CN107488833B - 一种磁电薄膜材料及其制备方法 - Google Patents
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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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract
一种新型的磁电薄膜材料及其制备方法，属于功能复合材料制备技术领域。所述磁电薄膜材料包括依次沉积于非晶玻璃基片上的具有铁磁性的FeSiBC非晶材料和具有铁电性的Sm离子改性的铁酸铋，所述FeSiBC非晶材料为Fe81Si3.5B13.5C2，所述Sm离子改性的铁酸铋的化学式为Bi1‑xSmxFeO3，其中x＝0.02～0.06。本发明磁电薄膜具有优良的磁电性能，可应用于小型化或微型化的多功能电磁器件上。
Description
技术领域
本发明属于功能复合材料制备技术领域，具体涉及一种磁电薄膜材料及其制备方法。
背景技术
随着科学技术、工业发展和国防需求的进步，性能单一的材料很难满足各种高要求的综合指标，使得功能复合材料的研究成为材料科学与工程领域的研究重点。复合磁电薄膜因其具有多功能性、磁电效应等特点，在小型化及微型化的多功能电磁器件上有巨大的应用潜力。磁电薄膜是一种具有磁电转换功能的多功能复合材料，它是由两种单项材料即铁磁相和铁电相复合得到的，同时具有铁磁性能和铁电性能，而且在外电场的作用下能在一定方向上发生磁化，在外磁场的作用下能在一定方向上发生极化，可以实现磁场能量与电场能量之间的转化。
磁电薄膜材料的应用相当广泛，主要体现在微波领域、高压输电线路的电流测量、宽波段磁探测以及磁场感应器等领域。另外，作为磁电薄膜材料，还可以利用材料的本征铁磁性和铁电性的有序耦合性质，以及具有磁矩有序和电偶极子有序共存的特性，在制作探测器、高密度存储器、多态记忆元、电场控制的磁共振装置以及压磁传感器等方面应用。
发明内容
本发明的目的在于提供一种磁电薄膜材料及其制备方法，通过在玻璃基片上磁控溅射铁磁相FeSiBC薄膜和铁电相Sm离子改性的铁酸铋薄膜，得到一种性能优良的磁电薄膜，可应用于小型化或微型化的多功能电磁器件上。
一种磁电薄膜材料，其特征在于，所述磁电薄膜材料包括依次沉积于非晶玻璃基片上的具有铁磁性的FeSiBC非晶材料和具有铁电性的Sm离子改性的铁酸铋，所述FeSiBC非晶材料为Fe81Si3.5B13.5C2，所述Sm离子改性的铁酸铋的化学式为Bi1-xSmxFeO3，其中x＝0.02～0.06。
进一步地，所述FeSiBC非晶材料的厚度为0.2～2μm，所述Sm离子改性的铁酸铋的厚度为0.1～1μm。
进一步地，所述FeSiBC非晶材料采用磁控溅射法沉积于非晶玻璃基片上，其中，溅射靶材为Fe81Si3.5B13.5C2合金靶材，工作气压为0.6～1.2Pa，溅射功率为60～85W，保护气体为Ar气等惰性气体，溅射过程中提供大小为50～300Oe的平行于基片方向的外加磁场，溅射时间0.5～2h。
进一步地，所述Sm离子改性的铁酸铋采用磁控溅射法沉积于FeSiBC非晶材料上，其中，溅射靶材为按照Bi1-xSmxFeO3的化学计量比的原料通过固相合成法得到的铁电靶材，工作气压6×10-4～7×10-4Pa，溅射功率为50～70W，保护气体为Ar气等惰性气体，溅射时间0.5～2h。
一种磁电薄膜材料的制备方法，包括以下步骤：
步骤1、按照Bi1-xSmxFeO3(BSFO，x＝0.02～0.06)的化学计量比称取原料Bi2O3，Sm2O3和Fe2O3，通过固相合成法得到Sm离子改性的铁酸铋，作为铁电靶材；
步骤2、在非晶玻璃基片上采用磁控溅射法沉积FeSiBC非晶薄膜，其中，溅射靶材为Fe81Si3.5B13.5C2合金靶材，工作气压为0.6～1.2Pa，溅射功率为60～85W，保护气体为Ar气等惰性气体，溅射过程中提供大小为50～300Oe的平行于基片方向的外加磁场，溅射时间0.5～2h，溅射厚度为0.2～2μm；
步骤3、在步骤2得到的FeSiBC非晶薄膜上采用磁控溅射法沉积Sm离子改性的铁酸铋薄膜层，其中，溅射靶材为步骤1得到的铁电靶材，工作气压6×10-4～7×10-4Pa，溅射功率为50～70W，保护气体为Ar气等惰性气体，溅射时间0.5～2h，溅射厚度为0.1～1μm。
进一步地，步骤1所述原料Bi2O3，Sm2O3和Fe2O3的纯度均不低于99.99％。
进一步地，步骤2所述Fe81Si3.5B13.5C2合金靶材的纯度不低于99.99％。
本发明的有益效果为：
1、本发明提供的一种磁电薄膜材料，是采用磁控溅射法在非晶玻璃基片上依次沉积FeSiBC非晶材料和Sm离子改性的铁酸铋得到的，通过对FeSiBC非晶薄膜和BSFO薄膜的厚度以及Sm改性的铁酸铋材料中Sm离子的含量的不断调整和试验，得到了性能优良的磁电薄膜。
2、本发明提供的FeSiBC非晶材料和Sm改性的铁酸铋结合得到的新型磁电薄膜材料，从材料特性到薄膜结构，都在良好的磁电性能方面起到关键性作用，对磁电薄膜材料的研究具有重要的推动作用，并有望用于实现磁电薄膜器件的微型化和小型化，对提高器件的集成度和高密度起到很好的奠基作用。
附图说明
图1为本发明提供的一种磁电薄膜材料的结构示意图；
图2为本发明中Sm离子改性的铁酸铋铁电靶材的制备工艺流程图；
图3为实施例1得到的磁电薄膜材料的磁电效应测试曲线；
图4为实施例2得到的磁电薄膜材料的磁电效应测试曲线；
图5为实施例3得到的磁电薄膜材料的磁电效应测试曲线。
具体实施方式
下面结合附图和实施例，详述本发明的技术方案。
实施例1
一种磁电薄膜材料的制备方法，包括以下步骤：
步骤1、按照Bi0.98Sm0.02FeO3(BSFO，x＝0.02)的化学计量比，称量0.49mol的Bi2O3，0.01mol的Sm2O3和0.5mol的Fe2O3，用去离子水做磨介，一次球磨18h，烘干，在725℃下预烧结2h；然后进行二次球磨12h，加入粘合剂，压制，在820℃烧结30min，即可得到Sm离子改性的铁酸铋靶材，作为铁电靶材；
步骤2、选取市售的纯度为99.99％的Fe81Si3.5B13.5C2合金靶材作为铁磁靶材；
步骤3、选取10×5mm的非晶玻璃基片作为衬底，将非晶玻璃基片分别在无水乙醇、丙酮中超声清洗4次；
步骤4、在步骤3清洗后的非晶玻璃基片上采用磁控溅射法沉积FeSiBC非晶薄膜，其中，溅射靶材为步骤2选取的市售的Fe81Si3.5B13.5C2合金靶材，工作气压为0.8Pa，溅射功率为70W，温度为室温，保护气体为Ar气，溅射过程中提供大小为150Oe的平行于基片方向的外加磁场，溅射时间1h；
步骤5、在步骤4得到的FeSiBC非晶薄膜上采用磁控溅射法沉积Sm离子改性的铁酸铋薄膜层，其中，溅射靶材为步骤1得到的铁电靶材，工作气压6×10-4Pa，溅射功率为60W，温度为室温，保护气体为Ar气，溅射时间1h；即可得到所述磁电薄膜材料。
图3为实施例1得到的磁电薄膜材料的磁电效应测试曲线；VSM测试显示该磁电薄膜材料具有较好的磁电效应现象，在0kV/cm和2kV/cm的作用下，其磁电效应区别明显。
实施例2
实施例2与实施例1的区别在于：步骤1中Sm离子改性的铁酸铋为Bi0.96Sm0.04FeO3(BSFO，x＝0.04)，称取的原料为0.48mol的Bi2O3，0.02mol的Sm2O3和0.5mol的Fe2O3。其余步骤与实施例1相同。
图4为实施例2得到的磁电薄膜材料的磁电效应测试曲线；VSM测试显示该磁电薄膜材料具有较好的磁电效应现象，当Sm的含量x＝0.04时，基于本发明的双层结构，铁电相的作用效果更强，该薄膜材料在0kV/cm和2kV/cm的作用下，磁电效应区别明显，材料更容易被磁化饱和。
实施例3
实施例3与实施例1的区别在于：步骤1中Sm离子改性的铁酸铋为Bi0.94Sm0.06FeO3(BSFO，x＝0.06)，称取的原料为0.47mol的Bi2O3，0.03mol的Sm2O3和0.5mol的Fe2O3。其余步骤与实施例1相同。
图5为实施例3得到的磁电薄膜材料的磁电效应测试曲线；VSM测试显示该磁电薄膜材料具有较好的磁电效应现象，当Sm的含量x＝0.06时，基于本发明的双层结构，铁电相的作用更强，该薄膜材料在0kV/cm和2kV/cm的作用下，磁电效应区别更加明显。
Claims (7)
1.一种磁电薄膜材料，其特征在于，所述磁电薄膜材料包括依次沉积于非晶玻璃基片上的FeSiBC非晶材料和Sm离子改性的铁酸铋，所述FeSiBC非晶材料为Fe81Si3.5B13.5C2，所述Sm离子改性的铁酸铋的化学式为Bi1-xSmxFeO3，其中x＝0.02～0.06。
2.根据权利要求1所述的磁电薄膜材料，其特征在于，所述FeSiBC非晶材料的厚度为0.2～2μm，所述Sm离子改性的铁酸铋的厚度为0.1～1μm。
3.根据权利要求1所述的磁电薄膜材料，其特征在于，所述FeSiBC非晶材料采用磁控溅射法沉积于非晶玻璃基片上，其中，溅射靶材为Fe81Si3.5B13.5C2合金靶材，工作气压为0.6～1.2Pa，溅射功率为60～85W，保护气体为惰性气体，溅射过程中提供大小为50～300Oe的平行于基片方向的外加磁场，溅射时间0.5～2h。
4.根据权利要求1所述的磁电薄膜材料，其特征在于，所述Sm离子改性的铁酸铋采用磁控溅射法沉积于FeSiBC非晶材料上，其中，溅射靶材为按照Bi1-xSmxFeO3的化学计量比的原料通过固相合成法得到的铁电靶材，工作气压6×10-4～7×10-4Pa，溅射功率为50～70W，保护气体为惰性气体，溅射时间0.5～2h。
5.一种磁电薄膜材料的制备方法，包括以下步骤：
步骤1、按照Bi1-xSmxFeO3的化学计量比称取原料Bi2O3，Sm2O3和Fe2O3，通过固相合成法得到Sm离子改性的铁酸铋，作为铁电靶材，其中x＝0.02～0.06；
步骤2、在非晶玻璃基片上采用磁控溅射法沉积FeSiBC非晶薄膜，其中，溅射靶材为Fe81Si3.5B13.5C2合金靶材，工作气压为0.6～1.2Pa，溅射功率为60～85W，保护气体为惰性气体，溅射过程中提供大小为50～300Oe的平行于基片方向的外加磁场，溅射时间0.5～2h，溅射厚度为0.2～2μm；
步骤3、在步骤2得到的FeSiBC非晶薄膜上采用磁控溅射法沉积Sm离子改性的铁酸铋薄膜层，其中，溅射靶材为步骤1得到的铁电靶材，工作气压6×10-4～7×10-4Pa，溅射功率为50～70W，保护气体为惰性气体，溅射时间0.5～2h，溅射厚度为0.1～1μm。
6.根据权利要求5所述的磁电薄膜材料的制备方法，其特征在于，步骤1所述原料Bi2O3，Sm2O3和Fe2O3的纯度均不低于99.99％。
7.根据权利要求5所述的磁电薄膜材料的制备方法，其特征在于，步骤2所述Fe81Si3.5B13.5C2合金靶材的纯度不低于99.99％。
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