CN111816716A - 一种高效光电探测性能的核壳异质结阵列电极制备方法 - Google Patents
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Abstract
本发明属于纳米光电子材料技术领域,公开了一种高效光电探测性能的核壳异质结阵列电极制备方法。本发明采用上下层垂直异质结结构生长策略,通过改变基底膜层的生产工艺,可控制备出ZnO/PdSe2异质结结构。具有制备工艺简单,产物结构稳定,光电性能好等优势。克服了传统制备方法中的产物结构设计难度,制备工艺不可控,光电流密度小,光电转换效率低等问题。本发明具有重要的工程实用意义,在军工、航天、能源及光电子等领域具有广阔的应用前景。
Description
技术领域
本发明涉及一种高效光电探测性能的核壳异质结阵列电极制备方法,属于纳米光电子材料技术领域。
背景技术
光电检测技术在军工,工业,航天,电子,能源等领域有着重要的应用前景。根据工作机理的不同,光电探测器可分为光子探测器和导热探测器两种类型。其中,光电化学(PEC)式探测器被认为是光电检测器中最重要的应用之一。同时,PEC分解水也是将太阳能转化为化学燃料的一种有前景策略。另外,PEC光电探测器由于反应条件温和、制备工艺简单、光电流密度大、高灵敏度、超快响应和高可靠性等优点引起了学术界极大关注。其中,类石墨烯的二维层状过渡金属二硫属化合物MX2(M为Pt、Pd、Mo、W等过渡金属;X为S、Se、Te等硫属元素),如MoS2、WS2、PtSe2和PdSe2等,是光电探测领域不可缺少的材料之一,成为当今研究的热点。其中,第Viii族过渡金属硫属化合物如层状的PtSe2或PdSe2,即典型的窄带隙半导体材料。PtSe2单层和多层带隙分别对应1.2eV和0.21eV,且随着层数增加,PtSe2逐渐变为带隙为零的半金属,具有探测范围广、载流子迁移率高、催化活性位点多的析氢性能等优势,因此研究的意义十分重大。然而,该电极材料存在制备工艺难度大,大面积合成难,目前多处于理论研究,实验较难展开。紫外探测的最佳电极材料ZnO,一种典型宽带隙半导体材料,具有价格便宜、制备简单及载流子迁移率高等优势。但是ZnO(Eg约等于3.2eV)带隙较宽,仅适用紫外探测性能方面,对于可见光及近红外探测响应很弱,几乎无响应,因此如何利用带隙可调、材料掺杂等方法设计异质结或肖特基结构,将有效加快异质结材料本身的电子空穴对的分离,缩短少数载流子的扩散路径,降低复合率,提高器件光电转换效率,有利于增强光吸收,最大范围内实现紫外-可见-近红外探测。
发明内容
本发明是为避免上述现有技术所存在的不足之处,提供一种高效光电探测性能的核壳异质结阵列电极制备方法,旨在解决现有纯ZnO可见光光电流密度小,光电转换效率低等问题,同时提高该异质结材料在可见及近红外探测性能。
本发明解决技术问题采用如下技术方案:
一种高效光电探测性能的核壳异质结阵列电极制备方法,包括如下步骤:
a、配置好0.1-0.5mmol/L醋酸锌溶液,使用滴管取3-5滴醋酸锌溶液放到清洗干净的FTO玻璃上,将FTO玻璃基底置于溶胶机上吸盘固定,先慢速旋涂10-50s,再快速旋涂10-50s,随后于300-400℃下退火10-60分钟,最后将其放入浓度为0.05mol/L Zn(NO3)2和0.05mol/L的乌洛托品溶液中,水浴反应3-6小时,温度设定90℃,连续更换反应液3-5次,得初始产物ZnO;
b、将初始产物ZnO作为基底生长材料,使用氩气作为保护气,利用电子束蒸发方法蒸镀1-10nm Pd膜,待镀膜结束后,取出,得到产物ZnO/Pd;
c、将ZnO/Pd作为基底材料,通过化学气相沉积(CVD)方法,将产物ZnO/Pd置于高温区,温度设定为400℃,硒粉置于低温区,温度设定为250℃,硒化时间设定为1-2小时,待硒化反应结束后,取出,得到目标产物ZnO/PdSe2;
d、将所得目标产物ZnO/PdSe2作为光电化学测试系统的工作电极,光源采用的是太阳光模拟光源,波长范围为400-800nm,测试其光电流,暗电流,最终比较电极之间的光电性能。
作为本发明的进一步改进,所述步骤b中Pd膜为1nm;
作为本发明的进一步改进,所述步骤b中Pd膜为10nm;
与已有技术相比,本发明的有益效果体现在:
1.本发明提供了一种高效光电探测性能的核壳异质结阵列电极制备方法,采用自上而下的设计方案,制备出ZnO/PdSe2异质结,结构新颖;
2.本发明的制备工艺简单、反应条件温和,成本低廉;
3.本发明的最终产物有望批量生产;
4.本发明制备的核壳异质结纳米线阵列在光电探测方面有着较好的应用,尤其适用于可见光探测器的工作电极材料。在低偏压下,相比较纯ZnO电极材料,ZnO/PdSe2核壳异质结纳米线阵列电极具有较高的光电流密度及光转换效率。
附图说明
图1(a)为本发明实施例1样品制备工艺流程图;
图1(b-c)为本发明实施例1样品的扫描电子显微镜图(SEM);
图2为本发明实施例1和2样品的X-射线衍射谱图;
图3(a)为本发明实施例1和2样品Zn 2p的X-射线光电子能谱谱图;
图3(b)为本发明实施例1和2样品O1s的X-射线光电子能谱谱图;
图3(c)为本发明实施例1和2样品Pd 3d的X-射线光电子能谱谱图;
图3(d)为本发明实施例1和2样品Se 3d的X-射线光电子能谱谱图;
图4为本发明实施例1和2样品的拉曼光谱图;
图5(a)为本发明实施例1样品在偏压为0.8V下的光电流和暗电流图;
图5(b)为本发明实施例1样品短时间(400s)的光电响应图。
具体实施方式
下面结合具体实施例和附图对本发明做进一步说明,而不限制于本发明的范围。
a、配置好0.1-0.5mmol/L醋酸锌溶液,使用滴管取3-5滴醋酸锌溶液放到清洗干净的FTO玻璃上,将FTO玻璃基底置于溶胶机上吸盘固定,先慢速旋涂10-50s,再快速旋涂10-50s,随后于300-400℃下退火10-60分钟,最后将其放入浓度为0.05mol/L Zn(NO3)2和0.05mol/L的乌洛托品溶液中,水浴反应3-6小时,温度设定90℃,连续更换反应液3-5次,得初始产物ZnO;
b、将初始产物ZnO作为基底生长材料,使用氩气作为保护气,利用电子束蒸发方法蒸镀1-10nm Pd膜,待镀膜结束后,取出,得到产物ZnO/Pd;
c、将ZnO/Pd作为基底材料,通过化学气相沉积(CVD)方法,将产物ZnO/Pd置于高温区,温度设定为400℃,硒粉置于低温区,温度设定为250℃,硒化时间设定为1-2小时,待硒化反应结束后,取出,得到目标产物ZnO/PdSe2;
d、将所得目标产物ZnO/PdSe2作为光电化学测试系统的工作电极,光源采用的是太阳光模拟光源(400-800nm),测试其光电流,暗电流,最终比较电极之间的光电性能。
作为本发明的进一步改进,所述步骤b中Pd膜为1nm;
作为本发明的进一步改进,所述步骤b中Pd膜为10nm;
实施例1
本实施例按如下步骤制备ZnO/PdSe2核壳纳米线阵列:
a、配置好0.1-0.5mmol/L醋酸锌溶液,使用滴管取3-5滴醋酸锌溶液放到清洗干净的FTO玻璃上,将FTO玻璃基底置于溶胶机上吸盘固定,先慢速旋涂10-50s,再快速旋涂10-50s,随后于300-400℃下退火10-60分钟,最后将其放入浓度为0.05mol/L Zn(NO3)2和0.05mol/L的乌洛托品溶液中,水浴反应3-6小时,温度设定90℃,连续更换反应液3-5次,得初始产物ZnO;
b、将初始产物ZnO作为基底生长材料,使用氩气作为保护气,利用电子束蒸发方法蒸镀1nm Pd膜,待镀膜结束后,取出,得到产物ZnO/Pd;
c、将ZnO/Pd作为基底材料,通过化学气相沉积(CVD)方法,将产物ZnO/Pd置于高温区,温度设定为400℃,硒粉置于低温区,温度设定为250℃,硒化时间设定为1-2小时,待硒化反应结束后,取出,得到目标产物ZnO/PdSe2;
d、将所得目标产物ZnO/PdSe2作为光电化学测试系统的工作电极,光源采用的是太阳光模拟光源(400-800nm),测试其光电性能。
实施例2
本实施例按如下步骤制备PdSe2/ZnO核壳异质结:
a、配置好0.1-0.5mmol/L醋酸锌溶液,使用滴管取3-5滴醋酸锌溶液放到清洗干净的FTO玻璃上,将FTO玻璃基底置于溶胶机上吸盘固定,先慢速旋涂10-50s,再快速旋涂10-50s,随后于300-400℃下退火10-60分钟,最后将其放入浓度为0.05mol/L Zn(NO3)2和0.05mol/L的乌洛托品溶液中,水浴反应3-6小时,温度设定90℃,连续更换反应液3-5次,得初始产物ZnO;
b、将初始产物ZnO作为基底生长材料,使用氩气作为保护气,利用电子束蒸发方法蒸镀10nm Pd膜,待镀膜结束后,取出,得到产物ZnO/Pd;
c、将ZnO/Pd作为基底材料,通过化学气相沉积(CVD)方法,将产物ZnO/Pd置于高温区,温度设定为400℃,硒粉置于低温区,温度设定为250℃,硒化时间设定为1-2小时,待硒化反应结束后,取出,得到目标产物ZnO/PdSe2;
d、将所得目标产物ZnO/PdSe2作为光电化学测试系统的工作电极,光源采用的是太阳光模拟光源(400-800nm),测试其光电流,暗电流,最终比较电极之间的光电性能。
对比实施例1和2可知,区别在于电子束蒸发方法蒸镀的Pd膜层厚度。
图1为实施例1和2所得样品的形成机理图及扫描电子显微镜图。图a是制备工艺的流程图,首先制备ZnO种子层,经垂直导向作用生长纳米线阵列,再利用镀膜及化学气相沉积法,最终形成ZnO/PdSe2核壳异质结结构。其中,ZnO/PdSe2核壳形成过程,主要通过化学气相反应沉积法实现。在N2保护气下,Se蒸汽沉积在Pd表面,并与Pd原子反应,形成所述的PdSe2膜层,图b和c是ZnO/PdSe2核壳结构的场发射扫描电子显微镜图,从图中可以看出,ZnO纳米线长约1微米,阵列表面附着一层非连续的材料,类似形成一种核壳结构。
图2为实施例1和2所得样品的X射线衍射图。其中,ZnO/PdSe2对应的XRD在23°衍射角处均出现弱峰,对应PdSe2标准PDF卡片的(002)峰,表明产物中存在微量的PdSe2(其中标准卡片JCPDS 80-0019);而26°、32°处衍射角分别对应ZnO的标准图谱(JCPDS 36-1451),其余杂峰则是FTO玻璃基板的峰。通过对比标准PDF卡片可知,产物中存在ZnO和PdSe2。膜厚为10nm时得到的产物峰值未发生变化,表明产物结构未发生变化。
图3为实施例1和2所得样品的X射线光电子能谱图。从图a-d中分析可知,ZnO/PdSe2核壳结构中有Zn的2p峰、O的1s峰、Pd的3d峰以及Se的3d峰存在,分别对应Zn2+,O2-,Pd4 +,Se2-,表明产物中存在各个元素对应的价态,也形成了Zn-O和Pd-Se键。对于10nm Pd膜,ZnO/PdSe2异质结而言,两者峰值位置并未发现变化,表明不同Pd膜对产物结构无影响。
图4为实施例1和2所得样品的拉曼光谱图。其中,实验测得的ZnO的拉曼峰位置在440nm处,PdSe2拉曼峰位置在160nm和260nm处,而ZnO/PdSe2的拉曼峰则同时出现了ZnO的Ag峰以及PdSe2的宽峰,表明异质结产物中有ZnO和PdSe2两种物质,且两种产物是以异质结或合金相形式存在,且膜厚对产物无影响。
图5为实施例1所得样品的光电化学性能图。在紫外可见光照射下,图a分别测试了ZnO,PdSe2,ZnO/PdSe2电极材料在偏压在1V下的光电流密度值,图中明显看出ZnO的光电流密度值较小,而ZnO/PdSe2异质结的光电流值最大,且呈现倍增现象,表明形成的ZnO/PdSe2核壳异质结在可见光光照条件下,异质结界面处缺陷增多,激发电子空穴分离,促进异质结界面处电子传输。具体原因可解释如下。暗反应条件下,由于界面态的存在,ZnO形成背靠背式肖特基二极管,阻止异质结界面处的载流子传输,相反,异质结材料受光照时,由于PdSe2较高的化学稳定性及活性位点,进一步促进了界面处的电子空穴对分离,有利于电极材料的光电转换,因此异质结光电性能更好。图b是比较ZnO/PdSe2有光无光下的光电流响应曲线。偏压为0.8V时,ZnO/PdSe2的光响应均较ZnO有2个数量级的提升,表明异质结结构能够促进电子孔空穴分离,有利于光电流生成。
Claims (3)
1.一种高效光电探测性能的核壳异质结阵列电极制备方法,其特征在于,包括如下步骤:
a、配置好0.1-0.5mmol/L醋酸锌溶液,使用滴管取3-5滴醋酸锌溶液放到清洗干净的FTO玻璃上,将FTO玻璃基底置于溶胶机上吸盘固定,先慢速旋涂10-50s,再快速旋涂10-50s,随后于300-400℃下退火10-60分钟,最后将其放入浓度为0.05mol/L Zn(NO3)2和0.05mol/L的乌洛托品溶液中,水浴反应3-6小时,温度设定90℃,连续更换反应液3-5次,得初始产物ZnO;
b、将初始产物ZnO作为基底生长材料,使用氩气作为保护气,利用电子束蒸发方法蒸镀1-10nm Pd膜,待镀膜结束后,取出,得到产物ZnO/Pd;
c、将ZnO/Pd作为基底材料,通过化学气相沉积方法,将产物ZnO/Pd置于高温区,温度设定为400℃,硒粉置于低温区,温度设定为250℃,硒化时间设定为1-2小时,待硒化反应结束后,取出,得到目标产物ZnO/PdSe2;
d、将所得目标产物ZnO/PdSe2作为光电化学测试系统的工作电极,光源采用的是太阳光模拟光源,波长范围为400-800nm,测试其光电流,暗电流,最终比较电极之间的光电性能。
2.如权利要求1所述的一种高效光电探测性能的核壳异质结阵列电极制备方法,其特征在于,所述步骤b中Pd膜为1nm。
3.如权利要求1所述的一种高效光电探测性能的核壳异质结阵列电极制备方法,其特征在于,所述步骤b中Pd膜为10nm。
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