溶胶-凝胶法制备纳米羟基磷灰石粉体的研究进展

目的利用溶胶-凝胶法制备纳米羟基磷灰石粉体的方法进行研究.方法综述了溶胶-凝胶法的基本原理和分类,介绍了制备纳米羟基磷灰石粉体采用的溶胶-凝胶方法,提出了相关待解决的问题.结果溶胶-凝胶法的研究已取得一定的进展.结论利用该方法有望制备出形状可控、粒度均匀的纳米羟基磷灰石粉体.     

快速溶胶-凝胶法制备纳米级羟基磷灰石

目的以四水硝酸钙和五氧化二磷为原料，无水乙醇为溶剂采用溶胶-凝胶法合成纳米羟基磷灰石。方法利用TG—DTA曲线分析凝胶的特性，利用XRD和FTIR研究干凝胶烧结后的组成变化，并采用TEM观察合成粉体的形貌与尺寸。结果经700℃焙烧可得到最大粒径25nm左右，分散良好的纳米羟基磷灰石。加入聚乙二醇(PEG)作络合剂，可得到粒径25nm左右，尺寸分布均匀的纳米羟基磷灰石。结论采用该溶胶一凝胶法可以合成颗粒大小均匀，分散性好的纳米羟基磷灰石粉体。该法的优点是无需调节pH值，且无需剧烈搅拌和长时间的水解即可成胶，HA的合成周期较短，所得纳米粉体的稳定性好。     

快速溶胶-凝胶法制备纳米级羟基磷灰石

目的以四水硝酸钙和五氧化二磷为原料,无水乙醇为溶剂采用溶胶-凝胶法合成纳米羟基磷灰石.方法利用TG-DTA曲线分析凝胶的特性,利用XRD和FTIR研究干凝胶烧结后的组成变化,并采用TEM观察合成粉体的形貌与尺寸.结果经700℃焙烧可得到最大粒径25nm左右,分散良好的纳米羟基磷灰石.加入聚乙二醇(PEG)作络合剂,可得到粒径25nm左右,尺寸分布均匀的纳米羟基磷灰石.结论采用该溶胶-凝胶法可以合成颗粒大小均匀,分散性好的纳米羟基磷灰石粉体.该法的优点是无需调节pH值,且无需剧烈搅拌和长时间的水解即可成胶,HA的合成周期较短,所得纳米粉体的稳定性好.     

纳米羟基磷灰石的制备及其抗肿瘤活性的研究

采用溶胶凝胶法合成了含CO32 - 的纳米羟基磷灰石 ,研究了热处理温度对羟基磷灰石结晶性能、粒子大小和形貌的影响。并采用体外细胞培养的方法对含CO32 - 纳米羟基磷灰石的抗肿瘤活性进行了初步的探索。结果表明 :以Ca(NO3) 2 ·4H2 O和PO(CH3O) 3为原料 ,采用溶胶凝胶法 ,6 0 0℃处理可得到结晶性能良好、分散均匀、5 0nm左右大小的含CO32 - 的羟基磷灰石粉体。MTT比色法研究结果表明纳米HAP粒子对正常肝细胞L 0 2的抑制率较小 ,而对BEL 74 0 2肝癌细胞有明显的抑制作用 ,且呈现明显的浓度和时间依赖性。荧光显微照片显示纳米HAP粒子能够诱导BEL 74 0 2肝癌细胞的凋亡。     

煅烧温度对纳米羟基磷灰石性能的影响

目的探讨煅烧温度对羟基磷灰石结晶性能、晶粒尺寸、形貌的影响。方法以四水硝酸钙和五氧化二磷为原料,无水乙醇为溶剂,采用溶胶-凝胶法制备出羟基磷灰石(HAP)纳米粉体。利用X射线衍射分析(XRD)和红外光谱(FTIR)研究煅烧温度对羟基磷灰石结晶性能、晶粒尺寸、形貌的影响。采用扫描电镜(SEM)观察制备粉体的表面形貌和尺寸。结果500℃可初步形成结晶度不太高的HAP;650℃则晶化程度提高;到800℃时晶化程度更高。凝胶HAP经500℃煅烧后,颗粒以团聚为主,边界不清;650℃时结晶粒度大小为48nm,800℃时为78nm。结论采用溶胶凝胶法,650℃处理可得到结晶性能良好、分散均匀、50nm左右大小的羟基磷灰石粉体。煅烧温度对羟基磷灰石粉体的制备有重要影响,温度过低,晶化程度差,晶粒尺度小,提高煅烧温度有利于HAP晶化程度的提高。     

煅烧温度对纳米羟基磷灰石性能的影响

目的 探讨煅烧温度对羟基磷灰石结晶性能、晶粒尺寸、形貌的影响.方法 以四水硝酸钙和五氧化二磷为原料,无水乙醇为溶剂,采用溶胶-凝胶法制备出羟基磷灰石(HAP)纳米粉体.利用X射线衍射分析(XRD)和红外光谱(FTIR)研究煅烧温度对羟基磷灰石结晶性能、晶粒尺寸、形貌的影响.采用扫描电镜(SEM)观察制备粉体的表面形貌和尺寸.结果 500℃可初步形成结晶度不太高的HAP;650℃则晶化程度提高;到800℃时晶化程度更高.凝胶HAP经500℃煅烧后,颗粒以团聚为主,边界不清;650℃时结晶粒度大小为48 nm,800 ℃时为78 nm.结论 采用溶胶凝胶法,650℃处理可得到结晶性能良好、分散均匀、50 nm左右大小的羟基磷灰石粉体.煅烧温度对羟基磷灰石粉体的制备有重要影响,温度过低,晶化程度差,晶粒尺度小,提高煅烧温度有利于HAP晶化程度的提高.     

钽表面碳酸钙薄膜水热合成羟基磷灰石薄膜及性能

采用溶胶-凝胶法在碱液预处理的钽片表面制备碳酸钙薄膜,然后分别采用磷酸氢二铵、磷酸氢钙及β-甘油磷酸钠进行水热处理,合成羟基磷灰石薄膜。结构和成分分析表明,溶胶-凝胶法在钽表面形成了由密集的纳米颗粒组成的碳酸钙薄膜,在磷酸氢二铵和磷酸氢钙溶液中水热处理的试样表面形成了羟基磷灰石纳米晶体。水接触角和动电位极化测试表明,这两种溶液处理的试样均具有良好的亲水性和耐蚀性。     

羟基磷灰石/聚苯硫醚复合材料的制备及体外生物相容性

背景:利用传统固相复合工艺难以将纳米级羟基磷灰石粉体与聚苯硫醚进行复合,从而无法发挥纳米材料的优势,并且目前缺少羟基磷灰石/聚苯硫醚复合材料生物相容性的相关研究。目的:应用液相复合工艺制备纳米羟基磷灰石/聚苯硫醚复合材料,评价其体外生物相容性。方法:应用液相复合工艺制备纳米羟基磷灰石/聚苯硫醚复合材料粉体和片材,利用红外光谱分析仪及扫描电镜分析复合材料的成分结构;利用接触角测试仪评估材料的亲水性,利用兔血及L929小鼠成纤维细胞进行材料的溶血实验及体外细胞毒性实验。结果与结论:通过液相复合工艺制备的羟基磷灰石/聚苯硫醚复合材料混合均匀,结合紧密;聚苯硫醚粉体的接触角为81.25°,而纳米羟基磷灰石/聚苯硫醚复合材料粉体接触角为16.1°;聚苯硫醚片材的接触角为83.5°,纳米羟基磷灰石/聚苯硫醚复合材料片材的接触角为42.5°,对比可知,纳米羟基磷灰石的加入明显改善了单纯聚苯硫醚材料的亲水性能。纳米羟基磷灰石/聚苯硫醚复合材料的溶血率为1.66%(5%),提示材料血液相容性良好;L929细胞在材料浸提液中生长良好,CCK-8法检测提示体外细胞毒性属无毒范畴(0至1级)。以上结果表明羟基磷灰石/聚苯硫醚复合材料制备成功,体外生物相容性良好。     

纳米羟基磷灰石粉体的合成与分散技术进展

本文综合论述了羟基磷灰石粉体的主要制备方法.在对纳米羟基磷灰石颗粒团聚机理探讨的基础上,分析了该粉体几种主要分散技术研究现状,提出通过改进湿法制备工艺获得高分散性医用羟基磷灰石粉体的技术思路.     

溶胶-凝胶法制备纳米羟基磷灰石超薄薄膜及其表征

分别使用有机溶胶-凝胶以及无机溶胶作为羟基磷灰石（HA）前驱体，利用浸渍涂层（Dip-coating）技术在钛表面制备纳米超薄薄膜。利用扫描电镜（SEM）和X射线衍射（XRD）表征薄膜形态、微晶尺寸分布（D）和微观应变（ε）。结果表明：在大于400℃热处理后，薄膜开始呈现磷灰石结构；在400℃～600℃范围内，热处理温度对两种磷灰石薄膜D和ε的影响显著；SEM结果证明HA前驱体种类严重影响两种纳米HA薄膜的颗粒团聚尺寸；有机溶胶-凝胶和无机凝胶在钛表面制备的HA薄膜颗粒团聚尺寸分别为25nm和100nm，薄膜厚度分别为2．5μm和5．0μm。浸渍涂层技术制备的HA薄膜表面／界面形态完整，薄膜表面无明显微裂纹。     

三种方法对硼酸铝晶须表面改性作用及其对复合树脂性能的影响

分别采用三种不同方法对硼酸铝晶须(AlBw)进行表面改性。方法一:将AlBw与商品纳米二氧化硅(SiO2)在一定工艺下直接高温熔附;方法二:将正硅酸乙酯(TEOS)用溶胶-凝胶法水解形成Si-O网络结构的膜,同时包裹于AlBw表面,进一步与商品纳米SiO2高温熔附;方法三:用溶胶-凝胶法在一定工艺条件下使TEOS水解得到纳米SiO2,同时沉积于AlBw表面,然后高温熔附。透射电镜(TEM)和扫描电镜(SEM)观察不同方法改性AlBw后其表面形态的变化。按一定质量比加入树脂基质中,测试树脂弯曲性能,SEM观察断口形貌。结果表明:晶须改性后可以提高复合树脂的弯曲性能,不同改性方法作用不同;商品SiO2纳米颗粒直接熔附于AlBw进行表面改性,复合树脂的弯曲强度达(95.28±4.53)MPa,但AlBw、纳米SiO2间团聚明显;采用TEOS溶胶-凝胶法对AlBw进行表面处理后与商品SiO2纳米颗粒混合,团聚有改善,但分布不均匀;采用TEOS溶胶-凝胶法直接生成纳米SiO2改性AlBw,是一种理想的改性方法,经此法改性的AlBw-SiO2复合体可以显著提高复合树脂的弯曲性能,复合树脂的弯曲强度达(130.29±8.38)MPa,SiO2粒径分布均匀,AlBw表面有分布较均匀的、分散的SiO2纳米颗粒熔附,团聚程度降低。     

Hard-tissue-engineered zirconia porous scaffolds with hydroxyapatite sol-gel and slurry coatings

A zirconia (ZrO(2)) porous scaffold was coated with a gradient apatite layer to induce osteoconductivity with the use of a combination of sol-gel and powder slurry methods. The ZrO(2) was used to impart mechanical strength and the apatite layer was coated for functional biocompatibility. The coating layer, from the outside in, was composed of sol-gel hydroxyapatite (HA)/slurry HA/slurry FA. The sol-gel coating powder had a lower crystallinity than the slurry coating powder. The sol-gel HA coating over the HA/FA slurry coating layer made the surface very smooth. The sol-gel coating over the slurry coating layer enhanced the bonding strength up to 33 MPa. The dissolution rate of the sol-gel/slurry coating layer was much higher than that of the slurry coating. Moreover, the rate could be controlled by altering the heat-treatment temperature of the sol-gel HA layer. The MG63 cells cultured on these materials grew and spread in a different manner, depending on the coating layer. However, the proliferation rates of the cells on both coating systems were not much different.     

Sol-gel processed porous silica carriers for the controlled release of diclofenac diethylamine

Silica xerogels doped with diclofenac diethylamine were prepared by the sol-gel method from a hydrolysed tetraethoxysilane (TEOS) solution containing diclofenac diethylamine. Two different catalysts, drying conditions and levels of water content were used to alter the microstructure of the silica xerogels. The aim of this study was to determine the rate of Diclofenac release from the silica xerogels. This in vitro study showed that the sol-gel method is useful for entrapping Diclofenac in the pores of xerogels. It also showed that, in vitro, Diclofenac is released from the silica xerogel, through the pores, by diffusion. Base-catalysed gels proved to be much more effective than acid-catalyzed gels.     

Biocompatibility of titanium implants modified by microarc oxidation and hydroxyapatite coating

A thin hydroxyapatite (HA) layer was coated on a microarc oxidized titanium (MAO-Ti) substrate by means of the sol-gel method. The microarc oxidation (anodizing) enhanced the biocompatibility of the Ti, and the bioactivity was improved further by the sol-gel HA coating on the anodized Ti. The HA sol was aged fully to obtain a stable and phase-pure HA, and the sol concentration was varied to alter the coating thickness. Through the sol-gel HA coating, the Ca and P concentrations in the coating layer increased significantly. However, the porous morphology and roughness of the MAO-Ti was altered very little by the sol-gel treatment. The proliferation and alkaline phosphatase (ALP) activity of the osteoblast-like cells on the MAO/HA sol-gel-treated Ti were significantly higher than those on the MAO-Ti without the HA sol-gel treatment.     

磁性SiO2微球的制备、表面修饰及其在生物医学领域的应用

磁性SiO2微球是一种新型的功能材料,在生物医学领域有着广泛的应用前景,可用于靶向药物、免疫磁珠、蛋白和核酸分离、固定化酶及天然产物的分离与纯化等方面。综述了磁性SiO2微球的制备、表面修饰及其在生物医学领域的应用发展趋势和前景,重点分析了核壳型和分散型微球所采用的几种制备方法,如溶胶一凝胶法、液相沉积法、自组装法和微乳液法等。     

磁性SiO2微球的制备、表面修饰及其在生物医学领域的应用

磁性SiO2微球是一种新型的功能材料,在生物医学领域有着广泛的应用前景,可用于靶向药物、免疫磁珠、蛋白和核酸分离、固定化酶及天然产物的分离与纯化等方面.综述了磁性SiO2微球的制备、表面修饰及其在生物医学领域的应用发展趋势和前景,重点分析了核壳型和分散型微球所采用的几种制备方法,如溶胶-凝胶法、液相沉积法、自组装法和微乳液法等.     

磁性SiO2微球的制备、表面修饰及其在生物医学领域的应用

磁性SiO2微球是一种新型的功能材料,在生物医学领域有着广泛的应用前景,可用于靶向药物、免疫磁珠、蛋白和核酸分离、固定化酶及天然产物的分离与纯化等方面.综述了磁性SiO2微球的制备、表面修饰及其在生物医学领域的应用发展趋势和前景,重点分析了核壳型和分散型微球所采用的几种制备方法,如溶胶-凝胶法、液相沉积法、自组装法和微乳液法等.     

Collagen-silica xerogel nanohybrid membrane for guided bone regeneration

A collagen-silica xerogel hybrid membrane was fabricated by a sol-gel process for guided bone regeneration (GBR). The silica xerogel synthesized by the sol-gel method was distributed uniformly within the collagen matrix in the form of nanoparticles. The hybridization of the silica xerogel with collagen improved the biological properties of the membrane significantly. Preosteoblast cells were observed to adhere well and grow much more actively on the hybrid membrane than on the pure collagen membrane. In particular, the hybrid membrane containing 30% of the silica xerogel showed the highest level of osteoblast differentiation. Moreover, the GBR ability, as assessed by the in vivo animal test, was superior to that of the pure collagen membrane. These findings suggest that the collagen-silica xerogel hybrid can be used as a GBR membrane.     

A synthesis route to nanoparticle dicalcium silicate for biomaterials research

Dicalcium silicate (Ca? SiO?) has been reported as an interesting candidate for biomaterials use due to its attractive bioactive properties. Here, we report on how dicalcium silicate was prepared by a sol-gel route using calcium nitrate tetrahydrate and tetraorthosilicate as the precursors chemicals for CaO and SiO? , respectively. The synthesized powders were characterized using thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) method, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). High purity dicalcium silicate at a CaO/SiO? molar ratio of 2:1 could be formed by the sol-gel method without a washing process and was then calcined at 800°C. The effects of the molar ratio of CaO/SiO? , the washing process, and the calcination temperature have been shown to affect the purity, the formation, and the particle size of the nanoparticles, which have been investigated and discussed.     

Surface and biological evaluation of hydroxyapatite-based coatings on titanium deposited by different techniques.

Hydroxyapatite coatings have been deposited on titanium cp by plasma spray, sol-gel, and sputtering techniques for dental implant applications. The latter two techniques are of current interest, as they allow coatings of micrometer dimensions to be deposited. Coating morphology, composition, and structure have been investigated by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). All coatings were homogeneous and exhibited a rough morphology suitable for implant applications. The sputtered (after annealing), plasma spray, and sol-gel coatings all showed diffraction peaks corresponding to hydroxyapatite. The surface contaminants were observed to be different for the different coating types. The sputtered coatings were found to have a composition most similar to hydroxyapatite; the sol-gel deposits also showed a high concentration of hydroxyl ions. A discrepancy in the Ca/P ratio was observed for the plasma spray coatings, and a small concentration of carbonate ions was found in the sputter-deposited coatings. The in vitro cell-culture studies using MG63 osteoblast-like cells demonstrated the ability of cells to proliferate on the materials tested. The sol-gel coating promotes higher cell growth, greater alkaline phosphatase activity, and greater osteocalcin production compared to the sputtered and plasma-sprayed coatings.