本文關(guān)鍵詞： APTES-HAuCl4 空心金納米殼 “碗”狀硅-金納米結(jié)構(gòu) 空心多孔金納米結(jié)構(gòu)　出處：《吉林大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：金納米粒子具有較低的毒性、良好的生物相容性及表面易功能化等特點,在生物檢測、生物成像、光熱治療、靶向藥物輸送等方面都有著非常廣闊的應(yīng)用前景。通過改變粒子的尺寸、形狀、長寬比、周圍介質(zhì)的介電常數(shù)、表面形態(tài)和粒子的聚集程度等來優(yōu)化SPR(表面等離子體共振)峰的位置,進(jìn)而拓寬其應(yīng)用的范圍。其中,空心金納米殼是一種由可溶解的填充介質(zhì)和多晶金殼組成的具有特殊性質(zhì)的納米材料。通過調(diào)節(jié)核的尺寸及殼層厚度得到不同直徑的納米粒子,所得粒子的光譜可以從可見光區(qū)調(diào)節(jié)到近紅外光區(qū),以滿足生物醫(yī)用等方面的應(yīng)用要求。2015年本課題組研究發(fā)現(xiàn),將一定濃度的APTES(氨丙基三乙氧基硅烷)分散到水中后,依次加入氯金酸水溶液、還原劑硼氫化鈉以及穩(wěn)定劑BSA(牛血清白蛋白),可以制備得到不同尺寸的空心金納米殼材料,其光譜連續(xù)可調(diào)。但是,空心金納米殼的形成機制并不清楚,單分散性也有待進(jìn)一步優(yōu)化。本文主要對空心金納米殼的形成機制進(jìn)行了詳細(xì)研究,并在此基礎(chǔ)上調(diào)控制備出兩種不同形貌的納米材料。本文的研究內(nèi)容主要包括以下兩個方面:第一,將APTES分散到水中無法形成穩(wěn)定的結(jié)構(gòu),會迅速發(fā)生自催化水解;而加入氯金酸水溶液后,氨基與金之間形成配位鍵,最終形成穩(wěn)定的單分散的APTES-HAuCl4復(fù)合物前體,這是形成空心納米金殼的關(guān)鍵。然后,通過UV-Vis、TEM、DLS、FTIR等表征手段,對APTES-HAuCl4的形成條件以及自身的行為做了詳細(xì)的研究。APTES/HAuCl4摩爾比R在2.83-11.33之間可以形成穩(wěn)定的APTES-HAuCl4,并且R=5.67時穩(wěn)定性最好。APTES-HAuCl4(APTES 8.5 mM,HAuCl4 1.5 mM)分散在水溶液中會隨著時間發(fā)生變化,在40 min內(nèi),隨著時間的延長前體的尺寸減小,單分散性變好,加入還原劑后可以得到空心金結(jié)構(gòu)的納米殼。最后,利用APTES-HAuCl4自身具備的特殊性質(zhì),引入一定濃度的氨水催化APTES-HAuCl4水解縮合,最終得到“碗”狀硅-金納米結(jié)構(gòu)。第二,利用CTAB與APTES的協(xié)同作用制備空心多孔金納米結(jié)構(gòu)。通過改變醇水比(1:19-6:14)對粒子的尺寸及光譜性質(zhì)進(jìn)行調(diào)控,隨著乙醇體積的增加等離子體共振峰從600 nm紅移到750 nm,對應(yīng)的尺寸從34.2 nm增加到84.2nm。并且制備的空心多孔金納米結(jié)構(gòu)具有較好的穩(wěn)定性以及抗鹽能力。在醇水比在1:9,2:8和3:7三個條件下合成的三種不同尺寸的空心多孔金納米結(jié)構(gòu)材料,具有一定增強拉曼信號(SERS)的性質(zhì)。同時三種不同尺寸的粒子在水相中可以催化硼氫化鈉還原對硝基苯胺反應(yīng),均可以在280 s內(nèi)完成,具有較好的催化活性。
[Abstract]:Gold nanoparticles have low toxicity, good biocompatibility and easy surface functionalization, in biological detection, biological imaging, photothermal therapy, The target drug delivery has a very broad application prospect. By changing the particle size, shape, aspect ratio, the dielectric constant of the surrounding medium, The surface morphology and particle aggregation degree are used to optimize the position of the SPRs peak, and then to broaden the scope of its application. The hollow gold nanoshell is a special material with special properties composed of soluble filling medium and polycrystalline gold shell. By adjusting the size of the core and the thickness of the shell, different diameter nanoparticles can be obtained. The spectra of the obtained particles can be adjusted from the visible region to the near infrared region to meet the requirements of biomedical applications. In 2015, our research group found that APTES (aminopropyl triethoxysilane) was dispersed into water at a certain concentration. In turn, the hollow gold nanoshell materials of different sizes can be prepared by adding chlorgold acid aqueous solution, sodium borohydride and stabilizer BSA, the spectrum of which can be continuously adjusted. The formation mechanism of hollow gold nanoshell is not clear, and the monodispersity needs to be further optimized. In this paper, the formation mechanism of hollow gold nanoshell is studied in detail. On the basis of this, two kinds of nanomaterials with different morphologies were prepared. The main contents of this paper are as follows: first, the stable structure of APTES can not be dispersed into water, and the autocatalytic hydrolysis will occur rapidly; After the addition of chloruronic acid aqueous solution, the coordination bond between amino group and gold was formed, and finally the stable monodisperse precursor of APTES-HAuCl4 complex was formed, which was the key to the formation of hollow nanocrystalline gold shell. The formation conditions of APTES-HAuCl4 and its own behavior were studied in detail. APTES / HAuCl _ 4 molar ratio R = 2.83-11.33 could form stable APTES-HAuCl _ 4, and the stability of APTES-HAuCl _ 4 was the best when R = 5.67. The dispersion of APTES-HAuCl _ 4 in aqueous solution would change with time and within 40 min. With the prolongation of the time, the size of the precursor decreases and the monodispersity becomes better. The hollow gold nanoshell can be obtained by adding the reductant. Finally, using the special properties of APTES-HAuCl4 itself, a certain concentration of ammonia water is introduced to catalyze the hydrolysis and condensation of APTES-HAuCl4. Finally, the "bowl" silicon-gold nanostructures were obtained. Secondly, the hollow porous gold nanostructures were prepared by the synergistic action of CTAB and APTES. The size and spectral properties of the particles were regulated by changing the ratio of alcohol to water (1: 19-6: 14). With the increase of ethanol volume, the plasmon resonance peak shifted from 600 nm red to 750 nm, and the corresponding size increased from 34.2 nm to 84.2 nm. The hollow porous gold nanostructures had good stability and salt resistance. Three kinds of hollow porous gold nanostructures of different sizes synthesized under the conditions of 1: 9, 2: 8 and 3: 7, At the same time, three kinds of particles with different sizes can catalyze the reduction of p-nitroaniline by sodium borohydride in water, which can be completed in 280 s, and have good catalytic activity.
【學(xué)位授予單位】：吉林大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O614.123;TB383.1

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