CN106835045A - 一种钛酸钡薄膜的制备方法 - Google Patents

一种钛酸钡薄膜的制备方法 Download PDF

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CN106835045A
CN106835045A CN201710082174.0A CN201710082174A CN106835045A CN 106835045 A CN106835045 A CN 106835045A CN 201710082174 A CN201710082174 A CN 201710082174A CN 106835045 A CN106835045 A CN 106835045A
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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
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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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Abstract

本发明公开了一种钛酸钡薄膜的制备方法，该制备方法采用BaTiO3作为靶材，在经过特殊工艺处理过的绝缘基片上，采用离子溅射工艺沉积得到BaTiO3薄膜材料，该方法显著改善和控制了材料的组织结构，使得衬底和钛酸钡完美匹配，得到的产品稳定性高，性能优良。

Description

一种钛酸钡薄膜的制备方法
技术领域
本发明涉及半导体材料制造领域，具体涉及一种钛酸钡薄膜的制备方法。
背景技术
高介电常数的BaTiO3薄膜在嵌入式电容和高储能元件等领域有重要的应用前景，近年来引起了广泛关注，但因衬底和薄膜之间失配引起的残余应力及氧空位迁移、再分布等引起的漏电流更是吸引了人们的目光。
实验过程中发现多层BaTiO3薄膜形成的同质界面的势垒高度也要大于晶界形成的背靠背的双肖特基势垒高度。此外，研究表明面内压应力可以提高BaTiO3基-多层陶瓷电容器的介电常数（平行于衬底表面）。而随着薄膜厚度的增加，残余压应力呈下降趋势。因此有必要研发一种以阻碍氧空位的迁移，增加BaTiO3薄膜面内压应力，同时可以起到降低介电损耗和提高介电常数作用的多层薄膜结构。
总之，现有技术中的钛酸钡薄膜，存在稳定性差、纯度低、对制备工艺条件要求高等问题。
发明内容
本发明提供一种钛酸钡薄膜的制备方法，该制备方法采用BaTiO3作为靶材，在经过特殊工艺处理过的绝缘基片上，采用离子溅射工艺沉积得到BaTiO3薄膜材料，该方法显著改善和控制了材料的组织结构，使得衬底和钛酸钡完美匹配，得到的产品稳定性高，性能优良。
为了实现上述目的，本发明提供了一种钛酸钡薄膜的制备方法，该方法包括如下步骤：
（1）基片处理
将绝缘基片切削研磨后，将绝缘基片依次用洗洁精、去离子水超声清洗10-15min，然后用质量百分数35％的浓氨水/质量百分数20％的双氧水/去离子水的混合溶液65-75℃处理20-25min，所述浓氨水、双氧水和去离子水的体积比为1:3:4，最后用去离子水超声清洗150-200s，取出、用干燥氮气吹干；
（2）制备钛酸钡靶材
将纳米BaTiO3粉末在1000℃下压制成直径为75-100mm的BaTiO3靶材；
将BaTiO3靶材依次用无水乙醇、去离子水中分别清洗5-10min，以将BaTiO3靶材表面的杂质清洁干净，然后再在烘箱中将BaTiO3靶材烘干；
（3）将上述干燥后的绝缘基片的温度调至100-150℃，采用磁控溅射法，将所述钛酸钡靶材在所述绝缘基片上制成所述铁磁半导体薄膜材料；
磁控溅射制成所述铁磁半导体薄膜材料的具体条件为，溅射腔压强1-5Pa，溅射腔气氛为氩气，溅射功率为12-15W/cm2，沉积速率为10-100nm/min，溅射时间为3-5h。
优选的，在所述步骤（1）中，所述切削需利用切削液进行，该切削液采用如下工艺制得：
向水中依次加入聚乙二醇、羟乙基乙二胺、三乙醇胺，混合均匀，静置20min，再加入FA/QB螯合剂，混合搅拌均匀，静置30min，得到切削液，其中切削液的各组分的重量百分比为：聚乙二醇15-25%，羟乙基乙二胺20-25%，三乙醇胺5-10%，FA/QB螯合剂10-15%，余量为水。
具体实施方式
实施例一
将绝缘基片切削研磨后，将绝缘基片依次用洗洁精、去离子水超声清洗10min，然后用质量百分数35％的浓氨水/质量百分数20％的双氧水/去离子水的混合溶液65℃处理20min，所述浓氨水、双氧水和去离子水的体积比为1:3:4，最后用去离子水超声清洗150s，取出、用干燥氮气吹干。所述切削需利用切削液进行，该切削液采用如下工艺制得：向水中依次加入聚乙二醇、羟乙基乙二胺、三乙醇胺，混合均匀，静置20min，再加入FA/QB螯合剂，混合搅拌均匀，静置30min，得到切削液，其中切削液的各组分的重量百分比为：聚乙二醇15%，羟乙基乙二胺20%，三乙醇胺5%，FA/QB螯合剂10%，余量为水。
将纳米BaTiO3粉末在1000℃下压制成直径为75mm的BaTiO3靶材。
将BaTiO3靶材依次用无水乙醇、去离子水中分别清洗5min，以将BaTiO3靶材表面的杂质清洁干净，然后再在烘箱中将BaTiO3靶材烘干。
将上述干燥后的绝缘基片的温度调至100℃，采用磁控溅射法，将所述钛酸钡靶材在所述绝缘基片上制成所述铁磁半导体薄膜材料。
磁控溅射制成所述铁磁半导体薄膜材料的具体条件为，溅射腔压强1Pa，溅射腔气氛为氩气，溅射功率为12W/cm2，沉积速率为10nm/min，溅射时间为3h。
实施例二
将绝缘基片切削研磨后，将绝缘基片依次用洗洁精、去离子水超声清洗15min，然后用质量百分数35％的浓氨水/质量百分数20％的双氧水/去离子水的混合溶液75℃处理25min，所述浓氨水、双氧水和去离子水的体积比为1:3:4，最后用去离子水超声清洗200s，取出、用干燥氮气吹干。所述切削需利用切削液进行，该切削液采用如下工艺制得：向水中依次加入聚乙二醇、羟乙基乙二胺、三乙醇胺，混合均匀，静置20min，再加入FA/QB螯合剂，混合搅拌均匀，静置30min，得到切削液，其中切削液的各组分的重量百分比为：聚乙二醇25%，羟乙基乙二胺25%，三乙醇胺10%，FA/QB螯合剂15%，余量为水。
将纳米BaTiO3粉末在1000℃下压制成直径为100mm的BaTiO3靶材。
将BaTiO3靶材依次用无水乙醇、去离子水中分别清洗10min，以将BaTiO3靶材表面的杂质清洁干净，然后再在烘箱中将BaTiO3靶材烘干。
将上述干燥后的绝缘基片的温度调至150℃，采用磁控溅射法，将所述钛酸钡靶材在所述绝缘基片上制成所述铁磁半导体薄膜材料。
磁控溅射制成所述铁磁半导体薄膜材料的具体条件为，溅射腔压强5Pa，溅射腔气氛为氩气，溅射功率为15W/cm2，沉积速率为100nm/min，溅射时间为5h。

Claims (2)

1.一种钛酸钡薄膜的制备方法，该方法包括如下步骤：
（1）基片处理
将绝缘基片切削研磨后，将绝缘基片依次用洗洁精、去离子水超声清洗10-15min，然后用质量百分数35％的浓氨水/质量百分数20％的双氧水/去离子水的混合溶液65-75℃处理20-25min，所述浓氨水、双氧水和去离子水的体积比为1:3:4，最后用去离子水超声清洗150-200s，取出、用干燥氮气吹干；
（2）制备钛酸钡靶材
将纳米BaTiO3粉末在1000℃下压制成直径为75-100mm的BaTiO3靶材；
将BaTiO3靶材依次用无水乙醇、去离子水中分别清洗5-10min，以将BaTiO3靶材表面的杂质清洁干净，然后再在烘箱中将BaTiO3靶材烘干；
（3）将上述干燥后的绝缘基片的温度调至100-150℃，采用磁控溅射法，将所述钛酸钡靶材在所述绝缘基片上制成所述铁磁半导体薄膜材料；
磁控溅射制成所述铁磁半导体薄膜材料的具体条件为，溅射腔压强1-5Pa，溅射腔气氛为氩气，溅射功率为12-15W/cm2，沉积速率为10-100nm/min，溅射时间为3-5h。
2.如权利要求1所述的方法，其特征在于，在所述步骤（1）中，所述切削需利用切削液进行，该切削液采用如下工艺制得：
向水中依次加入聚乙二醇、羟乙基乙二胺、三乙醇胺，混合均匀，静置20min，再加入FA/QB螯合剂，混合搅拌均匀，静置30min，得到切削液，其中切削液的各组分的重量百分比为：聚乙二醇15-25%，羟乙基乙二胺20-25%，三乙醇胺5-10%，FA/QB螯合剂10-15%，余量为水。
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CN112490309A (zh) * 2020-12-07 2021-03-12 中国科学院长春光学精密机械与物理研究所 一种薄膜紫外探测器及其制备方法

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CN106319464A (zh) * 2016-08-20 2017-01-11 苏州思创源博电子科技有限公司 一种在钨合金基底上制备钛酸钡薄膜的方法

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CN112490309A (zh) * 2020-12-07 2021-03-12 中国科学院长春光学精密机械与物理研究所 一种薄膜紫外探测器及其制备方法
CN112490309B (zh) * 2020-12-07 2022-10-25 中国科学院长春光学精密机械与物理研究所 一种薄膜紫外探测器及其制备方法

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