CN108417641A - 一种可控的热焊接法制备高性能场效应晶体管的方法 - Google Patents
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Abstract
本发明公开了一种可控的热焊接法制备高性能场效应晶体管的方法，采用溶液法制备ZrO2高k介质薄膜；采用静电纺丝技术制备纳米纤维网络，通过高温煅烧，利用热蒸发沉积源漏电极。本发明的有益效果是可以在大面积衬底上获得分布均匀的纳米纤维。
Description
技术领域
本发明属于静电纺丝纳米纤维场效应晶体管制备技术领域，涉及一种制备高性能、低功耗场效应晶体管的方法。
背景技术
无机电子材料到目前为止仍然是微电子工业最重要的材料。第一代晶体管就是基于Ge材料的点接触晶体管，且Ge三极管的导通电阻只有0.2-0.3V，正向导通电阻只有几百欧姆；硅在晶体管的应用过程中占据绝对的主导地位，极大地促进了第三次科技革命的进程，是整个半导体业的重要组成部分；砷化镓由于电子迁移率比硅大7倍，使其在微波器件和高速数字电路方面得到了重要应用；氮化镓在电源转换和功率密度方面比硅有了性能的飞跃，使其逐渐应用到服务器、逆变器、通讯电源等终端领域。但是制备基于以上材料的器件都需要复杂的工艺过程，严格的制备环境和昂贵的制备成本。因此，经过对半导体材料不断的探究，科学家提出了以宽禁带的金属氧化物来代替传统的半导体材料(Nature 432,488,2004)。金属氧化物除了传统无机半导体材料的固有特性外，还有高透过率、易于实现大面积与柔性制备、制备工艺简单以及成本低廉等优势。此外，金属氧化物半导体的制备工艺与硅材料兼容、选材范围广，在产业化应用方面拥有广阔的发展空间和发展价值。
由于具有纳米尺度的直径、较大的长度/直径比和比表面积，以及不同于大块样品的熔点、磁学、光学、导电、导热等理化特性，一维纳米结构材料比如纳米线/粒/管/片/棒、碳纳米管、和高分子纳米纤维等是目前纳米科学的研究热点，它们在高密度存储记忆元件、超微型纳米阵列激光器、传感器、过滤装置、高效能量转化器件、巨磁阻效应、纳米复合材料以及生物医学等领域有广阔的应用前景(Chem.Soc.Rev.41,5285,2012)。一维纳米结构材料的制备方法包括电弧放电法、化学气相沉积法、激光溅射法、模板法、自组装的溶液生长法、电子束曝光、离子束刻蚀以及静电纺丝法等。相比较之下，静电纺丝(Electrospinning)被认为是一种简单有效的、可纺物质种类繁多、工艺可控、纺丝成本低廉、可大规模制备均匀、连续的纳米材料的方法(Adv.Mater.16,1151,2004)，已成为制备纳米纤维材料的主要途径之一。静电纺丝是一种特殊的纤维制造工艺。聚合物的溶液或者熔体在强电场的作用下，针头处的液滴会由球形逐渐变为锥形(即“泰勒锥”)。当超过某一临界值后，进一步激发形成射流并在空气中急剧震荡和鞭动，从而拉伸细化，最终沉降在收集板上。这种方式可以生产出纳米级直径的聚合物纤维，具有操作简单和适用性强等优点。近年来，随着纳米技术的日新月异，静电纺丝也获得了快速发展，在此期间，静电纺丝的发展大致经历了以下四个阶段：第一阶段主要是研究各种聚合物的可纺性,纺丝工艺参数对纤维直径、性能的影响及对工艺参数的优化等；第二阶段主要研究电纺纳米纤维成分的多样化,以及对结构的精准调控；第三个阶段主要研究了电纺在能源、生物医学、光电、环境等领域的应用；第四阶段主要研究纺纤维的量产问题。上述四个阶段相互交融，并没有明显的界线。使用静电纺丝法制备一维纳米材料已成为科研人员广泛关注的课题(Prog.Polym.Sci.38,963,2013)。
结合金属氧化物的材料优势和静电纺丝的技术优势，科研人员期望开辟一条新的微电子技术发展路线。尽管研究者做了很多的尝试，但是，电纺纳米纤维场效应晶体管的器件性能还是不尽如人意，很大程度上限制了这个研究方向的发展。通过对器件结构进行分析，我们发现导致器件性能恶劣的主要原因有两个：一个是纳米纤维与衬底的接触并不紧密；另一个是纤维与纤维之间的接触点处存在较大的接触电阻，而这也是影响器件性能的最主要因素。我们从场效应晶体管的工作原理可知，当栅极接高电位时，电子会被诱导到有源层和介电层的界面处(仅有几nm厚)，再在漏源极加电压就会产生电流。然而，由于电纺过程的快速而随意性，导致了纳米纤维在电场中运动时，就已经发生了固化，当沉积到收集板上时，纤维与衬底和纤维与纤维之间的接触就是松散的物理堆垛，会形成一种三维的网络结构，使得纳米纤维与纳米纤维之间的接触不紧密，导致很大的接触电阻，使得器件性能恶化。目前为止，已经可以通过热压、溶剂蒸汽焊接来增强纤维的粘附性问题，但是热压不能应用于高熔点温度的聚合物，蒸汽焊接需要精确控制蒸汽压和焊接时间。同时，难以大面积应用和复杂的操作流程也限制了这两种技术的应用。
发明内容
本发明的目的在于提供一种可控的热焊接法制备高性能场效应晶体管的方法，本发明的最终目的是使静电纺丝技术的稳定性和重复性变好，可以在大面积衬底上获得分布均匀的纳米纤维，通过调整纳米纤维的分布密度能有效的调节器件的电学性能；In2O3是一种十分理想透明半导体功能材料，具有较大的禁带宽度、较小的电阻率，因此它的大迁移率(＞100cm2V-1s-1)将显著的提高TFT的电流驱动能力；将二者结合能获得性能优良且重复性好的器件。
本发明所采用的技术方案是按照以下步骤进行：
步骤1：采用溶液法制备ZrO2高k介质薄膜；
将水合硝酸锆加入N，N-二甲基甲酰胺中，配制介电层前驱体溶液，使用磁力搅拌器中搅拌，得到澄清透明的溶液；选用单面抛光重掺杂P型低阻硅作为衬底和栅电极，硅衬底依次用丙酮和酒精超声波清洗，去离子水反复冲洗后，用高纯氮气吹干；使用匀胶机在等离子体处理后的P型硅衬底上旋涂ZrO2前驱体溶液；置于烤胶台上150℃烘烤；UV光处理；高温退火，得到均匀致密的ZrO2高k介质薄膜；
步骤2：采用静电纺丝技术制备纳米纤维网络；
将三氯化铟、聚乙烯吡咯烷酮、环氧树脂加入到N，N二甲基甲酰胺中，磁力搅拌器搅拌，得到粘性的透明前驱体溶液；将制备得到的介电层衬底附在收集板上，针头处连接直流高压电源正极，收集板处接地；前驱体溶液喷出并剧烈抖动，飘向衬底过程中溶剂挥发，直径显著下降，最终被收集板接收；将衬底样品置于烤胶台上烘烤，使之发生交联反应，完成对纳米纤维的焊接；
步骤3：高温煅烧；
将衬底样品进行高温煅烧，分解其中的有机物，形成高质量的氧化物纳米纤维，煅烧温度为500℃，时间为120分钟；
步骤4：利用热蒸发沉积源漏电极；
将清洗干净的钨丝挂在蒸发电极的两侧，并将铝丝挂在钨丝上；抽真空，将样品放入蒸发室；对钨丝使用电流加热，等待铝丝熔成小球，当铝丝熔成小球以后关闭蒸发电源，完成镀膜。
进一步，步骤1中将水合硝酸锆加入N，N二甲基甲酰胺中，配制浓度为0.15摩尔/升的介电层前驱体溶液；所述匀胶机先低速500转/分匀胶5秒，然后高速在5000转/分匀胶20秒。
进一步，步骤2中三氯化铟0.4克，聚乙烯吡咯烷酮130万分子量、2克，双酚A型环氧树脂0.31克、T31固化剂0.09g加入到10ml N，N二甲基甲酰胺中。进一步，步骤3中煅烧温度为500℃，时间为120分钟。
附图说明
图1为本发明的静电纺丝制备纳米纤维氧化物薄膜晶体管的结构示意图；
图2为本发明涉及的环氧树脂和固化剂的分子式和交联反应示意图；
图3为本发明使用交联剂焊接前后的纳米纤维形貌对比；
图4为本发明制备的纳米纤维场效应晶体管的转移特性曲线；
图5为本发明制备的纳米纤维场效应晶体管的输出特性曲线。
具体实施方式
图1为本发明的静电纺丝制备纳米纤维氧化物薄膜晶体管的结构示意图，下面结合具体实施方式对本发明进行详细说明。
实施例1：
(1)采用溶液法制备ZrO2高k介质薄膜：
步骤1：药品和试剂均购于Aldrich公司，将水合硝酸锆加入N，N二甲基甲酰胺中，配制浓度为0.15摩尔/升的介电层前驱体溶液，在磁力搅拌器中搅拌24小时，得到澄清透明的溶液，静置24小时备用；
步骤2：选用市售的单面抛光重掺杂P型低阻硅作为衬底(～0.0015Ω·cm)和栅电极，硅衬底依次用丙酮和酒精超声波清洗各10分钟，去离子水反复冲洗后，用高纯氮气吹干；
步骤3：用匀胶机在P型硅衬底上旋涂ZrO2前驱体溶液，匀胶机先低速500转/分匀胶5秒，然后高速在5000转/分匀胶20秒；
步骤4：将样品置于150℃的烤胶台上烘烤10分钟；
步骤5：高温550℃退火2小时，得到均匀致密的ZrO2高k介质薄膜；
(2)采用静电纺丝技术制备纳米纤维网络：
步骤1：将三氯化铟(0.4克)、聚乙烯吡咯烷酮(130万分子量，2克)、环氧树脂(双酚A型环氧树脂0.31克，T31固化剂0.09g)加入到10ml N，N二甲基甲酰胺中，磁力搅拌器搅拌18小时，得到粘性的透明前驱体溶液；
步骤2：将制备得到的介电层衬底附在收集板上，收集板距针头15cm，针头处连接直流高压电源；
步骤3：注射泵推进速度为0.5毫升/小时，直流高压为15千伏，在电场力、库仑力、表面张力等共同作用下，前驱体溶液喷出并剧烈抖动，飘向衬底过程中溶剂挥发，直径显著下降，最终被收集板接收；
步骤4：将衬底样品置于150℃的烤胶台上烘烤10分钟，使之发生交联反应，反应方程式如图2所示，完成对纳米纤维的焊接；交联和未交联的纤维形貌对比图如图3所示。
(3)高温煅烧：
将衬底样品进行高温煅烧，分解其中的有机物，形成高质量的氧化物纳米纤维，煅烧温度为500℃，时间为120分钟；
(4)利用热蒸发沉积源漏电极：
步骤1：将清洗干净的钨丝挂在蒸发电极的两侧，并将经过处理的1厘米的铝丝挂在钨丝上；
步骤2：抽真空，将样品放入蒸发室，首先使用机械泵进行粗抽，当真空度达到5Pa以下时，关闭机械泵，打开分子泵进行精抽，真空度达到高真空(3×10-3Pa)；
步骤3：对钨丝使用电流加热，缓慢转动蒸发电源对钨丝，当电流达到50A时蒸发电源停止转动，等待铝丝熔成小球，当铝丝熔成小球以后关闭蒸发电源，完成镀膜。
(5)器件性能测试
将制成的In2O3/ZrO2纳米纤维场效应晶体管器件进行测试，转移曲线测试如图4，输出曲线测试如图5。
本发明还具有如下优点：
1.交联剂焊接使纳米纤维与衬底粘附性变好，纳米纤维之间的结点由于是共价连接而变得十分紧密，减少了接触电阻和界面处的电子陷阱，有利于改善界面状态和载流子传输，并且提高了器件的操作稳定性和重复性；
2.基于ZrO2高k介电层的纳米纤维网络器件，操作电压将会明显降低，功耗也随之下降，有利于在便携式移动终端中的集成；
制得的ZrO2高k介电层的禁带宽度为6eV，介电常数达到7.8，其高介电特性符合现代显示技术对于高k材料的需求；并且ZrO2薄膜本身具有的高可见光透过率也符合透明电子器件的要求；
3.本发明以环氧树脂的交联反应作为理论支撑，制备了性能、稳定性和重复性好的器件，且工艺简单，成本低廉，有广阔的应用前景，为大面积、批量制备高性能的纳米纤维场效应晶体管提供了可靠的实验方案。
以上所述仅是对本发明的较佳实施方式而已，并非对本发明作任何形式上的限制，凡是依据本发明的技术实质对以上实施方式所做的任何简单修改，等同变化与修饰，均属于本发明技术方案的范围内。
Claims (4)
1.一种可控的热焊接法制备高性能场效应晶体管的方法，其特征在于按照以下步骤进行：
步骤1：采用溶液法制备ZrO2高k介质薄膜；
将水合硝酸锆加入N，N二甲基甲酰胺中，配制介电层前驱体溶液，在磁力搅拌器中搅拌，得到澄清透明的溶液；选用单面抛光重掺杂P型低阻硅作为衬底和栅电极，硅衬底依次用丙酮和酒精超声波清洗，去离子水反复冲洗后，用高纯氮气吹干；用匀胶机在P型硅衬底上旋涂ZrO2前驱体溶液；置于烤胶台上烘烤；高温退火，得到均匀致密的ZrO2高k介质薄膜；
步骤2：采用静电纺丝技术制备纳米纤维网络；
将三氯化铟、聚乙烯吡咯烷酮、环氧树脂加入到N，N二甲基甲酰胺中，磁力搅拌器搅拌，得到粘性的透明前驱体溶液；将制备得到的介电层衬底附在收集板上，针头处连接直流高压电源；前驱体溶液喷出并剧烈抖动，飘向衬底过程中溶剂挥发，直径显著下降，最终被收集板接收；将衬底样品置于烤胶台上烘烤，使之发生交联反应，完成对纳米纤维的焊接；
步骤3：高温煅烧；
将衬底样品进行高温煅烧，分解其中的有机物，形成高质量的氧化物纳米纤维，煅烧温度为500℃，时间为120分钟；
步骤4：利用热蒸发沉积源漏电极；
将清洗干净的钨丝挂在蒸发电极的两侧，并将铝丝挂在钨丝上；抽真空，将样品放入蒸发室；对钨丝使用电流加热，等待铝丝熔成小球，当铝丝熔成小球以后关闭蒸发电源，完成镀膜。
2.按照权利要求1所述一种可控的热焊接法制备高性能场效应晶体管的方法，其特征在于：所述步骤1中将水合硝酸锆加入N，N二甲基甲酰胺中，配制浓度为0.15摩尔/升的介电层前驱体溶液；所述匀胶机先低速500转/分匀胶5秒，然后高速在5000转/分匀胶20秒。
3.按照权利要求1所述一种可控的热焊接法制备高性能场效应晶体管的方法，其特征在于：所述步骤2中三氯化铟0.4克，聚乙烯吡咯烷酮130万分子量、2克，双酚A型环氧树脂0.31克、T31固化剂0.09g加入到10ml N，N二甲基甲酰胺中。
4.按照权利要求1所述一种可控的热焊接法制备高性能场效应晶体管的方法，其特征在于：所述步骤3中煅烧温度为500℃，时间为120分钟。
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