Titanium is applied in various industries due to its valuable properties and abundant reserves. Generally, if a highly uniform oxide structure and a high-density oxide film is formed on the surface through anodization treatment, the utility value such as color appearance and corrosion inhibition efficiency is further increased. The objective of this study was to determine improvement of water-repellent property by controlling titanium oxide parameters such as pore size and inter-pore distance to improve corrosion resistance. Oxide film structures of different shapes were prepared by controlling the anodization processing time and voltage. These oxide structures were then analyzed using a Field Emission Scanning Electron Microscope (FE-SEM). Afterwards, a Self-Assembled Monolayer (SAM) coating was performed for the oxide structure. The contact angle was measured to determine the relationship between the shape of the oxide film and the water-repellency. The smaller the solid fraction of the surface, the higher the water-repellent effect. The surface with excellent hydrophobic properties showed improved corrosion resistance. Such water-repellent surface has various applications. It is not only useful for corrosion prevention, but also useful for self-cleaning. In addition, a hydrophobic titanium may open up a new world of biomaterials to remove bacteria from the surface.
PURPOSE. This study aimed to compare the effect of different surface treatments and luting agent types on the shear bond strength of two ceramics to commercially pure titanium (Cp Ti). MATERIALS AND METHODS. A total of 160 Cp Ti specimens were divided into 4 subgroups (n = 40) according to surface treatments received (control, 50 ㎛ airborne-particle abrasion, 110 ㎛ airborne-particle abrasion, and tribochemical coating). The cementation surfaces of titanium and all-ceramic specimens were treated with a universal primer. Two cubic all-ceramic discs (lithium disilicate ceramic (LDC) and zirconia-reinforced lithium silicate ceramic (ZLC)) were cemented to titanium using two types of resin-based luting agents: self-cure and dual-cure (n = 10). After cementation, all specimens were subjected to 5000 cycles of thermal aging. A shear bond strength (SBS) test was conducted, and the failure mode was determined using a scanning electron microscope. Data were analyzed using three-way ANOVA, and the Tukey-HSD test was used for post hoc comparisons (P < .05). RESULTS. Significant differences were found among the groups based on surface treatment, resin-based luting agent, and ceramic type (P < .05). Among the surface treatments, 50 ㎛ air-abrasion showed the highest SBS, while the control group showed the lowest. SBS was higher for dual-cure resin-based luting agent than self-cure luting agent. ZLC showed better SBS values than LDC. CONCLUSION. The cementation of ZLC with dual-cure resin-based luting agent showed better bonding effectiveness to commercially pure titanium treated with 50 ㎛ airborne-particle abrasion.
Kim Myung-Joo;Kim Chang-Whe;Lim Young-Jun;Park Hyun-Joo
The Journal of Korean Academy of Prosthodontics
/
v.43
no.6
/
pp.751-763
/
2005
Statement of problem. To improve a direct implant fixation to the bone, various strategies have been developed focusing on the surface of materials. The surface quality of the implant depends on the chemical, physical, mechanical and topographical properties of the surface. The different properties will interact with each other and a change in thickness of the oxide layer may also result in a change in surface energy, the surface topography and surface, chemical composition. However, there is limited the comprehensive study with regard to changed surface and biologic behavior of osteoblast by anodization. Purpose of study. The aim of this study was to analyze the characteristics of an oxide layer formed and to evaluate the cellular biologic behaviors on titanium by anodic oxidation (anodization) by cellular proliferation, differentiation, ECM formation and gene expression. And the phospholipase activity was measured on the anodized surface as preliminary study to understand how surface properties of Ti implant are transduced into downstream cellular events. Methods and Materials. The surface of a commercially pure titanium(Grade 2) was modified by anodic oxidation. The group 1 samples had a machined surface and other three experimental specimens were anodized under a constant voltage of 270 V(Group 2), 350 V(Group 3), and 450 V(Group 4). The specimen characteristics were inspected using the following five categories; the surface morphology, the surface roughness, the thickness of oxide layer, the crystallinity, and the chemical composition of the oxide layer. Cell numbers were taken as a marker for cell proliferation. While the expression of alkaline phosphatase and Runx2 (Cbfa1) was used as early differentiation marker for osteoblast. The type I collagen production was determined, which constitutes the main structural protein of the extracellular matrix. Phospholipase $A_2$ and D activity were detected. Results. (1) The anodized titanium had a porous oxide layer, and there was increase in both the size and number of pores with increasing anodizing voltage. (2) With increasing voltage, the surface roughness and thickness of the oxide film increased significantly (p<0.01), the $TiO_2$phase changed from anatase to rutile. During the anodic oxidization, Ca and P ions were more incorporated into the oxide layer. (3) The in vitro cell responses of the specimen were also dependant on the oxidation conditions. With increasing voltage, the ALP activity, type I collagen production, and Cbfa 1 gene expression increased significantly (p<0.01), while the cell proliferation decreased. (4) In preliminary study on the relation of surface property and phospholipase, PLD activity was increased but $PLA_2$ activity did not changed according to applied voltage. Conclusion. The anodized titanium shows improved surface characteristics than the machined titanium. The surface properties acquired by anodization appear to give rise more mature osteoblast characteristics and might result in increased bone growth, and contribute to the achievement of a tight fixation. The precise mechanism of surface property signaling is not known, may be related to phospholipase D.
Kim, Sang-Tae;Vang, Mong-Sook;Yang, Hong-So;Park, Sang-Won;Park, Ha-Ok;Lim, Hyun-Pil
The Journal of Korean Academy of Prosthodontics
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v.45
no.4
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pp.522-533
/
2007
Statement of problem: Despite of the recent development of the titanium casting system methods, the casting defects such as imperfect casting and internal porosity were frequently observed. Purpose: The purposes of this study were to compare and measure the castability, microhardness, and surface reaction between Grade 2 pure titanium and Ti-6Al-4V by casting these alloys from the different sprue design conditions. Material and methods: Depending on the sprue designs and titanium alloys, 42 ready-made wax patterns were used. By analyzing the remodeling of the cast, internal porosity, microhardness, and titanium surface layer of SEM, there were several results we observed. Results: 1. The measured castability of titanium were categorized in the ascending order: individual sprue group, runner bar group, and single group. This data are based on the statistically signigicant differences. 2. The castability of titanium has not showed the statistically significant differences among the alloys. However, CP-Ti groups were superior to Ti-6Al-4V groups by showing the noticeable castability. 3. The surface layers of the castings of all groups have showed $5{\mu}m$ titanium oxide layers irrespective of sprue designs and titanium alloys. Conclusion: From the above study results, by fabricating the restorations from the centrifugal casting machine direct sprue designs revealed better castability. As we increased the number of sprues in the wax pattern, it revealed better castability. The castability of pure titanium rather than that of Ti-6Al-4V was remarkable. To fabricate the complex forms of the restorations, further researches on the efficient sprue designs and titanium alloys must be made.
The thermo-chemical treatment (TCT) process was applied to achieve surface hardening of CP titanium. The following three different surface modification conditions were tested so that the best surface hardening process could be selected:(a) PVD, (b) TCT+PVD, and (c) TCT+Aging+PVD. These specimens were tested and analyzed in terms of surface roughness, wear, friction coefficient, and the gradient of hardening from the surface of the matrix. The three test conditions were all beneficial to improve the surface hardness of CP titanium. Moreover, the TCT treated specimens, that is, (b) and (c), showed significantly improved surface hardness and low friction coefficients through the thickness up to $100{\mu}m$. This is due to the functionally gradient hardened surface improvement by the diffused interstitial elements. The hardened surface also showed improvement in bonding between the PVD and TCT surface, and this leads to improvement in wear resistance. However, TCT after aging treatment did not show much improvement in surface properties compared to TCT only. For the best surface hardening on CP titanium, TCT+PVD has advantages in surface durability and economics.
Kim, S. H.;Lim, J. G.;Ha, S. B.;Choi, H.;lee, J. C.
Proceedings of the Korean Society of Precision Engineering Conference
/
2000.11a
/
pp.870-874
/
2000
This investigation reports the grinding characteristics of titanium alloy(Ti-6Al-4V). Grinding experiments were performed at various grinding conditions and the grinding forces and specific grinding energies were measured to investigate the grindability of titanium alloy with the three different wheels including Diamond, Green carbide and Alumina. To investigate the grinding characteristics of titanium alloy grinding force, force-ratio, specific grinding energy and grinding -ratio, were measured. Surface roughness was also measured with tracer and the ground surfaces were observed with SEM. Force-ratio of grinding of titanium alloy was very lower than that of grinding of SKD-11. Specific grinding energy are almost five times larger and rougher surface was obtained in titanium grinding.
Purpose: With the significance of stable adhesion of alveolar bone and peri-implant soft tissue on the surface of titanium for successful dental implantation procedure, the purpose of this study was to apply microgrooves on the titanium surface and investigate their effects on peri-implant cells and tissues. Methods: Three types of commercially pure titanium discs were prepared; machined-surface discs (A), sandblasted, large-grit, acid-etched (SLA)-treated discs (B), SLA and microgroove-formed discs (C). After surface topography of the discs was examined by confocal laser scanning electron microscopy, water contact angle and surface energy were measured. Human gingival fibroblasts (hGFs) and murine osteoblastic cells (MC3T3-E1) were seeded onto the titanium discs for immunofluorescence assay of adhesion proteins. Commercially pure titanium implants with microgrooves on the coronal microthreads design were inserted into the edentulous mandible of beagle dogs. After 2 weeks and 6 weeks of implant insertion, the animal subjects were euthanized to confirm peri-implant tissue healing pattern in histologic specimens. Results: Group C presented the lowest water contact angle ($62.89{\pm}5.66{\theta}$), highest surface energy ($45{\pm}1.2mN/m$), and highest surface roughness ($Ra=22.351{\pm}2.766{\mu}m$). The expression of adhesion molecules of hGFs and MC3T30E1 cells was prominent in group C. Titanium implants with microgrooves on the coronal portion showed firm adhesion to peri-implant soft tissue. Conclusions: Microgrooves on the titanium surface promoted the adhesion of gingival fibroblasts and osteoblastic cells, as well as favorable peri-implant soft tissue sealing.
Using the mechanical treatments for mechanical properties improvement was rarely in the development scope before. This research approves through analytical ways that surface impacts can improve the quality of the surface significantly. This fact is approved for deposited titanium on silicone substrate. The new algorithm called minimum resultant error method (MREM) which is a direct combination of nanoindentation, FEM and dimensional analysis through a reverse method is utilized to extract the mechanical characteristics of the coating surface before and after impact. This method is extended to the time dependent behavior of the material to obtain strain rate coefficient. To implement this new approach, a new analysis technic is developed to define the residual stress field caused by surface impact as initial condition for nanoindentation. Analyzing the model in micro and macro scale at the same time was one of the main resolved challenges in this study. The result was obtaining of the constants of Johnson-Cook constitutive equation. Comparing the characteristics of the coating surface before and after impact shows high improvement in yield stress (34%), Elastic modulus (7.75%) and strain hardening coefficient (2.8%). The main achievement is that the strength improvement in titanium thin layer is much higher than bulk titanium. The yield strength shows 41.7% improvement for coated titanium comparing with 24% for bulk material. The rate of enhancement is about 6 times when it comes to the Young's modulus.
Journal of the Korean Crystal Growth and Crystal Technology
/
v.20
no.2
/
pp.80-84
/
2010
The temperature-programmed reduction of titanium oxide ($TiO_2$) with pure $CH_4$ was used for the preparation of titanium carbide crystallites. The synthesized materials had the different surface areas, indicating that the structural properties of these materials were strong functions of two different heating rates and space velocity employed. The titanium carbide crystallites were active for $NH_3$ decomposition. Since the reactivity varied with changes in the particle size, ammonia decomposition reactivity over the titanium carbides crystallites appeared to be related to the different active species. The reactivities of titanium carbide crystallites were two and three times lower than those of the vanadium and molybdenum carbide crystallites, respectively. These results suggested that the difference in activities might be related to the degree of electron transfer between metals and carbon.
Kim, Sang-Hun;Vang, Mong-Sook;Yang, Hong-So;Park, Sang-Won;Park, Ha-Ok;Lim, Hyun-Pil;Oh, Gye-Jeong
The Journal of Korean Academy of Prosthodontics
/
v.45
no.2
/
pp.182-190
/
2007
Statement of problem: Titanium has many advantages of high biocompatibility, physical properties, low-weight, low price and radiolucency, but it is incompatible with conventional dental porcelain due to titanium's oxidative nature. Many previous studies have shown that they used the method of sandblast for surface treatment prior to porcelain application, the researches are processing about the method of acid etching or surface coating. Purpose: The purpose of this research is to study the effect on bond strength of surface roughness between titanium and porcelain with the same surface topography. Material and method: In this study, we evaluated the bond strength by using 3-point bending test based on ISO 9693 after classified 8 groups - group P : polished with #1200 grit SiC paper, group S10 : $1.0{\mu}m$ surface roughness with sandblasting, group S15 : $1.5{\mu}m$ surface roughness with sandblasting, group S20 : $2.0{\mu}m$ surface roughness with sandblasting, group S25 : $2.5{\mu}m$ surface roughness with sandblasting, group S30 : $3.0{\mu}m$ surface roughness with sandblasting, group S35 : $3.5{\mu}m$ surface roughness with sandblasting, group E : $1.0{\mu}m$ surface roughness with HCl etching. Results: Within the confines of our research, the following results can be deduced. 1. In the results of 3-point bending test, the bond strength of sandblasting group showed significant differences from one of polishing group, acid etching group(P<.05). 2. The bond strength of sandblasting groups did not show significant differences. 3. After surface treatments, the group treated with sandblasting showed irregular aspect formed many undercuts, in the SEM photographs. The bond strength of sandblasting group was higher than 25 MPa, the requirement of ISO 9693. Conclusion: In above results, bond strength of titanium and low-fusing porcelain is influenced more to surface aspect than surface roughness. And titanium has clinically acceptable bond strength below surface roughness of $3.5{\mu}m$.
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