CN113745361A - 一种多孔GaN窄带紫外光电二极管及其制备方法 - Google Patents
一种多孔GaN窄带紫外光电二极管及其制备方法 Download PDFInfo
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Abstract
本发明提供一种多孔GaN窄带紫外光电二极管及其制备方法,包括衬底层;设置于衬底层上的半导体层,设置于半导体层上表面的多孔GaN层和CuZnS层;分别设置于多孔GaN层和CuZnS层上表面的金属触点层。本发明通过在衬底层上沉积GaN薄膜;对GaN薄膜进行清洗,并用离子液刻蚀GaN薄膜一部分,形成多孔GaN层;将GaN薄膜另一部分用水浴法在表面制得CuZnS层。本发明利用多孔GaN材料作为紫外光吸收层,改善光吸收降低材料缺陷;本发明利用的P型透明、高导电薄膜CuZnS具备了ZnS的高透过率和CuS的高导电特性;多孔GaN窄带紫外光电二极管半峰宽仅5nm,紫外响应波段为362~380nm,并具有高探测率,适用于弱光窄带光谱检测。
Description
技术领域
本发明涉及光电二极管技术领域,尤其是一种多孔GaN窄带紫外光电二极管及其制备方法。
技术背景
在军事应用领域,利用紫外探测技术可实现短距离的保密通讯、低误警率的导弹预警等;在民事领域,利用紫外探测技术可实现环境监测、火焰探测等。目前,较为成熟的紫外探测器件主要包括硅基紫外探测器和光电倍增管等。光电倍增管灵敏度高,但真空器件体积大,而且需要高压工作;硅基紫外光电探测器则需附带滤光片。因此,它们在工作中都存在一定的局限性。宽禁带半导体紫外探测器体积小、无须滤光片、节能而无需高压工作,成为目前研究热点。其中宽禁带GaN基紫外探测器耐高温、抗辐照,具有显著应用优势。
虽然国内外研究单位已经先后加入GaN基紫外探测器的研发,也取得了一定的研究进展,但是目前器件性能仍不够理想,无法全面取代现有主流的光电倍增管以及Si探测器。受材料自身性质、生长设备、衬底、p型掺杂等问题的影响,材料质量和器件结构都存在较多问题。
制备多孔GaN,形成纳米尺度的多孔结构可以有效的降低缺陷密度,减小由晶格失配所导致的应力。专利CN108520911A公开了一种具有纳米多孔GaN分布布拉格反射镜的InGaN基蓝光发光二极管的制备方法,并具体公开了如下技术内容:该方法首先采用电化学刻蚀法,以生长在c-面蓝宝石衬底层上的GaN/n-GaN周期性结构为阳极,以Pt丝为阴极,在硝酸、草酸或氢氟酸酸性溶液中刻蚀制备纳米多孔GaN分布布拉格反射镜;然后,采用MOCVD方法在纳米多孔GaN分布布拉格反射镜上外延生长InGaN基蓝光LED。所得InGaN基蓝光LED表面光滑平整,发光强度和荧光寿命分别是参比LED的5-8倍和3-5倍。所制备的具有纳米多孔GaN分布布拉格反射镜的InGaN基蓝光LED可用于照明、平面显示、生物医学器件等应用领域。此外,多孔GaN具有比表面积大、能量吸收好、紫外反射率低等特性,这些优良特性使得多孔GaN非常适用于紫外光电探测器。专利CN201710220056.1报道了一种基于多孔DBR的InGaN基谐振腔增强型探测器芯片。包括:一衬底;形成于衬底上的缓冲层;形成于缓冲层上的底部多孔DBR层;形成于底部多孔DBR层上的n型GaN层,n型GaN层的一侧向下形成有台面,另一侧为凸起;形成于n型GaN层上的有源区;形成于有源区上的p型GaN层;一侧壁钝化层,形成于所述p型GaN层部分的上表面及凸起的n型GaN层、有源区和p型GaN层的侧壁,该p型GaN层上表面的侧壁钝化层中间有一窗口;形成于侧壁钝化层及其窗口处p型GaN层上的透明导电层;形成于n型GaN层的台面上的n电极;制作在侧壁钝化层上表面周围的p电极;形成于透明导电层及p电极上的顶部介质DBR层。
以上报道均采用多孔GaN层作为DBR层,采用多孔GaN作为有源层的异质结高性能窄带响应紫外探测器未见报道。
发明内容
针对现有技术的空缺,本发明提供一种多孔GaN窄带紫外光电二极管及其制备方法,该紫外光电二极管具有窄带响应和高探测率的特点。
本发明的技术方案为:一种多孔GaN窄带紫外光电二极管,
包括衬底层;
半导体层,设置于衬底层的上表面,所述半导体层为GaN薄膜层;
多孔GaN层,相对设置于所述半导体层的上表面;
CuZnS层,设置于所述的半导体层的上表面;
金属触点层,分别设置于所述多孔GaN层和CuZnS层的上表面。
作为优选的,所述的衬底层为蓝宝石衬底层。
作为优选的,所述的半导体层的GaN薄膜层在室温下的载流子浓度范围为1×1015至1×1018cm-3,厚度为4-6μm。
作为优选的,所述的CuZnS层的厚度为30-100nm。
作为优选的,所述的金属触点层为欧姆接触层,所述的欧姆接触层的厚度为50-200nm。
本发明还提供一种多孔GaN窄带紫外光电二极管的制备方法,所述的方法包括:
S1)、在衬底层上沉积GaN薄膜;
S2)、对步骤S1)制备的GaN薄膜进行清洗,并用离子液刻蚀GaN薄膜一部分,形成多孔GaN层;
S3)、将GaN薄膜另一部分用水浴法在表面制得CuZnS层。
作为优选的,所述的步骤S2)中在刻蚀多孔GaN层之前,将0.2-0.5cm2的GaN放在王水中除去表面的钝化层;然后依次用丙酮、乙醇和去离子水中对GaN片进行超声清洗;随后在紫外臭氧清洗机中对GaN片进行亲水处理,用来增强GaN片和刻蚀剂的接触,亲水处理时间为10-30min。
作为优选的,步骤S2)中所用的离子液体为:1-乙基-3-甲基咪唑三氟甲磺酸盐或1-乙基-3-甲基咪唑三氟乙酸盐。
作为优选的,步骤S2)中多孔GaN层的具体制备方法为:
S201)、使用InGa合金作为电极,使电极与GaN片形成欧姆接触;
S202)、GaN片与电源正极相连,同样铂片与负极相连,将两个电极平行放置且固定好在铁架台,放置于氙灯前约10-30cm处,GaN刻蚀面朝向氙灯;
S203)、把GaN片与铂片浸泡在装好离子液的烧杯中,直流电源电压设为10-25V,刻蚀时长为5-20min。
作为优选的,步骤S3)中CuZnS层的具体制备方法为:
S301)、配制三种前驱体溶液,
溶液A:0.03g-0.12g硫酸铜和1-2g醋酸锌在100-200ml去离子水中混合;
溶液B:0.5-1g乙二胺四乙酸二钠与100ml的去离子混合溶解;
溶液C:0.5-1g的C2H5NS与50-200ml的去离子水混合溶解;
S302)、然后将溶液B与溶液A混合并超声20-40min;
S303)、随后将亲水处理的GaN基底垂直浸入混合溶液中,立即将溶液C加入到混合物中;密封好烧杯,对其加热,保持温度为75-90℃,时间50-80min。
本发明的有益效果为:
1、本发明利用多孔GaN材料作为紫外光吸收层,改善光吸收降低材料缺陷;
2、本发明所利用的P型透明、高导电薄膜CuZnS具备了ZnS的高透过率和CuS的高导电特性;
3、本发明的多孔GaN窄带紫外光电二极管响应带宽仅10nm,并具有高探测率,特别适用于弱光窄带光谱检测的应用。
附图说明
图1为本发明多孔GaN窄带响应紫外光电二极管的结构示意图;
图2为本发明窄多孔GaN带响应紫外光电二极管的多孔GaN层的扫描电镜图;
图3为本发明多孔GaN窄带响应紫外光电二极管在暗态和紫外光(370nm)照射下的电流-电压曲线图;
图4为本发明多孔GaN窄带响应紫外光电二极管在-2V偏压下的外量子效率和响应度图;
图5为本发明多孔GaN窄带响应紫外光电二极管的比探测率;
图中,100-衬底层,200-半导体层,300-多孔GaN层,400-CuZnS层,500-金属触点层。
具体实施方式
下面结合附图对本发明的具体实施方式作进一步说明:
实施例1
如图1和2所示,本实施例提供一种多孔GaN窄带紫外光电二极管,包括衬底层100、半导体层200、多孔GaN层300、CuZnS层400、金属触点层500,本实施例中,所述的衬底层100为蓝宝石衬底层,且所述的半导体层200设置于衬底层100的上表面,本实施例中所述半导体层200为GaN薄膜层;且所述的GaN薄膜层在室温下的载流子浓度范围为1×1015至1×1018cm-3,厚度为4-6μm。所述的半导体层200设置有多孔GaN层300和CuZnS层400,而所述多孔GaN层300和CuZnS层400的上表面设有金属触点层500。本实施例中所述的CuZnS层400的厚度为30-100nm。所述的金属触点层500为欧姆接触层,所述的欧姆接触层的厚度为50-200nm。
实施例2
本实施例提供一种多孔GaN窄带紫外光电二极管的制备方法,所述的方法包括:
S1)、在衬底层100上沉积GaN薄膜,其中,沉积的GaN薄膜厚度为5000nm;
S2)、对步骤S1)制备的GaN薄膜进行清洗,并用离子液刻蚀GaN薄膜一部分,形成多孔GaN层300;
S3)、将GaN薄膜另一部分用水浴法在表面制得CuZnS层400,其中Cu组分为20%。
作为本实施例优选的,步骤S2)中,在刻蚀多孔GaN层300之前,将1.0cm×0.3cm的GaN放在王水中除去表面的钝化层,五分钟后取出;然后依次用丙酮、乙醇和去离子水中对GaN片进行超声清洗,每次30分钟;随后在紫外臭氧清洗机中对GaN片进行亲水处理,用来增强GaN片和刻蚀剂的接触,亲水处理时间为30min;
作为本实施例优选的,步骤S2)中,所用的离子液体为:1-乙基-3-甲基咪唑三氟甲磺酸盐。
作为本实施例优选的,步骤S2)中,多孔GaN层300的具体制备方法为:使用InGa合金作为电极,使电极与GaN片形成欧姆接触;GaN片与电源正极相连,同样铂片与负极相连,将两个电极平行放置且固定好在铁架台,放置于300W氙灯前约10cm处,GaN刻蚀面朝向氙灯;把GaN片与铂片浸泡在装好离子液的烧杯中,直流电源电压设为10V,刻蚀时长为5min;
作为本实施例优选的,步骤S3)中,所述的CuZnS层400的具体制备方法为:首先配制三种前驱体溶液:
溶液A:0.06g硫酸铜和1.68g醋酸锌在100ml去离子水中混合;溶液B:0.96g乙二胺四乙酸二钠与100ml的去离子混合溶解;溶液C:0.6g的C2H5NS与100ml的去离子水混合溶解;
然后将溶液B与溶液A混合并超声30min;随后将亲水处理的GaN基底垂直浸入混合溶液中,立即将溶液C加入到混合物中;密封好烧杯,对其加热,保持温度为80℃,时间60min。
实施例3
本实施例提供一种多孔GaN窄带紫外光电二极管的制备方法,所述的方法包括:
S1)、在衬底层100上沉积GaN薄膜,其中,沉积的GaN薄膜厚度为5000nm;
S2)、对步骤S1)制备的GaN薄膜进行清洗,并用离子液刻蚀GaN薄膜一部分,形成多孔GaN层300;
S3)、将GaN薄膜另一部分用水浴法在表面制得CuZnS层400,其中Cu组分为10%。
作为本实施例优选的,步骤S2)中,在刻蚀多孔GaN层300之前,将1.0cm×0.3cm的GaN放在王水中除去表面的钝化层,五分钟后取出;然后依次用丙酮、乙醇和去离子水中对GaN片进行超声清洗,每次30分钟;随后在紫外臭氧清洗机中对GaN片进行亲水处理,用来增强GaN片和刻蚀剂的接触,亲水处理时间为30min;
作为本实施例优选的,步骤S2)中,所用的离子液体为:1-乙基-3-甲基咪唑三氟甲磺酸盐。
作为本实施例优选的,步骤S2)中,多孔GaN层300的具体制备方法为:使用InGa合金作为电极,使电极与GaN片形成欧姆接触;GaN片与电源正极相连,同样铂片与负极相连,将两个电极平行放置且固定好在铁架台,放置于300W氙灯前约10cm处,GaN刻蚀面朝向氙灯;把GaN片与铂片浸泡在装好离子液的烧杯中,直流电源电压设为10V,刻蚀时长为5min;
作为本实施例优选的,步骤S3)中,CuZnS层400的具体制备方法为:首先配制三种前驱体溶液,
溶液A:0.06g硫酸铜和3.36g醋酸锌在200ml去离子水中混合;溶液B:1.92g乙二胺四乙酸二钠与100ml的去离子混合溶解;溶液C:1.2g的C2H5NS与100ml的去离子水混合溶解;
然后将溶液B与溶液A混合并超声30min;随后将亲水处理的GaN基底垂直浸入混合溶液中,立即将溶液C加入到混合物中;密封好烧杯,对其加热,保持温度为80℃,时间60min。
实施例4
本实施例提供一种多孔GaN窄带紫外光电二极管的制备方法,所述的方法包括:
S1)、在衬底层100上沉积GaN薄膜,其中,沉积的GaN薄膜厚度为5000nm;
S2)、对步骤S1)制备的GaN薄膜进行清洗,并用离子液刻蚀GaN薄膜一部分,形成多孔GaN层300;
S3)、将GaN薄膜另一部分用水浴法在表面制得CuZnS层400,其中Cu组分为20%。
作为本实施例优选的,步骤S2)中,在刻蚀多孔GaN层300之前,将1.0cm×0.3cm的GaN放在王水中除去表面的钝化层,五分钟后取出;然后依次用丙酮、乙醇和去离子水中对GaN片进行超声清洗,每次30分钟;随后在紫外臭氧清洗机中对GaN片进行亲水处理,用来增强GaN片和刻蚀剂的接触,亲水处理时间为30min;
作为本实施例优选的,步骤S2)中,所用的离子液体为:1-乙基-3-甲基咪唑三氟甲磺酸盐。
作为本实施例优选的,步骤S2)中,多孔GaN层300的具体制备方法为:使用InGa合金作为电极,使电极与GaN片形成欧姆接触;GaN片与电源正极相连,同样铂片与负极相连,将两个电极平行放置且固定好在铁架台,放置于300W氙灯前约10cm处,GaN刻蚀面朝向氙灯;把GaN片与铂片浸泡在装好离子液的烧杯中,直流电源电压设为15V,刻蚀时长为5min;
作为本实施例优选的,步骤S3)中,CuZnS层400的具体制备方法为:首先配制三种前驱体溶液,
溶液A:0.12g硫酸铜和3.36g醋酸锌在200ml去离子水中混合;
溶液B:1.92g乙二胺四乙酸二钠与100ml的去离子混合溶解;
溶液C:1.2g的C2H5NS与100ml的去离子水混合溶解;
然后将溶液B与溶液A混合并超声30min;随后将亲水处理的GaN基底垂直浸入混合溶液中,立即将溶液C加入到混合物中;密封好烧杯,对其加热,保持温度为80℃,时间60min。
实施例5
本实施例对实施例1制得的多孔GaN窄带紫外光电二极管进行性能测试,测试在暗处以及370nm紫外光照射下紫外光电二极管的光暗电流比以及其他参数,由图3-5可知,该紫外光电二极管在370nm紫外光照射下器件光暗电流比达到585;在-2V偏压下,制备的光电探测器峰值响应度为41.7mA/W,峰值外量子效率为13.86%,探测率值超过了3.78×1012Jones。
由图可知,制备的多孔GaN窄带紫外光电二极管外量子效率、响应度和探测率均在紫外区370nm处取得峰值,半峰宽为5nm,且只在362~388nm紫外波段产生响应,表明制得的器件具有窄带响应性能。
上述实施例和说明书中描述的只是说明本发明的原理和最佳实施例,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。
Claims (10)
1.一种多孔GaN窄带紫外光电二极管,其特征在于,包括衬底层(100)、半导体层(200)、多孔GaN层(300)、CuZnS层(400)、金属触点层(500),所述的半导体层(200)设置于衬底层(100)的上表面,所述半导体层(200)为GaN薄膜层;
所述的半导体层(200)上设置有多孔GaN层(300)和CuZnS层(400),而所述多孔GaN层(300)和CuZnS层(400)的上表面设有金属触点层(500)。
2.根据权利要求1所述的一种多孔GaN窄带紫外光电二极管,其特征在于:所述的衬底层100为蓝宝石衬底层。
3.根据权利要求1所述的一种多孔GaN窄带紫外光电二极管,其特征在于:所述的GaN薄膜层在室温下的载流子浓度范围为1×1015至1×1018cm-3,厚度为4-6μm。
4.根据权利要求1所述的一种多孔GaN窄带紫外光电二极管,其特征在于:所述的CuZnS层400的厚度为30-100nm。
5.根据权利要求1所述的一种多孔GaN窄带紫外光电二极管,其特征在于:所述的金属触点层500为欧姆接触层,所述的欧姆接触层的厚度为50-200nm。
6.一种用于制备权利要求1-5任一项所述的多孔GaN窄带紫外光电二极管的方法,所述的方法包括:
S1)、在衬底层(100)上沉积GaN薄膜;
S2)、对步骤S1)制备的GaN薄膜进行清洗,并用离子液刻蚀GaN薄膜一部分,形成多孔GaN层(300);
S3)、将GaN薄膜另一部分用水浴法在表面制得CuZnS层(400)。
7.根据权利要求6所示的一种多孔GaN窄带紫外光电二极管的制备方法,其特征在于,所述的步骤S2)中在刻蚀多孔GaN层(300)之前,将0.2-0.5cm2的GaN放在王水中除去表面的钝化层;
然后依次用丙酮、乙醇和去离子水中对GaN片进行超声清洗;
随后在紫外臭氧清洗机中对GaN片进行亲水处理,用来增强GaN片和刻蚀剂的接触,亲水处理时间为10-30min。
8.根据权利要求6所示的一种多孔GaN窄带紫外光电二极管的制备方法,其特征在于,步骤S2)中所用的离子液体为:1-乙基-3-甲基咪唑三氟甲磺酸盐或1-乙基-3-甲基咪唑三氟乙酸盐。
9.根据权利要求6所示的一种多孔GaN窄带紫外光电二极管的制备方法,其特征在于,步骤S2)中多孔GaN层(300)的具体制备方法为:
S201)、使用InGa合金作为电极,使电极与GaN片形成欧姆接触;
S202)、GaN片与电源正极相连,同样铂片与负极相连,将两个电极平行放置且固定好在铁架台,放置于氙灯前约10-30cm处,GaN刻蚀面朝向氙灯;
S203)、把GaN片与铂片浸泡在装好离子液的烧杯中,直流电源电压设为10-25V,刻蚀时长为5-20min。
10.根据权利要求6所示的一种多孔GaN窄带紫外光电二极管的制备方法,其特征在于,步骤S3)中CuZnS层(400)的具体制备方法为:
S301)、配制三种前驱体溶液
溶液A:0.03g-0.12g硫酸铜和1-2g醋酸锌在100-200ml去离子水中混合;
溶液B:0.5-1g乙二胺四乙酸二钠与100ml的去离子混合溶解;
溶液C:0.5-1g的C2H5NS与50-200ml的去离子水混合溶解;
S302)、然后将溶液B与溶液A混合并超声20-40min;
S303)、随后将亲水处理的GaN基底垂直浸入混合溶液中,立即将溶液C加入到混合物中;密封好烧杯,对其加热,保持温度为75-90℃,时间50-80min。
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