CN108054241A - 一种增强CdIn2S4光学吸收的方法 - Google Patents
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Abstract
本发明公开了一种增强CdIn2S4光学吸收的方法,具体是在半导体CdIn2S4中掺杂非过渡金属原子Sn,诱导其带隙中产生中间杂质能带,从而产生新的光学吸收途径,达到增强CdIn2S4光学吸收的目的;具体地,按照CdIn2‑xSnxS4的化学计量比称取Cd、In、S和Sn原料,真空封装于石英玻璃管内升温至700‑800℃反应烧结,保温24‑48小时后随炉冷却,然后二次反应烧结即得。上述方法增强了CdIn2S4光学吸收能力,在光催化、光伏电池等领域具有广泛的应用前景。
Description
技术领域
本发明属于半导体光电材料技术领域,具体涉及一种增强CdIn2S4光学吸收的方法。
背景技术
太阳能作为一种可再生的清洁能源,有着资源丰富、不受地域限制使用等优点,利用半导体的光电转换效应可以直接把光转换成电,是人们利用太阳能的一种重要途径。一般的半导体材料只能吸收利用能量在带隙附近的光子,能量小于和超出带隙的光子无法被半导体直接利用,从而导致能量损失。通过半导体掺杂技术,在半导体带隙中引入中间能级或能带,能够实现对太阳光的多重吸收,从而更好地利用太阳光谱能量。具有杂质能级的太阳能电池理论极限效率为63.1%,大大超越传统的单带电池理论极限效率40.7%(Physical Review Letters,1997,78(26):5014-5017)。
CdIn2S4属于三元尖晶石结构化合物,光电性能优异,在光催化、发光二极管、光伏电池等领域具有潜在的应用前景。CdIn2S4光学带隙较氧化物较窄(2.1eV),能够较好地吸收可见光。为了进一步提高CdIn2S4光学吸收能力,可以通过元素掺杂方法在其带隙中引入杂质能级,从而构建新的光学吸收途径。理论研究发现,Ti、V、Cr、Mn掺杂CdIn2S4将导致中间杂质带形成,并通过计算受主半导体和掺杂材料的光学吸收谱证明杂质能级的产生能够改进光学吸收性能(1、Physical Review B,2010,81(7):075206;2、Journal of Alloys andCompounds,2014,591:22-28.);在实验研究方面,申请号CN201611151273.1的中国专利公开了利用过渡族元素Fe的3d电子在晶体场中产生轨道劈裂形成杂质能级,发现掺杂的半导体具有宽光谱吸收特征。
综上所述,现有技术中对CdIn2S4光学吸收的改进方法主要集中于过渡金属掺杂,并且大部分停留于理论研究,与实验严重脱节;另外,过渡金属d电子过于局域,不利于载流子分离,容易形成新的掺杂缺陷复合中心,影响半导体的实际光电转换性能。
发明内容
为克服现有技术的上述缺陷,针对CdIn2S4半导体只能吸收利用部分可见光的问题,本发明的目的在于提供一种增强CdIn2S4光学吸收的方法,采用半导体掺杂技术,首次提出利用非过渡金属Sn掺杂,诱导CdIn2S4杂质能级产生,调控受主半导体CdIn2S4的电子能带结构,构建新的光学吸收途径从而增强其光学吸收能力。
本发明的目的还在于提供由上述方法得到的Sn掺杂CdIn2S4半导体。
本发明的上述目的通过以下技术方案实现:
一种增强CdIn2S4光学吸收的方法,在半导体CdIn2S4中掺杂非过渡金属原子Sn,诱导CdIn2S4的带隙中产生中间杂质能带,其中,掺杂位置为用非过渡金属原子Sn取代所述半导体CdIn2S4中部分In原子,所得产物的化学分子式为CdIn2-xSnxS4,式中0<x<2,包括以下步骤:
S1、按照所述CdIn2-xSnxS4的化学计量比称取Cd、In、S和Sn原料,真空封装于石英玻璃管中;
S2、将步骤S1中所述的石英玻璃管置于程序控温马弗炉中,以2-5℃/分钟速率缓慢升温至700-800℃反应烧结,保温24-48小时后随炉冷却;
S3、将步骤S2中所述冷却后的产物倒出并研磨,重新真空封装于石英玻璃管内,并置于程序控温马弗炉中,再以2-5℃/分钟速率缓慢升温至700-800℃反应烧结,保温24-48小时后随炉冷却后再次研磨。
进一步地,步骤S1中所述的Cd、In、S和Sn原料包括单质或二元化合物,纯度均不低于99.99%。
进一步地,所述的中间杂质能带具有金属性。
进一步地,所述的中间杂质能带由Sn-5s态和S-3p态杂化而成。
进一步地,所述的非过渡金属原子Sn优化的掺杂含量不大于5at%。
一种由上述增强CdIn2S4光学吸收的方法得到的掺杂CdIn2S4半导体,化学分子式为CdIn2-xSnxS4,其中0<x<2。
在本发明的一个实施例中,所述Cd、In、S和Sn原料均为单质。
在本发明的另一个实施例中,所述Cd、In、S和Sn原料均为二元化合物。
在符合本领域常识的基础上,上述各优选条件可以任意组合即得本发明各较佳实例;另外本发明所用的原料和试剂除另有说明外均市售可得或为常规选择。
本发明中掺杂CdIn2S4半导体的表征手段中,结构采用X射线衍射图谱表征(XRD),元素分析采用能谱仪测得(EDX),价态分析采用光电子能谱(XPS)表征,紫外-可见-近红外吸收光谱在Hitachi U4100UV-Vis-NIR分光光度计上测得。
本发明首次提出利用非过渡金属Sn掺杂,诱导CdIn2S4杂质能级产生,形成的机制与过渡原子掺杂明显不同,用杂质原子Sn取代部分In原子,Sn元素具有5s5p电子构型,S具有3s3p电子构型,Sn原子5s电子能够与周围S3p电子杂化成键,从而在受主半导体的带隙中构建新的能带。
与现有技术相比,本发明的积极进步效果在于:
(1)CdIn2S4属于三元尖晶石结构化合物,CdIn2S4光学带隙较氧化物较窄(2.1eV),只能吸收利用部分可见光,本发明中上述方法在增强CdIn2S4光学吸收能力的同时,显著提高CdIn2S4的光电转换效率,在光催化、光伏电池等领域具有潜在的应用前景。
(2)本发明中掺杂CdIn2S4半导体的紫外-可见-近红外吸收光谱可以观测到两个吸收边,光学吸收能力明显增强,进一步证明非过渡金属Sn掺杂能够有效增强CdIn2S4的光学吸收能力。
附图说明
图1为CdIn2-xSnxS4(x=0,0.05,0.1)系列样品的XRD图谱;
图2为CdIn1.9Sn0.1S4的EDX元素分析图谱;
图3为CdIn1.9Sn0.1S4中Sn的3d XPS图谱;
图4为CdIn2-xSnxS4(x=0,0.05,0.1)系列样品的UV-Vis-NIR吸收光谱;
图5为Sn掺杂CdIn2S4后的能带结构图谱。
具体实施方式
下面结合实施例对本发明做进一步详细、完整地说明,但本发明绝非限于实施例。
实施例1CdIn2-xSnxS4(x=0,0.05,0.1)材料的制备
将Cd粉(纯度为99.99%)、In粒(纯度为99.999%)、S粉(纯度为99.999%)和Sn粉(纯度为99.99%)按照CdIn2-xSnxS4(x=0,0.05,0.1)的化学计量比称量,放入石英玻璃管中,并将石英玻璃管用氢氧焰熔封;将熔封的石英玻璃管放入程序控温马弗炉中,以2℃/分钟速率缓慢升温至750℃并保温24小时后随炉冷却至室温;再开管后,将所得样品置于玛瑙研钵中研磨,真空封装于石英玻璃管内,置于程序控温马弗炉中,以2℃/分钟速率缓慢升温至750℃再次烧结并保温48小时,样品随炉冷却至室温,开管后再次研磨即得。
实施例2CdIn2-xSnxS4(x=0,0.05,0.1)材料的制备
将纯度不低于99.99%的Cd、In、S和Sn的二元化合物按照CdIn2-xSnxS4(x=0,0.05,0.1)的化学计量比称量,放入石英玻璃管中,并将石英玻璃管用氢氧焰熔封;将熔封的石英玻璃管放入程序控温马弗炉中,以5℃/分钟速率缓慢升温至700℃并保温48小时后随炉冷却至室温;再开管后,将所得样品置于玛瑙研钵中研磨,真空封装置于石英玻璃管内,于程序控温马弗炉中,再以5℃/分钟速率缓慢升温至700℃再次烧结并保温24小时,样品随炉冷却至室温,开管后再次研磨即得。
实施例3CdIn2-xSnxS4(x=0,0.05,0.1)材料的制备
将Cd粉(纯度为99.99%)、In粒(纯度为99.999%)、S粉(纯度为99.999%)和Sn粉(纯度为99.99%)按照CdIn2-xSnxS4(x=0,0.05,0.1)的化学计量比称量,放入石英玻璃管中,并将石英玻璃管用氢氧焰熔封;将熔封的石英玻璃管放入程序控温马弗炉中,以3℃/分钟速率缓慢升温至750℃并保温24小时后随炉冷却至室温;再开管后,将所得样品置于玛瑙研钵中研磨,真空封装置于石英玻璃管内,于程序控温马弗炉中,再以3℃/分钟速率缓慢升温至800℃再次烧结并保温24小时,样品随炉冷却至室温,开管后再次研磨即得。
实施例4CdIn2-xSnxS4(x=0,0.05,0.1)材料的制备
将Cd粉(纯度为99.99%)、In粒(纯度为99.999%)、S粉(纯度为99.999%)和Sn粉(纯度为99.99%)按照CdIn2-xSnxS4(x=0,0.05,0.1)的化学计量比称量,放入石英玻璃管中,并将石英玻璃管用氢氧焰熔封;将熔封的石英玻璃管放入程序控温马弗炉中,以4℃/分钟速率缓慢升温至800℃并保温24小时后随炉冷却至室温;再开管后,将所得样品于玛瑙研钵中研磨,真空封装于石英玻璃管内,并置于程序控温马弗炉中,再以4℃/分钟速率缓慢升温至800℃再次烧结并保温24小时,样品随炉冷却至室温,开管后得到目标粉体样品,再次研磨。
实施例5CdIn2-xSnxS4(x=0,0.05,0.1)材料的制备
将纯度不低于99.99%的Cd,In,S和Sn的二元化合物按照CdIn2-xSnxS4(x=0,0.05,0.1)的化学计量比称量,放入石英玻璃管中,并将石英玻璃管用氢氧焰熔封;将熔封的石英玻璃管放入程序控温马弗炉中,以5℃/分钟速率缓慢升温至780℃并保温36小时后随炉冷却至室温;再开管后,将所得样品于玛瑙研钵中研磨,真空封装于石英玻璃管内,置于程序控温马弗炉中,再以5℃/分钟速率缓慢升温至800℃再次烧结并保温24小时,样品随炉冷却至室温,开管后再次研磨即得。
效果例实施例1中CdIn2-xSnxS4(x=0,0.05,0.1)材料的测试与表征
对实施例1中的掺杂CdIn2S4半导体的结构、元素分析、价态分析和紫外-可见-近红外吸收光谱进行分析测试,结果见附图1-5,其中,结构采用X射线衍射图谱表征,元素分析采用能谱仪测得,价态分析采用光电子能谱表征,紫外-可见-近红外吸收光谱在HitachiU4100UV-Vis-NIR分光光度计上测得。
参见附图1,CdIn2-xSnxS4(x=0,0.05,0.1)系列样品的XRD图谱可以看出所有衍射峰都与标准卡片相对应,说明所制备的样品为纯相。
参见附图2,CdIn1.9Sn0.1S4的EDX元素分析图谱分析可知,样品由Cd、In、S和Sn四种元素组成。
参见附图3,选择CdIn1.9Sn0.1S4样品进行XPS分析测试,结果进一步确认样品由Cd,In,S和Sn四种元素组成;附图3为Sn元素的3d谱图,通过拟合XPS谱图,Sn 3d5/2峰可以分成两个峰,分别位于486.3eV和487.0eV;Sn 3d3/2也可以分成两个峰,分别位于495.3eV和495.5eV;XPS分析可以推断Sn元素在化合物中以两种形式存在,分别为Sn2+和Sn4+。
参见附图4,为CdIn2-xSnxS4样品的UV-Vis-NIR吸收光谱,可以看到,在Sn掺杂以后可以观测到两个吸收边,验证其增强的光学吸收能力;其中Sn掺杂样品的吸收曲线首先从1350nm(1.09eV)附近开始升高,在700nm(1.77eV)达到第一个平台,然后从630nm(2.06eV)附近开始再次吸收增强,出现第二个吸收边。
参见附图5,为Sn掺杂CdIn2S4后的能带结构图谱,可以看到,在Sn掺杂以后,在导带底部引入一条新的能带,该能带由两条自旋劈裂的能级组成,并且费米能级穿越该能带,说明体系具有金属性,增加一个吸收起源于电子从价带到中间带的跃迁。
虽然,上文中已经用一般性说明及具体实施例对本发明作了详尽的描述,但在本发明基础上,可以对之作一些修改或改进,这对本领域技术人员而言是显而易见的。因此,在不偏离本发明精神的基础上所做的这些修改或改进,均属于本发明要求保护的范围。
Claims (7)
1.一种增强CdIn2S4光学吸收的方法,其特征在于,在半导体CdIn2S4中掺杂非过渡金属原子Sn,诱导CdIn2S4的带隙中产生中间杂质能带,其中,掺杂位置为用非过渡金属原子Sn取代所述半导体CdIn2S4中部分In原子,所得产物的化学分子式为CdIn2-xSnxS4,式中0<x<2,包括以下步骤:
S1、按照所述CdIn2-xSnxS4的化学计量比称取Cd、In、S和Sn原料,真空封装于石英玻璃管中;
S2、将步骤S1中所述的石英玻璃管置于程序控温马弗炉中,以2-5℃/分钟速率缓慢升温至700-800℃反应烧结,保温24-48小时后随炉冷却;
S3、将步骤S2中所述冷却后的产物倒出并研磨,重新真空封装于石英玻璃管内,并置于程序控温马弗炉中,再以2-5℃/分钟速率缓慢升温至700-800℃反应烧结,保温24-48小时后随炉冷却后再次研磨。
2.一种如权利要求1所述的增强CdIn2S4光学吸收的方法,其特征在于,步骤S1中所述的Cd、In、S和Sn原料包括单质或二元化合物,纯度均不低于99.99%。
3.一种如权利要求1所述的增强CdIn2S4光学吸收的方法,其特征在于,所述的中间杂质能带具有金属性。
4.一种如权利要求3所述的增强CdIn2S4光学吸收的方法,其特征在于,所述的中间杂质能带由Sn-5s态和S-3p态杂化而成。
5.一种如权利要求1所述的增强CdIn2S4光学吸收的方法,其特征在于,所述的非过渡金属原子Sn优化的掺杂含量不大于5at%。
6.一种掺杂CdIn2S4半导体,其特征在于,通过权利要求1-5任一项所述的增强CdIn2S4光学吸收的方法得到。
7.一种如权利要求6所述的掺杂CdIn2S4半导体,其特征在于,化学分子式为CdIn2- xSnxS4,其中0<x<2。
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