Surface properties and biocompatibility of acid-etched titanium

The purpose of this study was to evaluate the effects of acid-etched titanium on the biological responses of osteoblast-like MC3T3-E1 cells. Four types of treatments (polishing, sandblasting, concentrated H2SO4 etching, and concentrated H2SO4 etching with vacuum firing) were carried out on the surfaces of commercially pure titanium (cpTi) disks. MC3T3-E1 cells were then cultured on the treated cpTi surfaces. Through surface roughness measurement and SEM analysis, it was found that the acid-etched surfaces showed higher roughness values than the sandblasted ones. Scanning electron microscope analysis showed that the cells on the disks treated with acid-etching and acid-etching with vacuum firing spread as well as the sandblasted ones. There were no significant differences in cell proliferation and collagen production on cpTi among the four different surface treatments. Based on the results of this study, it was concluded that etching with concentrated sulfuric acid was a simple and effective way to roughen the surface of titanium without compromising its biocompatibility.     

Acid etching of titanium for bonding with veneering composite resins

Commercially pure titanium (cpTi) was etched using three concentrated acids: 18% HCl, 43% H3PO4, and 48% H2SO4. The bond strengths between five types of veneering composite resin and eight cpTi treatments (involving combinations of sandblasting, acid etching in 48% H2SO4, and vacuum firing) were determined before and after 10,000 and 20,000 thermal cycles. There were no significant differences in the bond strength of resin to cpTi after etching in 48% H2SO4 at 90 degrees C for 15 minutes, at 60 degrees C for 15, 30, or 60 minutes, and after sandblasting with and without vacuum firing (p > 0.05); moreover, these treatments yielded the highest values. As for vacuum firing, it had no significant effect on resin bond strength to cpTi before or after 10,000 and 20,000 thermal cycles. We therefore concluded that acid etching in concentrated H2SO4 is a simple and effective surface modification method of titanium for bonding to veneering composite resins.     

兔骨髓基质细胞在不同纯钛表面的早期粘附

目的：比较兔骨髓基质细胞在3种不同化学蚀刻纯钛表面的早期粘附情况。方法：分别用HNO3、热H2SO4／H2O2、热H2SO4／HCl处理纯钛片30min。采用扫描电子显微镜、X射线光电子能谱对试样表面形貌及成分进行分析。取兔骨髓基质细胞接种于钛片表面，培养30、60、120min，采用荧光显微镜和四唑盐比色法对细胞粘附进行观察和分析。结果：HNO3组表面形貌光滑，平整；H2SO4／HCl、H2SO4／H2O2组表面粗糙。3组钛片表面的主要成分为钛、氧和碳。细胞在H2SO4／HCl、HNO3组表面粘附伸展良好，在H2SO4／H2O2组表面伸展较差。结论：细胞在H2SO4／H2O2组表面的粘附不及H2SO4／HCl组，甚至不如HNO3组。     

纯钛种植体表面多孔结构的制备与分析

目的：利用喷砂、双重酸蚀和H2O2法构建粗化、改性种植体表面并对其形貌进行分析。方法：商业纯钛片经磨平、喷砂、清洗后分为6组,分别采用不同方法进行处理,从而得到不同的表面形貌。用扫描电镜（FSEM）观察表面形貌,能谱分析表面元素组成,X射线衍射（XRD）分析表面成分。结果：钛片表面经喷砂、超声清洗后．表面嵌有大量的喷砂颗粒,经低浓度HF／HNO3酸蚀后,仍有部分残留;同时,钛片表面形成大量纳米级孔洞。经高浓度HF／HNO3酸蚀后完全去除喷砂颗粒,钛片表面形成大量微米级孔洞。钛片再经HCl和H2SO4混合液酸蚀后,可以完全去除喷砂颗粒,同时得到多级孔洞结构。H2O2法处理,可使粗化表面得到锐钛矿晶相结构的TiO2层。结论：通过改变HF／HNO3浓度,可以得到不同孔径的孔洞;双重酸蚀处理,可以完全去除喷砂颗粒,并得到多级孔洞结构。H2O2法可将粗化表面的非晶态TiO2结晶转变为锐钛矿晶相结构。     

激光酸蚀联合纳米管与喷砂酸蚀粗化种植体的对比研究

目的研究激光酸蚀联合纳米管与喷砂酸蚀（SLA）的钛种植体表面粗化处理方法,分析比较不同表面理化特性的差异。方法自制表面光滑钛种植体分两组：一组依次采用LT-G20W光纤激光打标机轰击、18％盐酸和49％硫酸的混合物酸蚀、阳极氧化法制纳米管3个工序联合粗化光滑面的纯钛种植体表面;另一组依次采用喷砂（Al2O3颗粒）、18％盐酸和49％硫酸的混合物酸蚀法2个工序粗化钛金属表面。通过扫描电镜（SEM）观察两种植体表面形貌：应用表面电子探针（EPMA）对种植体表面的元素组成和元素化合状态进行分析：应用3D表面形貌仪在白光共聚焦扫描模式下对种植体表面粗糙度进行测试分析。并对两者的表面形貌、化学组分、表面粗糙度等指标进行比较分析。结果成功制备两种粗化的钛种植体表面。激光酸蚀联合纳米管表面的粗糙度大于SLA表面的粗糙度。激光酸蚀联合纳米管组：轮廓算术平方差Ra=（8．19±0．09）μm,轮廓各点高度均方根Rq=（10．64±2．10）μm,轮廓最大峰高度Rt=（43．42±6．18）μm;SLA组：Ra=（2．09±0．13）μm,Rq=（2．70±0．18）μm,Rt=（15．36±0．50）μm,两者统计学差异具有统计学意义（tRa=-16．709,tRq=-9．206,tRu=-10．178,P〈0．05）：激光酸蚀联合纳米管组的表面清洁;SLA组表面可见尖锐的边缘,散在的一些A12O3颗粒。结论采用激光酸蚀联合纳米管与SLA的钛表面处理方法均可以获得粗糙表面,前者较后者更为清洁规则．粗糙度更高,可控性更好。     

Response of rat bone marrow cells to commercially pure titanium submitted to different surface treatments

OBJECTIVES: Alterations in the commercially pure titanium (cpTi) surface may be undertaken to improve its biological properties. The aim of this study is to investigate the biocompatibility of cpTi submitted to different surface treatments. METHODS: The cpTi surfaces were prepared so that machined and blasted surfaces, either acid etched or not, were compared using rat bone marrow cells cultured to differentiated into osteoblast. For attachment evaluation, cells were cultured for 4 and 24h. Cell morphology was evaluated after 3 days. After 7, 14, and 21 days cell proliferation was evaluated. Total protein content and alkaline phosphatase (ALP) activity were evaluated after 14 and 21 days. For bone-like nodule formation, cells were cultured for 21 days. Data were compared by analysis of variance. RESULTS: Cell attachment, cell morphology, cell proliferation, and ALP activity were not affected by surface treatments. Total protein content was reduced by blasted and acid etched surface. Bone-like nodule formation was significantly reduced by blasted, acid etched, and a combination of both blasted and acid etched surfaces. CONCLUSIONS: Based on these results, it can be suggested that cpTi surfaces that were submitted only to machining treatment favor the final event of osteoblastic differentiation of the rat bone marrow cells, evidenced by increased bone-like nodule formation.     

In vitro preliminary study of osteoblast response to surface roughness of titanium discs and topical application of melatonin

Objectives: To observe human osteoblast behavior cultured in vitro on titanium discs (Ti) in relation to surface roughness and melatonin application. Study Design: Human osteoblasts (MG-63) were cultured on 60 Ti6Al4V discs divided into three groups: Group I: discs treated with dual acid etching; Group II dual acid etching and blasting with calcium phosphate particles; Group III (control) machined discs. Surface roughness and topography of the discs were examined with scanning electron microscope (SEM) and confocal laser scanning electron microscope( CLSM). Osteoblast adhesion, proliferation and cell morphology were determined by means of fluorescence microscopy with Image-Pro Plus software and SEM. Results: Group II presented the roughest discs, while the least rough were Group III. Cell adhesion was greatest in Group II. The addition of melatonin improved cell proliferation. Conclusions: 1. Surface treatments (dual acid etching, calcium phosphate impaction) increase surface roughness in comparison with machined titanium. 2. Greater surface roughness tends to favor cell adhesion after 24-hour cell culture. 3. The addition of melatonin tends to favor osteoblast proliferation. Key words:Osteoblasts, titanium, roughness, melatonin, dental implants, osseointegration.     

酸蚀及粘结剂对聚醚醚酮粘结强度的影响

目的:研究经过不同表面处理后的聚醚醚酮与饰面树脂间粘结强度的变化。实验方法:将聚醚醚酮样品随机分为4组进行表面处理:98%浓硫酸酸蚀组,粘结剂处理组,98%浓硫酸酸蚀+粘结剂处理组和未处理对照组。各处理组再随机分为2个亚组粘结饰面树脂:GC Gradia组,Ceramage组。每个亚组随机选出一半样品用37 ℃蒸馏水浸泡24 h,其余样品冷热循环10000次后,测量样品的剪切粘结强度,SPSS软件统计分析数据;体视显微镜检查样品断裂界面,统计粘结失败类型。结果:各表面处理实验组与空白对照组之间均存在统计学差异,经硫酸酸蚀处理的聚醚醚酮与Ceramage硬质树脂的粘结强度最高(19.38±5.34) MPa,且与其他实验组有统计学差异(P＜0.05)。在冷热循环后,除粘结Gradia Direct树脂的浓硫酸+粘结剂处理组外,其余实验组的粘结强度明显降低(P＜0.05)。结论:浓硫酸酸蚀与自酸蚀粘结剂均能提高聚醚醚酮与饰面树脂的粘结强度,Gradia Direct饰面树脂与经浓硫酸+粘结剂处理的聚醚醚酮表面可形成稳定的粘结作用。     

纤维连接蛋白与钙磷复合涂层的初步研究(一)复合涂层的制备

目的 探讨商用纯钛表面纤维连结蛋白与钙磷复合涂层的可行性。方法 采用纤维连结蛋白，钙磷共沉积的方法，对商用纯钛表面进行复合涂层的表面改性，结果 扫描电镜显示，单纯钙磷涂层和复合涂层的纯钛表面均见有晶体形成，但晶体形态存在一定的差异；EDX显示晶体的主要成份为钙磷，Ca/P=1.50。结论 本研究表明通过纤维连结蛋白与钙磷复合涂层对纯钛的表面改性具有可行性。     

铸造纯钛抛光方法的研究

目的 探讨不同抛光方法对纯钛铸件表面的抛光效果。方法 常规制作铸造纯钛试件35个,随机分为7组,除1个对照组外,其余6组分别用不同方法进行抛光处理。观察试件表面形貌,并测定表面粗糙度（Ra值）,计算抛光前后的减重率（Wt%）及单位面积损失的厚度（H）,比较各种抛光方法的抛光效果。结果 用氧化铝和氧化铬抛光膏抛光纯钛铸件可取得良好效果;铸件酸洗后进行电解抛光,表面粗糙度有一定改善。结论 氧化铝和氧化铬抛光膏可用于铸钛表面的机械抛光,电解抛光有一定效果,但电解工艺仍需改进。     

不同表面处理方法对CAD/CAM氧化锆种植体表面显微形貌的影响研究

目的：：研究采用不同表面处理方法对CAD/CAM氧化锆种植体表面显微形貌特征及粗糙度的影响。方法：通过CAD/CAM技术加工氧化锆圆盘与一段式氧化锆种植体( Y-TZP, WIELAND),根据表面处理方式分为终烧结表面、喷砂表面及喷砂加热酸蚀处理表面;标准对照组选用BEGO钛种植体表面。各组圆盘试件及种植体用扫描电子显微镜及Keyence 3D激光显微形貌测量显微镜进行表面显微形貌观察与测量。采用单因素方差分析比较各组统计学差异。结果：各组CAD/CAM氧化锆试件表面显微形貌观察显示,喷砂后表面出现边缘锐利的凹坑及沟槽;喷砂加热酸蚀处理后,氧化锆表面可见纳米级的微小孔隙及沟纹。氧化锆种植体粗糙度测量结果显示：终烧结组的表面粗糙度值(Ra=0.69μm)显著低于其他3组(P<0.001),喷砂组Ra值(Ra=1.30μm)显著低于喷砂加热酸蚀组(Ra=1.49μm)及BEGO钛种植体组(Ra=1.57μm)(P<0.01),而喷砂加热酸蚀组与BEGO钛种植体组则无显著差异(P=0.196)。结论：CAD/CAM氧化锆试件终烧结后喷砂或喷砂加热酸蚀处理均可获得较为理想的表面粗糙度,热酸蚀处理能够改变氧化锆表面的纳米级微观结构。     

Effects of implant microtopography on osteoblast cell attachment

PURPOSE: The overall aim of this project was to study osteoblast cell attachment on titanium surfaces with varying surface roughness. MATERIALS AND METHODS: Commercially pure titanium surfaces were prepared by polishing through 600-grit sandpaper, sandblasting, or sandblasting followed by acid etching to produce surfaces of varying roughness, as determined by scanning electron microscopy and atomic force microscopy. In vitro cell attachment of MC3T3-E1 osteoblasts was performed on the prepared surfaces in both serum-containing and serum-free media conditions. RESULTS: Cell attachment was directly related to the average surface roughness, with the highest levels of cell attachment observed on sandblasted and sandblasted-acidetched surfaces. Similar patterns of cell attachment were observed when serum-free conditions were employed. CONCLUSIONS: Combined surface analytical and cell/molecular biological techniques are powerful tools to broaden our understanding of biological events occurring at the implant-tissue interface. Data acquired from these in vitro techniques provide a translational application to in vivo clinical models leading to the next generation of dental implants.     

两种表面处理方法对改良型聚醚醚酮弯曲强度的影响

目的 通过三点弯曲试验,评价表面喷砂及酸蚀处理对改良型聚醚醚酮（PEEK）强度的影响。方法 制作15 mm×2 mm×1 mm的改良型PEEK（BioHPP）试件48个,随机分为A~H组,A、B、C组喷砂压力均为0.2 MPa,喷砂粒度依次为120、50、250 μm;D组则在0.7 MPa压力下120 μm粒径喷砂;E、F、G组分别采用98%浓硫酸酸蚀60、120、300 s,H组（对照组）不进行任何表面处理。处理完成后,从各组中随机抽取一个试件用扫描电镜（SEM）观察其表面形貌,其余试件则进行三点弯曲强度测试。采用SPSS 22.0软件对实验数据进行统计分析,检验其差异是否具有统计学意义。结果 SEM观察结果表明,处理后试件表面形貌发生了变化,呈现出不同程度的裂隙、凹坑或孔洞。通过三点弯曲测试发现,与对照组相比,经喷砂或浓硫酸处理后试件强度均有所下降（P<0.05）。相同压力下,A、B、C组间弯曲强度差异无统计学意义（P>0.05）;相同粒度下,D组试件的强度低于A组（P<0.05）。浓硫酸酸蚀处理后,E、F、G组试件的弯曲强度差异无统计学意义（P>0.05）。结论 表面喷砂或浓硫酸酸蚀均会使BioHPP的弯曲强度显著下降,其强度会随着喷砂的压力增加而明显下降,但不会随着喷砂粒径大小及酸蚀时长变化而发生显著的改变。     

两种表面处理方法对改良型聚醚醚酮弯曲强度的影响

目的 通过三点弯曲试验,评价表面喷砂及酸蚀处理对改良型聚醚醚酮（PEEK）强度的影响。方法 制作15 mm×2 mm×1 mm的改良型PEEK（BioHPP）试件48个,随机分为A~H组,A、B、C组喷砂压力均为0.2 MPa,喷砂粒度依次为120、50、250 μm;D组则在0.7 MPa压力下120 μm粒径喷砂;E、F、G组分别采用98%浓硫酸酸蚀60、120、300 s,H组（对照组）不进行任何表面处理。处理完成后,从各组中随机抽取一个试件用扫描电镜（SEM）观察其表面形貌,其余试件则进行三点弯曲强度测试。采用SPSS 22.0软件对实验数据进行统计分析,检验其差异是否具有统计学意义。结果 SEM观察结果表明,处理后试件表面形貌发生了变化,呈现出不同程度的裂隙、凹坑或孔洞。通过三点弯曲测试发现,与对照组相比,经喷砂或浓硫酸处理后试件强度均有所下降（P<0.05）。相同压力下,A、B、C组间弯曲强度差异无统计学意义（P>0.05）;相同粒度下,D组试件的强度低于A组（P<0.05）。浓硫酸酸蚀处理后,E、F、G组试件的弯曲强度差异无统计学意义（P>0.05）。结论 表面喷砂或浓硫酸酸蚀均会使BioHPP的弯曲强度显著下降,其强度会随着喷砂的压力增加而明显下降,但不会随着喷砂粒径大小及酸蚀时长变化而发生显著的改变。     

纯钛种植体表面纳米含氟磷灰石涂层的构建和表征

目的：在纯钛表面构建纳米含氟磷灰石涂层并进行性能表征。方法：采用溶胶凝胶法在纯钛表面构建纳米级含氟磷灰石涂层，用X线衍射、X线光电子能谱、扫描电镜和溶解度测试表征其晶体结构、化学组成、表面形貌、厚度以及化学稳定性；用体外成骨细胞培养评价其生物活性。结果：该涂层具有良好的晶体结构和均匀的纳米级表面形貌，化学稳定性理想。体外成骨细胞培养显示其具有良好的生物活性。结论：本实验构建的涂层具有良好的性能和应用前景。     

Enhanced biological responses of a hydroxyapatite/TiO2 hybrid structure when surface electric charge is controlled using radiofrequency sputtering

We investigated whether surface roughness and control of surface electric charge of a hydroxyapatite (HA)/titanium oxide (TiO2) hybrid coating could enhance biological responses associated with bone formation. After acid etching, a titanium surface was modified with HA and TiO2 by the dual sputtering deposition technique using radiofrequency sputtering. These surfaces were analyzed for surface roughness and surface electric charge intensity. Rat bone marrow-derived osteoblast-like cells were cultured on HA/TiO2 hybrid surfaces with different electric charges. The attachment and spreading behavior of these cells were significantly increased on the hybrid surface (p<0.05). In vivo experiment, the strength of bone-titanium implant integration with a hybrid surface was 3 times that of a control (p<0.05). The dual sputtering deposition technique created a HA/TiO2 hybrid structure. Our results show that the surface electric charge on a titanium surface is an important factor for enhancing biological responses.     

铸钛的不同表面处理对钛-聚合瓷结合强度影响的实验研究

目的 研究铸钛的不同表面处理方法对钛-聚合瓷结合强度的影响。方法 将24个铸钛试件随机分为光 滑组、粗糙组、酸蚀光滑组和酸蚀粗糙组,每组6个。根据分组不同分别采用不同的表面处理方式,粗糙组进行喷 砂处理,酸蚀光滑组进行酸蚀处理,酸蚀粗糙组喷砂后进行酸蚀,光滑组表面不做处理。表面处理后的钛试件与 聚合瓷制备成钛-聚合瓷试件,测试其剪切结合强度,并在扫描电镜下观察钛表面形貌和剪切试验后钛与聚合瓷断 裂面的形貌。结果 光滑组、粗糙组、酸蚀光滑组和酸蚀粗糙组的剪切结合强度分别为（3.08±0.45）、（6.05±0.74）、（6.27±0.80）、（10.16±0.82）MPa。粗糙组、酸蚀光滑组和酸蚀粗糙组的剪切结合强度高于光滑组（P<0.01）,其中酸 蚀粗糙组的剪切结合强度最高,粗糙组和酸蚀光滑组间的剪切结合强度无统计学差异（P>0.05）。各组的钛表面形
貌和剪切试验后钛与聚合瓷断裂面的形貌均有一定的差异。结论 钛表面酸蚀处理和喷砂处理可提高钛-聚合瓷的剪切结合强度,喷砂后酸蚀处理是一种有效地提高钛-聚合瓷剪切结合强度的表面处理方法。     

粗化处理对新型骨植入钛合金的生物相容性影响

目的研究国内新研制的骨植入钛合金TZS进行喷砂并酸蚀处理对成骨细胞生物学行为的影响。方法采用SD大鼠体外原代培养方法培养成骨细胞,并将细胞分别接种于新型钛合金（ 光滑表面）及表面处理的材料表面,建立体外共同培养模型。采用MTT比色法检测第3天成骨细胞的增殖率,扫描电镜（ SEM）观察细胞形态学变化,培养第5天进行细胞碱性磷酸酶功能活性检测。结果喷砂与酸蚀处理组表面的成骨细胞,在3 d时的细胞增殖率与光滑组比较有统计学差异（ P<0.05）;5 d时的处理组碱性磷酸酶活性检测值与光滑组比较无统计学差异（ P>0.05）;SEM观察成骨细胞在喷砂与酸蚀组表面具有典型形态特征,伸展良好,具有丰富的板状、丝状伪足,优于光滑组。结论喷砂并酸蚀处理的新型钛合金在体外实验表现为不同程度的促进成骨细胞增殖及功能活性表达。     

Bone contact around acid-etched implants: a histological and histomorphometrical evaluation of two human-retrieved implants

The surface characteristics of dental implants play an important role in their clinical success. One of the most important surface characteristics of implants is their surface topography or roughness. Many techniques for preparing dental implant surfaces are in clinical use: turning, plasma spraying, coating, abrasive blasting, acid etching, and electropolishing. The Osseotite surface is prepared by a process of thermal dual etching with hydrochloric and sulfuric acid, which results in a clean, highly detailed surface texture devoid of entrapped foreign material and impurities. This seems to enhance fibrin attachment to the implant surface during the clotting process. The authors retrieved 2 Osseotite implants after 6 months to repair damage to the inferior alveolar nerve. Histologically, both implants appeared to be surrounded by newly formed bone. No gaps or fibrous tissues were present at the interface. The mean bone-implant contact percentage was 61.3% (+/- 3.8%).