多孔磷酸三钙-羟基磷灰石对人牙龈成纤维细胞黏附行为的影响

目的　研究多孔磷酸三钙 羟基磷灰石 (tricalcium phosphate hydroxyapatite ,TCP HA)复合材料对人牙龈成纤维细胞黏附行为的影响。方法　应用离子束辅助沉积法在纯钛试件表面制备多孔TCP HA复合涂层材料和羟基磷灰石 (hydroxyapatite,HA)涂层材料 ,定量对比人牙龈成纤维细胞在涂层和未涂层材料表面初期黏附、增殖、细胞铺展面积、细胞外基质和黏着斑形成的情况。结果　TCP HA和HA涂层材料表面黏附的细胞数、细胞铺展面积高于纯钛未涂层组 ,差异有显著性(P <0 0 5 ) ,黏着斑的形成早于未涂层组 ;TCP HA表面黏附的细胞数和Ⅰ型胶原的形成都高于纯钛未涂层组和HA涂层组。在培养 2 4h后TCP HA组表面黏附细胞数为 198 1± 2 7 7,Ⅰ型胶原形成的荧光强度为 15 4 10± 31 5 6 ,同纯钛组表面的细胞数 ( 12 5 1± 2 9 9)和Ⅰ型胶原荧光强度( 132 6 3± 35 2 6 )相比 ,差异有显著性 (P <0 0 5 )。结论　与纯钛未涂层和HA涂层材料相比 ,多孔TCP HA复合涂层材料更有利于人牙龈成纤维细胞的初期黏附 ,具有更良好的生物相容性     

预阳极氧化和水热沉积复合法制备纯钛表面羟基磷灰石涂层

目的：研究阻止金属离子向体液中游离和改善纯钛的生物相容性。方法：采用预阳极氧化及水热沉积复合法对纯钛试件进行生物改性。用X射线衍射(XRD)及SEM和SEM附带的能谱(EOS)对涂层的组成和结构进行分析。结果：预氧化后，纯钛表面生成了致密的纯锐钛矿型二氧化钛薄膜，它可诱导骨样羟基磷灰石的形成，促进细胞的黏附和生长，还能阻止内层金属离子的溶出。结论：水热沉积后在致密的二氧化钛薄膜上生成了结晶状态完好、均匀多孔的骨样羟基磷灰石涂层，可提高纯钛植入体的生物相容性和生物活性。     

钛种植体SLA表面HA涂层对骨髓源成骨细胞生物学特性的影响

目的:探讨表面喷砂和酸蚀(SLA)处理后羟基磷灰石(HA)涂层的钛种植体(HA-SLA-Ti),对骨髓源成骨细胞(MOOBs)生物学特性的影响。方法:应用离子束辅助沉积技术(IBAD)在SLA处理的钛种植体(SLA-Ti)表面制备HA涂层,将MOOBs分别接种于HA-SLA-Ti和SLA-Ti表面,观察其生长情况,并对2组MOOBs增殖指数、碱性磷酸酶活性、骨钙素含量以及骨桥蛋白基因(opn)mRNA相对表达量进行比较。结果:MOOBs在HA-SLA-Ti表面生长良好,其细胞增殖指数、碱性磷酸酶活性以及骨钙素含量明显高于SLA-Ti组;且opnmRNA相对表达量是SLA-Ti组的3.25倍。结论:应用IBAD技术在钛种植体SLA表面制备HA涂层,可明显促进MOOBs的增殖及其成骨表型的表达,是一种有应用前景的种植体表面处理方法。     

羟基磷灰石涂层种植体—骨界面的生物力学研究

本项研究选用氧化铝作为种植体基体．在850℃和1050℃下分别在其表面烧结羟基磷灰石(简称HA)．制成HA1和HA2涂层种植体．以纯钛作对照。狗股骨穿皮质种植1、3、6个月后取材，行顶出试验．并对测试后的破坏断面行扫描电镜观察。结果发现：两种HA涂层种植体具有较好的生物力学性能．能在种植早期加速新骨形成、钙化，达到较高的界面结合强度；涂层种植体在顶出试验后．断裂发生在涂层材料内，而纯钛则发生在种植体—骨组织界面；涂层种植体的界面力学性能和烧结温度有关．HA2涂层种植体在各种植程期的界面结合强度均高于HA1涂层种植体。     

纯钛表面快速沉积羟基磷灰石涂层的实验研究

目的探讨在纯钛种植体表面快速沉积羟基磷灰石涂层的新方法。方法20片纯钛片均分为A、B两组。A组用H2SO54与HCI混合液酸蚀；B组用H2SO4与HCI混合液酸蚀，再用5mol／L NaOH溶液60℃处理24h后，600℃热处理1h。然后两组试件同时置于仿生液A液和B液中各1天。场发射扫描电子显微镜观察分析涂层的形貌。结果两组试件表面均可沉积致密的羟基磷灰石涂层，涂层由1—3μm的小球组成。X射线衍射分析证实其为碳酸化的羟基磷灰石。结论在纯钛表面可以快速沉积碳酸化的羟基磷灰石。     

生物活性玻璃-钛芯牙种植体临床十年效果观察

种植体经历了纯钛、涂层、表面处理等一系列过程 ,人们努力寻找既有生物活性又有生物相容性的材料 ,为此设想了许多方法 ,包括在 Ti或 Ti合金基体上用等离子喷涂羟基磷灰石涂层 ,但由于羟基磷灰石材料的热分解温度低及形成的涂层太软 ,又成为技术上及临床上的难题。生物玻璃涂层材料具有良好的生物活性和生物相容性 ,较高的机械强度及与 Ti合金相近的热膨胀系数 ,而为人们所关注的。生物活性玻璃 -钛芯牙种植体 (BAG- Ti I)是上海市硅酸盐研究所与我科共同研制的一种复合种植体 [1～ 4 ] ,用等离子体射流喷涂技术制备的生物玻璃涂层 ,具…     

微弧氧化钛基种植材料对成骨细胞早期黏附的影响

目的：检测纯钛种植体材料微弧氧化（microarc oxidation，MAO）表面改性后的成骨细胞生物相容性，探讨微弧氧化技术在钛种植体表面改性中的价值。方法：在纯钛种植体材料表面用微弧氧化法制备羟基磷灰石陶瓷薄膜，将MAO改性钛种植体材料作为实验组Ⅰ，将纯钛表面阳极氧化改性处理的种植体材料作为实验组Ⅱ．并设立对照组Ⅰ（纯钛种植体材料）和对照组Ⅱ（即细胞直接生长在培养板上），分别进行扫描电镜（SEM）、能谱分析（EDS）、X射线衍射图谱分析（XRD）等检测，比较成骨细胞的黏附水平，对数据采用SPSS11．0统计软件包进行单因素方差分析。结果：MAO改性后生成粗糙、多孔的陶瓷薄膜层，与处理前电解液成分相比，钙磷比无显著改变。MAO改性钛组黏附的细胞密度显著高于其他组（P〈0．01），而对照组Ⅰ、Ⅱ的细胞密度无显著差异（P〉0．05）。结论：与阳极氧化表面改性材料相比，该钛基微弧氧化薄膜层能够显著促进成骨细胞的附着，具有良好的细胞相容性。     

牙种植体纳米含氟羟基磷灰石涂层材料制备实验研究

目的 探讨用溶胶-凝胶法制备出的纳米含氟羟基磷灰石（nFHA）材料用于纯钛表面涂覆的理论依据。方法 本实验于2010年1-5月在中南大学粉末冶金研究院完成。采用溶胶-凝胶法制备nFHA和羟基磷灰石（HA）材料,通过X线衍射（XRD）、透射电镜（TEM）表征其物相组成及颗粒大小,扫描电镜（SEM）观察涂层在纯钛表面形貌。结果 XRD检测结果显示,运用溶胶-凝胶法可制备出nFHA材料,氟离子进入HA晶体中,以nFHA固溶体形式存在。TEM显示,nFHA晶体呈短棒状,粒径大部分在100 nm以下,符合纳米级别。SEM显示,热处理后的nFHA涂层,为多孔形貌,相互形成穿通结构,颗粒均匀分布,无明显裂纹。结论 （1） 采用溶胶-凝胶法可制备出nFHA涂层材料;（2） nFHA较HA在钛基表面涂层可形成更佳的孔隙结构。     

复合玻璃梯度涂层种植体的实验研究

目的:研究亚音速火焰喷涂方法制备的三种表面复合梯度涂层种植体的骨结合界面情况.方法:在钛合金(Ti-6Al-4V)表面形成三组涂层种植体,8Ti2G组:表面喷涂80％钛(Ti)粉+20％玻璃(G)粉(质量比=8∶2);HA组:喷涂80％钛(Ti)粉+20％玻璃(G)粉作为底层,在其上喷涂100％羟基磷灰石(HA)粉;8H2B组:喷涂80％钛(Ti)粉+20％玻璃(G)粉作为底层,在其上喷涂80％羟基磷灰石(HA)粉+20％生物活性玻璃(BG)粉.选择8只3月龄的杂种犬,拔除双侧下颌前磨牙,待拔牙创愈合后,将三组种植体分别植入双侧无牙区的下颌骨内,术后4周和12周分别处死犬4只.采用大体观察、组织学等方法观察种植体与骨的结合情况.结果:X射线显示在所有种植体周围无明显阴影,8Ti2G底釉涂层具有良好的生物相容性,8Ti2G/HA和8Ti2G/8H2B涂层种植体与骨组织均形成骨性结合,同一观察期,界面骨结合率比较有差异.结论:8Ti2G/8H2B种植体达到生物活性梯度变化,孔隙结构梯度变化.该研究为生物复合涂层的应用提供理论依据.     

生物陶瓷涂层牙种植体的稳定性研究进展

种植牙的表面处理有利于早期负荷，种植体表面工程包括表面形态设计、粗糙度控制、氮化处理、钝化处理等，其中较重要的研究方向之一就是表面涂层技术。羟基磷灰石(hydroxyapatite，HA)是一种生物相容性和活性很好的生物陶瓷材料，植入骨组织中的lu可以通过离子交换形式和骨组织结合成一个整体。因此，在钛种植牙表面形成HA涂层，所制成的牙种植体不需要像钛种植牙那样设计机械固位形，     

钛表面载银HA-TCP溶胶凝胶涂层的制备及其抗菌性的研究

目的：用溶胶凝胶法在钛表面制备载银HA-TCP涂层，并观察其抗菌性能。方法：采用溶胶凝胶法将Ag^＋导入HA-TCP溶胶，并在钛表面涂层。用X射线衍射（XRD）和傅立叶变换红外光谱（FTIR）对涂层结构进行表征分析，用X射线能谱（EDS）分析涂层表面元素构成和分布，用扫描电镜（SEM）观察涂层表面形貌。观察涂层对牙龈卟啉单胞菌P.g、具核梭杆菌F.n、伴放线放线杆菌A-a的生长抑制作用，并计算抗菌率。结果：载银HA-TCP溶胶在钛表面涂层均匀，由大量的亚微米及细微的介孔组成。XRD检测出HA、钛、锐钛矿和β-TCP的衍射峰；FTIR分析涂层含有OH^-．PO4^3-及CO3^2-的特征吸收峰。EDS检测发现钙、磷、钛、碳、氧和银在涂层表面的分布。与对照组比较，载银HA-TCP涂层对牙龈卟啉单胞菌P.g、具核梭杆菌F.n、伴放线放线杆菌A.a具有明显的抗菌效果。结论：本试验在钛表面涂覆载银HA-TCP溶胶，使钛植入体获得了具有生物活性及抗菌性的仿生涂层。     

Characterization of hydroxyapatite films obtained by pulsed-laser deposition on Ti and Ti-6AL-4v substrates.

OBJECTIVES: Pulsed-laser deposition (PLD) is a development process to obtain hydroxyapatite (HA) thin film. It is an alternative to hydroxyapatite deposition techniques usually employed to cover orthopaedic or dental titanium implant surfaces. The aim of this study is to find out the characteristic ratio for Ca/P (1.66) deposit on titanium implant with the PLD process. METHODS: In a preliminary study, the coating parameters of pure and highly crystalline HA on Ti or Ti-6Al-4V substrates were verified by analysing the deposit by Rutherford backscattering spectroscopy (RBS). Ablation parameters to reach a stoichiometric hydroxyapatite composition (ideal Ca/P atomic ratio) and to control the growth of crystalline phases were: 575 degrees C for the substrate temperature, 0.4 mbar H2O vapour pressure in the ablation chamber, the target substrate distance was 40 mm and the deposition time was 120 min. In a second part, the film properties were analysed by means of XRD, SEM, AFM. The coating adhesion of the HA to the substrate was determined with a micro scratch tester. RESULTS: The analysed HA thin films showed a perfect crystallized and textured deposit. Sample observation and surface quality analysis demonstrated a surface roughness and adhesion of the films to the substrates compatible with biological applications. SIGNIFICANCE: These results suggest that pulsed-laser deposition is a suitable technique to obtain crystalline and adherent hydroxyapatite films on Ti or Ti-6Al-4V substrates. The quality of the HA deposit with the PLD process could be an interesting option for coating dental implant.     

表面经喷砂和酸蚀及羟基磷灰石涂层的TA2纯钛种植体对富血小板血浆体外骨诱导能力的影响

目的以表面经喷砂和酸蚀(SLA)及羟基磷灰石(HA)涂层双重处理的TA2纯钛种植体(HA/SLA-TA2)为支架材料,探讨其对富血小板血浆(PRP)体外诱导骨髓基质细胞(BMSCs)向成骨细胞分化能力的影响。方法PRP分别作用于常规培养的BMSCs(对照组)和与HA/SLA-TA2联合培养的BMSCs(实验组),通过扫描电镜观察BMSCs在HA/SLA-TA2表面的生长情况,并对两组细胞的增殖指数、碱性磷酸酶活性、骨钙素含量进行比较。结果实验组细胞生长状态良好,具有成骨细胞特点,其细胞增殖指数于联合培养第5天起明显高于对照组(P<0.05),碱性磷酸酶活性以及骨钙素含量分别于联合培养第9、13天起明显高于对照组(P<0.01)。结论HA/SLA-TA2是种植体表面骨组织工程较理想的支架材料,BMSCs与HA/SLA-TA2联合培养后,可增强PRP诱导其向成骨细胞分化的能力。     

锶磷灰石涂层钛种植体骨结合的动物实验

目的 观察微弧氧化锶磷灰石(strontium-substituted hydroxyapatite,Sr-HA)涂层钛种植体的成骨活性,探讨锶元素掺入羟基磷灰石(hydroxyapatite,HA)涂层后对骨结合的影响.方法 分别对实验组(Sr-HA涂层种植体)和对照组(HA涂层种植体)的表面形貌进行扫描电镜观察,并采用X线衍射仪分析膜层相组成.将两组种植体各12枚植入新西兰兔双侧股骨髁下外侧、胫骨结节处,术后对实验动物进行多荧光序列标记,饲养4周和12周取材,采用组织学观察、种植-骨界面线扫描分析评价涂层的骨结合能力.结果 种植体微弧氧化膜层均呈现多级孔洞状结构;X射线衍射分析显示,锶元素的掺入引起HA的衍射峰向小角度方向偏移,晶格间距增大,稳定性下降;多荧光序列标记显示,Sr-HA涂层早期即表现出成骨活性,实验组骨矿化沉积率[(4.75±0.46)μm/d]显著高于对照组[(3.21±0.44)μm/d];组织染色及能谱分析显示,骨种植界面上有生物类骨磷灰石层形成,12周时该磷灰石层转化为成熟的骨组织并与涂层形成紧密的骨结合.结论 锶元素的掺入可提高Sr-HA涂层的生物学活性,加速其表面生物类骨磷灰石层的形成,增强膜层的成骨能力,促进膜层与骨组织的结合.     

In vitro corrosion behavior of bioceramic, metallic, and bioceramic-metallic coated stainless steel dental implants.

OBJECTIVES: The most common metals and alloys used in dentistry may be exposed to a process of corrosion in vivo that make them cytotoxic. The biocompatibility of dental alloys is primarily related to their corrosion behavior. The aim of this work was to evaluate the corrosion behavior and thus the biocompatibility of the uncoated and coated stainless steels and compare the effect of type of coatings on corrosion behavior. METHODS: Three types of coatings, hydroxyapatite (HA), titanium (Ti), and a double-layer HA/Ti on AISI 316L stainless steel were made. HA coating was produced using plasma-spraying technique and Ti coating was made using physical vapor deposition process. In order to perform a novel double-layer composite coating, a top layer of HA was plasma-sprayed over a physical vapor deposited Ti layer on AISI 316L stainless steel. Structural characterization techniques including XRD, SEM and EDX were used to investigate the microstructure, morphology and crystallinity of the coatings. Electrochemical potentiodynamic tests were performed in physiological solutions in order to determine and compare the corrosion behavior of the coated and uncoated specimens as an indication of biocompatibility. RESULTS: Double-layer HA/Ti coating on AISI 316L SS had a positive effect on improvement of corrosion behavior. The decrease in corrosion current densities was significant for these coated specimens and was much lower than the values obtained for uncoated and single HA coated specimens. Ti coating on AISI 316L SS also has a beneficial effect on corrosion behavior. The results were compared with the results of corrosion behavior of HA coated commercially pure titanium (cpTi) and uncoated cpTi. SIGNIFICANCE: These results demonstrated that the double-layer HA/Ti coated 316L SS can be used as an endodontic implant and two goals including improvement of corrosion resistance and bone osteointegration can be obtained simultaneously.     

Two-dimensional and 3-dimensional analysis of bone/dental implant interfaces with the use of focused ion beam and electron microscopy.

PURPOSE: To assess the usefulness of a dual-beam focused ion beam (FIB) and scanning electron microscope (SEM) instrument and FIB-based transmission electron microscopy (TEM) specimen preparation techniques to characterize bone/dental implant interfaces. MATERIALS AND METHODS: The FIB was used to site specifically polished cross-sections for direct FIB, SEM, and TEM imaging of bone osseointegration into a Nobel Biocare TiUnite failed dental implant (Nobel Biocare, Yorba Linda, CA). RESULTS: Bone was observed to grow into the porous structure of the coating, yielding direct evidence of a mechanical locking mechanism of the bone/implant interface. Multiple SEM images obtained from sequential FIB cross-sections were reconstructed into 3-dimensional tomograms that showed partial and full bone growth into the porous structure of the TiUnite coating. Sections thinned by FIB techniques were observed by transmission electron microscope (TEM) and related methods. Conventional bright field TEM showed that the coating, which was more than 2 microm thick, consisted of a nanocrystalline and porous structure. High-resolution TEM (HRTEM) showed the presence within the bone of hydroxyapatite crystallites that measured approximately 7 nm. TEM images showed that the bone does not form an intimate and homogenous interface with the implant coating in all regions. X-ray energy dispersive spectrometer (XEDS) line scans that used scanning TEM (STEM) methods showed interdiffusion of Ti, P, and Ca between the bone and the coating where intimate bone/coating contact was observed, suggesting that chemical bonding also exists within this interface. CONCLUSIONS: FIB methods for SEM and TEM were used to characterize bone/implant surfaces.     

The effects of ion beam-assisted deposition of hydroxyapatite on the grit-blasted surface of endosseous implants in rabbit tibiae

PURPOSE: This study was undertaken to evaluate ion beam-assisted deposition (IBAD) of hydroxyapatite (HA) on the grit-blasted surface of endosseous dental implants 6 weeks postplacement. MATERIALS AND METHODS: A total of 40 implants was placed in the tibiae of 10 New Zealand white rabbits. Twenty implants were grit-blasted only and the other 20 were grit-blasted and coated with HA by the IBAD method. After 6 weeks of healing, the rabbits were sacrificed and removal torque tests, histomorphometry, and morphometric analysis of microtomographic images were performed. RESULTS: The HA-coated group showed significantly higher removal torque, bone-to-implant contact, and bone volume than the other group. DISCUSSION AND CONCLUSION: In a previous study, the authors suggested that HA coating deposited on a machined surface by the IBAD method showed results comparable to or more favorable than the results obtained with a blasted surface. This study indicated that the HA coating produced by the IBAD method was also very effective on the aluminum oxide-blasted surface, as demonstrated by the early formation of osseointegration. Morphometric analysis by microtomography showed some promise in measuring the osseointegration rate. (More than 50 references.)     

Human histologic and histomorphometric analyses of hydroxyapatite-coated implants after 10 years of function: a case report

PURPOSE: No consensus exists on the long-term performance of hydroxyapatite (HA) coatings on dental implants. The aim of this study was to evaluate the long-term stability of the HA coating in a human autopsy specimen. MATERIALS AND METHODS: Two mandibular HA-coated implants were retrieved postmortem from a woman after 10 years of functional loading with an implant/tooth-supported fixed partial denture. After ground sectioning, the specimens were histomorphometrically analyzed. RESULTS: Direct bone-implant contact was found at 78.48% of the implant surface. HA coating disappearance had occurred in a few areas (22.75%), but bone was in direct apposition to the titanium surface. Bone volume measured 27.66%, and expected bone-implant contact was 37.55%. No inflammatory reaction was seen in the supracrestal soft tissues or the bone compartment. DISCUSSION: Most of the HA coating was maintained on the implants, and areas lacking HA were directly apposed by bone. This observation suggests that the underlying titanium surface should have a macro-texture to promote the adaptation of bone to the titanium surface in case of HA disappearance, as well as to decrease failure at the HA-titanium interface. CONCLUSIONS: In a patient in whom prosthetic treatment was appropriately performed and proper plaque control was maintained, the HA coating was not damaged and contributed to the success of the implant over 10 years of clinical functioning.