CN115029674A - 一种低偏析铝钪合金靶材及其制备方法 - Google Patents
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Abstract
一种低偏析铝钪合金靶材是采用Al包覆Sc的核壳结构，其Sc含量为20～50at％，成分波动在±0.2％之内，氧含量小于200ppm，相对密度不小于99.5％的AlSc合金靶材；其制备方法，包括：加入粘结剂的Sc粉与Al粉混粉，热处理烧结粉末，获得核壳结构AlSc合金粉末，热压烧结及获得低偏析铝钪合金靶材；本发明形成的合金粉后，不存在后期传输过程由于两种粉末性质不同造成的二次偏析现象，经过后期热压烧结后可获得低偏析的AlSc合金靶材。
Description
技术领域
本发明属于磁控溅射靶材制造技术领域，尤其涉及一种低偏析铝钪合金靶材及其制备方法。
背景技术
高纯AlSc合金靶材主要用于溅射高纯AlScN薄膜，相比AlN、ZnO、锆钛酸铅(PZT)等现有压电薄膜，其具有更强更优的压电性能，是高频移动通信(5G)射频滤波器芯片、MEMS微型先进传感器等制造核心材料。现在制备AlSc合金靶材的制备方法主要包括两种：第一种为熔炼方式，但由于Al与Sc的熔点差异大，Sc在Al中的固溶度非常低，随着Sc含量的增加，固液凝固区间加大，最终所获得的AlSc合金靶坯存在很严重的成分偏析现象；第二种为粉末冶金方式，大多采用单质Al粉与AlSc合金粉混合后压制的方式进行，虽然与熔炼方式相比最终所获得的AlSc合金靶材成分偏析现象有所减轻，但由于Al粉与AlSc合金粉混合后在后期传输过程中由于两种粉末的密度不同容易产生二次偏析，密度较大的AlSc合金粉容易在转粉时沉积在模具的底部，造成成分偏析。
发明内容
针对目前AlSc合金靶材成分偏析的问题，本专利提供了一种低偏析铝钪合金靶材，为采用Al包覆Sc的核壳结构，其Sc含量为20～50at％，成分波动在±0.2％之内，氧含量小于200ppm，相对密度不小于99.5％的AlSc合金靶材。其原理在于通过微湿润的大颗粒Sc粉与干燥的小颗粒Al粉之间的毛细作用，使Al粉均匀的吸附在Sc粉表面，然后通过低温烧结方式使Sc粉与Al粉之间形成烧结颈，形成Al包覆Sc的核壳结构AlSc合金粉。该种核壳结构的AlSc合金粉成分均匀，且形成合金粉后便不存在后期传输过程由于两种粉末性质不同造成的二次偏析现象，经过后期热压烧结后可获得低偏析的AlSc合金靶材。
本发明还公开的一种低偏析铝钪合金靶材制备的方法，包括：加入粘结剂的Sc粉与Al粉混粉，热处理烧结粉末，获得核壳结构AlSc合金粉末，热压烧结及获得低偏析铝钪合金靶材。具体的说，包括下述步骤：
步骤(1)、称量纯度为3N以上、氧含量小于300ppm、粒度为60～100μm的Sc粉，倒入至混粉机内；
步骤(2)、按照每100g Sc粉中加入1～5mL酒精的配比称量相应体积的酒精，倒入步骤(1)中的混粉机内进行充Ar气混制，混制时间为1～2h，获得表面微微湿润的Sc粉；
步骤(3)、所述混制结束后，称量相应配比纯度为5N以上、氧含量小于100ppm的5～10μm Al粉放置于步骤(2)的混粉机后继续充Ar气混制，混制时间为2～5h，获得Al粉吸附于Sc粉表面的混合粉末；
步骤(4)、将步骤(3)获得的所述AlSc混合粉末，放置于真空烧结炉中进行烘干烧结，去除酒精并使Al粉与Sc粉间形成烧结颈粘连到一起，形成Al包覆Sc的核壳结构AlSc合金粉末，烧结温度为100～300℃，烧结时间为1～3h；
步骤(5)、将步骤(4)获得的所述核壳结构AlSc合金粉末进行热压烧结，热压温度为300～650℃，烧结压力20～30MPa，烧结时间为3～5h，最终获得Sc含量成分波动在±0.2％之内，氧含量小于200ppm，相对密度不小于99.5％的AlSc合金靶材。
与现有技术相比，本技术方案具有以下优点：
(1)避免成分偏析：本专利所制备的核壳结构AlSc合金粉成分均匀，且不存在后期传输过程由于两种粉末性质不同造成的二次偏析现象，经过后期热压烧结后可获得低偏析的AlSc合金靶材。
(2)不开裂：采用普通熔炼方式或粉末冶金方式所制备的AlSc合金靶材中存在大量的脆性相及应力易产生碎裂的现象，本专利采用Al包覆Sc的核壳结构AlSc合金粉进行制备AlSc合金靶材时，Al核塑性强，在后期压力烧结过程中可作为“粘结剂”防止AlSc脆性相发生碎裂，还可以通过变形释放部分烧结过程中产生的内应力，进一步降低产生开裂的可能性；
(3)氧含量低：AlSc合金靶材中的氧含量主要由Sc带入，Al粉中本身氧含量低，使用大尺寸Sc粉末制备核壳结构AlSc合金粉可有效降低AlSc合金靶材中的氧含量。
下面通过附图及具体实施方式对本发明做进一步说明，但并不意味着对本发明保护范围的限制。
附图说明
图1为低偏析铝钪合金靶材制备流程图。其中，包括：加入粘结剂的Sc粉与Al粉混粉，热处理烧结粉末，获得核壳结构AlSc合金粉末，热压烧结及获得低偏析铝钪合金靶材。
具体实施方式
为更好的解释本发明，便于理解，下面通过具体实施案例及对比案例对本发明作详细描述。
实施例1～8
1.称量Sc粉：称量纯度为3N、氧含量小于300ppm、粒度为60～100μm的Sc粉，倒入至混粉机内；
2.加入酒精混制：按照每100g Sc粉中加入1mL酒精的配比称量相应体积的酒精，倒入混粉机内进行充Ar气混制，混制时间为2h，获得表面微微湿润的Sc粉；
3.混入Al粉：所述混制结束后，称量80at％配比纯度为5N、氧含量小于100ppm、粒度为10μm的Al粉放置于混粉机后，继续充Ar气混制，混制时间为5h，获得Al粉吸附于Sc粉表面的混合粉末；
4.烘干烧结：将获得的所述AlSc混合粉末，放置于真空烧结炉中进行烘干烧结，去除酒精并使Al粉与Sc粉间形成烧结颈粘连到一起，形成Al包覆Sc的核壳结构AlSc合金粉末，烧结温度为300℃，烧结时间为3h；
5.热压烧结：将获得的所述核壳结构AlSc合金粉末进行热压烧结，热压温度为300～650℃，烧结压力30MPa，烧结时间为3～5h，最终获得Sc含量成分波动在±0.2％之内，氧含量小于200ppm，相对密度不小于99.5％，无裂纹的AlSc合金靶材。
对比例1
1.称量：称量Al-20at％Sc配比的Al块及Sc块。
2.熔炼：将Al块及Sc块放入熔炼炉内进行升温熔炼，熔炼温度为1300℃，保温20min。
3.浇铸：将熔炼后的AlSc合金液体浇铸到模具内进行冷却获得AlSc合金铸锭；
4.轧制退火：将AlSc合金铸锭进行轧制后热处理退火，获得Sc含量波动为±7％，氧含量为95ppm，相对密度不小于99.5％，有裂纹的AlSc合金靶材。
对比例2
1.称量Al粉及Sc粉：称量粒度为1.5μm、纯度5N、氧含量小于150ppm、配比为Al-20at％Sc的Al粉及粒度为1.5μm、纯度3N、氧含量小于600ppm的Sc粉；
2.干混：将Al粉及Sc粉倒入混粉及内进行干混，混粉时间为5h；
3.热压烧结：将混合后的AlSc合金粉放置于热压烧结炉中进行烧结，热压温度为650℃，烧结时间为5h，最终获得Sc含量成分波动为±2％，氧含量为240ppm，无裂纹的AlSc合金靶材。
实施例1～8及对比例1、2中AlSc合金靶材主要制备工艺及性能见表1所示。
表1实施例及对比例AlSc合金靶材主要制备工艺及成分波动、氧含量及产生裂纹情况
由表1所示结果可以看到，本技术方案具有以下优点：
(1)避免成分偏析：本专利所制备的核壳结构AlSc合金粉成分均匀，且不存在后期传输过程由于两种粉末性质不同造成的二次偏析现象，经过后期热压烧结后可获得低偏析的AlSc合金靶材，其成分波动小于0.18％，而作为对比例的成分波动大于2％.
(2)不开裂：采用普通熔炼方式或粉末冶金方式所制备的AlSc合金靶材，对比例中，存在大量的脆性相及应力易产生碎裂的现象，而本专利采用Al包覆Sc的核壳结构AlSc合金粉进行制备AlSc合金靶材时，Al核塑性强，在后期压力烧结过程中可作为“粘结剂”防止AlSc脆性相发生碎裂。
(3)氧含量低：AlSc合金靶材中的氧含量主要由Sc带入，Al粉中本身氧含量低，使用大尺寸Sc粉末制备核壳结构AlSc合金粉可有效降低AlSc合金靶材中的氧含量。本发明实施例的结果，氧含量小于140ppm，而对比例2为大于200ppm。
Claims (2)
1.一种低偏析铝钪合金靶材，其特征为，
具有Al包覆Sc的核壳结构，Sc含量为20～50at％，成分波动在±0.2％之内，氧含量小于200ppm，相对密度不小于99.5％的AlSc合金靶材。
2.一种根据权利要求1所述低偏析铝钪合金靶材的制备方法，其步骤如下：
步骤(1)、称量纯度为3N以上、氧含量小于300ppm、粒度为60～100μm的Sc粉，倒入至混粉机内；
步骤(2)、按照每100g Sc粉中加入1～5mL酒精的配比称量相应体积的酒精，倒入步骤(1)中的混粉机内进行充Ar气混制，混制时间为1～2h，获得表面微微湿润的Sc粉；
步骤(3)、所述混制结束后，称量相应配比纯度为5N以上、氧含量小于100ppm的5～10μmAl粉，放置于步骤(2)的混粉机后，继续充Ar气混制，混制时间为2～5h，获得Al粉吸附于Sc粉表面的混合粉末；
步骤(4)、将步骤(3)获得的AlSc混合粉末放置于真空烧结炉中进行烘干烧结，去除酒精并使Al粉与Sc粉间形成烧结颈粘连到一起，形成Al包覆Sc的核壳结构AlSc合金粉末，烧结温度为100～300℃，烧结时间为1～3h；
步骤(5)、将步骤(4)获得的核壳结构AlSc合金粉末进行热压烧结，热压温度为300～650℃，烧结压力20～30MPa，烧结时间为3～5h，获得AlSc合金靶材。
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| CN108441827A (zh) * | 2018-04-17 | 2018-08-24 | 长沙迅洋新材料科技有限公司 | 铝钪合金靶材制备方法 |
| CN110093588A (zh) * | 2019-05-24 | 2019-08-06 | 福建阿石创新材料股份有限公司 | 一种细晶粒铝钪合金靶材及其制备方法和应用 |
| CN111485207A (zh) * | 2020-06-08 | 2020-08-04 | 福建阿石创新材料股份有限公司 | 一种细晶粒均相高钪含量的铝钪合金烧结靶材及其制备方法和应用 |
| CN111910160A (zh) * | 2020-07-15 | 2020-11-10 | 湖南稀土金属材料研究院 | 铝钪靶材的制备方法 |
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| CN108441827A (zh) * | 2018-04-17 | 2018-08-24 | 长沙迅洋新材料科技有限公司 | 铝钪合金靶材制备方法 |
| CN110093588A (zh) * | 2019-05-24 | 2019-08-06 | 福建阿石创新材料股份有限公司 | 一种细晶粒铝钪合金靶材及其制备方法和应用 |
| CN111485207A (zh) * | 2020-06-08 | 2020-08-04 | 福建阿石创新材料股份有限公司 | 一种细晶粒均相高钪含量的铝钪合金烧结靶材及其制备方法和应用 |
| CN111910160A (zh) * | 2020-07-15 | 2020-11-10 | 湖南稀土金属材料研究院 | 铝钪靶材的制备方法 |
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