CN102254696B - 一种染料敏化太阳能电池光阳极修饰材料 - Google Patents
一种染料敏化太阳能电池光阳极修饰材料 Download PDFInfo
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Abstract
Description
技术领域
本发明属于染料敏化太阳能电池光阳极修饰领域,涉及一种染料敏化太阳能电池光阳极修饰材料。
背景技术
光阳极是染料敏化太阳能电池的核心部件,主要作用是利用巨大的表面积来吸附单分子层染料,同时也是电荷分离和传输的载体。在染料敏化太阳能电池(DSSC)中应用的半导体薄膜材料主要有TiO2、ZnO、SnO2、Nb2O5、SrTiO3、Zn2SnO4等,到目前为止性能最为优良的仍是纳米TiO2半导体。但是半导体电极的巨大表面积也增加了电极表面的电荷复合几率,从而降低太阳能电池的光电转换效率。为了改善电池的光伏性能,需要进行TiO2表面钝化和保护,人们开发了多种物理化学修饰技术来改善纳米TiO2电极的特性,例如:(1) 在纳米TiO2表面包覆具有较高导带位置的半导体或绝缘层形成核-壳结构的阻挡层来减少电荷的复合,TiO2表面包覆ZnO、Nb2O5、SrTiO3等金属氧化物后电池效率均有明显提高(参见:Chem. Mater., 2001, 13, : 678-682; J. Phys. Chem. B, 2001, 105: 6347-6352; Chem. Mater., 2002, 13: 4629-4634)。
(2) 在纳米TiO2表面滴加一定浓度的树枝状聚酯溶液共吸附剂,作为半导体-电解质界面的阻挡层,可以有效的提高短路电流密度,而且对开路电压影响不大,但所用的聚酯价格较高(3806RMB/250mg, Adrich公司) (参见:Chem. Comm. 2011, 47, 1734-1736)。
(3) 以吡啶熔盐作为共吸附剂修饰纳米TiO2电极,参比电池的开路电压593mV,短路电流为8.87mAcm-2,效率为3.73%,只使用烟碱酸时开路电压增加到615mV,但短路电流下降到8.23 mAcm-2,最终导致效率下降到3.49%,使用吡啶熔盐时,由于含有I-,只使得效率略有增加,增加到4.04%-4.49%。(参见:Sol. Energy, 2011,85,174-179)。
(4) 专利号为200710119311.X的中国发明专利公开了一种染料敏化太阳能电池中染料敏化光阳极的后修饰方法,将制备好的纳米多孔TiO2光阳极吸附染料后,再修饰上金属化合物层。减小了TiO2导带中注入的电子与电解质中氧化还原对的反向复合,提高了太阳能电池的光电转换效率。但是我们可以从公开的的说明书里了解到参比电池放置一天后效率从2.60%下降到0.36%;实例一的效率从3.22%下降到3.20%,放置两天后降到1.98%。虽然修饰后效果比未修饰的要好,但电池的稳定性还是不理想的。
发明内容
本发明的发明目的是提供一种染料敏化太阳能电池光阳极修饰材料,以改善料敏化太阳能电池的性能和稳定性。
为达到上述发明目的,本发明采用的技术方案是:一种染料敏化太阳能电池光阳极修饰材料,所述染料敏化太阳能电池光阳极修饰材料为硅氧烷离子液体,其结构式为:
式中,R1为C1~C6的烷基,R2为C1~C15的亚烷基,选自:、或,其中,R4、R5分别独立选自C1~C8的烷基; 选自:I-、Br-、Cl-、SCN-、N(CN)2 -、C(CN)3 -、B(CN)4 -、BF4 -、PF6 -、CF3SO3 -、C2F5SO3 -、[N(SO2CF3)2]-、B(CN)4 - 、ClO4 -或CF3COO-中的一种。
上述染料敏化太阳能电池光阳极修饰材料的制备方法可参照文献:J. Am. Chem. Soc., 2002, 124, 12932-12933; Tetrahedron Letters, 2008, 49, 4865-4868,具体包括以下步骤:
(1) 取一份R3与一份无水条件下充分反应,洗涤分离后得到产物;其中,其中Y选自:I、Br或Cl;
(2) 取一份与过量的其他阴离子的金属盐MZ充分反应,交换阴离子,然后洗涤分离,则得到,其中,M选自:钠Na、锂Li、钾K或银Ag,Z选自:SCN、N(CN)2、C(CN)3、B(CN)4、BF4、PF6、CF3SO3、C2F5SO3、[N(SO2CF3)2]、B(CN)4、ClO4或CF3COO中的一种。
应用上述染料敏化太阳能电池光阳极修饰材料修饰光阳极的方法为:将上述染料敏化太阳能电池光阳极修饰材料硅氧烷离子液体与乙醇配成0.005~1 mol/L的溶液,把制备好的光阳极放入该溶液中进行吸附,吸附时间为1s~24h,并且可以通过控制吸附时间控制吸附量;乙醇冲洗除去未吸附的硅氧烷离子液体,晾干得到修饰的光阳极。
优选的技术方案中,染料敏化太阳能电池光阳极修饰材料硅氧烷离子液体与乙醇配成浓度为0.01~0.2mol/L的溶液;把制备好的光阳极放入该溶液中进行吸附,吸附时间为10min~5h。
进一步的技术方案中,采用液体电解质,凝胶电解质或固体电解质与修饰后光阳极组装成染料敏化太阳能电池。
由于上述技术方案运用,本发明与现有技术相比具有下列优点:
1.本发明所述染料敏化太阳能电池光阳极修饰材料简单易得,成本低,采用该材料修饰光阳极后制得的染料敏化太阳能电池稳定性高,电池的效率高,在室温环境,使用氙灯模拟太阳光,光强100mW/cm2条件下,测得电池(有效面积0.16cm2)光电转换效率最高为6.39%。
2.采用本发明所述染料敏化太阳能电池光阳极修饰材料修饰光阳极的方法简单:将吸附好染料的纳米TiO2电极,浸入一定浓度的硅氧烷离子液体的溶液中,取出,通过挥发掉表面的溶剂,组装成电池。
3.本发明所述染料敏化太阳能电池光阳极修饰材料为硅氧烷离子液体,应用在染料敏化太阳能电池时,若电解质中有少量的水,硅氧烷可以水解成网状物质,生成副产物可做溶剂,也可以减小电极表面电荷的复合,增加电池的效率。
4.本发明所述染料敏化太阳能电池光阳极修饰材料可通过设计方便得到,如果以I-,Br-,Cl-等阴离子的离子液体为前驱体,通过阴离子交换技术可以非常方便的获得各种阴离子型的离子液体,对纳米TiO2电极表面进行处理,进行优化,能够制备稳定性高,电池效率较高的染料敏化太阳能电池,应用前景广阔。
附图说明
图1是实施例二中参比电池的稳定性测试结果图;
图2是实施例二中采用硅氧烷离子液体2修饰光阳极后所得电池的稳定性测试结果图;
图3是实施例二中采用硅氧烷离子液体6修饰光阳极后所得电池的稳定性测试结果图。
具体实施方式
下面结合附图及实施例对本发明作进一步描述,但是,应当理解本发明并不限于这里所述的特殊实例和实施方案,还包括使用其它液体电解质、凝胶电解质和固体电解质,也包括ZnO染料敏化电池。这里包括的特殊实例和实施方案的目的在于帮助本领域的技术人员实践本发明。
实施例一:
硅氧烷离子液体3的合成:9.23g和4.11 g在80℃通氮气的环境下反应24h,待产物冷却到室温下,用乙醚洗5次后放到真空泵中抽掉多余的溶剂。取2.67g和1.36g NaC(CN)3在丙酮中室温交换反应48h,将沉淀物过滤,滤液旋蒸后放到真空泵中抽掉多余的溶剂,所得产物的 1 H NMR分析数据如下所示。
硅氧烷离子液体4的合成:9.94g和3.96g在75℃通氮气的环境下反应24h,待产物冷却到室温下,用乙醚洗5次后放到真空泵中抽掉多余的溶剂。取2.78g和1.32g NaBF4在丙酮中室温交换反应48h,将沉淀物过滤,滤液旋蒸后放到真空泵中抽掉多余的溶剂,所得产物的 1 H NMR分析数据如下所示。
硅氧烷离子液体5的合成:9.94g和5.06g在80℃通氮气的环境下反应24h,待产物冷却到室温下,用乙醚洗5次后放到真空泵中抽掉多余的溶剂。取3.0g 和2.21g KPF6在丙酮中室温交换反应48h,将沉淀物过滤,滤液旋蒸后放到真空泵中抽掉多余的溶剂,所得产物的 1 H NMR分析数据如下所示。
硅氧烷离子液体6的合成:12.04g和4.11 g在80℃通氮气的环境下反应24h,待产物冷却到室温下,用乙醚洗5次后放到真空泵中抽掉多余的溶剂。取3.23g和3.45g LiTFSI在乙腈中室温交换反应48h,将沉淀物过滤,滤液旋蒸后放到真空泵中抽掉多余的溶剂,所得产物的 1 H NMR分析数据如下所示。
硅氧烷离子液体7的合成:8.83g 和2.06g在80℃通氮气的环境下反应24h,待产物冷却到室温下,用乙醚洗5次后放到真空泵中抽掉多余的溶剂。取2.18g和0.93g KB(CN)4在丙酮中室温交换反应48h,将沉淀物过滤,滤液旋蒸后放到真空泵中抽掉多余的溶剂,所得产物的 1 H NMR分析数据如下所示。
硅氧烷离子液体8的合成:12.04g 和5.15g在80℃通氮气的环境下反应24h,待产物冷却到室温下,用乙醚洗5次后放到真空泵中抽掉多余的溶剂。取3.51g和3.45g LiTFSI在乙腈中室温交换反应48h,将沉淀物过滤,滤液旋蒸后放到真空泵中抽掉多余的溶剂,所得产物的 1 H NMR分析数据如下所示。
硅氧烷离子液体9的合成:7.07g 和2.06g在80℃通氮气的环境下反应24h,待产物冷却到室温下,用乙醚洗5次后放到真空泵中抽掉多余的溶剂。取1.83g和1.73g LiTFSI在乙腈中室温交换反应48h,将沉淀物过滤,滤液旋蒸后放到真空泵中抽掉多余的溶剂,所得产物的 1 H NMR分析数据如下所示。
对上述9种化合物进行
1
H NMR分析,数据如下所示:
硅氧烷离子液体1:1HNMR (400 MHz, CDCCl3): δ= 9.21 (s, 1H), 7.44 (s, 1H), 7.43 (s, 1H), 4.15-4.17 (t, 2H ), 3.85 (s, 3H), 1.94-1.97 (m, 2H), 3.55 (s, 9H), 0.59-0.62 (t, 2H)。以上数据证明所得化合物确为。
硅氧烷离子液体2: 1HNMR (400 MHz, CDCCl3): δ= 8.79 (s, 1H), 7.30 (s, 1H), 7.27 (s, 1H), 4.08-4.11 (t, 2H ), 3.92 (s, 3H), 1.87-1.90 (m, 2H), 3.54 (s, 9H), 0.58-0.62 (t, 2H)。以上数据证明所得化合物确为。
硅氧烷离子液体3: 1HNMR (400 MHz, CDCCl3): δ= 8.73 (s, 1H), 7.09 (s, 1H), 7.01 (s, 1H), 4.15-4.17 (t, 2H ), 3.85 (s, 3H), 1.94-1.97 (m, 2H), 3.55 (s, 9H), 0.59-0.62 (t, 2H)。以上数据证明所得化合物确为。
硅氧烷离子液体4:1HNMR (400 MHz, CDCCl3): δ= 8.74 (t, 1H), 8.46 (d, 2H), 8.22 (t, 2H), 3.50 (s, 9H), 3.11-3.14 (t, 2H ), 1.42-1.45 (m, 2H), 0.60-0.62 (t, 2H)。以上数据证明所得化合物确为。
硅氧烷离子液体5: 1HNMR (400 MHz, CDCCl3): δ= 3.57 (s, 9H), 3.28-3.31 (t, 2H), 3.24-3.27 (m, 6H), 1.80-1.82 (m, 2H), 1.25-1.29 (t, 9H ), 0.58-0.61 (t, 2H)。以上数据证明所得化合物确为。
硅氧烷离子液体6:1HNMR (400 MHz, CDCCl3): δ= 8.78 (s, 1H), 7.29 (s, 1H), 7.25 (s, 1H), 4.20-4.23 (t, 2H ), 3.96 (s, 3H), 3.80-3.87 (m, 6H), 1.97-2.01 (m, 2H), 1.21-1.25 (t, 9H), 0.58-0.62 (t, 2H)。以上数据证明所得化合物确为。
硅氧烷离子液体7: 1HNMR (400 MHz, CDCCl3): δ= 8.64 (s, 1H), 7.09 (s, 1H), 7.01 (s, 1H), 4.04-4.06 (t, 2H ), 3.84 (s, 3H), 3.83-3.89 (m, 6H), 1.80-1.85 (m, 18H), 1.21-1.24 (t, 9H), 0.57-0.59 (t, 2H)。以上数据证明所得化合物确为。
硅氧烷离子液体8:1HNMR (400 MHz, CDCCl3): δ= 8.71 (s, 1H), 7.22 (s, 1H), 7.19 (s, 1H), 4.11-4.15 (t, 2H ), 3.84-3.89 (m, 6H), 3.32 (t, 2H), 1.22-1.25 (t, 9H), 0.9-1.8 (m, 5H), 0.59-0.62 (t, 2H)。以上数据证明所得化合物确为。
硅氧烷离子液体9:1HNMR (400 MHz, CDCCl3): δ= 8.92 (s, 1H), 7.38 (s, 1H), 7.31 (s, 1H), 4.11-4.14 (t, 2H ), 3.79-3.82 (t, 2H), 3.72 (s, 3H), 1.53-1.58 (m, 2H), 1.40-1.44 (m, 2H), 0.90-0.95 (t, 9H), 0.59-0.62 (t, 2H)。以上数据证明所得化合物确为。
实施例二
取实施例一所得硅氧烷离子液体1~9各0.5mM,分别与20ml的乙醇配成溶液,把吸附好染料的TiO2导电玻璃,放入溶液中浸泡2h。乙醇冲洗除去未吸附的硅氧烷离子液体,晾干。把修饰过的光阳极与Pt对电极组装成染料敏化太阳能电池。在室温环境下,使用氙灯模拟太阳光,光强100mW/cm2条件下,测得电池(有效面积0.16cm2)光电参数见下表。
本实施例采用的示范性的电解质为:含0.1M LiI,0.05M I2,0.6M 1-丙基-3-甲基咪唑碘化盐(PMII),0.5M 叔丁基吡啶(TBP)的3-甲氧基丙腈溶液。
本实施例中染料敏化太阳能电池的制作方法为:FTO导电玻璃先清洗干净,FTO导电玻璃在70℃40mM TiCl4水溶液中保持30min,取出后用乙醇冲洗后自然晾干,在FTO导电玻璃表面形成一层致密的TiO2模。用刮涂技术,把P25浆料涂一层8μm厚的TiO2薄膜,P400浆料涂一层3μm厚的TiO2薄膜,不同温度煅烧,待导电玻璃冷却到80℃时,浸入Z907染料溶液中12h;用H2PtCl6溶液在另一块导电玻璃涂一薄层作为对电极;通过热塑膜把光阳极和对电极封在一起,电解质通过对电极上的小孔注入;通过真空填充技术组装成染料敏化太阳能电池。同时,没有进行阳极修饰的电池作为参比电池。(电池的制作参照Thin solid films, 2008,516,4613-4619 )。
对参比电池、采用硅氧烷离子液体2、6修饰的光阳极组成的电池的稳定性进行测定,得图1~3。从图1中可以看出,不进行光阳极表面修饰的染料敏化太阳能电池,由于开路电压和短路电流下降了很多,最终导致电池的效率下降。在测试的50天里,从图1中可以看出电池效率下降了7%左右。从图2、3可知:进行光阳极修饰后,在刚组装完的几天里电池效率还有所上升,之后电池的效率保持的很好。由此可见进行光阳极修饰后的电池性能有了很大的改善。
注:上述实施例中使用的各种硅氧烷衍生物,吡啶、各种咪唑衍生物,各种叔胺、各种碱、盐等原料来自市售。
Claims (1)
1.应用染料敏化太阳能电池光阳极修饰材料修饰光阳极的方法,所述染料敏化太阳能电池光阳极修饰材料为硅氧烷离子液体,其结构式为:
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