CN104393099B - 一种四氟钇钠碘氧铋复合太阳能薄膜的制备方法 - Google Patents
一种四氟钇钠碘氧铋复合太阳能薄膜的制备方法 Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- HOXKQCFUIVTLOQ-UHFFFAOYSA-J O.[F-].[F-].[F-].[F-].[Na+].[Y+3].[I+].[Bi+3] Chemical compound O.[F-].[F-].[F-].[F-].[Na+].[Y+3].[I+].[Bi+3] HOXKQCFUIVTLOQ-UHFFFAOYSA-J 0.000 title claims description 11
- 239000010408 film Substances 0.000 claims abstract description 31
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- 238000000151 deposition Methods 0.000 claims abstract description 11
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- HQHVZNOWXQGXIX-UHFFFAOYSA-J sodium;yttrium(3+);tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Na+].[Y+3] HQHVZNOWXQGXIX-UHFFFAOYSA-J 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 14
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 10
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- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 claims description 9
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- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000003780 insertion Methods 0.000 claims description 5
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- 238000005245 sintering Methods 0.000 claims description 4
- 238000009713 electroplating Methods 0.000 claims description 3
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- YBYGDBANBWOYIF-UHFFFAOYSA-N erbium(3+);trinitrate Chemical compound [Er+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YBYGDBANBWOYIF-UHFFFAOYSA-N 0.000 claims description 2
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- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 3
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- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
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- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 description 1
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- 230000001699 photocatalysis Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了四氟钇钠碘铋复合太阳能薄膜（NaYF4:Yb‑Er/BiIO）的制备方法。该方法是在导电玻璃衬底的一个侧面沉积有一层掺镱掺铥四氟钇钠上转换薄膜（NaYF4:Yb‑Er），然后在NaYF4:Yb‑Er薄膜自组装一层碘氧铋薄膜。制备的复合薄膜均匀致密，是对近红外光有响应的复合太阳能薄膜。本发明工艺方法简单、原料易得、成本低，能耗低，无毒，可以在常温常压压操作，有希望进行工业化生产。
Description
技术领域
本发明涉及一种四氟钇钠碘氧铋复合太阳能薄膜的制备方法。
背景技术
随着能源危机的到来，人们对清洁能源，绿色能源的应用研究成为热点，太阳能是清洁绿色的能源之一，但大部分太阳能电池只吸收所有可见光及紫外光部分，然而由太阳光能量分布知，约52%的红外光不能用与光催化，因此如果通过上转换材料将红外光转换为可见光用于光催化材料具有很大的研究价值，本发明专利第一次采用电化学沉积法，将上转换薄膜（NaYF4:Yb-Er）与太阳能电池薄膜结合，实现了近红外响应。
发明内容
本发明的目的是针对现有技术的不足，提出一种四氟钇钠碘氧铋复合太阳能薄膜（NaYF4:Yb-Er/BiIO）的制备方法。
本发明的目的是通过以下技术方案实现的：一种四氟钇钠碘氧铋复合太阳能薄膜的制备方法，是在导电玻璃衬底的一个侧面依次沉积NaYF4:Yb-Er薄膜然后自组装一层碘氧铋薄膜，步骤如下：
（1） 将硝酸钇、硝酸镱、硝酸铥按照摩尔配比72~94:6~25:1~5溶于水配成混合溶液A，其中硝酸钇的浓度为0.05~0.2mol/L，混合溶液总体积为3ml~10ml，向混合溶液中加入2ml~10ml浓度为0.05~0.35mol/L的EDTA二钠水溶液，形成三种金属的络合物，然后加入1ml~20ml浓度为0.1~1mol/L的抗坏血酸钠水溶液，再加入5ml~30ml浓度为0.1~1.5mol/L的氟化铵水溶液，用氢氧化钠水溶液调节PH值至5~10，得到电镀四氟钇钠上转换薄膜的电解液待用；
（2）以导电玻璃ITO为工作电极，铂金电极为对电极，Ag/AgCl/饱和KCl溶液电极为参比电极，在导电玻璃上进行薄膜沉积。将三电极插入步骤1配制的电解液中，在30-80°C下沉积10分钟~2小时。沉积电压为0.8 V~1.5 V （vs Ag/AgCl/KCl参比电极），在ITO上沉积得到四氟钇钠上转换薄膜，清洗并干燥；
（3）步骤（2）制备的带有四氟钇钠上转换薄膜氩气气氛炉内400°C下退火烧结4小时。
（4）将步骤（3）得到的薄膜浸入浓度为0.0001~0.001mol/L的硝酸铋溶液中5~30秒，然后移入去离子水中约10~20秒，然后浸入浓度为0.0002~0.002mol/L碘化钠溶液中5-30秒，再浸入去离子水中10-20秒；
（5）重复若干次步骤4，得到复合太阳能薄膜（NaYF4:Yb-Er/BiIO）。
本发明具有的有益效果是：本发明通过简单的电化学沉积方法和离子交换法过程，制得一种新型四氟钇钠碘氧铋近红外响应的复合太阳能薄膜（NaYF4:Yb-Er /BiIO），该复合薄膜，在980nm激光器下，有光电流响应。本发明工艺方法简单、原料易得、成本低，能耗低，无毒，便于工业化生产。
附图说明
图1是导电玻璃衬底上复合薄膜结构示意图：1. 碘氧铋薄膜，2. 掺铒掺镱四氟钇钠薄膜，3.导电玻璃衬底；
图2是实施例1所得产物的XRD谱图；
图3为实施例1制备的四氟钇钠薄膜产物的电镜照片；
图4为实施例1制备的NaYF4:Yb-Er/BiIO复合薄膜的电镜照片；
图5为实施例1制备的NaYF4:Yb-Er/BiIO复合薄膜的断面照片；
图6为实施例1制备的四氟钇钠薄膜和NaYF4:Yb-Er/BiIO复合薄膜的光谱图；
图7实施例1制备的NaYF4:Yb-Er/BiIO复合薄膜在980nm激光器下的光电流响应曲线图；
图8 本实验复合薄膜制备工艺流程图。
具体实施方式
如图1所示，本发明在导电玻璃衬底3的一个侧面沉积有一层掺铒掺镱四氟钇钠薄膜上转换发光薄膜2，再在掺铒掺镱四氟钇钠薄膜上组装一层碘氧铋薄膜1。所述的该复合薄膜的化学式为NaYF4:Yb-Er/BiIO，该薄膜材料在980nm激光器下，有光电流响应。
实施例1：
一种四氟钇钠碘氧铋复合太阳能薄膜的制备方法，步骤如下：
1） 将硝酸钇、硝酸镱、硝酸铥按照摩尔配比72:6:1溶于水配成混合溶液A，其中硝酸钇的浓度为0.05mol/L，混合溶液总体积为3mlml，向混合溶液中加入0.05mol/L的EDTA二钠水溶液2ml，形成三种金属的络合物，然后加入0.1mol/L的抗坏血酸钠1mlml，再加入0.1mol/L的氟化铵水溶液5mlml，用1mol/L的氢氧化钠水溶液调节溶液PH值为5，得到电镀四氟钇钠上转换薄膜的电解液待用；
2） 以导电玻璃ITO为工作电极，铂金电极为对电极，Ag/AgCl/饱和KCl溶液电极为参比电极，在导电玻璃上进行薄膜沉积。将三电极插入步骤1配制的电解液中，在80°C下沉积10分钟。沉积电压为1.5 V（vs Ag/AgCl/KCl参比电极），将得到的薄膜清洗并干燥。
3）将步骤2得到的带有镱掺铒四氟钇钠上转换薄膜的ITO在氩气气氛炉内400°C下退火烧结4小时得到上转换薄膜.
4）将步骤（3）得到的薄膜的ITO浸入0.001的硝酸铋溶液中5秒，然后移入去离子水中约10秒，然后浸入0.002mol/L碘化钠溶液中5秒，然后再浸入去离子水中10秒，如此循环50次，得到对近红外光有响应的复合太阳能薄膜（NaYF4:Yb-Er/BiIO）。
该薄膜的XRD图谱如图2所示。其扫描电镜图如图4和图5所示，结合图2和图4、图5，我们可以确定，最后制备的薄膜中同时含有四氟钇钠和碘氧铋。
从图6为四氟钇钠薄膜和NaYF4:Yb-Er/BiIO复合薄膜的光谱图，从图中可看出碘氧铋能够吸收上转换在680 nm以前的光。
从图7为复合薄膜在980nm激光器激发下的，光电流响应曲线，证明该复合薄膜对近红外光有响应，可作为新型近红外响应的复合薄膜电池。
实施例2
一种四氟钇钠碘氧铋复合太阳能薄膜的制备方法，是在导电玻璃衬底的一个侧面依次沉积NaYF4:Yb-Er薄膜和碘氧铋薄膜，步骤如下：
1） 将硝酸钇、硝酸镱、硝酸铒按照摩尔配比94:25:5溶于水配成混合溶液A，其中硝酸钇的浓度为0.2mol/L，混合溶液总体积为10ml，向混合溶液中加入0.35mol/L的EDTA二钠水溶液10ml，形成三种金属的络合物，然后加入1mol/L的抗坏血酸钠20ml，再加入1.5mol/L的氟化铵水溶液30ml，用1mol/L的氢氧化钠水溶液调节溶液PH值为10，得到电镀四氟钇钠上转换薄膜的电解液待用；
2）以导电玻璃ITO为工作电极，铂金电极为对电极，Ag/AgCl/饱和KCl溶液电极为参比电极，在导电玻璃上进行薄膜沉积。将三电极插入步骤1配制的电解液中，在30°C下沉积2小时。沉积电压为0.8 V （vs Ag/AgCl/KCl参比电极），将得到的薄膜清洗并干燥。
3）以步骤2制备的带有四氟钇钠上转换薄膜的ITO在氩气气氛炉内400°C下退火烧结4小时。
4） 将步骤（3）得到的上转换薄膜浸入0.0001mol/L的硝酸铋溶液中30秒，然后移入去离子水中约20秒，然后浸入0.0002mol/L碘化钠溶液中5-30秒，然后再浸入去离子水中20秒，如此循环80次，得到对近红外光有响应的复合太阳能薄膜（NaYF4:Yb-Er/BiIO）。
实施例3
一种四氟钇钠碘氧铋复合太阳能薄膜的制备方法，步骤如下：
1） 将硝酸钇、硝酸镱、硝酸铥按照摩尔配比86:15:3溶于水配成混合溶液A，其中硝酸钇的浓度为0.1mol/L，混合溶液总体积为8ml，向混合溶液中加入0.2mol/L的EDTA二钠水溶液8ml，形成三种金属的络合物，然后加入0.5mol/L的抗坏血酸钠10ml，再加入1.0mol/L的氟化铵水溶液20ml，用1mol/L的氢氧化钠水溶液调节溶液PH值为8，得到电镀四氟钇钠上转换薄膜的电解液待用；
2） 以导电玻璃ITO为工作电极，铂金电极为对电极，Ag/AgCl/饱和KCl溶液电极为参比电极，在导电玻璃上进行薄膜沉积。将三电极插入步骤1配制的电解液中，在60°C下沉积1小时。沉积电压为1.0 V （vs Ag/AgCl/KCl参比电极），将得到的薄膜清洗并干燥。
3）将步骤2制备的带有四氟钇钠上转换薄膜的ITO在氩气气氛炉内400°C下退火烧结4小时。
4）将步骤（3）得到的上转换薄膜浸入0.0005mol/L的硝酸铋溶液中15秒，然后移入去离子水中约15秒，然后浸入0.0008mol/L碘化钠溶液中15秒，然后再浸入去离子水中15秒，如此循环60次，得到对近红外光有响应的复合太阳能薄膜（NaYF4:Yb-Er/BiIO）。
Claims (1)
1.一种四氟钇钠碘氧铋复合太阳能薄膜的制备方法，该方法是在导电玻璃衬底的一个侧面依次沉积NaYF4:Yb-Er薄膜和碘氧铋薄膜，其特征在于：该方法的步骤如下：
（1） 将硝酸钇、硝酸镱、硝酸铒按照摩尔配比72~94:6~25:1~5溶于水配成混合溶液A，其中硝酸钇的浓度为0.05~0.2mol/L，混合溶液总体积为3ml~10ml，向混合溶液中加入2ml~10ml浓度为0.05~0.35mol/L的EDTA二钠水溶液，形成三种金属的络合物，然后加入1ml~20ml浓度为0.1~1mol/L的抗坏血酸钠水溶液，再加入5ml~30ml浓度为0.1~1.5mol/L的氟化铵水溶液，用氢氧化钠水溶液调节PH值至5~10，得到电镀四氟钇钠上转换薄膜的电解液待用；
（2）以导电玻璃ITO为工作电极，铂金电极为对电极，Ag/AgCl/饱和KCl溶液电极为参比电极，在导电玻璃上进行薄膜沉积；将三电极插入步骤（1）配制的电解液中，在30-80°C下沉积10分钟~2小时；沉积电压为0.8 V~1.5 V ，在ITO上沉积得到四氟钇钠上转换薄膜，清洗并干燥；
（3）将步骤（2）沉积后的ITO在氩气气氛炉内400°C下退火烧结4小时；
（4）将步骤（3）烧结后的薄膜浸入浓度为0.0001~0.001mol/L的硝酸铋溶液中5~30秒，然后移入去离子水中10~20秒，然后浸入浓度为0.0002~0.002mol/L碘化钠溶液中5-30秒，再浸入去离子水中10-20秒；
（5）重复步骤4若干次，得到四氟钇钠碘氧铋复合太阳能薄膜。
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