CN112079627A - 一种由ito废靶直接粉碎制粉并生产ito靶材的制备方法 - Google Patents

一种由ito废靶直接粉碎制粉并生产ito靶材的制备方法 Download PDF

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CN112079627A
CN112079627A CN202010974752.3A CN202010974752A CN112079627A CN 112079627 A CN112079627 A CN 112079627A CN 202010974752 A CN202010974752 A CN 202010974752A CN 112079627 A CN112079627 A CN 112079627A
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文宏福
李鹏
叶俊峰
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Shaoguan Oulai Hi Tech Material Co ltd
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Abstract

本发明公开了一种由ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，包括如下步骤：S1、将废靶材进行预处理得到预处理废靶材料；S2、将步骤S1得到的预处理废靶材料依次进行粗碎、中碎、粉碎得到废靶材粉末；S3、将废靶材粉末在500‑1000℃下煅烧得到ITO回收粉；S4、将ITO回收粉成型得到ITO生坯，ITO生坯在常压纯氧气氛条件下进行烧结得到ITO靶材。本发明将废靶材料预处理后进行三级破碎和粉碎工艺获得废靶材粉末，在适合温度下进行煅烧即得ITO回收粉，将ITO回收粉采用常规的成型和烧结工艺成型和烧结即可得到ITO靶材，ITO靶材纯度可达99.99％及以上，整体工艺简单易控，实现对废靶回收再利用，具有很好的经济效益。

Description

一种由ITO废靶直接粉碎制粉并生产ITO靶材的制备方法
技术领域
本发明属于磁控溅射技术领域，尤其涉及一种由ITO废靶直接粉碎制粉并生产ITO靶材的制备方法。
背景技术
铟锡氧化物靶材，Indium Tin Oxide靶材，简称ITO靶材，是氧化铟和氧化锡两种金属氧化物的混合物经高温烧结形成的陶瓷功能材料。由氧化锡掺杂氧化铟烧结的ITO靶材，经真空磁控溅射镀膜后，可在玻璃等透明基底上形成ITO透明导电膜，是液晶显示面板行业必需的关键材料。
ITO靶材在磁控溅射镀膜时，由于磁场强度在靶材表面分布的不均匀，靶材的消耗是不均匀的。一般TFT平面ITO靶材的利用率只有30％左右，旋转ITO靶材利用率约70-80％，产生大量的ITO废靶需要回收利用。此外，在ITO靶材的生产加工过程中，也会产生大量的边角料或不良品。这些ITO废靶原料，本身为99.99％纯度的材料，铟、锡、氧元素之外的杂质含量低于100ppm，实际上除了表面可能存在污染外，废靶材就是剩余的ITO靶材边角料，内部成分与ITO靶材纯度是一样的。
目前ITO废靶的回收，市场上一般是将ITO废靶作为提炼铟金属的原料，经过一系列复杂的化学和物理过程，将锡作为杂质去除，将铟金属提炼为99.99％的铟锭。这一过程，工艺流程长，需要大量使用酸碱化学试剂，产生废水排放。因此存在成本较高的问题，并且对环境存在污染风险。然后再由铟金属制备ITO粉末，也需要经过复杂的过程，生产成本较高。
如果能够将ITO废靶在去除杂质后，直接制成ITO粉，用于ITO靶材生产，相比于目前传统的提炼铟金属再由铟金属制备ITO粉末，可大幅度降低生产成本，减少环境污染。
中国专利申请CN 105366709A公开了一种回收ITO废靶的方法，将ITO废靶在汽化反应器内经过两次电弧汽化，直接制备为ITO粉末。但是，该方法存在能耗高、生产效率低等问题，并且石墨电极可能会对ITO粉末产生还原反应造成失氧，影响后续的ITO靶材生产质量。
中国专利申请CN 110498443A公开了一种回收ITO废靶的方法，将ITO废靶粉碎，然后盐酸溶解，再采用三电极电解方法获取ITO前驱体，再经过烘干和煅烧制备ITO粉末。该工艺流程较长，需要大量使用化学试剂，增加了杂质引入和环境污染风险。
中国专利申请CN109956746A公开了一种回收再利用ITO废靶的工艺方法，将ITO废靶破碎至100目后，采用热等静压工艺进行烧结生产ITO靶材。该工艺制备的ITO粉末粒度20-120um，颗粒较粗，烧结活性较差，ITO靶材烧结密度仅为99％，且纯度仅能达到99％，不能满足现有市场客户要求。
发明内容
基于背景技术所述技术问题，本发明提供了一种由ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，将废靶材料预处理后进行三级破碎和粉碎工艺得到废靶材粉末，配合烧结工艺得到ITO靶材，整体工艺简单易控，实现对废靶回收再利用，具有很好的经济效益。
本发明提出的一种由ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，包括如下步骤：
S1、将废靶材进行打磨、清洗和酸泡得到预处理废靶材料；
S2、将步骤S1得到的预处理废靶材料依次进行粗碎、中碎、粉碎得到废靶材粉末；其中，粗碎至粒径低于5mm；中碎至粒径低于1mm，粉碎至粒径低于200目；
S3、将废靶材粉末在500-1000℃下煅烧得到ITO回收粉；
S4、将ITO回收粉成型得到ITO生坯；ITO生坯在常压纯氧气氛条件下进行烧结得到ITO靶材。
本发明中，粗碎可采用颚式破碎机；中碎可采用对辊式破碎机；粉碎可采用气流粉碎机、球磨机或振动磨机。
优选地，步骤S1中，废靶材为溅射镀膜后产生的ITO残靶和/或ITO靶材生产过程中产生的边角料或不良品。
优选地，步骤S1中，预处理具体包括：打磨、清洗和酸泡。
优选地，酸泡的具体工艺为：采用浓度为10％的盐酸浸泡8-10小时；酸泡的目的是去除表面粘附的杂质与污物。
优选地，步骤S3中，ITO回收粉的粒径D50为0.2-2.5μm，比表面积为2-8m2/g，纯度为99.99％及以上。
优选地，步骤S4中，ITO生坯原料中还可加入氧化铟粉末和/或氧化锡粉末。
优选地，步骤S4中，氧化铟粉末和氧化锡粉末的粒径D50为0.2-2.5μm。
优选地，步骤S4中，采用注浆成型工艺或压力成型工艺进行成型。
优选地，步骤S4所得ITO靶材的纯度大于99.99％，相对密度大于99.7％。
优选地，步骤S4中，烧结温度为1550-1600℃，烧结时间为12-18h。
本发明中将废靶材料预处理后进行三级破碎和粉碎工艺获得粒径低于200目的废靶材粉末，然后在适合温度下进行煅烧即得ITO回收粉，将ITO回收粉采用常规的成型和烧结工艺成型和烧结即可得到ITO靶材，所得ITO靶材纯度可达99.99％及以上，相对密度大于99.7％，且整体工艺简单易控，实现对废靶回收再利用，具有很好的经济效益。
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
一种由ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，包括如下步骤：
S1、将ITO溅射残靶经打磨、清洗，再用10％盐酸浸泡8小时，得到预处理废靶材料；
S2、将步骤S1得到的预处理废靶材料用颚式破碎机进行粗碎至粒径低于5mm，接着用对辊式破碎机进行中碎至粒径低于1mm，最后用气流粉碎机进粉碎至粒径低于200目得到废靶材粉末；
S3、将废靶材粉末在900℃下煅烧得到粒径D50为1.52μm，比表面积BET＝3.4m2/g纯度为99.991％的ITO回收粉；
S4、将ITO回收粉采用常规注浆成型工艺成型得到ITO生坯，ITO生坯的相对密度为63.8％，ITO生坯在常压纯氧气氛中，1600℃下烧结15h得到ITO靶材；ITO靶材的尺寸为500*300*6mm，相对密度为99.72％，纯度为99.993％。
实施例2
一种由ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，包括如下步骤：
S1、将ITO靶材生产边角料经打磨、清洗，再用10％盐酸浸泡10小时，得到预处理废靶材料；
S2、将步骤S1得到的预处理废靶材料用颚式破碎机进行粗碎至粒径低于5mm，接着用对辊式破碎机进行中碎至粒径低于1mm，最后用气流粉碎机进粉碎至粒径低于200目得到废靶材粉末；
S3、将废靶材粉末在800℃下煅烧得到粒径D50为1.48μm，比表面积BET＝5.8m2/g，纯度为99.994％的ITO回收粉；
S4、按质量比1：1向ITO回收粉中加入氧化铟和氧化锡的混合粉末，其中，氧化铟和氧化锡的重量比为90：10，混合制浆后喷雾造粒，经35MPa模压和250MPa等静压成型，得到ITO生坯，ITO生坯的相对密度为62.5％，ITO生坯在常压纯氧气氛中，1550℃下烧结12h得到ITO靶材；ITO靶材的尺寸为600*280*8mm，相对密度为99.74％，纯度为99.995％。
实施例3
一种由ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，包括如下步骤：
S1、将ITO溅射残靶经打磨、清洗，再用10％盐酸浸泡10小时，得到预处理废靶材料；
S2、将步骤S1得到的预处理废靶材料用颚式破碎机进行粗碎至粒径低于5mm，接着用对辊式破碎机进行中碎至粒径低于1mm，最后用振动磨机进粉碎至粒径低于200目得到废靶材粉末；
S3、将废靶材粉末在500℃下煅烧得到粒径D50为0.25μm，比表面积BET＝7.8m2/g，纯度为99.992％的ITO回收粉；
S4、将ITO回收粉混合制浆后喷雾造粒，经35MPa模压和250MPa等静压成型，得到ITO生坯，ITO生坯的相对密度为60.3％，ITO生坯在常压纯氧气氛中，在1600℃下烧结18h得到ITO靶材；ITO靶材的尺寸为600*280*8mm，相对密度为99.70％，纯度为99.991％。
本发明具体实施例中使用的颚式破碎机颚板为硬质合金，其它与物料接触部位为PP材质，对辊式破碎机中对辊为氧化锆陶瓷材质，其它与物料接触部位为PP材质，气流粉碎机与物料接触部位为由ITO陶瓷靶材加工而成的陶瓷。
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)

1.一种由ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，其特征在于，包括如下步骤：
S1、将废靶材进行预处理得到预处理废靶材料；
S2、将步骤S1得到的预处理废靶材料依次进行粗碎、中碎、粉碎得到废靶材粉末；其中，粗碎至粒径低于5mm；中碎至粒径低于1mm，粉碎至粒径低于200目；
S3、将废靶材粉末在500-1000℃下煅烧得到ITO回收粉；
S4、将ITO回收粉成型得到ITO生坯，ITO生坯在常压纯氧气氛条件下进行烧结得到ITO靶材。
2.根据权利要求1所述的ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，其特征在于，步骤S1中，废靶材为溅射镀膜后产生的ITO残靶和/或ITO靶材生产过程中产生的边角料和不良品。
3.根据权利要求1或2所述的ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，其特征在于，步骤S1中，预处理具体包括：打磨、清洗和酸泡。
4.根据权利要求1-3中任一项所述的ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，其特征在于，步骤S3中，ITO回收粉的粒径D50为0.2-2.5μm，比表面积为2-8m2/g，纯度为99.99％及以上。
5.根据权利要求1-4中任一项所述的ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，其特征在于，步骤S4中，ITO生坯原料中还可加入氧化铟粉末和/或氧化锡粉末。
6.根据权利要求1-5中任一项所述的ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，其特征在于，步骤S4中，氧化铟粉末和氧化锡粉末的粒径D50为0.2-2.5μm。
7.根据权利要求1-6中任一项所述的ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，其特征在于，步骤S4中，采用注浆成型工艺或压力成型工艺进行成型。
8.根据权利要求1-7中任一项所述的ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，其特征在于，步骤S4所得ITO靶材的纯度大于99.99％，相对密度大于99.7％。
9.根据权利要求1-8中任一项所述的ITO废靶直接粉碎制粉并生产ITO靶材的制备方法，其特征在于，步骤S4中，烧结温度为1550-1600℃，烧结时间为12-18h。
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