CN111490093A - 电沉积制备石墨烯基晶体管及其沟道材料的方法 - Google Patents
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Abstract
本发明涉及一种电沉积制备石墨烯基晶体管沟道材料的方法,利用循环伏安法在源漏极上电沉积石墨烯基材料作为构成沟道。本发明通过电沉积氧化石墨烯(GO),氯金酸(HAuCl4)和氧化石墨烯(GO),氧氯化锆(ZrOCl2)和氧化石墨烯(GO),3,4‑乙烯二氧噻吩(EDOT)和氧化石墨烯(GO),制备出了石墨烯,金属与石墨烯复合,金属氧化物与石墨烯复合,聚合物与石墨烯复合的沟道材料,均得到了石墨烯特有的“U”型转移曲线。
Description
技术领域
本发明涉及的是一种新的制备晶体管沟道材料的方法,具体是利用在晶体管源漏极上电沉积得到石墨烯或石墨烯复合材料作为沟道材料。
背景技术
石墨烯因其独特的物理性质和二维结构而具有广阔的应用前景,晶体管传感器便是一种。目前应用广泛的石墨烯晶体管沟道材料多为单层石墨烯,其具有零带隙,较高的迁移率等优异性能,然而单层石墨烯使用成本较高,制备工艺复杂,且转移过程繁杂易被破坏,因此降低了其作为沟道材料的稳定性,准确性和实用性。
现有技术CN107907580A CN108593747A中,虽然分别制备了有机磷农药的晶体管化学传感器、葡萄糖的晶体管传感器,但是均采用了单层石墨烯作为沟道,并且均采用湿法转移将单层石墨烯转移到沟道上。该湿法转移过程中因实际操作流程困难复杂,常导致制备出的器件性能不稳定,重复性较差,且后续在石墨烯上进行修饰时也易破坏已转移好的石墨烯,从而影响对石墨烯沟道的修饰。
发明内容
本发明针对现有技术存在的不足,提供一种电沉积制备石墨烯基晶体管沟道材料的方法,解决了目前电化学晶体管中石墨烯沟道依赖湿法转移工艺所带来的操作困难、不易重复、成本过高的问题。
电沉积制备石墨烯基晶体管沟通材料的方法,主要步骤如下:
(1)在电化学晶体管的源极、漏极间确定沟道区域,滴加氧化石墨烯溶液,晾干后,得到氧化石墨烯修饰的沟道区域;
(2)步骤(1)所得电化学晶体管的沟道区域浸入氧化石墨烯溶液或者沟道材料的前驱体溶液中,通过循环伏安法在沟道区域沉积石墨烯或者石墨烯基复合材料作为沟道。
按上述方案,石墨烯基复合材料为前驱体溶液电沉积还原生成的固体产物的复合物。石墨烯与不同材料(包括金属,金属氧化物,聚合物)复合得到的沟道材料可用于检测不同待检测物质,前驱体溶液通过循环伏安法还原生成的固体产物用于与检测对象发生反应或催化检测对象的反应使沟道电流变化来实现对检测对象的定性或定量检测。
按上述方案,步骤(1)、步骤(2)中,所述氧化石墨烯溶液的浓度均为0.3-0.8mg/mL。
按上述方案,所述前驱体溶液为氯金酸溶液、3,4-乙烯二氧噻吩和柠檬酸钠混合溶液、氧氯化锆溶液等中的一种或几种。当前驱体溶液为氯金酸溶液时,通过循环伏安法在沟道区域沉积的石墨烯基材料为金与石墨烯的复合材料;当前驱体溶液为氧氯化锆溶液时,通过循环伏安法在沟道区域沉积的石墨烯基复合材料为二氧化锆与石墨烯的复合材料;当前驱体溶液为3,4-乙烯二氧噻吩和柠檬酸钠混合溶液时,通过循环伏安法在沟道区域沉积的石墨烯基复合材料为聚3,4-乙烯二氧噻吩与石墨烯的复合材料。
优选地,所述氯金酸溶液的浓度为1-5mM;所述氧氯化锆溶液的浓度为5-10mM;所述3,4-乙烯二氧噻吩和柠檬酸钠混合溶液中,3,4-乙烯二氧噻吩浓度为10-50mM,柠檬酸钠浓度为20-80mM。
按上述方案,所述电化学晶体管的源极、漏极为蒸发镀膜的金/铬电极,金层重叠于铬层上方,栅极优选Ag/AgCl电极。
进一步地,铬与玻璃的粘附性好,先在玻璃基底上蒸铬,然后在铬上蒸金,铬层的厚度控制在为0.3-1nm,金层的厚度控制在为30-100nm,作为电化学晶体管的电极,选定源极与漏极,源极与漏极之间的间距不超过400μm,优选100-300μm。
按上述方案,循环伏安法的扫描速度为10-100mV/s,扫描圈数20-60圈,同时在晶体管源极和漏极上进行电沉积,使沟道区域沉积上石墨烯或者石墨烯基复合材料从而联通源极和漏极。
在上述基础上,本发明还提供一种石墨烯基晶体管的制备方法,主要步骤如下:
(1)在电化学晶体管的源极、漏极间确定沟道区域,滴加氧化石墨烯溶液,干燥后,得到氧化石墨烯修饰的沟道区域;其中,源极与漏极之间间距不超过400μm;
(2)步骤(1)所得电化学晶体管的沟道区域浸入氧化石墨烯溶液或者沟道材料的前驱体溶液中,通过循环伏安法在沟道区域沉积石墨烯或者石墨烯基复合材料作为沟道;
(3)用Ag/AgCl电极作为晶体管栅极,与步骤(1)、(2)所制备的源极、漏极、沟道相结合,得到石墨烯基晶体管。
本发明与现有技术相比,采用了新方法——循环伏安法电沉积石墨烯或石墨烯复合材料来作为晶体管沟道材料,所制备的石墨烯基电化学晶体管具有石墨烯特有的“U”型转移曲线。
现有技术中采用石墨烯作为沟道的晶体管传感器,通常采用湿法转移单层石墨烯形成沟道,这是由于单层石墨烯氧化程度更低,能够直接得到高性能的石墨烯沟道。但是,湿法转移虽然是现有手段,其实湿法转移单层石墨烯的实际操作流程比较困难复杂,重复性也比较差,从而使得晶体管传感器的性能不稳定,重复性较差;而且后续在石墨烯沟道上进行修饰时也易破坏已转移好的单层石墨烯,从而限制了对石墨烯沟道的修饰。而本发明采用电沉积制备石墨烯基晶体管沟道材料的方法,在源漏极上电沉积石墨烯形成沟道,是由于沟道足够窄,使得源漏极沉积上的石墨烯能够联通作为沟道。本发明中,电沉积石墨烯作为沟道材料需要把控好沟道宽度(源漏极之间的距离),沉积圈数来使得石墨烯成功沉积。本发明所述方法易于操作,重现性好,成本低,利于后续得到稳定、重复性好的晶体管传感器。
附图说明
图1为实施例1中制备的石墨烯(A),金与石墨烯的复合材料(B),二氧化锆与石墨烯的复合材料(C),聚3,4-乙烯二氧噻吩与石墨烯的复合材料(D)的FE-SEM图;
图2为实施例1中沟道分别是石墨烯(A),金/石墨烯复合材料(B),二氧化锆/石墨烯复合材料(C),聚3,4-乙烯二氧噻吩/石墨烯复合材料(D)的晶体管的转移曲线。
具体实施方式
为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明不仅仅局限于下面的实施例。
实施例1
电沉积制备石墨烯基晶体管沟道材料以及制备石墨烯基晶体管的方法,其步骤如下:
第一步,通过蒸发镀膜法将金和铬镀到1x1cm的玻璃基底上,铬的厚度控制在为0.3-1nm左右,金的厚度控制在为30-100nm左右,作为晶体管的栅极、源极、漏极,源极与漏极之间间距为250μm;
第二步,用胶带在沟道处固定出5mm×5mm大小,将氧化石墨烯超声1h分散于超纯水后滴涂在固定好的沟道处,氧化石墨烯浓度为0.5mg/mL,自然晾干,晶体管的沟道区域修饰上氧化石墨烯;
第三步,1、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数20圈,将第二步所得晶体管的沟道区域在0.5mg/mL氧化石墨烯溶液中沉积得到石墨烯,作为晶体管的沟道;2、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数20圈,将第二步所得晶体管的沟道区域在2mM氯金酸溶液中沉积得到金与石墨烯复合材料,作为晶体管的沟道;3、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数20圈,将第二步所得晶体管的沟道区域在5mM氧氯化锆溶液中沉积得到二氧化锆与石墨烯复合材料;4、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数20圈,将第二步所得晶体管的沟道区域在20mM 3,4-乙烯二氧噻吩,30mM柠檬酸钠溶液中沉积得到聚3,4-乙烯二氧噻吩与石墨烯复合材料,作为晶体管的沟道;
第四步,设定数字源表的VDS=0.05V,VG从0到2V,用Ag/AgCl电极作为晶体管栅极,将器件浸入缓冲溶液中,用数字源表检测晶体管的转移曲线。
由图1可知:在晶体管沟道上电沉积石墨烯呈现褶皱状结构;在晶体管沟道上电沉积金与石墨烯复合材料可以看到金纳米粒子均匀附着在褶皱状的石墨烯表面;在晶体管沟道上电沉积二氧化锆与石墨烯复合材料同样呈现褶皱状结构,主要原因是二氧化锆结晶性能不好;在晶体管沟道上电沉积3,4-乙烯二氧噻吩与石墨烯复合材料表面呈网状交织结构。
由图2可知:电沉积石墨烯,金与石墨烯复合材料,二氧化锆与石墨烯复合材料,聚3,4-乙烯二氧噻吩与石墨烯复合材料均得到了石墨烯特有的“U”型曲线,此时分别对应的晶体管传感器可分别用于实际定性或定量检测过氧化氢,葡萄糖,甲基对硫磷,对乙酰氨基酚。“U”型曲线显示了石墨烯的双极性行为,在水溶液中石墨烯窄带隙,使得在栅电压和沟道电压作用下电子很容易从石墨烯价带转移到导带与空穴结合,随着栅电压增大,电子填满空穴并逐渐累积,导致载流子浓度先减小后增大,从而出现“U”型曲线,表示石墨烯沉积上了。
石墨烯与不同材料复合作为沟道,得到转移曲线显示出的狄拉克点不同。图2(A)中,电沉积石墨烯作为沟道的晶体管转移曲线狄拉克点为0.7V;图2(B)中,电沉积金与石墨烯复合材料作为沟道的晶体管转移曲线狄拉克点为1.17V;图2(C)中,电沉积二氧化锆与石墨烯复合材料作为沟道的晶体管转移曲线狄拉克点为1.1V;图2(D)中,电沉积聚3,4-乙烯二氧噻吩与石墨烯复合材料作为沟道的晶体管转移曲线狄拉克点为1.05V。
实施例2
电沉积制备石墨烯基晶体管沟道材料以及制备石墨烯基晶体管的方法,其步骤如下:
第一步,通过蒸发镀膜法将金和铬镀到1x1cm的玻璃基底上,铬的厚度控制在为0.3-1nm左右,金的厚度控制在为30-100nm左右,作为晶体管的栅极、源极、漏极,源极与漏极之间间距为100μm;
第二步,用胶带在沟道处固定出5mm×5mm大小,将氧化石墨烯超声1h分散于超纯水后滴涂在固定好的沟道处,氧化石墨烯浓度为0.8mg/mL,自然晾干,晶体管的沟道区域修饰上氧化石墨烯;
第三步,1、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数20圈,将第二步所得晶体管的沟道区域在0.5mg/mL氧化石墨烯溶液中沉积得到石墨烯,作为晶体管的沟道;2、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数20圈,将第二步所得晶体管的沟道区域在4mM氯金酸溶液中沉积得到金与石墨烯复合材料,作为晶体管的沟道;3、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数20圈,将第二步所得晶体管的沟道区域在8mM氧氯化锆溶液中沉积得到二氧化锆与石墨烯复合材料;4、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数20圈,将第二步所得晶体管的沟道区域在40mM 3,4-乙烯二氧噻吩,60mM柠檬酸钠溶液中沉积得到聚3,4-乙烯二氧噻吩与石墨烯复合材料,作为晶体管的沟道;
第四步,设定数字源表的VDS=0.05V,VG从0到2V,用Ag/AgCl电极作为晶体管栅极,将器件浸入缓冲溶液中,用数字源表检测晶体管的转移曲线。
电沉积石墨烯,金与石墨烯复合材料,二氧化锆与石墨烯复合材料,聚3,4-乙烯二氧噻吩与石墨烯复合材料均得到了石墨烯特有的“U”型曲线,可用于实际检测。石墨烯与不同材料复合作为沟道,得到转移曲线显示出的狄拉克点不同。
实施例3
电沉积制备石墨烯基晶体管沟道材料以及制备石墨烯基晶体管的方法,其步骤如下:
第一步,通过蒸发镀膜法将金和铬镀到1x1cm的玻璃基底上,铬的厚度控制在为0.3-1nm左右,金的厚度控制在为30-100nm左右,作为晶体管的栅极、源极、漏极,源极与漏极之间间距为250μm;
第二步,用胶带在沟道处固定出5mm×5mm大小,将氧化石墨烯超声1h分散于超纯水后滴涂在固定好的沟道处,氧化石墨烯浓度为0.3mg/mL,自然晾干,晶体管的沟道区域修饰上氧化石墨烯;
第三步,1、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数20圈,将第二步所得晶体管的沟道区域在0.5mg/mL氧化石墨烯溶液中沉积得到石墨烯,作为晶体管的沟道;2、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数30圈,将第二步所得晶体管的沟道区域在2mM氯金酸溶液中沉积得到金与石墨烯复合材料,作为晶体管的沟道;3、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数30圈,将第二步所得晶体管的沟道区域在5mM氧氯化锆溶液中沉积得到二氧化锆与石墨烯复合材料;4、使用电化学工作站设定循环伏安法的扫描速度为50mV/s,扫描圈数30圈,将第二步所得晶体管的沟道区域在20mM 3,4-乙烯二氧噻吩,30mM柠檬酸钠溶液中沉积得到聚3,4-乙烯二氧噻吩与石墨烯复合材料,作为晶体管的沟道;
第四步,设定数字源表的VDS=0.05V,VG从0到2V,用Ag/AgCl电极作为晶体管栅极,将器件浸入缓冲溶液中,用数字源表检测晶体管的转移曲线。
电沉积石墨烯,金与石墨烯复合材料,二氧化锆与石墨烯复合材料,聚3,4-乙烯二氧噻吩与石墨烯复合材料均得到了石墨烯特有的“U”型曲线,可用于实际检测。石墨烯与不同材料复合作为沟道,得到转移曲线显示出的狄拉克点不同。
以上所述仅是本发明的优选实施方式,应当指出,对于本领域的普通技术人员来说,在不脱离本发明创造构思的前提下,还可以做出若干改进和变换,这些都属于本发明的保护范围。
Claims (10)
1.电沉积制备石墨烯基晶体管沟通材料的方法,其特征在于主要步骤如下:
(1)在电化学晶体管的源极、漏极间确定沟道区域,滴加氧化石墨烯溶液,干燥后,得到氧化石墨烯修饰的沟道区域;其中,源极与漏极之间间距不超过400μm;
(2)步骤(1)所得电化学晶体管的沟道区域浸入氧化石墨烯溶液或者沟道材料的前驱体溶液中,通过循环伏安法在沟道区域沉积石墨烯或者石墨烯基复合材料作为沟道。
2.根据权利要求1所述的电沉积制备石墨烯基晶体管沟通材料的方法,其特征在于步骤(1)、步骤(2)中,所述氧化石墨烯溶液的浓度均为0.3-0.8mg/mL。
3.根据权利要求1所述的电沉积制备石墨烯基晶体管沟通材料的方法,其特征在于所述前驱体溶液为氯金酸溶液、3,4-乙烯二氧噻吩和柠檬酸钠混合溶液、氧氯化锆溶液中的一种;当前驱体溶液为氯金酸溶液时,通过循环伏安法在沟道区域沉积的石墨烯基材料为金与石墨烯的复合材料;当前驱体溶液为氧氯化锆溶液时,通过循环伏安法在沟道区域沉积的石墨烯基复合材料为二氧化锆与石墨烯的复合材料;当前驱体溶液为3,4-乙烯二氧噻吩和柠檬酸钠混合溶液时,通过循环伏安法在沟道区域沉积的石墨烯基复合材料为聚3,4-乙烯二氧噻吩与石墨烯的复合材料。
4.根据权利要求3所述的电沉积制备石墨烯基晶体管沟通材料的方法,其特征在于所述氯金酸溶液的浓度为1-5mM;所述氧氯化锆溶液的浓度为5-10mM;所述3,4-乙烯二氧噻吩和柠檬酸钠混合溶液中,3,4-乙烯二氧噻吩浓度为10-50mM,柠檬酸钠浓度为20-80mM。
5.根据权利要求1所述的电沉积制备石墨烯基晶体管沟通材料的方法,其特征在于源极与漏极之间的间距为100-300μm。
6.根据权利要求1所述的电沉积制备石墨烯基晶体管沟通材料的方法,其特征在于循环伏安法的扫描速度为10-100mV/s,扫描圈数20-60圈。
7.采用权利要求1所述方法制备的石墨烯基晶体管沟通材料。
8.采用权利要求7所述沟道材料的电化学晶体管传感器。
9.根据权利要求8所述的电化学晶体管传感器,其特征在于所述电化学晶体管的源极、漏极为金/铬电极,金层重叠于铬层上方,栅极为Ag/AgCl电极。
10.一种石墨烯基晶体管的制备方法,其特征在于主要步骤如下:
(1)在电化学晶体管的源极、漏极间确定沟道区域,滴加氧化石墨烯溶液,干燥后,得到氧化石墨烯修饰的沟道区域;其中,源极与漏极之间间距不超过400μm;
(2)步骤(1)所得电化学晶体管的沟道区域浸入氧化石墨烯溶液或者沟道材料的前驱体溶液中,通过循环伏安法在沟道区域沉积石墨烯或者石墨烯基复合材料作为沟道;
(3)用Ag/AgCl电极作为晶体管栅极,与步骤(1)、(2)所制备的源极、漏极、沟道相结合,得到石墨烯基晶体管。
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