CN105551935A - 一种用醋酸锌制备硫化锌光电薄膜的方法 - Google Patents
一种用醋酸锌制备硫化锌光电薄膜的方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 19
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 title claims abstract description 19
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000004246 zinc acetate Substances 0.000 title claims abstract description 9
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- 239000011521 glass Substances 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 19
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 18
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 17
- 239000010409 thin film Substances 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 16
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
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- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
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Abstract
一种用醋酸锌制备硫化锌光电薄膜的方法，属于太阳能电池用薄膜制备技术领域，本发明通过如下步骤得到，首先清洗二氧化锡导电玻璃基片，然后将C6H5Na3O7·2H2O、Zn(CH3COO)2、Na2S2O3·5H2O放入蒸馏水中，用电沉积法在导电玻璃片上得到前驱体薄膜，自然干燥，放入加有水合联氨的管式炉中，使前驱体薄膜样品不与水合联氨接触，其中水合联氨中加有升华硫粉，在密闭管式炉内加热，使前驱体薄膜硫化，最后取出样品进行干燥，得到硫化锌光电薄膜。本发明不需要高真空条件，对仪器设备要求低，生产成本低，生产效率高，易于操作。所得硫化锌光电薄膜有较好的连续性和均匀性，主相为ZnS相，可以实现低成本大规模的工业化生产。
Description
技术领域
本发明属于太阳能电池用薄膜制备技术领域，尤其涉及一种用醋酸锌制备硫化锌光电薄膜的方法。
背景技术
随着社会和经济的发展，我国能源消费总量剧增，能源危机及传统能源对环境造成的污日趋严重，因此开发利用清洁环保能源成为人类面临的重大课题。为了更充分地利用太阳能这种清洁、安全和环保的可再生资源，近年来太阳能电池材料的研究和发展日益受到重视。
在薄膜光伏材料中，ZnS是II-VI族化合物半导体，具有闪锌矿晶体结构，直接跃迁型能带结构，ZnS具有禁带宽(3.5~3.7eV)的优点，其对太阳光基本不吸收，这样可以使更多的高能量光子被传送到电极上，提高电池光电转换效率。此外，ZnS不仅对人体无毒无害，而且ZnS薄膜在窗口层和吸收层之间起结构缓冲、减小晶格适配度的作用，还能与吸收层结合好，电池转换效率高，在所有太能电池缓冲层材料中，无毒无害ZnS是有毒的CdS的理想替代者。因此，ZnS薄膜的制备和特性研究必将对太阳能电器件的发展应用起到积极的推动作用。
目前，硫化锌多晶制备技术很多，从合成反应类型上可分为湿法和干法；从合成的技术特点上可分为化学气相沉积法、气相反应法、液相合成法、元素直接反应法、化学浴沉积法、电化学沉积法、分子束外延法和光化学沉积法等。
如前面所述方法一样，其它方法也有不同的缺陷。与本发明相关的还有如下文献：
[1]QiL,MaoG,AoJ,Chemicalbath-depositedZnSthinfilms:preparationandcharacterization,AppliedSurfaceScience254(2008)5711-5714.
主要描述了利用化学水浴沉积的方法制备ZnS薄膜，研究了薄膜厚度和退火温度对其光学性能、晶体的带隙能量和晶粒大小的影响。
[2]BahloulA,NessarkB,ChelaliNE,GroultH,MaugerA,JulienCM,NewcompositecathodematerialforZn/MnO2cellsobtainedbyelectro-depositionofpolybithiopheneonmanganesedioxideparticles.SolidStateIonics204-205(2011)53-60.
主要描述了用磁控溅射的方法制备ZnS薄膜，并对其形貌组织进行了表征。
[3]CuiJ,ZengX,ZhouM,HuC,ZhangW,LuJ,TunableblueandorangeemissionsofZnS:MnthinfilmsdepositedonGaNsubstratesbypulsedlaserdeposition,JournalofLuminescence147(2014)310-5.
主要描述了用喷雾热解法制备ZnS薄膜，该薄膜为多晶的、有方向性的和高光传输性，并研究了其发光性和电致发光性。
[4]LimeiZhou,NanTang,SumeiWu,InfluenceofdepositiontemperatureonZnSthinfilmperformancewithchemicalbathdeposition,Surface&CoatingsTechnology228(2013)S146-S149.主要描述了通过化学浴沉积的方法制备ZnS薄膜，主要研究的是在不同的温度(75℃、80℃、85℃、90℃、95℃)对薄膜的厚度，微观表面形貌，结构和透射率的影响。
[5]ZhaoYangZhong,EouSikCho,SangJikKwon,CharacterizationoftheZnSthinfilmbufferlayerforCu(In,Ga)Se2solarcellsdepositedbychemicalbathdepositionprocesswithdifferentsolutionconcentrations,MaterialsChemistryandPhysics135(2012)287-292.
主要描述了用化学水浴的方法制备太阳能薄膜Cu(In,Ga)Se2的缓冲层ZnS薄膜，并研究了反应物质的浓度对薄膜的厚度、透明度和微观表面形貌的影响。
[6]GayouVL,Salazar-HernandezB,ConstantinoME,AndrésER,DíazT,MacuilRD,StructuralstudiesofZnSthinfilmsgrownonGaAsbyRFmagnetronsputtering,Vacuum,84(2010)1191-4.
主要描述了通过脉冲激光法在GaAs上制备ZnS薄膜，并研究了其组织结构。
发明内容
本发明为了解决现有制备硫化锌光电薄膜存在的问题，发明了一种用醋酸锌制备硫化锌光电薄膜的方法。
本发明采用电沉积后硫化法制备硫化锌薄膜，采用二氧化锡导电玻璃为基片，以Zn(CH3COO)2、Na2S2O3·5H2O为原料，以C6H5Na3O7·2H2O为络合剂，以蒸馏水为溶剂，按固定摩尔比配制电沉积溶液，先采用晶体管恒电位仪在一定电位和时间下制备前驱体薄膜，以水合联氨为还原剂，在水合联氨中加入升华硫粉保证硫气氛，在密闭管式炉内加热，使前驱体薄膜硫化并得到目标产物。
本发明的具体制备方法包括如下顺序的步骤：
a.进行二氧化锡导电玻璃基片的清洗，将大小为20mm×20mm的玻璃基片放入体积比丙酮：蒸馏水=5：1的溶液中，超声波清洗30min；再将基片放入乙醇中，超声波清洗30min；再在蒸馏水中将玻璃基片用超声振荡30min；将上述得到的玻璃基片排放在玻璃皿中送入烘箱中，在100℃下烘干供制膜用。
b.将C6H5Na3O7·2H2O、Zn(CH3COO)2、Na2S2O3·5H2O放入蒸馏水中，获得均匀稳定的电沉积溶液。具体地说，可以将1.0～2.0份C6H5Na3O7·2H2O、4.5～9.0份Zn(CH3COO)2、65.0～130.0份Na2S2O3·5H2O放入2700.0～5400.0份的蒸馏水中，使溶液中的物质溶解。
c.将步骤b所述电沉积溶液倒入三电极装置中，以饱和甘汞电极为参比电极，铂电极为辅助电极，二氧化锡导电玻璃为研究电极，采用晶体管恒电位仪在沉积电位为2V下常温沉积薄膜，沉积时间为30min，得到前驱体薄膜样品。
d.将步骤c所得前驱体薄膜样品置于支架上，在水合联氨中加入升华硫粉，前驱体薄膜样品不与水合联氨接触，将前驱体薄膜和水合联氨放入管式炉中。水合联氨放入为40.0～50.0份，升华硫粉为1.0～2.0份。将管式炉加热至250～400℃之间，保温时间3～9h，然后冷却到室温取出。
e.将步骤d所得物，使其常温自然干燥后，即得到硫化锌薄膜。
本发明不需要高真空条件，对仪器设备要求低，生产成本低，生产效率高，易于操作。所得硫化锌光电薄膜有较好的连续性和均匀性，主相为ZnS相，可以实现低成本大规模的工业化生产。
附图说明
无
具体实施方式
实施例1
a.二氧化锡导电玻璃基片的清洗：如前所述进行清洗玻璃基片，基片大小为20mm×20mm。
b.将1.0份C6H5Na3O7·2H2O、4.5份Zn(CH3COO)2、65.0份Na2S2O3·5H2O放入2700.0份的蒸馏水中，使溶液中的物质溶解。
c.将上述电沉积溶液倒入三电极装置中，以饱和甘汞电极为参比电极，铂电极为辅助电极，二氧化锡导电玻璃为研究电极，采用晶体管恒电位仪在沉积电位为2V下常温沉积薄膜，沉积时间为30min，得到前驱体薄膜样品。
d.将前驱体薄膜样品置于支架上，在水合联氨中加入升华硫粉，前驱体薄膜样品不与水合联氨接触，将前驱体薄膜和水合联氨放入管式炉中。水合联氨放入为40.0份，升华硫粉为1.0份。将管式炉加热至400℃，保温时间3h，然后冷却到室温取出。
e.将步骤d所得物，进行常温自然干燥，得到硫化锌光电薄膜。
Claims (4)
1.一种用醋酸锌制备硫化锌光电薄膜的方法，包括如下顺序的步骤：
a.二氧化锡导电玻璃基片的清洗；
b.将1.0～2.0份C6H5Na3O7·2H2O、4.5～9.0份Zn(CH3COO)2、65.0～130.0份Na2S2O3·5H2O放入2700.0～5400.0份的蒸馏水中，使溶液中的物质溶解；
c.采用电沉积法将步骤b所述溶液在导电玻璃片上沉积得到前驱体薄膜，自然干燥，得到前驱体薄膜样品；
d.将步骤c所得前驱体薄膜样品置于支架上，在水合联氨中加入升华硫粉，前驱体薄膜样品不与水合联氨接触，将前驱体薄膜和水合联氨放入管式炉中；将管式炉加热至250～400℃之间，保温时间3～9h，然后冷却到室温取出；
e.将步骤d所得物，进行自然干燥，得到硫化锌薄膜。
2.如权利要求1所述的一种用醋酸锌制备硫化锌光电薄膜的方法，其特征在于，步骤a所述清洗，是将导电玻璃基片大小为20mm×20mm，放入体积比丙酮：蒸馏水=5：1的溶液中，超声波清洗30min；再将基片放入乙醇中，超声波清洗30min；再在蒸馏水中将玻璃基片用超声振荡30min；将上述得到的玻璃基片排放在玻璃皿中送入烘箱中，在100℃下烘干供制膜用。
3.如权利要求1所述的一种用醋酸锌制备硫化锌光电薄膜的方法，其特征在于，步骤c所述，是将溶液加入三电极装置中，以饱和甘汞电极为参比电极，铂电极为辅助电极，二氧化锡导电玻璃为研究电极，采用晶体管恒电位仪在沉积电位为2V下常温沉积薄膜，沉积时间为30min，自然干燥得到前驱体薄膜样品。
4.如权利要求1所述的一种用醋酸锌制备硫化锌光电薄膜的方法，其特征在于，步骤d所述管式炉内放入40.0～50.0份水合联氨、1.0～2.0份升华硫粉。
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