本文選題：原子力顯微鏡 + 單分子力譜　； 參考：《吉林大學(xué)》2017年碩士論文

【摘要】：半結(jié)晶性高分子材料因其優(yōu)良的性能和使用價值而被廣泛應(yīng)用到人類生活中的多個領(lǐng)域。結(jié)晶相結(jié)構(gòu)對高分子材料許多方面力學(xué)性質(zhì)起決定作用。隨著人們對材料應(yīng)用性能要求的進(jìn)一步提高,揭示并調(diào)控材料晶體結(jié)構(gòu)-性能的關(guān)系,尤其是單分子水平結(jié)構(gòu)與材料宏觀性能關(guān)系的探索,變得非常重要。相關(guān)研究有助于更好地理解材料性能變化的微觀機(jī)理,從而指導(dǎo)高性能高聚物晶體材料的性能調(diào)控及設(shè)計(jì)與制備。傳統(tǒng)的實(shí)驗(yàn)方法難以給出分子水平的力學(xué)性質(zhì)信息,基于原子力顯微鏡(AFM)的單分子力譜技術(shù)(SMFS)的出現(xiàn)使相關(guān)研究成為可能。在本論文第一章中,系統(tǒng)地介紹了高分子結(jié)晶態(tài)及AFM成像的工作模式及其應(yīng)用,并對基于AFM的單分子力譜技術(shù)做了詳細(xì)的描述,包括其工作原理、單分子力-拉伸曲線的獲取、判定與分析及其在材料科學(xué)領(lǐng)域的重要應(yīng)用。本論文的研究思路主要是借助于AFM的單分子力譜技術(shù),探究間規(guī)聚丙烯(s PP)晶體材料不同微觀結(jié)構(gòu)的力學(xué)性能。本論文第二章的工作主要集中在具有不同晶型結(jié)構(gòu)的間規(guī)聚丙烯單晶的制備與表征。通過結(jié)晶條件篩選,分別制備出不同晶型結(jié)構(gòu)的間規(guī)聚丙烯溶液相單晶和熔融相單晶,并利用AFM、透射電子顯微鏡(TEM)、X-射線粉末衍射儀(XRD)、電子衍射(ED)等測試手段對間規(guī)聚丙烯單晶的形貌和晶體結(jié)構(gòu)進(jìn)行表征,結(jié)果表明成功制備了不同結(jié)構(gòu)的間規(guī)聚丙烯單晶,為其微觀尺度力學(xué)性質(zhì)研究奠定了基礎(chǔ)。第三章中主要是間規(guī)聚丙烯晶體單分子力譜實(shí)驗(yàn)的設(shè)計(jì)、實(shí)施與數(shù)據(jù)分析。經(jīng)過多次實(shí)驗(yàn)條件的摸索,建立了聚丙烯分子與AFM針尖的有效偶聯(lián)方法。通過分別對AFM探針針尖和間規(guī)聚丙烯單晶表面修飾氨基和羥基(磺酸基),增強(qiáng)針尖與聚丙烯的結(jié)合強(qiáng)度,使兩者之間可以形成橋聯(lián)結(jié)構(gòu);隨后分別對具有不同晶型結(jié)構(gòu)的間規(guī)聚丙烯單晶進(jìn)行表面隨機(jī)拉伸,得到單分子鏈力-拉伸曲線,從單分子水平上探究將單個聚丙烯鏈從晶體中解折疊的力學(xué)性能,同時對間規(guī)聚丙烯其他聚集態(tài)結(jié)構(gòu)(球晶結(jié)構(gòu)、介晶相結(jié)構(gòu))也進(jìn)行了探究。結(jié)果表明,不同晶型結(jié)構(gòu)的間規(guī)聚丙烯具有不同的力學(xué)穩(wěn)定性,I型單晶單分子力學(xué)穩(wěn)定性最強(qiáng);間規(guī)聚丙烯單晶力學(xué)性能具有晶體厚度依賴性;位于晶體不同晶面中的s PP分子體現(xiàn)出相近的納米力學(xué)性質(zhì)。上述實(shí)驗(yàn)結(jié)果從分子水平上加深了我們對間規(guī)聚丙烯結(jié)構(gòu)與力學(xué)性質(zhì)關(guān)系的認(rèn)識,為間規(guī)聚丙烯材料的性能優(yōu)化與調(diào)控提供了重要依據(jù)。
[Abstract]:Semi-crystalline polymer materials are widely used in many fields of human life because of their excellent properties and use value. Crystalline phase structure plays a decisive role in many aspects of mechanical properties of polymer materials. With the further improvement of material application performance, it is very important to reveal and regulate the relationship between crystal structure and properties, especially the relationship between the horizontal structure of single molecule and the macroscopic properties of materials. The related studies are helpful to better understand the microscopic mechanism of the change of material properties, and thus guide the performance control, design and preparation of high performance polymer crystal materials. The traditional experimental methods are difficult to give the information of the mechanical properties at the molecular level. The appearance of single molecular force spectroscopy (SMFS) based on atomic force microscope (AFM) makes the related research possible. In the first chapter of this thesis, the working mode and application of polymer crystalline state and AFM imaging are systematically introduced, and the single molecular force spectrum technology based on AFM is described in detail, including its working principle, the acquisition of single molecular force-tensile curve. Judgment and Analysis and its important Application in the Field of Materials Science. The main idea of this thesis is to explore the mechanical properties of syndiotactic polypropylene (SPP) crystal materials with the help of AFM single molecule force spectroscopy. The second chapter focuses on the preparation and characterization of syndiotactic polypropylene single crystals with different crystal structure. Through the screening of crystallization conditions, the syndiotactic polypropylene solution phase single crystals and the melt phase single crystals with different crystal structure were prepared, respectively. The morphologies and crystal structures of syndiotactic polypropylene single crystals were characterized by AFM, transmission electron microscopy (TEM) X-ray powder diffraction (XRD) and electron diffraction (Ed). The results showed that syndiotactic polypropylene single crystals with different structures were successfully prepared. It lays a foundation for the study of micro-scale mechanical properties. The third chapter is mainly about the design, implementation and data analysis of single molecule force spectrum experiment of syndiotactic polypropylene crystal. An effective coupling method between polypropylene molecule and AFM tip was established after many experiments. The surface modification of amino group and hydroxyl group (sulfonic group) on the tip of AFM probe and syndiotactic polypropylene single crystal were carried out to enhance the bonding strength between the tip and polypropylene, so that the bridging structure could be formed between them. Then the surface of syndiotactic polypropylene single crystal with different crystal structure was drawn randomly, and the single molecular chain force tensile curve was obtained. The mechanical properties of unfolding single polypropylene chain from crystal were explored from the single molecule level. At the same time, the other aggregation structure (spherulite structure, mesomorphic phase structure) of syndiotactic polypropylene was also studied. The results show that the syndiotactic polypropylene with different crystal structure has different mechanical stability and the mechanical properties of syndiotactic polypropylene single crystal are dependent on crystal thickness. The SPP molecules located in different crystal planes exhibit similar nanomechanical properties. The above experimental results deepen our understanding of the relationship between the structure and mechanical properties of syndiotactic polypropylene at the molecular level and provide an important basis for the performance optimization and control of syndiotactic polypropylene materials.
【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】：O632.12

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