CN114231951A - 利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法 - Google Patents
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 7
- 229920003169 water-soluble polymer Polymers 0.000 claims description 6
- 229910002340 LaNiO3 Inorganic materials 0.000 claims description 4
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- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 3
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- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明公开了利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,涉及导电薄膜技术领域,包括以下步骤:步骤S1:原料的准备;步骤S2:预处理,衬底清洗;衬底切片;步骤S3:前驱体制备,将步骤S1中的所述La源和所述Ni源进行混合、干燥、压制、一次煅烧和二次煅烧;步骤S4:放置和准备;步骤S5:制备;步骤S6:退火工艺;步骤S7:质检,对薄膜的质量进行检查,将结果数据进行统一和整合。本发明具备了通过脉冲激光沉积法,并辅以高分子材料的添加可提高原料的混合效果,使得制备后的导电薄膜具有优良的导电性能,和工艺简便,其表面粗糙度较小,具有实用性更佳的效果。
Description
技术领域
本发明涉及导电薄膜技术领域,具体为利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法。
背景技术
在电子器件方面,具有导电性的导电薄膜具有较为重要的使用前景。
目前现有的导电薄膜的制备方法中,常采用化学溶剂混合进行制备,因其方式步骤简单,使得制成的导电薄膜表面的均匀程度和电阻率较高。
发明内容
本发明的目的在于提供利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,具备了通过脉冲激光沉积法,并辅以高分子材料的添加可提高原料的混合效果,使得制备后的导电薄膜具有优良的导电性能,和工艺简便,其表面粗糙度较小,具有实用性更佳的效果,解决了上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,包括以下步骤:
步骤S1:原料的准备,将La2O3作为La源;将Ni2O3作为Ni源;并准备水溶性高分子材料、衬底、脉冲激光装置和沉积室;
步骤S2:预处理,衬底清洗;衬底切片;
步骤S3:前驱体制备,将步骤S1中的所述La源和所述Ni源进行混合、干燥、压制、一次煅烧和二次煅烧;
步骤S4:放置和准备,对所述沉积室进行抽真空;将步骤S3处理后的前驱体和步骤S2中处理好的衬底和所述脉冲激光装置一起置入所述沉积室内,并进行安装;
步骤S5:制备,打开所述脉冲激光装置进行外延生长,通过控制所述脉冲激光装置交替溅射在所述前驱体上,将所述前驱体进行沉积,得到薄膜前驱体;
步骤S6:退火工艺,采用层层退火工艺对步骤S5处理好的所述薄膜前驱体进行热处理,得到LaNiO3薄膜;
步骤S7:质检,对薄膜的质量进行检查,将结果数据进行统一和整合。
可选的,所述步骤S2中的衬底清洗,是采用玻璃清洗剂和去离子水依次对所述衬底进行清洗,并辅以超声波装置进行潮湿处理10-20min。
可选的,所述步骤S2中的衬底切片,是将每个衬底进行切割,并对衬底进行不同斜切角度的切割。
可选的,所述步骤S3中的混合,是将所述La源、所述Ni源、水所述水溶性高分子材料通过研磨和搅拌进行混合。
可选的,所述步骤S3中的压制,是将所述La源和所述Ni源形成的混合料置于磨具中进行压制,从而得到靶材前驱体。
可选的,所述步骤S3中的所述一次煅烧和所述二次煅烧之间进行再次的混合和压制。
可选的,所述步骤S4中还包括对所述衬底进行加热,同时向所述沉积室内通入少量氧气。
可选的,所述步骤S6中的热处理,是在氧气气氛下从350℃升温到450℃处理10min再提升温度至600℃,在氮气气氛下退火20分钟,退火温度为600℃。
与现有技术相比,本发明的有益效果如下:
一、本发明通过利用高分子材料可使得La源和Ni源的混合效果更佳,并辅以压制成型,和两次煅烧,使得La源和Ni源结合更为紧密。
二、本发明通过层层的退火工艺,且通过对温度的精准把控,可提高制备后LaNiO3薄膜表面的均匀程度和极化程度,使得其表面粗糙程度减少,电阻率较低。
三、本发明通过水溶性高分子材料的添加,可以在降低水表面的张力,可有助于水对固体的润湿,提高了内部原料的混合效果。
四、本发明通过对一次煅烧后的产物进行研磨和压制,使得可提高La源与Ni源的混合均匀程度,使得可加速La源与Ni源的反应速度。
五、本发明通过通入少量的氧气,可补充薄膜中的氧元素出现的损失,通过对衬底进行加热,使得可提高作业效率,保证了衬底的质量。
附图说明
图1为本发明结构的的方法流程图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
请参阅图1,本发明提供一种技术方案:利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,包括以下步骤:
步骤S1:原料的准备,将La2O3作为La源;将Ni2O3作为Ni源;并准备水溶性高分子材料、衬底、脉冲激光装置和沉积室。
步骤S2:预处理,衬底清洗;衬底切片,对衬底进行预处理,使得衬底满足设计需求,保证了后续的薄膜的成膜质量。
步骤S3:前驱体制备,将步骤S1中的La源和Ni源进行混合、干燥、压制、一次煅烧和二次煅烧,通过利用高分子材料可使得La源和Ni源的混合效果更佳,并辅以压制成型,和两次煅烧,使得La源和Ni源结合更为紧密。
步骤S4:放置和准备,对沉积室进行抽真空;将步骤S3处理后的前驱体和步骤S2中处理好的衬底和脉冲激光装置一起置入沉积室内,并进行安装,保证了沉积室的真空环境,在安装部件时,调整部件的位置,使得前驱体与衬底和脉冲激光装置之间的正对角度符合设计需求。
步骤S5:制备,打开脉冲激光装置进行外延生长,通过控制脉冲激光装置交替溅射在前驱体上,将前驱体进行沉积,得到薄膜前驱体,通过沉积法制成的薄膜其均匀程度较好,表面较为平顺和光滑,且操作便捷,实用性更佳。
步骤S6:退火工艺,采用层层退火工艺对步骤S5处理好的薄膜前驱体进行热处理,得到LaNiO3薄膜,通过层层的退火工艺,且通过对温度的精准把控,可提高制备后LaNiO3薄膜表面的均匀程度和极化程度,使得其表面粗糙程度减少,电阻率较低。
步骤S7:质检,对薄膜的质量进行检查,将结果数据进行统一和整合,通过输入至物联网中,达到数据的整合、集中和实时监控处理的效果。
进一步的,步骤S2中的衬底清洗,是采用玻璃清洗剂和去离子水依次对衬底进行清洗,并辅以超声波装置进行潮湿处理10-20min,通过玻璃清洗剂和去离子水依次的清理,使得可对衬底进行多重高效的清理,使得衬底保持洁净性,保住了后续薄膜的质量。
进一步的,步骤S2中的衬底切片,是将每个衬底进行切割,并对衬底进行不同斜切角度的切割,通过不同斜切角度的切割,使得值得后的薄膜其介电损耗有所降低,实用性更佳。
为了对后续的沉积法制备薄膜起辅助加速的效果,进一步的,步骤S3中的混合,是将La源、Ni源、水水溶性高分子材料通过研磨和搅拌进行混合,通过水溶性高分子材料的添加,可以在降低水表面的张力,可有助于水对固体的润湿,提高了内部原料的混合效果。
为了使得前驱体的质量符合设计规范,进一步的,步骤S3中的压制,是将La源和Ni源形成的混合料置于磨具中进行压制,从而得到靶材前驱体,压力优选为150~250MPa,使得得到的靶材前驱体的结构稳定性更佳。
为了提高原料之间的混合均匀程度,进一步的,步骤S3中的一次煅烧和二次煅烧之间进行再次的混合和压制,对一次煅烧后的产物进行研磨和压制,使得可提高La源与Ni源的混合均匀程度,使得可加速La源与Ni源的反应速度。
为了提高后续的作业效率,进一步的,步骤S4中还包括对衬底进行加热,同时向沉积室内通入少量氧气,通过通入少量的氧气,可补充薄膜中的氧元素出现的损失,通过对衬底进行加热,使得可提高作业效率,保证了衬底的质量。
为了使得薄膜之间的结构更为紧密,进一步的,步骤S6中的热处理,是在氧气气氛下从350℃升温到450℃处理10min再提升温度至600℃,在氮气气氛下退火20分钟,退火温度为600℃,通过此种热处理工艺,可以减少导电薄膜中的氧空位浓度,降低了薄膜的室温电阻。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (8)
1.利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,其特征在于:包括以下步骤:
步骤S1:原料的准备,将La2O3作为La源;将Ni2O3作为Ni源;并准备水溶性高分子材料、衬底、脉冲激光装置和沉积室;
步骤S2:预处理,衬底清洗;衬底切片;
步骤S3:前驱体制备,将步骤S1中的所述La源和所述Ni源进行混合、干燥、压制、一次煅烧和二次煅烧;
步骤S4:放置和准备,对所述沉积室进行抽真空;将步骤S3处理后的前驱体和步骤S2中处理好的衬底和所述脉冲激光装置一起置入所述沉积室内,并进行安装;
步骤S5:制备,打开所述脉冲激光装置进行外延生长,通过控制所述脉冲激光装置交替溅射在所述前驱体上,将所述前驱体进行沉积,得到薄膜前驱体;
步骤S6:退火工艺,采用层层退火工艺对步骤S5处理好的所述薄膜前驱体进行热处理,得到LaNiO3薄膜;
步骤S7:质检,对薄膜的质量进行检查,将结果数据进行统一和整合。
2.根据权利要求1所述的利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,其特征在于:所述步骤S2中的衬底清洗,是采用玻璃清洗剂和去离子水依次对所述衬底进行清洗,并辅以超声波装置进行潮湿处理10-20min。
3.根据权利要求1或2所述的利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,其特征在于:所述步骤S2中的衬底切片,是将每个衬底进行切割,并对衬底进行不同斜切角度的切割。
4.根据权利要求1所述的利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,其特征在于:所述步骤S3中的混合,是将所述La源、所述Ni源、水所述水溶性高分子材料通过研磨和搅拌进行混合。
5.根据权利要求1或2所述的利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,其特征在于:所述步骤S3中的压制,是将所述La源和所述Ni源形成的混合料置于磨具中进行压制,从而得到靶材前驱体。
6.根据权利要求1所述的利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,其特征在于:所述步骤S3中的所述一次煅烧和所述二次煅烧之间进行再次的混合和压制。
7.根据权利要求1所述的利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,其特征在于:所述步骤S4中还包括对所述衬底进行加热,同时向所述沉积室内通入少量氧气。
8.根据权利要求1或2所述的利用高分子辅助沉积法制备LaNiO3外延导电薄膜的方法,其特征在于:所述步骤S6中的热处理,是在氧气气氛下从350℃升温到450℃处理10min再提升温度至600℃,在氮气气氛下退火20分钟,退火温度为600℃。
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