本文選題：還原氧化石墨烯 + 聚酰亞胺�。� 參考：《蘭州大學(xué)》2017年博士論文

【摘要】：聚酰亞胺基薄膜修飾電極由于其良好的化學(xué)穩(wěn)定性和可加工性在光電器件的研發(fā)中受到越來越多的關(guān)注。本博士論文制備了具有導(dǎo)電性的還原氧化石墨烯/聚酰亞胺(rGO/PI)柔性復(fù)合薄膜,并以此柔性薄膜電極為基底,在其表面修飾不同類型的納米半導(dǎo)體材料;使用掃描電鏡(SEM)、透射電鏡(TEM)、X射線光電子能譜(XPS)、X射線衍射(XRD)等物理化學(xué)測試技術(shù)以及循環(huán)伏安法(CV)、線性掃描伏安法(LSV)、脈沖伏安法(DPV)以及開路電位-時(shí)間法(OCP-t)等電化學(xué)方法對復(fù)合薄膜修飾電極的形貌、結(jié)構(gòu)與性能進(jìn)行了系統(tǒng)表征;研究了修飾薄膜電極在傳感器和光電轉(zhuǎn)換中的應(yīng)用。主要內(nèi)容包括:1. Mo修飾的rGO/PI薄膜電極的制備及多巴胺的靈敏性檢測通過一步合成法制備了 Mo摻雜的rGO/PI多巴胺(DA)傳感器,結(jié)合XRD和XPS技術(shù)證明Mo以MoO2的形式存在于rGO/PI薄膜中。在最優(yōu)條件下,由LSV法測得Mo-rGO/PI電極上的電化學(xué)信號強(qiáng)度與 DA濃度有可信的正相關(guān)關(guān)系,其線性范圍為0.1- 2000 uM,檢測限為0.021 uM(S/N=3);對尿酸和抗壞血酸具有很強(qiáng)的抗干擾性,穩(wěn)定性和重復(fù)性良好;用該傳感器測定了人血清和醫(yī)用針劑實(shí)際樣品中DA的含量,所得測定結(jié)果、回收率和相對標(biāo)準(zhǔn)偏差等數(shù)據(jù)令人滿意。2.乙酰膽堿酯酶修飾的Au-MoS2-rGO/PI柔性薄膜傳感器的構(gòu)建及其對對氧磷的測定采用光還原法在MoS2-rGO/PI柔性薄膜電極表面制備了金納米顆粒(AuNPs),TEM表征結(jié)果顯示AuNPs的平均直徑約為10nm。DPV結(jié)果顯示乙酰膽堿酯酶修飾的AuNPs-MoS2-rGO/PI柔性薄膜電極催化水解氯化乙酰膽堿產(chǎn)生明顯的電化學(xué)信號;該電化學(xué)信號強(qiáng)度與對氧磷濃度間存在較寬的線性范圍(0.005-0.15 ug/mL),較低的檢測限(0.0014 ug/mL)和較高的靈敏度(4.44 uA/ug mL-1);所表現(xiàn)的重復(fù)性和穩(wěn)定性良好。該柔性薄膜傳感器能夠用于實(shí)際樣品中對氧磷的測定。3. MoSe_2在柔性薄膜rGO/PI表面的生長及其電催化和光電催化析氫性能的研究通過電化學(xué)沉積法在rGO/ PI柔性基底電極表面制備了 MoSe_2。通過SEM、TEM、XRD、XPS、電化學(xué)等技術(shù)對MoSe_2的形貌、結(jié)構(gòu)與性能進(jìn)行了表征。實(shí)驗(yàn)結(jié)果證明MoSe_2-rGO/PI復(fù)合薄膜電極具有優(yōu)良的的光電轉(zhuǎn)換效應(yīng),其光開關(guān)實(shí)驗(yàn)產(chǎn)生的電位差值能夠達(dá)到0.45 V,光電流響應(yīng)時(shí)間在0.6 s以內(nèi);此外MoSe_2-rGO/PI復(fù)合薄膜電極對氫離子還原有顯著的催化作用,在-0.3 V時(shí)的析氫電流達(dá)到7.9 mAcm-2;在光照的條件下,光能有效地促進(jìn)MoSe_2-rGO/PI復(fù)合薄膜電極催化析氫。4.基于rGO/PI基底表面稀磁半導(dǎo)體ZnMnSe_2的制備及其光電性質(zhì)的研究采用電化學(xué)沉積法在rGO/PI薄膜電極表面制備了稀磁半導(dǎo)體ZnMnSe_2。通過SEM、XRD、TEM等分析方法對rGO/PI表面的ZnMnSe_2進(jìn)行了形貌與結(jié)構(gòu)的研究,發(fā)現(xiàn)rGO/PI表面的ZnMnSe_2具有獨(dú)特的納米片網(wǎng)孔結(jié)構(gòu)。通過OCP-t實(shí)驗(yàn)得出ZnMnSe_2-rGO/PI電極具有良好的光電性質(zhì),其電位差值能夠達(dá)到270 mV,相對于二元化合物ZnSe和MnSe而言其光電性能明顯提高。該復(fù)合薄膜具有良好的磁性,是典型的鐵磁性半導(dǎo)體材料。5. ZnSe在新型基底CNTs/PVA電極表面的原位生長及其光電性質(zhì)的研究用i-t交替沉積的方法在新的柔性薄膜電極碳納米管/聚乙烯醇(CNTs/PVA)表面制備了 ZnSe,從而得到ZnSe-CNTs/PVA復(fù)合薄膜電極。實(shí)驗(yàn)中通過改變Zn與Se的濃度,研究了原子比例Zn: Se對化合物(ZnxSe1-x)形貌的影響,發(fā)現(xiàn)ZnSe的形貌是最均勻單一的,由納米棒組成。通過OCP-t實(shí)驗(yàn)研究了相似類型三種化合物的光電性質(zhì),發(fā)現(xiàn)均為p型半導(dǎo)體,且均具有良好的光電性質(zhì),其中ZnSe的光電效應(yīng)是最好的。
[Abstract]:Polyimide based film modified electrodes have attracted more and more attention in the development of optoelectronic devices because of their good chemical stability and machinability. This paper has prepared a conductive reduced graphene oxide / polyimide (rGO/PI) flexible composite film, which is based on the flexible thin film electrode and modified on its surface. The nano semiconductor materials of the same type are modified by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X ray photoelectron spectroscopy (XPS), X ray diffraction (XRD), cyclic voltammetry (CV), linear sweep voltammetry (LSV), pulse voltammetry (DPV) and open circuit potential time (OCP-t), and other electrochemical methods The application of modified thin film electrode in sensor and photoelectric conversion is studied. The main contents include: the preparation of 1. Mo modified rGO/PI film electrode and the sensitivity detection of dopamine, the Mo doped rGO/PI dopamine (DA) sensor is prepared by one step synthesis method, combined with XRD and XPS technology. It is proved that Mo exists in the form of rGO/PI in the form of MoO2. Under the optimal conditions, there is a credible and positive correlation between the electrochemical signal intensity on the Mo-rGO/PI electrode and the concentration of DA by LSV method. The linear range is 0.1- 2000 uM and the detection limit is 0.021 uM (S/N=3); it has strong anti-interference, stability and repeatability to uric acid and antiblood acid. Well, the content of DA in real samples of human serum and medical needle was measured with this sensor. The results of the determination, recovery and relative standard deviation were satisfactory for the construction of the Au-MoS2-rGO/PI flexible thin film sensor modified by.2. acetylcholinesterase and the determination of phosphor by photoreduction in MoS2-rGO/PI flexible thin film Gold nanoparticles (AuNPs) were prepared on the surface of the electrode. The TEM characterization showed that the average diameter of AuNPs was about 10nm.DPV. The AuNPs-MoS2-rGO/PI flexible membrane electrode modified by acetylcholinesterase catalyzed the hydrolysis of acetylcholine to produce obvious electrochemical signals, and the intensity of the electrochemical signal was wide with the concentration of oxyphosphoric acid. The range (0.005-0.15 ug/mL), lower detection limit (0.0014 ug/mL) and higher sensitivity (4.44 uA/ug mL-1); the reproducibility and stability are good. The flexible thin film sensor can be used to determine the growth of.3. MoSe_2 on the surface of the flexible film rGO/PI and the electrocatalysis and Photoelectrochemical Performance of hydrogen evolution in the actual samples. The morphology, structure and properties of MoSe_2. were characterized by electrochemical deposition on the surface of rGO/ PI flexible substrate by SEM, TEM, XRD, XPS, electrochemistry and other techniques. The experimental results show that the MoSe_2-rGO/PI composite film electrode has excellent photoelectric conversion effect and the potential difference energy produced by the optical switch experiment can be produced. The response time of the photocurrent is within 0.6 s enough to reach 0.45 V, and the MoSe_2-rGO/PI composite film electrode has a significant catalytic effect on the hydrogen ion reduction, and the hydrogen evolution current at -0.3 V reaches 7.9 mAcm-2. Under the light conditions, the light energy can effectively promote the catalytic hydrogen evolution of the MoSe_2-rGO/PI composite film electrode based on the dilute magnetic half surface of the rGO/PI substrate surface. Study on the preparation and photoelectrical properties of conductor ZnMnSe_2, the morphology and structure of the rGO/PI surface ZnMnSe_2 were studied by electrochemical deposition on the surface of rGO/PI thin film electrode by the methods of SEM, XRD, TEM and other analytical methods. It was found that ZnMnSe_2 of the rGO/PI surface has a unique nanoscale mesh structure. Through O, ZnMnSe_2 has been found. The CP-t experiment shows that the ZnMnSe_2-rGO/PI electrode has good photoelectric properties and its potential difference can reach 270 mV. Compared with the two element compound ZnSe and MnSe, the photoelectric property is obviously improved. The composite film has good magnetic properties. It is a typical ferromagnetic semiconductor material.5. ZnSe in situ growth on the surface of the new base CNTs/PVA electrode. The study of the optoelectronic properties of ZnSe was prepared on the surface of a new flexible film electrode carbon nanotube / polyvinyl alcohol (CNTs/PVA) on the surface of a new flexible thin film electrode by I-T, and the ZnSe-CNTs/PVA composite film electrode was obtained. In the experiment, the influence of the atomic proportion Zn: Se on the morphology of the compound (ZnxSe1-x) was studied by changing the concentration of Zn and Se, and ZnSe was found. The morphology is the most uniform and single, composed of nanorods. The photoelectric properties of three similar types of compounds were investigated by OCP-t experiments. All of them were found to be p type semiconductors with good photoelectric properties, and the optoelectronic effect of ZnSe was the best.

【學(xué)位授予單位】：蘭州大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2017
【分類號】：O646.54;TB383.2

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本文編號：1866284