本文選題：貴金屬　切入點(diǎn)：空心結(jié)構(gòu)　出處：《重慶理工大學(xué)》2015年碩士論文　論文類(lèi)型：學(xué)位論文

【摘要】：電化學(xué)傳感器因靈敏度高、穩(wěn)定性好、能進(jìn)行快速實(shí)時(shí)監(jiān)測(cè)等特點(diǎn),已在臨床診斷、環(huán)境監(jiān)測(cè)、食品檢測(cè)等領(lǐng)域得到廣泛的應(yīng)用。電極材料的電催化活性是影響傳感器參數(shù)指標(biāo)的重要因素,貴金屬催化劑以其較高的催化活性和化學(xué)穩(wěn)定性,成為當(dāng)前催化研究領(lǐng)域的熱點(diǎn)課題。具有空心結(jié)構(gòu)的貴金屬納米材料綜合了空心結(jié)構(gòu)和貴金屬納米粒子的優(yōu)點(diǎn),具有大的比表面積及豐富的孔洞結(jié)構(gòu),能夠容納大量的客體分子或尺寸較大的分子,具有較多的催化活性位點(diǎn),電催化活性大幅度提高,在生物化學(xué)、催化化學(xué)、材料科學(xué)等領(lǐng)域具有特殊的應(yīng)用前景。本論文擬以Cu2O為犧牲模板,利用Cu2O和貴金屬前驅(qū)體溶液之間的自發(fā)氧化還原反應(yīng)設(shè)計(jì)合成單元或二元的貴金屬空心結(jié)構(gòu)材料,同時(shí)對(duì)該空心結(jié)構(gòu)材料的微觀形貌進(jìn)行解構(gòu),對(duì)其成分進(jìn)行分析。研究了該空心材料修飾電極對(duì)葡萄糖和過(guò)氧化氫的電化學(xué)檢測(cè)能力,通過(guò)電化學(xué)方法對(duì)電化學(xué)傳感器的性能指標(biāo)進(jìn)行了標(biāo)定,該空心結(jié)構(gòu)對(duì)葡萄糖和過(guò)氧化氫均表現(xiàn)出較高的電催化活性。該論文的研究將為貴金屬空心結(jié)構(gòu)在生物分子電催化領(lǐng)域的應(yīng)用提供理論支持和指導(dǎo)意義,主要研究?jī)?nèi)容如下:(1)采用液相法制備了立方結(jié)構(gòu)的Cu2O,并用掃描電子顯微鏡(SEM)、透射電子顯微鏡(TEM)和X射線衍射(XRD)對(duì)其形貌和結(jié)構(gòu)進(jìn)行了表征,結(jié)果表明,實(shí)驗(yàn)得到了純凈的單相實(shí)心赤銅礦Cu2O晶體,平均粒徑400 nm左右。(2)以Cu2O為模板,將H2PtCl6溶液加入到Cu2O懸浮液中,兩者發(fā)生氧化還原反應(yīng)使鉑負(fù)載在Cu2O表面,隨后,酸蝕去除模板,得到Pt空心納米結(jié)構(gòu)材料。采用SEM和TEM對(duì)其形貌進(jìn)行了表征,構(gòu)建了基于Pt空心納米材料的葡萄糖電化學(xué)傳感器,采用循環(huán)伏安法(CV)和計(jì)時(shí)電流法(CA)研究了其修飾電極對(duì)葡萄糖的電催化氧化性能。實(shí)驗(yàn)結(jié)果表明,該傳感器對(duì)葡萄糖的催化氧化電流與其濃度在0.5mM-22.5 mM范圍內(nèi)呈現(xiàn)良好的線性關(guān)系,檢出限為0.26 mM,靈敏度為92.03μA/mM/cm2。(3)以Cu2O為模板,將H2PtCl6溶液和Na2PdCl4溶液按摩爾比1:1先后加入到Cu2O懸浮液中,酸蝕去除模板,得到Pt/Pd空心納米材料。采用SEM、TEM和X射線能量色散譜(EDS)對(duì)其形貌結(jié)構(gòu)進(jìn)行了表征,構(gòu)建了基于Pt/Pd空心納米材料的H2O2電化學(xué)傳感器,采用CV和CA研究了其修飾電極對(duì)H2O2的電催化性能。實(shí)驗(yàn)結(jié)果表明,該傳感器對(duì)H2O2的催化電流與其濃度在0.25 mM-30 mM范圍內(nèi)呈現(xiàn)良好的線性關(guān)系,檢出限為0.12 mM,靈敏度為77.66μA/mM/cm2。(4)采用相同的模板法制備空心金納米材料,通過(guò)研究氯金酸用量、腐蝕劑種類(lèi)等因素對(duì)產(chǎn)物形貌的影響后,均未得到期望的空心結(jié)構(gòu)。由于負(fù)載型金納米粒子同樣表現(xiàn)出極高的電催化活性,實(shí)驗(yàn)中研究了Au-Cu2O復(fù)合材料修飾電極對(duì)H2O2的電化學(xué)檢測(cè)性能。實(shí)驗(yàn)結(jié)果表明,Au-Cu2O復(fù)合材料對(duì)H2O2有較高的電催化活性,電化學(xué)傳感器的線性范圍為0.025 mM-11.2 mM,檢出限為1.05μM,靈敏度為292.89μA/mM/cm2,該材料在H2O2的快速檢測(cè)方面有潛在的應(yīng)用價(jià)值。
[Abstract]:Electrochemical sensor because of high sensitivity, good stability, can real-time monitoring and other features, has been in clinical diagnosis, environmental monitoring, widely used in food detection. The electrocatalytic activity of the material is an important factor affecting the parameters of the sensor, noble metal catalysts because of their relatively high catalytic activity and chemical stability, become a hot topic in the field of catalysis. With noble metal nanomaterials with hollow structure combines the advantages of hollow structure and noble metal nanoparticles, with large surface area and abundant pore structure, can accommodate a large number of guest molecules or the size of the molecules, the catalytic site has more, greatly improve the electrocatalytic activity in Biochemistry, chemistry, catalysis, has the application prospect of special materials science and other fields. This paper intends to use Cu2O as sacrificial templates, Cu2O and precious metals The hollow noble metal structure materials synthesis unit two yuan design or spontaneous oxidation between the precursor solution and reduction, morphology of the hollow structure material deconstruction, analysis its composition. Study on glucose and hydrogen peroxide electrochemical detection ability of the hollow materials modified electrode by electrochemical method on performance index electrochemical sensors were calibrated, the hollow structure of glucose and hydrogen peroxide exhibited higher electrocatalytic activity. The study will provide theoretical support and guidance for the application of hollow noble metal structure in the biological molecules in electrocatalysis, the main contents are as follows: (1) using the cubic structure Cu2O liquid method, by using scanning electron microscope (SEM), transmission electron microscopy (TEM) and X ray diffraction (XRD) on the morphology and structure were characterized. The results show that, The pure single-phase solid copper Cu2O crystal, the average particle size of about 400 nm. (2) using Cu2O as template, H2PtCl6 solution was added to the Cu2O suspension, the two oxidation platinum loading on the surface of Cu2O reduction reaction subsequently, etching to remove the template, Pt hollow nano structure materials are used. The morphology was characterized by SEM and TEM, constructed the Pt hollow glucose electrochemical sensor based on Nanomaterials by cyclic voltammetry (CV) and chronoamperometry (CA) on the electric catalytic oxidation performance of the modified glucose. The experimental results show that the sensor for glucose oxidation current and the concentration of a good linear relationship in the range of mM 0.5mM-22.5, the detection limit was 0.26 mM, the sensitivity is 92.03 A/mM/cm2. (3) using Cu2O as template, H2PtCl6 solution and Na2PdCl4 solution after the first molar of 1:1 added to the Cu2O suspension In the acid etching to remove the template, Pt/Pd hollow nano materials. By using SEM, TEM and X ray energy dispersive spectroscopy (EDS) on the morphology and structure were characterized by H2O2 Pt/Pd electrochemical sensor was constructed based on hollow nano materials, studied the electrocatalytic performance of H2O2 electrode modified by CV and CA. The experimental results show that the catalytic sensor current on H2O2 and concentration showed a good linear relationship in the range of mM 0.25 mM-30, the detection limit was 0.12 mM, the sensitivity is 77.66 A/mM/cm2. (4) preparation of hollow gold nanoparticles using the same template method, through the study of chloroauric acid dosage, corrosion agent and other factors on the morphology of the product after have not been expected. Due to the hollow structure of supported gold nanoparticles also showed high electrocatalytic activity, we have studied the electrochemical detection of Au-Cu2O composite modified electrode for H2O2 measurement. The experimental performance The results show that Au-Cu2O composite has high electrocatalytic activity for H2O2. The linear range of the electrochemical sensor is 0.025 mM-11.2 mM, the detection limit is 1.05 M, and the sensitivity is 292.89 A/mM/cm2 A/mM/cm2. The material has potential application in the rapid detection of H2O2.

【學(xué)位授予單位】：重慶理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類(lèi)號(hào)】：TB383.1;TP212.2

【參考文獻(xiàn)】

相關(guān)期刊論文 前1條

1 劉亞珍;幾種氣體傳感器的特性及其應(yīng)用[J];儀器儀表與分析監(jiān)測(cè);1998年01期

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本文編號(hào)：1612630