【摘要】：近年來(lái),金屬納米顆粒由于其獨(dú)特的物理和化學(xué)性質(zhì),在許多領(lǐng)域引起了廣泛的重視,成為材料科學(xué)的研究熱點(diǎn)。在各種各樣的金屬納米顆粒中,貴金屬納米顆粒贏得了研究者的重點(diǎn)關(guān)注,它們因?yàn)榫哂行路f、奇異的性質(zhì),而被廣泛應(yīng)用于催化、電子學(xué)、光譜學(xué)等領(lǐng)域。隨著社會(huì)經(jīng)濟(jì)的發(fā)展,“綠色化學(xué)”這一概念越來(lái)越受到人們的關(guān)注,綠色、環(huán)保的化學(xué)合成方法也越來(lái)越符合大眾的需求。傳統(tǒng)的貴金屬納米顆粒的合成方法,主要是化學(xué)液相還原法,過(guò)程中需要加入還原劑、表面活性劑等添加劑。為響應(yīng)綠色化學(xué)的要求,我們采用輻照的方法,在不添加任何添加劑的條件下,直接制備了貴金屬納米顆粒并研究了其應(yīng)用。具體內(nèi)容如下:(1)利用gamma射線(xiàn)輻照,在不添加任何還原劑和保護(hù)劑的情況下,直接合成了均勻穩(wěn)定的金納米顆粒,并通過(guò)掃描電鏡,X-射線(xiàn)粉末衍射儀,紫外-可見(jiàn)吸收光譜儀進(jìn)行表征分析。將所制備的金納米顆粒應(yīng)用于電化學(xué)檢測(cè),以葡萄糖和多巴胺作為被檢測(cè)分子,研究其電化學(xué)行為。實(shí)驗(yàn)結(jié)果表明,金納米顆粒修飾的電極表現(xiàn)出優(yōu)異的電化學(xué)性能,對(duì)葡萄糖和多巴胺的檢測(cè)具有高靈敏度性,并且具有良好的重復(fù)性和穩(wěn)定性。(2)以同樣的方法合成了銀納米顆粒,同時(shí)研究了金納米顆粒和銀納米顆粒的表面增強(qiáng)拉曼性能。用所合成的納米顆粒分別制作表面增強(qiáng)拉曼基底,以羅丹明6G作為客體分子,采用液體測(cè)試方式分別檢測(cè)了基底的表面增強(qiáng)拉曼性能。結(jié)果顯示,金納米顆粒制備的基底可清晰檢測(cè)到濃度為1×10-7 M的羅丹明6G分子,銀納米顆�；啄芮逦鷻z測(cè)到1×10-9 M的羅丹明6G分子。所制備活性基底不僅具有高靈敏性,也具有高穩(wěn)定性和重復(fù)性。隨機(jī)選取100點(diǎn)收集拉曼信號(hào),每個(gè)點(diǎn)都能采集到清晰的羅丹明6G的信號(hào),且主要峰的峰強(qiáng)的相對(duì)標(biāo)準(zhǔn)偏差均小于20%。(3)通過(guò)輻照還原的方法從氧化銀顆粒中直接還原出銀納米顆粒,并原位檢測(cè)其SERS活性。首先,通過(guò)濕化學(xué)法,在不添加穩(wěn)定劑的情況下合成氧化銀納米顆粒。同時(shí),采用液-液界面自組裝的方法,用所合成的氧化銀納米顆粒制作表面增強(qiáng)拉曼基底。分別以羅丹明6G和4-巰基苯甲酸作為被檢測(cè)物質(zhì),研究了所制備的表面增強(qiáng)拉曼基底的性能。實(shí)驗(yàn)結(jié)果顯示,隨著時(shí)間的累積,客體分子的特征峰越來(lái)越明顯,峰強(qiáng)也逐漸增加,當(dāng)時(shí)間累積到一定程度后,特征峰強(qiáng)度不再變化,基本處于平穩(wěn)狀態(tài)。曝光一定時(shí)間后,隨機(jī)連續(xù)收集多個(gè)點(diǎn)的拉曼信號(hào),每個(gè)點(diǎn)都能獲得高靈敏度的拉曼信號(hào),且具有較好的重現(xiàn)性。以上結(jié)果表明,所制備的貴金屬納米顆粒具有較好的電化學(xué)性質(zhì)和表面增強(qiáng)拉曼性能。輻照合成法作為一種可行的綠色、環(huán)保制備手段,可廣泛應(yīng)用于其他材料的合成,應(yīng)用前景廣闊。
[Abstract]:In recent years, metal nanoparticles have attracted extensive attention in many fields because of their unique physical and chemical properties. Among all kinds of metal nanoparticles, noble metal nanoparticles have attracted the attention of researchers. They have been widely used in catalysis, electronics, spectroscopy and other fields because of their novel and strange properties. With the development of social economy, people pay more and more attention to the concept of "green chemistry". The traditional method of synthesis of noble metal nanoparticles is mainly chemical liquid phase reduction, and additives such as reductant and surfactant are needed in the process. In order to meet the requirements of green chemistry, we have prepared noble metal nanoparticles directly and studied their applications by irradiation without adding any additives. The main contents are as follows: (1) the uniform and stable gold nanoparticles were synthesized by gamma irradiation without adding any reducer and protectant, and the X-ray powder diffractometer was used. UV-vis absorption spectrometer was used for characterization and analysis. The prepared gold nanoparticles were used for electrochemical detection. Glucose and dopamine were used as the detected molecules to study their electrochemical behavior. The results showed that the gold nanoparticles modified electrode showed excellent electrochemical performance and high sensitivity to the detection of glucose and dopamine. Silver nanoparticles were synthesized in the same way and the surface enhanced Raman properties of gold nanoparticles and silver nanoparticles were studied. The surface-enhanced Raman substrates were prepared from the synthesized nanoparticles, and the surface-enhanced Raman properties of the substrates were measured by liquid test using Rhodamine 6G as guest molecule. The results show that the concentration of Rhodamine 6G is 1 脳 10 ~ (-7) M and that of Rhodamine 6G of 1 脳 10 ~ (-9) M can be clearly detected on the substrate prepared by gold nanoparticles, while that of Rhodamine 6G at a concentration of 1 脳 10 ~ (-7) M can be clearly detected on the silver nanoparticles substrate. The prepared active substrate not only has high sensitivity, but also has high stability and repeatability. At random, 100 points were selected to collect Raman signals. Each point could collect a clear Rhodamine 6G signal, and the relative standard deviation of peak strength of the main peak was less than 20. (3) Silver nanoparticles were directly reduced from silver oxide particles by irradiation reduction. The SERS activity was detected in situ. First, silver oxide nanoparticles were synthesized by wet chemical method without adding stabilizer. At the same time, the surface-enhanced Raman substrate was fabricated by using the synthesized silver oxide nanoparticles by the liquid-liquid interface self-assembly method. Using Rhodamine 6G and 4-mercaptobenzoic acid as the detected substances, the properties of the surface-enhanced Raman substrates were studied. The experimental results show that with the accumulation of time the characteristic peak of the guest molecule becomes more and more obvious and the peak strength increases gradually. When the time accumulates to a certain extent the intensity of the characteristic peak does not change and is basically in a stable state. After exposure for a certain time, the Raman signals of multiple points are collected at random, each point can obtain a high sensitivity Raman signal, and it has good reproducibility. The results show that the prepared noble metal nanoparticles have good electrochemical properties and surface-enhanced Raman properties. As a feasible green and environmentally friendly preparation method, irradiation synthesis can be widely used in the synthesis of other materials.
【學(xué)位授予單位】：蘇州大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類(lèi)號(hào)】：O614.12;TB383.1

【參考文獻(xiàn)】

相關(guān)期刊論文 前3條

1 唐振艷;趙云昆;張愛(ài)敏;賀小昆;張永;;液相化學(xué)法制備貴金屬納米顆粒的研究進(jìn)展[J];材料導(dǎo)報(bào);2008年S3期

2 鞏雄,張桂蘭,湯國(guó)慶,陳文駒,楊宏秀;納米晶體材料研究進(jìn)展[J];化學(xué)進(jìn)展;1997年04期

3 ;Shape-controlled synthesis of highly monodisperse and small size gold nanoparticles[J];Science in China(Series B:Chemistry);2007年04期

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本文編號(hào)：2249620