CN106568811A - 一种基于Cu‑BTC/聚吡咯纳米线/石墨烯纳米复合材料的氨气传感器及其制备方法 - Google Patents
一种基于Cu‑BTC/聚吡咯纳米线/石墨烯纳米复合材料的氨气传感器及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于Cu‑BTC/聚吡咯纳米线/石墨烯纳米复合材料的氨气传感器及其制备方法,包括氨气传感器和氨敏感纳米复合材料,所述氨敏感纳米复合材料为Cu‑BTC、聚吡咯纳米线、石墨烯纳米复合材料,氨敏感纳米复合材料固定于ITO导电玻璃上。该氨气传感器可以在室温条件下定量检测氨气的浓度,而且操作简便,重现性好。所述聚吡咯纳米线/石墨烯复合材料具有良好的化学稳定性和独特的化学结构,诱导了纳米Cu‑BTC的合成,另一方面,Cu‑BTC有效地提高了复合材料的比表面积,对氨气有良好的吸附作用,两者协同作用,提高了在室温下氨气检测的灵敏度和选择性,而且还具有工艺简单,应用范围广和制造成本低等优点。
Description
技术领域
本发明涉及氨气传感器,具体地说是一种基于Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料的氨气传感器及其制备方法和应用。
背景技术
氨气(NH3)是一种无色弱碱性气体,极易溶于水,1体积水可以溶700体积的NH3,有强烈刺激性气味 ,有一定的腐蚀性。此外, NH3还对人体的感官有明显的刺激性,这都是因为氨气分子很小,极易泄漏,而且氨气无色,爆炸极限范围宽,遇明火即发生爆炸。一旦发生事故,将对人的生命和国家的财产安全造成严重的危害,因此,NH3检测显得尤为重要。现有的技术中对氨气泄露的检测一般采用敏感元件,多为无定量的检测,只给出简单的报警信息,而且大部分要在高温下才能实现检测,因此,定量检测室温空气中的氨气的含量显得尤为重要。
发明内容
本发明的目的在于提供了一种基于Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料的氨气传感器及其制备方法和应用。
为达到上述目的,本发明的技术方案是:
一种基于Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料的氨气传感器,包括氨气传感器和氨敏感纳米复合材料,所述氨敏感纳米复合材料为Cu-BTC、聚吡咯纳米线、石墨烯纳米复合材料,氨敏感纳米复合材料固定于ITO导电玻璃上。
所述氨气传感器的制备方法是,先制备Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料,再将其负载在到ITO导电玻璃上,最后组装成氨气传感器。
所述制备Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料,先采用原位化学聚合法合成聚吡咯纳米线/石墨烯纳米复合材料,再采用水热法,在聚吡咯纳米线/石墨烯复合材料上沉积Cu-BTC,其中石墨烯的重量负载量为0.1-10%,Cu-BTC的颗粒大小为50-100纳米。
所述制备Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料过程如下:
在烧瓶中加入0.1-1 mol/L的吡咯、0.1 -1mol/L的十六烷基三甲基溴化铵、0.1-1mol/L的柠檬酸和过量的去离子水,在磁力搅拌器上搅拌3小时;
然后,再在混合液中用滴定管缓慢加入0.5 mol/L的过硫酸铵溶液20-50 mL,继续搅拌4小时后取出,在溶剂过滤器上用去离子水和无水乙醇反复清洗,得到的固体物品在真空干燥箱中60℃干燥12小时后取出,得到聚吡咯纳米线/石墨烯复合材料;
取0.5 g制备的聚吡咯纳米线/石墨烯复合材料加入含有0.1-0.5mol/L均苯三甲酸、0.1-0.5 mol/L 硝酸铜、12-50 mLDMF,12-50 mL 乙醇和8-20mL 水的溶液中超声分散1h,转移到反应釜中,盖上盖子,置于80-120℃烘箱中反应24h, 过滤、洗涤、干燥得到Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料。
所述组装成氨气传感器包括如下步骤:
(1)在ITO导电玻璃上贴上两条导电铜箔,其大小为 0.5 cm×4 cm规格,两片铜箔间距为5 mm,
(2)取Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料粉末在5 mL的乙醇中超声30分钟,用注射器取出1 mL超声液加到两片铜箔胶之间并在空气中干燥,接上导线,即组装成氨气传感器。
本发明氨气传感器的应用,可通过氨敏感纳米复合材料电阻的变化来检测空气或样品气中氨气的浓度;其可以在常温常压下检测氨气的浓度,所检测氨气的质量浓度范围为10-200 ppm,而且对氢气、H2S、甲醇和CH4等气体具有良好的选择性。
本发明的工作原理:聚吡咯纳米线/石墨烯纳米复合材料为P型半导体材料,当在石墨烯上复合聚吡咯后,电荷从聚吡咯转移到石墨烯,从而使聚吡咯带上正电荷,而氨气为还原性气体,可以提供给聚吡咯纳米线/石墨烯纳米复合材料电子,从而使聚吡咯纳米线/石墨烯纳米复合材料电阻升高。但聚吡咯纳米线/石墨烯纳米复合材料的比表面积有效,吸附的氨气数量少,从而使其对氨气的响应差。Cu-BTC沉积在聚吡咯纳米线/石墨烯纳米复合材料后,使材料的比表面积显著增大,对气体的吸附也明显增强,从而提高了其对氨气检测的灵敏度。
本发明具有如下优点:
1.有效提高了氨气检测的灵敏度。由于Cu-BTC具有大的比表面积,对氨有特殊的亲和力,但其导电性差,因此不能独立用于电阻式气体传感器的敏感材料。但将其负载到聚吡咯纳米线/石墨烯复合材料上,可以起到富集氨气的作用。而聚吡咯纳米线/石墨烯复合材料复合材料对氨气有良好的响应,两者协同作用,可以提高了氨气检测的灵敏度。
2. Cu-BTC通常颗粒很大,一般粒径可达几个微米,但聚吡咯纳米线/石墨烯复合材料可以诱导纳米Cu-BTC的合成,得到具有更高比表面的复合材料。
3. 本发明采用Cu-BTC/聚吡咯纳米线/石墨烯复合材料作为氨气敏感材料来检测氨气,利用复合材料电阻的变化来检测氨气的浓度,可定量检测氨气的泄露。
4.应用效果好。Cu-BTC和聚吡咯纳米线/石墨烯相互作用,相互协同,提高了氨气检测的灵敏度和选择性。
5.制备工艺简单,产品性能稳定。复合材料的制备采用原位化学聚合和水热法相结合的方法完成,不需要复杂的步骤,适合大量的制备,而且保证了材料制备的重现性。
6.使用方便。本发明氨气传感器可以在室温条件下定量检测氨气的浓度,而且操作简便,重现性好。
7.本发明氨气传感器还具有工艺简单,应用范围广和制造成本低等优点。
附图说明
图1为本发明Cu-BTC和Cu-BTC/聚吡咯纳米线/石墨烯复合材料的扫描电镜图;
图2为实施例1的氨气传感器对氨气浓度的响应曲线;
图3为实施例1氨气传感器的工作曲线。
具体实施方式
实施例1
制备基于Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料的氨气传感器:
(1)在烧瓶中加入0.1mol/L的吡咯、0.1mol/L的十六烷基三甲基溴化铵、0.1 mol/L的柠檬酸和过量的去离子水,在磁力搅拌器上搅拌3小时;
(2)再步骤(1)在混合液中用滴定管缓慢加入0.5 mol/L的过硫酸铵溶液20 mL,继续搅拌4小时后,过滤,洗涤,60℃干燥;
(3)取0.5 g制备的聚吡咯纳米线/石墨烯复合材料加入含有0.1mol/L均苯三甲酸、0.1mol/L 硝酸铜、20 mLDMF,12 mL 乙醇和8 mL 水的溶液中超声分散1h;
(4)将步骤(3)中的溶液转移到反应釜中,盖上盖子,置于80℃烘箱中反应24h, 过滤、洗涤、干燥得到Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料,再将其负载在到ITO导电玻璃上;
(5)在ITO导电玻璃上贴上两条导电铜箔,其大小为 0.5 cm×4 cm规格,两片铜箔间距为5 mm;
(6)取Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料粉末在5 mL的乙醇中超声30分钟,用注射器取出1 mL超声液加到两片铜箔胶之间并在空气中干燥,接上导线,通过测试复合材料在氨气中的电阻变化来检测空气或样品气中氨气的浓度。
图1为本发明Cu-BTC和Cu-BTC/聚吡咯纳米线/石墨烯复合材料的扫描电镜图;从图1可以看出,Cu-BTC为棱柱状的颗粒,其大小约为15 微米,而在聚吡咯/石墨烯复合材料上的Cu-BTC粒径明显减小,其粒径约为100 nm。
图2为实施例1的氨气传感器对氨气浓度的响应曲线;从图2中可以看出,随着氨气浓度的增大,其响应也明显增大。
图3为实施例1氨气传感器的工作曲线;从图3中可以看出,在10-150 ppm范围内,表现出良好的线性关系。
实施例2
制备基于Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料的氨气传感器:
(1)在烧瓶中加入0.2mol/L的吡咯、0.15mol/L的十六烷基三甲基溴化铵、0.2 mol/L的柠檬酸和过量的去离子水,在磁力搅拌器上搅拌3小时;
(2)再步骤(1)在混合液中用滴定管缓慢加入0.5 mol/L的过硫酸铵溶液30 mL,继续搅拌4小时后,过滤,洗涤,60℃干燥;
(3)取0.5 g制备的聚吡咯纳米线/石墨烯复合材料加入含有0.1mol/L均苯三甲酸、0.2mol/L 硝酸铜、12 mL DMF,15 mL 乙醇和8 mL 水的溶液中超声分散1h;
(4)将步骤(3)中的溶液转移到反应釜中,盖上盖子,置于85℃烘箱中反应24 h, 过滤、洗涤、干燥得到Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料;
(5)在ITO导电玻璃上贴上两条导电铜箔,其大小为 0.5 cm×4 cm规格,两片铜箔间距为5 mm;
(6)取Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料粉末在5 mL的乙醇中超声30分钟,用注射器取出1 mL超声液加到两片铜箔胶之间并在空气中干燥,接上导线,通过测试复合材料在氨气中的电阻变化来检测空气或样品气中氨气的浓度。
Claims (7)
1.一种基于Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料的氨气传感器,包括氨气传感器,其特征在于:还包括氨敏感纳米复合材料,所述氨敏感纳米复合材料为Cu-BTC、聚吡咯纳米线、石墨烯纳米复合材料,氨敏感纳米复合材料固定于ITO导电玻璃上。
2.根据权利要求1所述的氨气传感器的制备方法,其特征在于:先制备Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料,再将其负载在到ITO导电玻璃上,最后组装成氨气传感器。
3.根据权利要求2所述的氨气传感器的制备方法,其特征在于:所述制备Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料,先采用原位化学聚合法合成聚吡咯纳米线/石墨烯纳米复合材料,再采用水热法,在聚吡咯纳米线/石墨烯复合材料上沉积Cu-BTC,其中石墨烯的重量负载量为0.1-10%,Cu-BTC的颗粒大小为50-100纳米。
4.根据权利要求3所述的氨气传感器的制备方法,其特征在于:所述制备Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料过程如下:
在烧瓶中加入0.1-1 mol/L的吡咯、0.1 -1mol/L的十六烷基三甲基溴化铵、0.1-1mol/L的柠檬酸和过量的去离子水,在磁力搅拌器上搅拌3小时;
然后,再在混合液中用滴定管缓慢加入0.5 mol/L的过硫酸铵溶液20-50 mL,继续搅拌4小时后取出,在溶剂过滤器上用去离子水和无水乙醇反复清洗,得到的固体物品在真空干燥箱中60℃干燥12小时后取出,得到聚吡咯纳米线/石墨烯复合材料;
取0.5 g制备的聚吡咯纳米线/石墨烯复合材料加入含有0.1-0.5mol/L均苯三甲酸、0.1-0.5 mol/L 硝酸铜、12-50 mLDMF,12-50 mL 乙醇和8-20mL 水的溶液中超声分散1h,转移到反应釜中,盖上盖子,置于80-120℃ 烘箱中反应24h, 过滤、洗涤、干燥得到Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料。
5.根据权利要求2所述的氨气传感器的制备方法,其特征在于,所述组装成氨气传感器包括如下步骤:
(1)在ITO导电玻璃上贴上两条导电铜箔,其大小为 0.5 cm×4 cm规格,两片铜箔间距为5 mm,
(2)取Cu-BTC/聚吡咯纳米线/石墨烯纳米复合材料粉末在5 mL的乙醇中超声30分钟,用注射器取出1 mL超声液加到两片铜箔胶之间并在空气中干燥,接上导线,即组装成氨气传感器。
6.根据权利要求2-5任一项所述制备方法制备的氨气传感器的应用,其特征在于:所述氨气传感器可通过氨敏感纳米复合材料电阻的变化来检测空气或样品气中氨气的浓度。
7.根据权利要求6所述氨气传感器的应用,其特征在于:所述氨气传感器可以在常温常压下检测氨气的浓度,所检测氨气的质量浓度范围为10-200 ppm,而且对氢气、H2S、甲醇和CH4气体具有良好的选择性。
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