金纳米粒子修饰的三维花状二硫化钼复合材料的制备及其用于检测过氧化氢的研究
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摘要
以Na_2MoO_4·2H_2O为钼源,硫脲为硫源和还原剂,氧化多壁碳纳米管(o-MWNTs)和氧化石墨烯(GO)为原料,采用水热法合成了三维花状MoS_2/GO/o-MWNTs纳米复合材料,并进一步采用原位还原法将金纳米粒子修饰至MoS_2/GO/o-MWNTs纳米复合材料表面。通过场发射扫描电镜、透射电镜、XRD、XPS等对上述复合材料进行表征。结果表明,该复合纳米材料具有3D花状球结构,且Au纳米粒子已成功生长在其花瓣状片层上。采用滴涂法制得该复合材料修饰的玻碳电极,研究了过氧化氢在该电极上的电化学行为。结果表明:该电极对过氧化氢的电还原表现出强催化活性。通过对不同浓度过氧化氢的催化还原,得出该电极对过氧化氢的线性范围为12.0×10~(-9)～31.0×10~(-6) mol/L,灵敏度为56.6μA/(mmol·L~(-1)),检出限为12.0×10~(-9) mol/L。
In this paper,the flowerlike MoS_2/GO/o-MWNTs composites were synthesized by using Na_2MoO_4·2 H_2O as molybdenum source,thiourea as sulfur source and reducing agent,and mixed oxidized multi-walled carbon nanotubes(o-MWNTs) and graphene oxide(GO) as raw material,respectively.Then,the gold nanoparticles were deposited on the surface of MoS_2/GO/o-MWNTs by in situ chemical reduction method.The characterization of this nanocomposites was performed by field emission scanning electron microscopy(FESEM),transmission electron microscopy(TEM),X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS).Results demonstrated that the MoS_2/GO/o-MWNTs composites were synthesized successfully via the hydrothermal method,and gold nanoparticles were modified on the flower sheets.The nanocomposites were modified on the glassy carbon electrode(GCE) to investigate the electrochemical behavior for H_2O_2.The results showed that the electrode exhibited a strong catalytic activity toward H_2O_2,and there was a linear relationship between the electrode and H_2O_2 in the concentration range of 12.0×10~(-9)-31.0×10~(-6) mol/L with a sensitivity of 56.6 μA/(mmol·L~(-1)) and a detection limit of 12.0×10~(-9) mol/L.
In this paper,the flowerlike MoS_2/GO/o-MWNTs composites were synthesized by using Na_2MoO_4·2 H_2O as molybdenum source,thiourea as sulfur source and reducing agent,and mixed oxidized multi-walled carbon nanotubes(o-MWNTs) and graphene oxide(GO) as raw material,respectively.Then,the gold nanoparticles were deposited on the surface of MoS_2/GO/o-MWNTs by in situ chemical reduction method.The characterization of this nanocomposites was performed by field emission scanning electron microscopy(FESEM),transmission electron microscopy(TEM),X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS).Results demonstrated that the MoS_2/GO/o-MWNTs composites were synthesized successfully via the hydrothermal method,and gold nanoparticles were modified on the flower sheets.The nanocomposites were modified on the glassy carbon electrode(GCE) to investigate the electrochemical behavior for H_2O_2.The results showed that the electrode exhibited a strong catalytic activity toward H_2O_2,and there was a linear relationship between the electrode and H_2O_2 in the concentration range of 12.0×10~(-9)-31.0×10~(-6) mol/L with a sensitivity of 56.6 μA/(mmol·L~(-1)) and a detection limit of 12.0×10~(-9) mol/L.
引文
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[3] Zhang W S,Zhang P P,Su Z Q,Wei G.Nanoscale,2015,7(44):18364-18378.
[4] Yang L,Wang S,Mao J,Deng J,Gao Q,Tang Y.Adv.Mater.,2013,25(8):1180-1184.
[5] Bindumadhavan K,Srivastava S K,Mahanty S.Chem.Commun.,2013,49(18):1823-1825.
[6] Su S,Sun H,Cao W,Chao J,Peng H,Zuo X,Yuwen L,Fan C,Wang L.ACS Appl.Mater.Interfaces,2016,8(11):6826-6833.
[7] Sun H F,Chao J,Zuo X L,Su S,Liu X F,Yuwen L H,Fan C H,Wang L H.RSC Adv.,2014,4(52):27625-27629.
[8] Huang K J,Wang L,Li J,Liu Y M.Sens.Actuators B,2013,178(5):671-677.
[9] Chen D H,Li M Q.Technol.Dev.Chem.Ind.(陈迪航,李绵庆.化工技术与开发),2011,40(3):32-35.
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[11] Wei H,Wang E.Anal.Chem.,2008,80(6):2250-2254.
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[13] Lingappan N,Van N H,Lee S,Kang D J.J.Power Sources,2015,280:39-46.
[14] Sun P,Zhang W,Hu X,Yuan L,Huang Y.J.Mater.Chem.A,2014,2:3498-3504.
[15] Koroteev V O,Bulusheva L G,Asanov I P,Shlyakhova E V,Vyalikh D V,Okotrub A V.J.Phys.Chem.C,2011,115(43):21199-21204.