好的迁移率。
具体实施方式
为更好的说明本发明的目的、技术方案和优点，下面将结合具体实施例对本发明作进一步说明。
实施例1
本实施例提供了本发明EIGZO靶材的制备方法的一种实施例。本实施例EIGZO靶材的制备方法包括以下步骤：
(1)将氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末、分散剂和水混合，球磨4h，得到固含量60％、粒径D50<0.5μm且粒径正态分布半峰宽<0.5的第一混合浆料，其中分散剂的重量为氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末总重量的1％，氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末的质量比为氧化铟：氧化镓：氧化铒：氧化锌＝60％：20％：3％：17％(以氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末的总重量为基准进行计算，下同)；
(2)加入第一混合浆料重量2％的醇类粘结剂，搅拌2h，得到pH值为10.46的第二混合浆料；
(3)将第二混合浆料进行喷雾干燥，得到粒粒度小于200微米的EIGZO粉粒，其中，喷雾干燥的温度为240℃，进料速度600mL/min；
(4)将EIGZO粉粒置于模具中，在50MPa下压制得到素坯，再将素坯在350MPa下冷等静压，得到相对密度为50.3％的素坯；
(5)将相对密度为50.3％的素坯以0.25℃/min的速率升温至400℃，保温4h，以进行脱脂烧结；
(6)继续以0.25℃/min的速率升温至600℃、800℃、1100℃、1250℃，各保温2h(即分别以0.25℃/min的速率升温至600℃，保温2h，再升温至800℃，保温2h，然后升温至1100℃，保温2h，之后升温至1250℃，保温2h，其他类似描述同理)；
(7)以50L/min的速率通入氧气，并继续以0.15℃/min的速率升温至1300℃、1380℃、1450℃，各保温2h，最后升温至1550℃保温8h，保温结束后以1℃/min冷却至室温，即得所述EIGZO靶材。
使用阿基米德法测定本实施例所得EIGZO靶材的密度，其相对密度为99％，平均晶粒尺寸为10μm，抗弯强度≥80MPa。
实施例2
本实施例提供了本发明EIGZO靶材的制备方法的一种实施例。本实施例EIGZO靶材的制备方法包括以下步骤：
(1)将氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末、分散剂和水混合，球磨4h，得到固含量60％、粒径D50<0.5μm且粒径正态分布半峰宽<0.5的第一混合浆料，其中分散剂的重量为氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末总重量的1％，氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末的质量比为氧化铟：氧化镓：氧化铒：氧化锌＝60％：20％：3％：17％；
(2)加入第一混合浆料重量3％的醇类粘结剂，搅拌2h，得到pH值为10.32的第二混合浆料；
(3)将第二混合浆料进行喷雾干燥，得到粒粒度小于200微米的EIGZO粉粒，其中，喷雾干燥的温度为240℃，进料速度800mL/min；
(4)将EIGZO粉粒置于模具中，在50MPa下压制得到素坯，再将素坯在380MPa下冷等静压，得到相对密度为53.4％的素坯；
(5)将相对密度为53.4％的素坯以0.3℃/min的速率升温至400℃，保温2h，以进行脱脂烧结；
(6)继续以0.20℃/min的速率升温至600℃、850℃、1150℃、1250℃，各保温2h；
(7)以50L/min的速率通入氧气，并继续以0.15℃/min的速率升温至1350℃、1400℃、1500℃，各保温2h，最后升温至1560℃保温8h，保温结束后以1℃/min冷却至室温，即得所述EIGZO靶材。
使用阿基米德法测定本实施例所得EIGZO靶材的密度，其相对密度为99.5％，平均晶粒尺寸为10μm，抗弯强度≥80MPa。
实施例3
本实施例提供了本发明EIGZO靶材的制备方法的一种实施例。本实施例EIGZO靶材的制备方法包括以下步骤：
(1)将氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末、分散剂和水混合，球磨4h，得到固含量60％、粒径D50<0.5μm且粒径正态分布半峰宽<0.5的第一混合浆料，其中分散剂的重量为氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末总重量的1％，氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末的质量比为氧化铟：氧化镓：氧化铒：氧化锌＝65％：15％：5％:15％；
(2)加入第一混合浆料重量2.5％的醇类粘结剂，搅拌2h，得到pH值为10.65的第二混合浆料；
(3)将第二混合浆料进行喷雾干燥，得到粒粒度小于200微米的EIGZO粉粒，其中，喷雾干燥的温度为240℃，进料速度600mL/min；
(4)将EIGZO粉粒置于模具中，在50MPa下压制得到素坯，再将素坯在400MPa下冷等静压，得到相对密度为55.1％的素坯；
(5)将相对密度为55.1％的素坯以0.25℃/min的速率升温至400℃，保温2h，以进行脱脂烧结；
(6)继续以0.25℃/min的速率升温至650℃、900℃、1150℃、1300℃，各保温2h；
(7)以50L/min的速率通入氧气，并继续以0.15℃/min的速率升温至1400℃、1450℃、1520℃，各保温2h，最后升温至1560℃保温8h，保温结束后以1℃/min冷却至室温，即得所述EIGZO靶材。
使用阿基米德法测定本实施例所得EIGZO靶材的密度，其相对密度为99.4％，平均晶粒尺寸为10μm，抗弯强度≥80MPa。
实施例4
本实施例提供了本发明EIGZO靶材的制备方法的一种实施例。本实施例EIGZO靶材的制备方法包括以下步骤：
(1)将氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末、分散剂和水混合，球磨4h，得到固含量60％、粒径D50<0.5μm且粒径正态分布半峰宽<0.5的第一混合浆料，其中分散剂的重量为氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末总重量的1％，氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末的质量比为氧化铟：氧化镓：氧化铒：氧化锌＝65％：15％：5％:15％；
(2)加入第一混合浆料重量3％的醇类粘结剂，搅拌2h，得到pH值为10.56的第二混合浆料；
(3)将第二混合浆料进行喷雾干燥，得到粒粒度小于200微米的EIGZO粉粒，其中，喷雾干燥的温度为240℃，进料速度600mL/min；
(4)将EIGZO粉粒置于模具中，在50MPa下压制得到素坯，再将素坯在400MPa下冷等静压，得到相对密度为58.3％的素坯；
(5)将相对密度为58.3％的素坯以0.15℃/min的速率升温至400℃，保温3h，以进行脱脂烧结；
(6)继续以0.15℃/min的速率升温至850℃、900℃、1050℃、1300℃，各保温2h；
(7)以50L/min的速率通入氧气，并继续以0.15℃/min的速率升温至1300℃、1450℃、1500℃，各保温2h，最后升温至1580℃保温8h，保温结束后以1℃/min冷却至室温，即得所述EIGZO靶材。
使用阿基米德法测定本实施例所得EIGZO靶材的密度，其相对密度为99.62％，平均晶粒尺寸为10μm，抗弯强度≥80MPa。
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (10)

1.一种EIGZO靶材的制备方法，其特征在于，所述制备方法包括以下步骤：
(1)将氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末、分散剂和水混合，球磨，得到第一混合浆料；
(2)在所述第一混合浆料中加入粘结剂，混匀，得到第二混合浆料；
(3)将所述第二混合浆料进行喷雾干燥，得到EIGZO粉粒；
(4)将所述EIGZO粉粒置于模具中进行压制，得到素坯，再将素坯进行冷等静压；
(5)将经冷等静压处理后的素坯以0.1～0.5℃/min的速率升温至150～400℃进行脱脂烧结；
(6)继续以0.1～0.5℃/min的速率升温至500～1300℃进行烧结；
(7)通入氧气，并继续以0.1～0.5℃/min的速率升温至1300～1580℃进行烧结，冷却，即得所述EIGZO靶材。
2.根据权利要求1所述的制备方法，其特征在于，以所述氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末的总重量为基准进行计算，所述氧化铟粉末、氧化镓粉末、氧化铒粉末、氧化锌粉末的质量比为氧化铟：氧化镓：氧化铒：氧化锌＝60～65％:15～20％:3～5％:15～17％。
3.根据权利要求1所述的制备方法，其特征在于，所述步骤(6)和步骤(7)中的烧结都为分阶段烧结。
4.根据权利要求3所述的制备方法，其特征在于，所述步骤(6)中的烧结分为4个阶段，相邻两阶段烧结温度相差50～300℃，每阶段保温时间为1～4h。
5.根据权利要求4所述的制备方法，其特征在于，所述步骤(6)中，第一阶段和第二阶段的烧结温度为600～900℃，第三阶段的烧结温度为1050～1150℃，第四阶段的烧结温度为1250～1300℃。
6.根据权利要求3所述的制备方法，其特征在于，所述步骤(7)中的烧结分为4个阶段，相邻两阶段烧结温度相差50～150℃，每阶段保温时间为2～8h。
7.根据权利要求6所述的制备方法，其特征在于，所述步骤(7)中，第一至第三阶段的烧结温度为1300～1520℃，第四阶段的烧结温度为1550～1580℃。
8.根据权利要求1所述的制备方法，其特征在于，所述步骤(7)中，氧气流量为50～100L/min。
9.根据权利要求1所述的制备方法，其特征在于，所述经冷等静压处理后的素坯的相对密度为50～60％。
10.根据权利要求1所述的制备方法，其特征在于，所述步骤(4)中，冷等静压的压力为300～400MPa；所述步骤(3)中，喷雾干燥的温度为240-260℃，进料速度600-1000mL/min，EIGZO粉粒粒度小于200微米；所述步骤(2)中，粘结剂的重量为第一混合浆料重量的2～3％，第二混合浆料的pH值为9～10；所述步骤(1)中，分散剂的重量为所述氧化铟粉末、氧化镓粉末、氧化铒粉末和氧化锌粉末的总重量的1-2％，球磨时间为3～10h，第一混合浆料的固含量为60～70％。
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