CN107742579A - 锆钛酸钡薄膜压控变容管的制备方法 - Google Patents
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- 239000010409 thin film Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 239000010408 film Substances 0.000 claims abstract description 18
- 238000000151 deposition Methods 0.000 claims abstract description 15
- 230000008021 deposition Effects 0.000 claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004549 pulsed laser deposition Methods 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 9
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000007772 electrode material Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 claims description 2
- 238000002207 thermal evaporation Methods 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEAHHGDAQKXNNG-UHFFFAOYSA-H C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-].[Zr+4].[Ba+2].C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-].C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-] Chemical compound C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-].[Zr+4].[Ba+2].C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-].C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-] VEAHHGDAQKXNNG-UHFFFAOYSA-H 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- H01G7/06—Capacitors in which the capacitance is varied by non-mechanical means; Processes of their manufacture having a dielectric selected for the variation of its permittivity with applied voltage, i.e. ferroelectric capacitors
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- C—CHEMISTRY; METALLURGY
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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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
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Abstract
本发明公开了一种锆钛酸钡薄膜压控变容管的制备方法，先按BaZr0.2Ti0.8O3的化学计量比，称取原料BaCO3、ZrO2和TiO2，于1200℃烧制BaZr0.2Ti0.8O3即BZT靶材；再将Pt‑Si衬底放入脉冲激光沉积制品台上，将脉冲激光沉积系统的本底真空抽至P＜4.0×10‑4Pa，然后加热衬底至350～750℃；打开进气阀，向系统中通入氧气，在Pt‑Si衬底上沉积得到厚度为150‑300nm的BaZr0.2Ti0.8O3薄膜；再在BaZr0.2Ti0.8O3薄膜上面利用掩膜版制备金属电极，制得锆钛酸钡薄膜压控变容管。本发明锆钛酸钡薄膜压控变容管的调谐率≥60％，测试频率为100kHz，且器件稳定性好，制备工艺简单、电学性能优良，具有良好的应用前景。
Description
技术领域
本发明是关于于电子信息材料与元器件的，具体涉及锆钛酸钡薄膜压控变容管及其制备方法。
背景技术
近年来，随着电子信息技术迅速发展，雷达面临着隐身飞行器、高速反辐射导弹、综合电子干扰和超低空突防等威胁。因此，对雷达性能的要求越来越高。相控阵雷达是采用多种高科技技术的产物，具有波束捷变的特点，可以满足对高性能雷达系统日益增长的需求。在相控阵雷达中，移相器是馈电系统重要的基本原件，其基本功能是改变微波信号的相位，紧连天线的辐射源与T/R组件，通过波控器控制移相器改变各阵元间的相对馈电相位，从而改变天线阵面上电磁波的相位分布。目前，移相器普遍采用铁氧体压控材料实现，这种材料的介电损耗很高，要求电路提供很高的控制电压，不利于系统小型化、低功耗和低成本的发展要求。利用微波介质压控材料的调谐特性，可实现对相控阵雷达系统的电子控制，介质移相器更适合在现代相控阵雷达系统中使用。
锆钛酸钡(BaZrxTi1-xO3，BZT)为Zr4+部分取代BaTiO3中的Ti4+，而形成的BaTiO3(BT)基钙钛矿氧化物，具有良好的压控调谐性能，此外Zr4+比Ti4+化学稳定性更好，Zr4+取代Ti4+之后将会抑制Ti4+与Ti3+之间的电子跃迁，从而减小了漏电流。我们利用脉冲激光沉积技术在Pt-Si衬底上沉积BZT薄膜，所得到的BZT调谐薄膜变容管的调谐率达到60％以上。因此，BZT薄膜在微波调谐介质器件中具有良好的应用前景。
发明内容
本发明的目的，利用脉冲激光沉积技术，提供一种制备高调谐率锆钛酸钡薄膜压控薄膜变容管的制备方法。本发明利用微波介质压控材料的调谐特性，可实现对相控阵雷达系统的电子控制，使介质移相器更适合在现代相控阵雷达系统中使用。
本发明通过如下技术方案予以实现。
一种锆钛酸钡薄膜压控变容管的制备方法，具体步骤如下：
(1)采用固相烧结法制备BZT靶材
按BaZr0.2Ti0.8O3的化学计量比，称取原料BaCO3、ZrO2和TiO2，充分混合后压制成型为坯体，坯体置于电炉中于1200℃烧制BaZr0.2Ti0.8O3即BZT靶材；
(2)将清洁干燥的Pt-Si衬底放入脉冲激光沉积制品台上，靶基距为4～10cm；
(3)将脉冲激光沉积系统的本底真空抽至P＜4.0×10-4Pa，然后加热衬底至350～750℃；
(4)打开进气阀，向步骤(3)系统中通入氧气，氧气压强为0.8～60Pa，在Pt-Si衬底上沉积得到厚度为150-300nm的BaZr0.2Ti0.8O3薄膜；
(5)步骤(4)停止后，待衬底温度降至100℃以下时，取出制品；
(6)在BaZr0.2Ti0.8O3薄膜上面利用掩膜版制备金属电极，制得锆钛酸钡薄膜压控变容管。
所述步骤(1)的原料纯度在99％以上。
所述步骤(4)的O2的纯度在99.99％以上，脉冲激光沉积系统中氧气压强为0.8Pa～60Pa。
所述步骤(4)通过调节靶基距或者沉积时间控制薄膜厚度。
所述步骤(6)的电极为圆形电极，直径≤0.3mm，电极厚度为100～600nm，电极材料为Au或Pt；电极制备方法为热蒸镀法或者溅射法。
所锆钛酸钡薄膜压控变容管的调谐率≥60％，测试频率为100kHz。
本发明公开的锆钛酸钡薄膜压控变容管调谐率高(≥60％，测试频率为100kHz)，且器件稳定性好，制备工艺流程简单、电学性能优良，具有良好的应用前景。
具体实施方式
下面结合具体实施例进一步阐述本发明，应理解，这些实施例仅用于说明本发明而不用于限制本发明的保护范围。
实施例1
1.采用固相烧结法制备BZT靶材，用电子天平按BaZr0.2Ti0.8O3对应化学计量比称取BaCO3、ZrO2和TiO2，原料质量纯度均为99％。经充分混合后压制成型为坯体，坯体置于箱式电炉中逐步升温至1200℃，并保温6小时，制得BaZr0.2Ti0.8O3(BZT)靶材。
2.将Pt-Si衬底经丙酮、乙醇和去离子水标准超声清洗，以N2吹干并放入脉冲激光沉积制品台上，靶基距为6cm。
3.将脉冲激光沉积系统的本底真空抽至3.0×10-4Pa，然后加热衬底，衬底温度为700℃。
4.通入高纯(99.99％)O2，氧气压强为0.8Pa，在Pt-Si衬底上沉积得到厚度250nm的BaZr0.2Ti0.8O3薄膜，通过调节靶基距或者沉积时间控制薄膜厚度。
5.待衬底温度降至100℃以下时，取出制品；
6.采用孔洞直径为0.2mm的掩膜版，在BaZr0.2Ti0.8O3薄膜上面沉积厚度为400nm的Au顶电极，制得锆钛酸钡薄膜压控变容管。
所制得的锆钛酸钡薄膜压控变容管制品的介电性能(电场可调)在400kV/cm的电场下调谐率为62％。
实施例2
1.采用固相烧结法制备BZT靶材，用电子天平按BaZr0.2Ti0.8O3对应化学计量比称取BaCO3、ZrO2和TiO2，原料质量纯度均为99％。经充分混合后压制成型最后置于箱式电炉中逐步升温至1200℃，并保温6小时，制得BaZr0.2Ti0.8O3靶材。
2.将Pt-Si衬底经丙酮、乙醇和去离子水标准超声清洗，以N2吹干并放入脉冲激光沉积制品台上，靶基距为6cm。
3.将脉冲激光沉积系统的本底真空抽至3.0×10-4Pa，然后加热衬底，衬底温度为700℃。
4.通入高纯(99.99％)O2，氧气压强为15Pa，在Pt-Si衬底上沉积得到厚度250nm的BaZr0.2Ti0.8O3薄膜，通过调节靶基距或者沉积时间控制薄膜厚度。
5.待衬底温度降至100℃以下时，取出制品；
6.采用孔洞直径为0.2mm的掩膜版，在BaZr0.2Ti0.8O3薄膜上面沉积厚度为400nm的Au顶电极，制得锆钛酸钡薄膜压控变容管。
所制得的锆钛酸钡薄膜压控变容管制品的介电性能(电场可调)在400kV/cm的电场下调谐率为70％。
Claims (6)
1.一种锆钛酸钡薄膜压控变容管的制备方法，具体步骤如下：
(1)采用固相烧结法制备BZT靶材
按BaZr0.2Ti0.8O3的化学计量比，称取原料BaCO3、ZrO2和TiO2，充分混合后压制成型为坯体，坯体置于电炉中于1200℃烧制BaZr0.2Ti0.8O3即BZT靶材；
(2)将清洁干燥的Pt-Si衬底放入脉冲激光沉积制品台上，靶基距为4～10cm；
(3)将脉冲激光沉积系统的本底真空抽至P＜4.0×10-4Pa，然后加热衬底至350～750℃；
(4)打开进气阀，向步骤(3)系统中通入氧气，氧气压强为0.8～60Pa，在Pt-Si衬底上沉积得到厚度为150-300nm的BaZr0.2Ti0.8O3薄膜；
(5)步骤(4)停止后，待衬底温度降至100℃以下时，取出制品；
(6)在BaZr0.2Ti0.8O3薄膜上面利用掩膜版制备金属电极，制得锆钛酸钡薄膜压控变容管。
2.根据权利要求所述的锆钛酸钡薄膜压控变容管的制备方法，其特征在于，所述步骤(1)的原料纯度在99％以上。
3.根据权利要求所述的锆钛酸钡薄膜压控变容管的制备方法，其特征在于，所述步骤(4)的O2的纯度在99.99％以上，脉冲激光沉积系统中氧气压强为0.8Pa～60Pa。
4.根据权利要求所述的锆钛酸钡薄膜压控变容管的制备方法，其特征在于，所述步骤(4)通过调节靶基距或者沉积时间控制薄膜厚度。
5.根据权利要求所述的锆钛酸钡薄膜压控变容管的制备方法，其特征在于，所述步骤(6)的电极为圆形电极，直径≤0.3mm，电极厚度为100～600nm，电极材料为Au或Pt；电极制备方法为热蒸镀法或者溅射法。
6.根据权利要求所述的锆钛酸钡薄膜压控变容管的制备方法，其特征在于，所锆钛酸钡薄膜压控变容管的调谐率≥60％，测试频率为100kHz。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531867A (zh) * | 2018-03-28 | 2018-09-14 | 天津大学 | 一种柔性bts/bzt/bts多层薄膜变容管的制备方法 |
| CN109112484A (zh) * | 2018-08-24 | 2019-01-01 | 西安交通大学 | 一种高可靠性bzt无铅外延单晶储能薄膜及其制备方法 |
| CN113215549A (zh) * | 2021-05-08 | 2021-08-06 | 南京邮电大学 | 一种基于射频磁控溅射的锆钛酸钡薄膜退火方法 |
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| CN109112484A (zh) * | 2018-08-24 | 2019-01-01 | 西安交通大学 | 一种高可靠性bzt无铅外延单晶储能薄膜及其制备方法 |
| CN113215549A (zh) * | 2021-05-08 | 2021-08-06 | 南京邮电大学 | 一种基于射频磁控溅射的锆钛酸钡薄膜退火方法 |
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