CN107663633B - 一种掺杂碳纳米管的氧化硅阻变薄膜的制备方法 - Google Patents
一种掺杂碳纳米管的氧化硅阻变薄膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种掺杂碳纳米管的氧化硅阻变薄膜的制备方法,包括以下步骤:步骤1,分别制备氧化硅溶胶和碳纳米管‑无水乙醇混合溶液;步骤2,先按照20:0.5‑1的体积比分别量取经步骤1得到的氧化硅溶胶和碳纳米管‑无水乙醇混合溶液,然后将量取后的氧化硅溶胶和碳纳米管‑无水乙醇混合溶液混合,并在密封条件下搅拌均匀,得到碳纳米管‑氧化硅混合溶液;步骤3,选取基板,并采用浸渍提拉法使基板在经步骤3得到碳纳米管‑氧化硅混合溶液中提拉成膜,制备出碳纳米管‑氧化硅凝胶薄膜,之后对制备出的碳纳米管‑氧化硅凝胶薄膜进行热处理,最终得到掺杂碳纳米管的氧化硅阻变薄膜。
Description
技术领域
本发明属于储存器薄膜材料制备技术领域,具体涉及一种掺杂碳纳米管的氧化硅阻变薄膜的制备方法。
背景技术
阻变存储器薄膜材料最早开发的是钙钛矿氧化物,如PCMO、LSMO等。之后作为过渡,金属二元氧化物以其成分简单、易于制备所需化学配比的氧化物、成本低、与CMOS工艺兼容等优点而受到极大的关注,并且得到众多半导体厂商的青睐;许多基于该类材料的阻变存储器具有双极性的存储特性,即通过施加极性相反的电压,电阻值可在高低两个状态之间进行可逆转换。但是阻变存储器在运行的过程中,存在易击穿、易疲劳以及耐电压能力差的缺点,致使其阻变性能较差,发展受到较大限制。
发明内容
本发明的目的是提供一种掺杂碳纳米管的氧化硅阻变薄膜的制备方法,解决阻变器件存在易击穿、易疲劳以及耐电压能力差的问题。
本发明所采用的技术方案是,一种掺杂碳纳米管的氧化硅阻变薄膜的制备方法,具体按照以下步骤实施:
具体按照以下步骤实施:
步骤1,以碳纳米管粉末为溶质,无水乙醇为溶剂,制备浓度为10-5g/mL的碳纳米管溶液;
步骤2,按照20:0.5-1的体积比分别量取氧化硅溶胶、经步骤1制备得到的碳纳米管溶液,将量取后的氧化硅溶胶和碳纳米管溶液混合并搅拌均匀,得到掺杂碳纳米管的氧化硅溶液;
步骤3,选取基板,将基板置于经步骤2得到的掺杂碳纳米管的氧化硅溶液中,并采用浸渍提拉法在其表面提拉一层凝胶薄膜;
步骤4,在惰性气体的保护下,对经步骤3提拉出的凝胶薄膜进行热处理,最终得到掺杂碳纳米管的氧化硅阻变薄膜。
本发明的特点还在于:
在所述步骤3中:所述基板的材质为铂。
在所述步骤4中:所述热处理的温度为200℃-700℃。
在所述步骤4中:所述热处理的时间为20min-30min。
在所述步骤4中:所述惰性气体为氩气。
本发明的有益效果是:本发明的制备方法无需复杂的制备工艺简便、工艺参数易于控制,能大大地降低生产成本;利用本发明制备方法制备出的掺杂碳纳米管的氧化硅阻变薄膜作为应用在阻变存储器上时,该阻变存储器在运行过程中不易击穿、而且抗疲劳性好和耐电压能力也好,具有较好的阻变性能。
附图说明
图1是利用本发明制备方法制备出的掺杂碳纳米管的氧化硅阻变薄膜在电子显微镜下的扫描图;
图2是利用本发明制备方法制备出的掺杂碳纳米管的氧化硅阻变薄膜在空气中进行热处理的电学性能测试图;
图3是利用本发明的通过制备方法制备出的掺杂碳纳米管的氧化硅阻变薄膜在氩气保护下进行热处理的电学性能测试图。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
本发明掺杂碳纳米管的氧化硅阻变薄膜的制备方法,具体按照以下步骤实施:
步骤1,以碳纳米管粉末为溶质,无水乙醇为溶剂,制备浓度为10-5g/mL的碳纳米管溶液;
步骤2,按照20:0.5-1的体积比分别量取氧化硅溶胶、经步骤1制备得到的碳纳米管溶液,将量取后的氧化硅溶胶和碳纳米管溶液混合并搅拌均匀,得到掺杂碳纳米管的氧化硅溶液;
步骤3,选取基板,基板的材质为铂,将基板置于经步骤2得到的掺杂碳纳米管的氧化硅溶液中,并采用浸渍提拉法在其表面提拉一层凝胶薄膜;
步骤4,在氩气保护下,用200℃-700℃的温度对经步骤3提拉出的凝胶薄膜进行20min-30min热处理,最终得到掺杂碳纳米管的氧化硅阻变薄膜。
如图1所示,通过本发明制备方法制备得到的掺杂碳纳米管的氧化硅阻变薄膜,由尺寸均匀的微粒构成,其表面较为平整,微粒的尺寸在15nm-20nm之间,微粒的高度在1.26nm-1.47nm之间,表面粗糙度在0.146nm-0.976nm。
在步骤4进行热处理的过程中,随着热处理温度的升高,碳纳米管会被逐渐氧化成为二氧化碳,故热处理时可采用氩氢保护气对碳纳米管进行保护。具体可采用气氛管式烧结炉,气氛管式烧结炉的型号NBD-T1700。
基板在渡上通过本发明制备方法制备得到的掺杂碳纳米管的氧化硅阻变薄膜后,放入溅射仪(溅射仪的型号为SBC-12,北京中科科仪技术发展有限责任公司生产)中进行电极溅射,电极溅射完毕后即得到阻变存储器,该阻变存储器具有掺杂碳纳米管的氧化硅阻变薄膜。采用吉时利电流电压源表(keithley公司生产,型号为2400)对这种阻变存储器的电阻反转特性的进行电学性能分析,结果如图3所示。
可通过上述方法制备另一个阻变存储器,不过该阻变存储器具有的掺杂碳纳米管的氧化硅阻变薄膜是通过本发明制备方法在空气中进行热处理得到的。采用吉时利电流电压源表(keithley公司生产,型号为2400)对该阻变存储器的电阻反转特性的进行电学性能分析,结果如图2所示。
由图2和图3可知,两个阻变存储器的负向电压的扫描区都呈现单极性,但是图3中阻变存储器的电阻转变效应明显优于图2中阻变存储器的电阻转变效应;图3中阻变存储器在加负向电压时,开始是高阻态,电流几乎为0,但是从-2V左右开始,阻态发生明显变化,呈现低组态,耐电压可达到-4.0V;图2中阻变存储器则看不到明显的阻态变化,耐电压只能达到-2.0V。
实施例1
本发明掺杂碳纳米管的氧化硅阻变薄膜的制备方法,具体按照以下步骤实施:
步骤1,以碳纳米管粉末为溶质,无水乙醇为溶剂,制备浓度为10-5g/mL的碳纳米管溶液;
步骤2,按照20:0.5的体积比分别量取氧化硅溶胶、经步骤1制备得到的碳纳米管溶液,将量取后的氧化硅溶胶和碳纳米管溶液混合并搅拌均匀,得到掺杂碳纳米管的氧化硅溶液;
步骤3,选取基板,将基板置于经步骤2得到的掺杂碳纳米管的氧化硅溶液中,并采用浸渍提拉法在其表面提拉一层凝胶薄膜;
步骤4,在氩气保护下,用200℃的温度对经步骤3提拉出的凝胶薄膜进行20min热处理,最终得到掺杂碳纳米管的氧化硅阻变薄膜。
实施例2
本发明掺杂碳纳米管的氧化硅阻变薄膜的制备方法,具体按照以下步骤实施:
步骤1,以碳纳米管粉末为溶质,无水乙醇为溶剂,制备浓度为10-5g/mL的碳纳米管溶液;
步骤2,按照20:0.6的体积比分别量取氧化硅溶胶、经步骤1制备得到的碳纳米管溶液,将量取后的氧化硅溶胶和碳纳米管溶液混合并搅拌均匀,得到掺杂碳纳米管的氧化硅溶液;
步骤3,选取基板,将基板置于经步骤2得到的掺杂碳纳米管的氧化硅溶液中,并采用浸渍提拉法在其表面提拉一层凝胶薄膜;
步骤4,在氩气保护下,用300℃的温度对经步骤3提拉出的凝胶薄膜进行22min热处理,最终得到掺杂碳纳米管的氧化硅阻变薄膜。
实施例3
本发明掺杂碳纳米管的氧化硅阻变薄膜的制备方法,具体按照以下步骤实施:
步骤1,以碳纳米管粉末为溶质,无水乙醇为溶剂,制备浓度为10-5g/mL的碳纳米管溶液;
步骤2,按照20:0.7的体积比分别量取氧化硅溶胶、经步骤1制备得到的碳纳米管溶液,将量取后的氧化硅溶胶和碳纳米管溶液混合并搅拌均匀,得到掺杂碳纳米管的氧化硅溶液;
步骤3,选取基板,将基板置于经步骤2得到的掺杂碳纳米管的氧化硅溶液中,并采用浸渍提拉法在其表面提拉一层凝胶薄膜;
步骤4,在氩气保护下,用450℃的温度对经步骤3提拉出的凝胶薄膜进行20min-30min热处理,最终得到掺杂碳纳米管的氧化硅阻变薄膜。
实施例4
本发明掺杂碳纳米管的氧化硅阻变薄膜的制备方法,具体按照以下步骤实施:
步骤1,以碳纳米管粉末为溶质,无水乙醇为溶剂,制备浓度为10-5g/mL的碳纳米管溶液;
步骤2,按照20:0.8的体积比分别量取氧化硅溶胶、经步骤1制备得到的碳纳米管溶液,将量取后的氧化硅溶胶和碳纳米管溶液混合并搅拌均匀,得到掺杂碳纳米管的氧化硅溶液;
步骤3,选取基板,将基板置于经步骤2得到的掺杂碳纳米管的氧化硅溶液中,并采用浸渍提拉法在其表面提拉一层凝胶薄膜;
步骤4,在氩气保护下,用600℃的温度对经步骤3提拉出的凝胶薄膜进行28min热处理,最终得到掺杂碳纳米管的氧化硅阻变薄膜。
实施例5
本发明掺杂碳纳米管的氧化硅阻变薄膜的制备方法,具体按照以下步骤实施:
步骤1,以碳纳米管粉末为溶质,无水乙醇为溶剂,制备浓度为10-5g/mL的碳纳米管溶液;
步骤2,按照20:1的体积比分别量取氧化硅溶胶、经步骤1制备得到的碳纳米管溶液,将量取后的氧化硅溶胶和碳纳米管溶液混合并搅拌均匀,得到掺杂碳纳米管的氧化硅溶液;
步骤3,选取基板,将基板置于经步骤2得到的掺杂碳纳米管的氧化硅溶液中,并采用浸渍提拉法在其表面提拉一层凝胶薄膜;
步骤4,在氩气保护下,用700℃的温度对经步骤3提拉出的凝胶薄膜进行30min热处理,最终得到掺杂碳纳米管的氧化硅阻变薄膜。
Claims (5)
1.一种掺杂碳纳米管的氧化硅阻变薄膜的制备方法,其特征在于,具体按照以下步骤实施:
步骤1,以碳纳米管粉末为溶质,无水乙醇为溶剂,制备浓度为10-5g/mL的碳纳米管溶液;
步骤2,按照20:0.5-1的体积比分别量取氧化硅溶胶、经步骤1制备得到的碳纳米管溶液,将量取后的氧化硅溶胶和碳纳米管溶液混合并搅拌均匀,得到掺杂碳纳米管的氧化硅溶液;
步骤3,选取基板,将基板置于经步骤2得到的掺杂碳纳米管的氧化硅溶液中,并采用浸渍提拉法在其表面提拉一层凝胶薄膜;
步骤4,在惰性气体的保护下,对经步骤3提拉出的凝胶薄膜进行热处理,最终得到掺杂碳纳米管的氧化硅阻变薄膜。
2.根据权利要求1所述的掺杂碳纳米管的氧化硅阻变薄膜的制备方法,其特征在于,在所述步骤3中:所述基板的材质为铂。
3.根据权利要求1所述的掺杂碳纳米管的氧化硅阻变薄膜的制备方法,其特征在于,在所述步骤4中:所述热处理的温度为200℃-700℃。
4.根据权利要求3所述的掺杂碳纳米管的氧化硅阻变薄膜的制备方法,其特征在于,在所述步骤4中:所述热处理的时间为20min-30min。
5.根据权利要求1所述的掺杂碳纳米管的氧化硅阻变薄膜的制备方法,其特征在于,在所述步骤4中:所述惰性气体为氩气。
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