CN113402277A - 一种FeSe1-xTex靶材的制备工艺 - Google Patents
一种FeSe1-xTex靶材的制备工艺 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
本发明公开了一种FeSe1‑xTex靶材的制备工艺，在热压烧结时，对烧结炉腔体以氩气抽洗三次，真空度保持在10‑2Pa，对模具中的粉胚施加27MPa的压强，在整个烧结过程中保持该压强，以30％的输出功率经由30min升温至400℃，再以50％的输出功率经由30min升温至目标温度400℃‑700℃，最终在400℃‑700℃保温12小时。本技术工艺制备的FeSe1‑xTex靶材相比于现有工艺所制备的靶材，其致密性得到了较大的提高，并且可以通过改变烧结目标温度连续调控FeSe1‑xTex靶材的致密性，同时制得的FeSe1‑xTex靶材成相好；解决了现有工艺制备的FeSe1‑xTex靶材不够致密，经脉冲激光多次轰击后易粉化的问题；本制备工艺易于实现工业化，可用于百米、千米级FeSe1‑xTex长带涂层导体的制备，具有良好的应用前景。
Description
技术领域
本发明属于靶材制备技术领域，特别是涉及一种FeSe1-xTex靶材的制备工艺。
背景技术
FeSe1-xTex材料凭借其高临界磁场、高临界电流密度和小的各向异性在下一代高场磁体的设计中具有重要的应用前景。绕制高场磁体要解决的首要问题是制备出高性能的FeSe1-xTex长带涂层导体。脉冲激光沉积(PLD)是当前FeSe1-xTex涂层导体制备的最主要方法。在FeSe1-xTex长带涂层导体的制备中，FeSe1-xTex靶材是通过PLD激光的轰击不断产生等离子体羽辉的溅射源。而现在通过传统的固相反应法制备得到的FeSe1-xTex靶材，其致密性都普遍不高。这样的靶材在PLD产生的高能量密度以及高频率的激光的轰击下，易粉化，致使后续的成膜不平整且均匀性不佳，无法实现长带涂层导体的制备。
发明内容
为了克服上述的问题，本发明提供了一种高质量、致密度可调控的FeSe1-xTex靶材的制备工艺。
本发明所采用的技术方案是：
一种FeSe1-xTex靶材的制备工艺，包括如下步骤：
步骤一：对原材料进行配比称量：铁粉为100目、硒粉为200目、碲粉为100目；
步骤二：称量后的粉末放置于玛瑙研钵中充分研磨30min，随后将研磨好的混合粉末以400Mpa的压强保持10min压制成片，封装在真空石英管中，进行第一次固相反应；
步骤三：以5℃/min的升温速率升至400℃，预反应24小时，再以5℃/min的速率升温至700℃，保温3天，随后降至室温；
步骤四：对片状混合粉末进行碾碎，研磨60min，再以400Mpa的压强保持10min压制成片，封装在真空石英管中，进行第二次固相反应；
步骤五：以2℃/min的速率升温至700℃，保温3天，随后降至室温；
步骤六：对片状混合粉末进行碾碎，研磨60min，再以400Mpa的压强保持10min压制成片，封装在真空石英管中，进行第三次固相反应；
步骤七：以2℃/min的速率升温至700℃，保温3天，随后降至室温。保证粉胚的反应充分；
步骤八：对片状混合粉末再进行碾碎，研磨60min，最后将三次烧结完成的粉胚预压成靶，用石墨纸包裹，放置在一个直径为20mm的石墨模具中；
步骤九：热压烧结：对烧结炉腔体以氩气抽洗三次，真空度保持在10-2Pa，避免靶材与氧气较多的接触而影响最终靶材的质量，对模具中的粉胚施加27MPa的压强，在整个烧结过程中保持该压强，以30％的输出功率经由30min升温至400℃，再以50％的输出功率经由30min升温至目标温度400℃-700℃，最终在400℃-700℃保温12小时，使预压靶材内部致密化，提高成品靶材的密度，与传统的只进行固相反应的靶材相比，热压后使得靶材能够在高能量的激光轰击下不至于粉末化，避免了成膜的不均匀性以及保证了薄膜在微观尺度仍然具有良好的平整度；
步骤十：靶材的修整：将靶材表面以1500目、2000目、2500目的砂纸依次打磨，最后以型号为DNW0.5的水溶金刚石研磨膏进行抛光处理，得到一个平整光滑的靶材表面。
其中，步骤一中铁粉的纯度为99.95％，硒粉、碲粉的纯度均为99.99％。
其中，步骤二、四、六、八中研磨过程都在一个充满氩气保护的、水值小于0.1ppm、氧值小于0.1ppm的手套箱中进行，确保原料与氧气较少的接触，避免对成品靶材的不利影响。
本发明的优点如下：
本技术工艺制备的FeSe1-xTex靶材相比于现有工艺所制备的靶材，其致密性得到了较大的提高，并且可以通过改变烧结目标温度连续调控FeSe1-xTex靶材的致密性，同时制得的FeSe1-xTex靶材成相好；解决了现有工艺制备的FeSe1-xTex靶材不够致密，经脉冲激光多次轰击后易粉化的问题；本制备工艺易于实现工业化，可用于百米、千米级FeSe1-xTex长带涂层导体的制备，具有良好的应用前景。
附图说明
图1为本发明的固相反应法烧结后靶材密度随烧结前冷压压强大小的变化示意图；
图2是本发明的27Mpa的压强下热压烧结后靶材密度随烧结温度的变化示意图；
图3是本发明的根据制备工艺制备出的直径为60mm的大尺寸高密度FeSeTe靶材的示意图。
具体实施方式
下面对本发明作进一步的说明，但本发明并不局限于这些内容。
实施例
本发明提供了一种FeSe1-xTex靶材的制备工艺，包括如下步骤：
对原材料进行配比称量：铁粉为100目，纯度99.95％，硒粉为200目，纯度为99.99％，碲粉为100目，纯度为99.99％；称量后的粉末放置于玛瑙研钵中充分研磨30min，随后将研磨好的混合粉末以400Mpa的压强保持10min压制成片，封装在真空石英管中，进行第一次固相反应；以5℃/min的升温速率升至400℃，预反应24小时，再以5℃/min的速率升温至700℃，保温3天，随后降至室温；对片状混合粉末进行碾碎，研磨60min，再以400Mpa的压强保持10min压制成片，封装在真空石英管中，进行第二次固相反应；以2℃/min的速率升温至700℃，保温3天，随后降至室温；对片状混合粉末进行碾碎，研磨60min，再以400Mpa的压强保持10min压制成片，封装在真空石英管中，进行第三次固相反应；以2℃/min的速率升温至700℃，保温3天，随后降至室温。保证粉胚的反应充分；对片状混合粉末再进行碾碎，研磨60min，最后将三次烧结完成的粉胚预压成靶，用石墨纸包裹，放置在一个直径为20mm的石墨模具中；所有的研磨过程都在一个充满氩气保护的、水值小于0.1ppm、氧值小于0.1ppm的手套箱中进行，确保原料与氧气较少的接触，避免对成品靶材的不利影响；热压烧结：对烧结炉腔体以氩气抽洗三次，真空度保持在10-2Pa，避免靶材与氧气较多的接触而影响最终靶材的质量，对模具中的粉胚施加27MPa的压强，在整个烧结过程中保持该压强，以30％的输出功率经由30min升温至400℃，再以50％的输出功率经由30min升温至400℃-700℃，最终在400℃-700℃保温12小时，使预压靶材内部致密化，提高成品靶材的密度，与传统的只进行固相反应的靶材相比，热压后使得靶材能够在高能量的激光轰击下不至于粉末化，避免了成膜的不均匀性以及保证了薄膜在微观尺度仍然具有良好的平整度；靶材的修整：将靶材表面以1500目、2000目、2500目的砂纸依次打磨，最后以型号为DNW0.5的水溶金刚石研磨膏进行抛光处理，得到一个平整光滑的靶材表面。
如图1所示，为固相反应法烧结后靶材密度随烧结前冷压压强大小的变化；
如图2所示，为27Mpa的压强下热压烧结后靶材密度随烧结温度的变化，圆圈代表热压前预压(冷压)的靶材密度，可见热压烧结后靶材密度明显增大；
如图3所示，为根据制备工艺制备出的直径为60mm的大尺寸高密度FeSeTe靶材。
指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。
Claims (3)
1.一种FeSe1-xTex靶材的制备工艺，其特征在于：包括如下步骤：
步骤一：对原材料进行配比称量：铁粉为100目、硒粉为200目、碲粉为100目；
步骤二：称量后的粉末放置于玛瑙研钵中充分研磨30min，随后将研磨好的混合粉末以400Mpa的压强保持10min压制成片，封装在真空石英管中，进行第一次固相反应；
步骤三：以5℃/min的升温速率升至400℃，预反应24小时，再以5℃/min的速率升温至700℃，保温3天，随后降至室温；
步骤四：对片状混合粉末进行碾碎，研磨60min，再以400Mpa的压强保持10min压制成片，封装在真空石英管中，进行第二次固相反应；
步骤五：以2℃/min的速率升温至700℃，保温3天，随后降至室温；
步骤六：对片状混合粉末进行碾碎，研磨60min，再以400Mpa的压强保持10min压制成片，封装在真空石英管中，进行第三次固相反应；
步骤七：以2℃/min的速率升温至700℃，保温3天，随后降至室温；
步骤八：对片状混合粉末再进行碾碎，研磨60min，最后将三次烧结完成的粉胚预压成靶，用石墨纸包裹，放置在一个直径为20mm的石墨模具中；
步骤九：热压烧结：对烧结炉腔体以氩气抽洗三次，真空度保持在10-2Pa，对模具中的粉胚施加27MPa的压强，在整个烧结过程中保持该压强，以30％的输出功率经由30min升温至400℃，再以50％的输出功率经由30min升温至目标温度400℃-700℃，最终在400℃-700℃保温12小时；
步骤十：靶材的修整：将靶材表面以1500目、2000目、2500目的砂纸依次打磨，最后以型号为DNW0.5的水溶金刚石研磨膏进行抛光处理，得到一个平整光滑的靶材表面。
2.根据权利要求1所述的一种FeSe1-xTex靶材的制备工艺，其特征在于：所述的步骤一中铁粉的纯度为99.95％，硒粉、碲粉的纯度均为99.99％。
3.根据权利要求1所述的一种FeSe1-xTex靶材的制备工艺，其特征在于：所述的步骤二、四、六、八中研磨过程都在一个充满氩气保护的、水值小于0.1ppm、氧值小于0.1ppm的手套箱中进行。
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