CN108611618A - 一种磁控溅射沉积铁膜和氧化铁膜的方法 - Google Patents

一种磁控溅射沉积铁膜和氧化铁膜的方法 Download PDF

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CN108611618A
CN108611618A CN201810817871.0A CN201810817871A CN108611618A CN 108611618 A CN108611618 A CN 108611618A CN 201810817871 A CN201810817871 A CN 201810817871A CN 108611618 A CN108611618 A CN 108611618A
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iron
film
magnetron sputtering
oxide film
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高斐
高蓉蓉
武鑫
王昊旭
雷婕
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Shaanxi Normal University
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021Reactive sputtering or evaporation
    • C23C14/0036Reactive sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • C23C14/085Oxides of iron group metals
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/18Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering

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Abstract

本发明公开了一种磁控溅射沉积铁膜和氧化铁膜的方法,通过在靶枪和铁靶中间安插一定厚度的非铁磁性的金属圆片,如铝圆片、铜圆片等,来降低铁靶的磁屏蔽效应,从而可成功地溅射沉积铁膜及氧化铁膜。本发明方法操作简单,制得的铁膜及氧化铁膜致密,且均匀性好,与基底的结合力好,制得的铁膜具有较好的铁电特性。

Description

一种磁控溅射沉积铁膜和氧化铁膜的方法
技术领域
本发明属于溅射镀膜技术领域,具体涉及一种用磁控溅射制备铁膜及氧化铁膜的方法。
背景技术
磁控溅射技术可制备装饰薄膜、硬质薄膜、耐腐蚀摩擦薄膜、超导薄膜、磁性薄膜、光学薄膜,以及各种具有特殊功能的薄膜,是一种十分有效的薄膜沉积方法,在各个工业领域应用非常广泛。磁控溅射所得到的薄膜附着力强。磁控溅射的基本原理即是以磁场改变电子运动方向,束缚和延长电子的运动轨迹,提高了电子对工作气体的电离率和有效利用了电子的能量,使正离子对靶材轰击引起的靶材溅射更有效。但对于铁这种靶材而言,用常规磁控溅射方法难以沉积铁膜及氧化铁膜。这是由于其铁具有高导磁性,大部分磁场从铁靶材内部通过,严重的磁屏蔽使铁靶材表面的磁场过小,将导致无法进行磁控溅射沉积铁膜及氧化铁膜。
发明内容
本发明所要解决的技术问题在于解决上述磁控溅射制备铁膜和氧化铁膜所存在的铁靶磁屏蔽问题,提出在靶枪和铁靶中间安插一定厚度的非磁性的材料,来降低铁靶的磁屏蔽效应,从而可成功地溅射沉积铁膜及氧化铁膜。
解决上述技术问题所采用的技术方案是:在靶枪和铁靶之间放一个非铁磁性的金属圆片,采用磁控溅射在玻璃衬底上沉积一层铁膜或氧化铁膜。
上述非铁磁性的金属圆片具体可以是铝圆片、铜圆片等,其厚度为3~5mm,直径与铁靶相同。
采用本发明方法磁控溅射沉积铁膜的具体操作过程为:将清洗干净的玻璃衬底装在磁控溅射设备的样品夹具上,将非铁磁性的金属圆片放在靶枪上面,接着将铁靶放在非铁磁性的金属圆片上,关上磁控溅射设备的真空室盖子,用机械泵和分子泵将沉积室抽真空至5.0×10-4~7.0×10-4Pa,接着打开氩气通气阀,并打开质量流量计,控制氩气流速为25.0~30.0sccm,先调节沉积室压强至1.5~2.0Pa、溅射功率为28~30W启辉,再调节沉积室压强至0.5~0.6Pa、溅射功率至110~115W,预溅射1~2分钟以除去铁靶表面的污染,接着打开挡板开始沉积,沉积结束后自然冷却至室温,即得到铁膜。
采用本发明方法磁控溅射沉积氧化铁膜的具体操作过程为:将清洗干净的玻璃衬底装在磁控溅射设备的样品夹具上,将非铁磁性的金属圆片放在靶枪上面,接着将铁靶放在非铁磁性的金属圆片上,关上磁控溅射设备的真空室盖子,用机械泵和分子泵将沉积室抽真空至5.0×10-4~7.0×10-4Pa,接着打开氩气通气阀和氧气通气阀,并打开质量流量计,控制氧气流速为10.0~15.0sccm、氩气流速为15.0~20.0sccm,并控制氩气和氧气的总流速为25.0~30.0sccm,先调节沉积室压强至1.5~2.0Pa、溅射功率为28~30W启辉,再调节沉积室压强至0.5~0.6Pa、溅射功率至110~115W,预溅射1~2分钟以除去铁靶表面的污染,接着打开挡板开始沉积,沉积结束后自然冷却至室温,即得到氧化铁膜。
本发明的有益效果如下:
本发明通过在靶枪和铁靶中间安插一定厚度的非铁磁性的金属圆片,来降低铁靶的磁屏蔽效应,从而可成功地溅射沉积铁膜及氧化铁膜。本发明方法操作简单,制得的铁膜及氧化铁膜致密,且均匀性好,制得的铁膜具有较好的铁电特性。
附图说明
图1是实施例1所沉积的铁膜的X射线衍射图谱。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明,但本发明的保护范围不仅限于这些实施例。
实施例1
将玻璃衬底用蘸有乙醇的无尘纸擦拭干净,然后再将玻璃衬底依次在丙酮、乙醇中超声清洗30分钟,用氮气吹干,装在磁控溅射设备的样品夹具上。将3mm厚的铝圆片放在靶枪上面,接着将铁靶放在铝圆片上,铝圆片的大小与铁靶相同。关上磁控溅射设备的真空室盖子,用机械泵和分子泵将沉积室抽真空至5.0×10-4Pa,接着打开氩气通气阀,并打开质量流量计,控制氩气流速为30.0sccm,先调节沉积室压强至2.0Pa、溅射功率为30W启辉,再调节沉积室压强至0.6Pa、溅射功率至110W,预溅射1分钟以除去铁表面的污染,接着打开挡板开始沉积,沉积时间为25分钟,沉积结束后,自然冷却至室温,得到厚度为570~580nm的铁膜。图1是所沉积的铁膜的X射线衍射图谱。由图可见,在2θ角度为45.39°处出现了铁晶面(002)的衍射峰。
实施例2
本实施例中,打开氩气通气阀和氧气通气阀,并打开质量流量计,控制氧气流速为10.0sccm、氩气流速为20.0sccm,其他步骤与实施例1相同,得到厚度为570~580nm的氧化铁膜。
实施例3
本实施例中,用3mm厚的铜圆片替换实施例1中的铝圆片,其他步骤与实施例1相同,得到厚度为570~580nm的氧化铁膜。
实施例4
本实施例中,用3mm厚的铜圆片替换实施例2中的铝圆片,其他步骤与实施例2相同,得到厚度为570~580nm的氧化铁膜。

Claims (5)

1.一种磁控溅射沉积铁膜和氧化铁膜的方法,其特征在于:在靶枪和铁靶之间放一个非铁磁性的金属圆片,采用磁控溅射在玻璃衬底上沉积一层铁膜或氧化铁膜。
2.根据权利要求1所述的磁控溅射沉积铁膜和氧化铁膜的方法,其特征在于:所述非铁磁性的金属圆片为铝圆片或铜圆片。
3.根据权利要求2所述的磁控溅射沉积铁膜和氧化铁膜的方法,其特征在于:所述铝圆片或铜圆片的厚度为3~5mm,直径与铁靶相同。
4.根据权利要求1~3任意一项所述的磁控溅射沉积铁膜和氧化铁膜的方法,其特征在于磁控溅射沉积铁膜的具体操作过程为:将清洗干净的玻璃衬底装在磁控溅射设备的样品夹具上,将非铁磁性的金属圆片放在靶枪上面,接着将铁靶放在非铁磁性的金属圆片上,关上磁控溅射设备的真空室盖子,用机械泵和分子泵将沉积室抽真空至5.0×10-4~7.0×10-4Pa,接着打开氩气通气阀,并打开质量流量计,控制氩气流速为25.0~30.0sccm,先调节沉积室压强至1.5~2.0Pa、溅射功率为28~30W启辉,再调节沉积室压强至0.5~0.6Pa、溅射功率至110~115W,预溅射1~2分钟以除去铁靶表面的污染,接着打开挡板开始沉积,沉积结束后自然冷却至室温,即得到铁膜。
5.根据权利要求1~3任意一项所述的磁控溅射沉积铁膜和氧化铁膜的方法,其特征在于:其特征在于磁控溅射沉积氧化铁膜的具体操作过程为:将清洗干净的玻璃衬底装在磁控溅射设备的样品夹具上,将非铁磁性的金属圆片放在靶枪上面,接着将铁靶放在非铁磁性的金属圆片上,关上磁控溅射设备的真空室盖子,用机械泵和分子泵将沉积室抽真空至5.0×10-4~7.0×10-4Pa,接着打开氩气通气阀和氧气通气阀,并打开质量流量计,控制氧气流速为10.0~15.0sccm、氩气流速为15.0~20.0sccm,并控制氩气和氧气的总流速为25.0~30.0sccm,先调节沉积室压强至1.5~2.0Pa、溅射功率为28~30W启辉,再调节沉积室压强至0.5~0.6Pa、溅射功率至110~115W,预溅射1~2分钟以除去铁靶表面的污染,接着打开挡板开始沉积,沉积结束后自然冷却至室温,即得到氧化铁膜。
CN201810817871.0A 2018-07-23 2018-07-23 一种磁控溅射沉积铁膜和氧化铁膜的方法 Pending CN108611618A (zh)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4401546A (en) * 1981-03-27 1983-08-30 Nihon Shinku Gijutsu Kabushiki Kaisha Ferromagnetic high speed sputtering apparatus
CN102330060A (zh) * 2011-09-27 2012-01-25 中国科学院金属研究所 用于电弧离子镀沉积磁性材料涂层的复合结构靶材及应用
CN105603371A (zh) * 2015-10-29 2016-05-25 杭州立昂微电子股份有限公司 一种磁性溅射靶材

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4401546A (en) * 1981-03-27 1983-08-30 Nihon Shinku Gijutsu Kabushiki Kaisha Ferromagnetic high speed sputtering apparatus
CN102330060A (zh) * 2011-09-27 2012-01-25 中国科学院金属研究所 用于电弧离子镀沉积磁性材料涂层的复合结构靶材及应用
CN105603371A (zh) * 2015-10-29 2016-05-25 杭州立昂微电子股份有限公司 一种磁性溅射靶材

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Application publication date: 20181002