CN108484885A - 一种基于多环芳烃的共轭聚合物及其应用 - Google Patents
一种基于多环芳烃的共轭聚合物及其应用 Download PDFInfo
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- CN108484885A CN108484885A CN201810299092.6A CN201810299092A CN108484885A CN 108484885 A CN108484885 A CN 108484885A CN 201810299092 A CN201810299092 A CN 201810299092A CN 108484885 A CN108484885 A CN 108484885A
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Abstract
本发明涉及一种基于多环芳烃的共轭聚合物及其应用,共轭聚合物用于有机场效应晶体管光可编程线性存储器中,有机场效应晶体管光可编程线性存储器包括衬底,在所述衬底的上表面设置有栅电极,在所述栅电极的上表面设置有栅绝缘层,在所述栅绝缘层的上表面设置有共轭聚合物薄膜层,所述共轭聚合物薄膜层的上表面中部具有沟道区域,在所述共轭聚合物薄膜层的上表面位于沟道区域两侧设置有源漏电极。本发明的优点是通过简单的工艺手段使器件既有半导体性能又有存储性能,获得存储容量、开关速度和光响应能力、线性存储能力优异的有机场效应晶体管存储器。
Description
技术领域
本发明涉及一种基于多环芳烃的共轭聚合物及其在有机场效应晶体管光可编程线性存储器中的应用,属于半导体行业存储器技术领域。
背景技术
有机存储器件由于其材料来源广泛、可柔性制备、高响应速度、高存储密度并可穿戴性而获得广泛关注。现有的基于电容电阻结构的有机存储器件因其电荷易泄露,尺寸大,器件耐受性差和难以集成化等缺点,限制了其商业化推广。相比而言,有机场效应晶体管(OFET)存储器具有非破坏性读取,可多阶存储并且可大面积应用于集成电路等特点,非常适合下一代可穿戴电子,代表了有机存储器新的发展方向。相比于传统的晶体管,OFET在半导体层和控制栅极之间设有有机存储活性层,根据其有机存储活性层的材料,将OFET分为铁电型、浮栅型及驻极体型三大类,使得OFET能够识别出“0”和“1”的数字状态。在这些存储器中,浮栅型存储器具有低成本,低功耗且存储密度大等优点,获得较为广泛的关注,因此在电子信息领域具有广泛的应用前景。
通常,有机场效应晶体管存储器的有机存储活性层包含至少两种材料,例如采用并五苯和其他聚合物分别成膜,构成双层异质结构,能实现电可擦写的存储器。然而,具有推拉电子结构的共轭聚合物在OFET器件中虽然能够实现双极传输和高迁移率,往往不能作为单一组分实现晶体管存储特性。已报道的基于共轭聚合物的晶体管存储器的存储行为主要是依赖于介电层或使用多组分活性层来实现有效存储。这样的有机场效应晶体管存储器通常存在存储功能单一、对器件工艺敏感、多活性层组分相分离依赖性强等问题。此外,晶体管存储器一直面临着存储特性无法对外加电压实现线性存储的问题。
发明内容
本发明的目的在于:针对现有技术存在的缺陷,提出一种基于多环芳烃共轭聚合物,同时给出了其应用,该应用于OFET存储器,既能充当存储器的半导体层,又能充当存储器的电荷存储层,提高了存储器的存储性能,使其轻松实现光编程,并且可对其线性存储特性进行有效控制
为了达到以上目的,本发明提供了一种基于多环芳烃的共轭聚合物,所述基于多环芳烃的共轭聚合物的结构式为:
其中,Ar、A、X均独立代表式中所示的基团或元素中的任意一种,即Ar 为噻吩并噻吩或硒吩X为N、Si或C,R1为具有6~12个碳原子的直链烷基、支链烷基或烷氧基苯基,R2为具有6~12个碳原子的直链或支链烷基,A为苯并噻二唑苯并硒二唑吡啶并噻二唑5,6-二氟苯并噻二唑5-氟苯并噻二唑4,7-二芳基-5,6-二烷氧基苯并噻二唑4, 7-二芳基苯并噻二唑4,7-二芳基苯并硒二唑4, 7-二芳基吡啶并噻二唑4,7-二芳基-5,6-二氟苯并噻二唑或4,7-二芳基-5-氟苯并噻二唑R3为具有6~12 个碳原子的直链或支链烷基,B为噻吩、硒吩、并噻吩或苯并噻吩。
本发明还提供了一种基于多环芳烃的共轭聚合物的应用,所述共轭聚合物应用于有机场效应晶体管光可编程线性存储器中。
优选地,所述有机场效应晶体管光可编程线性存储器包括衬底,在所述衬底的上表面设置有栅电极,在所述栅电极的上表面设置有栅绝缘层,在所述栅绝缘层的上表面设置有共轭聚合物薄膜层,所述共轭聚合物薄膜层的上表面中部具有沟道区域,在所述共轭聚合物薄膜层的上表面位于沟道区域两侧设置有源漏电极。
进一步优选地,所述共轭聚合物薄膜层即为有机半导体多晶相活性层,其材质为具有多环芳烃结构的共轭聚合物。
优选地,所述衬底为重掺杂硅片,所述栅电极的材质为重掺杂硅、铝、铜、银或金中的一种;所述栅绝缘层的材质为二氧化硅、氧化铝、氧化锆、聚苯乙烯或聚乙烯吡咯烷酮中的一种;所述源漏电极的材质为金或银。
本发明中有机场效应晶体管光可编程线性存储器的制备方法,包括以下步骤:
第一步、将共轭聚合物溶于溶剂中,得到浓度为10~30mg/mL的聚合物溶液,按照体积比1:(0.02~0.3)取聚合物溶液和试剂混合,搅拌0.5~2h得到混合物溶液;
第二步、以衬底为基片,在基片上依次形成栅电极和栅绝缘层,将形成有栅电极和栅绝缘层的基片清洗干净后,烘干;
第三步、对烘干后的基片进行紫外臭氧处理3~5min;
第四步、在紫外臭氧处理后的基片上表面旋涂混合物溶液,旋涂转速为2000 ±1000r/min,旋涂时间为30±5s,将旋涂好的基片在110~140℃条件下干燥5min,得到样品;
第五步、在样品的上表面制作源漏电极,得到有机场效应晶体管光可编程线性存储器。
优选地,所述溶剂为高沸点溶剂,所述高沸点溶剂为甲苯、邻二甲苯、间三甲苯、氯苯或二氯苯中的一种,上述溶剂无需除水处理;所述试剂为二苯醚或二甲亚砜。
优选地,第四步中,在基片上表面旋涂混合物溶液时采用溶液旋涂成膜法;第五步中,源漏电极的制作方法为磁控溅射法、喷墨打印法或真空蒸镀法。
进一步优选地,采用溶液旋涂成膜法时,旋涂过程在手套箱或空气中进行,当旋涂过程在空气中进行时,控制空气湿度为40~50%;采用真空蒸镀法时,蒸镀速率为源漏电极的厚度控制在60~100nm。
优选地,所述栅绝缘层的厚度为50~300nm;所述共轭聚合物薄膜层的厚度为35~65nm;所述源漏电极的厚度为60~100nm。
本发明将共轭聚合物应用于有机场效应晶体管存储器中,通过二甲亚砜、二苯醚和N,N-二甲基甲酰胺等试剂对多环芳烃共轭聚合物在高沸点溶剂中的链舒展形态、成膜形貌和多晶相行为等进行调控,使得共轭聚合物既能充当器件的半导体活性层,又能充当电荷存储层。本发明的这种薄膜处理方式能够获得具有多晶相态结构的均匀聚合物薄膜,一方面,多晶相结构中相态连续分布,是理想晶体管相态,另一方面,其晶相界面处电荷集聚,使其晶区核芯聚合物可俘获电荷,从而形成电荷集聚,形成存储器特性。此外,该聚合物分子中的多环芳烃结构单元之间的强堆积作用力能有效保持多晶相结构的稳定性,从而提高制得的存储器的稳定性和耐受性能力。
本发明的优点是:
1.本发明在不用驻极体结构的情况下,实现了光编程和线性存储,为有机晶体管存储器的商业化推广提供了一种可行的思路;
2.本发明提供的有机场效应晶体管存储器,结构简单,其制备方法简单、便于操作,显著降低了人力成本;
3.本发明的共轭聚合物通过简单的旋涂工艺,能够在不增加工艺复杂程度且适用简单设备制备的前提下,用于有机场效应晶体管存储器中,既能充当半导体层,又能充当存储层。
总之,本发明通过简单的工艺手段使器件既有半导体性能又有存储性能,获得存储容量、开关速度和光响应能力、线性存储能力优异的有机场效应晶体管存储器。
附图说明
下面结合附图对本发明作进一步的说明。
图1为本发明中共轭聚合物有机场效应晶体管存储器的结构示意图。
图2为本发明实施例1中聚合物PDIDTSeNBT的合成路线图。
图3为本发明实施例2中聚合物PDIDSeDTBTC8的合成路线图。
图4为本发明实施例3中聚合物PDIDSe-DF-BT的合成路线图。
图5为本发明实施例4中聚合物PDIDSe-F-DTBT的合成路线图。
图6为本发明实施例5中共轭聚合物有机场效应晶体管存储器的转移特性曲线图。
图7为本发明实施例5中共轭聚合物有机场效应晶体管存储器的负向存储窗口特性曲线图。
图8为本发明实施例5中共轭聚合物有机场效应晶体管存储器的负向写入- 读取-擦除-读取特性曲线图。
图9为本发明实施例5中共轭聚合物有机场效应晶体管存储器的负向存储性能维持时间特性曲线图。
图10为本发明实施例5中共轭聚合物有机场效应晶体管存储器在黑暗条件下的回滞曲线图。
图11为本发明实施例5中共轭聚合物有机场效应晶体管存储器在加光条件下的回滞曲线图。
图12为本发明实施例5中共轭聚合物有机场效应晶体管存储器的负向线性存储特性曲线图。
具体实施方式
本发明所用原料为已知化合物,可在市场上购得,或可用本领域已知方法合成。
实施例1
本实施例提供了一种基于多环芳烃的共轭聚合物PDIDSe-N-BT,共轭聚合物PDIDSe-N-BT的结构式如下:
共轭聚合物PDIDSe-N-BT的合成路线如图2所示。取0.42g(0.29 mmol)DIDSe-Sn,0.088g(0.30mmol)4,7-二溴-2,1,3-吡啶并噻二唑加入到 50mL反应管中,然后向反应管中依次加入0.01g(0.01mmol)催化剂三(二亚苄基丙酮)二钯,0.02g(0.06mmol)配体三邻甲基苯基磷,10mL无水甲苯和0.5 mL无水N,N-二甲基甲酰胺,在110℃以及氩气保护条件下搅拌反应24h,得到聚合物。将聚合物冷却至室温,慢慢倒入70mL甲醇中,沉淀的聚合物过滤后在索式提取器中依次用甲醇、正己烷来洗涤,最后用三氯甲烷溶解后沉淀到甲醇中,过滤,100℃真空干燥12h得到深紫色的固体粉末聚合物,产率70%,其数均分子量为Mw=18.0K,分散度PDI=1.69。
DIDSe-Sn、4,7-二溴-2,1,3-吡啶并噻二唑的结构式如图2所示。
实施例2
本实施例提供了一种基于多环芳烃的共轭聚合物PDIDSeDTBTC8,共轭聚合物PDIDSeDTBTC8的结构式如下:
共轭聚合物PDIDSeDTBTC8的合成路线如图3所示。取0.42g(0.29mmol) DIDSe-Sn,0.21g,(0.29mmol)DTBTC8加入到50mL反应管中,然后向反应管中依次加入0.01g(0.01mmol)催化剂三(二亚苄基丙酮)二钯,0.02g(0.06mmol) 配体三邻甲基苯基磷,10mL无水甲苯和0.5mL无水N,N-二甲基甲酰胺,在110℃以及氩气保护条件下,搅拌反应24h,得到聚合物。将聚合物冷却至室温后,慢慢倒入150mL甲醇中,沉淀的聚合物过滤后在索式提取器中依次用甲醇、正己烷来洗涤,最后用三氯甲烷溶解后沉淀到甲醇中,过滤,100℃真空干燥12h,得到紫红色的固体粉末聚合物,产率78%,其数均分子量为Mw=37.0 K,分散度PDI=1.88。
DIDSe-Sn,DTBTC8的结构式如图3所示。
实施例3
本实施例提供了一种基于多环芳烃的共轭聚合物PDIDSe-DF-BT,共轭聚合物PDIDSe-DF-BT的结构式如下:
共轭聚合物PDIDSe-DF-BT的合成路线如图4所示。取0.42g(0.29 mmol)DIDSe-Sn,0.09g(0.29mmol)4,7-二溴-5,6-二氟-苯并噻二唑(DF-BT) 加入到50mL反应管中,然后向反应管中依次加入0.01g(0.01mmol)催化剂三(二亚苄基丙酮)二钯,0.02g(0.06mmol)配体三邻甲基苯基磷,10mL无水甲苯和0.5mL无水N,N-二甲基甲酰胺,在110℃以及氩气保护条件下,搅拌反应24h,得到聚合物。将聚合物冷却至室温后,慢慢倒入150mL甲醇中,形成沉淀,沉淀的聚合物过滤后在索式提取器中依次用甲醇、正己烷来洗涤,最后用三氯甲烷溶解后沉淀到甲醇中,过滤,100℃真空干燥12h得到紫红色的固体粉末聚合物,产率84%,其数均分子量为Mw=18.0K,分散度PDI=1.74。
DIDSe-Sn、4,7-二溴-5,6-二氟-苯并噻二唑的结构式如图4所示。
实施例4
本实施例提供了一种基于多环芳烃的共轭聚合物PDIDSe-F-DTBT,共轭聚合物PDIDSe-F-DTBT的结构式如下:
共轭聚合物PDIDSe-F-DTBT的合成路线如图5所示。取0.42g(0.29mmol) DIDSe-Sn,0.14g(0.29mmol)F-DTBT加入到50mL反应管中,然后向反应管中依次加入0.01g(0.01mmol)催化剂三(二亚苄基丙酮)二钯,0.02 g(0.06mmol)配体三邻甲基苯基磷,10mL无水甲苯和0.5mL无水N,N-二甲基甲酰胺,在110℃以及氩气保护条件下,搅拌反应24h,得到聚合物。将聚合物冷却至室温后,慢慢倒入150mL甲醇中沉淀,沉淀的聚合物过滤后在索式提取器中依次用甲醇、正己烷来洗涤,最后用三氯甲烷溶解后沉淀到甲醇中,过滤,100℃真空干燥12h得到紫红色的固体粉末聚合物,产率78%,其数均分子量为Mw=24.0K,分散度PDI=1.75。
DIDSe-Sn、F-DTBT结构式如图5所示。
实施例5
本实施例提供了一种基于共轭聚合物PDIDSe-N-BT的有机场效应晶体管光可编程线性存储器,其结构如图1所示,包括:衬底;形成于衬底之上的栅电极;形成于衬底及栅电极之上的栅绝缘层;形成于栅绝缘层之上的具有一维多并苯九元环结构的共轭聚合物薄膜层;形成于具有一维多并苯九元环结构的共轭聚合物薄膜层表面沟道区域两侧的源漏电极。
上述有机场效应晶体管光可编程线性存储器中,重掺杂硅作为衬底和栅电极;一层300nm厚的二氧化硅作为栅绝缘层;具有一维九元环芳烃结构的共轭聚合物作为有机半导体多晶相活性层,其厚度为35~45nm;在有机半导体多晶相活性层的表面导电沟道两侧蒸镀金属金作为源漏电极。
本实施例的存储器具体制备步骤如下:
(1)配置聚合物溶液:以具有一维多并苯九元环结构的聚合物PDIDSe-N-BT 为溶质,溶于溶剂中,溶剂为未经额外除水处理的氯苯,配置成浓度为10mg/mL 的聚合物溶液,然后静置12h,使其分散均匀,最后在聚合物溶液中加入占聚合物溶液体积分数为2%的二甲亚砜,继续搅拌0.5h,得到混合物溶液。
(2)以重掺杂硅片作为衬底材料,以衬底材料作为基片,在基片上形成栅电极,然后在形成有栅电极的基片上形成一层厚度为300nm的二氧化硅作为栅绝缘层,依次用丙酮、乙醇、去离子水各超声清洗10min,超声频率为100KHz,再用高纯氮气将基片表面液体吹干以保证基片表面洁净,最后放入120℃的烘箱中烘干。
(3)将烘干的基片放置入紫外臭氧机中处理5min。
(4)在空气中,控制空气湿度为40~50%,将处理好的基片表面旋涂配置好的混合物溶液,旋涂转速为2000r/min,旋涂时间为30s,薄膜厚度控制在35 nm左右;将旋涂好的基片放在130℃的烘箱中退火5min。
(5)在退火后的薄膜表面真空蒸镀金充当源漏电极,蒸镀速率控制源漏电极厚度在60~80nm;掩模板的沟道宽度为2000μm,长度为100μm。
在制备时,实验室室温保持在25℃左右,室内湿度保持在50%以下,旋涂成膜过程可在手套箱或空气中进行。
存储器制备完成后,其电学性能由吉时利A4200半导体分析仪进行表征,数据处理绘制成的转移曲线如图6所示,迁移率达到0.003cm2/Vs,开关比达 103。器件负向存储特性转移曲线如图7所示,器件的写入窗口很大,达到60V, 而且仅施加光就可完全擦除回初始位置,体现器件具有很好的低功耗、高光响应特性。写入-读取-擦除-读取特性数据曲线如图8所示,表示该存储器具有良好的反复擦写能力,经过一定周期的擦写循环后,器件的擦写窗口基本没有变化。器件数据保持能力如图9所示,经过10000s之后,器件的存储开关比仍旧保持在103以上,说明器件的存储可靠性高。图7表示器件在加光条件下的回滞曲线,器件在黑暗条件下的回滞曲线如图10所示,表示有很大的窗口(120V 左右),且每一圈扫描曲线几乎重合,有很好的稳定性。器件负向存储特性转移曲线如图图11所示,器件的写入窗口很大,达到86V,而且仅施加光就可完全擦除回初始位置,体现器件反应灵敏,具有很好的低功耗、高光响应特性。器件的线性存储能力如图12所示,在不同编程电压的情况下,有着对应的存储窗口。随着编程电压的增大,写入窗口也逐渐增大,几乎呈线性关系。说明器件可以轻松实现线性存储。
所有测试结果表明,本实施例所涉及的一种共轭聚合物有机场效应晶体管存储器件性能良好,可实现线性存储,可光编程,稳定性好,数据保持可靠性高,而且制备过程操作简单,成本低廉,主要工艺过程在溶液中完成、节约能源,并且能够大规模生产。
除上述实施例外,本发明还可以有其他实施方式。凡采用等同替换或等效变换形成的技术方案,均落在本发明要求的保护范围。
Claims (10)
1.一种基于多环芳烃的共轭聚合物,其特征在于,所述共轭聚合物的结构式为:
其中,Ar为噻吩、并噻吩或硒吩,X为N、Si或C,R1为具有6~12个碳原子的直链烷基、支链烷基或烷氧基苯基,R2为具有6~12个碳原子的直链或支链烷基,A为苯并噻二唑、苯并硒二唑、吡啶并噻二唑、5,6-二氟苯并噻二唑、5-氟苯并噻二唑、4,7-二芳基-5,6-二烷氧基苯并噻二唑、4,7-二芳基苯并噻二唑、4,7-二芳基苯并硒二唑、4,7-二芳基吡啶并噻二唑、4,7-二芳基-5,6-二氟苯并噻二唑或4,7-二芳基-5-氟苯并噻二唑,R3为具有6~12个碳原子的直链或支链烷基,B为噻吩、硒吩、并噻吩或苯并噻吩。
2.根据权利要求1所述一种基于多环芳烃的共轭聚合物的应用,其特征在于,所述共轭聚合物应用于有机场效应晶体管光可编程线性存储器中。
3.根据权利要求2所述一种基于多环芳烃的共轭聚合物的应用,其特征在于,所述有机场效应晶体管光可编程线性存储器包括衬底,在所述衬底的上表面设置有栅电极,在所述栅电极的上表面设置有栅绝缘层,在所述栅绝缘层的上表面设置有共轭聚合物薄膜层,所述共轭聚合物薄膜层的上表面中部具有沟道区域,在所述共轭聚合物薄膜层的上表面位于沟道区域两侧设置有源漏电极。
4.根据权利要求3所述一种基于多环芳烃的共轭聚合物的应用,其特征在于,所述共轭聚合物薄膜层的材质为具有多环芳烃结构的共轭聚合物。
5.根据权利要求4所述一种基于多环芳烃的共轭聚合物的应用,其特征在于,所述衬底为重掺杂硅片,所述栅电极的材质为重掺杂硅、铝、铜、银或金中的一种;所述栅绝缘层的材质为二氧化硅、氧化铝、氧化锆、聚苯乙烯或聚乙烯吡咯烷酮中的一种;所述源漏电极的材质为金或银。
6.根据权利要求5所述一种基于多环芳烃的共轭聚合物的应用,其特征在于,所述有机场效应晶体管光可编程线性存储器的制备方法包括以下步骤:
第一步、将共轭聚合物溶于溶剂中,得到浓度为10~30mg/mL的聚合物溶液,按照体积比1:(0.02~0.3)取聚合物溶液和试剂混合,搅拌0.5~2h得到混合物溶液;
第二步、以衬底为基片,在基片上依次形成栅电极和栅绝缘层,将形成有栅电极和栅绝缘层的基片清洗干净后,烘干;
第三步、对烘干后的基片进行紫外臭氧处理3~5min;
第四步、在紫外臭氧处理后的基片上表面旋涂混合物溶液,旋涂转速为2000±1000r/min,旋涂时间为30±5s,将旋涂好的基片在110~140℃条件下干燥5min,得到样品;
第五步、在样品的上表面制作源漏电极,得到有机场效应晶体管光可编程线性存储器。
7.根据权利要求6所述一种基于多环芳烃的共轭聚合物的应用,其特征在于,所述溶剂为高沸点溶剂,所述高沸点溶剂为甲苯、邻二甲苯、间三甲苯、氯苯或二氯苯中的一种;所述试剂为二苯醚或二甲亚砜。
8.根据权利要求6所述一种基于多环芳烃的共轭聚合物的应用,其特征在于,第四步中,在基片上表面旋涂混合物溶液时采用溶液旋涂成膜法;第五步中,源漏电极的制作方法为磁控溅射法、喷墨打印法或真空蒸镀法。
9.根据权利要求8所述一种基于多环芳烃的共轭聚合物的应用,其特征在于,采用溶液旋涂成膜法时,旋涂过程在手套箱或空气中进行,当旋涂过程在空气中进行时,控制空气湿度为40~50%;采用真空蒸镀法时,蒸镀速率为 源漏电极的厚度控制在60~100nm。
10.根据权利要求6所述一种基于多环芳烃的共轭聚合物的应用,其特征在于,所述栅绝缘层的厚度为50~300nm;所述共轭聚合物薄膜层的厚度为35~65nm;所述源漏电极的厚度为60~100nm。
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