Surface modification of titanium using steel slag ball and shot blasting treatment for biomedical implant applications

Surface modification is often performed using grit or shot blasting treatment for improving the performances of biomedical implants. The effects of blasting treatments using steel slag balls and spherical shots on the surface and subsurface of titanium were studied in this paper. The treatments were conducted for 60-300 s using 2-5 mm steel slag bails and 3.18 mm spherical shots. The surface morphology, roughness, and elemental composition of titanium specimens were examined prior to and after the treatments. Irregular and rough titanium surfaces were formed after the treatment with the steel slag balls instead of the spherical shots. The former treatment also introduced some bioactive elements on the titanium surface, but the latter one yielded a harder surface layer. In conclusion, both steel slag ball and shot blasting treatment have their own specialization in modifying the surface of metallic biomaterials. Steel slag ball blasting is potential for improving the osseointegration quality of implants; but the shot blasting is more appropriate for improving the mechanical properties of temporary and load bearing implants, such as osteosynthesis plates.

Titanium Alloy Cage Implantation for the Treatment of Ischemic Necrosis of Femoral Head in Dogs

To study the effect of titanium alloy cage on the treatment of the ischemic necrosis of femoral head in dog, the model of the ischemic necrosis of femoral head was made with the liquid nitrogen in 15 hybrid adult dogs. The titanium alloy cage made of a hollow cylinder was driven into the subchondral bone of necrotic femoral head via central channel. The dogs were divided into 3 groups, each group was sacrificed 3, 6, 12 weeks after the operation respectively. No collapse of femoral head was observed after the operation. The position of the cages was good on radiograph. Microscopically, the cancellous bone of necrotic femoral head rebuilt gradually and grew into cage. After 12 weeks of creeping substitution, the cancellous bone filled up the hollow cavity and holes of the cages. It is concluded that the titanium alloy cage can provide structural support for the subchondral bone and prevent collapse and can be used for the treatment of the ischemic necrosis of femoral head.

Effect of high density electropulsing treatment on formability of TC4 titanium alloy sheet

An annealed TC4 titanium alloy sheet was treated by high density electropulsing(Jmax=(5.09-5.26)×103A/mm2,tp=110μs)under ambient conditions.The effect of electropulsing treatment(EPT)on the plastic deformation behavior of TC4 titanium alloysheet was studied using uniaxial tension tests.The experimental results indicate that electropulsing treatment significantly changesthe mechanical properties of sheet metal:the uniform elongation is increased by 35%,the yield stress is decreased by 19.8%and theyield to tensile ratio is decreased by 17.6%.It is of significant meaning to improve the formability of TC4 titanium alloy sheet.Theoptical microscope and scanning electron microscope(SEM)were used to examine the changes of the microstructure and the fracturemorphology before and after the electropulsing treatment.It is found that recrystallization occurs in the sheet metal and dimples infracture surface are large and deep after the electropulsing treatment.The research results show that the electropulsing treatment is aneffective method to improve the formability of titanium alloy sheets.

Effect of nitriding-sulfurizing composite treatment on the tribological behavior of titanium alloys

A composite layer was prepared on the surface of Ti-6Al-4V alloy by nitriding-sulfurizing composite treatment,and its microstructure and phase structure were examined by scanning electron microscopy（SEM） and X-ray diffraction（XRD）,respectively.The tribological performance was measured to investigate its dependence on the nitriding-sulfurizing composite treatment process.The results indicated that the composite layer was mainly comprised of Ti2N,TiN,and TiS2.It was found that the composite layer exhibited superior tribological properties under dry friction and absolute sliding conditions due to the formation of sulfides with self-lubricating function.

A New Aging Treatment Way for Near α High Temperature Titanium Alloys

Two near α titanium alloys, Ti-5.6Al-4.8Sn-2.0Zr-1Mo-0.35Si （1#） and Ti-6.0AI-4.8Sn-2.0Zr-1Mo-0.35Si （2#）, were solution-treated in the upper α＋β phase fields, and the duplex mixture microstructures consisting of the less volume fraction primary α phase （αp） and the transformed β phase （βt） were obtained. The aging treatments were carried out at 700℃ for 1# alloy and 760℃ for 2# alloy under varied terms, respectively. It guaranteed α2 ordered phase to precipitate only in αp but not in βt for the two alloys. The slower precipitation and growth of the α2 ordered phase and silicide was observed in 1# alloy in comparison with 2# alloy. The mechanical properties including tensile strength and ductility, the creep and lasting properties at 600℃ were investigated. Prolonging aging time did not predominantly change the tensile strength and ductility for the two alloys. The 600℃/100 h thermal exposure caused a notable decrease of tensile ductility in 2# alloy though no distinct decrease could be observed in 1# alloy after the thermal exposure. The lasting property of i# alloy was increased with prolonging aging time and finally was equal to or even better than that of 2# alloy. Nevertheless, no evident increase emerged in 2# alloy with prolonging aging time. Similarly, the creep property of 1# alloy monotonously increased with increasing aging time and finally was equal to or even better than that of 2# alloy. No evident increase could be observed for 2# alloy. It can be deduced that the overgrowth of α2 ordered phase and silicide is unable to enhance hot strength properties but cause an unacceptable damage to tensile ductility. The optimum equilibrium of the comprehensive properties depending on the proper control of α2 ordered phase and silicide can be achieved by properly selecting aging temperature and time.

Effect of heat treatment of titanium substrates on the properties of IrO_2-Ta_2O_5 coated anodes

The Ti substrates of IrO 2 -Ta 2 O 5 coated anodes were treated by solid-solution and aging, stress relieving annealing, and recrystallization annealing, and the coatings were prepared by thermal decomposition of a mixture of H 2 IrCl 6 ·6H 2 O dissolved in hydrochloric acid and TaCl 5 dissolved in alcohol. Scanning electron microscopy （SEM）, cyclic voltammetry （CV）, electrochemical impedance spectroscopy （EIS）, and accelerated life test （ALT） were employed to study the microstructure and electrochemical properties of the anodes. Compared with the anode without heat treatment, the anodes with heat treatment are of higher electrochemical activity and longer accelerated life; especially, the anode with recrystallization annealing treatment has the best electrochemical properties and the longest accelerated life.

In Vivo Evaluation of Titanium Implants Bioactivated by a Modified Kokubo’s Treatment

In this study a modified Kokubo’s treatment (MKT) was used to bioactivate titanium implants. Titanium surfaces were alumina-blasted and etched in HCl/H2SO4 solution followed by treatment in autoclave at 120°C for 1, 3, 5 hour periods with chemical solutions containing 1, 2 and 3 M of NaOH. The materials were characterized by surface angle measurements, roughness, field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), and in vivo tests. Statistical analysis by polynomial regression showed that solutions within 2.2 and 2.8 M NaOH lead to surface contact angles close to zero degree after 1 h of treatment. XPS analysis carried out on a sample treated 1 h in 2.2 M NaOH indicated the presence of a titanate film. This solution was selected to treat titanium implants for in vivo tests. These tests were performed on sheep in three types of separating surfaces: machined group (standard), SLA group (A) and MKT group (B) divided into two time intervals of 3 and 6 weeks. The samples in group B displayed better results compared to group A only after 6 weeks in terms of counter torque and bone implant contact (BIC).

Effects of thermohydrogen treatment on microstructures of α+β and β titanium alloy as-cast

The effects of thermohydrogen treatment on the microstructures of TC21 and Ti40 alloys as-cast were researched. The results show that the β phase content increases after charged hydrogen. Compound TixHy appears if H content reaches a certain content,which perfectly gathers on the grain-boundaries and/or dislocations and then diffuses into the grains. The microstructure of TC21 alloy after thermohydrogen treatment becomes fine and the best H content is 0.4%(mass fraction). However,the influence of thermohydrogen treatment on Ti40 microstructure is not obvious.

High Osteoconductive Surface of Pure Titanium by Hydrothermal Treatment

Surface properties of Ti implants (especially surface hydrophilicity) influence biological responses at the interface between the bone tissue and the implant. However, only a little research reported the effect of surface hydrophilicity on osteoconductivity by in vivo test. We have investigated the surface characteristics and osteoconductivity of titanium implant produced by hydrothermal treatment using distilled water at temperature of 180°C for 3 h, and compared with as-polished and those of implants produced by anodizing in 0.1 M H2SO4 with applied voltage from 0 V to 100 V at 0.1 Vsˉ1 and anodizing followed by hydrothermal treatment. The relationship between hydrophilic surface and osteoconductivity in various surface modifications was examined by in vivo test. In order to maintain the hydrophilicity of the hydrothermal sample surface, it was kept in to the phosphate buffered saline solution (PBS) with 5 times concentration: 5PBS(-) in room temperature. The surface characteristics were evaluated by scanning electron microscopy, XRD, X-ray photoelectron spectroscopy, surface roughness and contact angle measurement using a 2 μL droplet of distilled water. In in vivo testing, the rod samples (Φ2 × 5 mm) were implanted in male rat’s tibiae for 14 days and the bone-implant contact ratio, RB-I, was used to evaluate the osteoconductivity in the cortical and cancellous bone parts, respectively. As a result, hydrothermal treatment without anodizing still produced a smooth surface like an initial surface roughness of as-polished samples, Ra/μm B-I = 50% in cortical bone part (about four times higher than as-polished Ti) were provided by only hydrothermal process without anodizing after immersing into 5PBS(-).

HEAT TREATMENT BEHAVIOR OF CAN-FORGED TITANIUM ALUMINIDE ALLOY IN (α+γ) REGION

Ｔｉｔａｎｉｕｍａｌｕｍｉｎｉｄｅｂａｓｅｄａｌｏｙｈａｓｂｅｅｎｃｏｎ－ｓｉｄｅｒｅｄａｓａｐｒｏｍｉｓｉｎｇｈｉｇｈｔｅｍｐｅｒａｔｕｒｅｍａｔｅｒｉａｌ，ｅｓｐｅｃｉａｌｙｆｏｒｒｏｔａｒｙｃｏｍｐｏｎｅｎｔｓ．Ｈａｖｉｎｇｂｅｅｎｓｔｕｄｉｅ...

Low cycle fatigue improvement of powder metallurgy titanium alloy through thermomechanical treatment

A low-cost β type Ti-1.5Fe-6.8Mo-4.8Al-1.2Nd (mass fraction, %)(T12LCC) alloy was produced by blended elemental powder metallurgy(P/M) method and subsequent thermomechanical treatment. Low cycle fatigue(LCF) behavior of P/M T12LCC alloy before and after thermomechanical treatment was studied. The results show that the LCF resistance of P/M titanium alloy is significantly enhanced through the thermomechanical treatment. The mechanisms for the improvement of LCF behavior are attributed to the elimination of residual pores, the microstructure refining and homogenization.

The Effect of Titanium Nano Oxide and Heat Treatment on Physical Properties of Hornbeam (<i>Carpinus betulus</i>) in Golestan Province

The use of wood has been considered for a long time and to this day, it has a special place in human life. Modification of wood and lignocellulosic materials is done by various methods, including modification of physical, mechanical, chemical and thermal, that as a new technology, it leads to the improvement of their undesirable features. Among these methods, heat correction is a useful method to improve dimensional stability and leads to increased resistance to water absorption and decay. The main purpose of this study is to investigate the titanium Nano oxide and heat treatment on the physical properties of hornbeam species. Samples were saturated with titanium Nano oxide solution at a concentration of 5000 ppm and pressurized 7 times in a pressure tank. The samples were divided into three groups: control, heat and Nano thermal treatment. Heat and saturated samples with titanium Nano oxide were heat treated at three temperature levels of 150℃, 175℃ and 200℃ for 4 and 6 hours. All three groups underwent physical tests. Heat and Nano thermal oxide treatments led to reduced water absorption and thickness swelling. Comparison between heat and Nano thermal treatment showed a further decrease in water absorption and thickness swelling in Nano thermal samples.

Impact of Annealing Treatment on the Behaviour of Titanium Dioxide Nanotube Layers

In this work, we study the influence of the annealing treatment on the behaviour of titanium dioxide nanotube layers. The heat treatment protocol is actually the key parameter to induce stable oxide layers and needs to be better understood. Nanotube layers were prepared by electrochemical anodization of Ti foil in 0.4 wt% hydrofluoric acid solution during 20 minutes and then annealed in air atmosphere. In-situ X-ray diffraction analysis, coupled with thermogravimetry, gives us an inside on the oxidation behaviour of titanium dioxide nanotube layers compared to bulk reference samples. Structural studies were performed at 700°C for 12 h in order to follow the time consequences on the oxidation of the material, in sufficient stability conditions. In-situ XRD brought to light that the amorphous oxide layer induced by anodization is responsible for the simultaneous growths of anatase and rutile phase during the first 30 minutes of annealing while the bulk sample oxidation leads to the nucleation of a small amount of anatase TiO2. The initial amorphous oxide layer created by anodization is also responsible for the delay in crystallization compared to the bulk sample. Thermogravimetric analysis exhibits parabolic shape of the mass gain for both anodized and bulk sample;this kinetics is caused by the formation of a rutile external protective layer, as depicted by the associated in-situ XRD diffractograms. We recorded that titanium dioxide nanotube layers exhibit a lower mean mass gain than the bulk, because of the presence of an initial amorphous oxide layer on anodized samples. In-situ XRD results also provide accurate information concerning the sub-layers behavior during the annealing treatment for the bulk and nanostructured layer. Anatase crystallites are mainly localized at the interface oxide layer-metal and the rutile is at the external interface. Sample surface topography was characterized using scanning electron microscopy (SEM). As a probe of the photoactivity of the annealed TiO2 nanotube layers, degradation of an acid orange 7 (AO7) dye solution and 4-chlorophenol under UV irradiation (at 365 nm) were performed. Such titanium dioxide nanotube layers show an efficient photocatalytic activity and the analytical results confirm the degradation mechanism of the 4-chlorophenol reported elsewhere.

Influence of TiCl_4 treatment on performance of dye-sensitized solar cell assembled with nano-TiO_2 coating deposited by vacuum cold spraying

Titanium tetrachloride (TiCl4) treatment was employed to TiO2 coating deposited on fluoride-doped tin oxide (FTO) conducting glass and indium oxide doped tin oxide (ITO) conducting glass, respectively. The nano-crystalline TiO2 coating was deposited using a composite powder composed of polyethylene glycol (PEG) and 25 nm TiO2 particles by vacuum cold spraying (VCS) process. A commercial N-719 dye was used to adsorb on the surface of TiO2 coating to prepare TiO2 electrode, which was applied to assemble dye-sensitized solar cell (DSC). The cell performance was measured under simulated solar light at an intensity of 100 mW·cm-2. Results show that with an FTO substrate the DSC composed of a VCS TiO2 electrode untreated by TiCl4 gives a short-circuit current density of 13.1 mA·cm-2 and an open circuit voltage of 0.60 V corresponding to an overall conversion efficiency of 4.4%. It is found that after TiCl4 treatment to the VCS TiO2 electrode with an FTO substrate, the short circuit current density of the cell increases by 31%, the open-circuit voltage increases by 60 mV and a higher conversion yield of 6.5% was obtained. However, when an ITO substrate is used to deposit TiO2 coating by VCS, after TiCl4 treatment, the conversion efficiency of the assembled cell reduces slightly due to corrosion of the conducting layer on the ITO glass by TiCl4.

Effect of a Hybrid Micro/Nano-integrated Titanium Surface on Behavior of Rat Osteoblasts

The objective of this study was to investigate the effect of a new combined micro/nanoscale implant surface feature on osteoblasts＇ behaviors including cell morphology, adhesion, proliferation, differentiation, and mineralization in vitro. A new micro/nano-hybrid topography surface was fabricated on commercial pure titanium（Cp Ti） by a two-step sandblasted acid-etching and subsequent alkali-and heattreatment（SA-AH）. The conventional sandblasted/acid-etching（SA） treatment and alkali and heat（AH） treatment were also carried out on the Cp Ti as controls. Surface microstructures of the Ti disc samples were assessed by scanning electron microscopy（SEM）. The neonatal rat calvaria-derived osteoblasts were seeded on these discs and the initial cell morphology was evaluated by SEM and immunofluorescence. Initial adhesion of the cells was then assayed by DAPI staining at 1, 2, and 4 h after seeding. The Cell Counting Kit-8（CCact K8） assay, gene expression of osteoblastic markers（ALP, Col 1, OCN, BSP, OSX, Cbfα1） and Alizarin Red S staining assays were monitored respectively for cell proliferations, differentiation and mineralization. The results show significant differences in osteoblast＇s behaviors on the four kinds of Ti surfaces. Compared with Cp Ti surface, the SA and AH treatment can significantly promote cell adhesion, differentiation and mineralization of osteoblasts. In particular, the combined SA and AH treatments exhibit synergistic effects in comparison with the treatment of SA and AH individually, and are more favorable for stimulating a series of osteogenous responses from cell adhesion to mineralization of osteoblasts. In summary, this study provides some new evidence that the integrated micro/nanostructure on the Cp Ti surface may promote bone osseointegration between the Ti implantbone interfaces in vitro.

Effect of Post Weld Heat Treatment on Microstructure and Fracture Toughness of Friction Welded Joint

The effect of post weld heat treatment on the microstructure and fracture toughness of friction welded joints of Ti-6.5Al-1Mo-1V-2Zr alloy was studied. The experimental results show that equiaxial grains were formed at the center of the weld metal while highly deformed grains were observed in the thermomechanically affected zone. The fracture toughness of the weld metal was lower than that of the thermomechanically affected zone under as-weld and post weld heat treatment conditions. With increasing temperature of post weld heat treatment, the fracture toughness of weld center and thermomechanically affected zone increased. The fractographic observation revealed that the friction welded joints fractured in a ductile mode.

Optimal Selection and Control for Precipitation of α_2 Phase in Near α High Temperature Ti Alloys during Aging Treatment

The characteristic of the precipitation and growth of α2 ordered phase during aging treatment in near α Ti alloys have been investigated in terms of the influences of aging temperature, aging time and aging manner. The results exhibit that aging temperatures influence the distribution of α2 phase precipitated and cause the changes in growth speed of α2 phase. For various aging temperatures, the time to finish precipitation of α2 phase is different. The facts that various distribution characteristics and growth speed of α2 ordered phase are caused by changed aging condition imply optimal selection and control for precipitation of α2 ordered phase reachable. Some discussions on adoptable aging steps are presented.

Heat treatment process for improving ductility of Ti-25V-15Cr-2Al-0.2C alloy

The effect of heat treatment and thermal exposure on the microstructure and mechanical properties of non burning β titanium alloy Ti 25V 15Cr 2Al 0.2C (mass fraction, %) was investigated. It is found that the amount of α precipitation in samples after solution treatment followed by air cooling increases with increasing solution temperature. After solution treatment, the alloy was subjected to two different heat treatments to stabilize the material. The results show that the single ageing treatment(700 ℃, 4 h, AC) leads to a large amount of α precipitation, while the triplex treatment(850 ℃, 2 h, FC+700 ℃, 6 h, FC+540 ℃, 6 h, AC) significantly suppresses the formation of α precipitates. It is more important that after long term exposure at 540 ℃(the expected application temperature) samples heat treated by the triplex treatment have markedly higher ductility than those given the single aging treatment. The intermetallic compound TiCr 2 is observed in samples after long term exposure, which further degrades the ductility of the alloy.

Microstructural Evolution of Ti-5.6Al-4.8Sn-2Zr-1Mo-0.35Si-0.7Nd Titanium Alloy with Carbon Additions

The effect of carbon addition on microstructural evolution was studied in a near-α titanium alloy （Ti-5.6Al- 4.8Sn-2Zr-1Mo-0.35Si-0.7Nd）. It was found that flake and ribbon titanium carbides with a NaCl crystal structure formed in the as-cast alloys with carbon additions of over 0.17 wt pct. Flake carbide particles are the product of eutectic transformation and precipitate from the high-temperature β phase. The ribbon carbide particles are primary phases formed prior to the nucleation of any metallic phases. The as-cast alloys with carbide precipitation after heat-treatment at βt-30℃ followed by water quenching showed the spheroidization of α lamellae and partial dissolution of carbide particles. After annealing at βt＋15℃, carbide particles are mostly distributed at the grain boundary and spheroidized through mixed grain boundary plus bulk diffusions.