本文關(guān)鍵詞：具有球形形貌的羥基磷灰石納米顆粒的合成研究　出處：《哈爾濱理工大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 羥基磷灰石 碳量子點(diǎn) 硬模板 球形顆粒

【摘要】：羥基磷灰石與人體硬組織的化學(xué)成分和晶體結(jié)構(gòu)極為相似,具有獨(dú)特的生物活性和生物相容性,植入體內(nèi)安全、無(wú)毒,并能與骨中膠原蛋白形成良好的化學(xué)鍵合,被廣泛的用于組織工程、骨的修復(fù)與替代和牙科材料等。近年來(lái),隨著藥物與基因載體研究的發(fā)展,人們逐漸擴(kuò)展了納米HAP的許多其他新用途,如作為蛋白質(zhì)、基因、藥物、生長(zhǎng)因子的控制釋放載體。目前,制備規(guī)整形貌和不同空間結(jié)構(gòu)的羥基磷灰石微納米顆粒,成為了生物材料領(lǐng)域研究的熱點(diǎn)。本研究的目的在于采用模板法制備出單分散球形的羥基磷灰石納米顆粒。本文中,首先探索采用表面活性劑十六烷基三甲基溴化銨(CTAB)在水熱條件下誘導(dǎo)HAP的成核與生長(zhǎng),并研究不同CTAB濃度和反應(yīng)溫度對(duì)產(chǎn)物粒徑和形貌的影響。借助X射線衍射、紅外分析、掃描電鏡、透射電鏡、能譜分析、N2吸附-脫附等檢測(cè)手段對(duì)產(chǎn)物進(jìn)行表征。采用水熱法合成的產(chǎn)物為高結(jié)晶度的HAP顆粒,但是形貌不規(guī)整,顆粒間發(fā)生不可避免的團(tuán)聚現(xiàn)象。為了改善產(chǎn)物的形貌與分散性,開創(chuàng)性的首次將碳量子點(diǎn)(CQDs)引入合成體系中,以其為核誘導(dǎo)磷酸鈣鹽在其表面均相沉積,從而獲得規(guī)整形貌的HAP顆粒,在此過(guò)程中考察CQDs濃度、CTAB用量、反應(yīng)物用量、溶液p H、反應(yīng)溫度、反應(yīng)時(shí)間和不同添加劑對(duì)產(chǎn)物形貌和粒徑的影響。通過(guò)上述的檢測(cè)手段對(duì)合成產(chǎn)物進(jìn)行分析。透射電鏡結(jié)果表明引入的CQDs平均粒徑約5 nm、呈球形、高度分散。然后以CQDs作為核,在其表面吸附表面活性劑CTAB分子層,隨后PO43-通過(guò)靜電引力在CQDs的表面形成PO43-吸附層,與之后引入的鈣源反應(yīng),生成磷酸鈣鹽涂層,調(diào)整反應(yīng)條件使得磷酸鈣鹽均勻的包覆在CQDs的表面從而得到規(guī)整形貌的HAP顆粒。實(shí)驗(yàn)結(jié)果表明:最佳反應(yīng)條件為溶液p H為10,CTAB:Na3PO4的摩爾比為1:1,加入環(huán)己烷,在80℃下反應(yīng)8 h。在最佳條件下合成產(chǎn)物為準(zhǔn)球形的HAP納米顆粒,粒徑約60 nm,顆粒分散性較高。產(chǎn)物Ca/P摩爾比為1.61,略低于HAP中Ca/P的化學(xué)計(jì)量比1.67。比表面積、BJH吸附孔徑和孔容分別為93.5 m2/g,25 nm和0.5682 ml/g,介孔來(lái)源于顆粒間堆積產(chǎn)生的空隙。
[Abstract]:The chemical composition and crystal structure of hydroxyapatite and the hard tissues of the human body is very similar, with unique compatibility and bioactivity in vivo, safe, non-toxic, and can form a good chemically bonded with bone collagen, is widely used in tissue engineering, bone repair and replacement and dental materials etc.. In recent years, with the development of drug and gene carrier research, people have gradually expanded many other new uses of nano HAP, such as the controlled release carrier as protein, gene, drug and growth factor. At present, the preparation of hydroxyapatite micronanoparticles with regular morphology and different spatial structures has become a hot topic in the field of biomaterials. The purpose of this study is to prepare monodisperse spherical hydroxyapatite nanoparticles by template method. In this paper, we first explored the nucleation and growth of HAP under hydrothermal conditions by using surfactant sixteen alkyl three methyl ammonium bromide (CTAB), and studied the effect of different CTAB concentration and reaction temperature on the particle size and morphology of the product. The products were characterized by X ray diffraction, infrared analysis, scanning electron microscopy, transmission electron microscopy, energy spectrum analysis and N2 adsorption desorption. The products synthesized by hydrothermal method are HAP particles with high crystallinity, but the morphology is not regular, and the inevitable agglomeration occurs between the particles. In order to improve the dispersion and the morphology of the product, groundbreaking for the first time the carbon quantum dots (CQDs) into the synthesis system, the induction of calcium phosphate on the surface of sedimentary facies, to obtain HAP regular particles morphology, in this process, the effects of CQDs concentration, CTAB dosage, dosage, reaction effect P H solution, reaction temperature, reaction time and different additives on the morphology and particle size. The synthetic products were analyzed by the above methods. The results of transmission electron microscopy showed that the average particle size of CQDs introduced was about 5 nm, and it was spherical and highly dispersed. Then take the CQDs as the core, on the surface adsorption of surfactant CTAB molecular layer, then PO43- through electrostatic attraction on the surface of the CQDs formation of PO43- adsorption layer, and after the introduction of the source of calcium reaction, formation of calcium phosphate coating, coated calcium phosphate salt makes the adjustment of the reaction conditions to obtain uniform regular particles morphology in CQDs HAP the surface. The experimental results show that the optimum reaction condition is that the solution P H is 10, the molar ratio of CTAB:Na3PO4 is 1:1, and cyclohexane is added, and the reaction is 8 h at 80. Under the best conditions, the synthetic products are quasi spherical HAP nanoparticles, with a particle size of about 60 nm and a high particle dispersion. The molar ratio of the product Ca/P is 1.61, which is slightly lower than the stoichiometric ratio of Ca/P in HAP by 1.67. The specific surface area, BJH pore size and pore volume are 93.5 m2/g, 25 nm and 0.5682 ml/g, respectively. The mesoporous pores are derived from the gap between particles.
【學(xué)位授予單位】：哈爾濱理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：R318;TB383.1

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