粉末冶金制备TNZS基生物材料的组成、结构和性能

采用高能球磨48 h制备Ti-24Nb-4Zr-7.9Sn(TNZS)、5%TiO_2/TNZS及5%HA/TNZS混合粉末(质量分数,下同)并进行冷压烧结,研究了3种混合粉末的形貌、物相及冷压烧结后3种TNZS基生物材料的组织、成分、相组成、孔隙特征及弹性模量。高能球磨48 h的3种混合粉末都发生机械合金化;烧结后TNZS相组成为α-Ti和β-Ti,5%TiO_2/TNZS相组成为α-Ti、β-Ti、金红石TiO_2和锐钛矿TiO_2,5%HA/TNZS相组成除α-Ti、β-Ti、HA外,还有Ti_2O、Ca TiO_3、CaO和TixPy新相生成;三者孔隙率分别为2.466%、5.030%和13.027%;三者弹性模量分别为64.00、103.93和119.43 GPa。     

球磨冷压烧结制备TNZS基生物材料的摩擦学性能

采用机械高能球磨、常规模压和真空无压烧结相结合的粉末冶金法制备TNZS、TiO_2/TNZS及HA/TNZS 3种钛基生物医用材料,对比研究3种材料的显微硬度及在不同摩擦条件下的摩擦磨损行为。结果表明:TiO_2/TNZS的显微硬度值最高,TNZS、TiO_2/TNZS及HA/TNZS三者的显微硬度值(HV)分别为5254.3、5512.3和4792.7 MPa;在干摩擦条件下,HA/TNZS具有最好的耐磨损性,三者的摩擦系数分别为0.4323、0.5643和0.4338,平均磨痕宽度分别为0.33、0.26和0.18 mm,磨损机理都以磨粒磨损为主,氧化磨损、粘着磨损为辅;三者在人工体液摩擦条件下的摩擦磨损行为都优于干摩擦下的摩擦磨损行为,HA/TNZS的耐磨性优于其它两者,三者的平均摩擦系数分别为0.3309、0.4301和0.3840,平均磨痕宽度分别为0.27、0.19和0.17 mm,磨损机理都以磨粒磨损为主,伴有轻微氧化磨损和粘着磨损。     

粉末冶金制备TNZS基生物材料的组织与弹性模量

采用高能球磨48h制备Ti-24Nb-4Zr-7.9Sn(TNZS)、5wt.%TiO2/TNZS及5wt.%HA/ TNZS混合粉末并进行冷压烧结,研究了三种混合粉末的形貌、物相以及冷压烧结后三种TNZS基生物材料的组织、成分、相组成、孔隙特征及弹性模量。高能球磨48h的三种混合粉末都发生机械合金化;烧结后TNZS相组成为α-Ti和β-Ti,TiO₂/TNZS相组成为α-Ti、β-Ti、金红石TiO₂和锐钛矿TiO₂,HA/TNZS相组成除α-Ti、β-Ti、HA外,还有Ti₂O、CaTiO₃、CaO和Ti_xP_y新相生成;三者孔隙率分别为2.466%、5.030%和13.027%;三者弹性模量分别为64.00 GPa、103.93 GPa和119.43 GPa。     

纯钛材与大变形纯钛材微弧氧化-水热合成复合陶瓷膜层的细胞相容性研究

采用微弧氧化-水热法分别在纯钛材及大变形纯钛材表面制备了TiO_2/HA复合陶瓷膜层,从细胞毒性实验、细胞增殖实验、细胞黏附实验等方面评价膜层的细胞相容性。结果表明:纯钛材与大变形纯钛材微弧复合陶瓷膜层均无细胞毒性。与纯钛材微弧复合陶瓷膜层相比,大变形纯钛材微弧复合陶瓷膜层表面粗糙度更适宜,结晶形核的HA晶粒的形状及Ca/P比更接近人骨HA,更能有效促进成骨细胞的黏附和铺展,随着培养时间的延长,成骨细胞双层重叠生长结构更为明显。成骨细胞在大变形纯钛材微弧复合陶瓷膜层表面各时间点的吸光度值均更高,细胞相容性更好。     

CVI C／C复合材料及其表面HA涂层成骨细胞体外响应行为对比研究

采用声电化学工艺在CVI C／C复合材料表面制备了HA涂层，分别用SEM，XPS，EDAX和XRD表征了CVI C／C和HA的表面形貌、组成和结构，同时对比了成骨细胞在其表面的粘附、增殖和碱性磷酸酶活性的表达。制备的HA涂层为球状形貌，由纳米片状晶体构成。细胞培养初期，粘附于HA涂层表面的细胞数与CVI C／C表面的细胞数无显著差别，成骨细胞在CVI C／C表面易铺展在孔的边缘，8h后粘附于HA表面的成骨细胞数显著多于CVI C／C表面。HA涂层提高了细胞的增殖能力，成骨细胞碱性磷酸酶在HA涂层表面的表达也优于CVI C／C材料。结果表明，声电化学制备的HA涂层提高了CVI C／C材料的生物活性和生物相容性，可以加速成骨细胞的粘附、增殖、分化和成熟。成骨细胞在材料表面的粘附机制是由多因素综合作用的，材料的表面形貌和生物活性在细胞粘附过程的早期发挥着重要作用。     

锌锶共掺杂TiO_2多孔涂层的抗菌及生物相容性

为改善钛的抗菌性能和生物活性,采用微弧氧化(MAO)技术在纯钛表面制备了锌掺杂TiO_2涂层(M-Zn)、锶掺杂的TiO_2涂层(M-Sr)和锌锶共掺杂TiO_2涂层(M-Zn/Sr)。利用扫描电子显微镜(SEM)和X射线衍射仪(XRD)对制备的涂层的组织结构和成分进行分析;采用平板计数法研究了涂层的抗菌性能;利用细胞荧光染色和甲基噻唑基四唑(MTT)的方法探究了细胞在材料表面的生长状况。结果表明:形成的TiO_2涂层都是典型的多孔结构,主要由金红石和锐钛矿相组成,锌、锶的掺杂对涂层形貌影响不大。M-Zn/Sr涂层中锌、锶的原子数分数分别为7.9%和1.7%。M-Zn及M-Zn/Sr涂层大肠杆菌展现了良好的抗菌性能,抗菌率接近100%。M-Zn、M-Sr和M-Zn/Sr均能促进成骨细胞增殖,M-Zn/Sr涂层具有抗菌和细胞增殖的双重功能。     

微弧氧化法制备钛基HA/CS涂层及其生物学特性

采用微弧氧化法在医用钛表面制备羟基磷灰石（HA）/壳聚糖（CS）涂层。通过扫描电镜（SEM）、X射线衍射（XRD）仪、红外光谱（FTIR）仪分析涂层的形貌和物相,评价HA/CS涂层对成骨细胞的毒性及其在动物体内的生物活性,分析微弧氧化法制备钛基HA/CS涂层的特征及其在骨修复中应用的可能性。结果表明：微弧氧化法可在钛表面生成HA/CS涂层,厚度40±2 mm、粗糙度3.3±0.1 mm、孔隙率(30±2)%,孔隙近圆形、直径几微米到20 mm,结合强度20.5±1.1 MPa;涂层中HA与CS之间没有形成化学键,晶体HA占10%,平均粒径37 nm,非晶体HA占90%;钛基HA/CS涂层材料对成骨细胞增殖具有促进作用,无细胞毒性,在动物体内能够诱导骨小梁形成,具有高的生物活性。微弧氧化法制备的高生物活性钛基HA/CS涂层材料,在骨修复方面具有良好的应用前景     

生物活性多孔钽支架的构建及其初步生物学评价

表面生物活性涂层构建是提升金属内植物骨整合能力的有效途径,本研究利用电化学沉积技术在多孔钽支架表面构建生物活性羟基磷灰石(HA)涂层。通过接触角和比表面积测试发现,HA涂层的构建显著提升了多孔钽表面亲水性,并增加了其比表面积。利用模拟体液浸泡试验评估支架生物活性,发现仅浸泡3天后,多孔钽支架表面就已被类骨磷灰石沉积所覆盖。建成骨细胞培养模型,通过激光共聚焦观察及细胞增殖测试发现,所有支架均具有良好的细胞相容性。并且,细胞共培养5天后,HA涂层化多孔钽支架表面细胞的增殖率分别是未改性材料组和空白对照组的1.1和1.4倍,呈现了更大的促细胞增殖潜力。本研究中所制备的生物活性多孔钽支架具备快速诱导类骨磷灰石沉积能力,能够促进成骨细胞在其表面的贴附和增殖,在骨修复领域具有较大的临床应用前景。     

骨组织工程用镁基泡沫生物材料的制备与其体外降解行为（英文）

采用熔体发泡法制备了一种镁基泡沫生物材料,其中以镁钙合金为基体材料,羟基磷灰石(HA)为增粘剂,碳酸镁(Mg CO3)为发泡剂。对结构均匀的镁基泡沫生物材料进行测试,研究其生物可降解行为。用腐蚀前后的孔结构、浸泡试验和电化学测试对镁基泡沫材料的生物可降解性进行表征。结果表明,在固定时间内随着试样孔隙率的增加,失重率不断增加;相比于添加了HA的样品,不含HA颗粒的样品呈现出更高的质量损失率。同时,Mg基泡沫生物材料的总孔隙率和HA含量均对Mg基泡沫材料的开孔率有重要的影响。在相同时间内,开孔率随试样总孔隙率的增加而增加。在模拟体液(SBF)介质中,含有HA的Mg基泡沫生物材料比不添加HA的试样具有更高的耐腐蚀性。     

用于骨组织工程的镁基泡沫生物材料的制备与体外降解行为

采用熔体发泡法制备了一种镁基泡沫生物材料,其中以镁钙合金为基体材料,羟基磷灰石(HA)为增粘剂,以碳酸镁(MgCO3)为发泡剂。对结构均匀的镁基泡沫生物材料进行测试,研究其生物可降解行为。用腐蚀前后孔结构、浸泡试验和电化学测试对镁基泡沫材料的生物可降解性进行表征。结果表明,在固定时间内随着试样孔隙率的增加,失重率不断增加;相比于添加了羟基磷灰石(HA)的样品,不含HA颗粒地样品呈现出更高质量损失率。同时,Mg基泡沫生物材料的总孔隙率和羟基磷灰石(HA)含量均对Mg基泡沫材料的开孔率有重要的影响。在相同时间内,开孔率随试样总孔隙率的增加而增加。在模拟体液(SBF)介质中,含有羟基磷灰石(HA)的Mg基泡沫生物材料比不添加羟基磷灰石(HA)的试样具有更高的耐腐蚀性。     

Bioactive Ca-P scaffolds used for bone reconstruction

1　INTRODUCTIONSkeletalreconstructionorregenerationisre quiredincasesinvolvinglargedefectscreatedbytu morresection ,trauma ,andskeletalabnormalities .Graftsandflapsofautogenoustissuearetwoofthemostsuccessfulmeansofreconstructionbecausetheyallowthetransplantationofbonecontainingbioactivemolecules,livecells ,andfrequently ,avascularsup plythatallowthetransplanttosurviveandremodeleveninhostileradiatedenvironments .However ,onlyaminimalamountoftissuecanbeharvestedforauto grafts,anditisverydiff…     

低压沉积-微弧氧化制备钛金属HA-TiO2复合膜层

采用低压沉积-微弧氧化法,在钛金属表面直接制备了具有生物活性的HA-TiO2复合膜层,通过XRD和SEM分别分析了膜层的相结构和表面形貌,探讨了沉积参数对膜层中HA含量与表面形貌的影响.结果表明:低压沉积处理是微弧氧化法制备HA-TiO2复合膜层的必要条件;复合膜层主要由金红石型和锐钛矿型TiO2及HA组成,HA以白色...     

电解液成分对纯钛表面微弧氧化膜结构与生物活性的影响

采用微弧氧化处理技术,在纯钛TA2表面制备了含钙磷的多孔复合氧化膜,用SEM、XRD、EPMA等分析了电解液成分对氧化膜形貌、成分、相构成及生物活性的影响。结果表明:纯钛表面微弧氧化后原位生成的含钙磷多孔性复合氧化膜由锐钛矿相TiO2,金红石相TiO2和基体Ti组成;随电解液中钙磷摩尔比(Ca/P)值的增大,表面孔洞数量增多、直径变小,膜中Ca/P值增大,锐钛矿相TiO2减少、金红石相TiO2增多;当电解液中Ca/P=5时得到的氧化膜的Ca/P值为1.528,将该样品经碱液处理后再在快速钙化溶液(FCS)中浸泡2 d后即有羟基磷灰石HA形成,表明其具有良好的生物活性。     

Corrosion behaviour of single and double layer hydroxyapatite coatings on 316L stainless steel by plasma spray

AISI316L stainless steel is extensively used in orthopedic and dental applications. However, this alloy exhibits low integration behaviour when it comes in contact with surrounding bone tissue and implant healing duration can be as much as few months. The aim of this study is the fabrication of biocompatible hydroxyapatite (HA) coatings on stainless steel substrate in order to accelerate the process of osseointegration of implants. The biocompatible single layer of Titania (TiO₂), Hydroxyapatite and bi-layer TiO₂/HA coatings were deposited by atmospheric plasma spray on 316L stainless steel. Coated and uncoated stainless steel specimens were incubated in simulated body fluids and 0.9% NaCl solutions for 1h and 7 days. In vitro electrochemical-corrosion evaluation of coated and uncoated stainless steel specimens have been investigated by Tafel extrapolation and linear polarization methods. Results indicates that corrosion resistance of single layer HA coated stainless steel specimens are superior to single layer TiO₂ and bi-layer HA/TiO₂ coated stainless steel specimens.     

Sol-gel derived HA/TiO2 double coatings on Ti scaffolds for orthopaedic applications

Hydroxyapatite/titania （HA/TiO2） double layers were coated onto Ti scaffolds throughout for orthopaedic applications by sol-gel method. Differential scanning calorimetry （DSC）, thermogravimetric analysis （TG） and X-ray diffractometry （XRD） were used for the characterisation of the phase transformations of the dried gels and coated surface structures. Scanning electron microscope （SEM） equipped with energy dispersive spectrometry （EDS） was used for the observation and evaluation of the morphology and phases of the surface layers and for the assessment of the in vitro tests. The in vitro assessments were performed by soaking the HA/TiO2 double coated samples into the simulated body fluid （SBF） for various periods. The TiO2 layer was coated by a dipping-coating method at a speed of 12 cm/min, followed by a heat treatment at 600 ℃ for 20 min. The HA layer was subsequently dipping-coated on the outer surface at the same speed and then heat-treated at difference temperatures. The results indicat that the HA phase begins to crystallize after a heat treatment at 560 ℃. The crystallinity increases obviously at 760 ℃. SEM observations find no delamination or crack at the interfaces of HA/TiO2 and TiO2/Ti. The HA/TiO2 coated Ti scaffolds displays excellent bone-like apatite forming ability when it is soaked into SBF. Ti scaffolds after HA/TiO2 double coatings can be anticipated as promising implant materials for orthopaedic applications     

甘油磷酸钙浓度对钛合金MAO涂层性能的影响

目的 提高医用钛合金的生物活性。方法 在含葡萄糖酸钙(Ca Glu₂)、葡萄糖酸镁(MgGlu₂)、植酸钠(Na₁₂Phy)和磷酸(H₃PO₄)的基本溶液中,分别添加8、10、12 g/L甘油磷酸钙(Ca-GP),采用MAO方法在Ti-6Al-4V表面制备3种涂层。使用SEM、EDS、XRD、XPS和AFM检测涂层表面形貌、化学成分、物相结构、元素存在状态和表面粗糙度,并测试涂层的接触角、结合强度以及体外生物活性。结果 经过MAO处理后,钛合金表面可成功生长出多孔陶瓷涂层,Ca-GP参与了MAO涂层形成。当Ca-GP的质量浓度为8 g/L时,涂层非常粗糙,Ca和Mg的原子数分数分别为7.56%和1.74%。随着Ca-GP浓度的增加,微孔均匀性变好,表面微裂纹减少,且钙磷原子比(Ca/P)显著提高。在含8、10 g/L的Ca-GP溶液中,制备的涂层以Ti、锐钛矿和金红石型Ti O2组成为主;在12g/L的Ca-GP溶液中生成的涂层,Ca/P原子比可达1.77,含有Ti P     

Cross-sectional analysis on microstructure of plasma-sprayed HA＋TiO2 composite coatings on titanium substrate

The cross-sectional analysis on hydroxyapatite (HA) coating and HA TiO2 composite coating was conducted by using electron probe microanalyser (EPMA). The results reveal that annealing at 650℃ leads to the cracking within the HA coating or along the coating/substrate interface. The ribbon-like regions in HA coating are verified to contain less PO4^4- groups resulted from the high temperature melting of HA particles in plasma flame. From the viewpoint of microstructural observation, it can be concluded that the addition of TiO2 into HA coating can effectively strengthen and toughen the whole coating system with a shift of the well-bonded interface from the THA (top HA) coating/HTBC (HA TiO2 bond coat) interface in the as-sprayed THBC (top HA-HTBC) coating to the HTBC/Ti substrate interface in the heat treated THBC coating. The THA coating bonds well to Ti substrate per-haps via its TiO2 hobnobbing with the Ti oxides formed on the Ti substrate.     

Development of osteoblast colonies on new bioactive coatings

The aging baby boomer population coupled with an increase in life expectancy is leading to a rising number of active elderly persons in occidental countries. As a result, the orthopedic implant industry is facing numerous challenges such as the need to extend implant life, reduce the incidence of revision surgery, and improve implant performance. This paper reports results of an investigation on the bioperformance of newly developed coating-substrate systems. Hydroxyapatite (HA) and nano-titania (nano-TiO₂) coatings were produced on Ti-6Al-4V and fiber reinforced polymer composite substrates. In vitro studies were conducted to determine the capacity of bioactive coatings developed to sustain osteoblast cells (fetal rat calvaria) adherence, growth, and differentiation. As revealed by scanning electron microscopy (SEM) observations and alkaline phosphatase activity, cell adhesion and proliferation demonstrated that HA coatings over a polymer composite are at least as good as HA coatings made over Ti-6Al-4V substrate in terms of osteoblast cell activity. Nano-TiO₂ coatings produced by high-velocity oxyfuel (HVOF) spraying led to different results. For short-term cell culture (4.5 and 24 h), the osteoblasts appeared more flattened when grown on nano-TiO₂ than on HA. The surface cell coverage after seven days of incubation was also more complete on nano-TiO₂ than HA. Preliminary results indicate that osteoblast activity after 15 days of incubation on nano-TiO₂ is equivalent to or greater than that observed on HA. This article was originally published inBuilding on 100 Years of Success, Proceedings of the 2006 International Thermal Spray Conference (Seattle, WA), May 15–18, 2006, B.R. Marple, M.M. Hyland, Y.-Ch. Lau, R.S. Lima, and J. Voyer, Ed., ASM International, Materials Park, OH, 2006.