CN108516821A - 低电阻率氧化铟锡靶材的制备方法 - Google Patents

低电阻率氧化铟锡靶材的制备方法 Download PDF

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CN108516821A
CN108516821A CN201810753021.9A CN201810753021A CN108516821A CN 108516821 A CN108516821 A CN 108516821A CN 201810753021 A CN201810753021 A CN 201810753021A CN 108516821 A CN108516821 A CN 108516821A
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章波
郭元
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Wuhu Corey Yuen New Mstar Technology Ltd
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Abstract

本发明提出了一种低电阻率氧化铟锡靶材的制备方法，包括以下步骤：1)预混液制备：将分散剂和粘结剂加入水中，搅拌均匀，然后用pH调节剂调节pH值至8～10，得预混液；2)悬浮浆料的制备：向预混液中加入以化学共沉淀法制备的ITO粉体和烧结助剂，再于球磨机中进行球磨，球磨后得到混合浆料，搅拌，抽真空除去浆料中的气泡；所述烧结剂由氧化钇、导电炭黑和Nb2O5组成；3)注浆后坯体成型：把铝制模装在石膏板上，将步骤2)所得浆料注入铝制模中；吸浆成型后脱模干燥，得ITO坯体；4)烧结。该方法过程容易控制，降低了烧结温度促进致密化的同时提升了电性能，烧结出的靶材成分更均匀，电阻率低、相对密度高。

Description

低电阻率氧化铟锡靶材的制备方法
技术领域
本发明属于陶瓷技术领域，具体涉及一种低电阻率氧化铟锡靶材的制备方法。
背景技术
ITO(氧化铟锡)薄膜可由ITO靶材经磁控溅射法制备得到，在工业生产中，大多采用磁控溅射法，将ITO靶材在玻璃上溅射成极薄的一层透明导电膜(厚度100nm左右)，对薄膜进行刻蚀，以制备平板显示器用的电极材料。
要制备出高品质的ITO膜，须采用均匀性好且密度高的ITO靶。这是因为低密度靶内有许多孔洞，孔洞内的不确定元素在溅射过程中也进入到ITO膜，从而影响ITO膜导电性能。另外低密度ITO靶面在溅射过程中容易产生一些黑化的低价氧化物称其为结瘤，因此在溅射过程中会出现飞弧现象(即局部击穿放电)，从而导致溅射工艺不稳定，使ITO膜中出现杂质缺陷。再者低密度ITO靶热导率低，在溅射过程中由于存在热应力而使靶开裂等。
低电阻率氧化铟锡靶材的烧结温度一般高于1550℃。由于在1450℃以上In2O3和SnO2的挥发和分解会急剧加重，而且，在较高烧结温度下(&gt；1500℃)晶粒尺寸太大会严重损害ITO薄膜光电性能的均匀性，因此在相对较低温度下得到高密度、低电阻率的ITO靶材仍具有一定挑战。目前降低烧结温度的主要方法有，热等静压法(CN101407904)、热压法(CN1326909)和微波烧结法等或通过添加低熔点金属氧化物烧结助剂来降低烧结温度。这些方法烧结设备昂贵且生产效率低，而添加单一的烧结助剂不能同时提升致密度和电性能。
发明内容
本发明提供一种低电阻率氧化铟锡靶材的制备方法，该方法过程容易控制，降低了烧结温度促进致密化的同时提升了电性能，烧结出的靶材成分更均匀，电阻率低、相对密度高。
本发明的技术方案是这样实现的：
一种低电阻率氧化铟锡靶材的制备方法，包括以下步骤：
1)预混液制备：将分散剂和粘结剂加入水中，搅拌均匀，然后用pH调节剂调节pH值至8～10，得预混液，所述分散剂为重量比为1：1～3的酒石酸和十六烷基三甲基溴化铵的混合物；
2)悬浮浆料的制备：向预混液中加入以化学共沉淀法制备的ITO粉体和烧结助剂，再于球磨机中进行球磨，球磨后得到混合浆料，搅拌，抽真空除去浆料中的气泡；所述烧结剂由氧化钇、导电炭黑和Nb2O5组成；
3)注浆后坯体成型：把铝制模装在石膏板上，将步骤2)所得浆料注入铝制模中；吸浆成型后脱模干燥，得ITO坯体；
4)烧结：干燥后的ITO坯体在常压纯氧气的气氛下烧结，温度为1340～1560℃，保温时间为3～10小时，得低电阻率氧化铟锡靶材。
其中，优选地，所述分散剂的加入量为ITO粉体质量的0.3～0.5％，粘结剂的加入量为ITO粉体质量的0.5～2％。
其中，优选地，所述粘结剂为聚乙烯醇或聚乙烯醇缩丁醛。
其中，优选地，所述烧结助剂的添加量为ITO粉体质量的2～8％。
其中，优选地，所述氧化钇、导电炭黑和Nb2O5的质量之比为5～6:2～3:1。
本发明的有益效果：
1)与现有技术相比，本发明的创新在于通过掺杂氧化钇、导电炭黑和Nb2O5，在常压纯氧气的气氛下烧结ITO靶材。通过在共沉淀方法合成的铟锡氧化物粉体中添加烧结剂，在烧结的过程中，在较低温度发生固溶和液相烧结的作用。
2)本发明制备的低电阻率氧化铟锡靶材的相对密度为99.0～99.6％，抗弯强度为116～132MPa，电阻率在1.6×10-4Ω·cm到2.1×10-4Ω·cm之间。与现有技术相比，本方法获得的产品致密度高、电阻率低及晶粒尺寸分布均匀。本发明适用于高密度、大尺寸ITO靶材的制备。
具体实施方式
实施例1
一种低电阻率氧化铟锡靶材的制备方法，包括以下步骤：
1)预混液制备：将分散剂和粘结剂加入水中，搅拌均匀，然后用pH调节剂调节pH值至8，得预混液，所述分散剂为重量比为1：2的酒石酸和十六烷基三甲基溴化铵的混合物；分散剂的加入量为ITO粉体质量的0.4％，粘结剂的加入量为ITO粉体质量的1.4％。
2)悬浮浆料的制备：向预混液中加入以化学共沉淀法制备的ITO粉体和烧结助剂，再于球磨机中进行球磨，球磨后得到混合浆料，搅拌，抽真空除去浆料中的气泡；所述烧结剂由氧化钇、导电炭黑和Nb2O5组成；所述烧结助剂的添加量为ITO粉体质量的4％，所述氧化钇、导电炭黑和Nb2O5的质量之比为5:3:1。
3)注浆后坯体成型：把铝制模装在石膏板上，将步骤2)所得浆料注入铝制模中；吸浆成型后脱模干燥，得ITO坯体。
4)烧结：干燥后的ITO坯体在常压纯氧气的气氛下烧结，温度为1460℃，保温时间为6小时，得低电阻率氧化铟锡靶材。
本实施例制备的低电阻率氧化铟锡靶材的相对密度为99.4％，抗弯强度为120MPa，电阻率在1.9×10-4Ω·cm。
实施例2
一种低电阻率氧化铟锡靶材的制备方法，包括以下步骤：
1)预混液制备：将分散剂和粘结剂加入水中，搅拌均匀，然后用pH调节剂调节pH值至9，得预混液，所述分散剂为重量比为1：1的酒石酸和十六烷基三甲基溴化铵的混合物；分散剂的加入量为ITO粉体质量的0.3％，粘结剂的加入量为ITO粉体质量的2％。
2)悬浮浆料的制备：向预混液中加入以化学共沉淀法制备的ITO粉体和烧结助剂，再于球磨机中进行球磨，球磨后得到混合浆料，搅拌，抽真空除去浆料中的气泡；所述烧结剂由氧化钇、导电炭黑和Nb2O5组成；所述烧结助剂的添加量为ITO粉体质量的2％，所述氧化钇、导电炭黑和Nb2O5的质量之比为5:3:1。
3)注浆后坯体成型：把铝制模装在石膏板上，将步骤2)所得浆料注入铝制模中；吸浆成型后脱模干燥，得ITO坯体。
4)烧结：干燥后的ITO坯体在常压纯氧气的气氛下烧结，温度为1530℃，保温时间为3小时，得低电阻率氧化铟锡靶材。
本实施例制备的低电阻率氧化铟锡靶材的相对密度为99.6％，抗弯强度为132MPa，电阻率在2.1×10-4Ω·cm。
实施例3
一种低电阻率氧化铟锡靶材的制备方法，包括以下步骤：
1)预混液制备：将分散剂和粘结剂加入水中，搅拌均匀，然后用pH调节剂调节pH值至10，得预混液，所述分散剂为重量比为1：3的酒石酸和十六烷基三甲基溴化铵的混合物；分散剂的加入量为ITO粉体质量的0.5％，粘结剂的加入量为ITO粉体质量的0.5％。
2)悬浮浆料的制备：向预混液中加入以化学共沉淀法制备的ITO粉体和烧结助剂，再于球磨机中进行球磨，球磨后得到混合浆料，搅拌，抽真空除去浆料中的气泡；所述烧结剂由氧化钇、导电炭黑和Nb2O5组成；所述烧结助剂的添加量为ITO粉体质量的8％，所述氧化钇、导电炭黑和Nb2O5的质量之比为6:2:1；
3)注浆后坯体成型：把铝制模装在石膏板上，将步骤2)所得浆料注入铝制模中；吸浆成型后脱模干燥，得ITO坯体；
4)烧结：干燥后的ITO坯体在常压纯氧气的气氛下烧结，温度为1320℃，保温时间为10小时，得低电阻率氧化铟锡靶材。
本实施例制备的低电阻率氧化铟锡靶材的相对密度为99.0％，抗弯强度为116MPa，电阻率在1.6×10-4Ω·cm。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (5)

1.一种低电阻率氧化铟锡靶材的制备方法，其特征在于，包括以下步骤：
1)预混液制备：将分散剂和粘结剂加入水中，搅拌均匀，然后用pH调节剂调节pH值至8～10，得预混液，所述分散剂为重量比为1：1～3的酒石酸和十六烷基三甲基溴化铵的混合物；
2)悬浮浆料的制备：向预混液中加入以化学共沉淀法制备的ITO粉体和烧结助剂，再于球磨机中进行球磨，球磨后得到混合浆料，搅拌，抽真空除去浆料中的气泡；所述烧结剂由氧化钇、导电炭黑和Nb2O5组成；
3)注浆后坯体成型：把铝制模装在石膏板上，将步骤2)所得浆料注入铝制模中；吸浆成型后脱模干燥，得ITO坯体；
4)烧结：干燥后的ITO坯体在常压纯氧气的气氛下烧结，温度为1340～1560℃，保温时间为3～10小时，得低电阻率氧化铟锡靶材。
2.根据权利要求1所述的低电阻率氧化铟锡靶材的制备方法，其特征在于，所述分散剂的加入量为ITO粉体质量的0.3～0.5％，粘结剂的加入量为ITO粉体质量的0.5～2％。
3.根据权利要求2所述的低电阻率氧化铟锡靶材的制备方法，其特征在于，所述粘结剂为聚乙烯醇或聚乙烯醇缩丁醛。
4.根据权利要求1所述的低电阻率氧化铟锡靶材的制备方法，其特征在于，所述烧结助剂的添加量为ITO粉体质量的2～8％。
5.根据权利要求1所述的低电阻率氧化铟锡靶材的制备方法，其特征在于，所述氧化钇、导电炭黑和Nb2O5的质量之比为5～6:2～3:1。
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