Electronic microscopy analysis of HAP single crystals prepared by hydrothermal method

Hydroxyapatite(HAP,Ca10(PO4)6(OH)2in one of the quite important bone implant materials.The hydroxyapatite crystals were synthesized under hydrothermal condition.The specimen was verified to be HAP crystal by the X-ray powder diffractometry(XRD).Then the specimen was distinguished single crystal from polycrystal by the use of the transmission electron microscope(TEM).The diffraction pattern of the specimen is neatly affanged diffraction spots,that verified the crystals were single crystals.The interplanar distance d calculated from diffraction spot is coincided with that of HAP‘s JCPD card.Moreover,crystal face angles calculated from crystal face index are coincided with the values by measuring on the pattern.The HAP crystals are needle-like in shape with about 3μm in diameter and 180μm in length.Most of the crystals are whiskers.Their length/diameter ratio ranges from 40 to 100.The average ratio is about 60.     

等离子体熔融钛与羟基磷灰石混合粉颗粒的形态和相组成

利用等离子喷涂设备将Ti与羟基磷灰石（HA）的混合粉末喷射入水，采用扫描电子显微镜和X射线衍射仪研究了Ti HA入水颗粒的形态和相组成，结果表明，经等离子熔融喷射入水后，钛粒子的尺寸小于HA粒子，主要原因之一是HA内形成了空心结构，空心结构的形成是由于HA在熔融时生成气相P2O5和H2O，它们在颗粒内聚集形成气泡，入水Ti HA粒子主要是由晶相和非晶相HA，分角相磷酸三钙（TCP）和磷酸四钙（TTCP）以及Ti的化合物所组成，由于与Ti的混合，HA的分解加剧，而Ti与HA粒子的融合及元素的扩散在飞行过程中已经发生。     

烧结对羟基磷灰石微球微观结构和性能的影响

利用扫描电镜（SEM）、激光粒度分析仪（LDPSA）、X射线衍射仪（XRD）以及比表面积分析仪（SSA）等检测方法，研究了烧结对于羟基磷灰石微球的微观结构、形貌以及粒径、比表面积和孔隙率等性能的影响。结果表明，经800℃热处理，微球的比表面积、孔隙率及其表面形貌均会发生明显的变化；经1000℃烧结后，部分羟基磷灰石相发生热分解，生成较多的的     

Effects of anodizing voltage on the anodized and hydrothermally treated titanium surface

Anodic oxidation is the process of creating a titanium oxide layer with various defects more dense and stable. In this study, a dense, stable and porous oxide layer was formed using anodic spark oxidation on pure titanium surface and hydroxyapatite crystals were formed on its surface via a hydrothermal treatment. A mixture of 0.02M−GP (Glycerolphosphate disodium salt) and 0.2M-CA (Calcium acetate) was used as an electrolyte. By increasing the anodizing voltage to 220, 260, 300, and 360 V, the effects of the anodizing voltage were examined by evaluating the film properties after anodization and a hydrothermal treatment. Breakdown occurred around 230 V. As the voltage increased after breakdown, the pore size increased. After the hydrothermal treatment, the amount of HA crystal precipitation was also increased as the voltage increased. The mean surface roughness (Ra) of the anodizing surface was also increased as the voltage increased. The Ra value was larger in the hydrothermally treated group compared with the group treated with anodization as a result of the HA crystals present on the surface after the hydrothermal treatment. Corrosion resistance of the surface modified by anodization was significantly increased in a saline solution compared to that for the non-treated group; this increased further after the hydrothermal treatment. These increases were most likely due to a thick stable oxide layer formed through anodization. Thus, it is believed that titanium with its surface modified through anodic spark oxidation would be a suitable biomaterial due to its corrosion resistance and biocompatibility.     

钛合金表面声电沉积／碱热处理法制备HA涂层研究

为了使钛合金（Ti-6Al-4V）具有生物活性，可在其表面施加生物活性羟基磷灰石（HA）涂层。对比了声电沉积法和碱热处理法实验结果，采用扫描电镜（SEM）、X射线衍射仪（XRD）、电子能谱（EDS）、傅立叶红外透射光谱（FTIR）以及划痕测试等进行了分析。结果表明，直接采用声电沉积法在钛合金表面制备的羟基磷灰石涂层，经热处理后存在龟裂剥落现象；通过碱热处理法，对钛合金基体表面进行预处理，然后，借助声电沉积法，在钛金属表面沉积了透钙磷石涂层，经热碱液处理转变成的羟基磷灰石涂层，涂层完整，未出现剥落。经进一步高温烧结处理，所制涂层仍呈片状形貌，其由部分含钠的羟基磷灰石组成，而且HA涂层破坏的临界载荷未烧结前的4．365N提高至烧结后的8．175N。     

Thermal spraying of biomaterials

Osteoconductive hydroxyapatite coatings for metallic endoprostheses for hip and knee joint replacement provide a state-of-the-art template for enhanced in-growth of bone cells. However, the high temperature of the plasma jet leads to large scale dehydroxylation and decomposition of the starting powder. A model is being developed to explain the formation of chemically and mechanically inhomogeneous porous calcium phosphate coatings deposited by atmospheric plasma spraying onto titanium alloy substrates. In addition the biofunctionality is being discussed of titania bond coats and their influence on the in vivo performance of hydroxyapatite-titania duplex coating systems.     

海藻酸钠/羟基磷灰石复合纤维的制备工艺

利用海藻酸钠和羟基磷灰石复合制备复合纤维,并采用正交试验和单因素分析方法研究海藻酸钠质量分数、第一凝固浴质量分数、第一凝固浴温度、纺丝头牵伸比和第二凝固浴组分等制备工艺对纤维断裂强度和镉离子吸附量的影响。综合考虑断裂强度和吸附性能的指标,确定了适宜的制备工艺:海藻酸钠质量分数为3%,第一凝固浴CaCl2质量分数为5%,第一凝固浴温度为15℃,纺丝头牵伸比为负牵伸,第二凝固浴组分为水溶液。     

HA-ZrO2生物复合材料的制备

首先以H3PO4和Ca(OH)2为主要原料利用湿化学方法合成了结晶良好的羟基磷灰石粉体(HA),在该粉体中分别引入15%、20%和25wt%的m-ZrO2粉体,经成型后分别在900℃、1 000℃、1 100℃和1 200℃温度下煅烧1h,详细研究ZrO2含量和烧结温度对该复合材料物相及体积密度的影响规律.结果表明:随着烧成温度的升高,该复合材料的体积密度呈上升趋势,当温度为1 000℃时达到最大值,当温度进一步升高时,体积密度下降.而复合材料中的HA相随温度的升高而不断降低,当温度超过1 000℃时该趋势更加明显.随ZrO2的引入材料体积密度有一定提高,但当ZrO2含量超过20%时,其体积密度有所降低,当ZrO2含量为20%时,杂质含量最低.     

新型基因枪微弹材料可行性初步研究-Ⅰ

基因枪在未来临床基因转导中很有前途,但目前所用微弹材料金、钨都属于重金属,其长期存在于人体的安全性尚无法估计。提出用羟基磷灰石(HAP)微粒来代替金或钨微粒,从理论上推导了这种取代的可行性,并报告了一种HAP微粒的制备及其负载DNA的研究结果。理论推导完全按照物理学方法进行。实验部分的方法:将稳定剂H以一定速度和比例滴入一定浓度的Ca(H2PO4)2溶液中,再按照一定的速度和比例滴入Ca(OH)2饱和溶液,期间或完成后超声处理一定时间,将所得HAP微粒溶液与亚精胺和DNA以一定比例和浓度在一定pH条件下混合。结论:所得HAP粒径值符合要求,并且能够高效负载DNA。     

Sol-gel prepared β-TCP/FHA biphasic coatings

β-tricalcium phosphate/fluoridated hydroxyapatite (β-TCP/FHA) biphasic coatings were prepared on titanium alloy substrate by means of sol-gel method. The coatings combine the initial dissolution of β-TCP with the long-term stability of FHA to create a high quality bioactive coating. Ca(NO₃)₂, P₂O₅ and HPF₆ were dissolved in ethanol respectively and mixed in designed sequence and Ca : P : F ratios to form a sol. After the sol was refluxed for 24 h, the as-refluxed sol was used for FHA coating. β-TCP powders were dispersed into the sols to form colloidal sols for β-TCP/FHA biphasic coatings. The as-refluxed sols with different Ca : P : F ratios only resulted in apatite coatings with low F content. Biphasic coatings were prepared with the colloidal sols. The β-TCP contents of the coatings could be tailored by varying the amount of the powders in the colloidal sols. The surface morphology of the coatings becomes rougher with increasing amount of the powders, which favors cell attachment. However, excessive amount of powders results in powder agglomeration, leading to more cracks in the coatings. Fine powders and good dispersion are essential factors for good biphasic coatings.