CN105514273A - 一种高电学稳定性的铁电/半导体/pmma三元复合阻变薄膜及其制备方法 - Google Patents
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Abstract
本发明属于阻变存储器技术领域,具体为一种高电学稳定性的铁电/半导体/PMMA三元复合阻变薄膜及其制备方法。本发明的三元复合阻变薄膜是对铁电/半导体复合薄膜进行聚甲基丙烯酸甲脂(PMMA)掺杂而得到,PMMA的掺杂量与铁电聚合物的质量比为0.1:10-0.3:10。该三元复合薄膜的表面粗糙度、抗电疲劳特性和阻态保持性能都得到明显改善。由于PMMA与铁电聚合物P(VDF-TrFE)互溶性佳,可有效降低铁电相的漏电特性;而PMMA与有机半导体,如P3HT,形成层状相分离结构,可有效抑制半导体相的漏电,降低半导体相电击穿的风险。
Description
技术领域
本发明属于阻变存储器技术领域,具体涉及一种铁电/半导体复合阻变薄膜及其制备方法。
背景技术
阻变存储器具有结构简单、读写速度快、制造成本低、器件等比例缩小性能优、与半导体工艺兼容性佳等特点,受到学术界和产业界的广泛关注,有望成为未来存储技术发展的方向。有机半导体/铁电复合结构因其具有电双稳和整流特性,是目前制备阻变存储器的一种简单工艺。这里铁电聚合物一般为偏二氟乙烯和三氟乙烯的共聚物P(VDF-TrFE),而有机半导体材料可以为聚(3-己基噻吩-2,5-二基)(P3HT),聚[(9,9-二正辛基芴基-2,7-二基)-alt-(苯并[2,1,3]噻二唑-4,8-二基)](F8BT),聚[(9,9-二辛基芴基-2,7-二基)-co-并噻吩](F8T2),[6,6]-苯基C61丁酸甲酯(PCBM)等聚合物材料。然而,由于半导体相和铁电相在溶液法成膜过程中形成相分离结构,因而采用旋涂工艺制得的复合薄膜表面极为粗糙,其表面粗糙度与薄膜的厚度相当,从而导致器件漏电增加,削弱了器件的阻变特性,造成该复合阻变存储结构的产率下降。而且,由于有机半导体本身的电学不稳定性,导致铁电/半导体阻变器件经受反复写入/擦除操作后,半导体相被击穿,器件丧失阻变性能。
发明内容
本发明的目的在于提供一种电学稳定性高、工艺简单的铁电/半导体复合阻变薄膜及其制备方法。
本发明提供的铁电/半导体复合阻变薄膜,是引入第三相掺杂得到,即对铁电/半导体复合薄膜进行聚甲基丙烯酸甲脂(PMMA)掺杂,通过PMMA掺杂量的严格控制,即PMMA的掺杂量与铁电聚合物(P(VDF-TrFE))的质量比介于0.1:10到0.3:10之间,可获得高电学稳定性的铁电/半导体/PMMA三元复合阻变薄膜。该三元复合薄膜的表面粗糙度、抗电疲劳特性和阻态保持性能都得到明显改善。由于PMMA与铁电聚合物P(VDF-TrFE)互溶性佳,可有效降低铁电相的漏电特性;而PMMA与有机半导体,如P3HT,形成层状相分离结构,可有效抑制半导体相的漏电,有效降低半导体相电击穿的风险。
本发明提供的PMMA/半导体/铁电三元复合阻变薄膜的制备方法,具体步骤如下:
(1)在基片(如玻璃、硅片、聚酰亚胺PI片、聚对苯二甲酸乙二酯PET片,等等)上,采用真空技术沉积条状金属电极,电极材料为银或铝,条状电极线条宽度小于1mm(例如,一般电极线条宽度为1μm-1mm);
(2)称取一定量P3HT和P(VDF-TrFE)材料放入四氢呋喃溶剂中,P3HT与P(VDF-TrFE)的质量比小于1:5(例如,一般两者的质量比为1:5--1:20),在磁力搅拌仪上用磁性转子搅拌,直至获得P3HT和P(VDF-TrFE)两种材料的澄清的混合溶液;
(3)称取适量的PMMA加入P3HT和P(VDF-TrFE)混合溶液中,PMMA与P(VDF-TrFE)的质量比介于0.1:10到0.3:10之间,搅拌均匀,获得三种材料的澄清混合溶液;
(4)采用旋涂法,将混合溶液旋涂在步骤(1)所制备的带有金属电极的基片上,获得三种材料组成的复合薄膜。复合薄膜经1小时以上(例如,一般为1-5小时)退火处理,退火温度介于120℃和148℃之间(例如,一般为135℃);
(5)采用真空沉积技术,在复合薄膜表面沉积条状金属电极,并与步骤(1)所沉积电极形成交叉结构,电极材料为银或铝,线条宽度小于1mm(例如,一般电极线条宽度为1μm-1mm)。
本发明的应用在于:经由优化的PMMA掺杂,极大提高半导体/铁电复合阻变薄膜的抗击穿特性、抗电疲劳特性和阻态保持特性,提高了基于半导体/铁电复合薄膜的阻变器件的稳定性和可靠性。
附图说明
图1:不同PMMA掺杂量对PMMA/P3HT/P(VDF-TrFE)三元复合阻变薄膜表面粗糙度和阻变性能的影响。(a)PMMA掺杂量对三元复合薄膜表面粗糙度的影响;图(b)到图(d)为PMMA:P3HT:P(VDF-TrFE)三相质量比分别为0:1:10,0.2:1:10,0.5:1:10时三元复合薄膜的阻变特性曲线。图(c)和图(d)中数值标注了阻变薄膜所经历的写入/擦除次数。
图2:PMMA:P3HT:P(VDF-TrFE)三相质量比为0:1:10和0.2:1:10时三元复合阻变薄膜的阻态保持性能。(a)开态和关态电流的保持性能,其中正方形和圆形数据点表示PMMA:P3HT:P(VDF-TrFE)三相质量比为0:1:10时的开态和关态电流;三角形和菱形数据点表示PMMA:P3HT:P(VDF-TrFE)三相质量比为0.2:1:10时的开态和关态电流。(b)开态和关态电流比值(开关比)随时间的改变,其中正方形数据点表示PMMA:P3HT:P(VDF-TrFE)三相质量比为0:1:10时的开关比;圆形数据点表示PMMA:P3HT:P(VDF-TrFE)三相质量比为0.2:1:10时的开关比。
具体实施方式
下面将结合实施例,阐述适量PMMA掺杂,可明显改善P3HT/P(VDF-TrFE)阻变薄膜的表面粗糙度、抗电击穿、抗电疲劳性能和阻态保持性能。
实施例1
本实施例阐述最佳的PMMA掺杂量。
按照发明内容中三元复合阻变薄膜的制备工艺制备PMMA/P3HT/P(VDF-TrFE)复合薄膜,其中在配置四氢呋喃溶液时,保持P(VDF-TrFE)的质量百分比为3%,PMMA:P3HT:P(VDF-TrFE)质量比为x:1:10,x为介于0到0.5之间的变量。
薄膜的均方根表面粗糙度由原子力显微镜测得,结果如图1(a)所示,可见随着PMMA掺杂量(x从0到0.5)的增加,薄膜表面粗糙度明显降低,这有助于降低器件漏电流。
图(b)到(d)分别给出x=0,0.2和0.5时获得的阻变特性曲线。x=0时(图b),正负偏压幅值40V时获得明显的蝴蝶回线状的特性曲线,表明薄膜具有阻变特性,然而当偏压幅值增至60V,薄膜明显被击穿,表明薄膜抗电击穿性能差。x=0.2时(图c),正负偏压幅值100V时,薄膜仍表现出蝴蝶回线状的阻变特性曲线,表明薄膜抗击穿性能明显增强;而且薄膜经反复写入/擦除操作106次后,仍维持较好的阻变特性,表明薄膜抗电疲劳性能明显增强。x=0.5时(图d),正负偏压幅值100V时,薄膜仍未被击穿,表明薄膜较强抗击穿性能;然而由于PMMA的过量掺杂,阻变性能基本丧失,曲线仅展现出微弱的蝴蝶回线形状,表明此时的薄膜无法用做阻变器件。
通过这一系列不同PMMA掺杂所获得数据,确认最佳的PMMA掺杂量x应介于0.1到0.3之间。
实施例2
本实施例阐述优化PMMA掺杂量之后,所获得薄膜的阻态保持性能也得到明显改善。
按照发明内容中三元复合阻变薄膜的制备工艺制备PMMA/P3HT/P(VDF-TrFE)复合薄膜,其中在配置四氢呋喃溶液时,保持P(VDF-TrFE)的质量百分比为3%,PMMA:P3HT:P(VDF-TrFE)质量比为x:1:10,x为0(对应没有PMMA掺杂情况)或0.2(对应优化的PMMA掺杂量)。
图2(a)所示为开态和关态电流随时间的改变,与没有PMMA掺杂的情况(x=0)相比,PMMA掺杂(x=0.2)后,由于薄膜漏电流被有效抑制,所获得开态电流和关态电流的大小均比未PMMA掺杂时所获得开态和关态电流低。图2(b)所示为开态电流和关态电流的比值(开关比)随时间的改变,很明显经PMMA掺杂(x=0.2)后,开关比的衰减速度减缓,在1小时时间内仅从初始值的36.6衰减至29.8;而没有PMMA的阻变薄膜的开关比在20分钟时间内就从初始值的35衰减至20.7。
结果说明优化的PMMA掺杂有效地改善了阻变器件的阻态保持性能。
Claims (2)
1.一种铁电/半导体/PMMA三元复合阻变薄膜,其特征在于对铁电/半导体复合薄膜进行聚甲基丙烯酸甲脂(PMMA)掺杂而得到,PMMA的掺杂量与铁电聚合物的质量比为0.1:10-0.3:10。
2.一种铁电/半导体/PMMA三元复合阻变薄膜的制备方法,其特征在于具体步骤为:
(1)在基片上,采用真空技术沉积条状金属电极,电极材料为银或铝,条状电极线条宽度小于1mm;
(2)称取一定量P3HT和P(VDF-TrFE)材料放入四氢呋喃溶剂中,P3HT与P(VDF-TrFE)的质量比小于1:5,在磁力搅拌仪上用磁性转子搅拌,直至获得P3HT和P(VDF-TrFE)两种材料的澄清的混合溶液;
(3)称取适量的PMMA加入P3HT和P(VDF-TrFE)混合溶液中,PMMA与P(VDF-TrFE)的质量比0.1:10-0.3:10,搅拌均匀,获得三种材料的澄清混合溶液;
(4)采用旋涂法,将混合溶液旋涂在步骤(1)所制备的带有金属电极的基片上,获得三种材料组成的复合薄膜;对该复合薄膜进行退火处理,退火温度为120℃-145℃,退火时间为1小时以上;
(5)采用真空沉积技术,在复合薄膜表面沉积条状金属电极,并与步骤(1)所沉积电极形成交叉结构,电极材料为银或铝,线条宽度小于1mm。
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CN109961952A (zh) * | 2019-03-27 | 2019-07-02 | 哈尔滨理工大学 | 一种异质结构的多层聚合物基复合储能材料及其制备方法 |
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CN106252509A (zh) * | 2016-09-20 | 2016-12-21 | 哈尔滨工业大学深圳研究生院 | 一种基于有机铁电薄膜的电阻开关存储器及其制备方法 |
CN106252509B (zh) * | 2016-09-20 | 2019-06-18 | 哈尔滨工业大学深圳研究生院 | 一种基于有机铁电薄膜的电阻开关存储器及其制备方法 |
CN109961952A (zh) * | 2019-03-27 | 2019-07-02 | 哈尔滨理工大学 | 一种异质结构的多层聚合物基复合储能材料及其制备方法 |
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