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

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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.

热处理工艺对大规格TC17钛合金棒材组织与力学性能的影响

研究了固溶温度、冷却方式、保温时间及取样方向对两相区锻造的大规格TC17钛合金棒材显微组织和力学性能的影响,并根据实验结果选择最佳热处理制度。结果表明:TC17钛合金棒材的最佳热处理工艺为800℃/2h/WQ+630℃/8h/AC;固溶温度在两相区时,随着固溶温度的升高,合金强度升高,塑性降低;固溶空冷+时效的合金较相同温度固溶水冷+时效的合金强度高、塑性低;在相同温度固溶水冷条件下,缩短固溶保温时间,可改善合金的塑性;锻造后的TC17钛合金大规格棒材存在各向异性。

解剖型锁定钛板与髓内钉治疗胫骨远端骨折的疗效比较

【目的】对比应用解剖型锁定钛板与髓内钉治疗胫骨远端骨折的临床疗效与并发症情况。【方法】自2019年9月至2021年9月,于中山大学孙逸仙纪念医院诊断为胫骨远端AO-A型骨折的手术患者纳入本研究,共32例。其中15例采用钛板螺钉治疗,17例采用髓内钉治疗。比较两组一般手术指标、骨折愈合时间、术后并发症发生情况、手术前后VAS评分及术后踝关节功能。【结果】患者均获得随访,随访时间10~20个月,平均12个月。髓内钉组手术时间、术中透视次数均长于钛板螺钉组,但术前等待时间、住院天数少于钛板螺钉组,统计学差异显著(P<0.05);两组骨折愈合时间相比,差异无统计学意义(P>0.05);术后6周,两组VAS评分均低于术前,统计学差异显著(P<0.05);髓内钉组与钛板螺钉组相比,手术前后VAS评分差异无统计学意义(P>0.05);术后6月AOFAS评分、术后1年踝关节活动度、并发症发生率髓内钉组优于钛板螺钉组,统计学差异显著(P<0.05);术后1年AOFAS评分两组差异无统计学意义(P>0.05)。【结论】钛板螺钉与髓内钉均是治疗胫骨远端AO-A型骨折的有效术式,远期临床疗效无明显差异。髓内钉的软组织并发症较少,对踝关节活动度影响更小,康复更快,安全性更高,而钛板螺钉发生术后软组织感染的概率较大。我们建议在临床工作中,应该做好患者的术前评估,在把握适应症的前提下,髓内钉并发症更少,有一定优势。

BASCA热处理对TC10钛合金组织与断裂韧性的影响

本工作对TC10钛合金进行BASCA热处理(β退火+缓慢冷却+时效),通过改变BA温度(β退火温度),研究BASCA热处理对TC10钛合金微观组织与断裂韧性的影响。结果表明:BA温度对合金微观组织与断裂韧性起到决定作用,随着BA温度升高,合金微观组织类型由等轴组织转变为片层组织,断裂韧性不断增加,最大值为77 MPa·m^(1/2)。此外,研究了不同类型组织的裂纹尖端区域塑性变形量、裂纹扩展路径以及断口微观形貌,进一步揭示断裂机制。与片层组织相比,等轴组织的裂纹尖端区域塑性变形较大,裂纹扩展路径曲折程度较小。等轴组织的断口形貌光滑平顺,主要由韧窝构成;片层组织的断口形貌凹凸起伏明显,韧窝数量与尺寸均减小,并出现撕裂棱、空洞以及二次裂纹。

阴极钛材表面处理工艺对其表面状态及铜离子电沉积初期行为的影响

目的研究表面处理工艺对钛材表面状态的影响,进一步探究阴极钛材表面状态对铜离子电沉积初期形核行为的影响。方法利用砂纸研磨、机械/电解抛光、化学腐蚀等不同的表面处理工艺,制备出不同表面状态的钛材,对钛材的表面粗糙度和形貌分别进行测试和扫描电镜观察。以不同表面状态的钛材作为阴极,进行铜离子的电沉积实验,对初始沉积层组织进行扫描电镜观察,并统计铜晶核的尺寸、覆盖率。结果砂纸研磨的钛材表面粗糙度最大,随着砂纸目数的增加,粗糙度降低,划痕变得细密,沉积的铜晶核尺寸较小、分布均匀、面覆盖率较高;抛光可显著降低钛材表面粗糙度,电解抛光的粗糙度最低,但铜晶核难以牢固附着;化学腐蚀会在钛材表面残留金属颗粒或暴露晶界组织,沉积的铜晶核分布不均匀且易发生团簇。结论铜离子的初始沉积形核行为与阴极钛材的表面粗糙度和缺陷状态密切相关,采用3000#~4000#砂纸精细研磨的方式,可使钛材表面粗糙度Rz保持在1~1.2μm,且表面覆盖有高密度均匀细小的划痕缺陷,最有利于铜离子的高密度均匀形核。

镁处理对TiN液析行为的影响

为研究镁处理对钛微合金钢在凝固过程中TiN液析行为的影响,采用真空感应炉冶炼了试验钢.利用SEM-EDS结合图像处理软件,分析铸坯径向不同位置处镁处理钢对比非镁处理钢中夹杂物的成分和尺寸变化,并用FactSage软件对夹杂物的形成和析出进行了计算.结果表明:钢中TiN夹杂均在凝固前沿的液相中生成.氮含量增加,凝固过程中TiN的析出温度升高和析出量增加,并对后续Ti4C2S2和MnS的析出产生影响.非镁处理条件下,铸坯1/4处和中心处TiN夹杂的平均粒径分别为2.48和2.11μm,镁处理后,尺寸分别降为1.50,1.45μm和1.48,1.38μm,数密度也有所增大.添加微量Mg,MgO·Al_(2)O_(3)即可稳定存在于钢中并在钢液降温过程中成为TiN的凝固核心,促使TiN夹杂分布弥散,减少了大尺寸TiN的生成.

生物医用Ti合金处理工艺、力学性能及耐腐蚀性能研究进展

生物医用Ti合金的植入物为适应人体内部复杂的环境,要求植入物具有高强度、一定的塑韧性和低的弹性模量等优异的力学性能。当自腐蚀电位越高以及腐蚀电流密度越小时,合金的耐蚀性将越好。合金在医用过程中在体内释放的金属离子将越少,对病人造成二次伤害也就越小。对第三代生物医用Ti合金的处理工艺、力学性能和耐腐蚀性能进行综述,以期对材料研究者在生物合金的应用研究方面提供有价值的参考。