CN106115772A - 一种调控SnS和SnS2形貌和结构转换的简易方法 - Google Patents
一种调控SnS和SnS2形貌和结构转换的简易方法 Download PDFInfo
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- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 8
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- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000000376 reactant Substances 0.000 claims abstract description 5
- 235000011150 stannous chloride Nutrition 0.000 claims abstract 4
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- 238000003760 magnetic stirring Methods 0.000 claims description 2
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims 1
- PNOXNTGLSKTMQO-UHFFFAOYSA-L diacetyloxytin Chemical compound CC(=O)O[Sn]OC(C)=O PNOXNTGLSKTMQO-UHFFFAOYSA-L 0.000 claims 1
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- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims 1
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- 230000001105 regulatory effect Effects 0.000 abstract 1
- DZXKSFDSPBRJPS-UHFFFAOYSA-N tin(2+);sulfide Chemical compound [S-2].[Sn+2] DZXKSFDSPBRJPS-UHFFFAOYSA-N 0.000 description 28
- 239000000047 product Substances 0.000 description 12
- 229910052744 lithium Inorganic materials 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
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- 239000007789 gas Substances 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- -1 transition metal sulfide Chemical class 0.000 description 2
- OKIIEJOIXGHUKX-UHFFFAOYSA-L Cadmium iodide Inorganic materials [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 description 1
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
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- 238000004146 energy storage Methods 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
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- 238000001027 hydrothermal synthesis Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- 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
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- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0324—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIVBVI or AIIBIVCVI chalcogenide compounds, e.g. Pb Sn Te
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Abstract
本发明公开了一种方法，可以在仅调节前驱体SnCl2·2H2O和C2H5NS的摩尔比例且保持其它条件（反应温度、反应时间、溶剂油胺的量）不变的情况下，分别制备出纯相的SnS2六角形纳米片和SnS长方形纳米片，实现产物可控。在反应物前驱体SnCl2·2H2O和C2H5NS分别为0.48mmol和4.6mmol，油胺为8ml，反应温度为280℃，反应时间为30分钟的条件下生成SnS2六角形纳米片结构；在反应物前驱体SnCl2·2H2O和C2H5NS分别为1.44mmol和0.58mmol，油胺、反应温度和反应时间保持不变的条件下生成SnS长方形纳米片结构。本发明的优点在于：在同时需要SnS和SnS2两种材料时，不需要更换原材料仅通过调节其摩尔比例就可以获得。且采用湿化学法，原材料均为地球丰富资源，方法简单易操作且制备成本较低。
Description
技术领域
本发明涉及一种可作为薄膜型太阳能电池吸收层的IV-VI族半导体纳米片的制备工艺，还涉及到一种相关材料的结构和形貌控制的方法，以及一种在相同前驱体条件下自由控制产物类型的方法。
背景技术
金属硫化物作为一类典型的半导体材料，尤其是后过渡金属硫化物，在非线性光学、电子学、发光、催化、能量储存和转换等方面有广泛的应用．锡的硫化物包括SnS，Sn2S3，Sn3S4，Sn4S5和SnS2．SnS和SnS2是目前研究较多的一种．硫化亚锡(SnS)是一种重要的半导体材料，其光学直接带隙和间接带隙宽度分别为1.2~1.5 eV和1.0~1.1 eV，与太阳辐射有很好的光谱匹配，因而非常适合作为太阳能电池中的光吸收层，另外在电致发光显示器的近红外探测器和光电压器件中也有很好的应用。
二硫化锡(SnS2)是CdI2结构，具有六角形的结构，硫原子紧密堆积形成两个层，锡离子夹在两层中间形成八面体结构。禁带宽度大约为2.35eV，所以可用作太阳能电池材料，也可应用为全息记录系统和电转换系统，同时，人们普遍认为SnS2 与锂离子的反应与SnO2相似：在首次放电(嵌锂) 过程中，SnS2 首先同锂离子反应分解为Sn和Li2S，分解得到的Sn随后继续同锂离子反应，生成Li-Sn合金，再进行可逆的脱嵌锂反应。Li2S的作用是作为一个非活性的缓冲相，形成非活性Li2S/活性Sn体系，缓解Sn在脱嵌锂过程中的体积膨胀。因此也可以作为锂离子电池取代石墨电极的阴极材料。
纳米薄片晶体以其独特的结构具有许多奇异的物理化学和电学性能，具有重要的科学研究意义和广泛的应用前景，其研究引起了极大的关注。SnS2纳米薄片晶体，结果显示SnS2纳米薄片晶体电化学贮锂容量可以达到645 mAh/g，并具有稳定的循环性能。Kim等用SnCl4与硫或硫脲的水热反应合成了SnS2纳米片，研究发现所合成SnS2纳米片的电化学贮锂初始可逆容量为450～520mAh/g，50次循环以后没有明显的容量降低。上述研究显示了SnS2纳米薄片晶体作为锂离子电池负极材料具有良好的应用前景。
在同一反应条件下，仅通过调节前驱体比例实现产物可控，保持相对较纯的物相，这对SnS2材料和SnS材料的合成机理和材料性质也是一种补充。同时，采用湿化学法制SnS和SnS2纳米薄片晶体，工艺简单，成本较低，不需要昂贵的高真空设备，且原材料的利用率非常高，不失为制备SnS和SnS2材料的一种最佳方法。
发明内容
本发明的目的是提供一种制备方法，可以在仅调节前驱体SnCl2·2H2O和C2H5NS的摩尔比例且保持其它条件（反应温度、反应时间、溶剂油胺的量）不变的情况下，分别制备出纯相的SnS2六角形纳米片和SnS长方形纳米片。这一制备方法相对简单且易操作，原料来源广泛价格低廉且皆为地球的大量元素，所合成的SnS和SnS2材料都是太阳能电池中很重要的吸收层材料。
一种调控SnS长方形纳米片和SnS2六角形纳米片形貌和结构转换的简易方法，其特征在于有如下控制方法和反应过程：
a．在磁力搅拌下，将反应前躯体0.48mmol-1.44mmol SnCl2·2H2O和4.6mmol-0.58mmol C2H5NS加入100ml的四颈烧瓶中，再加入8ml油胺，将烧瓶固定在恒温磁力搅拌器上，并以550转/分钟的转速使转子保持转动；
b．在惰性气体保护下，将步骤a的反应体系在70-80ºC时保持20-30分钟后升温至170-180ºC保持20-30分钟，再升温至280-300ºC保持20-30分钟后降至室温；
c．用甲苯和无水乙醇作为清洗剂将产物用离心机离心清洗三遍，离心机的转速设定为12000转/分钟，收集下层沉淀物，即得六角形SnS2或长方形SnS纳米片。
本发明的优点在于：在同时需要SnS和SnS2两种材料时，不需要更换原材料仅通过调节其摩尔比例就可以获得。且采用湿化学法，方法简单易操作，原材料均为地球丰富资源，制备成本较低。
附图说明
下面结合附图对本发明作进一步详细说明。
图1是本发明的SnS2六角形纳米片的XRD图谱。
图2是本发明的SnS2六角形纳米片的EDS扫描图谱。
图3是本发明的SnS2六角形纳米片的SEM图。
图4是本发明的SnS长方形纳米片的XRD图谱。
图5是本发明的SnS长方形纳米片的EDS扫描图谱。
图6是本发明的SnS长方形纳米片的SEM图。
具体实施方式
下面给出本发明的较佳实施例，使能更好地理解本发明的过程。
实施例1
依次将磁子，反应前驱体0.48mmol SnCl2·2H2O、4.6mmol C2H5NS和8ml油胺加入到100ml的四颈烧瓶中，将烧瓶固定在恒温磁力搅拌器上，并以550转/分钟的转速使转子保持转动，装上热电偶，温度计，冷凝管，通入Ar气且气流稍大，在70ºC时保持30分钟，减小气流后升温至180ºC保持30分钟，再升温至280ºC保持30分钟后降至室温，用甲苯和无水乙醇作为清洗剂将产物用离心机离心清洗三遍，离心机的转速设定为12000转/分钟，收集下层沉淀物，即得SnS2六角形纳米片。
实施例2
再用反应物前驱体SnCl2·2H2O和C2H5NS分别为1.44mmol和0.58mmol，依次将磁子、反应前驱体和油胺加入到100ml的四颈烧瓶中，将烧瓶固定在恒温磁力搅拌器上，并以550转/分钟的转速使转子保持转动，装上热电偶，温度计，冷凝管，通入Ar气且气流稍大，在70ºC时保持30分钟，减小气流后升温至180ºC保持30分钟，再升温至280ºC保持30分钟后降至室温，用甲苯和无水乙醇作为清洗剂将产物用离心机离心清洗三遍，离心机的转速设定为12000转/分钟，收集下层沉淀物，得到的产物是SnS长方形纳米片。
有关本发明的仪器测试所得附图的解释说明
图1中标注的衍射峰(001)、(100)、(002)、(101)、(102)、(003)、(110)、(111)、(103)、(004)、(113)分别对应衍射角14.92º、28.42º、30.14º、31.99 º、41.55 º、46.12 º、49.89º、52.22 º、54.98 º、62.93 º、70.34 º，与SnS2的标准PDF卡片JCPDS#22-0951匹配较好。其次，如表1所示，通过EDS能谱分析数据可得，产物中Sn元素和S元素的摩尔比例为33.16：66.84，基本接近1：2。再由图2中产物的能谱图可看出，除Sn和S的峰位外没有其它杂峰。由此可得出产物是纯相的SnS2。
图3是产物SnS2的SEM图，可以清晰的看出产物SnS2的形貌是六角形片状结构，且尺寸较为均匀。
图4中标注的衍射峰(110)、(120)、(101)、(111)、(131)、(210)、(002)、(211)、(151)、(061)、(042)、(212)、(080)分别对应的衍射角为22º、26º、30.36º、31.82º、38.96º、42.52º、45.34º、48.72º、51.24º、54.18º、56.48º、64.14º、66.58º，与SnS的标准PDF卡片JCPDS#39-0354的衍射峰角度匹配较好。通过能谱仪测试其元素组分，由图5中产物的能谱图可看出，除Sn和S的峰位外没有其它杂峰。再如表2所示，Sn：S=51.20：48.80，组分比例接近1：1，因此可以认为产物是纯相的SnS。
图6是产物SnS的SEM图，可以清晰的看出产物SnS的形貌是长方形状结构，结晶性较好且没有其它杂相。
Claims (3)
1.一种调控SnS长方形纳米片和SnS2六角形纳米片形貌和结构转换的简易方法，其特征在于有如下控制方法和反应过程：
a．在磁力搅拌下，将反应前躯体0.48mmol-1.44mmol SnCl2·2H2O和4.6mmol-0.58mmolC2H5NS加入100ml的四颈烧瓶中，再加入8ml油胺，将烧瓶固定在恒温磁力搅拌器上，并以550转/分钟的转速使转子保持转动；
b．在惰性气体保护下，将步骤a的反应体系在70-80ºC时保持20-30分钟后升温至170-180ºC保持20-30分钟，再升温至280-300ºC保持20-30分钟后降至室温；
c．用甲苯和无水乙醇作为清洗剂将产物用离心机离心清洗三遍，离心机的转速设定为12000转/分钟，收集下层沉淀物，即得六角形SnS2或长方形SnS纳米片。
2.根据权利1要求所述的一种调控SnS长方形纳米片和SnS2六角形纳米片形貌和结构转换的简易方法，其特征在于：所述的反应物前驱体氯化亚锡可以用醋酸亚锡代替。
3.根据权利1要求所述的一种调控SnS长方形纳米片和SnS2六角形纳米片形貌和结构转换的简易方法，其特征在于：所述的反应物前驱体硫代乙酰胺可以用硫脲代替。
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