纳米缺钙羟基磷灰石生物陶瓷涂层中相组成和显微结构的控制

研究了低钙磷比溶液电沉积缺钙羟基磷灰石生物陶瓷涂层在水热合成和700℃,800℃,900℃焙烧后的相组成和显微组织结构;用扫描电镜(SEM)、X射线衍射(XRD)和透射电镜(TEM)对涂层进行分析。结果表明:在电沉积液Ca/P比1.30,沉积液温度25℃,电压4V条件下,Ti基体表面沉积了片状和条状HAP和CaHPO4·2H2O混合相涂层;在pH值为12的碱液中,150℃和200℃水热合成4h后涂层由针状纯HAP组成,Ca/P比约为1.61,且随着水热合成温度的升高,晶体结晶度提高,但晶体无明显长大趋势;700℃焙烧后,涂层仍由纯HAP组成,只是晶体因失水而发生团聚;800℃焙烧后,部分HAP发生分解,生成β-Ca3(PO4)2,且HAP与β-Ca3(PO4)2的体积比为90∶10,形貌为块状和板条状,其表面附着许多细小的针状颗粒;900℃焙烧后,β-Ca3(PO4)2的含量增加,HAP与β-Ca3(PO4)2的体积比为74∶26,小颗粒团聚成较大的块状和板条状颗粒。由此制备了对骨组织生长更有利的HAP+β-Ca3(PO4)2双相涂层结构。     

纯钛表面微弧氧化羟基磷灰石膜的制备

应用微弧氧化技术在纯钛表面制备了含羟基磷灰石的氧化物膜。在氧化过程中,将钛试件放入含磷酸二氢钠(NaH2PO4.H2O)和乙酸钙((CH3COO)2Ca.H2O)的电解液中,用双脉冲交流电源处理。用扫描电镜(SEM)观察试件的表面形貌,用普通光学显微镜(OM)观察试件的截面形貌,用X射线衍射(XRD)分析其显微结构。结果表明,微弧氧化处理后,纯钛表面生成了内层致密外层多孔的氧化膜。     

非理想化学计量配比掺锶磷灰石的高温热稳定性

采用水化方法制备出不同掺锶量的非理想化学计量配比掺锶磷灰石,使用XRD、IR与TEM等方法检测其高温热稳定性.结果表明:同一制备条件及相同非理想化学计量配比下,掺锶磷灰石的高温热稳定性不如纯磷灰石,且分解产物磷酸三钙锶(Ca,Sr)3(PO4)2)的相转变(α相→β相)温度低于纯磷酸三钙.掺锶量越多,分解产物磷酸三钙锶中含锶量越多.随加热温度升高,含锶磷灰石与纯磷灰石晶粒均逐渐长大.1200℃以下,掺锶磷灰石晶粒近似等轴状,纯磷灰石形状不规则.1300℃时,两种磷灰石粉末中的晶粒尺寸有大有小,大晶粒为长大的磷灰石,形状不规则;小晶粒为分解生成的磷酸三钙锶(或者磷酸三钙),呈球状.     

Sol-Gel法合成纳米羟基磷灰石及晶粒生长、结晶度的研究

以Ca(NO3)2·4H2O与H3PO4为前躯体,采用溶胶-凝胶法制备出纳米羟基磷灰石(HA)粉体。通过差热分析仪、X-射线衍射仪、SEM对HA粉体及烧结体进行了表征和分析,采用阿基米德排水法测试了样品密度。结果表明:粒径分布均匀、呈球形、团聚极少,a轴方向和c轴方向的晶粒尺寸分别为10~30nm和20~50nm,随着温度的升高颗粒的尺寸和结晶度增大。600℃烧结2h得到纯度高、晶化好的HA;800和900℃烧结样品中出现的少量Ca3(PO4)2和CaO是由于HA的分解和含磷前躯体的挥发所致。     

多孔TiNi合金表面沉积羟基磷灰石与表征

采用粉末冶金方法,以Ti、Ni纯元素粉末制备近等原子比TiNi合金,并通过仿生溶液生长法对合金进行表面改性。利用X射线衍射(XRD)、扫描电子显微镜(SEM)和X射线能谱(EDS)分析不同烧结温度(950,1000,1050,1100℃)、不同孔隙特性的金属基体表面羟基磷灰石相组成和微观结构。结果表明,采用粉末冶金方法制备的TiNi合金孔隙度较高,仿生矿化后的XRD图谱中羟基磷灰石相的衍射峰尖锐。在同等时间、同等矿化条件下,羟基磷灰石在1050和1100℃烧结而成的多孔TiNi合金表面结晶度较高,沉积层较厚,沉积效果相对较好。在一定范围内,孔隙率的增加有利于羟基磷灰石的形核与生长;而尺寸较小的孔洞底部会形成一个低离子浓度区域,不利于磷灰石的形核与长大。     

微束等离子喷涂氧化锆增韧羟基磷灰石复合涂层

采用微束等离子喷涂方法,在Ti-6Al-4V基体上制备了羟基磷灰石 氧化锆(70HA-30ZrO2,质量分数,%)复合涂层.将复合涂层置于模拟体液中分别浸泡了3,7,14,28 d并观察表面磷灰石的生长情况以评价涂层生物活性.采用扫描电镜(SEM)和X射线衍射(XRD)分析技术对涂层浸泡前后的表面形貌和相组成进行了研究.结果表明,涂层中ZrO2主要以立方相存在;喷涂过程中羟基磷灰石(HA)出现了一定的分解,产生大量的α-Ca3(PO4)2杂质相.HA涂层熔化效果很好,但涂层中有未熔化的ZrO2颗粒.涂层在模拟体液中浸泡28 d后表面可以形成磷灰石,说明涂层具有很好的生物活性.     

微波加速合成含碳酸根纳米羟基磷灰石

为加速合成仿自然骨的含碳酸根纳米羟基磷灰石（CHA），以Ca（NO3）2·4H2O、NH4HCO3和（NH4）2HPO4为原料，采用微波快速（1h）制备出纳米碳酸羟基磷灰石。采用TEM、XRD、IR测定了CHA的形貌和粒径、研究了CHA的取代类型及其热稳定性。研究结果表明：（1）微波加速合成的粉末为AB混合型取代，粒径为15～30nm、长约40nm的短捧状碳酸纳米羟基磷灰石；（2）煅烧温度对产物的相组成和CO3^2-的含量有很大影响，在700℃时，CHA稳定存在，CHA在900℃或900℃以上分解成TCP和HA的双相钙磷陶瓷粉末，并脱出部分CO2。说明微波法是一种快速合成热稳定性好的纳米碳酸羟基磷灰石的好方法。     

Ca(OH)_2-H_3PO_4体系合成羟基磷灰石粉末的工艺参数

采用Ca(OH)2-H3PO4体系合成羟基磷灰石粉末,研究了原料粒度、pH值、磷酸滴加速率、反应物浓度、反应时间、反应温度及煅烧温度对合成粉体性能的影响。应用X射线衍射(XRD)和透射电镜(TEM)测试方法对合成粉体的组成、颗粒形貌进行表征。用Nano Measurer软件计算粉体的粒度分布。结果表明:Ca(OH)2原料粒度在75~100?m区间,反应物浓度为0.15 mol/L,磷酸的滴定速率是8 mL/s,pH值大于7.5,在0℃反应6 h后,前驱体经过750℃煅烧后可获得纯度、结晶度、分散性和颗粒度均较好的HA粉体。     

采用水热方法在镍钛合金表面一步合成TiO2-羟基磷灰石纳米薄膜

采用高浓度的CaHPO4和Ca(H2PO4)2溶液对镍钛合金进行一步水热处理,以进行生物活性表面改性。经过处理的试样表面覆盖的薄膜由细晶粒(~70 nm)和大颗粒(100-250 nm)组成。X射线光电子能谱分析表明试样表面的钛以TiO2形式存在,检测不到镍,钙磷元素以磷酸钙存在。处理试样检测到锐钛矿TiO2和羟基磷灰石的X射线衍射峰。在无钙Hank’s平衡盐液中的动电位极化实验表明,处理试样的耐蚀性比抛光试样大大提高。本文提供的一步法生物活性表面改性方法易于操作,处理温度低,腐蚀性低,可用于生物医用多孔镍钛合金的表面改性。     

碳／碳复合材料表面声电沉积磷灰石动力学研究

采用声电沉积技术，在碳／碳复合材料表面制备了生物活性磷酸钙涂层。扫描电镜、X射线衍射、红外反射以及X射线能谱分析表明所制涂层呈现网状结构，其由钙磷比为1．64、含碳酸根的羟基磷灰石组成。根据扫描电镜观察，描述了磷灰石的形成过程。羟基磷灰石的沉积过程可简化为两步——钙磷离子向碳／碳阴极表面运动和羟基磷灰石在碳／碳表面生长。基于此描述，导出了羟基磷灰石沉积动力学公式，并且发现，沉积过程受扩散控制，扩散活化能是30．3kJ／mol．     

Effects of Post-weld Heat Treatment on Microstructure,Mechanical Properties and the Role of Weld Reinforcement in 2219 Aluminum Alloy TIG-Welded Joints

In as-welded state, each region of 2219 aluminum alloy TIG-welded joint shows diff erent microstructure and microhardness due to the diff erent welding heat cycles and the resulting evolution of second phases. After the post-weld heat treatment, both the amount and the size of the eutectic structure or θ phases decreased. Correspondingly, both the Cu content in α-Al matrix and the microhardness increased to a similar level in each region of the joint, and the tensile strength of the entire joint was greatly improved. Post-weld heat treatment played the role of solid solution strengthening and aging strengthening. After the post-weld heat treatment, the weld performance became similar to other regions, but weld reinforcements lost their reinforcing eff ect on the weld and their existence was more of an adverse eff ect. The joint without weld reinforcements after the post-weld heat treatment had the optimal tensile properties, and the specimens randomly crack in the weld zone.     

The First Phase of the SRIF Industrialized Base in ＂West Area＂ Has Been Put into Operation

After nearly two years＇ tense construction, the first phase of industrialized base of Shenyang Research Institute of Foundry （SRIF）, located at the Tiexi Casting and Forging Industrial Park in the west of Tiexi District, has now been completed and formally put into operation.     

Theoretical Analysis for the Motion and Temperature of Melt Droplets in Spray Degassing Process

The motion of melt droplets in spray degassing process was analyzed theoretically. The height of the treatment tank in spray degassing process could be determined by the results of theoretical calculation of motion of melt droplets. To know whether the melt droplets would solidify during spraying process, the balance temperature of melt droplets was also theoretically analyzed. Then proof experiments for theoretical results about temperature of melt droplets were carried. In comparison, the experimental results were nearly similar to the calculation results.     

Growth Kinetics of Single Inclusion Particle in Molten Melts

On the basis of the single-particle framework, a new theory on inclusion growth in metallurgical melts is developed to study the kinetics of inclusion growth on account of reaction and collision. The studies show that the early growth of inclusion depends on reaction growth and Brawnian motion collision, and where the former is decisive, the late growth depends on turbulence collision and Stokes＇ collision, and where the former is dominant; collision growth is very quick during the smelting process, lessened in the refining process, but nearly negligible in the continuous casting process.     

An Easy Way to Quantify the Adhesion Energy of Nanostructured Cu/X(X=Cr,Ta,Mo,Nb,Zr) Multilayer Films Adherent to Polyimide Substrates

An approach based on film buckling under simple uniaxial tensile testing was utilized in this paper to quantitatively estimate the interfacial energy of the nanostructured multilayer films(NMFs) adherent to flexible substrates. The interfacial energies of polyimide-supported NMFs are determined to be *5.0 J/m2 for Cu/Cr, *4.1 J/m2 for Cu/Ta,*2.8 J/m2 for Cu/Mo, *1.1 J/m2 for Cu/Nb, and *1.2 J/m2 for Cu/Zr NMFs. Furthermore, a linear relationship between the adhesion energy and the interfacial shear strength is clearly demonstrated for the Cu-based NMFs, which is highly indicative of the applicability and reliability of the modified models.     

High-Speed Friction Stir Welding of SiC_p/Al–Mg–Si–Cu Composite

A 17 vol% SiCp/Al–Mg–Si–Cu composite plate with a thickness of 3 mm was successfully friction stir welded(FSWed) at a very high welding speed of 2000 mm/min for the first time. Microstructural observation indicated that the coarsening of the precipitates was greatly inhibited in the heat-affected zone of the FSW joint at high welding speed, due to the significantly reduced peak temperature and duration at high temperature. Therefore, prominent enhancement of the hardness was achieved at the lowest hardness zone of the FSW joint at this high welding speed, which was similar to that of the nugget zone. Furthermore, the ultimate tensile strength of the joint was as high as 369 MPa, which was much higher than that obtained at low welding speed of 100 mm/min(298 MPa). This study provides an effective method to weld aluminum matrix composite with superior quality and high welding efficiency.     

新型的治疗阿尔茨海默氏症药物(1-二甲基磷酰基-2,2,2-三氯)-乙基-1-醇烟酸醋对体外神经细胞的作用

目的: 观察本实验室合成的一种治疗阿尔茨海默氏症(AD)的药物(1-二甲基磷酰基-2, 2, 2 -三氯)-乙基^-1-醇烟酸醋(NMF),对体外培养的皮层神经细胞活性的影响以及对海人藻酸(KA)所致的神经损伤的保护作用。方法: 采用体外培养皮层神经元的方法,解剖分离 15 d胚胎小鼠皮层神经细胞, 接种于 96孔板,48 h 后加药并培养 72 h,以 MIT 法 观察 NMF 对小鼠皮层神经细胞活性的影响;同时将接种于 24 孔板的细胞预先给予 NMF,d 3 时加或不加KA处理后,以台盼蓝染色鉴别并计数死、活细胞,可得出细胞的存活率。结果: NMF 明显促进胎鼠皮层神经元活性,其中 NMF1、0. 1、10nmol·L^-1促进神经元活性增殖率分别高达 34.7%、37.4%、36. 7%, NMF 明显促进正常胎鼠皮层神经元存活卒,与对照组比较,10nmol·L^-1 NMF 对皮层神经元的存活率分别提高 39.3%、73.5%。 NMF能显著 对抗 KA 所致的神经元损伤,与 KA 损伤组相比, NMF0.1、10、10nmol·L^-1对损伤皮层神经元的保护率分别为 77.30%、80.10%、84.15%。结论: NMF 明 显促进胎鼠皮层神经元的洁性、提高正常皮层神经元,的存活卒,并能有效地保护KA所致的神经元损伤,提示 NMF 是一种很有潜力的治疗 AD 的药物。     

A STUDY OF TEMPERATURE-DEPENDENT VALENCE BOND STRUCTURE OF TITANIUM

On the basis of energy and shape method for the determination of the valence bond (VB) structures of crystal, the valence bond structure of titanium is redetermined at room temperature and calculated in the whole temperature range of 0-1943K. The outer shell electronic distribution of Ti is e_c~(2.9907) · (s_c~(0.4980) d_c~(2.4927)) ef1.0093 in crystal. The temperature dependences of the VB structures of hcp and bcc phases are the same. The VB structures of hcp and bcc phases monotonically increase or decrease with the increase in temperature, but show discontinuous changes at the phase-transformation temperature 1155K.     

Structural Optimization of Electromagnetic Swirling Flow in Nozzle of Slab Continuous Casting

During the slab continuous casting process, the flow field of molten steel in the mold plays a decisive role in the quality of the slab. In this paper, electromagnetic swirling flow in nozzle technology is proposed to control the flow field in mold.This technology can drive molten steel to rotate inside the submerged entry nozzle by electromagnetic force, thereby controlling the flow field. This research shows that it can reduce the impact of molten steel on the bottom of nozzle and partly reduce the negative pressure at the upper part of nozzle outlet which is even eliminated by optimizing the structure and angle of nozzle. The area of heat flux of the mold wall becomes larger, and the crest value of heat flux gets lower than that without swirling in nozzle and any nozzle optimization. The meniscus fluctuates smoothly, and the flow velocity at the top surface is within a reasonable range. The temperature field distribution in the mold is uniform which was beneficial to the growth of equiaxed crystal and decreased element segregation.     

Effect of Rare Earth Doping on Impedance,Modulus and Conductivity Properties of Multiferroic Composites:0.5(BiLa_xFe_(1-x)O_3)–0.5(PbTiO_3)

The Lanthanum-doped bismuth ferrite–lead titanate compositions of 0.5(Bi LaxFe1-xO3)–0.5(Pb Ti O3)(x = 0.05,0.10,0.15,0.20)(BLxF1-x-PT) were prepared by mixed oxide method.Structural characterization was performed by X-ray diffraction and shows a tetragonal structure at room temperature.The lattice parameter c/a ratio decreases with increasing of La(x = 0.05–0.20) concentration of the composites.The effect of charge carrier/ion hopping mechanism,conductivity,relaxation process and impedance parameters was studied using an impedance analyzer in a wide frequency range(102–106Hz) at different temperatures.The nature of Nyquist plot confirms the presence of bulk effects only,and non-Debye type of relaxation processes occurs in the composites.The electrical modulus exhibits an important role of the hopping mechanism in the electrical transport process of the materials.The ac conductivity and dc conductivity of the materials were studied,and the activation energy found to be 0.81,0.77,0.76 and 0.74 e V for all compositions of x = 0.05–0.20 at different temperatures(200–300 °C).