CN103972514A - 一种新型三维纳米碳/不锈钢网复合生物阳极及其制备方法与用途 - Google Patents
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Abstract
本发明公开了一种新型三维纳米碳/不锈钢网复合生物阳极及其制备方法与用途,该三维生物阳极是以纳米碳和不锈钢网为原材料,通过折叠和吸附组装构建而成。该三维纳米碳/不锈钢网复合生物阳极显示出优异的导电性能和机械性能,易加工成型;同时其在微生物燃料电池中具有优异的微生物电化学性能,其产生的面积电流密度高达40~300A/m2,体积电流密度高达5~35kA/m3。该电极材料可作为微生物燃料电池的阳极,并应用于污水处理、生物修复等领域。
Description
技术领域
本发明涉及一种新型三维纳米碳/不锈钢网复合生物阳极及其制备方法与用途。
背景技术
电极材料的成本和性能对像微生物燃料电池(MFC)这样的微生物电化学系统的发展和应用起着非常关键的作用。碳材料具有良好的稳定性和微生物附着性能,因此不同结构的碳材料及其复合材料已被广泛用于作为MFCs的电极材料或集流体主要可分为一下两大类:(1)块状或粒状的多孔碳材料,如碳纸、碳纤维毡、网状的玻璃碳(RVC)、堆积的碳颗粒和石墨纤维刷、基于天然资源的三维多孔碳材料等;(2)粉状的碳材料,如碳纳米管、石墨烯、活性碳和碳黑等。块状多孔碳材料,一般直接作为电极使用或通过导电黏结剂固定在石墨或金属等集流体上制成电极使用。然而,块状碳电极具有机械强度低、本体电阻大、与外电连接的接触电阻大等缺点,其实际应用具有一定的局限性。粉状的碳材料可以通过以下两种方法制成电极:(1)黏结法:即采用聚合物粘结剂将粉状的碳材料固定到集流体上;(2)物理吸附法:以多孔聚合物为支撑体,通过分子间相互作用力吸附固定纳米碳,如碳纳米管、石墨烯等,形成纳米碳/聚合物复合电极。用黏结法制备的电极的孔隙率较低,其作为生物阳极时只能允许有限的微生物膜生长,产电效率低;其作为氧气还原阴极时,部分碳纳米材料催化剂的催化位点被粘结剂覆盖,利用率降低。采用物理吸附法制备的纳米碳/聚合物复合电极的支撑体为不导电的聚合物。电极主要靠吸附的纳米碳层导电,因此复合电极的内阻较大,其大规模应用将受到限制。
金属材料,如不锈钢等,具有高的导电性、优异的机械强度、耐腐蚀、低成本以及易成型加工等优点,被广泛用来作为MFC的电极或集流体。不锈钢表面的微生物附着性能相对较差,因此其直接作为生物阳极或生物阴极的产电效率较低【C. Dumas, A. Mollica, D. Feron, R. Basseguy, L. Etcheverry and A. Bergel, Electrochimica Acta, 2007, 53, 468-473】。采用化学气相沉积或火焰合成的方法,在不锈钢上原位修饰一层碳纳米材料,可以极大提高不锈钢电极表面的微生物附着性能【J. L. Lamp, J. S. Guest, S. Naha, K. A. Radavich, N. G. Love, M. W. Ellis and I. K. Puri, Journal of Power Sources, 2011, 196, 5829-5834】。但是,化学气相沉积或火焰合成等生长纳米碳的方法需要经历高温过程(如超过500 oC)。而高温热处理会改变不锈钢中金属的晶体结构和元素分布,产生元素偏析,从而极大降低了不锈钢基体的耐腐蚀性能。因此,采用该方法制备的纳米碳/不锈钢复合电极在MFC中的应用受到了极大的限制。
发明内容
针对目前MFC阳极规模化应用的限制,本发明结合纳米碳材料和不锈钢材料的优点,目的在于提供一种新型三维纳米碳/不锈钢网复合生物阳极及其制备方法。 为了实现上述目的,本发明采取的技术方案是:
(1) 将纳米碳材料均匀分散在分散介质中(如水、酒精等溶剂),形成均一的纳米碳分散液;
(2)将不锈钢网一定角度折叠形成的三维折叠结构,如图1所示;
(3)将三维折叠不锈钢网放入1 mol/L稀酸溶液 (如盐酸、硫酸和磷酸等) 浸泡1~4 h,进行表面处理,以达到一种粗糙表面的效果;
(4)将表面处理的三维折叠不锈钢网浸入到纳米碳分散液中,几分钟后取出烘干,并重复浸入/烘干循环1 ~ 5次;
纳米碳材料是碳纳米管、石墨烯和炭黑等具有1~ 100纳米尺寸的碳材料,分散介质为水、酒精等常用溶剂,分散液的浓度为2 ~ 20 g/L;
所示的不锈钢网,其材质包括SUS302、304、304L、316、316L、310s等,其孔隙大小为20 ~ 200目。
所述的一种新型三维纳米碳/不锈钢网复合生物阳极中的三维结构,其特征是按一定角度折叠而成的三维折叠结构,如图1所示。
所述的一种新型三维纳米碳/不锈钢网复合生物阳极,其折叠角度θ的范围为0 ~ 60o,电极厚度δ的范围为0.5 ~ 10 cm。
一种新型三维纳米碳/不锈钢网复合生物阳极,不锈钢网折叠成三维折叠结构,折叠后的不锈钢网表面覆盖有纳米尺寸的碳材料层形成复合生物阳极,其中不锈钢网折叠角度θ为0 ~ 60o,电极厚度δ的范围为0.5 ~ 10 cm。
所述的一种新型三维纳米碳/不锈钢网复合生物阳极的用途,所述新型三维纳米碳/不锈钢网复合生物阳极用于微生物燃料电池的生物阳极,其微生物电催化面积电流密度高达40 ~ 300 A/m2,体积电流密度高达5~ 35 kA /m3。
本发明结合了不锈钢材料的优点,高导电性,优异的机械性能等优点,以及碳纳米材料的优点优异的微生物附着性能,构建了复合的纳米碳/不锈钢网电极材料。其扫描电镜图如附图2;同时通过折叠形成三维结构,增加可供微生物生长的面积,从而可极大增加微生物数量和提高产电电流密度。因此,所述的新型三维纳米碳/不锈钢网复合生物阳极用于微生物燃料电池,其作用效果的特征是该阳极具有以下优异性能:
(a)优异的导电性能和机械性能;
(b)良好的微生物附着性能,其微生物电催化面积电流密度高达40 ~ 300 A/m2,体积电流密度高达5 ~ 35 kA /m3;
(c)低成本、易加工成型。
该新型三维纳米碳/不锈钢网复合电极可作为微生物燃料电池的阳极,并应用于污水处理、生物修复等领域。
附图说明
图1 新型三维纳米碳/不锈钢网复合生物阳极中的三维折叠结构示意图;
图2 纳米碳/不锈钢网复合电极的扫描电镜图;
图3 产电电流密度曲线,(A)纯不锈钢网(bare SSM)生物阳极,(B)炭黑/不锈钢网(CB/SSM)生物阳极;
图4(A和B)纯不锈钢网生物阳极以及(C和D)炭黑/不锈钢网生物阳极中的微生物膜的扫描电镜图片。
具体实施方式
实施实例:
1.单层的纳米碳/不锈钢网复合阳极的制备及产电性能测试
将目数为50目的304不锈钢网浸入1 mol/L 的硫酸溶液中浸泡1小时,用蒸馏水清洗干净后,浸入到5 g/L 的炭黑/酒精分散液中,取出烘干,并重复浸泡/烘干步骤3次,得到单层的纳米碳/不锈钢网复合阳极。
选用不同材质或目数的不锈钢网,重复上述步骤可制备不同孔隙大小的纳米碳/不锈钢网复合阳极。
阳极性能的测试条件见文献【Guanghua He, Yanli Gu, Shuijian He, Uwe Schreoer, Shuiliang Chen, Haoqing Hou. Effect of fiber diameter on the behavior of biofilm and anodic performance of fiber electrodes in microbial fuel cells. Bioresour. Technol.10763-10766 (2011)】,具体实验过程如下:以市政污水厂的活性污泥为接种体(南昌青山湖污水厂),通过电化学驯化1星期,筛选出电化学活性的微生物膜,并以之为阳极性能测试的接种体。以人造污水为媒介,醋酸钠为微生物的底物,采用电化学工作站的电流-时间技术来测试电极的阳极性能,即给工作电极施加0.2V(vs. Ag/AgCl参比电极)的电势,记录电流信号;测试过程中采用连续溶液或磁力搅拌溶液供给。在此条件下,测得以传统石墨板阳极的电流密度为11.1 A/m2,石墨毡(纤维直径10微米)阳极的电流密度为16.2 A/m2, 单层50目纯不锈钢网阳极的电流密度为0.025 A/m2,单层纳米碳/不锈钢网复合阳极的电流密度为15.5 A/m2。
不同目数的单层纳米碳/不锈钢网复合阳极的产电性能结果如下:
目数 | 不锈钢材质 | 电流密度 A/m2 |
10 | 304 | 8.9 |
20 | 304 | 10.4 |
30 | 304 | 12.7 |
50 | 304 | 15.5 |
50 | 316L | 13.8 |
60 | 304 | 14.1 |
2. 三维纳米碳/不锈钢网复合阳极的制备及产电性能测试
将目数为50目的304不锈钢网浸入1 mol/L 的硫酸溶液中浸泡1小时,用蒸馏水清洗干净后。将不锈钢网以30o 的角度折叠成厚度为6 mm 的三维不锈钢网,再将其浸入到5 g/L 的炭黑/酒精分散液中,取出烘干,并重复浸泡/烘干步骤3次,三维纳米碳/不锈钢网复合阳极。
重复上述步骤可制备角度分别为5o,10o,20 o,45 o,60 o,厚度任何尺寸的三维纳米碳/不锈钢网复合生物阳极。
不同尺寸三维纳米碳/不锈钢网复合阳极的性能测试结果如下:
角度 | 厚度/mm | 面积电流密度 A/m2 | 体积电流密度 A/m3 |
0 o | 6 | ||
5 o | 6 | 130.5 | 23.84 |
5 o | 10 | 180.5 | 20.11 |
5 o | 15 | 250.5 | 15.23 |
10 o | 6 | 101.6 | 18.42 |
20 o | 6 | 64.5 | 11.84 |
30 o | 6 | 47.9 | 8.97 |
45 o | 6 | 32.7 | 6.57 |
60 o | 6 | 25.9 | 4.32 |
与传统块三维多孔碳阳极材料相比,本发明所述的新型三维纳米碳/不锈钢网复合生物阳极具有更优异的导电性能和机械性能;同时,单层的纳米碳/不锈钢网复合生物阳极的产电电流密度为15 .5 A/m2(1.55 mA/cm2),如附图3 B,与传统石墨毡相当。单层的纳米碳/不锈钢网可加工成不同形状,形成三维阳极,具有更优异的产电性能,如附图3。
与纯不锈钢等金属电极相比,纳米碳/不锈钢网复合生物阳极具有更优的微生物附着性能。 纳米碳/不锈钢网复合生物阳极可产生比纯不锈钢网生物阳极的产电电流密度0.025 A/m2(0.0025 mA/cm2)高500多倍,如附图3A。附图4的微生物膜的扫描电镜形貌分析显示,产电后纳米碳/不锈钢网复合阳极被厚厚的微生物膜包裹,微生物膜的厚度超过了10微米;而纯SSM电极上微生物膜的比较稀疏,厚度只有约3微米。
Claims (5)
1.一种新型三维纳米碳/不锈钢网复合生物阳极,其特征在于:不锈钢网折叠成三维折叠结构,折叠后的不锈钢网表面覆盖有纳米尺寸的碳材料层形成复合生物阳极,其中不锈钢网折叠角度θ为0 ~ 60o,电极厚度δ的范围为0.5 ~ 10 cm。
2.一种权利要求1所述的一种新型三维纳米碳/不锈钢网复合生物阳极的用途,其特征在于所述新型三维纳米碳/不锈钢网复合生物阳极用于微生物燃料电池的生物阳极,其微生物电催化面积电流密度高达40 ~ 300 A/m2,体积电流密度高达5 ~ 35 kA /m3。
3.一种权利要求1中所述的新型三维纳米碳/不锈钢网复合生物阳极的制备方法,其特征是方法步骤如下:
(1) 将纳米碳材料均匀分散在分散介质中,形成均一的纳米碳分散液;
(2)将不锈钢网折叠形成三维折叠结构;
(3)将三维折叠不锈钢网放入稀的酸溶液浸泡1 ~ 4 h,进行表面处理,以达到一种粗糙表面的效果;
(4)将表面处理的三维折叠不锈钢网浸入到纳米碳分散液中,几分钟后取出烘干,并重复浸入/烘干循环1 ~ 5次。
4.根据权利要求1、3所述的一种新型三维纳米碳/不锈钢网复合生物阳极,其特征在于:纳米碳材料是碳纳米管、石墨烯和炭黑等具有1~ 100纳米尺寸的碳材料,分散介质为水、酒精等常用溶剂,分散液的浓度为2 ~ 20 g/L。
5. 根据权利要求1、3所述的一种新型三维纳米碳/不锈钢网复合生物阳极,其特征在于:所述的不锈钢网,其材质包括SUS302、304、304L、316、316L、310s等,其孔隙大小为20 ~ 200目。
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