碱热处理联合紫外光照后钛体外活性的研究

目的研究碱热处理加紫外光照后钛的微观结构变化及在模拟体液中诱导羟基磷灰石沉积的能力。方法将纯钛分组处理:SLA组:喷砂酸蚀;AAH组:SLA组加碱热处理;UV组:AAH组加紫外线辐照处理。测试各组理化性质,对其进行模拟体液浸泡实验。采用扫描电镜及X射线衍射仪观察分析沉积物。结果碱热处理加紫外光照的钛具有多级孔洞的微观粗糙结构,同时引入钙、钠元素,并有最佳的表面润湿性;模拟体液浸泡后,试样表面矿化物质量最多,沉积速度最快,X射线衍射仪分析沉积物为羟基磷灰石。结论碱热处理加紫外光照后纯钛种植体具有良好的体外生物活性。     

纯钛表面酸碱处理及生物矿化的初步研究

目的:探讨不同的酸、碱处理条件下纯钛表面生物矿化沉积磷灰石层的差异。方法:对商用纯钛分别采用磨光处理、酸处理、酸碱处理或酸碱及热处理,然后放入模拟体液(SBF)中矿化处理7天;采用SEM观察试样表面的形貌,采用XRD分析试样表面沉积层的相组成。结果:经酸碱处理后纯钛形成微粗糙表面,随着碱液浓度的升高和采用热处理,试样表面的粗糙度增加且更均匀;经碱液处理的试样矿化后其表面出现磷灰石沉积层;而未处理组未发现磷灰石沉积层;XRD图谱分析发现矿化表面沉积物为HCA,钙磷比为1.37。结论:碱液处理有利于磷灰石层的形成,而改变碱液浓度和是否采用热处理对磷灰石沉积能力有影响。     

喷砂酸蚀混合碱热处理后纯钛表面生物活性的研究

目的研究喷砂酸蚀混合碱热处理后的纯钛表面其生物活性。方法将经抛光(M)、喷砂酸蚀(SLA)、喷砂酸蚀混合碱热(AHH)处理后的纯钛试件分为3组。扫描电子显微镜(SEM)及能谱分析(EDS)对3组表面结构和表面化学元素及其含量进行分析;荧光显微镜下观察成纤维细胞在样品表面的粘附及铺展情况;并将各组试件浸泡模拟体液(SBF)中观察羟基磷灰石沉积情况。结果纯钛表面微纳复合结构中,微米孔直径3~5μm,纳米孔直径100~200 nm,同时在试件表面引入钙钠元素。成纤维细胞粘附:DAPI染色后细胞核呈蓝色荧光,罗丹明B染细胞骨架红色,SLA组、AHH组细胞铺展较M组好,呈空间铺展;且AHH组表面细胞数量明显多于其他两组。第1周时,AHH组表面沉积磷灰石明显可见,而未在M、SLA组检测到羟基磷灰石。结论喷砂酸蚀混合碱处理后的纯钛表面,表面活性好,有助于促进成纤维细胞早期粘附及其在空间上的铺展,同时又促进羟基磷灰石的沉积,进而体现了良好的生物性能,可以为种植体表面处理方法提供参考。     

釉基质蛋白对化学处理钛表面磷灰石生成的影响

目的:研究釉基质蛋白对双重热酸蚀及碱热处理纯钛表面仿生矿化沉积磷灰石层的影响.方法:提取猪未萌恒牙胚表面EMPs,用SDS-PAGE电泳进行验证.纯钛片经抛光清洗,分别进行双重热酸蚀和碱热处理,放入含EMPs(150 μg/mL)的改良模拟体液(m-SBF)中浸泡7d,对照组为不含EMPs的m-SBF.扫描电镜观察试件表面形貌,X射线能谱,X射线衍射及傅里叶红外光谱等分析其元素成分及晶相结构.结果:酸蚀组经仿生矿化.对照组试件表面无沉积物生成,实验组加入EMPs,钛片表面有一定量的沉积物生成,能谱分析显示主要由Ca、P、O和C等元素组成.碱热处理组经仿生矿化,对照组与实验组试件表面均有沉积层形成,但后者有较多直径约为300～600nm的孔隙生成,元素组成主要为Ca、P、O和C,X射线衍射及傅里叶红外光谱分析显示沉积物为碳羟基磷灰石.结论:碱热处理纯钛表面有利于磷灰石层的形成,加入EMPs能促进磷灰石层的形成并改变其形貌.     

阳极氧化处理后的新型钛合金体外诱导实验及对成骨细胞早期附着的影响

目的：研究新型医用钛合金Ti-24Nb-4Zr-7．9Sn（TNZS）经过阳极氧化（AD）技术处理后体外诱导活性及对人成骨样MG63细胞早期附着的影响。方法：采用阳极氧化处理TNZS合金，对其进行模拟体液（SBF）浸泡实验，分析其表面元素成分及相结构的变化；并将人成骨样MG63细胞接种于Ti6Al4V、TNZS、AD—TNZS表面，观察细胞的早期附着及形态学变化。结果：AD—TNZS在SBF中浸泡6d后，材料表面有羟基磷灰石形成。在MG63成骨样细胞接种60、120min时，人成骨样MG63细胞在AD—TNZS表面的附着率均明显高于Ti6Al4V和TNZS表面附着率（P〈0．05），并表现出良好的形态。结论：阳极氧化后的新型医用钛合金在模拟体液中可诱导羟基磷灰石形成；对成骨细胞的早期附着有一定的促进作用。     

四种钛种植体表面在模拟体液中诱导磷灰石沉积的研究

目的：检测四种钛植入体表面在细胞培养液中诱导生成磷灰石的能力及形貌特征。方法：直径15mm钝钛片打磨至600目，进行以下处理：（1）单纯光滑钛片；（2）钛片粗化处理，采用喷砂＋酸蚀法；（3）光滑钛片＋碱热处理；（4）粗化钛片＋碱热处理。以上四种表面之钛片分别浸入DMEM＋10％FCS细胞培养液中，分别于第6、12、18、24天取出一组钛片，扫描电镜观察表面形貌，能谱分析仪分析表面元素组成比例。对24d时钛片用X射线衍射仪分析表面组分。结果：在各时间点的光滑表面及单纯粗化表面均未见磷灰石形成，而在经碱热处理的实验组中，第6天时在碱热处理形成的网孔中可见磷灰石的形核的形成。粗化表面＋碱热处理组形核为纳米级的针状结晶物，随时间增长，形核逐渐长大成密集球状物；光滑＋碱热处理组表面为颗粒状形核。粗化表面＋碱热处理组较光滑钛片＋碱热处理组Ca、P沉积速度快，对第24天时经碱热处理试样XRD分析表明，表面沉积物主要为羟基磷灰石。结论：在含血清的细胞培养液中浸泡后，经碱热处理的钛表面显示了明显的诱导磷灰石沉积能力。表面沉积物成分为羟基磷灰石，粗化＋碱热处理表面沉积的磷灰石为纳米级针状结构且沉积速度较快。     

钛合金种植体（Ti6Al4V）表面接枝丙烯酸-衣康酸共聚物增强生物矿化的研究

目的通过在钛种植体（Ti6Al4V）表面接枝丙烯酸-农康酸共聚物以促进钛合金种植体表面羟基磷灰石的沉积。方法用异丙醇钛（TIP0）作偶联剂,在经氢氧化钠处理的钛种植体表面接枝丙烯酸-衣康酸共聚物,然后,将其浸入SBF溶液中一周进行生物矿化。运用扫描电子显做镜、X-射线衍射仪、X-射线能谱仪对表面矿化物的形貌、结构和组成进行表征和分析。结果接枝丙烯酸-衣康酸共聚物的钛种植体表面经SBF溶液浸泡后,其表面形成连续的针状矿化物,X-射线衍射仪、X-射线能谱仪证实其结构为羟基磷灰石。结论钛表面接枝丙烯酸-衣康酸共聚物后,能加快羟基磷灰石在表面的沉积,并调整其晶体形貌。     

粗化、改性种植体表面的构建及形貌分析

目的：利用喷砂、酸蚀和碱热处理技术构建粗化、改性植入人体表面并对其形貌进行分析。方法：直径15mm的TA2纯钛棒，加工成厚1mm的圆片，晶相砂纸逐渐打磨至600目。40目金刚砂喷砂、草酸酸蚀、5mol/LnaOH溶液处理24h，600℃加热，构建成粗化、改性钛表面，以SEM观察表面形貌，能谱分析表面元素组成。结果：光滑钛表面仅见规则划痕，粗化表面形成多级孔洞状结构，能谱分析表面元素为100％Ti。经碱热处理，可见钛表面在孔洞的基础上形成了大量的微网状结构，能谱分析发现大量Na^ 及O元素的存在。经体外模拟体液浸泡实验，发现经碱热处理的钛表面有大量的钙结节沉积。结论：经粗化加碱热处理的钛表面上形成了多级孔基础的网状TiO2水凝胶层，该层具有诱导钙质沉积的能力。     

釉基质蛋白对碱热处理纯钛表面磷灰石生成的影响

目的：研究釉基质蛋（EMPs）对碱热处理纯钛表面磷灰石涂层生成的影响。方法：采用乙酸法提取猪EMPs。纯钛片碱热处理后,在含不同浓度EMPs（0、50、100、150、200μg／mL）的模拟体液中浸泡1周、2周后取出。扫描电镜观察表面形貌,x射线衍射分析晶相结构。结果：各组试件表面均有类骨磷灰石（CHA）生成。EMPs浓度为50、100μg／mL时,钙磷涂层的沉积受到抑制;EMPs浓度为150、200μg／mL时,钙磷涂层的沉积增强,且涂层粗糙度增加,有直径约300～600nm孔隙生成,晶体呈（002）方向择优取向生长。结论：EMPs对碱热处理纯钛表面磷灰石生成的影响与浓度密切相关,较高浓度EMPs可促进钛表面生成CHA,并改变磷灰石晶体的形态与生长方向。     

表面形貌及碱热处理对纯钛表面在DMEM培养液中诱导磷灰石沉积的影响

目的：检测表面形貌及碱热处理钛植入表面对钛表面在细胞培养液中诱导生成磷灰石的能力。方法：纯钛片打磨至600目，进行以下处理：(1)单纯光滑钛片；(2)钛片粗化处理，采用喷砂 酸蚀法；(3)光滑钛片 碱热处理；(4)粗化钛片 碱热处理。以上4种表面之钛片分别浸入DMEM细胞培养液中，分别于第1、2、3周取出一组钛片，扫描电镜观察表面形貌，EDX分析表面元素组成比例。对第3周时的钛片用X射线衍射仪分析表面组分。结果：第1周末时，在碱热处理形成的网孔中可见磷灰石形核形成。粗化表面 碱热处理组形核为纳米级的针状结晶物，随时间增长，形核逐渐长大成密集球状物，进而形成由球状体组成的面状沉积体；光滑 碱热处理组表面为颗粒状形核。对经碱热处理试样的XRD分析表明，表面沉积物主要为羟基磷灰石。结论：在细胞培养液中浸泡后，经碱热处理的钛表面显示了明显的诱导磷灰石沉积能力。表面沉积物成分为羟基磷灰石，粗化 碱热处理表面沉积的磷灰石为纳米级针状结构。     

一步微弧氧化法处理钛合金的体外生物相容性研究

目的　研究一步微弧氧化法处理钛合金（Ti6Al4V）的体外生物学性能,为下一步临床应用微弧氧化法处理钛合金种植体提供前期理论基础。方法　通过一步微弧氧化法在Ti6Al4V表面生成膜层并表征膜层形态（实验组）,设置对照组为未处理的Ti6Al4V和喷砂酸蚀处理的Ti6Al4V,3组分别与成骨细胞共同培养,测定成骨细胞的增殖、碱性磷酸酶（alkaline phosphatase,ALP）活性以及Ⅰ型胶原蛋白（collagen Ⅰ,COL-Ⅰ）、骨钙素（osteocalcin,OC）的mRNA相对表达情况。结果　微弧氧化处理后Ti6Al4V表面含有大量的陶瓷烧结颗粒,以羟基磷灰石（hydroxyapatite,HA）为主要成分。3组试样的体外实验结果表明,经微弧氧化处理的Ti6Al4V表面的细胞增殖高于其他两组,细胞内的ALP活性、COL-Ⅰ、OC的mRNA相对表达也均高于其他两组。结论　通过微弧氧化法在Ti6Al4V表面生成的陶瓷膜对成骨细胞的增殖分化有促进作用,有良好的生物相容性。     

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??Objective??To study the in vitro biocompatibility of titannium alloy treated with micro-arc oxidation??MAO????in order to provide the theoretical basis for the next application of MAO in the treatment of titanium alloy implants. Methods??The biofilm layer containing hydroxyapatite ??HA?? was formed on the surface of Ti6Al4V by one-step  MAO ??experiment group??. The control groups were the untreated Ti6Al4V and the sandblasted Ti6Al4V. The three groups were co-cultured with osteoblasts to determine the proliferation??alkaline phosphatase ??ALP?? activity and mRNA expression of collagen ?? ??COL-?? and osteocalcin ??OC??. Results??The surface after the treatment was "crater" structure with a large number of HA. The in vitro results of three groups of materials showed that the cell proliferation rate of the Ti6Al4V treated with MAO was higher than that of the other two groups??and the ALP activity and COL-??and OC mRNA expression of cells were higher than those in the other two groups. Conclusion??The biofilm layer formed on the surface of Ti6Al4V by  MAO  has a beneficial effect on the adhesion and proliferation of cells??which promotes the differentiation  and shows good biocompatibility.     

不同电压阳极氧化处理对金属钛表面形态和羟基磷灰石沉积作用的研究

目的探讨不同电压阳极氧化对二氧化钛(TiO2)纳米管形貌的影响及不同形貌TiO2纳米管体外沉积羟基磷灰石能力的差异。方法控制阳极氧化的电压(10V、20V、30V和40V),在钛基底表面制备不同结构TiO2纳米管,利用扫描电子显微镜观察纳米管的形貌。配置模拟体液(SBF),将未经阳极氧化处理的对照组及各试验组试件分别浸泡在SBF中3d、7d和14d,利用扫描电子显微镜观察各试件表面羟基磷灰石沉积状况,通过X射线光电子能谱分析(XPS)对钛试件表面沉积物进行定性、定量分析。结果随着氧化电压的增加,TiO2纳米管管径逐渐增大。随着在SBF中浸泡时间增加,沉积物增多。浸泡相同时间,60nmTiO2纳米管(氧化电压为30V)表面羟基磷灰石沉积物最多。结论阳极氧化的电压可以影响TiO2纳米管的形貌,浸泡模拟体液的时间与钛试件表面形貌均会影响羟基磷灰石的沉积。提示纳米管管径为60nm时,钛试件在模拟体液中促进羟基磷灰石沉积的能力最佳。     

Attachment of Porphyromonas gingivalis to Corroded Commercially Pure Titanium and Titanium‐Aluminum‐Vanadium Alloy

Background: Titanium dental material can become corroded because of electrochemical interaction in the oral environment. The corrosion process may result in surface modification. It was hypothesized that a titanium surface modified by corrosion may enhance the attachment of periodontal pathogens. This study evaluates the effects of corroded titanium surfaces on the attachment of Porphyromonas gingivalis. Methods: Commercially pure titanium (cp‐Ti) and titanium‐aluminum‐vanadium alloy (Ti‐6Al‐4V) disks were used. Disks were anodically polarized in a standard three‐electrode setting in a simulated oral environment with artificial saliva at pH levels of 3.0, 6.5, or 9.0. Non‐corroded disks were used as controls. Surface roughness was measured before and after corrosion. Disks were inoculated with P. gingivalis and incubated anaerobically at 37°C. After 6 hours, the disks with attached P. gingivalis were stained with crystal violet, and attachment was expressed based on dye absorption at optical density of 550 nm. All assays were performed independently three times in triplicate. Data were analyzed by two‐way analysis of variance, the Tukey honestly significant difference test, t test, and Pearson's correlation test (α = 0.05). Results: Both cp‐Ti and Ti‐6Al‐4V alloy‐corroded disks promoted significantly more bacterial attachment (11.02% and 41.78%, respectively; P <0.0001) than did the non‐corroded controls. Significantly more (11.8%) P. gingivalis attached to the cp‐Ti disks than to the Ti‐6Al‐4V alloy disks (P <0.05). No significant difference in P. gingivalis attachment was noted among the corroded groups for both cp‐Ti and Ti‐6Al‐4V alloy (P >0.05). There was no significant correlation between surface roughness and P. gingivalis attachment. Conclusion: A higher degree of corrosion on the titanium surface may promote increased bacterial attachment by oral pathogens.     

Effect of surface roughness and thermal cycling on bond strength of C.P. titanium and Ti-6Al-4V alloy to ceramic

PurposeStudying the effect of surface roughness and thermal cycling on titanium–ceramic bonding.MethodsOne hundred fourteen samples in the form of bar for the C.P. titanium and Ti–6Al–4V alloy were used. They were divided into two groups according to the type of bar. Each group was then subdivided according to the type of surface treatment to three subgroups, control, airborne-particle abrasion and silica coated. Each subgroup was subdivided into two classes according to the type of test (surface roughness and bond strength). Samples used for the bond strength test were veneered. These samples were subdivided into two subclasses according to thermal cycling; whether without thermal cycling or after 6000 thermal cycles.ResultsThe surface roughness test results showed that silica coating recorded the highest surface roughness. Also C.P. titanium gave higher value of surface roughness than Ti–6Al–4V alloy. As regard the bond strength, the airborne-particle abrasion classes and the silica coated classes recorded bond strength values above the acceptable limit of 25 MPa determined in ISO 9693. As regard thermal cycling, the results showed that aging by thermal cycling decreased the metal–ceramic bond strength.ConclusionsThe airborne-particle abrasion and the silica coating are acceptable treatments for titanium–ceramic restorations. Increasing surface roughness of C.P. titanium and Ti–6Al–4V alloy not necessarily results in an increase in their bond strength to ceramics. Aging affects the metal–ceramic bond strength.     

Effect of surface contamination on adhesive bonding of cast pure titanium and Ti-6Al-4V alloy

STATEMENT OF PROBLEM: There is little information regarding bond strengths of resin cements to cast titanium surfaces contaminated by investment material. PURPOSE: This study examined the effect of surface contamination on the shear bond strength of resin cements to cast titanium and Ti-6Al-4V alloy. MATERIAL AND METHODS: Two types of disks were cast from commercially pure titanium (CP-Ti) and Ti-6Al-4V alloy ingots using an argon-arc pressure casting unit and a phosphate-bonded Al2 O3 /LiAlSiO6 investment. After casting, disks were subjected to 3 surface treatments: (1) cast surface sandblasted (50 microm-sized Al2 O3 ) for 30 seconds; (2) metal surface sanded with silicon-carbide paper (600 grit) after grinding the contaminated cast surface (approximately 200 microm in thickness); and (3) metal surface sandblasted for 30 seconds after treatment 2. Surface structures were examined after each treatment with SEM and optical microscopy. Each type of disk was then bonded with 2 types of luting materials. Bonded specimens were subjected to thermocycling for up to 50,000 cycles, and shear bond strengths were determined after 0 (baseline) and 50,000 thermocycles. Results were statistically analyzed with 3-way ANOVA (P <.05). RESULTS: Microscopic observation of cast CP-Ti and Ti-6Al-4V exhibited noticeable structures on the cast surfaces apparently contaminated with investment material. However, there were no statistical differences (P >.05) in the bond strengths of both cements between contaminated (treatment 1) and uncontaminated surfaces (treatment 3) for both metals at baseline and after 50,000 thermocycles. The bond strength of specimens sanded with silicon-carbide paper (treatment 2) deteriorated dramatically after 50,000 thermocycles. CONCLUSIONS: Contamination of the cast metal surfaces by elements of the investment during casting did not affect bond strengths of the luting materials to CP-Ti and Ti-6Al-4V.     

Effect of surface reaction layer on grindability of cast titanium alloys.

OBJECTIVE: The purpose of this study was to investigate the effect of the cast surface reaction layer on the grindability of titanium alloys, including free-machining titanium alloy (DT2F), and to compare the results with the grindability of two dental casting alloys (gold and Co-Cr). METHODS: All titanium specimens (pure Ti, Ti-6Al-4V and DT2F) were cast using a centrifugal casting machine in magnesia-based investment molds. Two specimen sizes were used to cast the titanium metals so that the larger castings would be the same size as the smaller gold and Co-Cr alloy specimens after removal of the surface reaction layer (alpha-case). Grindability was measured as volume loss ground from a specimen for 1 min using a handpiece engine with a SiC abrasive wheel at 0.1 kgf and four circumferential wheel speeds. RESULTS: For the titanium and gold alloys, grindability increased as the rotational speed increased. There was no statistical difference (p>0.05) in grindability for all titanium specimens either with or without the alpha-case. Of the titanium metals tested, Ti-6 Al-4V had the greatest grindability at higher speeds, followed by DT2F and CP Ti. The grindability of the gold alloy was similar to that of Ti-6 Al-4V, whereas the Co-Cr alloy had the lowest grindability. SIGNIFICANCE: The results of this study indicated that the alpha-case did not significantly affect the grindability of the titanium alloys. The free-machining titanium alloy had improved grindability compared to CP Ti.     

Interfacial oxidations of pure titanium and titanium alloys with investments

External oxides of a commercially pure titanium (cpTi), Ti6Al4V alloy, and an experimental beta-type titanium alloy (Ti 53.4 wt%, Nb 29 wt%, Ta 13 wt%, and Zr 4.6 wt%) were characterized after heating to 600, 900, 1150, and 1400 degrees C in contact with three types of investments (alumina cement, magnesia cement, and phosphate-bonded) in air. XRD studies demonstrated that MgO, Li2TiO3 and/or Li2Ti3O7 were formed through reactions with the metal and the constituents in the magnesia cement-investment after heating to 900, 1150, and 1400 degrees C. Except for these conditions, TiO2 (rutile) was only formed on cpTi. For titanium alloys, the other components apart from Ti also formed simple and complex oxides such as Al2O3 and Al2TiO5 on Ti6Al4V, and Zr0.25Ti0.75Nb2O7 on the beta-type titanium alloy. However, no oxides containing V or Ta were formed. These results suggest that the constituents of titanium alloys reacted with the investment oxides and atmospheric oxygen to form external oxides due to the free energy of oxide formation and the concentration of each element on the metal surface.