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。     

Comparative study of chemical and mechanical retentive systems for bonding of indirect composite resin to commercially pure titanium

This study evaluated the effect of chemical and mechanical surface treatments for cast metal alloys on the bond strength of an indirect composite resin (Artglass) to commercially pure titanium (cpTi). Thirty cylindrical metal rods (3 mm diameter x 60 mm long) were cast in grade-1 cpTi and randomly assigned to 6 groups (n=5) according to the received surface treatment: sandblasting; chemical treatment; mechanical treatment - 0.4 mm beads; mechanical treatment - 0.6 mm beads; chemical/mechanical treatment - 0.4 mm; and chemical/mechanical treatment - 0.6 mm beads. Artglass rings (6.0 mm diameter x 2.0 mm thick) were light cured around the cpTi rods, according manufacturer's specifications. The specimens were invested in hard gypsum and their bond strength (in MPa) to the rods was measured at fracture with a universal testing machine at a crosshead speed of 2.0 mm/min and 500 kgf load cell. Data were analyzed statistically by one-way ANOVA and Tukey test (a=5%). The surface treatments differed significantly from each other (p<0.05) regarding the recorded bond strengths. Chemical retention and sandblasting showed statistically similar results to each other (p=0.139) and both had significantly lower bond strengths (p<0.05) than the other treatments. In conclusion, mechanical retention, either associated or not to chemical treatment, provided higher bond strength of the indirect composite resin to cpTi.     

钛种植体表面生物化学改性的研究进展

通过对钛及其合金种植体的表面进行生化改性,以提高种植体表面的生物活性,促进骨整合的发生,使种植体得到早期稳定和长期的临床效果,这是近年来钛及其合金种植体的研究热点之一,本文综述了这一方面的研究现状和发展趋势,着重点在于介绍各种生物活性分子。     

Adhesive bonding of resin cements to cast titanium with adhesive primers

The purpose of this study was to evaluate the effects of adhesive primer applications on the bond strength of resin cements to cast titanium. Four adhesive primers - Metaltite, Metal Primer II, Alloy Primer and Ceramic Primer - and their respective resin cements - Bistite II DC, Link Max, Panavia F 2.0, RelyX Unicem and RelyX ARC - were tested. Cast plates were prepared from titanium ingots (n=6 specimens/cement) and had their surfaces airborne-particle abraded with Al2O3 (50 μ m). Three resin cement cylinders were built on each bonded titanium surface, using a cylindrical translucent tubing mold and were subjected to micro-shear testing. Data were analyzed statistically by two-way ANOVA and Tukey's post-hoc test (α=0.05). The application of Metal Primer II and Ceramic Primer resulted in significant higher bond strength for Link Max and RelyX Unicem resin cements, respectively, than nonuse of adhesive primers. Panavia F 2.0 and RelyX ARC yielded high bond strength means with or without adhesive primers. The use of adhesive primers might increase the bond strength to cast titanium depending on the resin cement used.     

Zirconate coupling agent for bonding resin luting cement to pure zirconium

PURPOSE: To evaluate the shear bond strengths of two dual-cured resin luting cements to pure zirconium and the effect of zirconate coupling agent on the bond strength. METHODS: The two different-shaped pure zirconium specimens (99.9%) were untreated or treated with one of the four primers including zirconate coupler and then cemented together with one of the two dual-cured resin luting cements. Half of the specimens were stored in water at 37 degrees C for 24 hours and the other half thermocycled 20,000 times before shear bond strength testing. RESULTS: Regardless of the resin luting cement and thermocycling, specimens treated with the mixture of zirconate coupler and resin bonding agent showed the highest shear bond strength among the five treatments. Surface treatment with the mixture of zirconate coupler and resin bonding agent showed significantly greater shear bond strength compared with other treatments at 20,000 thermocycles. The application by the mixture of zirconate coupler and resin bonding agent on the pure zirconium metal surface appears to be effective for bonding between zirconium and dual-cured resin luting cements.     

Adhesive bonding of resin composite to various titanium surfaces using different metal conditioners and a surface modification system

Objective

This study evaluated the effect of three metal conditioners on the shear bond strength (SBS) of a prosthetic composite material to cpTi grade I having three surface treatments.

Material and Methods

One hundred sixty eight rivet-shaped specimens (8.0x2.0 mm) were cast and subjected to polishing (P) or sandblasting with either 50 mm (50SB) or 250 mm (250SB) Al₂O₃. The metal conditioners Metal Photo Primer (MPP), Cesead II Opaque Primer (OP), Targis Link (TL), and one surface modification system Siloc (S), were applied to the specimen surfaces, which were covered with four 1-mm thick layers of resin composite. The resin layers were exposed to curing light for 90 s separately. Seven specimens from each experimental group were stored in water at 37ºC for 24 h while the other 7 specimens were subjected to 5,000 thermal cycles consisting of water baths at 4ºC and 60ºC (n=7). All specimens were subjected to SBS test (0.5 mm/min) until failure occurred, and further 28 specimens were analyzed using scanning electron microscope (SEM) and X-ray energy-dispersive spectroscopy (EDS). Data were analyzed by 3-way ANOVA followed by post-hoc Tukey''s test (α=0.05).

Results

On 50SB surfaces, OP groups showed higher SBS means than MPP (P<0.05), while no significant difference was found among OP, S, and TL groups. On 250SB surfaces, OP and TL groups exhibited higher SBS than MPP and S (P<0.05). No significant difference in SBS was found between OP and TL groups nor between MPP and S groups. The use of conditioners on 250SB surfaces resulted in higher SBS means than the use of the same products on 50SB surfaces (P<0.05).

Conclusion

Sandblasting associated with the use of metal conditioners improves SBS of resin composites to cpTi.     

纯钛表面离子注氮后的金瓷结合观察

目的:探讨纯钛表面离子注入氮对钛瓷结合的影响。方法:用线切割法加工28mm×3mm×0.5mm纯钛金属试条20个,分为注氮组(10个试件)和对照组(10个试件),用等离子体基离子注入法(PBII)对注氮组10个试件表面进行注氮处理,随机在两组各取1个试件,用X射线衍射仪(XRD)分析注入层的相结构。再于余下18个试件中份8mm×3mm处熔附钛材专用瓷。用3点弯曲法测试两组试件钛瓷分离时的载荷。结果:注入层内生成了TiN新相,氮化组试件钛瓷分离加载(7.257±0.804)N大于对照组试件分离加载(5.958±0.537)N,经统计学检验,两组样本间有极显著性差异(P<0.01)。结论:纯钛表面经注氮处理后,在注入层内形成了TiN,提高了钛瓷结合强度。     

Effect of 4-MET- and 10-MDP-based primers on resin bonding to titanium

The purpose of this study was to investigate the effect of a 4-MET- and 10-MDP-based primer on the bond strength of two resin cements (SuperBond C&B, Sun Medical; Panavia Fluoro Cement, Kuraray) to titanium (Ti). Ti plates were treated with six experimental primers consisting of, respectively, 10-MDP and 4-MET in concentrations of 0.1, 1 and 10wt%, or were kept untreated (control). The highest tensile bond strength of Panavia Fluoro Cement to Ti was obtained when the Ti surface was pre-treated with 10wt% 10-MDP and was significantly higher than that when a lower concentrated 10-MDP-based primer or any 4-MET-based primer was used. On the contrary, no significant difference in tensile bond strength of SuperBond C&B was found for the untreated and six pre-treated Ti surfaces, although pre-treatment with each 10-MDP-based primer resulted in a higher tensile bond strength as compared to any 4-MET pre-treatment. Altogether, the data obtained strongly suggest that 10-MDP is effective to improve the adhesive performance of resin to titanium.     

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提要：钛和钛合金因具有良好的机械力学性能和生物相容性被广泛用作牙科种植体。种植体植入机体后,与骨的骨性结合是关系到种植体在体内维持时间长短的关键。种植体进入机体后,首先是其表面与组织接触,因此对种植体表面改性是提高种植体与骨的骨性结合的有效方法。本文对目前钛和钛合金表面改性的方法进行简要概述。     

Effects of a metal etchant and two primers on resin bonding durability to titanium

The purpose of this study was to investigate the efficacy of an etchant in titanium bonding. The aqueous etchant consisted of 0, 5, or 10 wt% ammonium hydrogen fluoride (AHF) in combination with 0, 0.03, 0.3, or 3 wt% cupric chloride (CC). The two primers used were a phosphate-methacrylate primer and a thiophosphate-methacrylate primer, and two self-curing resins (Super-Bond C&B and MT) were employed as luting agents. Disk specimens were cast with a commercially pure titanium. The surface was air-abraded with 50 microm alumina, etched for 10 s, rinsed with water, and then air-dried. The primer was applied to the bonding area (5 mm in diameter), and an acrylic rod was bonded to the specimen with the luting agent. Shear bond strengths were evaluated after 24 h of water storage and following 10,000 thermocycles (4 degrees C and 60 degrees C). The post-thermocycling bond strength was significantly increased with each of the two primers compared with the unprimed controls. The etchant containing 5 wt% AHF and 0.3 wt% CC further increased their durability, and microscopic observation revealed that innumerable submicron crystals were created on the etched specimen. The present results suggest that the chemical etching improved the resin bonding durability to titanium in combination with the primer used.     

Surface modification of titanium by etching in concentrated sulfuric acid

OBJECTIVE: The purpose of this study was to characterize the etching behavior of titanium in concentrated sulfuric acid and discuss its application on surface modification of titanium for biological use. METHODS: Commercially pure titanium (cpTi) plate was etched in 48% H2SO4 at RT -90 degrees C for 0.25-8 h. The weight loss was derived from the weight differences before and after etching. The surfaces after etching were characterized by surface roughness, X-ray diffractometry, and scannning electron spectroscopy. The apparent activation energy of the dissolution of cpTi into acid was derived from an Arrhenius plot of the rate of weight loss versus the acid temperature. RESULTS: The surface roughness of cpTi increased with the acid temperature and etching time. The surface roughness was strongly related to the weight loss. The weight loss increased drastically with the acid temperature after an initial period, which shortened with increasing acid temperature. The apparent activation energy for the dissolution of cpTi in H2SO4 was derived as 67.8 kJ/mol. SIGNIFICANCE: This study indicates that etching with concentrated sulfuric acid is an effective way to modify the surface of titanium for biological applications.     

不同表面处理对钛-树脂粘接强度的影响

目的 探讨不同表面处理方式对钛-树脂粘接强度的影响.方法 使用CAD/CAM技术切削出56个底面直径10 mm,厚3 mm的商业Ⅱ级纯钛片,并随机分为7组(n=8).试件表面分别进行喷砂(B组)、涂布硅烷偶联剂(C组)、涂布金属处理剂(D组)、喷砂+硅烷偶联剂(E组)、喷砂+金属处理剂(F组)及喷砂+偶联剂+金属处理剂(G组)处理,而对照组(A组)则不作任何处理.粘接试件使用万能实验机测试剪切粘接强度,结果进行单因素方差分析,并使用Tukey检验进行组间比较(α=0.05).观察断裂模式.结果 与对照组相比,各实验组均表现出较高的粘接强度(P<0.05),其中F组的粘接强度最高,为(20.9±4.3)MPa,与G组之间无统计学差异;F、G组与其他组之间,B、D组与A、C组之间存在统计学差异(P<0.05).断裂模式分析显示,各实验组以界面断裂和混合断裂为主.结论 对纯钛表面进行适当的表面处理,尤其是喷砂与金属处理剂联合处理有利于提升树脂粘接强度.     

不同表面处理对钛-树脂粘接强度的影响

目的 探讨不同表面处理方式对钛-树脂粘接强度的影响.方法 使用CAD/CAM技术切削出56个底面直径10 mm,厚3 mm的商业Ⅱ级纯钛片,并随机分为7组(n=8).试件表面分别进行喷砂(B组)、涂布硅烷偶联剂(C组)、涂布金属处理剂(D组)、喷砂+硅烷偶联剂(E组)、喷砂+金属处理剂(F组)及喷砂+偶联剂+金属处理剂(G组)处理,而对照组(A组)则不作任何处理.粘接试件使用万能实验机测试剪切粘接强度,结果进行单因素方差分析,并使用Tukey检验进行组间比较(α=0.05).观察断裂模式.结果 与对照组相比,各实验组均表现出较高的粘接强度(P<0.05),其中F组的粘接强度最高,为(20.9±4.3)MPa,与G组之间无统计学差异;F、G组与其他组之间,B、D组与A、C组之间存在统计学差异(P<0.05).断裂模式分析显示,各实验组以界面断裂和混合断裂为主.结论 对纯钛表面进行适当的表面处理,尤其是喷砂与金属处理剂联合处理有利于提升树脂粘接强度.     

不同表面处理对钛-树脂粘接强度的影响

目的 探讨不同表面处理方式对钛-树脂粘接强度的影响.方法 使用CAD/CAM技术切削出56个底面直径10 mm,厚3 mm的商业Ⅱ级纯钛片,并随机分为7组(n=8).试件表面分别进行喷砂(B组)、涂布硅烷偶联剂(C组)、涂布金属处理剂(D组)、喷砂+硅烷偶联剂(E组)、喷砂+金属处理剂(F组)及喷砂+偶联剂+金属处理剂(G组)处理,而对照组(A组)则不作任何处理.粘接试件使用万能实验机测试剪切粘接强度,结果进行单因素方差分析,并使用Tukey检验进行组间比较(α=0.05).观察断裂模式.结果 与对照组相比,各实验组均表现出较高的粘接强度(P<0.05),其中F组的粘接强度最高,为(20.9±4.3)MPa,与G组之间无统计学差异;F、G组与其他组之间,B、D组与A、C组之间存在统计学差异(P<0.05).断裂模式分析显示,各实验组以界面断裂和混合断裂为主.结论 对纯钛表面进行适当的表面处理,尤其是喷砂与金属处理剂联合处理有利于提升树脂粘接强度.     

Chemical modification of pure titanium surfaces for oral implants.

A technique that achieves different pure titanium surfaces depending on acid concentration and exposure time is described. It is possible to obtain, with the same chemical treatment, both large pits and small rugosities. This technique may have interesting applications in oral implants.     

纯钛表面含氢类金刚石镀膜的实验研究

目的:观察纯钛表面不同修饰方法对提高表面润湿性及其与热凝树脂结合强度影响的效果。方法:制作5组纯钛试件,分别镀制含氢类金刚石膜、单纯类金刚石膜、TiN膜、阳极氧化膜以及空白对照组。采用接触角测定仪测量试件的接触角并计算表面自由能,使用万能材料试验机测量修饰后的试件与热凝树脂的结合强度。结果:含氢类金刚石膜的表面自由能与树脂的结合强度大于其余各组,TiN的表面自由能与树脂的结合强度最低,阳极氧化组与单纯类金刚石膜的应用,对于提高纯钛表面的润湿性和提高纯钛与热凝树脂结合强度作用不明显。结论:纯钛表面经含氢类金刚石膜修饰后,提高了表面润湿性和戴用舒适性,同时提高了与热凝树脂的结合强度。     

除气和预氧化对纯钛金瓷结合强度的影响

目的研究上瓷前纯钛除气和预氧化对其金瓷结合强度的影响。方法用ISO9693[1]规定的三点弯曲测试法测定A组（除气＋预氧化）、B组（无热处理）试件的金瓷结合强度,用电镜扫描和X线衍射分析金瓷界面。结果金瓷结合强度：A组32.61±5.62Mpa,B组24.19±3.57Mpa,两者之间具有显著性差异（P=0.001）;扫描电镜（SEM）：A组金瓷之间过渡层约65μm,金瓷结合紧密。B组金瓷间过渡层平均约35μm,可见孔洞和裂隙。x射线衍射（EDS）：两组金瓷界面附近的主要元素均为O、Si、Ti、Sn,A组Ti在界面呈单纯扩散曲线。B组Ti在界面呈不规则扩散。结论纯钛除气和预氧化后能获得较高的金瓷结合强度,大于ISO规定的25Mpa,能满足临床要求;无热处理试件金瓷结合强度较低,小于25Mpa,不能满足临床要求。     

精氨酸-甘氨酸-天冬氨酸修饰钛材料表面的研究进展

钛及其合金因良好的生物学性能被广泛应用于口腔医学领域,但钛金属是惰性材料,植入后不能直接和骨形成较好的结合,因此对钛及其合金表面进行生物改性一直是生物材料领域的研究热点.精氨酸-甘氨酸-天冬氨酸(RGD)作为钛材料表面修饰的候选蛋白质,广泛存在于纤连蛋白、玻连蛋白和骨涎腺蛋白等多种细胞外基质蛋白中,可调节细胞与血清及细胞外基质的附着,因此,本文就目前国内外对RGD修饰钛及其合金表面的主要研究进展作一综述.     

钛基底表面处理对钛-树脂粘接强度的影响

目的：探讨不同钛基底表面处理对钛与树脂粘接强度的影响。方法将纯钛试件随机平均分组：光滑组（A组）、酸蚀组（B组）、喷砂组（C组）、喷砂+酸蚀组（D组）、微弧氧化组（E组）、氮化钛涂层组（F组）。根据以上分组,对试件进行相应的表面处理,用粗糙度仪进行钛表面粗糙度测量,后与Cemerage冠桥树脂结合,扫描电子显微镜（SEM）观察试件表面形貌,能谱分析仪（EDS）对表面元素进行分析,万能试验机检测试件与Cemerage冠桥树脂的粘接强度。结果各组的粗糙度分别为A组（0.370±0.039）μm;B组（1.456±0.044）μm;C组（2.044±0.019）μm;D组（1.970±0.047）μm,E组（0.683±0.023）μm;F组（2.195±0.066）μm。各组的剪切强度分别为A组（5.84±0.30）MPa;B组（10.22±0.63）MPa;C组（10.78±0.45）MPa;D组（12.24±0.46）MPa;E组（13.82±0.61）MPa;F组（16.81±0.74）MPa。结论钛基底表面喷砂结合酸蚀,微弧氧化及氮化钛涂层处理均可有效提高树脂与钛的粘接强度。