CN107017309A - 一种溶液法制备三元p型金属氧化物薄膜晶体管的方法 - Google Patents
一种溶液法制备三元p型金属氧化物薄膜晶体管的方法 Download PDFInfo
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Abstract
本发明属于薄膜晶体管制备技术领域，涉及一种溶液法制备三元p型金属氧化物薄膜晶体管的方法，用于三元p型金属氧化物半导体薄膜及薄膜晶体管制备场合；解决传统TFT器件载流子迁移率低，制备成本昂贵，反应条件苛刻的难题，实现低成本制备高性能低能耗的三元p型金属氧化物薄膜晶体管，制得的产物为Ni/CuCrO2/SiO2/Si结构的薄膜晶体管；用低阻硅作为衬底，用致密的SiO2作为栅介电层，采用“两步退火”技术和溶胶凝胶技术制备三元p型CuCrO2半导体薄膜作为沟道层；其工艺简单，原理可靠，节能环保，制备成本低廉，产品性能好，能够用于工业化生产，具有良好的经济效益和广阔的市场前景。
Description
技术领域：
本发明属于薄膜晶体管制备技术领域，涉及一种金属氧化物薄膜晶体管的制备方法，尤其是一种溶液法制备三元p型金属氧化物薄膜晶体管的方法，用于三元p型金属氧化物半导体薄膜及薄膜晶体管制备场合。
背景技术：
近年来，金属氧化物薄膜晶体管(Metal-Oxide Thin-Film Transistor，简称MOTFT)在有源矩阵驱动液晶显示器件(Active Matrix Liquid Crystal Display,简称AMLCD)中发挥了重要作用。从低温非晶硅薄膜晶体管到高温多晶硅薄膜晶体管，技术越来越成熟，应用对象也从只能驱动液晶显示器件(Liquid Crystal Display，简称LCD)发展到既可以驱动LCD又可以驱动有机发光显示器(Organic Light Emitting Display，简称OLED)，甚至电子纸。薄膜晶体管(简称TFT)已经成为平板显示行业的核心部件，每台显示器都集成了数百万甚至上亿个TFT器件。目前研究与应用最多的金属氧化物材料为ZnO、SnO2和In2O3体系(Nature,432488,2004；Nature Materials,10382,2011)。然而，这些氧化物材料均为n型半导体，极大的限制了互补金属氧化物半导体(Complementary Metal OxideSemiconductor,简称CMOS)器件和数字集成电路的发展。为了实现高共模输入范围和高输出电压摆幅的CMOS器件，有机TFT通常被用作其中的p型单元器件(Advanced Materials223598,2010)。但是有机TFT的低迁移率和环境不稳定性仍然是目前难以攻克的难关。基于上述原因，发展p型金属氧化物材料及其TFT器件对于大规模CMOS集成电路的发展具有重要的意义。
目前，用作TFT器件沟道层的p型金属氧化物主要以二元为主，一般为CuO、Cu2O、NiO、SnO等金属氧化物，但由于二元p型金属氧化物非常有限，对p型材料的探索已逐步拓展到三元。二元p型金属氧化物是指包括两种元素，一种为氧元素，另一种为金属元素，以空穴作为载流子传导电荷的一类金属氧化物；三元p型金属氧化物则包含三种元素，如CuCrO2、CuAlO2、CuGaO2等。三元p型金属氧化物主要应用于太阳能电池的窗口层、平板显示器、低辐射窗、触摸屏、飞机和冰箱的除霜窗口、气体传感器、抗静电涂料的制备，鲜有研究记载将三元p型金属氧化物用作TFT沟道层；此外，三元p型金属氧化物的制备大多基于真空沉积方法，如磁控溅射、脉冲激光沉积、热蒸发等，这类真空制备工艺需要依托昂贵的设备且难以实现大面积成膜，制约了低成本电子器件的生产；考虑到将来电子器件发展的新方向─“印刷电子器件”，因此，研究低成本大规模制备三元p型金属氧化物作为TFT沟道层的方法是推动透明电子学发展应用的关键，目前，尚无关于溶液法制备三元p型金属氧化物薄膜晶体管的方法的研究记载。
发明内容：
本发明的目的在于克服现有技术存在的不足，寻求设计一种溶液法制备三元p型金属氧化物薄膜晶体管的方法，解决传统TFT器件载流子迁移率低，制备成本昂贵，反应条件苛刻的难题，实现低成本制备高性能低能耗的三元p型金属氧化物薄膜晶体管，制得的产物为Ni/CuCrO2/SiO2/Si结构的薄膜晶体管。
为了实现上述目的，本发明涉及的溶液法制备三元p型金属氧化物薄膜晶体管的方法，采用“两步退火”技术和溶胶凝胶技术制备三元p型CuCrO2半导体薄膜作为沟道层，用低阻硅作为衬底，用致密的SiO2作为栅介电层，制备成三元p型金属氧化物薄膜晶体管，具体工艺步骤为：
(1)清洗衬底：首先选取电阻率为0.0015Ω·cm的低阻硅作为衬底，并依次用丙酮和无水乙醇超声波清洗衬底各5-15分钟，用去离子水冲洗3-5次，再用纯度为99.99％的氮气吹干备用；
(2)热氧化法制备SiO2栅介电层的制备：接着将切好的厚度为200-800微米的硅片放入管式炉内，800-1200℃条件下退火20-200分钟，制得均匀致密的SiO2栅介电层薄膜成品，完成栅介电层薄膜的制备；
(3)采用两步退火法制备沟道层：然后以乙二醇甲醚作为溶剂，称量适量纯度均大于98％的醋酸铜Cu(COOCH3)2和九水硝酸铬Cr(NO3)2.9H2O加入溶剂中，其中，混合液中金属阳离子总量为0.01-0.5mol/L，Cu和Cr离子原子比为0到1:5；在20-90℃条件下磁力搅拌1-24小时形成澄清的溶液，完成沟道层前驱体溶液的配制；将配制的沟道层前驱体溶液旋涂在步骤(2)制得的SiO2栅介电层薄膜成品上，旋涂次数为1-5次，每增加一次旋涂薄膜厚度增加5-20nm，5000-8000转/分转速下匀胶10-35秒，旋涂结束后先将制得的p型金属氧化物半导体薄膜半成品放到烤胶台上，300-450℃空气条件下退火15-35分钟，然后再放到管式炉内，500-900℃氮气氛围下退火2-4小时，氮气纯度大于99％，制得CuCrO2半导体薄膜成品，完成沟道层半导体薄膜的制备；
(4)热蒸发法制备源、漏电极：最后通过热蒸发的方式，在步骤(3)制得的沟道层半导体薄膜上用宽长比为1000/100μm的不锈钢掩膜版制备厚度为80-120nm的金属Ni作为源、漏电极，制得Ni/CuCrO2/SiO2/Si结构的薄膜晶体管，完成三元p型金属氧化物薄膜晶体管的制备。
制得的Ni/CuCrO2/SiO2/Si结构的薄膜晶体管的载流子迁移率为2.03cm2/V s,开关比达到103以上。
本发明涉及的溶液法制备三元p型金属氧化物薄膜晶体管的方法的工作原理为：首先利用致密的SiO2作为三元p型TFT器件的栅介电层；然后采用两步退火法制备沟道层，前期在空气中退火，其目的为蒸发溶剂并分解前躯体溶液中的有机物，后期在氮气氛围中退火使Cu2+被还原为Cu+,促进CuCrO2晶向的生成；最后通过热蒸发法制备源、漏电极，完成基于SiO2介电层的三元p型CuCrO2/SiO2薄膜晶体管的制备，制得的产物具有优异的电学性能，为高性能CMOS器件的发展奠定良好的科学基础。
本发明与现有技术相比，一是采用“溶胶凝胶法”制备，其制备工艺不依赖昂贵的真空镀膜设备，解决了传统真空技术制备三元p型金属氧化物高昂制备成本的难题；同时，能够满足未来“印刷电子器件”的要求，也是本领域首次采用溶液技术制备三元p型金属氧化物TFT器件；二是采用“两步退火”技术，首先在空气中退火分解前躯体溶液中的有机物，然后氮气氛围中退火使Cu2+被还原为Cu+从而实现制备CuCrO2半导体薄膜的可能；三是制得的CuCrO2/SiO2TFT器件展现出优异的电学性能，其迁移率远大于传统SiO2基的二元p型金属氧化物TFT器件的迁移率，其报道的最大值仅为0.32cm2/V s；四是制得的三元CuCrO2相对于二元的p型CuO具有禁带宽度大的优势。因此，在低能耗电子显示、CMOS集成领域具有有广阔的应用前景，其工艺简单，原理可靠，节能环保，制备成本低廉，产品性能好，能够用于工业化生产，具有良好的经济效益和广阔的市场前景。
附图说明：
图1为本发明涉及的溶液法制备三元p型金属氧化物薄膜晶体管的方法的流程框图。
图2为本发明涉及的三元p型金属氧化物薄膜晶体管的主体结构原理示意图。
图3为氮气氛围下退火过程中晶向转变的原子结构示意图。
图4为本发明制备的Ni/CuCrO2/SiO2/Si结构的薄膜晶体管的转移特性曲线图，其中，5条曲线分别为500℃,600℃,700℃,800℃,900℃下的氮气氛围中的退火的转移曲线。
具体实施方式：
下面通过具体实施例并结合附图作进一步说明。
实施例1：
本实施例涉及的溶液法制备三元p型金属氧化物薄膜晶体管的方法如图1所示，具体包括以下工艺步骤：
(1)清洗衬底：首先选取电阻率为0.0015Ω·cm的低阻硅作为衬底，并依次用丙酮和无水乙醇超声波清洗衬底各10分钟，用去离子水冲洗3-5次，再用纯度为99.99％的氮气吹干备用；
(2)热氧化法制备栅介电层：将切好的厚度为200-800微米硅片放入管式炉内1000℃退火，升温速率为7℃/min,保温时间为100分钟,制得均匀连续的SiO2栅介电层薄膜成品，完成栅介电层薄膜的制备；
(3)采用两步退火法制备沟道层：称量10mL的乙二醇甲醚作为溶剂，称量适量的醋酸铜Cu(COOCH3)2和九水硝酸铬Cr(NO3)2.9H2O加入溶剂中，其中，金属阳离子总量0.01-0.5mol/L，Cu和Cr离子原子比为0到1:5；醋酸铜和九水硝酸铬均购于Aldrich公司，醋酸铜和九水硝酸铬的纯度均大于99％，在20-90℃条件下磁力搅拌1-24小时形成澄清的溶液，完成沟道层前驱体溶液的配制；将配制的沟道层前驱体溶液旋涂在步骤(2)制得的SiO2栅介电层薄膜成品上，旋涂次数为1-5次，每增加一次旋涂薄膜厚度增加5-20nm，旋涂时在5000-8000转/分转速下匀胶10-35秒，旋涂结束后先将制得的p型金属氧化物半导体薄膜半成品放到烤胶台上300-450℃空气退火15-35分钟，然后再放到管式炉内退火，采用纯度大于99％的氮气作为保护气体，退火温度分别为500，600,700,800,900℃，退火时间为2-4小时，制得CuCrO2半导体薄膜成品，完成三元p型金属氧化物半导体薄膜的制备，其能够用作三元p型金属氧化物薄膜晶体管的沟道层；
(4)热蒸发法制备源、漏电极：最后通过热蒸发的方式，在步骤(3)制得的沟道层半导体薄膜上用宽长比为1000/100μm的不锈钢掩膜版制备厚度为80-120nm的金属Ni作为源、漏电极，制备得到Ni/CuCrO2/SiO2/Si结构的薄膜晶体管。
制得的Ni/CuCrO2/SiO2/Si结构的薄膜晶体管的载流子迁移率为2.03cm2/V s,开关比达到103以上。
对制得的三元p型金属氧化物薄膜晶体管进行测试，图2为主体结构原理示意图；图3为氮气氛围下退火过程中晶向转变的原子结构示意图,由图3可知，氮气氛围下Cu2+被还原为Cu+，实现了CuCr2O4到CuCrO2的晶向转变；图4为不同退火温度下的器件的转移曲线，由图4可知，随着栅压的减小，源漏电流逐渐增大，表现出典型的P型半导体性质，同时随着退火温度从500度升高至800度，器件的开态电流逐渐提高，表明器件的电流调制能力得到提高，测试结果均由吉时利2634B半导体源表测试得到。
Claims (4)
1.一种溶液法制备三元p型金属氧化物薄膜晶体管的方法，其特征在于具体工艺步骤为：
(1)清洗衬底：首先选取电阻率为0.0015Ω·cm的低阻硅作为衬底，并依次用丙酮和无水乙醇超声波清洗衬底各5-15分钟，用去离子水冲洗3-5次，再用纯度为99.99％的氮气吹干备用；
(2)热氧化法制备SiO2栅介电层的制备：接着将厚度为200-800微米的硅片放入管式炉内，800-1200℃条件下退火20-200分钟，制得均匀致密的SiO2栅介电层薄膜成品，完成栅介电层薄膜的制备；
(3)采用两步退火法制备沟道层：然后以乙二醇甲醚作为溶剂，称量适量纯度均大于98％的醋酸铜Cu(COOCH3)2和九水硝酸铬Cr(NO3)2·9H2O加入溶剂中，其中，混合液中金属阳离子总量为0.01-0.5mol/L，Cu和Cr离子原子比为0到1:5；在20-90℃条件下磁力搅拌1-24小时形成澄清的溶液，完成沟道层前驱体溶液的配制；将配制的沟道层前驱体溶液旋涂在步骤(2)制得的SiO2栅介电层薄膜成品上，旋涂次数为1-5次，每增加一次旋涂薄膜厚度增加5-20nm，在5000-8000转/分转速下匀胶10-35秒，旋涂结束后先将制得的三元p型金属氧化物半导体薄膜半成品放到烤胶台上，300-450℃空气条件下退火15-35分钟，然后再放到管式炉内，500-900℃氮气氛围下退火2-4小时，氮气纯度大于99％，制得CuCrO2半导体薄膜成品，完成沟道层半导体薄膜的制备；
(4)热蒸发法制备源、漏电极：最后通过热蒸发的方式，在步骤(3)制得的沟道层半导体薄膜上用宽长比为1000/100μm的不锈钢掩膜版制备厚度为80-120nm的金属Ni作为源、漏电极，制得Ni/CuCrO2/SiO2/Si结构的薄膜晶体管，完成三元p型金属氧化物薄膜晶体管的制备。
2.如权利要求1所述的溶液法制备三元p型金属氧化物薄膜晶体管的方法，其特征在于采用该方法制得的Ni/CuCrO2/SiO2/Si结构的薄膜晶体管，其载流子迁移率为2.03cm2/V s，开关比达到103以上。
3.如权利要求1所述的溶液法制备三元p型金属氧化物薄膜晶体管的方法，其特征在于采用该方法制得的三元p型金属氧化物半导体薄膜的具体工艺步骤为：首先以乙二醇甲醚作为溶剂，称量适量纯度均大于98％的醋酸铜Cu(COOCH3)2和九水硝酸铬Cr(NO3)2.9H2O加入溶剂中，其中，混合液中金属阳离子总量为0.01-0.5mol/L，Cu和Cr离子原子比为0到1:5；在20-90℃条件下磁力搅拌1-24小时形成澄清的溶液，完成沟道层前驱体溶液的配制；将配制的沟道层前驱体溶液旋涂在SiO2栅介电层薄膜成品上，旋涂次数为1-5次，每增加一次旋涂薄膜厚度增加5-20nm，在5000-8000转/分转速下匀胶10-35秒，旋涂结束后先将制得的三元p型金属氧化物半导体薄膜半成品放到烤胶台上，300-450℃空气条件下退火15-35分钟，然后再放到管式炉内，500-900℃氮气氛围下退火2-4小时，氮气纯度大于99％，制得CuCrO2半导体薄膜成品，完成三元p型金属氧化物半导体薄膜的制备。
4.如权利要求3所述的溶液法制备三元p型金属氧化物薄膜晶体管的方法，其特征在于采用该方法制得的CuCrO2半导体薄膜能够用作三元p型金属氧化物薄膜晶体管的沟道层。
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| CN110690107B (zh) * | 2019-12-09 | 2020-05-12 | 广州新视界光电科技有限公司 | 一种半导体氧化物薄膜、其制备方法及包含其的薄膜晶体管 |
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