CN110590375A - 氮化铝掺氮化钪靶材的生产工艺 - Google Patents

氮化铝掺氮化钪靶材的生产工艺 Download PDF

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CN110590375A
CN110590375A CN201910970535.4A CN201910970535A CN110590375A CN 110590375 A CN110590375 A CN 110590375A CN 201910970535 A CN201910970535 A CN 201910970535A CN 110590375 A CN110590375 A CN 110590375A
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scandium
powder
aluminum nitride
nitride
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吴文斌
舒小敏
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JIANGXI KETAI NEW MATERIALS CO Ltd
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Abstract

本发明公开了一种氮化铝掺氮化钪靶材的生产工艺，将高纯钪金属和铝金属粉末冷压成疏松块状，分别装入坩埚，移入真空加热炉，抽真空，通入氮气，采用程度升温气固合成法分别合成ScN、AlN，破碎、球磨成‑100目粉末。ScN、AlN粉末检验合格后，按规定比例混合，以此为原料进行热压烧结，制得氮化铝掺氮化钪靶坯。对靶坯进行机械加工得到靶材。本发明采用程序升温气固合成技术分别合成氮化铝、氮化钪，制成粉末，然后通过真空热压烧结成型技术，制备规定比例的氮化铝掺氮化钪靶材，制备出的氮化铝掺氮化钪靶材是SAW厂家制备Sc掺杂氮化铝功能薄膜的前端产品，质量好、性能优异。

Description

氮化铝掺氮化钪靶材的生产工艺
技术领域
本发明涉及氮化铝掺氮化钪靶材的生产技术领域，涉及一种氮化铝掺氮化钪靶材的生产技术。
背景技术
压电薄膜材料是制备薄膜声表面波(Surface Acoustic Wave， SAW)器件的关键材料，其性能决定着SAW器件的性能。氮化铝是一种良好的压电薄膜材料，具有高声波波速、高热导率、 低介质损耗、 优异的温度稳定性、 可与 CMOS 工艺兼容等优点， 是制备高频、高功率及高集成化SAW 器件的理想材料。在AlN中掺入ScN（与Sc掺杂AlN是一回事，不同说法而已）可有效提升AlN较低的压电系数和机电耦合系数，改善AlN作为压电薄膜材料的性能，从而制备出性能更优秀的SAW器件。 目前，国内外制备Sc掺杂AlN薄膜，大多采用反应溅射的方式，将铝钪金属靶材装入反应溅射设备，抽真空后，通入氩气和氮气，氩气是工作气体，氮气是反应气体。在电磁作用下，电离后的氩正离子沿一定夹角方向轰击铝钪金属靶表面，铝钪金属成份从靶材表面逸出，沿轰击方向的对称方向飞出，飞向基材表面，在溅射过程中铝钪金属与氮气发生反应，生成AlN和ScN沉积在基材表面，结晶，形成一层功能薄膜。这种反应溅射方式制备薄膜的方法要同时兼顾溅射镀膜和化合反应，似是一举两得，其实制备条件难控制，如铝、钪与氮气反应条件的差异、反应条件与溅射条件的差异、氮气客串工作气体的问题等，这些差异和问题及其衍生的深层次问题都要综合考虑。虽然通过研究可获得一套综合最优的工作参数，但因为要反应和溅射两者兼顾，必然会有一些自身难以克服的缺点。如制备过程中的靶材中毒现象、薄膜中会可能存在未完全氮化的金属杂质或低价氮化物、薄膜可能会出现部分非晶态、薄膜的形貌可能不令人满意等，从而产生成本增加、生产效率降低、薄膜性能不高等诸多不利因素。
发明内容
为了克服上述现有技术的不足，本发明一种氮化铝掺氮化钪靶材的生产工艺。采用程序升温气固合成技术分别合成氮化铝、氮化钪，制成粉末，然后通过真空热压烧结成型技术，制备规定比例的氮化铝掺氮化钪靶材。
本发明一种碲化锌掺碲化亚铜靶材的生产工艺，包括以下步骤：
(1)、程序升温气固合成技术分别合成氮化铝、氮化钪
Ⅰ、 合成AlN ：将99.99%以上纯度的铝粉冷压成疏松块状，装入坩埚中，将坩埚移入真空加热炉，抽真空至1~5Pa，通入氮气至100~200kPa，加热，500~600 0C保温0.5h，除去铝粉表面氧化物。继续加热到800~850 0C，保温1~2h，使铝粉与氮气充分反应，随炉冷却至室温，取出合成产物，破碎，球磨，重复上述过程，在1100~12000C二次氮化0.5h，随炉冷却，做XRD测试，无AlN物相以外的杂相为合格。将合格的产物破碎、球磨至-300目AlN粉末待用。
Ⅱ、合成ScN：将99.99%以上纯度的钪粉冷压成疏松块状，装入坩埚中，将坩埚移入真空加热炉，抽真空至1~5Pa，通入氮气至100~200kPa，加热到800~900 0C，保温1~2h，使钪粉与氮气充分反应，随炉冷却至室温，取出合成产物，破碎，球磨，随炉冷却，做XRD测试，无ScN物相以外的杂相为合格。如有未氮化的金属钪需进行二次氮化。将合格的产物破碎、球磨至-300目ScN粉末待用。
（2）热压烧结成形
将上述制得的粉末，按理论比例预先算好的用量，装入模具中，移入真空热压炉内烧结成形，烧结温度1500~16000C，施加压力12~25MPa，烧结时间30~80min，得到氮化铝掺氮化钪靶材的毛坯。
（3）将制得的靶材进行结构、成分等测试，并进行磁控溅射成膜，通过薄膜性能测试获得靶材的质量信息。
进一步，还包括以下步骤：热压烧结成形的氮化铝掺氮化钪毛坯经热处理，热处理温度0.4Tm，再经水切割、外圆磨、平面磨、机床加工、抛光等机械加工工序制成可出售的靶材。尺寸上可按客户要求。其指标为：
1）、相对密度99%以上；
2）、纯度为99.99%以上，主要杂质含量之和小于100μg/g；
3）、晶粒尺寸≤50μm。
本发明采用程序升温气固合成技术分别合成氮化铝、氮化钪，制成粉末，然后通过真空热压烧结成型技术，制备规定比例的氮化铝掺氮化钪靶材，制备出的氮化铝掺氮化钪靶材是SAW厂家制备Sc掺杂氮化铝功能薄膜的前端产品，将氮化铝掺氮化钪靶材产品提供给SAW器件厂家，SAW器件厂家可使用氮化铝掺氮化钪靶材进行磁控溅射镀膜，不需要在镀膜的同时还要兼顾铝钪与氮气反应的问题，这样制备薄膜的方法，制备条件易控制、稳定，制备过程中的机理简单，制备的薄膜成份均匀、致密、质量好、性能优异。
具体实施方式
实施例1
本发明一种碲化锌掺碲化亚铜靶材的生产工艺，包括以下步骤：
(1)、程序升温气固合成技术分别合成氮化铝、氮化钪
Ⅰ、 合成AlN ：将99.99%以上纯度的铝粉冷压成疏松块状，装入坩埚中，将坩埚移入真空加热炉，抽真空至3Pa，通入氮气至120kPa，加热，500 0C保温0.5h，除去铝粉表面氧化物。继续加热到800 0C，保温1h，使铝粉与氮气充分反应，随炉冷却至室温，取出合成产物，破碎，球磨，重复上述过程，在11000C二次氮化0.5h，随炉冷却，做XRD测试，无AlN物相以外的杂相为合格。将合格的产物破碎、球磨至-300目AlN粉末待用。
Ⅱ、合成ScN：将99.99%以上纯度的钪粉冷压成疏松块状，装入坩埚中，将坩埚移入真空加热炉，抽真空至3Pa，通入氮气至120kPa，加热到800 0C，保温1h，使钪粉与氮气充分反应，随炉冷却至室温，取出合成产物，破碎，球磨，随炉冷却，做XRD测试，无ScN物相以外的杂相为合格。如有未氮化的金属钪需进行二次氮化。将合格的产物破碎、球磨至-300目ScN粉末待用。
（2）热压烧结成形
将上述制得的粉末，按理论比例预先算好的用量，装入模具中，移入真空热压炉内烧结成形，烧结温度15000C，施加压力12MPa，烧结时间30min，得到氮化铝掺氮化钪靶材的毛坯。
（3）将制得的靶材进行结构、成分等测试，并进行磁控溅射成膜，通过薄膜性能测试获得靶材的质量信息。
实施例2
一种碲化锌掺碲化亚铜靶材的生产工艺，包括以下步骤：
(1)、程序升温气固合成技术分别合成氮化铝、氮化钪
Ⅰ、 合成AlN ：将99.999%纯度的铝粉冷压成疏松块状，装入坩埚中，将坩埚移入真空加热炉，抽真空至5Pa，通入氮气至200kPa，加热， 600 0C保温0.5h，除去铝粉表面氧化物。继续加热到850 0C，保温2h，使铝粉与氮气充分反应，随炉冷却至室温，取出合成产物，破碎，球磨，重复上述过程，在12000C二次氮化0.5h，随炉冷却，做XRD测试，无AlN物相以外的杂相为合格。将合格的产物破碎、球磨至-300目AlN粉末待用。
Ⅱ、合成ScN：将99.999%以上纯度的钪粉冷压成疏松块状，装入坩埚中，将坩埚移入真空加热炉，抽真空至5Pa，通入氮气至200kPa，加热到900 0C，保温2h，使钪粉与氮气充分反应，随炉冷却至室温，取出合成产物，破碎，球磨，随炉冷却，做XRD测试，无ScN物相以外的杂相为合格。如有未氮化的金属钪需进行二次氮化。将合格的产物破碎、球磨至-300目ScN粉末待用。
（2）热压烧结成形
将上述制得的粉末，按理论比例预先算好的用量，装入模具中，移入真空热压炉内烧结成形，烧结温度16000C，施加压力25MPa，烧结时间80min，得到氮化铝掺氮化钪靶材的毛坯。
（3）将制得的靶材进行结构、成分等测试，并进行磁控溅射成膜，通过薄膜性能测试获得靶材的质量信息。
进一步，还包括以下步骤：热压烧结成形的氮化铝掺氮化钪毛坯经热处理，热处理温度0.4Tm，再经水切割、外圆磨、平面磨、机床加工、抛光等机械加工工序制成可出售的靶材。尺寸上可按客户要求。其指标为：
1）、相对密度99%以上；
2）、纯度为99.99%以上，主要杂质含量之和小于100μg/g；
3）、晶粒尺寸≤50μm。

Claims (2)

1.一种氮化铝掺氮化钪靶材的生产工艺，其特征在于，包括如下步骤：
程序升温气固合成技术分别合成氮化铝、氮化钪,
Ⅰ、 合成AlN ：将99.99%以上纯度的铝粉冷压成疏松块状，装入坩埚中，将坩埚移入真空加热炉，抽真空至1~5Pa，通入氮气至100~200kPa，加热，500~600 0C保温0.5h，除去铝粉表面氧化物;
继续加热到800~850 0C，保温1~2h，使铝粉与氮气充分反应，随炉冷却至室温，取出合成产物，破碎，球磨，重复上述过程，在1100~12000C二次氮化0.5h，随炉冷却，做XRD测试，无AlN物相以外的杂相为合格;
将合格的产物破碎、球磨至-300目AlN粉末待用;
Ⅱ、合成ScN：将99.99%以上纯度的钪粉冷压成疏松块状，装入坩埚中，将坩埚移入真空加热炉，抽真空至1~5Pa，通入氮气至100~200kPa，加热到800~900 0C，保温1~2h，使钪粉与氮气充分反应，随炉冷却至室温，取出合成产物，破碎，球磨，随炉冷却，做XRD测试，无ScN物相以外的杂相为合格;
如有未氮化的金属钪需进行二次氮化;
将合格的产物破碎、球磨至-300目ScN粉末待用;
（2）热压烧结成形, 将上述制得的粉末，按理论比例预先算好的用量，装入模具中，移入真空热压炉内烧结成形，烧结温度1500~16000C，施加压力12~25MPa，烧结时间30~80min，得到氮化铝掺氮化钪靶材的毛坯;
（3）将制得的靶材进行结构、成分等测试，并进行磁控溅射成膜，通过薄膜性能测试获得靶材的质量信息。
2.根据权利要求1所述的一种氮化铝掺氮化钪靶材的生产工艺，其特征在于还包括以下步骤：热压烧结成形的氮化铝掺氮化钪毛坯经热处理，热处理温度0.4Tm，再经水切割、外圆磨、平面磨、机床加工、抛光等机械加工工序制成可出售的靶材;
其指标为：
1）、相对密度99%以上；
2）、纯度为99.99%以上，主要杂质含量之和小于100μg/g；
3）、晶粒尺寸≤50μm。
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111962021A (zh) * 2020-08-28 2020-11-20 江西科泰新材料有限公司 氮化铝掺氮化钪镀膜材料
CN112133800A (zh) * 2020-08-27 2020-12-25 西安电子科技大学 基于高温扩散形成p型ScAlN层的高效发光二极管及制备方法
CN112723893A (zh) * 2021-02-02 2021-04-30 邱从章 一种氮化铝钪靶材及其制备方法
CN112962071A (zh) * 2021-02-02 2021-06-15 长沙淮石新材料科技有限公司 一种掺杂的氮化铝钪靶材及其制备方法和应用

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105483615A (zh) * 2014-09-18 2016-04-13 清华大学 具有闪锌矿结构的磁性氮化铝薄膜材料及其制备方法与应用

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105483615A (zh) * 2014-09-18 2016-04-13 清华大学 具有闪锌矿结构的磁性氮化铝薄膜材料及其制备方法与应用

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
姚守拙等: "《元素化学反应手册》", 31 July 1998, 湖南教育出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112133800A (zh) * 2020-08-27 2020-12-25 西安电子科技大学 基于高温扩散形成p型ScAlN层的高效发光二极管及制备方法
CN111962021A (zh) * 2020-08-28 2020-11-20 江西科泰新材料有限公司 氮化铝掺氮化钪镀膜材料
CN112723893A (zh) * 2021-02-02 2021-04-30 邱从章 一种氮化铝钪靶材及其制备方法
CN112962071A (zh) * 2021-02-02 2021-06-15 长沙淮石新材料科技有限公司 一种掺杂的氮化铝钪靶材及其制备方法和应用

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