CN107098377A - 一种暴露高能（001）晶面超薄CdS纳米带的制备方法 - Google Patents
一种暴露高能（001）晶面超薄CdS纳米带的制备方法 Download PDFInfo
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Abstract
本发明公开了一种暴露(001)晶面的超薄CdS纳米带的制备方法，制备过程如下：(1)将无机镉盐，去离子水，二亚乙基三胺和硫粉混均，在搅拌下进行溶剂热反应；得溶剂热产物；(2)将溶剂热产物分散于去离子水中，超声剥离，制得暴露(001)晶面的超薄CdS纳米带。本发明具有如下技术效果：1.制备出CdS纳米带主要暴露(001)高能晶面，具有电子定向传输且传输速率快、特殊的光学性能等特点；2.CdS纳米带厚度很薄，可增大了比表面积，大大缩短了光生电荷传输到催化剂表面的迁移距离，有效抑制了光生电子和空穴对发生体相复合几率；3.在波长大于420nm可见光辐照下，并不负载任何助催化剂的情况下，CdS纳米带的产氢效率高达59.7mmol/h/g催化剂，并且光照50h，催化活性无明显降低；4.本发明具有操作简单、反应温度低、重复性好等优点。
Description
技术领域
本发明属于光催化技术领域，具体涉及一种暴露高能(001)晶面超薄CdS纳米带的制备方法。
背景技术
CdS是一种禁带宽度窄、具有优异的可见光响应特性的半导体光催化材料，具有六方纤锌矿和立方闪锌矿两种晶体结构。由于其独特的光学、电学及催化特性，被广泛应用于太阳能电池、发光二极管、激光器以及催化领域。
自2001年王中林教授报道ZnO纳米带以来，一维纳米带材料由于具有电子定向传输、较大的纵横比及各向异性等特性，被广泛关注。目前CdS纳米带的制备方法常用化学气相沉积法(Nanotechnology,2011,22(13):135702；Advanced Materials,2010,22(29):3161-3165；ACS nano,2012,6(6):5283-5290)，该方法反应温度高，制备出的CdS纳米带厚度较厚约为30-200nm,宽度为数百纳米不等，长约几微米。CdS纳米带厚度、宽度过大，一方面导致催化材料的比表面积较小，另一方面将会增大光生电荷体相传输距离，增加光生电荷复合几率。这两方面都制约了CdS纳米带光催化效率的提升。
光催化材料的活性除了与晶体结构、尺寸、形貌等有关，还与晶体的表面性质有关。自2008年Yang等人成功制备出TiO2暴露高能(001)晶面以来，可控合成暴露特定晶面的半导体材料引起了众研究学者的兴趣。一般来说，根据总表面能最底优化原则，具有高表面能晶面在晶体生长过程中越易消失。因此，制备暴露高活性晶面的半导体材料仍然是一大挑战。(001)晶面是六方纤锌矿CdS半导体各晶面中表面能最高的(Nanotechnology,2008,19:225601)。目前，已有报道采用水热法合成出暴露(001)晶面的CdS纳米树叶结构(Journal of Materials Chemistry,2012,22(45):23815-23820.)、由纳米片组成的花状结构(Materials Research Bulletin,2012,47(11):3070-3077.)和采用回流法制备CdS纳米片(CN 104085915 B)。该些合成方法，反应温度均高于180℃，较高的反应温度，对设备要求高、增加能耗，不利于大规模工业化生产。因此如何在低温下制备厚度薄、暴露高能(001)晶面的CdS纳米带仍是一个大难题。
发明内容
本发明的目的在于提供一种过程简单，可得到厚度薄、主要暴露(001)高能晶面CdS纳米带的制备方法。
本发明的技术方案是：一种暴露(001)晶面的超薄CdS纳米带的制备方法，制备过程如下：
(1)将无机镉盐，去离子水，二亚乙基三胺和硫粉混均，所述无机镉盐与二亚乙基三胺物质的量之比为1：100～600，去离子水与二亚乙基三胺物质的量之比为1：200～1000，硫粉与二亚乙基三胺物质的量之比为1：30～200；在搅拌下进行溶剂热反应；得溶剂热产物；
(2)将溶剂热产物分散于去离子水中，超声剥离，制得暴露(001)晶面的超薄CdS纳米带。
所述无机镉盐是Cd(NO3)2、CdCl2、Cd(CH3COO)2、Cd(NO3)2·4H2O、CdCl2·2.5H2O或Cd(CH3COO)2·2H2O之任一种或二种以上之混合物；所述溶剂热反应温度为60～120℃，反应时间为24～72h，搅拌速率为30～600转/分钟。
所述暴露(001)晶面的超薄CdS纳米带的厚度为1～4nm，宽度为5～20nm，长度为80～120nm。
所述超声剥离过程溶液的PH值为8～10.5，超声剥离时间为1～10h。
本发明具有如下技术效果：1.制备出CdS纳米带主要暴露(001)高能晶面，CdS纳米带的厚度仅约1～4nm；一维结构的CdS纳米带，相比于零维、二维和三维结构，具有电子定向传输且传输速率快、特殊的光学性能等特点；2.CdS纳米带厚度很薄：一方面可增大了比表面积，提供了更多反应活性位；另一方面大大缩短了光生电荷传输到催化剂表面的迁移距离，有效抑制了光生电子和空穴对发生体相复合几率；此外，还可暴露出更多的高活性(001)晶面，有利用于CdS纳米带光催化活性的提高；3.在波长大于420nm可见光辐照下，并在不负载任何助催化剂的情况下，CdS纳米带的产氢效率高达59.7mmol/h/g催化剂，并且光照50h，催化活性无明显降低，表明该催化剂具有优异的光解水产氢活性及稳定性；4.本发明具有操作简单、反应温度低、重复性好等优点。
附图说明
图1为实施例2制备的超薄暴露高能(001)晶面CdS纳米带的XRD图及纤锌矿型CdS半导体标准PDF卡片(41-1049)。
图2为实施例2制备的超薄暴露高能(001)晶面CdS纳米带透射电镜(TEM)图。
图3为实施例2制备的超薄暴露高能(001)晶面CdS纳米带透射电镜(TEM)图。
图4为实施例2制备的超薄暴露高能(001)晶面CdS纳米带快速傅立变换(FFT)及反傅立叶变换图。
图5为实施例2制备的超薄暴露高能(001)晶面CdS纳米带快速傅立变换(FFT)及反傅立叶变换图。
图6为实施例2制备的超薄暴露高能(001)晶面CdS纳米带的氮气等温吸附脱附曲线图。
图7为对比例制备的CdS纳米带透射电镜(TEM)图。
图8为实施例2制备的超薄暴露高能(001)晶面CdS纳米带在波长大于420nm可见光辐照下的光解水产氢时间关系曲线。
具体实施方式
以下通过具体的实施例对发明的技术方案作进一步描述。
实施例1：
将10.0mmol Cd(NO3)2，33.4mmol S粉，5.0mmol去离子，1000.0mmol二亚乙基三胺充分搅拌分散均匀，随后置于120ml聚四氟乙烯反应釜中，在反应温度60℃、搅拌速率600转/分钟的条件下，溶剂热反应72h。自然冷却至室温后，离心收集溶剂热产物。然后将产物分散于去离子水中，调节溶液PH值为8，超声剥离10h，得到超薄暴露高能(001)晶面CdS纳米带。通过原子力显微镜测得CdS纳米带的厚度约1nm，宽约5nm，长约100nm。
实施例2：
将1.7mmol CdCl2·2.5H2O，15.0mmol S粉，1.0mmol去离子，1000.0mmol二亚乙基三胺充分搅拌分散均匀，随后置于120ml聚四氟乙烯反应釜中，在反应温度80℃、搅拌速率300转/分钟的条件下，溶剂热反应48h。自然冷却至室温后，离心收集溶剂热产物。然后将产物分散于去离子水中，调节溶液pH值为9.0，超声剥离2h，得到超薄暴露高能(001)晶面CdS纳米带。通过原子力显微镜测得CdS纳米带的厚度约1nm，宽约10nm，长约100nm。
如图1所示，CdS半导体标准PDF卡片的(002)和(101)晶面衍射峰强度差别不大，而采用本发明方法所制备的CdS纳米带的(001)晶面衍射峰强度远高于(101)晶面，表明CdS纳米带可能择优暴露(001)晶面。
如图2所示，所制备的纳米带宽约约10nm，长约100nm。
如图3所示，高分辨TEM图晶格条纹进一步表明，CdS纳米带的宽度约10nm。为了更好地确定纳米带的暴露晶面，选取图中虚线方框区域进行快速傅立变换(FFT)及反傅立叶变换得到图4及图5。
如图4所示，明亮的晶格点阵表明该CdS纳米带为单晶，其各晶面夹角均约为60°，分别对应于(100)，(010)及晶面，表明CdS纳米带择优暴露(001)晶面。
如图5所示，晶格条纹0.36nm可分别归属于(100)，(010)及晶面，且其晶面夹角均约为120°，进一步证实CdS纳米带择优暴露(001)晶面。
如图6所示，根据BET公式，计算可得比表面积为105.0m2/g。
如图7所示，在未加去离子水和搅拌的条件下，制备的CdS形貌为纳米片(对比例)。对比实施例2及对比例，可以推断，去离子水及搅拌在纳米带的形成过程起到了关键作用。
如图8所示，催化剂用量为2mg，Na2S+Na2SO3为牺牲剂。产氢速率高达59.7mmol/h/g催化剂，并且光照50h，催化活性无明显降低，表明该催化剂具有优异的光解水产氢活性及稳定性。
实施例3：
将3.0mmol CdCl2，1.0mmol Cd(CH3COO)2、5.0mmol S粉，3.0mmol去离子，1000.0mmol二亚乙基三胺充分搅拌分散均匀，随后置于120ml聚四氟乙烯反应釜中，在反应温度100℃、搅拌速率30转/分钟的条件下，溶剂热反应72h。自然冷却至室温后，离心收集溶剂热产物。然后将产物分散于去离子水中，调节溶液pH值为10.5，超声剥离6h，得到超薄暴露高能(001)晶面CdS纳米带。通过原子力显微镜测得纳米带的厚度约3nm，宽约15nm，长约100nm。
实施例4：
将1.0mmol Cd(NO3)2·4H2O，1.0mmol Cd(CH3COO)2·2H2O，10.0mmol S粉，5.0mmol去离子，1000.0mmol二亚乙基三胺充分搅拌分散均匀，随后置于120ml聚四氟乙烯反应釜中，在反应温度120℃、搅拌速率200转/分钟的条件下，溶剂热反应36h。自然冷却至室温后，离心收集溶剂热产物。然后将产物分散于去离子水中，调节溶液pH值为10.0，超声剥离1h，得到超薄暴露高能(001)晶面CdS纳米带。通过原子力显微镜测得纳米带的厚度约4nm，宽约20nm，长约100nm。
对比例：
将1.7mmol CdCl2·2.5H2O，15.0mmol S粉，1000.0mmol二亚乙基三胺充分搅拌分散均匀，随后置于120ml聚四氟乙烯反应釜中，在反应温度80℃、不搅拌(搅拌速率0转/分钟)的条件下，溶剂热反应48h。自然冷却至室温后，离心收集溶剂热产物。然后将产物分散于去离子水中，调节溶液pH值为9.0，超声剥离2h，得到产物为CdS纳米片。
在相同条件下，对比例所制备的CdS纳米片光解水产氢速率约36.0mmol/h/g催化剂，仅约为CdS纳米带产氢速率(59.7mmol/h/g)的60％。表明本发明方法制备的CdS纳米具有良好的光催化活性，本发明方法具有明显优势。
Claims (4)
1.一种暴露(001)晶面的超薄CdS纳米带的制备方法，其特征在于：制备过程如下：
(1)将无机镉盐，去离子水，二亚乙基三胺和硫粉混均，所述无机镉盐与二亚乙基三胺物质的量之比为1：100～600，去离子水与二亚乙基三胺物质的量之比为1：200～1000，硫粉与二亚乙基三胺物质的量之比为1：30～200；在搅拌下进行溶剂热反应；得溶剂热产物；
(2)将溶剂热产物分散于去离子水中，超声剥离，制得暴露(001)晶面的超薄CdS纳米带。
2.根据权利要求1所述的一种暴露(001)晶面的超薄CdS纳米带的制备方法，其特征在于：所述无机镉盐是Cd(NO3)2、CdCl2、Cd(CH3COO)2、Cd(NO3)2·4H2O、CdCl2·2.5H2O或Cd(CH3COO)2·2H2O之任一种或二种以上之混合物；所述溶剂热反应温度为60～120℃，反应时间为24～72h，搅拌速率为30～600转/分钟。
3.根据权利要求1所述的一种暴露(001)晶面的超薄CdS纳米带的制备方法，其特征在于：所述暴露(001)晶面的超薄CdS纳米带的厚度为1～4nm，宽度为5～20nm，长度为80～120nm。
4.根据权利要求1所述一种暴露(001)晶面的超薄CdS纳米带的制备方法，其特征在于：所述超声剥离过程溶液的PH值为8～10.5，超声剥离时间为1～10h。
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| CN106698500A (zh) * | 2015-11-16 | 2017-05-24 | 天津大学 | 一种硫化镉超薄纳米片状材料的制备方法及其应用 |
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