CN116536048B - 一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点合成方法及应用 - Google Patents
一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点合成方法及应用 Download PDFInfo
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- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0322—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIBIIICVI chalcopyrite compounds, e.g. Cu In Se2, Cu Ga Se2, Cu In Ga Se2
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Abstract
一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点合成方法及应用，属于纳米材料和能源器件领域。采用热注入法可控合成、尺寸、化学组分可调节的CuInSe2/CuInS2核壳结构量子点，并通过电泳沉积方法将其沉积到介孔TiO2薄膜上，制得光阳极；其与对电极、参比电极和电解液共同组成光电化学电池，在标准测试条件下，可获得8 mA/cm2以上的光电流密度，表明电子‑空穴可有效分离和传输，在光电催化分解水产氢领域展现出较高的应用潜力。该方法具有操作简单、可重复性高等优势，量子点尺寸、化学组分的变化影响能带结构与电荷分离，从而可获得较高的电荷分离和传输效果，减少复合，提升光电器件性能。
Description
技术领域
本发明属于半导体量子点及其能源器件领域，具体涉及一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点合成方法与光电化学电池的应用。
背景技术
随着社会发展，能源和环境问题日益突出。不可再生的化石能源仍作为世界能源使用结构的主体，其燃烧后会产生大量温室气体CO2，导致全球气候变暖，并引发一系列环境问题。因此，开发清洁可代替能源实现碳中和成为当前一个重要任务。在众多的可再生能源体系中，氢能具有能量密度高、零碳排放的优点，是理想的清洁可再生能源。如能通过光催化技术实现太阳能分解水制氢，将能量密度低、分散性强的太阳能转化为氢能，将推动人类社会进入一个能源清洁、环境和谐的新时代。
自1972年Fujishima和Honda(Nature,1972,238(5358):37-38)报道了TiO2在紫外光下将水分解为氢气和氧气的现象，光催化分解水制氢技术因能源清洁可再生、环境友好无碳排放等优点受到了科研界的高度关注。光催化技术包括光催化和光电催化两种形式，光催化的产物是氢气与氧气的混合气体，还需要经过后续分离步骤，而光电催化分解水生成的氢气和氧气分别出现在两个不同的电极上，可直接收集到较纯净的氢气，因此更具优势。实现高效光电催化制氢的关键是制备高效催化剂。近五十年来，科学家开发了数百种半导体光催化材料，如TiO2(Energy&Environmental Science,2015,8(8):2377-2382.)、BiVO4(Advanced Materials,2019,31(20):1806938)等。现阶段光催化材料对太阳能的转化效率低等局限使该技术迟迟未获实际应用，其中的原因主要包括：1)上述材料大多仅能吸收太阳光中的紫外光和部分可见光，对太阳能的利用率较低；2)材料表面存在大量缺陷，导致严重的电荷复合。因此开发高效新型光催化材料具有重要的意义。
半导体量子点和块体材料相比，具有诸多独特的物理性质，如量子限域效应、高消光系数和多重激子效应，且具有更大的比表面积，可以提供更多表面活性位点，因此，在光电催化领域展现出巨大的应用潜力。目前研究较多、性能较好的主要是Cd系量子点，但是这类量子点对光的吸收只能覆盖可见光区域，且含有毒重金属Cd，对环境和人类健康造成危害，限制其应用。CuInSe2量子点具有低毒性、较高的光吸收系数和较窄的禁带宽度(1.04eV)，其吸收可达近红外区域(～1200nm)，在光催化领域展现出巨大的应用潜力。然而，由于CuInSe2量子点表面缺陷较多，导致严重的界面电荷复合，从而降低其光电催化性能。构建核壳结构是钝化表面缺陷，提高光电性能的有效手段。通常在CuInSe2量子点表面生长宽带隙壳层材料ZnS或ZnSe，虽然ZnS、ZnSe对CuInSe2核心的表面缺陷有较好的钝化作用，但是由于Zn离子与Cu离子尺寸接近，在壳层生长过程中极易发生阳离子交换反应，导致核心发生合金化，从而拓宽量子点带隙，缩小光谱吸收范围，降低对太阳光的利用率。同为I-III-VI2族的三元半导体的CuInS2，带隙为1.55eV，具有与CuInSe2相似的晶体结构，同时可以与CuInSe2形成II型核壳结构，促进载流子分离。Tong等(Advanced Energy Materials2018,8,1701432)以CdS/CdSe核壳结构量子点为模板，通过离子交换法制备了CuInSe2/CuInS2核壳结构量子点，并应用到光电化学电池中，获得3.1mA/cm2的电流密度。随后，Li等(Applied Catalysis B:Environmental,2021,280:119402)进一步优化了这一结构，同样使用离子交换法合成了具有梯度层的CuInSe2/(CuInSexS1-x)5/CuInS2核壳结构量子点，由于存在梯度层，核心的光生电子更容易转运，进一步提升了光电性能，获得4.5mA/cm2的光电流密度。上述结果表明，构建CuInSe2/CuInS2核壳结构可有效促进电荷分离和传输，在光电催化领域具有较大的应用潜力。虽然通过离子交换法实现了CuInS2/CuInSe2核壳结构的制备，但是一方面可能会有模板阳离子残余，且尺寸不可调控，另一方面离子交换过程常在低温下进行会引入新的缺陷，对量子点光电性能造成不利影响。除了构建核壳结构，量子点的尺寸、化学组分对量子点的能带结构、表面缺陷等存在较大影响，进而影响光生载流子的分离与传输。因此，发展新的控制合成方法，制备尺寸、化学组分可调的CuInSe2/CuInS2核壳结构并应用于光电催化具有重要意义。
发明内容
为克服现有技术不足，本发明提供了一种尺寸、化学组成可调的CuInSe2/CuInS2核壳结构量子点合成方法与光电化学电池，通过发展可控的合成方法，在CuInSe2量子点表面直接原位生长CuInS2壳层，制备尺寸及化学组成可调的CuInSe2/CuInS2核壳结构量子点；并用于光电化学电池，以期实现光电催化分解水制氢。该方法操作简单、可重复性高，并且可以实现一锅合成核壳结构的量子点，实现壳层原位生长，形成II型核壳结构，降低缺陷，并促进载流子分离和传输，提升光电性能。
为实现上述目的，解决现有技术中存在的问题，本发明使用技术方案如下：
一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点合成方法，包括以下合成步骤：
S1、将铜盐和铟盐按照摩尔比1:2～1:4的比例，加入由非配位溶剂和配位溶剂按体积比1:2组成的混合溶液中，置于加热装置的反应容器中，搅拌、抽真空，并升温至80～120℃，获得含有Cu和In离子的阳离子前驱体溶液；
S2、将硒粉、油胺、正十二硫醇按照摩尔比1:2:1～1:2.8:1.7比例，搅拌混合，获得Se前驱体；
S3、在惰性气体氛围下，将阳离子前驱体溶液升温至140～170℃，按照铜盐与硒粉摩尔比1:0.6～1:2比例注入Se前驱体，保温30～90分钟，然后升温至210～240℃，保温30～90分钟，待保温结束后冷却至室温，使用正己烷和乙醇的混合溶液洗涤量子点，使用非极性溶剂重新分散，获得0.005～0.01摩尔浓度的不同尺寸、化学组分的CuInSe2/CuInS2核壳结构量子点溶液。
所述铜盐为碘化铜、溴化亚铜、氯化亚铜或醋酸亚铜中的任意一种。
所述铟盐为氯化铟、溴化铟、碘化铟、醋酸铟及其水合物中的任意一种。
所述非配位溶剂为十八烯或石蜡油。
所述配位溶剂为油胺、油酸、正十二硫醇、辛硫醇中的两种按体积比1:1配制。
所述非极性溶剂为甲苯、正己烷或二氯甲烷中的一种。
一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点的光电化学电池，光电化学电池中光阳极所需的CuInSe2/CuInS2核壳结构量子点采用上述方法合成得到。
所述光阳极包括以下制备步骤：
X1、将乙基纤维素、纳米TiO2粉末和松油醇按照质量比1:1:4～1:3.5:8比例，搅拌混合，获得TiO2浆料；
X2、使用流延法将TiO2浆料涂覆在掺氟氧化锡透明导电玻璃基底上，干燥后在450～550℃退火20～40分钟，获得介孔TiO2薄膜电极；
X3、使用电泳沉积法将0.005～0.01摩尔浓度的不同尺寸、化学组分的CuInSe2/CuInS2核壳结构量子点溶液沉积到介孔TiO2薄膜电极上，获得光电化学电池光阳极。
进一步，所述光化学电池的制备方法如下：
Y1、使用连续离子层吸附和反应方法在上述方法制备的光阳极表面包覆ZnS保护层；
Y2、将带有ZnS保护层的光阳极、对电极、参比电极浸入到电解液中，获得光电化学电池。
所述电解液为硫化钠和亚硫酸钠混合溶液、氢氧化钠溶液或硫酸钠溶液中的一种。
本发明的有益效果：采用热注入法合成尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点。通过调整铟前驱体浓度，增加了CuInSe2核心的形核量，从而明显降低了反应体系中的反应物浓度，使晶粒长大所需的反应物减少，实现尺寸可调节；同时，由于CuInSe2核心中的化学键长错配(RCu-Se≠RIn-Se)，导致其内部存在很高比例的固有点缺陷(如铜空位、铟取代铜的反位缺陷)，这些点缺陷使得量子点偏离化学计量比，而点缺陷浓度可以通过改变前驱体浓度来调控，由此实现量子点化学组分可调节。然后通过电泳沉积方法将CuInSe2/CuInS2核壳结构量子点沉积到介孔TiO2薄膜上，制得光阳极，并与对电极、参比电极和电解液共同组成光电化学电池。
该方法具有操作简单、可重复性高等优势，量子点尺寸、化学组分的变化影响能带结构与电荷分离，从而可获得较高的电荷分离和传输效果，减少复合，提升光电器件性能。
在标准测试条件下，可获得8mA/cm2以上的光电流密度，表明电子-空穴可有效分离和传输，在光电催化分解水产氢领域展现出较高的应用潜力。
附图说明
图1是CuInSe2核心和CuInSe2/CuInS2核壳结构量子点透射电镜照片。
图2是CuInSe2核心和CuInSe2/CuInS2核壳结构量子点XRD图。
图3是Cu/In＝1:5时产物的透射电镜照片和XRD图。
图4是CuInSe2核心和CuInSe2/CuInS2核壳结构量子点光致发光光谱和瞬态光致发光光谱。
图5是光电极照片。
图6是对比例与实施例中电流密度-电压曲线。
具体实施方式
下文将结合具体附图详细描述本发明具体实施例。应当注意的是，下述实施例中描述的技术特征或者技术特征的组合不应当被认为是孤立的，它们可以被相互组合从而达到更好的技术效果。
实施例1
将CuI和In(OAc)3按照摩尔比1:2混合，加入由十八烯、油胺和正十二硫醇按体积比1:1:1组成的混合溶液中，置于加热装置的反应容器中，搅拌、抽真空，升温至100℃，获得阳离子前驱体溶液；将硒粉、油胺和正十二硫醇按照摩尔比1:2.1:1.3比例，搅拌混合，获得Se前驱体；在惰性气体氛围下，将阳离子前驱体升温至170℃，按照CuI与Se摩尔比1:1比例注入Se前驱体，保温80分钟，然后升温至235℃，保温80分钟，待保温结束后，冷却至室温，向反应溶液中加入正己烷和乙醇，并进行离心，然后使用甲苯重新分散，获得摩尔浓度为0.006的CuInSe2/CuInS2(Cu/In＝1:2)核壳结构量子点溶液。量子点平均尺寸约为4.4nm，发射波长为893nm,其元素比例为：Cu:In:Se:S＝1:0.79:1.27:0.62。
实施例2
将CuI和In(OAc)3按照摩尔比1:3混合，加入由十八烯、油胺和正十二硫醇按体积比1:1:1组成的混合溶液中，置于加热装置的反应容器中，搅拌、抽真空，升温至100℃，获得阳离子前驱体溶液；将硒粉、油胺和正十二硫醇按照摩尔比1:2.1:1.3比例，搅拌混合，获得Se前驱体；在惰性气体氛围下，将阳离子前驱体升温至170℃，按照CuI与Se摩尔比1:1比例注入Se前驱体，保温80分钟，然后升温至235℃，保温80分钟，待保温结束后，冷却至室温，向反应溶液中加入正己烷和乙醇，并进行离心，然后使用甲苯重新分散，获得摩尔浓度为0.006的CuInSe2/CuInS2(Cu/In＝1:3)核壳结构量子点溶液。量子点平均尺寸约为3.6nm，发射波长为837nm,其元素比例为：Cu:In:Se:S＝1:1.34:2.34:1.25。
实施例3
将CuI和In(OAc)3按照摩尔比1:4混合，加入由十八烯、油胺和正十二硫醇按体积比1:1:1组成的混合溶液中，置于加热装置的反应容器中，搅拌、抽真空，升温至100℃，获得阳离子前驱体溶液；将硒粉、油胺和正十二硫醇按照摩尔比1:2.1:1.3比例，搅拌混合，获得Se前驱体；在惰性气体氛围下，将阳离子前驱体升温至170℃，按照CuI与Se摩尔比1:1比例注入Se前驱体，保温80分钟，然后升温至235℃，保温80分钟，待保温结束后，冷却至室温，向反应溶液中加入正己烷和乙醇，并进行离心，使用甲苯重新分散，获得摩尔浓度为0.006的CuInSe2/CuInS2(Cu/In＝1:4)核壳结构量子点溶液。量子点平均尺寸约为3.0nm，发射波长为801nm，其元素比例为：Cu:In:Se:S＝1:1.97:2.22:2.18。
对比例1
将CuI和In(OAc)3按照摩尔比1:1混合，加入由十八烯、油胺和正十二硫醇按体积比1:1:1组成的混合溶液中，置于加热装置的反应容器中，搅拌、抽真空，升温至100℃，获得阳离子前驱体溶液；将硒粉、油胺和正十二硫醇按照摩尔比1:2.1:1.3比例，搅拌混合，获得Se前驱体；在惰性气体氛围下，将阳离子前驱体升温至170℃，按照CuI与Se摩尔比1:2比例注入Se前驱体，保温80分钟，然后冷却至室温，向反应溶液中加入正己烷和乙醇，并进行离心，然后使用甲苯重新分散，获得摩尔浓度为0.006的CuInSe2核心量子点溶液。量子点平均尺寸约为3.1nm，发射波长为847nm，其元素比例为：Cu:In:Se＝1:1.13:3.64。
对比说明：尺寸虽与元素比例1:4的尺寸接近，但结构上有差异，也无法达到本申请的效果。
通过分步调控反应温度分别实现核心形成和壳层生长，即首先在较低温度(低于170℃)下制备CuInSe2核心，然后升温至较高温度(大于220℃)，使CuInS2壳层在核心上原位生长，其中硫前驱体来源于硫醇在高温(大于220℃)下分解。制备的核壳量子点具有准Ⅱ型核壳结构，有利于载流子在核心与壳层之间分离。
对比例2
将CuI和In(OAc)3按照摩尔比1:1混合，加入由十八烯、油胺和正十二硫醇按体积比1:1:1组成的混合溶液中，置于加热装置的反应容器中，搅拌、抽真空，升温至100℃，获得阳离子前驱体溶液；将硒粉、油胺和正十二硫醇按照摩尔比1:2.1:1.3比例，搅拌混合，获得Se前驱体；在惰性气体氛围下，将阳离子前驱体升温至170℃，按照CuI与Se摩尔比1:1比例注入Se前驱体，保温80分钟，然后升温至235℃，保温80分钟，待保温结束后，冷却至室温，向反应溶液中加入正己烷和乙醇，并进行离心，然后使用甲苯重新分散，获得摩尔浓度为0.006的CuInSe2/CuInS2(Cu/In＝1:1)核壳结构量子点溶液。量子点平均尺寸约为6.6nm，发射波长为893nm,其元素比例为：Cu:In:Se:S＝1:0.79:1.27:0.62。
对比说明：虽然CuInSe2/CuInS2(Cu/In＝1:1)核壳结构量子点与Cu:In＝1:4时具有相同的结构，但产物中较低的In元素含量和较大的尺寸影响了量子点导带与TiO2导带的相对位置，进而影响了光生电荷向TiO2传输层转移，因此也无法达到本申请的效果。
对比例3
将CuI和In(OAc)3按照摩尔比1:5混合，加入由十八烯、油胺和正十二硫醇按体积比1:1:1组成的混合溶液中，置于加热装置的反应容器中，搅拌、抽真空，升温至100℃，获得阳离子前驱体溶液；将硒粉、油胺和正十二硫醇按照摩尔比1:2.1:1.3比例，搅拌混合，获得Se前驱体；在惰性气体氛围下，将阳离子前驱体升温至170℃，按照CuI与Se摩尔比1:1比例注入Se前驱体，保温80分钟，然后升温至235℃，保温80分钟，待保温结束后，冷却至室温，向反应溶液中加入正己烷和乙醇，并进行离心，然后使用甲苯重新分散，获得摩尔浓度为0.006的纳米晶体溶液。纳米晶平均尺寸约为62.31nm。
对比说明：元素比例1:5时，较大的尺寸影响了纳米晶体在TiO2传输层中的负载量，且因为纳米晶不再是准Ⅱ型核壳结构，影响了光生电荷的分离与转移，进而效果也不好。
通过对比例1-3可知：量子点的化学组成、结构以及尺寸均会影响光电化学电池的性能，通过构建便于光生电荷离域的核壳结构以及调整量子点的尺寸和化学组成使其与传输层的能级更加匹配，来获得更好的光电化学性能，即当Cu/In比在本申请限定的情况下，才可获得较好的性能。
实施例4
将乙基纤维素、纳米TiO2粉末和松油醇按照质量比1:2:7比例，搅拌混合，获得TiO2浆料；利用流延法将TiO2浆料涂覆在FTO基底上，然后在500℃退火30分钟，获得TiO2介孔薄膜电极；取4片介孔TiO2薄膜电极，两片为一组作为电极，分别浸入到实施例1-3合成的量子点溶液中，TiO2面对立放置，电极距离为1厘米，然后在电极上施加200V直流电，维持120分钟，从而将量子点沉积到介孔TiO2薄膜上，获得TiO2/[量子点]光电极；将TiO2/[量子点]光电极浸入到0.1摩尔浓度的醋酸锌(Zn(OAc)2)的甲醇溶液中1分钟，使用甲醇冲洗后氮气流干燥，然后再将TiO2/[量子点]光电极浸入到0.1摩尔浓度的硫化钠的甲醇/水(v/v＝1:1)溶液中1分钟，使用甲醇冲洗后氮气流干燥，获得1层ZnS，重复操作，获得具有3层ZnS保护层的TiO2/[量子点]/ZnS光电极；将TiO2/[量子点]/ZnS光电极、铂对电极和Ag/AgCl参比电极浸入到Na2S和Na2SO3混合溶液中，组成三电极体系的光电化学电池。在光照条件下使用CHI660e电化学工作站测试光电化学电池的电化学性能，具体为：在AM 1.5G、100mW/cm2光照条件下，测得电流密度-电压曲线，最终可获得8mA/cm2以上的光电流密度。
Claims (8)
1.一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点合成方法，其特征在于，包括以下合成步骤：
S1、将铜盐和铟盐按照摩尔比1:2~1:4的比例，加入由非配位溶剂和配位溶剂按体积比1:2组成的混合溶液中，置于加热装置的反应容器中，搅拌、抽真空，并升温至80~120℃，获得含有Cu和In离子的阳离子前驱体溶液；
所述非配位溶剂为十八烯，所述配位溶剂为油胺与正十二硫醇按体积比1:1配制；
S2、将硒粉、油胺、正十二硫醇按照摩尔比1:2:1~1:2.8:1.7比例，搅拌混合，获得Se前驱体；
S3、在惰性气体氛围下，将阳离子前驱体溶液升温至140~170℃，按照铜盐与硒粉摩尔比1:0.6~1:2比例注入Se前驱体，保温30~90 分钟，然后升温至210~240℃，保温30~90分钟，待保温结束后冷却至室温，使用正己烷和乙醇的混合溶液洗涤量子点，使用非极性溶剂重新分散，获得0.005~0.01摩尔浓度的不同尺寸、形貌的CuInSe2/CuInS2核壳结构量子点溶液。
2.根据权利要求1所述的一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点合成方法，其特征在于，所述铜盐为碘化铜、溴化亚铜、氯化亚铜或醋酸亚铜中的任意一种。
3.根据权利要求1所述的一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点合成方法，其特征在于，所述铟盐为氯化铟、溴化铟、碘化铟、醋酸铟及其水合物中的任意一种。
4.根据权利要求1所述的一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点合成方法，其特征在于，所述非极性溶剂为甲苯、正己烷或二氯甲烷中的一种。
5.一种尺寸、化学组分可调的CuInSe2/CuInS2核壳结构量子点的光电化学电池，其特征在于，光电化学电池中光阳极所需的CuInSe2/CuInS2核壳结构量子点采用权利要求1中方法合成得到。
6.根据权利要求5所述的光电化学电池，其特征在于，所述光阳极包括以下制备步骤：
X1、将乙基纤维素、纳米TiO2粉末和松油醇按照质量比1:1:4~1:3.5:8比例，搅拌混合，获得TiO2浆料；
X2、使用流延法将TiO2浆料涂覆在掺氟氧化锡透明导电玻璃基底上，干燥后在450~550℃退火20~40分钟，获得介孔TiO2薄膜电极；
X3、使用电泳沉积法将0.005~0.01摩尔浓度的不同尺寸、化学组分的CuInSe2/CuInS2核壳结构量子点溶液沉积到介孔TiO2薄膜电极上，获得光电化学电池光阳极。
7.根据权利要求6所述的光电化学电池，其特征在于，所述光电化学电池的制备方法如下：
Y1、使用连续离子层吸附和反应方法在权利要求6制备得到的光阳极表面包覆ZnS保护层；
Y2、将带有ZnS保护层的光阳极、对电极、参比电极浸入到电解液中，获得光电化学电池。
8.根据权利要求7所述的光电化学电池，其特征在于，所述电解液为硫化钠和亚硫酸钠混合溶液、氢氧化钠溶液或硫酸钠溶液中的一种。
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