CN113999168A - 一种有机修饰的铜硫二维半导体材料及应用 - Google Patents
一种有机修饰的铜硫二维半导体材料及应用 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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- C07D213/70—Sulfur atoms
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- G—PHYSICS
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- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J1/00—Photometry, e.g. photographic exposure meter
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- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Abstract
一种有机修饰的铜硫二维半导体及光电应用。本发明的目的在于提供一种具有超薄铜硫单层的半导体材料及一种以双重键型构筑二维材料的方法。通过选择碘化亚铜，5‑氯‑2‑巯基吡啶为反应原料，在溶剂热条件下通过原位自助装构筑[Cu(CMP)]的晶态材料，并获得其均一微米片。该微米片制备的薄膜器件表现出折优取向，显著增强的光暗电流响应和良好的光响应稳定性，可利用其特性用于光电转换，紫外及可见区的光探测。
Description
技术领域
本发明涉及一种二维杂化半导体材料，特别是涉及一种有机修饰的铜硫单层半导体材料[Cu(CMP)]（CMP = 5-氯-2-巯基吡啶）的合成及应用。
背景技术
具有超薄结构的二维半导体材料，如氧化石墨烯，黑磷和层状金属硫化物是极具有吸引力的一类材料，它们表现出杰出的光、电和机械性能，在光电器件和生物医学领域具有潜在应用。材料的电学结构决定着二维半导体材料的电子传输和光学等性能，是材料的重要特性。电学结构主要受到二维半导体材料的厚度和原子间键联关系的影响。到目前为止，好几种策略都用于调节二维材料的厚度和键联关系方面，如通过共价作用修饰有机分子，掺杂杂原子或将两种材料合金化。在这些策略中，将有机分子共价修饰在二维材料上受到更多的研究关注，这是因为这种策略不仅丰富了二维材料的键联类型，也将有机分子的功能引入目标材料中，如额外的光学吸收，有机溶剂中具有更好的分散性以及对毒害物质表现出选择性探测。
由于具有丰富、易得和具有可调节带隙的特点，硫化铜（Cu2-xS，0≤x≤1）已经成为广泛研究的金属硫化物材料。它们在柔韧光电导薄膜，传感器、热电器件，光热治疗和能源存储用电极材料等领域表现出与众不同的化学和物理应用。然而，与传统的层状过渡金属双硫化物，如MoS2和WS2不同，硫化铜块体材料并不具有层状的结构。它们主要以具有不同形貌和结构的纳米结构材料进行应用。与此相对应，只有较少的研究关注它们的结构调控，尽管键联类型和厚度等结构因素可以极大地影响它们的性能。例如，强亲铜相互作用可以增强材料的导电性，赋予材料有趣的光学和催化性能。二维材料的厚度可极大地影响材料的光学吸收能力。在这一领域，为了更好开发硫化铜在二维形态方面的应用，一种有机配体修饰-剥离的策略最近被提出，并用于制备层状有机修饰的铜硫属化物纳米片。有机分子插入到块体结构中与铜原子配位，进而把材料的三维结构降低到二维层。然而，只有共价键用于稳定材料的铜硫原子层。此外，有科学家报道采用具有长烷基链的烷基硫醇为有机配体，获得一个具有较好量子井效应的铜硫层状结构，然而材料含有两层铜原子，因此它没有办法获得超薄结构。层状有机铜硫属化物的键联关系和厚度调控仍是一项及具有挑战性的任务；特别地，采用多种键联关系稳定超薄铜硫单层结构至今还未报道。
发明内容
本发明的目的在于合成一种新结构类型的铜硫层状材料[Cu(CMP)] (CMP = 5-氯-2-巯基吡啶)，材料中的铜和硫原子依靠两种键联关系结合形成具有单原子厚度的导电层，该材料可用于光电转换和光电探测领域。
本发明包括如下技术方案：
1. 一种有机修饰的铜硫二维半导体材料[Cu(CMP)]（CMP = 5-氯-2-巯基吡啶），其特征在于：该化合物为单斜晶系，结晶于空间群P21/c，单胞参数为a = 13.61(2) Å, b =6.00(2) Å, c = 7.45(2) Å,α= γ= 90 º, β = 99.16 º。材料外观为橙色块状晶体，其分子结构由5-氯-2-巯基吡啶配体利用其N和S原子连接铜原子构成；铜和硫原子间通过配位键和铜铜相互作用形成一个无机铜硫单层结构，厚度为0.18 nm；，氯吡啶组分通过共价键悬挂在铜硫无机单层两侧，相邻两层间无任何氢键、卤键相互作用力，仅表现为范德华相互作用力。
2. 一种权利要求1所述的铜硫二维半导体材料的制备方法，其特征在于：材料结构由有机配体与金属盐通过原位自组装反应获得；反应物碘化亚铜、5-氯-2-巯基吡啶、水和乙腈，在140 ℃下恒温反应3天，然后降至室温。
3. 一种权利要求1所述的铜硫二维半导体材料的用途，其特征在于：该化合物是一种杂化半导体材料，其微米尺度晶体表现出取向光电导特性，用于光电转换及可见区的光探测应用。
具体实施方式
我们选择了碘化亚铜和5-氯-2-巯基吡啶为反应原料，水和乙腈为溶剂，在溶剂热条件下得到化合物[Cu(CMP)]的单晶。通过单晶X射线衍射，红外，元素分析和X射线光电子能谱等表征，确定其晶体结构。
本发明所提供的有机修饰铜硫纳米单层杂化半导体材料[Cu(CMP)]，结构中铜和硫原子间通过铜硫配位键和铜铜相互作用组装层纳米单层结构，厚度薄于目前已报道的无机铜硫和有修饰的铜硫结构；该材料的合成提供了一种利用多重键制备超薄二维材料的新思路，且该思路操作简单；以铜硫单层半导体微米片制备的薄膜具有显著增强的导电性，稳定性和光电响应。
附图说明：
图1为实施例1化合物的不对称单元图。每个铜为三配位与两个巯基S原子和一个吡啶N原子配位形成(CuS2N)平面三角形；相邻两个铜之间存在铜铜相互作用，铜铜间距为2.677 Å。
图2为实施例1化合物包含的无机铜硫原子单层；铜和硫原子间通过配位键和铜铜相互作用连接；图中虚线表示铜铜相互作用。
图3为实施例1化合物依靠库仑力形成的三维堆积结构图。层层之间无卤键和氢键相互作用。
图4为实施例1化合物的红外光谱图，辅佐证明了结构中的有机组分为5-氯-2-巯基吡啶。
图5为实施例1化合物的在各种条件下的粉末衍射图，实验测试粉末衍射花样与单晶结构数据模拟的相吻合，说明收集的样品较纯；微米片薄膜的粉末衍射表现出有规律的(h00)衍射峰，说明样品晶粒表现出明显的折优取向。
图6为实施例1化合物的固体吸收谱图，在200-600 nm的紫外及可见光范围内有良好的光学吸收，同时也与其颜色相符合；左下角插图：晶体光学照片；右上角插图：Kubelka-Munk图显示其光学带隙为2.44 eV。
图7为实施例1化合物的微米片薄膜在施加光照前后的I-V曲线，on/off导电性比值约为11.0。
图8为实施例1化合物微米片薄膜的光电信号响应和时间图。该光电导器件表现出良好的光响应稳定性。
实施例1：
化合物的制备
1）毫米尺寸晶体制备：称取CuI (0.20 mmol)，KI (1.5 mmol)，5-氯-2-巯基吡啶(0.25 mmol)，然后加入氢碘酸 (1.0 mL)，去离子水 (3 mL)，乙腈 (3 mL)，装入密闭的25mL的反应釜中，采用溶剂热合成方法，在140 ℃恒温3天，随后取出自然降至室温，便可得到橙色块状晶体，经单晶结构测定表明该晶体为[Cu(CMP)]。
微米片制备：称取CuI (0.20 mmol)，5-氯-2-巯基吡啶 (0.25 mmol)，溴化十六烷基三甲基铵 (0.07 mmol)，然后加入去离子水 (3 mL)和乙腈 (3 mL)，搅拌30分钟，装入密闭的25 mL的反应釜中，采用溶剂热合成方法，在140 ℃恒温6小时，随后取出自然降至室温，可得到规整微米片状晶体。
化合物性能测试
1、光学吸收性能
室温下在Shimadzu UV-310 PC UV-vis光谱仪上进行，以BaSO4覆盖薄玻璃片为载体，Kubelka-Munk函数α/S = (1-R)2/2R 1, α为吸收系数，S为散射系数，R为发射系数，结果显示材料的能带宽度为2.44 eV，为半导体材料。
2、半导体性能测试
光电化学测量是基于金叉指电极进行的。5 mg的微米片状晶态样品首先分散在200 微升的乙醇中。吸取3.5 微升的上述悬浊液滴涂在金叉指电极上，控制滴涂面积形成约等于10×5 mm2的薄膜，并将此膜在40 °C下真空干燥。用500 W的氙灯作为光电测试光源，选择不同范围的带通滤光片获得365-700 nm范围的内的特定波长的光。所有光源的光强都通过光强度计进行调校，所有测试都在Solartron ModuLab XM测试平台上进行。
Claims (2)
1.一种有机修饰的铜硫二维半导体[Cu(CMP)]（CMP = 5-氯-2-巯基吡啶），其特征在于：该材料结晶于单斜晶系P21/c空间群，单胞参数为a = 13.61(2) Å, b = 6.00(2) Å, c = 7.45(2) Å,α = γ = 90 º, β = 99.16 º，材料外观为橙色块状晶体，分子结构由5-氯-2-巯基吡啶配体利用N和S原子连接铜原子构成，铜和硫原子间通过配位键和铜铜相互作用形成一个无机铜硫单层纳米片状结构，氯吡啶组分通过共价键悬挂在铜硫无机单层两侧，晶体结构中层与层之间仅存在范德华作用力。
2.一种权利要求1所述的铜硫二维半导体的用途，其特征在于：该材料是一种杂化半导体材料，晶态薄膜表现出取向光电导特性，用于光电转换及紫外和可见光区的光探测。
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