本文選題：二氧化硅包覆的羥基磷灰石 + 生物玻璃�。� 參考：《武漢理工大學(xué)》2013年博士論文

【摘要】：多孔羥基磷灰石(HAP)基生物陶瓷因?yàn)榕c人體骨骼的無機(jī)化合成分相似,具有很好的生物相容性和成骨與誘導(dǎo)骨形成的導(dǎo)向作用,已被廣泛用作生物體硬組織修復(fù)。目前,有關(guān)多孔HAP陶瓷在醫(yī)學(xué)領(lǐng)域的研究已經(jīng)延伸到將其作為藥物載體以及抗腫瘤活性上,且發(fā)現(xiàn)將多孔陶瓷作為藥物載體有廣泛的應(yīng)用前景和重要的研究價(jià)值。本論文以多孔陶瓷作為藥物控釋緩釋載體為研究背景,為制備出滿足實(shí)際需要的多孔體,對材料的組成進(jìn)行了設(shè)計(jì),研制了以納米生物玻璃作為增強(qiáng)相、納米炭粉為成孔劑的工藝,并對多孔材料的結(jié)構(gòu)和性能進(jìn)行了表征。采用不同溶液對多孔陶瓷進(jìn)行了滲透與反滲透評估,通過體外RSC96細(xì)胞與材料的作用,對其進(jìn)行生物學(xué)評價(jià)等。主要內(nèi)容如下： 合成了形貌不同的羥基磷灰石納米粒子,并分析討論了影響HAP形貌的主要參數(shù)。通過異質(zhì)凝結(jié)機(jī)制,利用TEOS水解對經(jīng)十二烷醇酯化后的HAP納米粒子進(jìn)行表面SiO2包覆改性(HAPSi050),研究了不同SiO2含量對產(chǎn)物包覆率及其在水和酸溶液中溶解性能的影響。改性后獲得的粒子通過FT-IR、XRD、 SEM-EDS、HR-TEM、TG-DSC和Zeta電位等分析方法表征合成的SiO2改性HAP的結(jié)構(gòu)與性能,并觀察了其在水溶液中的懸浮穩(wěn)定性能。結(jié)果表明：SiO2包覆層厚度大約為3nm,表面改性后,Zeta電勢均為負(fù)值,粒子在水溶液中的懸浮穩(wěn)定性提高了5倍,抗酸溶解能力增強(qiáng)。 通過W/O型微乳液技術(shù)合成了SiO2-CaO-P2O5系統(tǒng)生物活性玻璃納米粒子,探討了水與表面活性劑的摩爾比ω的變化對合成的納米粒子結(jié)構(gòu)和性能的影響。并對合成的粒子進(jìn)行了體外降解和與RSC96細(xì)胞聯(lián)合培養(yǎng)的研究。采用FTIR、 XRD、SEM-EDS、XRF、TEM、BET比表面積分析儀和激光粒度分析儀等手段對合成的和經(jīng)過降解的納米玻璃粒子進(jìn)行表征,結(jié)果表明：合成的球形納米玻璃粒子尺寸在100nnm左右,分布均勻,分散性較好；顆粒之間彼此連接而具有微孔結(jié)構(gòu),測得的比表面積和孔體積分別為137.9cm3/g和0.37cm3/g。測定降解過程中降解介質(zhì)pH值、離子溶出行為表明：材料在生理環(huán)境中,經(jīng)過較短的時間即可在玻璃顆粒表面形成類骨HCA,同時有離子溶出現(xiàn)象發(fā)生,說明材料具有較高的體外生物活性和良好的降解性能。材料在降解過程中溶液的pH值略呈上升的趨勢,基本處于中性。MTT實(shí)驗(yàn)測試細(xì)胞增殖表明材料能促進(jìn)細(xì)胞的增殖,說明合成的納米玻璃粒子有良好的細(xì)胞親和性,可作為生物材料使用。 以HAPSi050納米粉體為原料,SiO2-CaO-P2O5系統(tǒng)生物玻璃為增強(qiáng)相,納米活性炭粉作造孔劑,制備出了孔徑彼此貫通、分布均勻、且孔隙率可調(diào)的多孔生物陶瓷。利用XRD、SEM等手段測試多孔體的相組成及微觀形貌,采用萬能試驗(yàn)機(jī)、硬度計(jì)以及滲透率測試儀測定多孔孔體的力學(xué)性能及流體滲透率。并應(yīng)用ANSYS軟件和圖像處理技術(shù)進(jìn)一步分析孔形貌對力學(xué)性能的影響。結(jié)果發(fā)現(xiàn)：抗折強(qiáng)度隨燒結(jié)溫度和生物玻璃含量的增加而升高,氣孔率和滲透率則隨相應(yīng)因素的升高而降低。氣孔率和滲透率隨炭粉含量增加呈上升趨勢,但是抗彎強(qiáng)度卻逐漸降低。圖像處理和ANSYS分析表明：試樣中孔越圓、近圓形孔的數(shù)量越多、孔分布越均勻,多孔體力學(xué)性能越高。 多孔陶瓷經(jīng)模擬體液浸泡,測定礦化過程中材料失重率、抗折強(qiáng)度的變化和采用掃描電子顯微鏡(SEM)觀察材料微觀結(jié)構(gòu)變化表明：浸泡初期試樣表面即有類骨磷灰石形成,預(yù)示著材料有較好的生物礦化能力。但同時,試樣的質(zhì)量和抗折強(qiáng)度降低。之后,隨著試樣表面類骨磷灰石數(shù)量的增多,試樣的質(zhì)量和強(qiáng)度又開始回升并逐漸增加。將RSC96細(xì)胞與多孔陶瓷體外聯(lián)合培養(yǎng),通過細(xì)胞增殖、細(xì)胞毒性、SEM觀察進(jìn)行生物學(xué)評價(jià)。噻唑藍(lán)(MTT)比色法表明多孔體材料能促進(jìn)細(xì)胞的增殖；吉姆薩和熒光探針技術(shù)測試細(xì)胞毒性表明多孔材料與對照組單相HAP一致；SEM觀察表明RSC96細(xì)胞在多孔材料上鋪展良好,證明多孔體具有良好的細(xì)胞親和性和生物活性。
[Abstract]:Porous hydroxyapatite (HAP) based bioceramics have been widely used as hard tissue repair for biological compatibility and osteogenesis and induced bone formation because they are similar to the inorganic compounds of human skeleton, and have been widely used in the medical field as a drug carrier. As well as the anti-tumor activity, porous ceramics as drug carrier have wide application prospects and important research value. In this paper, porous ceramics are used as drug controlled release sustained-release carriers as research background. In order to prepare porous bodies to meet the actual needs, the composition of materials is designed and nano glass is developed. The structure and properties of the porous materials were characterized by the enhancement phase and the nano carbon powder as the pore forming agent. The porous ceramics were evaluated by permeation and reverse osmosis by different solutions. The biological evaluation of the porous ceramics by the effect of RSC96 cells and materials in vitro was carried out. The main contents were as follows:
The hydroxyapatite nanoparticles with different morphologies were synthesized and the main parameters affecting the HAP morphology were analyzed and discussed. The surface SiO2 coating modification (HAPSi050) of the HAP nanoparticles after twelve alkanols was hydrolyzed by TEOS hydrolysis by the heterogeneous condensation mechanism. The coating rate of the products and the solution in water and acid solution were studied with different SiO2 content. The properties of the modified particles were characterized by FT-IR, XRD, SEM-EDS, HR-TEM, TG-DSC and Zeta potential, and the structure and properties of the synthesized SiO2 modified HAP were characterized, and the suspension stability was observed in the aqueous solution. The results showed that the thickness of the SiO2 coating layer was about 3nm, and the Zeta potential was negative after surface modification. The stability of the suspension in aqueous solution increased by 5 times and the ability to resist acid dissolution increased.
SiO2-CaO-P2O5 system bioactive glass nanoparticles were synthesized by W/O microemulsion technology. The influence of the change of molar ratio omega of water and surfactant on the structure and properties of synthesized nanoparticles was investigated. The degradation of synthesized particles in vitro and co culture with RSC96 cells were studied. FTIR, XRD, SEM-EDS, XRF, TE were used. M, BET ratio surface area analyzer and laser particle size analyzer are used to characterize the synthesized and degraded nanoscale glass particles. The results show that the size of the spherical nano glass particles is around 100nnm, the distribution is uniform and the dispersibility is good; the particles are connected to each other with microporous structure, the specific surface area and pore body are measured. The integration of 137.9cm3/g and 0.37cm3/g. to determine the pH value of degradation medium in the degradation process, the dissolution behavior of ion shows that the material can form bone like HCA on the surface of glass particles in a short time in physiological environment, and the phenomenon of ion dissolution occurs, indicating that the material has higher biological activity in vitro and good degradation performance. In the process of degradation, the pH value of the solution is slightly rising, and the proliferation of the cells can be promoted by the neutral.MTT test. It shows that the synthesized nano glass particles have good cell affinity and can be used as biomaterials.
The porous bioceramics with HAPSi050 nano powder as raw material, SiO2-CaO-P2O5 system Bioglass as enhanced phase and nano activated carbon powder as pore making agents, the porous bioceramics with pore penetration, uniform distribution and adjustable porosity were prepared. The phase composition and Micromorphology of the porous body were tested by means of XRD and SEM, and the universal testing machine, hardness meter and seepage were used. The mechanical properties and fluid permeability of porous pores were measured by the permeability test instrument. The effect of pore morphology on the mechanical properties was further analyzed by ANSYS software and image processing technology. The results showed that the flexural strength increased with the increase of sintering temperature and the content of Bioglass, and the porosity and permeability decreased with the increase of the corresponding factors. The porosity and permeability increase with the increase of carbon powder content, but the bending strength decreases gradually. The image processing and ANSYS analysis show that the holes in the specimen are round, the number of near circular holes is more, the distribution of holes is more uniform and the mechanical properties of the porous body are higher.
Porous ceramics were soaked in simulated body fluid to determine the material weight loss rate, the change of fracture strength and the microstructure change of the material observed by scanning electron microscope (SEM). It showed that the surface of the sample was formed at the initial surface of the sample, indicating the better biomineralization ability of the material, but at the same time, the quality and the bending resistance of the specimen were also found. Then, with the increase in the number of apatite on the surface of the specimen, the quality and strength of the sample began to recover and gradually increase. RSC96 cells were co cultured with porous ceramics in vitro, and biological evaluation was carried out through cell proliferation, cytotoxicity, and SEM observation. MTT colorimetric assay showed that porous material could promote cell growth. Proliferation, the test of cytotoxicity by Giemsa and fluorescence probe showed that the porous material was the same as the single phase HAP in the control group, and the SEM observation showed that the RSC96 cells spread well on the porous material, which proved that the porous body had good cell affinity and biological activity.

【學(xué)位授予單位】：武漢理工大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2013
【分類號】：R318.08

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本文編號：1868765