CN114773260A - 一种紫精π-聚集体的卤化铅光致变色化合物 - Google Patents
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Abstract
本发明公开了一种紫精π‑聚集体的卤化铅光致变色化合物,其结构通式为[(CQ)Pb3X6(H2O)]·2H2O[X=Cl(1)和Br(2)],CQ=N‑4,4’‑Bipyridiniopropionate,其晶体结构为具有离子插层式的二维结构,属于三斜晶系,空间群为P‑1,对应空间群号为2。本发明同时公开了制备方法,以卤化铅和有机配体按1:1摩尔比的两个水溶液混合,混合溶液75℃加热5小时后趁热过滤后在黑暗处室温下放置14天,得到光致变色半导体材料。本发明获得的光致变色半导体材料,在光致电子转移变色后,其导电性没有发生明显的变化,这为从根本上了解结构因素对电子转移后电学性能的影响,从而为刺激响应型半导体的开发提供了基础。
Description
技术领域
本发明涉及光半导体材料及材料合成领域,具体涉及一种紫精π-聚集体的卤化铅无机-有机杂化光致变色化合物及其制备方法。
背景技术
半导体电子器件的核心是载流子传输,比如目前的场效应晶体管、发光二极管、太阳能电池以及传感器等。研究半导体电性能的变化规律对此领域具有重要意义。目前调节半导体电性能往往是通过使半导体晶体结构发生明显变化,使其结构失去有序周期性来实现,比如掺杂、表面功能化、晶体缺陷或者其它化学方法。由于单晶衍射法难以确定被调控的单晶结构,使得电导率与结构之间的关系难以研究。即使目前发现掺杂某些元素是可以调节半导体的电性能,但是要了解掺杂元素周围的化学环境以及半导体本身故有的结构如何相互作用是不可能的,更不用说半导体结构内的相互作用能。因此目前很难提出理论思路来指导合成方向和结构设计。
在最近的许多研究中,提出了通过物理方法调控半导体的电学性质,比如光刺激和热刺激。将具有氧化还原活性的紫精(N,N’-4,4’-双取代联吡啶)引入到半导体的无机骨架中,使半导体具有电子转移的光致变色特性。根据刺激方法不同,它们被称为光致变色半导体或者热致变色半导体。刺激响应半导体可以在外界刺激后在不同电学性质的双稳态之间可逆转换。在变色过程中,半导体中只发生电子转移,而结构没有发生变化。因此刺激响应半导体是研究其电学性能与结构关系的理想对象。
发明内容
为解决上述问题,本发明提供一种紫精π-聚集体的卤化铅光致变色化合物及制备方法。
为实现上述目的,本发明采用以下技术方案:
一种紫精π-聚集体的卤化铅光致变色化合物,其结构通式为[(CQ)Pb3X6(H2O)]·2H2O[X=Cl(1)和Br(2)],CQ=N-4,4’-Bipyridiniopropionate,其晶体结构为具有离子插层式的二维结构,属于三斜晶系,空间群为P-1,对应空间群号为2。
进一步地,该化合物的晶胞参数分别为: α=107.784(3)°β=103.145(3)°γ=91.535(3)°(1); α=108.335(5)°β=103.815(3)°γ=90.716(5)°(2)。
本发明同时公开了一种制备上述的紫精π-聚集体的卤化铅光致变色化合物的方法,其特征在于,包括以下步骤:
1)首先通过联吡啶和丙烯酸合成有机配体CQ;
2)将卤化铅PbX2[X=Cl(1)和Br(2)]溶解于30mL水中,并在75℃加热1小时,获得澄清无色溶液,将有机配体CQ溶解于30mL水中,之后与所述澄清无色溶液混合,继续在75℃加热5小时,得到黄色溶液,趁热过滤,得到澄清黄色溶液,所述卤化铅PbX2[X=Cl(1)和Br(2)]与有机配体CQ的摩尔比为1:1;
3)将得到的澄清黄色溶液放置于黑暗中室温下挥发14天得到浅黄色的针状晶体,所得到的浅黄色针状晶体即为最终产物。
优选地,所述卤化铅为氯化铅或溴化铅。
采用上述技术方案后,本发明具有如下有益效果:
本发明获得的具有罕见的Ⅱ-堆积的紫精π-聚集体的卤化铅无机-有机杂化光致变色半导体材料,与具有常见的Ⅰ-堆积的紫精π-聚集体的卤化铅无机-有机杂化光致变色半导体材料进行对比,在光致电子转移变色后,它的导电性没有发生明显的变化。这同时解释了为什么此类半导体的电性能在发生电子转移后没有发生明显变化的原因,这为合成刺激响应型半导体提供了基础。
附图说明
图1实施例1制备的光致变色半导体材料的晶体照片;
图2实施例1制备的光致变色半导体材料的结构图;
图3实施例1制备的光致变色半导体材料变色前后的粉末衍射图;
图4实施例1制备的光致变色半导体材料变色前后的紫外吸收光谱图;
图5实施例1制备的光致变色半导体材料变色前后的顺磁信号谱图;
图6实施例1制备的光致变色半导体材料变色前后的电导性;
图7实施例1制备的光致变色半导体材料变色前后的活化能。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。
实施例1
1)首先按照文献《Angew.Chem.Int.Ed.》(德国应用化学)(2012年第57卷3432-3435页)所提供的方法,通过联吡啶和丙烯酸合成有机配体CQ。
2)将卤化铅PbX2[X=Cl(1)和Br(2)]溶解于30mL水中并75℃加热1小时获得澄清无色溶液。将有机配体CQ溶解于30mL水中,之后将两个溶液混合继续75℃加热5小时得到黄色溶液,趁热过滤,得到澄清的黄色溶液。其中卤化铅和有机配体的摩尔比为1:1。
3)将得到的澄清黄色溶液放置于黑暗中室温下挥发14天得到浅黄色的针状晶体。
4)得到的浅黄色的针状晶体即是具有光致变色半导体材料。
对实施例1的表征与性能测试:
(1)晶体结构测定
在显微镜下挑选大小合适、形状规则且透亮的单晶,通过BrukerAPEX II CCD衍射仪,在175(2)K下,采用石墨单色器单色化的Mo-Kα射线( )作为入射光源以收集晶体衍射数据。在结构解析中使用Shelextl-97程序以直接法对晶体结构进行解析和精修,同时非氢原子及其各向异性化处理参数利用全矩阵最小二乘法进行修正,所有的氢原子通过理论加氢得到,所得晶体结构图如图2所示。部分晶体学数据以及精修参数见表1。
表1:化合物的晶体参数表
(2)实施例1粉末衍射表征:
取适量所上述方法制备的单晶,将其充分研磨成粉末,在常温下测得半导体材料的粉末衍射图(图3)与根据单晶衍射数据模拟的衍射峰的对比可知,实验测定结果与Mercury软件拟合结果吻合的较好,由此可说明该化合物为纯相。其中晶体的各向异性导致了部分衍射峰在峰强上有所差异。同时粉末在光照变色后,其粉末衍射图与未变色时相同,证明半导体材料在电子转移后没有发生结构变化。
(3)实施例1紫外吸收光谱表征:
如图4所示,化合物在光照变色后出现新的吸收峰,在412、566、618nm处化合物1的宽吸收带和562、612nm处化合物2的宽吸收带主要归因于卤素原子的电子转移到N+,生成紫精自由基。
(4)实施例1顺磁信号光谱表征:
如图5所示,半导体在光照前不存在信号,而在光照后出现g=2.0030处出现新的信号,这是由于半导体在光照后生成紫精自由基。化合物在黑暗中放置一段时间褪色后,信号消失,这是由于紫精自由基发生氧化反应,变成N+,这说明变色是可逆的。
(5)实施例1的光照前后的导电性和活化能:
如图6和7所示,半导体在变色前后,它的导电性没有发生明显的变化。变色前后的活化能也证明了这一点。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求的保护范围为准。
Claims (4)
1.一种紫精π-聚集体的卤化铅光致变色化合物,其特征在于,其结构通式为[(CQ)Pb3X6(H2O)]·2H2O[X=Cl(1)和Br(2)],CQ=N-4,4’-Bipyridiniopropionate,其晶体结构为具有离子插层式的二维结构,属于三斜晶系,空间群为P-1,对应空间群号为2。
3.一种制备权利要求1或2所述的紫精π-聚集体的卤化铅光致变色化合物的方法,其特征在于,包括以下步骤:
1)首先通过联吡啶和丙烯酸合成有机配体CQ;
2)将卤化铅PbX2[X=Cl(1)和Br(2)]溶解于30mL水中,并在75℃加热1小时,获得澄清无色溶液,将有机配体CQ溶解于30mL水中,之后与所述澄清无色溶液混合,继续在75℃加热5小时,得到黄色溶液,趁热过滤,得到澄清黄色溶液,所述卤化铅PbX2[X=Cl(1)和Br(2)]与有机配体CQ的摩尔比为1:1;
3)将得到的澄清黄色溶液放置于黑暗中室温下挥发14天得到浅黄色的针状晶体,所得到的浅黄色针状晶体即为最终产物。
4.如权利要求3所述的一种制备紫精π-聚集体的卤化铅光致变色化合物的方法,其特征在于,所述卤化铅为氯化铅或溴化铅。
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