Mechanism of surface modification of a porous-coated Ti-6Al-4V implant fabricated by electrical resistance sintering

A porous-coated Ti-6Al-4V implant was fabricated by electrical resistance sintering, using 480 F capacitance and 1.5 kJ input energy. X-ray photoelectron spectroscopy (XPS) was used to study the surface characteristics of the implant material before and after sintering. There were substantial differences in the content of O and N between as-received atomized Ti-6Al-4V powders and the sintered prototype implant, which indicates that electrical resistance sintering alters the surface composition of Ti-6Al-4V. Whereas the surface of atomized Ti-6Al-4V powders was primarily TiO₂, the surface of the implant consisted of a complex of titanium oxides as well as small amounts of titanium carbide and nitride. It is proposed that the electrical resistance sintering process consists of five stages: stage I – electronic breakdown of oxide film and heat accumulation at the metal-oxide interface; stage II – physical breakdown of oxide film; stage III – neck formation and neck growth; stage IV – oxidation, nitriding, and carburizing; and stage V – heat dissipation. The fourth stage, during which the alloy repassivates, is responsible for the altered surface composition of the implant.     

Fibroblast Adhesion and Proliferation on a New β Type Ti-39Nb-13Ta-4.6Zr Alloy for Biomedical Application

Cell attachment and spreading on Ti-based alloy surfaces is a major parameter in implant technology. Ti39Nb-13Ta-4.6Zr alloy is a new β type Ti alloy developed for biomedical application. This alloy has low modulus and high strength, which indicates that it can be used for medical purposes such as surgical implants.To evaluate the biocompatibility and effects of the surface morphology of Ti-39Nb-13Ta-4.6Zr on the cellular behaviour, the adhesion and proliferation of rat gingival fibroblasts were studied with substrates having different surface roughness and the results were also compared with commercial pure titanium and Ti-6Al-4V. The results indicate that fibroblast shows similar adhesion and proliferation on the smooth surfaces of commercial pure titanium (Cp Ti), Ti-39Nb-13Ta-4.6Zr, and Ti-6Al-4V, suggesting that Ti-39Nb-13Ta-4.6Zr has similar biocompatibility to Cp Ti and Ti-6Al-4V. The fibroblast adhesion and spreading was lower on rough surfaces of Cp Ti, Ti-39Nb-13Ta-4.6Zr and Ti-6Al-4V than on smooth ones. Surface roughness appeared to be a dominant factor that determines the fibroblast adhesion and proliferation.     

Fibroblast Adhesion and Proliferation on a New β Type Ti-39Nb-13Ta-4.6Zr Alloy for Biomedical Application

Cell attachment and spreading on Ti-based alloy surfaces is a major parameter in implant technology. Ti-39Nb-13Ta-4.6Zr alloy is a new β type Ti alloy developed for biomedical application. This alloy has low modulus and high strength, which indicates that it can be used for medical purposes such as surgical implants. To evaluate the biocompatibility and effects of the surface morphology of Ti-39Nb-13Ta-4.6Zr on the cellular behaviour, the adhesion and proliferation of rat gingival fibroblasts were studied with substrates having different surface roughness and the results were also compared with commercial pure titanium and Ti-6Al-4V. The results indicate that fibroblast shows similar adhesion and proliferation on the smooth surfaces of commercial pure titanium （Cp Ti）, Ti-39Nb-13Ta-4.6Zr, and Ti-6Al-4V, suggesting that Ti-39Nb-13Ta-4.6Zr has similar biocompatibility to Cp Ti and Ti-6Al-4V. The fibroblast adhesion and spreading was lower on rough surfaces of Cp Ti, Ti-39Nb-13Ta-4.6Zr and Ti-6Al-4V than on smooth ones. Surface roughness appeared to be a dominant factor that determines the fibroblast adhesion and proliferation.     

The cell attachment and morphology of neonatal rat calvarial osteoblasts on the surface of Ti-6Al-4V and plasma-sprayed HA coating: Effect of surface roughness and serum contents

The biocompatibility of material plays an important role in the bone–implant interface for the prosthetic implant fixation. The biocompatibility of implants is associated with the chemical composition, surface topography, surface energy and surface roughness of biomaterials. The effects of two factors, surface roughness and serum contents, on osteoblast behavior at the surface of Ti-6Al-4V and plasma sprayed HA coating were investigated in the experiment. The osteoblasts derived from neonatal rat calvarial were cultured in Dulbeccos modified Eagle medium (DMEM) with fetal bovine serum (FBS) on the surface of polished Ti-6Al-4V (Ti-p), grit-blasted Ti-6Al-4V (Ti-b), polished HA coating (HAC-p), and as-sprayed HA coating (HAC). Under culture medium containing 4% FBS, the level of cell attachment to the polished surface is significantly higher than the rough surface of the same experimental materials during all culture periods. Increasing the contents of FBS up to 10%, the difference of osteoblast attachment is not found between Ti-p and Ti-b. Under 4% serum condition, the cell morphology attached to smooth surfaces (Ti-p and HAC-p) is spread faster and are more flattened than the one to rough surface of the same experimental materials by SEM. After 24 h culture, the corroded cracks are easily observed at the surface of polished HA coatings, and the cell morphology on HAC-p coatings are elongated and less flattened compared with Ti-p. The result is consistent with statistical difference of cell attachment between Ti-p and HAC-p under 4% serum condition.     

Corrosion behavior of PIRAC nitrided Ti-6Al-4V surgical alloy

Hard titanium nitride (TiN) coatings were obtained on the surface of Ti-6Al-4V alloy using an original PIRAC nitriding method, based on annealing the samples under a low pressure of monatomic nitrogen created by selective diffusion of N from the atmosphere. PIRAC nitrided samples exhibited excellent corrosion resistance in Ringer's solution in both potentiodynamic and potentiostatic tests. The anodic current and metal ion release rate of PIRAC nitrided Ti-6Al-4V at the typical corrosion potential values were significantly lower than those of the untreated alloy. This, together with the excellent adhesion and high wear resistance of the TiN coatings, makes PIRAC nitriding an attractive surface treatment for Ti-6Al-4V alloy surgical implants.     

Interfacial reaction kinetics of SiC fiber-reinforced Ti3Al matrix composites

• 1.(1) SiC fibers reacted with Ti₃Al + Nb to form multilayer reaction products during consolidation and extended isothermal exposure. Complex carbides and silicides genertated from the reactions between Ti, Nb, Al and SiC appears to be the major components in the reaction zone. The C-rich layer on the surface of a SiC fiber affects the development of the reaction zone and the distribution of the reaction products.
• 2.(2) The fiber/matrix interfacial reaction is diffusion-controlled with an activation energy of 271.49 KJ/mole and 218.11 KJ/mole for the SCS-6/Ti-24A1-11Nb and Sigma/Ti-24Al-11Nb composites, respectively, at the early stage of reaction.
• 3.(3) The results of this study indicate that in the SCS-6/Ti-24Al-11Nb composite, the activation energy is higher, the growth rate of reaction zone is slower, and the consumption of C-rich layer is much slower than that in the SCS-6/Ti-6Al-4V composite.

     

Corrosion behavior of a low modulus β-Ti-45%Nb alloy for use in medical implants

The corrosion and electrochemical behavior of a low stiffness β -Ti-45wt.%Nb (Ti45Nb) was studied in solutions that resemble body environment, as compared to Ti6Al4V and Ti-55wt.%Ni (Ti55Ni, Nitinol) alloys currently used in surgical implants. In Ringers' solution, Ti45Nb alloy exhibited an excellent corrosion resistance, comparable to that of Ti6Al4V and much better than that of Nitinol. In acidic environments, β -Ti45Nb remained passive under conditions where active dissolution was observed for both Ti6Al4V and Nitinol alloys. The results warrant further corrosion and biocompatibility studies of β -Ti45Nb alloy to establish its suitability as implant material.     

Selective electron beam manufactured Ti-6Al-4V lattice structures for orthopedic implant applications: Current status and outstanding challenges

Additively manufactured Ti-6Al-4V lattices display unique mechanical and biological properties by virtue of their engineered structure. These attributes enable the innovative design of patient-specific medical implants that (i) are conformal to the intended surgical geometry, (ii) mimic the mechanical properties of natural bone, and (iii) provide superior biological interaction to traditional implants. Selective electron beam melting (SEBM) is an established metal additive manufacturing (AM) process that has enabled the design and fabrication of a variety of novel intricate lattices for implant applications over the last 15?years. This article reviews the technical and clinical characteristics of SEBM Ti-6Al-4V lattices, including (i) the SEBM process and its capabilities, (ii) the structures of human bones with an exhaustive list of corresponding mechanical properties from literature, (iii) the mechanical properties of SEBM Ti-6Al-4V lattices of various designs and their shortcomings when compared to human bones, (iv) microstructural control of SEBM Ti-6Al-4V lattices for improved performance, (v) the lattice manufacturability and associated geometric errors, and (vi) clinical cases. Existing literature on the mechanical response of SEBM Ti-6Al-4V lattice structures is exhaustively evaluated for documentation quality using established theoretical models. This extensive data-set allows novel insights into the effect of lattice design on mechanical response that is not possible with the individual data; and provides a comprehensive database for those who are actively involved in patient-specific SEBM implant design. On this basis, outstanding challenges and research opportunities for SEBM Ti-6Al-4V lattices in the biomedical domain are identified and discussed.     

Spine rod straightening as a possible cause for revision

In a previous study, the authors examined the elastic and short-term anelastic springback of Ti6Al4V, CoCrMoC and A316L stainless steel spine rods to observe how the rods mechanically respond in OR contouring. In that study rods were 200?mm long and only the movement at the tip was recorded. The implication of that work was that rods will straighten in-vivo, however, in order for the mechanism of straightening to be determined, the movement of individual bends over time must first be elucidated. Spine rods used were, commercially pure titanium (CP Ti) a primarily α-phase; Ti-6Al-4V; α/β-phase titanium alloy from two different suppliers (denoted by, Ti-6Al-4V (L) and Ti-6Al-4V); β-phase titanium (TNTZ) and CoCrMoC. Following contouring the rods were aged unconstrained, in normal atmosphere or simulated body fluid (SBF) in a CO₂ incubator for up to 288?h. Elastic springback is significantly different between alloys with different microstructures. Both types of Ti6Al4V rods, while meeting the ASTM F136 industry standard, have significantly different properties, most importantly yield strength, flexural modulus, and springback. Environment showed no significant impact on anelasticity. The anelastic response of Ti6Al4V L sample, which has relatively more beta phase than the Ti6Al4V sample, follows the pure beta phase TNTZ in its extended time response. CoCrMoC and CP Ti have a very reduced anelastic response compared to the other alloys. This potentially can have unanticipated effects on the outcome of spine procedures, as the surgeon is reliant on the rods having similar properties to achieve a desired outcome.     

Improved properties of Ti-6Al-4V by combining isothermal equal-channel angular processing and hot-extrusion

The aim of this work was to study effects of hot extrusion on the microstructure of Ti-6Al-4V (wt-%) alloy processed by ECAP. Firstly, an isothermally Ti–6Al–4V alloy processed by Equal channel angular pressing(ECAP) was preheated at 950°C for 6?min and then hot extruded at 900°C. The hot extrusion minimised the grain size and maximised the mechanical strength. Therefore, it was demonstrated that hot extrusion of Ti-6Al-4V alloys that processed by ECAP could be performed without compromising any mechanical properties. Therefore, it is possible to use the ability to apply a reduced cross-section in hot extrusion for an Ti-6Al-4V processed by ECAP without concern about the reduction of properties.     

Titanium levels in rats implanted with Ti6Al4V treated samples in the absence of wear

The effect of implantation time and implant nitriding on titanium ion concentration in several tissues of rats carrying Ti6Al4V implants was studied by means of inductively coupled plasma-mass spectroscopy (ICP-MS). Histological studies were also performed in order to check for tissue degeneration due to the Ti6Al4V implantation. The animals were divided into four groups: one received Ti6Al4V implants, the second received nitrided Ti6Al4V implants, the third group received nitrided and descaled Ti6Al4V implants and the last one was the control group. Half the animals of the implanted groups received the Ti6Al4V implant for 30 days, while the other half received the implant for 120 days. Spleen, muscle, kidney, lung, brain and bone samples were retrieved from these rats as well as the control group. Ion concentration measures did not show significant differences between control and implanted rats for the studied period of time, although histological studies showed minor differences, especially on liver tissue samples.     

Wettability modification and the subsequent manipulation of protein adsorption on a Ti6Al4V alloy by means of CO<Subscript>2</Subscript> laser surface treatment

Improvements in the wettability of the Ti6Al4V alloy following CO₂ laser treatment were identified as being due mainly to the increase in surface roughness, surface oxygen content and surface energy of the material. Untreated and mechanically roughened samples had higher amounts of adsorbed albumin and lower amounts of adsorbed fibronectin than CO₂ laser treated samples. Moreover, as the wettability of the Ti6Al4V alloy increased the adsorbed amounts of fibronectin increased, while the adsorbed amounts of albumin decreased—indicating the controllability of the CO₂ laser process. From this finding it is possible to assert that the wettability of the Ti6Al4V alloy was the prime influence on the observed changes in in vitro protein adsorption. Further, the noted considerable change in the polar component of surface energy, , on the protein adsorption implied that the protein adsorption on the Ti6Al4V alloy was probably due to the polar and chemical interactions. This work has demonstrated that CO₂ laser radiation could be a suitable means to modify the wettability of the Ti6Al4V alloy and thereby manipulate protein adsorption and consequently render the material more bone cell responsive.     

Fabrication of TiC/TiB/Ti3AlC2 phases reinforced coatings on Ti-6Al-4V substrate

Intermetallic matrix composite coatings reinforced by TiC, TiB₂, and Ti₃AlC₂ were fabricated by laser cladding the mixed power Ti, Al, and B₄C on the Ti-6Al-4V alloy. X-ray diffraction, scanning electron microscope, and energy dispersive spectroscopy were chosen to investigate the structures and morphologies of the coatings. Results showed that the coatings mainly consisted of the reinforcements of TiC, TiB₂, and Ti₃AlC₂ and the matrix of Ti₃Al, TiAl, TiAl₃, and α-Ti. The hardness and wear-resisting property of the prepared specimens of Ti-45Al-10B₄C and Ti-45Al-20B₄C were studied contrastively. It was found that the coating was metallurgical bonded to the Ti-6Al-4V substrate. The micro-hardness and dry sliding wear-resisting properties of the specimen of Ti-45Al-20B₄C were enhanced further. And the micro-hardness of Ti-45Al-20B₄C was from 900 HV_0.2 to 1225 HV_0.2. The wear-resisting property of Ti-45Al-20B₄C was four times as large as that of the Ti-6Al-4V alloys.     

激光化学气相反应生长Ti（C,N）薄膜的成分及微观结构

运用ＸＲＤ，ＥＰＭＡ，ＴＥＭ等手段分析在Ｔｉ－６Ａｌ－４Ｖ基材上用激光化学气相色反应生长的Ｔｉ（Ｃ，Ｎ）薄膜的成分，结构，显微结构，可在基材表面的形成大面积均匀的Ｔｉ（Ｃ，Ｎ）膜层，为无明显择优取向的等轴纳米晶，其中有少量的Ｔｉ２Ｎ相，且Ａｌ，Ｖ含量低于基材。     

Untersuchungen zur Eignung von ionenplattierten metallischen Schutzschichten auf Ti-6Al-4V bei Schwingungsverschleißbeanspruchung

Investigations on the Suitability of lon-Plated Metallic Coatings on Ti-6Al-4V at Fretting Fatigue Load To provide fretting fatigue damage flat specimens of the alloy Ti-6Al-4V were supplied with metallic coatings. For that purpose specimens were coated with Cu, Cr, V, Ti and with an Al/Cu-combination. These coated specimens were then tested in a fretting bridge equipment. It was found that all coatings except the Al/Cu-combination lead to considerable improvement of fretting fatigue life. As SEM-investigations show, a separation of the functions of specimen-body and specimen-surface was achieved by the coatings, so that the effectiveness of coatings of rather low wear-resistance is explicable.     

Pr激光表面合金化提高Ti－6Al－4V抗氧化性

采用激光Ｐｒ合金化表面处理，研究了Ｔｉ合金的高温氧比行为，结果表明，加入Ｐｒ改变了氧化膜结构，抑制了氧的短路扩散，并改善膜的附着性和塑性，氧化速度显著下降．     

Characterization and tribological evaluation of duplex treatment by depositing carbon nitride films on plasma nitrided Ti-6Al-4V

Carbon nitride (CN_X) films (with N/C ratio of 0.5) were deposited on both untreated and plasma nitrided Ti-6Al-4V substrates by D.C. magnetron sputtering using a graphite target in nitrogen plasma. TEM and XPS analysis revealed the formation of both amorphous CN_X structure and crystalline -C₃N₄ phases in the deposited coatings. Nano-indentation tests showed that the film hardness was about 18.36 GPa. Both the scratch tests and indentation tests showed that compared with CN_X film deposited directly on Ti-6Al-4V, the load bearing capacity of CN_X film deposited on plasma nitrided Ti-6Al-4V was improved dramatically. Ball-on-disk wear tests under both dry sliding and lubricated conditions (with simulated body fluids) were performed to evaluate the friction and wear characteristics of the deposited coatings. Results showed that under both dry and lubricated conditions, the duplex treated system (i.e., with CN_X film deposited on plasma nitrided Ti-6Al-4V substrate) was more effective in maintaining a favorable low and stable coefficient of friction and improving wear resistance than both individual plasma nitriding and CN_X films on Ti-6Al-4V substrate. Under dry sliding conditions, the generated wear debris of spalled films were accumulated on the wear track, mechanically alloyed and graphitized, thus significantly reducing the coefficient of friction and preventing wear of the substrate. However, under lubricated conditions, due to the flowing of the fluids, the lubricating wear debris was taken away by the fluids, and therefore, the direct contact of two original surfaces resulted in high coefficient of friction and extensive abrasive wear of the substrate for CN_X films deposited on Ti-6Al-4V substrate. Also when there was some small-area spallation of CN_X films, the fluids could seep into the interface between the film and substrate, thus degrading the interfacial adhesion and resulting in a large area spallation.     

超重力场反应连接制备TiB_2-TiC/1Cr18Ni9Ti和TiB_2-TiC/Ti-6Al-4V梯度复合材料

以1Cr18Ni9Ti、Ti-6Al-4V为金属基底,通过在B4C+Ti体系中引入CrO_3+Al铝热剂,调整反应体系绝热温度依次为3 193、3 282、3 290及3 473K,采用超重力场反应连接制备TiB_2-TiC/1Cr18Ni9Ti和TiB_2-TiC/Ti-6Al-4V梯度复合材料,发现随着反应绝热温度升高,陶瓷/金属界面区厚度不仅因金属熔深增加而增大,并且残存于界面上的Al_2O_3夹杂也随之增多。分别对B4C+Al体系与CrO_3+Al铝热剂进行配制、球磨活化、压制成坯并依次填料入坩埚后,发现残存于界面上的Al_2O_3夹杂完全消除,同时发现在TiB_2-TiC/1Cr18Ni9Ti界面上生成三维网络陶瓷/金属梯度复合结构,而在TiB_2-TiC/Ti-6Al-4V界面上形成跨尺度多层次梯度复合结构。     

Identification of failure mechanisms in retrieved fractured dental implants

Dental implants treatment complications include mechanical failures. These complications were considered minor until now but several clinical trials showed that mechanical complications are common in implantology and in implant rehabilitation. The aim of the study was to perform a detailed systematic failure analysis on Ti–6Al–4V and CP-Ti retrieved dental implants.A total number of 10 CP-Ti and 8 Ti–6Al–4V retrieved fractured dental implants and implant parts were collected and there metal composition was identified using SEM–EDX (energy dispersive X-ray spectroscopy).The identification of the implants failure mechanisms was done by comparing the fracture surfaces of retrieved fractured dental implants to fracture surfaces of implants fractured in lab conditions in room air, and also in an environment mimicking the intraoral environment, which includes artificial saliva and fluoride (exemplar testing). The analysis was done by using Scanning Electron Microscopy (SEM).The overall fracture mechanisms that were identified on the retrieved Ti–6Al–4V and of CP-Ti dental implants were identical to those found on fatigue fracture surfaces of the specimens’ fractured in lab conditions. No evidence was found for corrosion products on the metal surface, which might suggest the operation of a corrosion processes participating in the crack formation.This study clearly shows that fatigue is the main failure mechanism for Ti–6Al–4V and CP-Ti retrieved dental implants. The fractographic analysis showed that implants and their parts might be broken at relatively low cyclic load levels, of the kind that matches the load levels generated during mastication.     

Biocompatibility studies of human fetal osteoblast cells cultured on gamma titanium aluminide

Ti-48Al-2Cr-2Nb (at. %) (γTiAl), a gamma titanium aluminide alloy originally designed for aerospace applications, appears to have excellent potential for bone repair and replacement. The biological response to γTiAl implant is expected to be similar to other titanium-based biomaterials. Human fetal osteoblast cells were cultured on the surface of γTiAl and Ti-6Al-4V disks with variable surface roughness for both SEM and immunofluorescent analysis to detect the presence of collagen type I and osteonectin, proteins of the bone extracellular matrix. Qualitative results show that cell growth and attachment on γTiAl was normal compared to that of Ti-6Al-4V, suggesting that γTiAl is not toxic to osteoblasts. The presence of collagen type I and osteonectin was observed on both γTiAl and Ti-6Al-4V. The results obtained suggest γTiAl is biocompatible with the osteoblast cells.