CN110171842B - 一种混合价态锡基氧化物半导体材料的制备方法及应用 - Google Patents
一种混合价态锡基氧化物半导体材料的制备方法及应用 Download PDFInfo
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 30
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 239000002159 nanocrystal Substances 0.000 claims abstract description 9
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 230000005693 optoelectronics Effects 0.000 claims description 9
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 5
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 4
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 4
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- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 4
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
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- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 4
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- 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 description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- PNOXNTGLSKTMQO-UHFFFAOYSA-L diacetyloxytin Chemical compound CC(=O)O[Sn]OC(C)=O PNOXNTGLSKTMQO-UHFFFAOYSA-L 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000001119 stannous chloride Substances 0.000 claims description 2
- 235000011150 stannous chloride Nutrition 0.000 claims description 2
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical group F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 claims description 2
- 229960002799 stannous fluoride Drugs 0.000 claims description 2
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 2
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 claims description 2
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 2
- YUOWTJMRMWQJDA-UHFFFAOYSA-J tin(iv) fluoride Chemical group [F-].[F-].[F-].[F-].[Sn+4] YUOWTJMRMWQJDA-UHFFFAOYSA-J 0.000 claims description 2
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 claims description 2
- YQMWDQQWGKVOSQ-UHFFFAOYSA-N trinitrooxystannyl nitrate Chemical compound [Sn+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YQMWDQQWGKVOSQ-UHFFFAOYSA-N 0.000 claims description 2
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- XDXWNHPWWKGTKO-UHFFFAOYSA-N 207739-72-8 Chemical compound C1=CC(OC)=CC=C1N(C=1C=C2C3(C4=CC(=CC=C4C2=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC(=CC=C1C1=CC=C(C=C13)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 XDXWNHPWWKGTKO-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- -1 but not limited to Chemical class 0.000 description 2
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
本发明公开了一种混合价态锡基氧化物半导体材料的制备方法及应用,将四价锡盐和二价锡盐按照预设摩尔比例溶于水中,加入沉淀剂进行沉淀;进行离心分离和去离子水清洗;将产物置于水热反应装置中,加入矿化剂,并加水分散经水热反应得到锡基氧化物半导体材料纳米晶。所得的锡基氧化物半导体材料可以作为太阳能电池、发光二极管、光电探测器和场效应管等光电器件中的载流子传输层或者缓冲层,由于混合价态锡基氧化物组分可调,从而具有载流子迁移率、能带结构、透光率、导电性等半导体材料性能可调的优点,同时本发明制备方法工艺简单,反应条件温和,在光电器件领域对器件的灵活设计与性能优化有着明显的促进作用,有很大的工业化应用前景。
Description
技术领域
本发明属于半导体材料制备技术领域,更具体地,涉及一种混合价态锡基氧化物半导体材料的制备方法及应用。
背景技术
半导体产业被认为是二十一世纪全球经济发展的战略性行业之一,其市场价值不断增加,全球总产值早已达到数千亿美元。它涉及到了生活中的方方面面,具体包括光伏发电产业、照明产业、显示产业和激光产业。据统计,2016年仅LED光电产业产值就达5260多亿元人民币,较2015年增长22.8%。中国LED产业的从业人员已达数十万人。截至2016年底,我国光伏制造业总产值超过3360亿元,光伏发电装机容量突破34GW。多晶硅产量约为19.4万吨,占全球总产量的33%;2015年,硅片产量约为68亿片,电池片产量约为28GW,占全球总产量的60%,保持了全球太阳能电池生产第一大国的地位。光伏发电作为使用区域限制少、设备相对简单易安装的发电方式,近年来在我国得到了快速发展。
光电产业以光电技术为核心,光电器件则是光电技术的具体展现。光电器件能把光和电这两种物理量联系起来,使光和电互相转化。光电器件的发展离不开半导体材料的发展,氧化物半导体以其自身优异的性能在光电子器件中被广泛使用。现如今常被人们使用的氧化物半导体材料有TiO2,ZnO,SnO2,ITO,FTO等。例如,在钙钛矿太阳能电池、染料敏化太阳能电池中,常常使用TiO2,ZnO,SnO2作为电子收集层,用来透过太阳光以及收集从本征层扩散过来的电子;在硅基太阳能电池和薄膜太阳能电池中,往往使用FTO作为导电基板;在GaN基白光LED中,如果用ITO替代Ni/Au作为P型电极芯片的亮度要比采用通用电极的芯片高20%-30%。
由此可见,在不同类型的光电器件的应用中,为了满足不同的需求以及实现不同材料之间的良好匹配,需要使用不同类型的氧化物半导体材料。为了进一步满足各种器件的不同需求,提升光电器件设计制作的灵活性,开发出新的性能可调控的半导体材料十分关键。
发明内容
针对现有技术的缺陷或改进需求,本发明提供了一种混合价态锡基氧化物半导体材料的制备方法及应用,其目的在于制备满足不同器件要求的性能可调控的半导体材料。
为实现上述目的,按照本发明的一方面,提供了一种混合价态锡基氧化物的制备方法,该锡基氧化物为Sn4+ xSn2+ yO2- z,可简写为Sn(x+y)Oz,Sn的价态为+4价或者+2价,分子式中x>0,y>0,z>0,且满足2x+y=z。
锡基氧化物半导体材料的制备方法,包括如下步骤:
步骤1:将四价锡盐和二价锡盐按照预设摩尔比例溶于水中,加入沉淀剂进行沉淀;
步骤2:将步骤1的产物进行离心分离和去离子水清洗;
步骤3:将步骤2的产物置于水热反应装置中,加入矿化剂,并加水分散经水热反应得到锡基氧化物半导体材料纳米晶。
优选地,将步骤1的产物进行烘烤,即可以得到干燥后的锡基氧化物半导体材料纳米晶。
优选地,四价锡盐包括但不限于四氟化锡、四氯化锡、硫酸锡、硝酸锡、醋酸锡或所述任意一种盐的水合物。
优选地,二价锡盐包括但不限于氟化亚锡、氯化亚锡、硫酸亚锡、硝酸亚锡、醋酸亚锡或所述任意一种盐的水合物。
优选地,四价锡盐和二价锡盐的摩尔比例为x:y,通过改变所述摩尔比例可以合成不同的锡基氧化物Sn(x+y)Oz,其中,x>0,y>0,z>0,且满足2x+y=z。
优选地,沉淀剂为碱性水溶性化合物,包括但不限于氨水、氢氧化钾、氢氧化锂、氢氧化钠、碳酸钠、碳酸氢钠、氢氧化钙、氢氧化钡。
优选地,矿物剂为碱性水溶性化合物,包括但不限于氨水、氢氧化钾、氢氧化锂、氢氧化钠、碳酸钠、碳酸氢钠、氢氧化钙、氢氧化钡。
按照本发明的另一方面,提供了一种如上述的制备方法制备的混合价态锡基氧化物的应用,包括用于光电器件中的载流子传输层或者缓冲层。
优选地,光电器件为太阳能电池、发光二极管、光电探测器和场效应管。
通过本发明所构思的以上技术方案,与现有技术相比,能够取得以下有益效果:
1、本发明提供了一种组分可调的混合价态锡基氧化物半导体材料的制备方法,通过控制不同价态的锡盐比例可以选择性地合成不同的锡基氧化物,不同的锡基氧化物半导体材料的载流子迁移率、能带结构、透光率和导电性都不同,因此可以满足不同类型的光电器件的需求;
2、本发明提供的混合价态锡基氧化物半导体材料的制备方法工艺简单,反应条件温和,设备要求低,成本低廉,具有良好的可加工性能,在光电器件领域对器件的灵活设计与性能优化有着明显的促进作用,有很大的工业化应用前景。
附图说明
图1是本发明实施例1制备的Sn2O3纳米晶的HRTEM图片;
图2是本发明实施例1制备的Sn2O3薄膜的表面SEM图片;
图3是本发明实施例2制备的Sn3O4纳米晶的HRTEM图片。
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仅用以解释本发明,并不用于限定本发明。此外,下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间不构成冲突就可以相互组合。
本发明提供了一种混合价态锡基氧化物半导体材料的制备方法,包括以下步骤:
步骤1:将四价锡盐和二价锡盐按照预设摩尔比例溶于水中,加入沉淀剂进行沉淀;
步骤2:将沉淀进行离心分离和去离子水清洗;
步骤3:将步骤2的产物置于水热反应装置中,加入矿化剂,并加水分散经水热反应得到锡基氧化物半导体材料纳米晶。
以下结合附图及具体实施例来进一步阐释本发明提供的二维金属化合物材料的制备方法。
实施例1:Sn2O3的制备,包括以下步骤:
(1)分别称取282mg SnCl2*2H2O溶于10mL去离子水,438mg SnCl4*5H2O溶于10mL去离子水,两者摩尔比例为1:1,磁力搅拌混合均匀;
(2)加入1ml浓氨水,得到沉淀,用去离子水离心洗涤三次,离心条件为:转速8000rpm,时间3mins;
(3)将(2)中洗涤后的沉淀分散于20mL去离子水中,置于水热釜中反应,具体条件为:填充度为80%,升温速率为10℃/min至200℃,保温10h;
(4)将(3)中水热反应产物取出制备得到Sn2O3纳米颗粒分散液。
如图1所示是实施例1制备的Sn2O3纳米晶的HRTEM图片,可以看出颗粒大小均匀,分散较好,通过局部放大,测量得到0.330nm的晶格条纹,对应Sn2O3的(011)晶面,表明样品为Sn2O3。以所得的Sn2O3应用在钙钛矿太阳能电池中,将Sn2O3纳米颗粒分散液旋涂在清洗干净的ITO导电玻璃基板上,得到Sn2O3薄膜,如图2所示为Sn2O3薄膜的表面SEM图片,可以看出薄膜均匀致密,形貌良好,随后在其上旋涂制备卤化物钙钛矿薄膜MAPbI3,接着在钙钛矿薄膜上旋涂Spiro-OMeTAD,最后在Spiro-OMeTAD上蒸镀金电极,完成器件的制备。相关器件表现出了15%的光电转换效率。
实施例2:Sn3O4的制备,包括以下步骤:
(1)分别称取564mg SnCl2*2H2O溶于10mL去离子水,438mg SnCl4*5H2O溶于10mL去离子水,两者摩尔比例为2:1,磁力搅拌混合均匀;
(2)加入1ml浓氨水,得到沉淀,用去离子水离心洗涤三次,离心条件为:转速8000rpm,时间3mins;
(3)将(2)中洗涤后的沉淀分散于20mL去离子水中,置于水热釜中反应,具体条件为:填充度为80%,升温速率为10℃/min至200℃,保温6h;
(4)将(3)中水热反应产物取出制备得到Sn3O4纳米颗粒分散液。
本领域的技术人员容易理解,以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种光电器件中的电子传输层,其特征在于,所述电子传输层的材料为混合价态锡基氧化物半导体材料,化学式表示为Sn4+ xSn2+ yO2- z,Sn的价态有+4价和+2价,分子式中x>0,y>0,z>0,且满足2x+y=z;且所述电子传输层的制备方法包括如下步骤:
步骤1:将四价锡盐和二价锡盐按照预设摩尔比例溶于水中,加入沉淀剂进行沉淀,其中根据已确定的x和y值来调控所述预设摩尔比例;
步骤2:将步骤1的产物进行离心分离和去离子水清洗;
步骤3:将步骤2的产物置于水热反应装置中,加入矿化剂,并加水分散经水热反应得到所述已确定的x和y值所对应的混合价态锡基氧化物半导体材料纳米颗粒分散液;
步骤4:对步骤3得到的混合价态锡基氧化物半导体材料纳米颗粒分散液直接进行旋涂,制得所需的电子传输层。
2.根据权利要求1所述的一种光电器件中的电子传输层,其特征在于,所述制备方法还包括将所述步骤1的产物进行烘烤,得到干燥后的锡基氧化物半导体材料纳米晶。
3.根据权利要求1所述的一种光电器件中的电子传输层,其特征在于,所述四价锡盐为四氟化锡、四氯化锡、硫酸锡、硝酸锡、醋酸锡或任意一种所述四价锡盐的水合物。
4.根据权利要求1所述的一种光电器件中的电子传输层,其特征在于,所述二价锡盐为氟化亚锡、氯化亚锡、硫酸亚锡、硝酸亚锡、醋酸亚锡或任意一种所述二价锡盐的水合物。
5.根据权利要求1所述的一种光电器件中的电子传输层,其特征在于,所述四价锡盐和所述二价锡盐的摩尔比例为x:y,通过改变所述摩尔比例可以合成不同的锡基氧化物,其中,x>0,y>0。
6.根据权利要求1所述的一种光电器件中的电子传输层,其特征在于,所述沉淀剂为碱性水溶性化合物,包括氨水、氢氧化钾、氢氧化钠、氢氧化锂、碳酸钠、碳酸氢钠、氢氧化钙、氢氧化钡。
7.根据权利要求1所述的一种光电器件中的电子传输层,其特征在于,所述矿化剂为碱性水溶性化合物,包括氨水、氢氧化钾、氢氧化钠、氢氧化锂、碳酸钠、碳酸氢钠、氢氧化钙、氢氧化钡。
8.根据权利要求1至7任一项所述的一种光电器件中的电子传输层,其特征在于,所述光电器件为太阳能电池、发光二极管或光电探测器。
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