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CN109267020B - 一种铝氮钪合金靶材的制备方法和应用 - Google Patents

一种铝氮钪合金靶材的制备方法和应用 Download PDF

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CN109267020B
CN109267020B CN201811144407.6A CN201811144407A CN109267020B CN 109267020 B CN109267020 B CN 109267020B CN 201811144407 A CN201811144407 A CN 201811144407A CN 109267020 B CN109267020 B CN 109267020B
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丁照崇
李勇军
何金江
王兴权
雷继锋
庞欣
贺昕
刘晓
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Grinm Advanced Materials Co ltd
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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    • C22C29/16—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides
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    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0068—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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Abstract

本发明公开了属于磁控溅射靶材制备技术领域的一种铝氮钪合金靶材的制备方法和应用。该方法以AlN粉、Sc粉为原料，经混合、压力烧结成型、机加工得到铝氮钪合金靶材，所得铝氮钪合金靶材的相对密度大于97％，能够应用于溅射沉积氮化物膜，溅射镀膜过程中，无需通入反应气体氮气即能稳定成膜。

Description

一种铝氮钪合金靶材的制备方法和应用
技术领域
本发明属于磁控溅射靶材制备技术领域，特别涉及一种铝氮钪合金靶材的制备方法和应用。
背景技术
在新型微机电系统(MEMS)及射频滤波器等领域，铝氮钪薄膜由于具有优异的压电耦合系数，成为当前研究的热点。目前的现有技术，主要通过反应溅射铝钪合金靶来沉积铝氮钪薄膜，在溅射过程中需持续通入氮气，以作为反应气体；由于溅射过程中氮气会和靶材发生很强的电化学反应，靶面易覆盖一层化合物，使得溅射刻蚀区域异常放电，影响镀膜性能；此外，制造出的氮化物膜层中氮原子易缺失，造成薄膜合金成分比例失配。
发明内容
本发明的目的在于提供一种铝氮钪合金靶材的制备方法和应用，具体技术方案如下：
一种铝氮钪合金靶材的制备方法包括以下步骤：
(1)配料：按照目标铝氮钪合金靶材的合金成分，以AlN粉、Sc粉为原料进行配比；
其中，原料粉AlN粉粒径优选为0.1～50μm，Sc粉粒径优选为1～150μm。
(2)混粉：利用混料机将原料粉末均匀混合，或利用球磨机球磨、均匀混合；
(3)压力烧结：将步骤(2)所得混合粉末热压烧结或热等静压烧结成靶坯，其中烧结温度为1250～1520℃，压力为30～150MPa，保温保压时间为4～6h；
其中，步骤(2)中混粉过程、步骤(3)压力烧结过程均在真空条件或惰性气氛下进行，以避免原料粉末氧化；其中，真空度大于0.1Pa，惰性气体为Ar或其他不与原料粉发生反应的惰性气体。
(4)将步骤(3)所得靶坯机加工成铝氮钪合金单体成品靶材；所得铝氮钪合金靶材中铝氮钪合金(AlN)1-xScx，x为0.1％～99.9％，余量为AlN；靶材的相对密度达到97％以上。
其中，还可采用常用技术手段包括焊接、咬合等方式，将步骤(3)所得靶坯经机加工后固定于背板上得到铝氮钪复合成品靶材。
利用所述制备方法制备的铝氮钪合金靶材或铝氮钪复合成品靶材，能够应用于溅射沉积氮化物膜。相比于现有技术，由于在块体靶材中已合金化氮，在溅射镀膜过程中，无需通入反应气体氮气，即可稳定地将铝、钪与氮的反应物按所需的化学配比稳定成膜，所得镀膜不易异常放电、工艺窗口宽、稳定性好。
本发明的有益效果为：本发明采用易于制造或购买的AlN、Sc粉为原料，利用压力烧结成型制备铝氮钪合金靶材，工艺简单，适合大批量工业化生产；所得靶材致密度高、不易开裂，应用于溅射镀膜中，能显著改善现有技术中存在的膜层氮原子缺失问题，即能确保薄膜合金成分比例。
附图说明
附图1为本发明铝氮钪合金靶材的制备方法流程图。
具体实施方式
本发明提供了一种铝氮钪合金靶材的制备方法和应用，下面结合实施例和附图对本发明做进一步的说明。
实施例1～8
根据附图1所示方法制备铝氮钪合金靶材：
(1)配料
按照表1中铝氮钪合金靶材成分，进行原材料配料：靶材化学成分为(AlN)1-xScx，其中，Sc质量含量x为1～99％，余量为AlN；其中AlN粉粒径0.1～50μm，Sc粉粒径1～150μm。
(2)混粉
将配比的两种原料放入混料机或球磨机内球磨混合均匀；混合过程中，为了防止粉末氧化，混料机或球磨机处于真空状态或利用惰性气体Ar气保护。
(3)压力烧结
将混合粉末采用热压烧结或热等静压烧结成靶坯，其中烧结温度为1250～1520℃，压力为30～150MPa，保温保压时间为4～6h。
(4)机加工/焊接
对压力烧结靶坯进行机加工制造出铝氮钪合金单体成品靶材，或机加工后与背板焊接为复合成品靶材。
实施例1～8铝氮钪合金靶材的主要制造工艺及性能结果见表1，从表1可以看出，实施例1～8制备的铝氮钪合金靶材相对密度均大于97％，致密度强、不易开裂。
表1
Figure BDA0001816468550000041

Claims (7)

1.一种铝氮钪合金靶材的制备方法，其特征在于，以AlN粉、Sc粉为原料，经混合、压力烧结成型、机加工得到铝氮钪合金靶材，其中铝氮钪合金(AlN)1-xScx，x为0.1％～99.9％；
所述压力烧结为热压烧结或热等静压烧结，压力烧结的烧结温度为1250～1520℃，压力为30～150MPa，保温保压时间为4～6h。
2.根据权利要求1所述的制备方法，其特征在于，所述AlN粉粒径0.1～50μm，Sc粉粒径1～150μm。
3.根据权利要求1所述的制备方法，其特征在于，所述混合在混料机或球磨机中进行。
4.根据权利要求1所述的制备方法，其特征在于，所述混合、压力烧结均在真空条件或惰性气氛下进行。
5.根据权利要求4所述的制备方法，其特征在于，所述真空度大于0.1Pa。
6.根据权利要求1所述的制备方法，其特征在于，所述铝氮钪合金靶材的相对密度达到97％以上。
7.权利要求1～6任一项所述制备方法制备的铝氮钪合金靶材应用于溅射沉积氮化物膜，其特征在于，无需通入反应气体氮气。
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