CN1898807A - 用于纳米颗粒层的电解工程的方法 - Google Patents
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Abstract
一种用于制造染料太阳能电池的纳米颗粒电极的方法，包括以下步骤：提供导电基板，在该基板上形成纳米颗粒层，将染料施加到纳米颗粒层，以及在电解液中对纳米颗粒层进行电解处理。
Description
技术领域
本发明涉及纳米结构材料及其应用，以及这种材料的制造方法。本发明更特别涉及形成在基板上的纳米颗粒氧化层。
背景技术
纳米材料，特别是纳米颗粒材料和纳米颗粒氧化物被广泛用于以下应用：包括但不限于传感器、电池、电容器、光电电池(例如，染料太阳能电池(Dye Solar Cell))、电致变色设备、燃料电池和用于水的光催化裂解和净化的设备。
染料太阳能电池技术的高商业潜力是通过具有设计好的孔隙度的纳米颗粒结构的氧化层获得的，该氧化层保证了高表面面积，因而增强了吸收充足量染料的能力，从而能在染料层和电解质之间的分界面上有效地捕获太阳光。
已经发现，对于使基于纳米颗粒材料的设备获得高性能，纳米颗粒的表面性能起决定性作用。
上述性能的改变可通过用另一种材料的薄层覆盖每个颗粒来实现。这种覆层的目的是多样的：
·生成(例如，在具有不同电子特性的两种材料之间接合的)阻挡层。阻挡层的好处包括生成供电子单向转移用的内部电场(二极管效应)。
·生成阻隔层(使颗粒的全部或部分表面与电解质或腐蚀性材料电绝缘)。
·沉积吸入UV-可见光-红外光谱的材料。
·电子屏蔽纳米结构氧化物(NSO)。邻近NSO表面或位于NSO表面中的某些材料能提供电子屏蔽，这样能防止通过表面和电解质之间分界面的不期望的电荷转移。这种电荷转移会导致漏电流、电压损耗和不期望的副反应，这会引起设备性能下降。优选地，该电子屏蔽材料(ESM)是光学透明的和化学稳定的。
当前的方法包括溶胶-凝胶化学方法和几种不同的真空沉积技术。每种技术部有局限性，因为它们每种都不能实现快速且精确的沉积并且不能获得期望的各层性能。
发明内容
本发明的目的是提供用于纳米氧化物的表面改性的方法和改进染料太阳能电池的性能。
根据一个方面，本发明提供了通过对基板施加负电势和对相对电极施加正电势来直接从胶体溶液中在导电基板的表面上或表面中形成完全或不完全的纳米颗粒层的方法。纳米颗粒还通过在熔炉中熔结或者施加足够幅度的AC电场(诸如导致对局部接触点的加热并使颗粒熔合在一起的穿过颗粒之间的局部强电流)，而被互连到基板的材料上或者与彼此互连起来。
根据本发明的另一个方面，纳米颗粒被染料覆层。通过将电极浸入染料溶液中和施加促使溶液中带电染料朝纳米氧化物层移动并在随后促使染料分子结合到纳米氧化物颗粒的电场，来进行该覆层过程。
在根据本发明该方面的一个实施例中，在施加(apply)染料之后施加另一种染料或者施加用于阻隔还没有被第一种施加的染料覆盖的纳米颗粒区域的另一种吸收剂。另一种染料或另一种吸收剂的施加，是以和施加第一种染料相同的方式进行的，例如，从溶液中进行，并且借助于促使染料分子朝向通常为纳米氧化物但不必需是纳米氧化物的纳米材料移动的电场。
根据本发明的另一个方面，阻挡层被形成在上述纳米材料的表面上。为了达到本发明的目的，该表面包括从分界面到大约40埃或大约10个单位晶格的深度的区域。该阻挡层典型地包括电子特性与原纳米颗粒层不同的金属氧化物。施加这样的阻挡层，是在溶液中通过生成这样的电场来进行的：该电场促使阻挡层的离子形态的材料朝纳米颗粒移动，并随后促使该材料沉积在纳米颗粒的表面上。
在根据本发明该方面的一个实施例中，两种或更多种电子特性不同的材料被沉积。
在根据本发明该方面的另一个实施例中，随后通过加热和/或利用氧气来处理基板，以确保将沉积的材料稳定地结合到纳米颗粒上和/或以确保沉积材料的氧化。
根据本发明的另一个方面，用电解处理来改变纳米材料的表面性能。在一个实施例中，通过对表面材料进行电解溶解来获得干净且有活性的纳米颗粒表面。在另一个实施例中，电解氧化确保了纳米颗粒材料的无碳层。
而根据本发明的另一个方面，上面公开的电解沉积是在加有电压限制的恒定电流条件下进行的，诸如当电压达到预定限度(相对于参考电极测量的)时，控制电路从恒定电流切换到恒定电压模式，并保持该恒定电压模式直到电流降到预定值以下或者直到预定量的电荷已穿过电解质溶液为止。
已经发现，在逐渐增加通过电解质溶液转移的电荷的一系列循环中执行上述沉积是有利的。每个循环包括插入和提取半循环。在插入半循环期间，电场促使要沉积的材料向纳米材料沉积。在提取半循环期间，该材料被从纳米材料中移除。插入和提取半循环都是在有电流限制的条件下执行的，直到电压达到电压预置幅度为止，然后在有电压限制的条件下继续沉积，直到沉积电流降到电流预置幅度或者已经传递了预置的电荷为止，然后终止沉积。
已经发现，将恒定电流/恒定电压插入/提取模式与施加的AC电场相叠加是有利的。在一个实例中，AC电场是平行于基板施加的，在另一个实例中，AC电场是垂直于基板施加的。
附图说明
以上已经宽泛地描述了本发明的特征，以下将仅通过举例和说明的方式来描述本发明的实施例。在以下描述中，将参照附图来说明。
图1是用于纳米颗粒电极的电解处理的配置的图示。
图2显示了经处理的和未经处理的DSC电极在0.3sun的光电性能的对比。
具体实施方式
参照图1，工作的纳米颗粒电极包括基板1和纳米材料的纳米颗粒层2。以如下方式将工作电极插入电解液6中：用溶液来覆盖被选来进行电解处理的纳米颗粒层的区域。参考电极3位于纳米颗粒层1的附近。相对电极4与工作电极相对。相对电极的形状和位置被选择成能确保相对电极和工作电极之间的均匀电场。所有这3个电极被连接到可编程的稳压器5。
在这个实例中提供有以下材料：
工作电极：沉积在导电玻璃基板(3mm厚的Pilkington TEC-15玻璃)上的12-15微米厚的二氧化钛(氧化钛)纳米颗粒层。
氧化钛层(大约11mm×8mm)通过如下方式形成：先网印氧化钛糊剂，接着在最高550摄氏度下烧制以使氧化钛颗粒(平均颗粒尺寸为12-15nm)得到良好的烧结和互连。通过使用可从先有技术中获得的用于染料太阳能电池技术工艺的标准来制备工作电极。
工作电极的电解处理按如下方式执行：
参考电极：银/氯化银标准微参考电极。
相对电极：铂金属丝网。
电解液：将1.4克YCl3·6H2O溶解在10毫升异丙醇中；将1ml水加入到溶液中。
电特性：
·电流密度＝0.1mA/cm2，
·具有小充电电平(在插入半循环中为5mC/cm2)的5个全循环，
·具有中等充电电平(在插入半循环中为10mC/cm2)的5个全循环，
·1个插入半循环-10mC/cm2的充电电平。
后处理：
在电解处理之后，将标准DSC染料施加到经处理的纳米颗粒氧化钛上，并构造标准电池。在一些情况下，工作电极以各种温度进行后烧制。0.3sun的光电测试显示出经处理的样品在开路电压和填充系数方面的显著改进。对于以250摄氏度进行后烧制的样品(如图2所示)，能获得最大效率。
参照图2，对经处理的和未经处理的DSC电极的光电测试显示出，光电处理会导致在光电电压和功率方面的显著改进。
Claims (13)
1.一种用于制造染料太阳能电池的纳米颗粒电极的方法，包括以下步骤：提供导电基板，在所述基板上形成纳米颗粒层，将染料施加到所述纳米颗粒层，以及在电解液中对所述纳米颗粒层进行电解处理的附加步骤。
2.如权利要求1所述的方法，其特征在于，所述电解液包含在化学性质上不同于所述纳米颗粒层的离子，并且所述电解处理包括将来自所述电解液的离子形态的材料转移到所述纳米颗粒层的表面中，从而形成阻挡层，所述阻挡层的电子特性与所述原纳米颗粒层的电子特性不同。
3.如权利要求2所述的方法，其特征在于，在所述电解处理之后进行加热以确保将所述阻挡层稳固结合到所述纳米颗粒层。
4.如权利要求1所述的方法，其特征在于，所述电解处理包括将材料从所述纳米颗粒层部分地移除到所述电解液。
5.如权利要求1所述的方法，其特征在于，所述电解液包含UV、可见光和/或红外吸收材料的离子。
6.如权利要求4所述的方法，其特征在于，所述吸收材料是染料。
7.如上述任一权利要求所述的方法，其特征在于，所述纳米颗粒层包括金属或混合金属氧化物。
8.如权利要求7所述的方法，其特征在于，所述金属氧化物是二氧化钛。
9.一种用于制造DSC的纳米颗粒电极的方法，包括以下步骤：提供基板，从电解液中对所述纳米颗粒层进行电解沉积，以及将染料施加到所述纳米颗粒层。
10.如上述任一权利要求所述的方法，其特征在于，所述电解处理至少包括一个这样的步骤，即在所述电解液和所述纳米颗粒层之间转移预定量的电荷。
11.如权利要求10所述的方法，其特征在于，所述电荷在施加有电压限制的恒定电流条件下被转移，诸如当电压达到所述施加的限制时，控制电路从所述恒定电流切换到恒定电压模式，并保持所述恒定电压模式直到电流降到预定电流值以下或者直到预定量的电荷已通过所述电解质溶液和所述纳米颗粒电极之间为止。
12.如权利要求10和11所述的方法，其特征在于，所述电解处理至少包括两个后续的步骤(半循环)，每个步骤都转移预定量的电荷；在第一半循环中，通过离子从所述电解液到所述纳米颗粒层的移动来转移所述电荷，在第二半循环中，通过离子从所述纳米颗粒层到所述电解液的移动来转移所述电荷。
13.如权利要求12所述的方法，其特征在于，所述电解处理至少包括两个循环，并且所述第二循环中的预定量的电荷大于所述第一循环中的预定量的电荷。
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|---|---|---|---|
| AU2003906985A AU2003906985A0 (en) | 2003-12-18 | Method for electrolytic engineering of nano-particulate layers | |
| AU2003906985 | 2003-12-18 |
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| CN1898807A true CN1898807A (zh) | 2007-01-17 |
| CN100477287C CN100477287C (zh) | 2009-04-08 |
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| JP (1) | JP4909740B2 (zh) |
| KR (1) | KR101056514B1 (zh) |
| CN (1) | CN100477287C (zh) |
| CA (1) | CA2550422A1 (zh) |
| WO (1) | WO2005060008A1 (zh) |
| ZA (1) | ZA200605869B (zh) |
Cited By (1)
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| CN105593409A (zh) * | 2013-08-07 | 2016-05-18 | 艾克泽基因公司 | 传感器生长控制器 |
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| WO2005060008A1 (en) * | 2003-12-18 | 2005-06-30 | Dyesol Ltd | Method for electrolytic engineering of nano-particulate layers |
| CN100433373C (zh) * | 2005-12-28 | 2008-11-12 | 大连海事大学 | 一种纳米TiO2－M薄膜紫外光传感器及其制备方法 |
| EP2050319A4 (en) * | 2006-07-21 | 2010-12-08 | Valtion Teknillinen | METHOD FOR THE PRODUCTION OF LADDERS AND SEMICONDUCTORS |
| FI122014B (fi) | 2007-06-08 | 2011-07-15 | Teknologian Tutkimuskeskus Vtt | Menetelmä ja laite nanopartikkelijärjestelmien toiminnallistamiseksi |
| DE202008001599U1 (de) | 2008-02-04 | 2008-06-26 | Knöchel, Arndt, Prof. Dr. | Elektrolytische Zusammensetzung für eine Farbstoffsolarzelle |
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| US4142947A (en) * | 1977-05-12 | 1979-03-06 | Uri Cohen | Electrodeposition of polycrystalline silicon from a molten fluoride bath and product |
| US4666567A (en) * | 1981-07-31 | 1987-05-19 | The Boeing Company | Automated alternating polarity pulse electrolytic processing of electrically conductive substances |
| EP0983282B1 (en) * | 1997-05-07 | 2003-11-12 | Ecole Polytechnique Federale De Lausanne | Metal complex photosensitizer and photovoltaic cell |
| JPH11144773A (ja) | 1997-09-05 | 1999-05-28 | Fuji Photo Film Co Ltd | 光電変換素子および光再生型光電気化学電池 |
| US6444189B1 (en) * | 1998-05-18 | 2002-09-03 | E. I. Du Pont De Nemours And Company | Process for making and using titanium oxide particles |
| JP3437475B2 (ja) * | 1998-12-28 | 2003-08-18 | キヤノン株式会社 | 酸化亜鉛膜の形成方法及び該酸化亜鉛膜を用いた光起電力素子 |
| US6340633B1 (en) * | 1999-03-26 | 2002-01-22 | Advanced Micro Devices, Inc. | Method for ramped current density plating of semiconductor vias and trenches |
| US6359211B1 (en) * | 1999-06-17 | 2002-03-19 | Chemmotif, Inc. | Spectral sensitization of nanocrystalline solar cells |
| JP4500420B2 (ja) * | 2000-09-20 | 2010-07-14 | 富士フイルム株式会社 | 光電変換素子および光電池 |
| JP4278080B2 (ja) * | 2000-09-27 | 2009-06-10 | 富士フイルム株式会社 | 高感度受光素子及びイメージセンサー |
| JP4461656B2 (ja) | 2000-12-07 | 2010-05-12 | セイコーエプソン株式会社 | 光電変換素子 |
| JP4461657B2 (ja) * | 2000-12-07 | 2010-05-12 | セイコーエプソン株式会社 | 光電変換素子 |
| KR100866055B1 (ko) | 2001-02-21 | 2008-10-30 | 쇼와 덴코 가부시키가이샤 | 색소증감형 태양전지용 금속 산화물 분산액, 광활성 전극및 색소증감형 태양전지 |
| US20020145826A1 (en) * | 2001-04-09 | 2002-10-10 | University Of Alabama | Method for the preparation of nanometer scale particle arrays and the particle arrays prepared thereby |
| JP2003030891A (ja) * | 2001-07-12 | 2003-01-31 | Sony Corp | 光ピックアップ |
| EP1289028B1 (en) * | 2001-09-04 | 2008-01-16 | Sony Deutschland GmbH | Photovoltaic device and method for preparing the same |
| JP2003100357A (ja) * | 2001-09-20 | 2003-04-04 | Fuji Photo Film Co Ltd | 光電変換素子の作製方法、光電変換素子及び光電池 |
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| WO2005060008A1 (en) * | 2003-12-18 | 2005-06-30 | Dyesol Ltd | Method for electrolytic engineering of nano-particulate layers |
| KR20070075186A (ko) * | 2006-01-12 | 2007-07-18 | 삼성전자주식회사 | 분산제 기능을 갖는 염료 및 이를 채용한 태양 전지 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105593409A (zh) * | 2013-08-07 | 2016-05-18 | 艾克泽基因公司 | 传感器生长控制器 |
Also Published As
| Publication number | Publication date |
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| CN100477287C (zh) | 2009-04-08 |
| JP2007521623A (ja) | 2007-08-02 |
| JP4909740B2 (ja) | 2012-04-04 |
| CA2550422A1 (en) | 2005-06-30 |
| EP1697999A1 (en) | 2006-09-06 |
| ZA200605869B (en) | 2007-10-31 |
| KR20070041665A (ko) | 2007-04-19 |
| KR101056514B1 (ko) | 2011-08-12 |
| US20080105362A1 (en) | 2008-05-08 |
| EP1697999A4 (en) | 2010-12-01 |
| US8002960B2 (en) | 2011-08-23 |
| WO2005060008A1 (en) | 2005-06-30 |
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