取向碳纳米管及其复合膜的制备和应用
摘要
碳纳米管具有优异的光学、电学、热学和机械性能,因而在光电、能源、生物、医学等诸多领域都显示重要的应用前景。为了实现大规模生产应用,目前研究的主要方向是发展宏观尺度的碳纳米管本体材料,包括阵列、膜和纤维三种形貌,其中碳纳米管膜因其方便的制备和广泛的应用而受到重点关注。但是,因为碳纳米管在膜中无规聚集,无法有效控制和进一步提高碳纳米管膜的结构和性能,这严重限制了碳纳米管膜在多个领域的应用。比如在能源领域,为了解决能源危机,太阳能电池特别是被称为第三代的染料敏化太阳能电池(dye-sensitized solar cell, DSSC),因为较低的成本引起学术界和工业界的广泛兴趣,而如何进一步提高DSSC的光电转换效率和稳定性,是决定其应用的关键因素。目前的主要策略之一是发展新型电极材料,如碳纳米管膜已经被广泛研究用作对电极,但电荷在无规碳纳米管网络中传输的效率很低。本学位论文重点提出和发展了两种制备取向碳纳米管膜及其复合膜的新方法,比较系统地研究了取向碳纳米管作为对电极在DSSC中的应用前景。研究工作主要包括如下几个方面：
超高碳纳米管阵列的制备。为了得到具有优异机械和电学性能的取向碳纳米管膜或复合膜,一个简单且有效的方法是基于高度取向的碳纳米管阵列来制备,因此合成高质量的碳纳米管阵列非常重要。本学位论文主要通过化学气相沉积法来合成多壁碳纳米管阵列(碳纳米管直径7-20纳米),比较系统地研究了催化剂、气体流量、温度、反应时间等实验参数对碳纳米管阵列高度、密度、纯度等的影响规律,确定了制各高质量的较高碳纳米管阵列的最佳条件。
超长取向碳纳米管膜的制备及其在DSSC中的应用。目前取向碳纳米管膜主要通过干法纺丝从碳纳米管阵列中制备,目前合成可纺碳纳米管阵列的实验条件比较苛刻,并且可纺碳纳米管阵列的高度往往在300-400微米,最高一般不超过1毫米,由于单根碳纳米管的电阻极低,因而取向碳纳米管膜的电阻主要来自碳纳米管之间的接触电阻。碳纳米管越长,碳纳米管之间接触点越少,越有利于电子的快速传输,所以增加碳纳米管长度是提高取向碳纳米管膜电极应用的关键因素。本学位论文提出了一种新的粘附转移法,通过普通胶带将碳纳米管从阵列直接转移到各种基底上。该方法操作简单、效率高,尤其适用于高碳纳米管阵列。通过粘附转移法制备的超长取向碳纳米管膜的室温电导率达到1150S/cm,大大超过干法纺丝得到的取向碳纳米管膜的电导率(-500S/cm)。超长取向碳纳米管膜具有良好的柔性,弯曲180。后电导率基本保持不变,即使弯曲500次电导率仅下降1%。以上结果表明超长取向碳纳米管膜代表了一类新型、高效率的电极材料,特别是可用作柔性电极材料。本学位论文以其取代传统铂对电极,构建DSSC,光电转换效率超过9.00%,远高于在同等条件下干法纺丝得到的取向碳纳米管膜作为对电极时的4.18%,也高于铂对电极8.05%。比较系统地研究了超长取向碳纳米管膜厚度以及碳纳米管密度和长度对DSSC性能的影响规律,发现膜厚度为4微米和碳纳米管密度为2×1011cm-2时电池效率最高,且电池效率随着碳纳米管长度的增加而增加。另外,以超长取向碳纳米管膜作为对电极,构建高效率的柔性DSSC,光电转化效率为2.29%,也远高于干法纺丝得到的取向碳纳米管膜在同等条件下的1.22%。
平行取向碳纳米管/环氧树脂复合膜的制备及其在DSSC中的应用。碳纳米管具有优异的机械和电学性能,而高分子来源广泛、结构可控、制备方便,通过形成复合材料可以充分发挥二者的优势。本学位论文发展了一种新的切片技术,制备平行取向碳纳米管/高分子复合薄膜。概括来说,高分子溶液或熔体加入到碳纳米管阵列中,固化后通过传统的切片技术纵向切片即可得到高质量的复合薄膜,膜的厚度可在50纳米到50微米内比较精确地进行调控,复合膜显示良好的柔性、较好的透明性、较高的导电率。以平行取向碳纳米管/环氧树脂复合膜为例,当膜厚度为75纳米时透光率达到94%。因为复合膜具有良好的柔性,所以主要以其作为对电极,构建柔性的DSSC。
垂直取向碳纳米管/石蜡复合膜的制备及其应用。通常制备的取向碳纳米管复合膜主要采用环氧树脂、聚苯乙烯等高分子体系作为填充组分,在很多情况下,虽然可以通过溶剂、燃烧等方法去除,但常常存在后处理和残余物较多等问题。而且在这些复合膜中碳纳米管主要为平行取向,在垂直膜的方向物理性能都比较低。本学位论文以石蜡作为填充组分,通过横向切片制备了垂直取向碳纳米管／石蜡复合膜,复合膜的厚度也可以在50纳米到50微米内进行精确控制。通过真空升华的方法可以轻松有效地去除石蜡,分离出干净的碳纳米管。因为碳纳米管垂直于膜表面且上下贯通,因此碳纳米管长度和直径分布都比较窄。进一步通过加热和超声处理,可以将碳纳米管沿轴向剪开,获得多层石墨烯纳米带,产率接近100%。因为碳纳米管长度和直径都可以比较精确地控制,所以通过本方法可以有效地控制多层石墨烯纳米带的长度和宽度。
综上所述,本论文发展了制备取向碳纳米管膜及其复合膜的两种新方法,这些方法操作方便、效率高,也具有较好的普适性,可以大规模推广使用。取向碳纳米管膜及其复合膜显示优异的光学、电学和机械性能,可广泛用作各种电极材料,这里重点以其作为对电极构建新型DSSC,发现基于取向碳纳米管的DSSC显示较高的效率。
Due to the novel electrical, optical, and mechanical properties, carbon nanotubes (CNTs) exhibit promising applications in a wide variety of fields, such as electrical and optical devices, energy, and biomedicine. However, in many cases, CNTs are required to be further assembled into bulk materials including array, film, and fiber. Among them, the CNT film may represent the most studied system. Unfortunately, as CNTs tend to aggregate during the conventional solution or melt process, it still remains challenging to control and improve the structure and property in the film, which has largely hindered the application in many fields. For instance, CNT films have been widely proposed as electrodes in organic solar cells such as dye-sensitized solar cells (DSSCs). DSSCs have been considered as the third generation solar cells and extensively investigated due to a low cost, easy fabrication, and high energy conversion efficiency. The development of new electrode materials represents a promising direction to improve the cell efficiency with target for a practical application. Therefore, CNT films have been widely explored for the electrode in DSSCs, particularly, as counter electrode to replace the conventional expensive and unstable platinum. However, the aggregated structure of CNTs has greatly lowered the efficiency of the resulting cell. To further improve the structure and property of CNT film, it is critically important to realize a high alignment of CNTs. Herein, two new methods have been developed for the preparation of aligned CNT films and composite films, and the use of them as counter electrodes to fabricate highly efficient DSSCs was carefully studied in this thesis. The main work is summarized as bellow.
Synthesis of ultrahigh CNT array. To prepare aligned CNT films and aligned CNT composite films with remarkable electrical and mechanical properties, a simple and effective method is to use highly aligned CNT arrays as building materials, so the quality of CNT arrays is very important at this point. Herein, CNT arrays with a high quality were synthesized by chemical vapor deposition. The resulting CNT show a multi-walled structure with diameters of7-20nm. The effect of growth parameters including catalyst, gas flow rate, temperature, and time has been carefully explored in the synthesis of CNT arrays. The optimal conditions for the synthesis of ultrahigh CNT arrays were discovered.
Preparation of ultralong aligned CNT films and their application in DSSCs. Currently, aligned CNT films are generally dry-spun from CNT arrays. However, the synthesis of spinnable CNT array remains challenging. In addition, the spinnable array mainly shows a height of300-400μm (typically less than1mm), the resistance of CNT film is very high. It has been well known that the resistance of a CNT film is dominated by the contact resistances among CNTs as the resistances of individual CNTs are very low. Shorter CNTs produce more contact points with higher contact resistances. Therefore, the increase of CNT lengths is critical to improve the application of CNT film in electrode. Herein, a new approach called "adhesion and transfer method" has been developed to produce ultralong aligned CNT films. It represents a general approach in the preparation of CNT films, particularly appropriate for ultrahigh CNT arrays. The resulting ultralong and aligned CNT film indicated a conductivity of1150S/cm at room temperature, compared with～500S/cm for an aligned CNT film by a dry-spinning method. The aligned ultralong CNT film was further used as counter electrode to fabricate DSSCs. The energy conversion efficiency has achieved9.00%, much higher than4.18%for the cell based on the aligned CNT film synthesized by the dry-spinning process and8.05%based on the conventional platinum.
Preparation of horizontally aligned CNT/epoxy composite films and their application in DSSCs. CNTs exhibit high mechanical strength and high electrical conductivity, while polymers could be easily processed with broad source and low cost. The above advantages may be combined by producing a CNT/polymer composite material. Herein, the conventional slice technology has been developed to prepare aligned CNT/epoxy composite film in which CNTs are aligned along the slicing direction. The thickness of the composite film can be accurately controlled from50nm to50μm. The resulting composite film could be also highly flexible, transparent, and conductive, which enable a promising application in electrode. Herein, the composite film has been used as counter electrode to fabricate DSSCs.
Preparation and application of perpendicularly aligned CNT/olefin composite films. Polymer materials such as epoxy, polystyrene, and poly (methy1methacrylate) have been generally used as a second phase in the preparation of CNT composite materials, and solution or burning process has been mainly applied to remove the second phase in case that pure CNTs are required. However, the above post-treatments shares a big and common problem, i.e., difficulty in preparing high-purity CNTs as some impurities are often attached on CNTs. Herein, olefin has been mainly used to prepare vertically aligned CNT composite films also by using a slicing technique. The thickness of the composite film may be controlled from50nm to50μm. Olefin can be then easily removed by evaporation at high temperature at which CNTs would not be affected in both structure and property. Because CNTs are perpendicularly penetrated through the composite film, the lengths of CNTs are accordingly tuned from50nm to50μm. The CNTs were further unzipped into graphene nanoribbons after heating and ultrasonic treatments.
In summary, two new methods have been developed for the preparation of aligned CNT films and composite films with high efficiency. The aligned CNT films showed excellent optical, electrical, and mechanical properties, and exhibited promising applications in various fields, particularly, as a new family of electrode materials. The use of them as counter electrodes in DSSCs have been studied as a demonstration.
超高碳纳米管阵列的制备。为了得到具有优异机械和电学性能的取向碳纳米管膜或复合膜,一个简单且有效的方法是基于高度取向的碳纳米管阵列来制备,因此合成高质量的碳纳米管阵列非常重要。本学位论文主要通过化学气相沉积法来合成多壁碳纳米管阵列(碳纳米管直径7-20纳米),比较系统地研究了催化剂、气体流量、温度、反应时间等实验参数对碳纳米管阵列高度、密度、纯度等的影响规律,确定了制各高质量的较高碳纳米管阵列的最佳条件。
超长取向碳纳米管膜的制备及其在DSSC中的应用。目前取向碳纳米管膜主要通过干法纺丝从碳纳米管阵列中制备,目前合成可纺碳纳米管阵列的实验条件比较苛刻,并且可纺碳纳米管阵列的高度往往在300-400微米,最高一般不超过1毫米,由于单根碳纳米管的电阻极低,因而取向碳纳米管膜的电阻主要来自碳纳米管之间的接触电阻。碳纳米管越长,碳纳米管之间接触点越少,越有利于电子的快速传输,所以增加碳纳米管长度是提高取向碳纳米管膜电极应用的关键因素。本学位论文提出了一种新的粘附转移法,通过普通胶带将碳纳米管从阵列直接转移到各种基底上。该方法操作简单、效率高,尤其适用于高碳纳米管阵列。通过粘附转移法制备的超长取向碳纳米管膜的室温电导率达到1150S/cm,大大超过干法纺丝得到的取向碳纳米管膜的电导率(-500S/cm)。超长取向碳纳米管膜具有良好的柔性,弯曲180。后电导率基本保持不变,即使弯曲500次电导率仅下降1%。以上结果表明超长取向碳纳米管膜代表了一类新型、高效率的电极材料,特别是可用作柔性电极材料。本学位论文以其取代传统铂对电极,构建DSSC,光电转换效率超过9.00%,远高于在同等条件下干法纺丝得到的取向碳纳米管膜作为对电极时的4.18%,也高于铂对电极8.05%。比较系统地研究了超长取向碳纳米管膜厚度以及碳纳米管密度和长度对DSSC性能的影响规律,发现膜厚度为4微米和碳纳米管密度为2×1011cm-2时电池效率最高,且电池效率随着碳纳米管长度的增加而增加。另外,以超长取向碳纳米管膜作为对电极,构建高效率的柔性DSSC,光电转化效率为2.29%,也远高于干法纺丝得到的取向碳纳米管膜在同等条件下的1.22%。
平行取向碳纳米管/环氧树脂复合膜的制备及其在DSSC中的应用。碳纳米管具有优异的机械和电学性能,而高分子来源广泛、结构可控、制备方便,通过形成复合材料可以充分发挥二者的优势。本学位论文发展了一种新的切片技术,制备平行取向碳纳米管/高分子复合薄膜。概括来说,高分子溶液或熔体加入到碳纳米管阵列中,固化后通过传统的切片技术纵向切片即可得到高质量的复合薄膜,膜的厚度可在50纳米到50微米内比较精确地进行调控,复合膜显示良好的柔性、较好的透明性、较高的导电率。以平行取向碳纳米管/环氧树脂复合膜为例,当膜厚度为75纳米时透光率达到94%。因为复合膜具有良好的柔性,所以主要以其作为对电极,构建柔性的DSSC。
垂直取向碳纳米管/石蜡复合膜的制备及其应用。通常制备的取向碳纳米管复合膜主要采用环氧树脂、聚苯乙烯等高分子体系作为填充组分,在很多情况下,虽然可以通过溶剂、燃烧等方法去除,但常常存在后处理和残余物较多等问题。而且在这些复合膜中碳纳米管主要为平行取向,在垂直膜的方向物理性能都比较低。本学位论文以石蜡作为填充组分,通过横向切片制备了垂直取向碳纳米管／石蜡复合膜,复合膜的厚度也可以在50纳米到50微米内进行精确控制。通过真空升华的方法可以轻松有效地去除石蜡,分离出干净的碳纳米管。因为碳纳米管垂直于膜表面且上下贯通,因此碳纳米管长度和直径分布都比较窄。进一步通过加热和超声处理,可以将碳纳米管沿轴向剪开,获得多层石墨烯纳米带,产率接近100%。因为碳纳米管长度和直径都可以比较精确地控制,所以通过本方法可以有效地控制多层石墨烯纳米带的长度和宽度。
综上所述,本论文发展了制备取向碳纳米管膜及其复合膜的两种新方法,这些方法操作方便、效率高,也具有较好的普适性,可以大规模推广使用。取向碳纳米管膜及其复合膜显示优异的光学、电学和机械性能,可广泛用作各种电极材料,这里重点以其作为对电极构建新型DSSC,发现基于取向碳纳米管的DSSC显示较高的效率。
Due to the novel electrical, optical, and mechanical properties, carbon nanotubes (CNTs) exhibit promising applications in a wide variety of fields, such as electrical and optical devices, energy, and biomedicine. However, in many cases, CNTs are required to be further assembled into bulk materials including array, film, and fiber. Among them, the CNT film may represent the most studied system. Unfortunately, as CNTs tend to aggregate during the conventional solution or melt process, it still remains challenging to control and improve the structure and property in the film, which has largely hindered the application in many fields. For instance, CNT films have been widely proposed as electrodes in organic solar cells such as dye-sensitized solar cells (DSSCs). DSSCs have been considered as the third generation solar cells and extensively investigated due to a low cost, easy fabrication, and high energy conversion efficiency. The development of new electrode materials represents a promising direction to improve the cell efficiency with target for a practical application. Therefore, CNT films have been widely explored for the electrode in DSSCs, particularly, as counter electrode to replace the conventional expensive and unstable platinum. However, the aggregated structure of CNTs has greatly lowered the efficiency of the resulting cell. To further improve the structure and property of CNT film, it is critically important to realize a high alignment of CNTs. Herein, two new methods have been developed for the preparation of aligned CNT films and composite films, and the use of them as counter electrodes to fabricate highly efficient DSSCs was carefully studied in this thesis. The main work is summarized as bellow.
Synthesis of ultrahigh CNT array. To prepare aligned CNT films and aligned CNT composite films with remarkable electrical and mechanical properties, a simple and effective method is to use highly aligned CNT arrays as building materials, so the quality of CNT arrays is very important at this point. Herein, CNT arrays with a high quality were synthesized by chemical vapor deposition. The resulting CNT show a multi-walled structure with diameters of7-20nm. The effect of growth parameters including catalyst, gas flow rate, temperature, and time has been carefully explored in the synthesis of CNT arrays. The optimal conditions for the synthesis of ultrahigh CNT arrays were discovered.
Preparation of ultralong aligned CNT films and their application in DSSCs. Currently, aligned CNT films are generally dry-spun from CNT arrays. However, the synthesis of spinnable CNT array remains challenging. In addition, the spinnable array mainly shows a height of300-400μm (typically less than1mm), the resistance of CNT film is very high. It has been well known that the resistance of a CNT film is dominated by the contact resistances among CNTs as the resistances of individual CNTs are very low. Shorter CNTs produce more contact points with higher contact resistances. Therefore, the increase of CNT lengths is critical to improve the application of CNT film in electrode. Herein, a new approach called "adhesion and transfer method" has been developed to produce ultralong aligned CNT films. It represents a general approach in the preparation of CNT films, particularly appropriate for ultrahigh CNT arrays. The resulting ultralong and aligned CNT film indicated a conductivity of1150S/cm at room temperature, compared with～500S/cm for an aligned CNT film by a dry-spinning method. The aligned ultralong CNT film was further used as counter electrode to fabricate DSSCs. The energy conversion efficiency has achieved9.00%, much higher than4.18%for the cell based on the aligned CNT film synthesized by the dry-spinning process and8.05%based on the conventional platinum.
Preparation of horizontally aligned CNT/epoxy composite films and their application in DSSCs. CNTs exhibit high mechanical strength and high electrical conductivity, while polymers could be easily processed with broad source and low cost. The above advantages may be combined by producing a CNT/polymer composite material. Herein, the conventional slice technology has been developed to prepare aligned CNT/epoxy composite film in which CNTs are aligned along the slicing direction. The thickness of the composite film can be accurately controlled from50nm to50μm. The resulting composite film could be also highly flexible, transparent, and conductive, which enable a promising application in electrode. Herein, the composite film has been used as counter electrode to fabricate DSSCs.
Preparation and application of perpendicularly aligned CNT/olefin composite films. Polymer materials such as epoxy, polystyrene, and poly (methy1methacrylate) have been generally used as a second phase in the preparation of CNT composite materials, and solution or burning process has been mainly applied to remove the second phase in case that pure CNTs are required. However, the above post-treatments shares a big and common problem, i.e., difficulty in preparing high-purity CNTs as some impurities are often attached on CNTs. Herein, olefin has been mainly used to prepare vertically aligned CNT composite films also by using a slicing technique. The thickness of the composite film may be controlled from50nm to50μm. Olefin can be then easily removed by evaporation at high temperature at which CNTs would not be affected in both structure and property. Because CNTs are perpendicularly penetrated through the composite film, the lengths of CNTs are accordingly tuned from50nm to50μm. The CNTs were further unzipped into graphene nanoribbons after heating and ultrasonic treatments.
In summary, two new methods have been developed for the preparation of aligned CNT films and composite films with high efficiency. The aligned CNT films showed excellent optical, electrical, and mechanical properties, and exhibited promising applications in various fields, particularly, as a new family of electrode materials. The use of them as counter electrodes in DSSCs have been studied as a demonstration.
引文
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