CN113233871B - 一种ito残靶回收料制备ito蒸发料的方法 - Google Patents

一种ito残靶回收料制备ito蒸发料的方法 Download PDF

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CN113233871B
CN113233871B CN202110469072.0A CN202110469072A CN113233871B CN 113233871 B CN113233871 B CN 113233871B CN 202110469072 A CN202110469072 A CN 202110469072A CN 113233871 B CN113233871 B CN 113233871B
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余芳
文崇斌
朱刘
童培云
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Vital Thin Film Materials Guangdong Co Ltd
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Abstract

本发明公开了一种ITO残靶回收料制备ITO蒸发料的方法，包括以下步骤：(1)将ITO残靶经过预处理，得预处理后的ITO残靶；(2)将所述预处理后的ITO残靶破碎，过筛，得破碎好的ITO粉末；(3)将所述破碎好的ITO粉末装入模具中，然后置于热压炉内，在50～100MPa下进行预压；(4)预压结束后，热压炉内抽真空到＜10Pa后，升温至600～1200℃，并保温50～80min，在保温的同时升压至100～200MPa保持30～50min，冷却，即得所述ITO蒸发料。本发明所述方法通过调节制备工艺中热压的条件，可以制备不同密度的ITO蒸发料，节约了回收费用，充分利用了In材料。

Description

一种ITO残靶回收料制备ITO蒸发料的方法
技术领域
本发明涉及资源回收技术领域，具体涉及一种ITO残靶回收料制备ITO蒸发料的方法。
背景技术
目前用于液晶显示行业的ITO，一般为靶材，有平面靶和旋转靶，一般平面靶材的利用率为15-30％，旋转靶的利用率为60-80％，由于ITO靶材含有稀散金属In，因此溅射后的靶材，通常是重新回收，但是这样不仅造成了资源的浪费，同时在回收过程中也会对环境造成一定的污染。
真空蒸镀，简称蒸镀，是指在真空条件下，采用一定的加热蒸发方式蒸发镀膜材料(或称膜料)并使之气化，粒子飞至基片表面凝聚成膜的工艺方法，ITO蒸镀料作为真空蒸镀ITO薄膜的原材料，同时也被广泛应用，不同的蒸镀工艺对ITO的密度要求各不相同。
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ITO残靶回收料制备ITO蒸发料的方法。
为实现上述目的，本发明采取的技术方案为：一种ITO残靶回收料制备ITO蒸发料的方法，包括以下步骤：
(1)将ITO残靶经过预处理，得预处理后的ITO残靶；
(2)将所述预处理后的ITO残靶破碎，过筛，得破碎好的ITO粉末；
(3)将所述破碎好的ITO粉末装入模具中，然后置于热压炉内，在50～100MPa下进行预压；
(4)预压结束后，热压炉内抽真空到＜10Pa后，升温至600～1200℃，并保温50～80min，在保温的同时升压至100～200MPa，在100～200MPa下保持30～50min，冷却，即得所述ITO蒸发料。
步骤(3)中的预压操作可防止抽真空喷粉；通过控制步骤(4)中的温度、压强和时间可以控制所得ITO蒸发料的密度在55－99.8％范围内。
作为本发明所述ITO残靶回收料制备ITO蒸发料的方法的优选实施方式，步骤(1)中，所述预处理为：对ITO残靶的表面进行打磨抛光并清洗。
作为本发明所述ITO残靶回收料制备ITO蒸发料的方法的优选实施方式，步骤(2)中，所述过筛为过325目筛。
作为本发明所述ITO残靶回收料制备ITO蒸发料的方法的优选实施方式，步骤(4)中，所述升温的速率为5～10℃/min。
作为本发明所述ITO残靶回收料制备ITO蒸发料的方法的优选实施方式，步骤(4)中，所述冷却为随炉冷却。
作为本发明所述ITO残靶回收料制备ITO蒸发料的方法的优选实施方式，步骤(4)中，所述冷却后还包括：将经过CNC加工、破碎或切割至所需尺寸。
作为本发明所述ITO残靶回收料制备ITO蒸发料的方法的优选实施方式，所述升压的时间为≤20min。
本发明的有益效果在于：本发明提供了一种ITO残靶回收料制备ITO蒸发料的方法，本方法通过ITO残靶回收粉制备ITO蒸发料，通过调节制备工艺中热压的条件，可以制备不同密度的ITO蒸发料，同时节约了回收的费用，残靶回收充分利用了In材料，避免了环境污染。
具体实施方式
为更好地说明本发明的目的、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
本发明所述ITO残靶回收料制备ITO蒸发料的方法的一种实施例，本实施例所述方法包括以下步骤：
(1)对ITO残靶的表面进行打磨抛光并清洗，得预处理后的ITO残靶；
(2)将所述预处理后的ITO残靶破碎，过325目筛，得破碎好的ITO粉末；
(3)将所述破碎好的ITO粉末装入模具中，然后置于热压炉内，在50MPa下进行预压；
(4)预压结束后，热压炉内抽真空到＜10Pa后，以8℃/min升温到600℃，保温80min，在保温的同时在20分钟内升压至150MPa，并在150MPa下保持35min，随炉降温冷却，经过CNC加工，得到ITO蒸发料块，根据需求，破碎或者切割到所需要的尺寸，即得所述ITO蒸发料。
实施例2
本发明所述ITO残靶回收料制备ITO蒸发料的方法的一种实施例，本实施例所述方法包括以下步骤：
(1)对ITO残靶的表面进行打磨抛光并清洗，得预处理后的ITO残靶；
(2)将所述预处理后的ITO残靶破碎，过325目筛，得破碎好的ITO粉末；
(3)将所述破碎好的ITO粉末装入模具中，然后置于热压炉内，在100MPa下进行预压；
(4)预压结束后，热压炉内抽真空到＜10Pa后，以10℃/min升温到1200℃，保温80min，在保温的同时在20分钟内升压至200MPa，并在200MPa下保持40min，随炉降温冷却，经过CNC加工，得到ITO蒸发料块，根据需求，破碎或者切割到所需要的尺寸，即得所述ITO蒸发料。
实施例3
本发明所述ITO残靶回收料制备ITO蒸发料的方法的一种实施例，本实施例所述方法包括以下步骤：
(1)对ITO残靶的表面进行打磨抛光并清洗，得预处理后的ITO残靶；
(2)将所述预处理后的ITO残靶破碎，过325目筛，得破碎好的ITO粉末；
(3)将所述破碎好的ITO粉末装入模具中，然后置于热压炉内，在60MPa下进行预压；
(4)预压结束后，热压炉内抽真空到＜10Pa后，以8℃/min升温到900℃，保温70min，在保温的同时在20分钟内升压至180MPa，并在180MPa下保持50min，随炉降温冷却，经过CNC加工，得到ITO蒸发料块，根据需求，破碎或者切割到所需要的尺寸，即得所述ITO蒸发料。
通过阿基米德排水法测试实施例1～3所述ITO蒸发料的相对密度，测试结果见表1。
表1
组别 蒸发料的相对密度 纯度
实施例1 61％ 4N
实施例2 85％ 4N
实施例3 73％ 4N
从表1可以看出，通过残靶回收料可以制得与新料纯度相近的蒸发料，可以通过改变工艺条件制得不同密度需求的蒸发料。
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 (2)

1.一种ITO残靶回收料制备ITO蒸发料的方法，其特征在于，包括以下步骤：
(1)将ITO残靶经过预处理，得预处理后的ITO残靶；所述预处理为：对ITO残靶的表面进行打磨抛光并清洗；
(2)将所述预处理后的ITO残靶破碎，过325目筛，得破碎好的ITO粉末；
(3)将所述破碎好的ITO粉末装入模具中，然后置于热压炉内，在50～100MPa下进行预压；
(4)预压结束后，热压炉内抽真空到＜10Pa后，以5～10℃/min的升温速率升温至600～1200℃，并保温50～80min，在保温的同时升压至100～200MPa，在100～200MPa下保持30～50min，随炉冷却，即得所述ITO蒸发料；所述升压的时间为≤20min。
2.如权利要求1所述ITO残靶回收料制备ITO蒸发料的方法，其特征在于，步骤(4)中，所述冷却后还包括：将经过CNC加工、破碎或切割至所需尺寸。
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