CN112500155B - 一种镧掺杂钛酸钡靶材的制备方法 - Google Patents

一种镧掺杂钛酸钡靶材的制备方法 Download PDF

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CN112500155B
CN112500155B CN202011236290.1A CN202011236290A CN112500155B CN 112500155 B CN112500155 B CN 112500155B CN 202011236290 A CN202011236290 A CN 202011236290A CN 112500155 B CN112500155 B CN 112500155B
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耿寒松
曹彦伟
张如意
裴宇娟
宋洋
毕佳畅
彭邵勤
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

本发明公开一种镧掺杂钛酸钡靶材的制备方法，包括以下步骤：1）将BaCO3和TiO2、La2O3和TiO2分别混合球磨得到两种浆料，然后将两种浆料干燥后的得到的粉料分别煅烧，制得BaTiO3、La2Ti2O7粉料；2）按一定比例将BaTiO3、La2Ti2O7粉料混合进行二次球磨后，干燥得到混合粉料；3）将干燥后的混合粉料采用聚乙烯醇溶液造粒、过筛，得到粒径均匀的粉料；4）将造粒后的粉料放入靶材模具，压制、脱模制成生坯；5）将生坯进行排胶、烧结后使用研磨抛光机将烧结成的靶材外表面抛光，清洗后干燥，得到BLTO靶材。

Description

一种镧掺杂钛酸钡靶材的制备方法
技术领域
本发明涉及溅射靶材制备技术领域，具体讲是一种镧掺杂钛酸钡（BLTO）靶材的制备方法。
背景技术
极性金属是指一种兼具铁电性与金属性的材料，非常少见。该材料是研发具有强磁电耦合特性的金属性材料的基础，有望被用于新型的自旋场效应晶体管。这里，铁电性是指某些材料中存在自发的电极化，并在外加电场的作用下电极化可以被反转的特性。经典理论认为，具有铁电性（或极性）的材料都是绝缘体，这是因为金属性材料中的导电电子会屏蔽电偶极距，从而无法产生长程的铁电序。除了探索具有非中心对称晶体结构的导电材料之外，另一种更常用的方法是通过掺杂绝缘的铁电材料来诱导金属性的产生，从而实现极性金属。但在这些体系中，铁电性随着电子密度的增加而减弱，并在某一临界密度时被完全压制。因此，阐明连续电子掺杂对铁电材料中铁电性和金属性的调控规律具有重要的意义。然而，目前相关的溅射靶材非常缺乏，严重制约了该领域的发展。
钛酸钡是一种传统的铁电材料，通过掺杂镧和生长过程中的气氛控制可能同时实现铁电性和金属性。其中，新材料前沿探索对高质量的掺杂钛酸钡靶材有大量的需求，这也是实验制备高质量薄膜材料的前提。其中操作简单易行固相烧结法是制备陶瓷材料靶材的常用方法之一。
发明内容
针对上述技术问题，本发明提供了一种高质量镧掺杂钛酸钡（BLTO）靶材的制备方法。
本发明采用的技术方案为：一种镧掺杂钛酸钡靶材的制备方法，包括以下步骤：
1）将碳酸钡（BaCO3）和二氧化钛（TiO2）、氧化镧（La2O3）和二氧化钛（TiO2）分别混合球磨得到两种浆料，然后将两种浆料干燥后的得到的粉料分别煅烧，制得钛酸钡（BaTiO3）、钛酸镧（La2Ti2O7）粉料；
2）按一定比例将BaTiO3、La2Ti2O7粉料混合进行二次球磨后，干燥得到混合粉料；
3）将干燥后的混合粉料采用聚乙烯醇溶液造粒、过筛，得到粒径均匀的粉料；
4）将造粒后的粉料放入靶材模具，压制、脱模制成生坯；
5）将生坯进行排胶、烧结后使用研磨抛光机将烧结成的靶材外表面抛光，清洗后干燥，得到BLTO靶材。
作为优化，步骤1）中，La2O3、TiO2的物质的量之比为2:1；BaCO3、TiO2的物质的量之比为1:1；球磨时间为5-7小时；干燥温度为80-120℃，干燥时间为8-10小时；制备La2Ti2O7粉料的煅烧温度为1200-1250℃，煅烧时间为3-5小时；制备BaTiO3粉料的煅烧温度为1100-1150℃，煅烧时间为3-5小时。
作为优化，步骤2）中，二次球磨过程中，La2Ti2O7、BaTiO3的物质的量之比为x/（1-2x）；其中，x为大于0小于1的任意数值。
最佳地，步骤3）中聚乙烯醇溶液浓度为5 wt.%，添加量为混合粉料重量的2%。
较佳地，步骤3）中过筛的上层为40-60目，下层为100-120目，取中间均匀粉末。
作为优化，步骤4）中靶材压制成型的压力为20-40MPa。
作为优化，步骤5）中排胶条件为在400-600℃下排胶3-4h。
作为优化，步骤5）中烧结温度为1350-1450℃，烧结时间为3-4小时。
作为进一步优化，步骤5）中烧结时的温度控制，先以5℃/min的升温速度升至900℃，再以3℃/min的升温速率升高至1350-1450℃，保温3-4小时后，再以3℃/min的降温速率降至900℃，最后自然冷却至室温。
La2Ti2O7与BaTiO3分别制备是因为两者皆为较稳定的物质，并且可以更好地以相应的比例制备固溶体。
附图说明
图1为BLTO靶材的 (a) SEM形貌图；(b) La Kα1 Mapping图；(c) Ba Kα1 Mapping图；(d) Ti Kα1 Mapping图；(e) O Kα1 Mapping图。
图2为BLTO薄膜晶面的衍射峰。
具体实施方式
下面用具体实施例对本发明做进一步详细说明，但本发明不仅局限于以下具体实施例。
实施例1
（1）将所有实验用具采用去离子水或无水乙醇超声清洗干净。
（2）按物质的量1:2比例分别称取La2O3、TiO2粉料；按物质的量1:1分别称取BaCO3、TiO2粉料，将上述称量好的粉料、无水乙醇、氧化锆球按1:1:2的比例分别置于两不同尼龙罐中，使用行星球磨机混料6小时。
（3）将均匀的浆料倒入烘箱中进行干燥，其中干燥箱温度为120℃，干燥时间为8小时。
（4）将干燥后的粉末放入坩埚，置于马弗炉中以1250℃烧结，时间为4小时，制得La2Ti2O7粉末；使用相同方法制得BaTiO3粉末，其中烧结温度为1200℃，时间为4小时。
（5）按物质的量之比1:6分别称取La2Ti2O7、BaTiO3粉料，将上述称量好的粉料、无水乙醇、氧化锆球按1:1:2的比例置于尼龙罐中，使用行星球磨机混料6小时，将均匀的浆料倒入烘箱中进行干燥。
（6）将干燥后的粉末放入坩埚，置于马弗炉中以1450℃煅烧，时间为4小时，制得BLTO粉末。
（7）将煅烧的粉料在行星磨中进行二次球磨并干燥，其中混合粉料、无水乙醇、氧化锆球之比为1:1:2。
（8）使用5wt.%聚乙烯醇进行造粒，过筛，上层筛采用60目，下层筛选择120目。取中间粉料放入2英寸的靶材模具中，在30MPa压力下压制后脱模制得生坯。
（10）将生坯在500℃下进行排胶，时间为3小时，之后放入马弗炉中进行烧结，烧结温度为1450℃，烧结时间为4小时。其中烧结时先以5℃/min的升温速率升高至900℃，再以3℃/min的升温速率升至1450℃，保温4小时，再以3℃/min的降温速率降至900℃，最后自然冷却至室温。
（11）使用研磨抛光机打磨靶材外表面，用无水乙醇超声清洗后干燥，得到BLTO（La原子与Ba原子之比为1:3）靶材。
实施例2
将所有实验器皿采用去离子水或无水乙醇超声清洗干净。按物质的量1:2比例分别称取La2O3、TiO2粉料，将上述称量好的粉料、无水乙醇、氧化锆球按1:1:2的比例置于尼龙罐中，使用行星球磨机混料6小时。将均匀的浆料倒入烘箱中进行干燥，其中干燥箱温度为120℃，干燥时间为8小时。将干燥后的粉末放入坩埚，置于马弗炉中以1200℃烧结，时间为4小时，制得钛酸镧（La2Ti2O7）粉末。按物质的量1:1分别称取BaCO3、TiO2粉料，使用上述相同方法制得BaTiO3粉末，其中烧结温度为1150℃，时间为4小时。按物质的量1:2比例分别称取La2Ti2O7、BaTiO3粉料，将上述称量好的粉料、无水乙醇、氧化锆球按1:1：2的比例置于尼龙罐中，使用行星球磨机混料6小时，将均匀的浆料倒入烘箱中进行干燥。将干燥后的粉末放入坩埚，置于马弗炉中以1450℃煅烧，时间为4小时，制得BLTO粉末。将煅烧的粉料在行星磨中进行二次球磨并干燥，使用5wt.%聚乙烯醇进行造粒，过筛，上层筛采用60目，下层筛选择120目，取中间粉料放入2英寸的靶材模具中，在20MPa压力下压制10min后脱模制得生坯。将生坯在500℃下进行排胶，时间为3小时，之后放入马弗炉中进行烧结，烧结温度为1450℃，烧结时间为4小时。其中烧结时先以5℃/min的升温速率升高至900℃，再以3℃/min的升温速率升至1450℃，保温4小时，再以3℃/min的降温速率降至900℃，最后自然冷却至室温。使用研磨抛光机打磨靶材外表面，用无水乙醇超声清洗后干燥，得到BLTO（La原子与Ba原子之比为1:1）靶材。
使用扫描电子显微镜（Scanning Electron Microscopy, SEM）结合能谱仪(Energy Dispersive Spectrometer，EDS)对得到的BLTO靶材的微区元素种类进行分析，结果显示靶材表面平整、成分纯净，La、Ba、Ti、O元素分布均匀，说明靶材质量较好。
使用射频磁控溅射在 SrTiO3(001)单晶衬底上生长BLTO薄膜，生长过程在氩气气氛下进行，生长温度为700℃，生长气压控制在0.02Torr，生长时间为5小时。之后采用高分辨X射线衍射仪对薄膜进行表征，通过XRD测量结果显示，得到了高质量单晶外延的BLTO薄膜。从而证明了制得的高质量BLTO靶材是可以应用于磁控溅射或脉冲激光沉积来制备单晶薄膜材料。
以上仅是本发明的特征实施范例，对本发明保护范围不构成任何限制。凡采用同等交换或者等效替换而形成的技术方案，均落在本发明权利保护范围之内。

Claims (9)

1.一种镧掺杂钛酸钡靶材的制备方法，其特征在于，包括以下步骤：
1）将BaCO3和TiO2、La2O3和TiO2分别混合球磨得到两种浆料，然后将两种浆料干燥后的得到的粉料分别煅烧，制得BaTiO3、La2Ti2O7粉料；
2）按一定比例将BaTiO3、La2Ti2O7粉料混合进行二次球磨后，干燥得到混合粉料；
3）将干燥后的混合粉料采用聚乙烯醇溶液造粒、过筛，得到粒径均匀的粉料；
4）将造粒后的粉料放入靶材模具，压制、脱模制成生坯；
5）将生坯进行排胶、烧结后使用研磨抛光机将烧结成的靶材外表面抛光，清洗后干燥，得到BLTO靶材。
2.根据权利要求1所述的镧掺杂钛酸钡靶材的制备方法，其特征在于，步骤1）中，La2O3、TiO2的物质的量之比为1:2；BaCO3、TiO2的物质的量之比为1:1；球磨时间为5-7小时；干燥温度为80-120℃，干燥时间为8-10小时；制备La2Ti2O7粉料的煅烧温度为1200-1250℃，煅烧时间为3-5小时；制备BaTiO3粉料的煅烧温度为1100-1150℃，煅烧时间为3-5小时。
3.根据权利要求1所述的镧掺杂钛酸钡靶材的制备方法，其特征在于，步骤2）中，二次球磨过程中，La2Ti2O7、BaTiO3的物质的量之比为x/（1-2x）；其中，x为大于0小于1的任意数值。
4.根据权利要求1所述的镧掺杂钛酸钡靶材的制备方法，其特征在于，步骤3）中聚乙烯醇溶液浓度为5 wt.%，添加量为混合粉料重量的2%。
5.根据权利要求1所述的BLTO 靶材的制备方法，其特征在于，步骤3）中过筛的上层为40-60目，下层为100-120目，取中间均匀粉末。
6.根据权利要求1所述的镧掺杂钛酸钡靶材的制备方法，其特征在于，步骤4）中靶材压制成型的压力为20-40MPa。
7.根据权利要求1所述的镧掺杂钛酸钡靶材的制备方法，其特征在于，步骤5）中排胶条件为在400-600℃下排胶3-4h。
8.根据权利要求1所述的镧掺杂钛酸钡靶材的制备方法，其特征在于，步骤5）中烧结温度为1350-1450℃，烧结时间为3-4小时。
9.根据权利要求1所述的镧掺杂钛酸钡靶材的制备方法，其特征在于，步骤5）中烧结时的温度控制，先以5℃/min的升温速度升至900℃，再以3℃/min的升温速率升高至1350-1450℃，保温3-4小时后，再以3℃/min的降温速率降至900℃，最后自然冷却至室温。
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