纳米传感材料制备及性能研究
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摘要
本文分别利用苯胺的化学及电化学原位聚合制备了聚苯胺(PANI)纳米纤维,分别在丝网印刷电极(SPE)及石墨箔(GF)上,构建了PANI纳米纤维传感元件Nano-PANI/SPE及Nano-PANI/GF。通过电化学氧化膨胀石墨箔,制备了附着于石墨箔上的氧化石墨烯GONS。
在丝网印刷电极分支间绝缘带上,采用0.2mol·dm-3苯胺的1.0mol·dm-3盐酸溶液,以FeCl3为氧化剂原位聚合苯胺,制备PANI纳米纤维,构建nano-PANI/SPE传感元件。利用SEM观测了位于Nano-PANI/SPE碳电极分支间绝缘带上PANI的形貌,发现PANI在以直径约60nm的纳米纤维形式存在,纳米纤维相互交叉,形成孔径约为300～400nm的均匀多孔结构。
监测了Nano-PANI/SPE传感元件对挥发性有机化合物及氨气的电阻响应,分析了这些气体对PANI电阻的影响。Nano-PANI/SPE传感元件对氯代甲烷、小分子醇、甲苯、三乙胺及氨气均有迅速的电阻响应。由于氨气对PANI具有强脱质子掺杂作用,传感元件对氨气响应灵敏度最高、检测限最低,理论检测限达0.45ppb。Nano-PANI/SPE传感元件具有较好的电阻稳定性,空气中放置一周后,电阻仅增加3.86%。
石墨箔为工作电极,在含有0.2mol·dm-3苯胺的1.0mol·dm-3的盐酸溶液中,通过循环伏安法进行苯胺的电化学聚合,制备了PANI纳米纤维修饰石墨箔电极Nano-PANI/GF。利用FTIR研究了修饰电极上聚合物的振动吸收,利用SEM观测了其形貌。用循环伏安法研究了Nano-PANI/GF修饰电极在0.1mol·dm-3的磷酸盐缓冲溶液(pH6.9)中的电化学活性。发现1～6次循环伏安扫描聚合后,制备的Nano-PANI/GF修饰电极的电化学活性随着聚合扫描次数增加而增加。但由于该PANI在中性溶液中的电化学活性源于石墨箔与PANI之间的电荷传递作用,增加循环伏安扫描次数继续聚合苯胺对电化学活性基本无贡献。
利用循环伏安法研究了Nano-PANI/GF修饰电极对抗坏血酸电化学氧化的催化作用。计时电流实验结果表明,在0.2V电位条件下,1.7～2.0×103μmol·dm-3浓度范围内,抗坏血酸在Nano-PANI/GF修饰电极上的氧化电流与浓度成线性关系,线性方程式为i(mA)=0.0031+0.00013[AA](mmol·dm-3),R2=O.9994,灵敏度为0.13mA·cm-2·mmol-1·dm3,检测限为1.7μmol·dm-3。
以石墨箔为原料,通过电化学氧化膨胀制备了附着于石墨箔表面的氧化石墨烯(GONS)。利用XPS和FTIR分析了氧化石墨烯组成,利用SEM观测其形貌,发现氧化石墨烯片层最低可达到4nm。
利用循环伏安法研究了GONS对抗坏血酸(AA)电化学氧化的催化活性。OV的计时电流实验结果表明,在5.0×10-4～1.0mmol·dm-3浓度范围内,GONS上的响应电流与AA浓度成线性关系,线性方程式为i(mA)=0.0022+0.10[AA](mmol·dm-3),R2=0.9967;灵敏度为0.10mA·cm-2·mol-1·dm3,检测限为0.5μmol·dm-3。浓度为0.25mmol·dm-3的AA的3次测试相对标准偏差为3.8%。柠檬酸(CA)、葡萄糖(Glu)、乳酸(LA)、尿酸(UA)和多巴胺(DA)等常见干扰物在GONS上的氧化电位较高,对AA测试无明显干扰。利用GONS检测了三种饮料中的AA,加入标准样品的回收率达92.0～100.5%。
循环伏安及脉冲伏安实验结果表明,GONS对多巴胺(DA)、尿酸(UA)和对乙酰氨基酚(APAP)也有很好的电流响应。在25～200μmol·dm-3浓度范围内,DA的氧化峰电流与其浓度呈现良好的线性关系,线性相关方程为ip(μA)=4.6+0.90[DA](μmol·dm-3),R2=0.9908。DA在GONS上的检测限为4.6μmol·dm-3,灵敏度为0.90μA·cm-2·μmol-1·dm3,3次测定80μmol·dm-3DA的相对标准偏差为2.3%。在25～130μmol·dm-3浓度范围内,UA的氧化峰电流与其浓度呈现良好的线性关系,线性相关方程为ip(μA)=0.010+0.90[UA](μmol·dm-3),R2=0.9975。UA在GONS上的检测限为2.4μmol·dm-3,灵敏度为0.90μA·cm-2·μmol-1·dm3,3次测定80μmol·dm-3UA得到相对标准偏差为4.3%。在40～200μmol·dm3浓度范围内,APAP的氧化峰电流与其浓度呈现良好的线性关系,线性相关方程为ip(μA)=-0.055+1.8[APAP](μmol·dm-3),R2=0.9961.APAP在GONS上的检测限为1.9μmol·dm-3,灵敏度为1.8μA·cm-2·μmol-1·dm3,3次测定200μmol·dm-3APAP得到相对标准偏差为4.4%。
GONS的循环伏安曲线及差分脉冲伏安曲线上,AA、DA、UA和APAP的氧化峰相互独立,峰电位相差70mV以上,表明在磷酸盐缓冲溶液(pH6.9)的中,AA、DA、UA和APAP在GONS上同时检测有很好的可行性。
Polyaniline (PANI) nanofibers were prepared through in situ chemical and electrochemical polymerization of aniline. PANI nanofibers were fabricated onto screen-printed electrode (SPE) and graphite foil (GF) to construct sensors of Nano-PANI/SPE and Nano-PANI/GF respectively. Graphene oxide nano sheets (GONS) were prepared by electrochemical exfoliation of graphite foil.
Nano-PANI/SPE sensor was constructed by in situ chemical polymerization of aniline on the insulate gap of the SPE by drop coating method, using iron chloride as oxidant. The morphologies of the PANI on the gap were investigated by scanning electron microscopy (SEM). It can be seen from the SEM images that the film was composed of interconnected nanofibers of ca.60nm in diameter to form pores of ca.300-400nm in diameter.
The responses of the Nano-PANI/SPE sensor upon exposure to common volatile organic compounds (VOCs) and ammonia were investigated. It was found that the sensor responsed quickly on exposure to chloromethane, small molecular alcohols, toluene, triethylamine and ammonia. The sensor has higher sensitivity and lower detection limit (0.45ppb) when it was used in sensing ammonia because of the strong de-protonation of PANI by ammonia. The Nano-PANI/SPE sensor has better stability, the resistant of the sensor increased only about3.86%when it was on exposure to air for one week.
Polyaniline nano fiber (Nano-PANI) modified graphite foil (GF), Nano-PANI/GF was prepared by electrochemical polymerization of aniline on GF electrode in a solution of0.2mol·dm-3aniline and1.0mol·dm-3HCl. The polymer on the modified electrode Nano-PANI/GF was characterized by FTIR. The morphologies of the modified electrode were investigated by SEM. The electrochemistry activity of Nano-PANI/GF was investigated in0.1mol·dm-3phosphate buffer solution (pH6.9) by cyclic voltammetry (CV). The electrochemistry activity of Nano-PANI/GF increased along with the cyclic number of CV for the electropolymerization of aniline in the first six cycles as the electroactivity was related to charge transfer between graphite foil and PANI.
The electrocatalytic properties of the Nano-PANI/GF modified electrode towards ascorbic acid (AA) oxidation were studied through cyclic voltammetry. The current for AA oxidation on the modified electrode at0.2V showed linear response to the concentration of AA in the range of1.7～2.0×103μmol·dm-3. The linear equation is i(mA)=0.0031+0.00013[AA](mmol·dm-3), R2=0.9994and the sensitivity is0.13mA·cm-2·mmol-1·dm3. The detection limit of AA on the modified electrode is1.7μmol·dm-3
Graphene oxide nano sheets (GONS) were prepared by electrochemical exfoliation of graphite foil. The composition of GONS was analyzed by XPS and FTIR, and the morphologies were investigated by SEM. It can be seen from the SEM images that the thickness of GONS is as thin as4nm.
The electrocatalytic properties of GONS towards AA oxidation were studied through cyclic voltammetry. The current for AA oxidation on GONS at0V showed linear response to the concentration of AA in the range of5.0×10-4～1.0mmol·dm-3. The linear equation is i(mA)=0.0022+0.10[AA](mmol·dm-3), R2=0.9967, and the sensitivity is0.10mA·cm-2·mmol-1·dm3. The detection limit of AA on GONS is0.5μmol·dm-3. The relative standard deviation (RSD) is3.8%for three times detection of0.25mmol·dm-3AA. Common interfering substances (such as citric acid (CA), glucose (Glu), lactic acid (LA), uric acid (UA) and dopamine (DA)) have higher oxidation potential on GONS than AA, so they have no obvious influence on AA sensing. AA in three kinds of beverage were detected by GONS, the results showed the recovery of the additional standard sample was92.0～100.5%。
The CV and differential pulse voltammetry (DPV) experimental results showed that GONS also had good current responses to dopamine (DA), uric acid (UA) and acetaminophen (APAP). The oxidant current of DA on GONS shows linear response to the concentration of DA in the range of25～200μmol·dm-3. The linear equation is ip (μA)=4.6+0.90[DA](μmol·dm-3), R2=0.9908, and the sensitivity is0.90μA·cm-2μmol-1·dm3. The detection limit of DA on GONS is4.6μmol·dm-3. The RSD is2.3%for three times detection of80μmol·dm-3DA. The oxidant current of UA on GONS shows linear response to the concentration of DA in the range of25～130μmol·dm-3. The linear equation is ip(μA)=0.010+0.90[UA](μmol·dm3), R2=0.9975, and the sensitivity is0.90μA·cm2·μmol-1·dm3. The detection limit of UA on GONS is2.4μmol·dm-3. The RSD is4.3%for three times detection of80μmol·dm-3UA.The oxidant current of APAP on GONS shows linear response to the concentration of APAP in the range of40～200μmol·dm-3. The linear equation is ip(μA)=-0.055+1.8[APAP](μmol·dm-3), R2=0.9961, and the sensitivity is1.8μA·cm-2·μmol-1·dm3. The detection limit of APAP on GONS is1.9μmol·dm-3. The RSD is4.4%for three times detection of200μmol·dm-3APAP.
The oxidation potential on CV and DPV curves of AA, DA, UA and APAP on GONS were separated by more than70mV for each other. Based on the peak separations, simultaneous analysis of all these bioactive molecules is possible in0.1mol·dm-3phosphate buffer solution (pH6.9).
在丝网印刷电极分支间绝缘带上,采用0.2mol·dm-3苯胺的1.0mol·dm-3盐酸溶液,以FeCl3为氧化剂原位聚合苯胺,制备PANI纳米纤维,构建nano-PANI/SPE传感元件。利用SEM观测了位于Nano-PANI/SPE碳电极分支间绝缘带上PANI的形貌,发现PANI在以直径约60nm的纳米纤维形式存在,纳米纤维相互交叉,形成孔径约为300～400nm的均匀多孔结构。
监测了Nano-PANI/SPE传感元件对挥发性有机化合物及氨气的电阻响应,分析了这些气体对PANI电阻的影响。Nano-PANI/SPE传感元件对氯代甲烷、小分子醇、甲苯、三乙胺及氨气均有迅速的电阻响应。由于氨气对PANI具有强脱质子掺杂作用,传感元件对氨气响应灵敏度最高、检测限最低,理论检测限达0.45ppb。Nano-PANI/SPE传感元件具有较好的电阻稳定性,空气中放置一周后,电阻仅增加3.86%。
石墨箔为工作电极,在含有0.2mol·dm-3苯胺的1.0mol·dm-3的盐酸溶液中,通过循环伏安法进行苯胺的电化学聚合,制备了PANI纳米纤维修饰石墨箔电极Nano-PANI/GF。利用FTIR研究了修饰电极上聚合物的振动吸收,利用SEM观测了其形貌。用循环伏安法研究了Nano-PANI/GF修饰电极在0.1mol·dm-3的磷酸盐缓冲溶液(pH6.9)中的电化学活性。发现1～6次循环伏安扫描聚合后,制备的Nano-PANI/GF修饰电极的电化学活性随着聚合扫描次数增加而增加。但由于该PANI在中性溶液中的电化学活性源于石墨箔与PANI之间的电荷传递作用,增加循环伏安扫描次数继续聚合苯胺对电化学活性基本无贡献。
利用循环伏安法研究了Nano-PANI/GF修饰电极对抗坏血酸电化学氧化的催化作用。计时电流实验结果表明,在0.2V电位条件下,1.7～2.0×103μmol·dm-3浓度范围内,抗坏血酸在Nano-PANI/GF修饰电极上的氧化电流与浓度成线性关系,线性方程式为i(mA)=0.0031+0.00013[AA](mmol·dm-3),R2=O.9994,灵敏度为0.13mA·cm-2·mmol-1·dm3,检测限为1.7μmol·dm-3。
以石墨箔为原料,通过电化学氧化膨胀制备了附着于石墨箔表面的氧化石墨烯(GONS)。利用XPS和FTIR分析了氧化石墨烯组成,利用SEM观测其形貌,发现氧化石墨烯片层最低可达到4nm。
利用循环伏安法研究了GONS对抗坏血酸(AA)电化学氧化的催化活性。OV的计时电流实验结果表明,在5.0×10-4～1.0mmol·dm-3浓度范围内,GONS上的响应电流与AA浓度成线性关系,线性方程式为i(mA)=0.0022+0.10[AA](mmol·dm-3),R2=0.9967;灵敏度为0.10mA·cm-2·mol-1·dm3,检测限为0.5μmol·dm-3。浓度为0.25mmol·dm-3的AA的3次测试相对标准偏差为3.8%。柠檬酸(CA)、葡萄糖(Glu)、乳酸(LA)、尿酸(UA)和多巴胺(DA)等常见干扰物在GONS上的氧化电位较高,对AA测试无明显干扰。利用GONS检测了三种饮料中的AA,加入标准样品的回收率达92.0～100.5%。
循环伏安及脉冲伏安实验结果表明,GONS对多巴胺(DA)、尿酸(UA)和对乙酰氨基酚(APAP)也有很好的电流响应。在25～200μmol·dm-3浓度范围内,DA的氧化峰电流与其浓度呈现良好的线性关系,线性相关方程为ip(μA)=4.6+0.90[DA](μmol·dm-3),R2=0.9908。DA在GONS上的检测限为4.6μmol·dm-3,灵敏度为0.90μA·cm-2·μmol-1·dm3,3次测定80μmol·dm-3DA的相对标准偏差为2.3%。在25～130μmol·dm-3浓度范围内,UA的氧化峰电流与其浓度呈现良好的线性关系,线性相关方程为ip(μA)=0.010+0.90[UA](μmol·dm-3),R2=0.9975。UA在GONS上的检测限为2.4μmol·dm-3,灵敏度为0.90μA·cm-2·μmol-1·dm3,3次测定80μmol·dm-3UA得到相对标准偏差为4.3%。在40～200μmol·dm3浓度范围内,APAP的氧化峰电流与其浓度呈现良好的线性关系,线性相关方程为ip(μA)=-0.055+1.8[APAP](μmol·dm-3),R2=0.9961.APAP在GONS上的检测限为1.9μmol·dm-3,灵敏度为1.8μA·cm-2·μmol-1·dm3,3次测定200μmol·dm-3APAP得到相对标准偏差为4.4%。
GONS的循环伏安曲线及差分脉冲伏安曲线上,AA、DA、UA和APAP的氧化峰相互独立,峰电位相差70mV以上,表明在磷酸盐缓冲溶液(pH6.9)的中,AA、DA、UA和APAP在GONS上同时检测有很好的可行性。
Polyaniline (PANI) nanofibers were prepared through in situ chemical and electrochemical polymerization of aniline. PANI nanofibers were fabricated onto screen-printed electrode (SPE) and graphite foil (GF) to construct sensors of Nano-PANI/SPE and Nano-PANI/GF respectively. Graphene oxide nano sheets (GONS) were prepared by electrochemical exfoliation of graphite foil.
Nano-PANI/SPE sensor was constructed by in situ chemical polymerization of aniline on the insulate gap of the SPE by drop coating method, using iron chloride as oxidant. The morphologies of the PANI on the gap were investigated by scanning electron microscopy (SEM). It can be seen from the SEM images that the film was composed of interconnected nanofibers of ca.60nm in diameter to form pores of ca.300-400nm in diameter.
The responses of the Nano-PANI/SPE sensor upon exposure to common volatile organic compounds (VOCs) and ammonia were investigated. It was found that the sensor responsed quickly on exposure to chloromethane, small molecular alcohols, toluene, triethylamine and ammonia. The sensor has higher sensitivity and lower detection limit (0.45ppb) when it was used in sensing ammonia because of the strong de-protonation of PANI by ammonia. The Nano-PANI/SPE sensor has better stability, the resistant of the sensor increased only about3.86%when it was on exposure to air for one week.
Polyaniline nano fiber (Nano-PANI) modified graphite foil (GF), Nano-PANI/GF was prepared by electrochemical polymerization of aniline on GF electrode in a solution of0.2mol·dm-3aniline and1.0mol·dm-3HCl. The polymer on the modified electrode Nano-PANI/GF was characterized by FTIR. The morphologies of the modified electrode were investigated by SEM. The electrochemistry activity of Nano-PANI/GF was investigated in0.1mol·dm-3phosphate buffer solution (pH6.9) by cyclic voltammetry (CV). The electrochemistry activity of Nano-PANI/GF increased along with the cyclic number of CV for the electropolymerization of aniline in the first six cycles as the electroactivity was related to charge transfer between graphite foil and PANI.
The electrocatalytic properties of the Nano-PANI/GF modified electrode towards ascorbic acid (AA) oxidation were studied through cyclic voltammetry. The current for AA oxidation on the modified electrode at0.2V showed linear response to the concentration of AA in the range of1.7～2.0×103μmol·dm-3. The linear equation is i(mA)=0.0031+0.00013[AA](mmol·dm-3), R2=0.9994and the sensitivity is0.13mA·cm-2·mmol-1·dm3. The detection limit of AA on the modified electrode is1.7μmol·dm-3
Graphene oxide nano sheets (GONS) were prepared by electrochemical exfoliation of graphite foil. The composition of GONS was analyzed by XPS and FTIR, and the morphologies were investigated by SEM. It can be seen from the SEM images that the thickness of GONS is as thin as4nm.
The electrocatalytic properties of GONS towards AA oxidation were studied through cyclic voltammetry. The current for AA oxidation on GONS at0V showed linear response to the concentration of AA in the range of5.0×10-4～1.0mmol·dm-3. The linear equation is i(mA)=0.0022+0.10[AA](mmol·dm-3), R2=0.9967, and the sensitivity is0.10mA·cm-2·mmol-1·dm3. The detection limit of AA on GONS is0.5μmol·dm-3. The relative standard deviation (RSD) is3.8%for three times detection of0.25mmol·dm-3AA. Common interfering substances (such as citric acid (CA), glucose (Glu), lactic acid (LA), uric acid (UA) and dopamine (DA)) have higher oxidation potential on GONS than AA, so they have no obvious influence on AA sensing. AA in three kinds of beverage were detected by GONS, the results showed the recovery of the additional standard sample was92.0～100.5%。
The CV and differential pulse voltammetry (DPV) experimental results showed that GONS also had good current responses to dopamine (DA), uric acid (UA) and acetaminophen (APAP). The oxidant current of DA on GONS shows linear response to the concentration of DA in the range of25～200μmol·dm-3. The linear equation is ip (μA)=4.6+0.90[DA](μmol·dm-3), R2=0.9908, and the sensitivity is0.90μA·cm-2μmol-1·dm3. The detection limit of DA on GONS is4.6μmol·dm-3. The RSD is2.3%for three times detection of80μmol·dm-3DA. The oxidant current of UA on GONS shows linear response to the concentration of DA in the range of25～130μmol·dm-3. The linear equation is ip(μA)=0.010+0.90[UA](μmol·dm3), R2=0.9975, and the sensitivity is0.90μA·cm2·μmol-1·dm3. The detection limit of UA on GONS is2.4μmol·dm-3. The RSD is4.3%for three times detection of80μmol·dm-3UA.The oxidant current of APAP on GONS shows linear response to the concentration of APAP in the range of40～200μmol·dm-3. The linear equation is ip(μA)=-0.055+1.8[APAP](μmol·dm-3), R2=0.9961, and the sensitivity is1.8μA·cm-2·μmol-1·dm3. The detection limit of APAP on GONS is1.9μmol·dm-3. The RSD is4.4%for three times detection of200μmol·dm-3APAP.
The oxidation potential on CV and DPV curves of AA, DA, UA and APAP on GONS were separated by more than70mV for each other. Based on the peak separations, simultaneous analysis of all these bioactive molecules is possible in0.1mol·dm-3phosphate buffer solution (pH6.9).
引文
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