CN113054055A - 一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器及其制备方法 - Google Patents
一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器及其制备方法 Download PDFInfo
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Abstract
本发明属于光探测技术领域,具体涉及一种自驱动光电探测器,该自驱动光电探测器,由上至下依次包括导电银胶点电极、金属钯前电极、硒化锡纳米薄膜层、二氧化锡多层球壳结构薄膜层、硅单晶基底和金属铟背电极。二氧化锡多层球壳结构薄膜层通过水热法、煅烧法、丝网印刷技术等方法制备,硒化锡薄膜层由直流磁控溅射技术制备,器件表现出良好的自驱动光探测性能,稳定性好,从紫外到近红外区域都具有响应特性。
Description
技术领域
本发明属于光探测技术领域,具体涉及一种自驱动光电探测器及其制备方法。
技术背景
光信号到电信号的转换是现在日常生活中许多技术的核心,光电探测器就是通过光电效应实现这一光电转换的电子器件。它的一些应用已经趋于成熟,例如视频成像、光学信息、生物成像、夜视仪等。随着应用的需求和发展,对于光电探测中更快的响应、更宽的波长响应范围,以及灵活性,高效性等要求也越来越高。[Inorg.Chem.Front.,2019,6,1968]金属氧化物具有优异的耐热性、抗毒性和稳定性等,并且无毒、廉价、容易制备,二氧化锡(SnO2)作为一种优秀的透明导电半导体氧化物,具有超宽的禁带宽度,SnO2材料制成的纳米结构对紫外光具有较好的吸收,在可见和红外区域也具有良好的透光性,因此在光电领域具有较高的应用价值。但由于其载流子的分离、复合率高,导致其光谱响应较差,这极大的限制了SnO2在光学领域的应用。因此拓宽其光谱响应范围、降低其载流子的复合速率,与此同时保持SnO2在光电探测中的稳定性,是当前研究的重难点。[Advanced ElectronicMaterials,2019:1901048.]通过水热法、煅烧法等手段制备出SnO2多层球壳结构,这一多层球壳结构存在丰富的空腔,可以对光线进行多次折射和反射,可以提高探测器的光线吸收能力。
硒化锡(SnSe)作为一种窄带隙的二维半导体材料,对太阳光谱具有较宽范围的吸收,从紫外到近红外区域都具有良好的光响应特性,在宽光带光电探测器领域具有广阔的应用前景。[Ceramics International,45,2019,13275-13282]将SnSe与SnO2相结合,有望提高SnO2基光电探测器在近红外区域的光响应特性。
发明内容
本发明的目的在于提供一种具有自驱动光响应功能,且周期性好的SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器及其制备方法,可以提高目前SnO2基自驱动光电探测器在近红外区域的光电探测性能。
本发明为实现上述目的所要解决的技术问题是,通过水热法、煅烧法、丝网印刷法、磁控溅射法等方法,提高光电探测器的性能,即通过水热法、煅烧法、丝网印刷技术等在硅基底表面制备SnO2多层球壳结构薄膜层,再通过磁控溅射法在SnO2表面溅射SnSe薄膜层,以获得具有优异性能的自驱动光电探测器。
本发明为实现上述目的所采用的技术方案是,一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器,其特征在于,所制备探测器为层状结构,由上至下依次包括导电银胶点电极、金属Pd前电极、SnSe纳米薄膜层、SnO2多层球壳结构薄膜层、Si单晶基底和金属In背电极。
本发明所阐述的一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器的制备方法,其特征在于包括以下步骤:
(1)切出所需大小Si片,分别用离子水、丙酮、无水乙醇依次清洗,去除表面污染物;
(2)对清洗完成后的Si基底进行干燥;
(3)将10.27克蔗糖溶解于60毫升去离子水中,磁力搅拌5~10分钟至蔗糖溶解,把蔗糖溶液倒入100毫升聚四氟乙烯反应釜内衬中进行水热反应,在180~200摄氏度下反应4~6小时,自然冷却至室温;
(4)将步骤(3)得到的黑色产物用去离子水和无水乙醇交替进行真空抽滤6~8次,将固体产物置于60~70摄氏度的恒温干燥箱中干燥3~4小时,再次用无水乙醇进行抽滤,再干燥12~24小时;
(5)取步骤(4)干燥后的碳球,研磨备用,将0.12克氢氧化钠溶于60毫升去离子水,磁力搅拌5~10分钟得到氢氧化钠溶液,用电子天平称取2~3克碳球溶于氢氧化钠溶液,静置碱化5~6小时,用去离子水对碱化碳球抽滤3至4次,置于60~70摄氏度的恒温干燥箱中12~24小时;
(6)称取25克~30克五水四氯化锡晶体溶于20毫升去离子水和20毫升无水乙醇的混合溶液,磁力搅拌至晶体完全溶解,称取步骤(5)得到的样品1克,置于四氯化锡溶液中超声分散20分钟,随后放置于磁力搅拌器搅拌5小时,样品用去离子水真空抽滤3至4次,置于60~70摄氏度的恒温干燥箱中12~24小时;
(7)取步骤(6)的黑色产物研磨均匀,分散至石英舟置于马弗炉中煅烧,在空气气氛中以每分钟1摄氏度的升温速率升温至500摄氏度,保温2小时,自然冷却至室温;
(8)取3~4克乙基纤维素缓慢加入20毫升无水乙醇中,磁力搅拌30~40小时;
(9)取0.1~0.2克步骤(8)溶胀后的乙基纤维素、0.3克松油醇、步骤(7)得到的SnO2白色粉末,1毫升乙酸,1毫升乙醇置于大小合适的研钵中研磨1小时,用250目~350目的丝网印刷板将浆料刮涂在Si片上,刮涂2至3次,每次刮涂之间将样品置于60~70摄氏度干燥箱中干燥10分钟;
(10)取步骤(9)的样品置于马弗炉煅烧,以每分钟2摄氏度的升温速率升至450摄氏度,450摄氏度下保温2小时,冷却至室温;
(11)将步骤(10)得到的样品放入磁控溅射仪的溅射室,在氩气环境下,采用直流磁控溅射技术,通过电离出的氩离子轰击SnSe靶材,在SnO2多壳球层结构薄膜层表面溅射SnSe薄膜,所用SnSe靶材纯度为99.9%,背景真空为5×10-4帕斯卡,氩气气氛维持1.0帕斯卡,溅射功率为10瓦,靶基距为50毫米,薄膜的沉积温度为450摄氏度,所有样品溅射完成后在450摄氏度下退火30分钟,随后冷却至室温;
(12)将步骤(11)得到的样品取出,并在SnSe薄膜层表面覆盖正方形掩膜片,将样品放入磁控溅射仪的溅射室;选取直流磁控溅射技术,利用电离出的氩离子轰击金属Pd靶材,在SnSe薄膜层表面沉积金属Pd前电极;所用靶材为金属Pd靶,靶材纯度为99.9%;氩气气压维持5.0帕斯卡,靶基距为50毫米,Pd电极的沉积温度为室温,金属Pd前电极厚度为5~15纳米;
(13)在pd前电极滴涂导电银胶,在Si基底面涂覆In电极,并引出金属Cu导线,完成器件的制备。
优选的,步骤(1)中,所述硅基底为n型硅单晶基底,尺寸为10毫米×10毫米,电阻率为0.1~1欧姆·厘米。
优选的,步骤(3)中,所述水热反应温度为200摄氏度,反应时间为4小时。
优选的,步骤(12)中,所述掩模片为不锈钢材质,厚度为0.1毫米,尺寸为12毫米×12毫米,孔径尺寸为5毫米×5毫米。
优选的,步骤(13)中,所述金属In电极所用原料In的纯度为99.5%,金属Pd前电极上金属In电极大小和厚度分别为1毫米×1.5毫米和1毫米,Si基底上金属In电极大小和厚度均分别为10毫米×10毫米和2毫米,Cu导线直径为0.1毫米。
经上述步骤所制光电探测器在室温,无外加偏压下具有光响应特性,可实现从紫外到近红外的光探测,器件有优异的稳定性和周期重复性,本发明所涉及的光电探测器及制备方法无毒、成本低廉、光响应性能显著,可广泛应用于光电探测器领域。
附图说明
图1为所制备器件光电探测性能测量的结构示意图。
图2为所制备器件的对数伏安特性曲线。
图3为所制备器件在无外加偏压时器件对不同光功率密度光的响应性能。
图4为所制备器件在无外加偏压时在不同波长单色光照射下对应的响应度(R)、灵敏度(S)、探测度(D*)。
具体实施方式
本发明利用水热法、煅烧法,丝网印刷等方法,在Si半导体基底上制备SnO2多层球壳结构薄膜层,通过磁控溅射法在SnO2表面溅射SnSe薄膜层,再通过直流磁控溅射技术沉积金属Pd前电极,分别在Pd前电极上滴涂导电银胶点电极以及Si基底背面压制金属In电极并分别连接金属导线,形成器件,当光照射到器件时,由于光电效应以及内建电场的存在,器件可以实现自驱动光响应。
下面结合实施例和附图,对本发明进行详细说明。
本发明是一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器,包括SnSe薄膜层、SnO2多层球壳结构薄膜层和Si半导体基底。
进一步地说,在SnSe薄膜层表面溅射Pd前电极时,表面覆盖有掩模片,掩模片位于SnSe薄膜层与金属Pd前电极之间,掩模片所用材料为不锈钢,厚度为0.1毫米,尺寸为12毫米×12毫米,中心是5毫米×5毫米正方形孔径;金属Pd前电极是利用直流磁控溅射技术制备的,厚度为5~15纳米。
上述器件的制备方法,具体包括以下步骤:
(1)切出所需大小Si片,分别用离子水、丙酮、无水乙醇依次清洗,去除表面污染物;
(2)对清洗完成后的Si基底进行干燥;
(3)将10.27克蔗糖溶解于60毫升去离子水中,磁力搅拌5~10分钟至蔗糖溶解,把蔗糖溶液倒入100毫升聚四氟乙烯反应釜内衬中进行水热反应,在180~200摄氏度下反应4~6小时,自然冷却至室温;
(4)将步骤(3)得到的黑色产物用去离子水和无水乙醇交替进行真空抽滤6~8次,将固体产物置于60~70摄氏度的恒温干燥箱中干燥3~4小时,再次用无水乙醇进行抽滤,再干燥12~24小时;
(5)取步骤(4)干燥后的碳球,研磨备用,将0.12克氢氧化钠溶于60毫升去离子水,磁力搅拌5~10分钟得到氢氧化钠溶液,用电子天平称取2~3克碳球溶于氢氧化钠溶液,静置碱化5~6小时,用去离子水对碱化碳球抽滤3至4次,置于60~70摄氏度的恒温干燥箱中12~24小时;
(6)称取25克~30克五水四氯化锡晶体溶于20毫升去离子水和20毫升无水乙醇的混合溶液,磁力搅拌至晶体完全溶解,称取步骤(5)得到的样品1克,置于四氯化锡溶液中超声分散20分钟,随后放置于磁力搅拌器搅拌5小时,样品用去离子水真空抽滤3至4次,置于60~70摄氏度的恒温干燥箱中12~24小时;
(7)取步骤(6)的黑色产物研磨均匀,分散至石英舟置于马弗炉中煅烧,在空气气氛中以每分钟1摄氏度的升温速率升温至500摄氏度,保温2小时,自然冷却至室温;
(8)取3~4克乙基纤维素缓慢加入20毫升无水乙醇中,磁力搅拌30~40小时;
(9)取0.1~0.2克步骤(8)溶胀后的乙基纤维素、0.3克松油醇、步骤(7)得到的SnO2白色粉末,1毫升乙酸,1毫升乙醇置于大小合适的研钵中研磨1小时,用250目~350目的丝网印刷板将浆料刮涂在Si片上,刮涂2至3次,每次刮涂之间将样品置于60~70摄氏度干燥箱中干燥10分钟;
(10)步骤(9)的样品置于马弗炉煅烧,以每分钟2摄氏度的升温速率升至450摄氏度,450摄氏度下保温2小时,冷却至室温;
(11)将步骤(10)得到的样品放入磁控溅射仪的溅射室,在氩气环境下,采用直流磁控溅射技术,通过电离出的氩离子轰击SnSe靶材,在SnO2多壳球层结构薄膜层表面溅射SnSe薄膜,所用SnSe靶材纯度为99.9%,背景真空为5×10-4帕斯卡,氩气气氛维持1.0帕斯卡,溅射功率为10瓦,靶基距为50毫米,薄膜的沉积温度为450摄氏度,所有样品溅射完成后在450摄氏度下退火30分钟,随后冷却至室温;
(12)将步骤(11)得到的样品取出,并在SnSe薄膜层表面覆盖正方形掩膜片,将样品放入磁控溅射仪的溅射室;选取直流磁控溅射技术,利用电离出的氩离子轰击金属Pd靶材,在SnSe薄膜层表面沉积金属Pd前电极;所用靶材为金属Pd靶,靶材纯度为99.9%;氩气气压维持5.0帕斯卡,靶基距为50毫米,Pd电极的沉积温度为室温,金属Pd前电极厚度为5~15纳米;
(13)在pd前电极滴涂导电银胶,在Si基底面涂覆In电极,并引出金属Cu导线,完成器件的制备。
下面结合性能测量结果进一步说明本发明的效果:
图1为所制备器件光电探测性能测量的结构示意图。
图2为所制备器件的对数伏安特性曲线,结果表明器件具有半导体特性以及光伏效应。
图3为所制备器件在无外加偏压时器件对不同光功率密度光的响应性能,结果表明,在无外加偏压时,器件表现出稳定性,并且光电流随光功率密度的增大而增大,说明该器件的自驱动性能优异。
图4为所制备器件在无外加偏压时在不同波长单色光照射下对应的响应度(R)、灵敏度(S)、探测度(D*),结果表明,器件在波长从紫外到近红外范围的光的照射下都具有光响应,说明该器件可以进行宽光带光探测。
Claims (8)
1.一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器,特征在于:包括导电银胶点电极、金属Pd前电极、SnSe纳米薄膜层、SnO2多层球壳结构薄膜层、Si单晶基底和金属In背电极。
2.根据权利要求1所述的自驱动光电探测器,SnO2多层球壳结构薄膜层置于Si基底表面,SnSe纳米薄膜层置于SnO2多层球壳薄膜层表面,金属Pd前电极在SnSe纳米薄膜层表面,导电银胶点电极滴涂于Pd前电极表面,金属In电极压制于Si基底表面。
3.根据权利要求1-2任一所述的自驱动光电探测器,其特征在于:所述Si基底为n型Si单晶基底,尺寸为10毫米×10毫米,电阻率为0.1~1欧姆·厘米。
4.根据权利要求1-3任一所述的自驱动光电探测器,其特征在于:SnSe薄膜层的厚度为50~100纳米,SnO2多层球壳结构薄膜层的厚度为1~2微米,Si层的厚度为0.5~2毫米。
5.一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器的制备方法,其特征在于包括以下步骤:
(1)切出所需大小Si片,分别用离子水、丙酮、无水乙醇依次清洗,去除表面污染物;
(2)对清洗完成后的Si基底进行干燥;
(3)将10.27克蔗糖溶解于60毫升去离子水中,磁力搅拌5~10分钟至蔗糖溶解,把蔗糖溶液倒入100毫升聚四氟乙烯反应釜内衬中进行水热反应,在180~200摄氏度下反应4~6小时,自然冷却至室温;
(4)将步骤(3)得到的黑色产物用去离子水和无水乙醇交替进行真空抽滤6~8次,将固体产物置于60~70摄氏度的恒温干燥箱中干燥3~4小时,再次用无水乙醇进行抽滤,再干燥12~24小时;
(5)取步骤(4)干燥后的碳球,研磨备用,将0.12克氢氧化钠溶于60毫升去离子水,磁力搅拌5~10分钟得到氢氧化钠溶液,用电子天平称取2~3克碳球溶于氢氧化钠溶液,静置碱化5~6小时,用去离子水对碱化碳球抽滤3至4次,置于60~70摄氏度的恒温干燥箱中12~24小时;
(6)称取25克~30克五水四氯化锡晶体溶于20毫升去离子水和20毫升无水乙醇的混合溶液,磁力搅拌至晶体完全溶解,称取步骤(5)得到的样品1克,置于四氯化锡溶液中超声分散20分钟,随后放置于磁力搅拌器搅拌5小时,样品用去离子水真空抽滤3至4次,置于60~70摄氏度的恒温干燥箱中12~24小时;
(7)取步骤(6)的黑色产物研磨均匀,分散至石英舟置于马弗炉中煅烧,在空气气氛中以每分钟1摄氏度的升温速率升温至500摄氏度,保温2小时,自然冷却至室温;
(8)取3~4克乙基纤维素缓慢加入20毫升无水乙醇中,磁力搅拌30~40小时;
(9)取0.1~0.2克步骤(8)溶胀后的乙基纤维素、0.3克松油醇、步骤(7)得到的SnO2白色粉末,1毫升乙酸,1毫升乙醇置于大小合适的研钵中研磨1小时,用250目~350目的丝网印刷板将浆料刮涂在Si片上,刮涂2至3次,每次刮涂之间将样品置于60~70摄氏度干燥箱中干燥10分钟;
(10)取步骤(9)的样品置于马弗炉煅烧,以每分钟2摄氏度的升温速率升至450摄氏度,450摄氏度下保温2小时,冷却至室温;
(11)将步骤(10)得到的样品放入磁控溅射仪的溅射室,在氩气环境下,采用直流磁控溅射技术,通过电离出的氩离子轰击SnSe靶材,在SnO2多壳球层结构薄膜层表面溅射SnSe薄膜,所用SnSe靶材纯度为99.9%,背景真空为5×10-4帕斯卡,氩气气氛维持1.0帕斯卡,溅射功率为10瓦,靶基距为50毫米,薄膜的沉积温度为450摄氏度,所有样品溅射完成后在450摄氏度下退火30分钟,随后冷却至室温;
(12)将步骤(11)得到的样品取出,并在SnSe薄膜层表面覆盖正方形掩膜片,将样品放入磁控溅射仪的溅射室;选取直流磁控溅射技术,利用电离出的氩离子轰击金属Pd靶材,在SnSe薄膜层表面沉积金属Pd前电极;所用靶材为金属Pd靶,靶材纯度为99.9%;氩气气压维持5.0帕斯卡,靶基距为50毫米,Pd电极的沉积温度为室温,金属Pd前电极厚度为5~15纳米;
(13)在pd前电极滴涂导电银胶,在Si基底面涂覆In电极,并引出金属Cu导线,完成器件的制备。
6.一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器,其特征在于:所述光电探测器件在无外加偏压下,对波长从紫外到近红外范围的光的照射都具有光响应。
7.根据权利要求5所述的一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器的制备方法,其特征在于:步骤(12)中,所述掩模片为不锈钢材质,厚度为0.1毫米,尺寸为12毫米×12毫米,孔径尺寸为5毫米×5毫米。
8.根据权利要求5所述的一种基于SnSe/SnO2多层球壳/Si异质结的自驱动光电探测器的制备方法,其特征在于:步骤(13)中,所述金属In电极所用原料In的纯度为99.5%,金属Pd前电极上金属In电极大小和厚度分别为1毫米×1.5毫米和1毫米,Si基底上金属In电极大小和厚度均分别为10毫米×10毫米和2毫米,Cu导线直径为0.1毫米。
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