微束等离子喷涂制备羟基磷灰石涂层微观结构的特征研究

目的 通过与大气等离子喷涂和超音速火焰啧涂的对比,研究微束等离子喷涂制备的羟基磷灰石涂层的微观组织特点.方法 以高结晶度的羟基磷灰石粉末为原料,采用三种不同的喷涂方法(微束等离子喷涂、大气等离子喷涂和超音速火焰喷涂),在Ti-6Al-4V基体上制备羟基磷灰石(HA)涂层.利用冷场发射扫描电子显微镜和X射线衍射仪,对三种涂层的形貌、相组成和择优取向进行分析.结果 与大气等离子喷涂及超音速火焰喷涂制备的涂层相比,应用该设备制备的羟基磷灰石涂层表面平整致密,无大量的气孔存在;涂层截面呈典型的层状结构,在近三分之一表面处观察到柱状晶;涂层中仅有少量的非晶相及分解相,结晶度高达90％以上.这些特征均有利于羟基磷灰石涂层在体液环境中的稳定性.结论 比较三种喷涂方法,采用微束等离子喷涂制备的羟基磷灰石涂层致密,结晶度高,杂相少,且存在择优取向的柱状晶.     

热喷涂NiCoCrAlYTa+7YSZ热障涂层颗粒沉积行为

分别采用低压等离子喷涂和大气等离子喷涂在K4169基体上收集了NiCoCrAlYTa颗粒沉积物及涂层,并对颗粒沉积物的形貌及涂层性能进行了观察分析。结果表明:低压等离子喷涂收集到的单个NiCoCrAlYTa扁平颗粒主要呈圆盘状,涂层致密且氧含量低。而大气等离子喷涂收集到的扁平颗粒主要呈溅射状,涂层孔隙率和氧含量均较高。又在经镜面抛光的NiCoCrAlYTa涂层和K4169基体上分别收集了7YSZ颗粒沉积物,并对其沉积形貌进行了观察分析,结果表明:在K4169基体上收集到的7YSZ颗粒沉积物主要呈圆盘状,表面存在大量的网状微裂纹及宏观环状贯通裂纹。在镜面抛光的NiCoCrAlYTa涂层表面收集的7YSZ颗粒沉积物,周围有少量的指状溅射物,中心部存在一定数量的网状微裂纹,但宏观环状裂纹消失。     

热处理对微束等离子喷涂羟基磷灰石涂层的影响

羟基磷灰石由于其良好的生物活性,被广泛的用作医用植入体的表面涂层材料.采用微束等离子喷涂(Microplasma Spraying,MPS)I艺在Ti-6Al-4V基体上制备羟基磷灰石涂层,通过扫描电镜(SEM)、X射线衍射(XRD)和傅里叶红外光谱(FTIR)分析了热处理对涂层相组成和表面形貌的影响规律.研究表明:微束等离子喷涂制备的羟基磷灰石涂层在经过热处理后结晶度提高,并且非晶相和杂质相转化成为HA结晶相.同时,羟基和磷酸根的完整性得到了恢复.过高的热处理温度易引起涂层裂纹等缺陷的增加,也容易造成羟基脱离造成HA分解.合理的热处理温度范围为600～700℃,保温时间为3 h.     

TiB2-SiC粉末喷雾造粒及其等离子喷涂沉积机理研究

利用喷雾干燥对TiB_2-SiC复合粉末进行造粒,研究了浆料固含量、粘结剂含量及SiC含量对喷雾干燥粉体颗粒形貌等的影响。采用大气等离子喷涂技术,以抛光的石墨为基体,在不同预热温度和不同喷距下对TiB_2-SiC粉末进行粒子收集,研究不同工艺参数对TiB_2-SiC粒子铺展形貌的影响,并制备了TiB_2-SiC涂层。结果表明:当浆料固含量为50%,粘结剂含量为5%,SiC含量为10%时,喷雾造粒获得球形度高、流动性好的TiB_2-SiC粉末;随着基体预热温度的升高,喷距的增大,扁平粒子的溅射逐渐减弱,形成规则的圆盘状粒子;在等离子焰流作用下,TiB_2-SiC粒子熔化加速并与基体发生碰撞,熔融粒子扁平化,急速冷却凝固,不断堆叠、搭接为宏观涂层。     

微束等离子喷涂气体对HA涂层结晶度的影响

采用微束等离子喷涂方法,分别选用工业纯氩气和含50%氦气的氦氩混合气体为工作气体,在Ti-6Al-4V基体上制备羟基磷灰石涂层.通过SEM和XRD对涂层形貌、相组成和结晶度进行研究.结果表明,两种工作气体均可以制备杂质相含量少且不产生TTCP(磷酸四钙)和CaO等杂质相的涂层,结晶度高于70%,对植入体在体内的稳定性有利.采用氦氩混合气体为工作气体的微束等离子弧热焓值高于氩气工作气体,前者涂层中的结晶相主要以再结晶的为主,后者结晶相以大量未熔HA内核为主.     

微束等离子喷涂羟基磷灰石涂层的体外生物活性研究

采用微束等离子喷涂(MPS)方法在Ti6A14V基体上制备羟基磷灰石(HA)涂层.利用扫描电镜(SEM)和x射线衍射(XRD)分析技术对HA涂层的表面形貌、相组成和结晶度进行表征,并通过模拟体液进行体外生物活性试验.结果表明,微束等离子喷涂制备的HA涂层具有一定粗糙度,存在气孔以及微裂纹.涂层存在热分解现象,涂层中含有HA、α-TCP、β-TCP和非晶相,不含CaO等杂质相.模拟体液试验表明,微束等离子喷涂工艺制备的HA涂层具有较好的生物活性和稳定性.涂层表面均有较大比例的CaP沉积层,且涂层整体保持完整,没有出现明显的剥离.     

微束等离子喷涂氧化锆增韧羟基磷灰石复合涂层

采用微束等离子喷涂方法,在Ti-6Al-4V基体上制备了羟基磷灰石 氧化锆(70HA-30ZrO2,质量分数,%)复合涂层.将复合涂层置于模拟体液中分别浸泡了3,7,14,28 d并观察表面磷灰石的生长情况以评价涂层生物活性.采用扫描电镜(SEM)和X射线衍射(XRD)分析技术对涂层浸泡前后的表面形貌和相组成进行了研究.结果表明,涂层中ZrO2主要以立方相存在;喷涂过程中羟基磷灰石(HA)出现了一定的分解,产生大量的α-Ca3(PO4)2杂质相.HA涂层熔化效果很好,但涂层中有未熔化的ZrO2颗粒.涂层在模拟体液中浸泡28 d后表面可以形成磷灰石,说明涂层具有很好的生物活性.     

微束等离子喷涂制备羟基磷灰石涂层

采用微束等离子喷涂系统制备羟基磷灰石涂层,通过扫描电子显微分析(SEM)和X射线衍射分析(XRD)对涂层形貌、相组成和结晶度进行了研究.结果表明,随着喷涂电流和离子气流量的增加,羟基磷灰石粒子的熔化和撞击后的铺展更充分,在70～130 mm范围内随着喷涂距离的增加粒子熔化程度增加.适当的喷涂工艺条件下微束等离子喷涂制备羟基磷灰石涂层的结晶度可以相当或高于传统大气等离子喷涂制备的涂层,有利于涂层在体液环境中稳定性的提高.     

Fe基非晶合金涂层的等离子喷涂成形特征

采用大气等离子喷涂法在Q235钢基材表面制备了Fe基非晶合金涂层，研究表明，涂层基本上由非晶相组成，在涂层中分布着少量的尺寸为2-5μm的淬态核结晶相，涂层中氧化物的含量较少。涂层由条带状粒子相互搭接、逐层堆积而成，具有典型的层状结构形貌。尺寸约为60μm的球形喷涂粒子在涂层中变形为高度尺寸约为6μm扁平状粒子，保证了高非晶相含量涂层的顺利形成。在涂层中的粒子边界还包含着少量的孔隙、微细的球形粒子等缺陷。涂层与基材、涂层中粒子问主要以机械结合为主，涂层与基材的结合区为涂层-基材体系中的最薄弱处。     

HVOF喷涂WC-12Co粒子在不同基体上的沉积行为

采用超音速火焰喷涂方法(HVOF)在铝合金、紫铜和不锈钢基体上制备WC-12Co扁平粒子,利用扫描电子显微镜(SEM)对半熔化两相粒子的扁平行为及与基体结合状况进行观察分析,并将半熔化WC-Co粒子与基体碰撞模型简化为液相的Co粒子和固相的WC颗粒分别与基体相互作用的过程,通过改进后的数学模型计算基体与粒子的相对形变比λ。结果表明:HVOF喷涂WC-12Co扁平粒子在铝、铜和不锈钢基体上分别呈现半球状、薄饼状和溅射状形貌,不同形貌的扁平粒子形变比λ不同。与半球状(λ1)和溅射状(λ1)扁平形式相比,形成薄饼状(λ≈1)的扁平粒子时粒子与基体均发生适度的变形,有助于增加粒子与基体的有效结合面积,提高结合强度。     

Effects of Post-weld Heat Treatment on Microstructure,Mechanical Properties and the Role of Weld Reinforcement in 2219 Aluminum Alloy TIG-Welded Joints

In as-welded state, each region of 2219 aluminum alloy TIG-welded joint shows diff erent microstructure and microhardness due to the diff erent welding heat cycles and the resulting evolution of second phases. After the post-weld heat treatment, both the amount and the size of the eutectic structure or θ phases decreased. Correspondingly, both the Cu content in α-Al matrix and the microhardness increased to a similar level in each region of the joint, and the tensile strength of the entire joint was greatly improved. Post-weld heat treatment played the role of solid solution strengthening and aging strengthening. After the post-weld heat treatment, the weld performance became similar to other regions, but weld reinforcements lost their reinforcing eff ect on the weld and their existence was more of an adverse eff ect. The joint without weld reinforcements after the post-weld heat treatment had the optimal tensile properties, and the specimens randomly crack in the weld zone.     

The First Phase of the SRIF Industrialized Base in ＂West Area＂ Has Been Put into Operation

After nearly two years＇ tense construction, the first phase of industrialized base of Shenyang Research Institute of Foundry （SRIF）, located at the Tiexi Casting and Forging Industrial Park in the west of Tiexi District, has now been completed and formally put into operation.     

Thermodynamics Study on the Decomposition of Chromite with KOH

Institute of Process Engineering, Chinese Academy of Sciences, China, has proposed a method for oxidative leaching of chromite with potassium hydroxide. Understanding the mechanism of chromite decomposition, especially in the potassium hydroxide fusion, is important for the optimization of the operating parameters of the oxidative leaching process. A traditional thermodynamic method is proposed and the thermal decomposition and the reaction decomposition during the oxidative leaching of chromite with KOH and oxygen is discussed, which suggests that chromite is mainly destroyed by reactions with KOH and oxygen. Meanwhile, equilibrium of the main reactions of the above process was calculated at different temperatures and oxygen partial pressures. The stable zones of productions, namely, K2CrO4 and Fe2O3, increase with the decrease of temperature, which indicates that higher temperature is not beneficial to thermodynamic reactions. In addition, a comparison of the general alkali methods is carried out, and it is concluded that the KOH leaching process is thermodynamically superior to the conventional chromate production process.     

Influence of Heat Treatment on Damping Behaviour of the Magnesium Wrought Alloy AZ61

The effect of isochronal heat treatments for 1h on variation of damping, hardness and microstructural change of the magnesium wrought alloy AZ61 was investigated. Damping and hardness behaviour could be attributed to the evolution of precipitation process. The influence of precipitation on damping behaviour was explained in the framework of the dislocation string model of Granato and Lücke.     

Effect of Rare Earth Doping on Impedance,Modulus and Conductivity Properties of Multiferroic Composites:0.5(BiLa_xFe_(1-x)O_3)–0.5(PbTiO_3)

The Lanthanum-doped bismuth ferrite–lead titanate compositions of 0.5(Bi LaxFe1-xO3)–0.5(Pb Ti O3)(x = 0.05,0.10,0.15,0.20)(BLxF1-x-PT) were prepared by mixed oxide method.Structural characterization was performed by X-ray diffraction and shows a tetragonal structure at room temperature.The lattice parameter c/a ratio decreases with increasing of La(x = 0.05–0.20) concentration of the composites.The effect of charge carrier/ion hopping mechanism,conductivity,relaxation process and impedance parameters was studied using an impedance analyzer in a wide frequency range(102–106Hz) at different temperatures.The nature of Nyquist plot confirms the presence of bulk effects only,and non-Debye type of relaxation processes occurs in the composites.The electrical modulus exhibits an important role of the hopping mechanism in the electrical transport process of the materials.The ac conductivity and dc conductivity of the materials were studied,and the activation energy found to be 0.81,0.77,0.76 and 0.74 e V for all compositions of x = 0.05–0.20 at different temperatures(200–300 °C).     

Quantitative Analysis of the Crystallographic Orientation Relationship Between the Martensite and Austenite in Quenching–Partitioning–Tempering Steels

The orientation relationships(ORs)between the martensite and the retained austenite in low-and medium-carbon steels after quenching–partitioning–tempering process were studied in this work.The ORs in the studied steels are identified by selected-area electron diffraction(SAED)as either K–S or N–W ORs.Meanwhile,the ORs were also studied based on numerical fitting of electron backscatter diffraction data method suggested by Miyamoto.The simulated K–S and N–W ORs in the low-index directions generally do not well coincide with the experimental pole figure,which may be attributed to both the orientation spread from the ideal variant orientations and high symmetry of the low-index directions.However,the simulated results coincide well with experimental pole figures in the high-index directions{123}_(bcc).A modified method with simplicity based on Miyamoto’s work was proposed.The results indicate that the ORs determined by modified method are similar to those determined by Miyamoto’method,that is,the OR is near K–S OR for the low-carbon Q–P–T steel,and with the increase of carbon content,the OR is closer to N–W OR in medium-carbon Q–P–T steel.     

Using Finite Element and Contour Method to Evaluate Residual Stress in Thick Ti-6Al-4V Alloy Welded by Electron Beam Welding

This work was to reveal the residual stress profile in electron beam welded Ti-6Al-4V alloy plates(50 mm thick) by using finite element and contour measurement methods.A three-dimensional finite element model of 50-mmthick titanium component was proposed,in which a column–cone combined heat source model was used to simulate the temperature field and a thermo-elastic–plastic model to analyze residual stress in a weld joint based on ABAQUS software.Considering the uncertainty of welding simulation,the computation was calibrated by experimental data of contour measurement method.Both test and simulated results show that residual stresses on the surface and inside the weld zone are significantly different and present a narrow and large gradient feature in the weld joint.The peak tensile stress exceeds the yield strength of base materials inside weld,which are distinctly different from residual stress of the thin Ti-6Al-4V alloy plates presented in references before.     

Microstructures and Tensile Properties of Ultrafine-Grained Ni–(1–3.5) wt% SiC_(NP) Composites Prepared by a Powder Metallurgy Route

Silicon carbide nanoparticle-reinforced nickel-based composites(Ni–Si CNP),with a Si CNPcontent ranged from1 to 3.5 wt%,were prepared using mechanical alloying and spark plasma sintering.In addition,unreinforced pure nickel samples were also prepared for comparative purposes.To characterize the microstructural properties of both the unreinforced pure nickel and the Ni–Si CNPcomposites transmission electron microscopy(TEM) was used,while their mechanical behavior was investigated using the Vickers pyramid method for hardness measurements and a universal tensile testing machine for tensile tests.TEM results showed an array of dislocation lines decorated in the sintered pure nickel sample,whereas,for the Ni–Si CNPcomposites,the presence of nano-dispersed Si CNPand twinning crystals was observed.These homogeneously distributed Si CNPwere found located either within the matrix,between twins or on grain boundaries.For the Ni–Si CNPcomposites,coerced coarsening of the Si CNPassembly occurred with increasing Si CNPcontent.Furthermore,the grain sizes of the Ni–Si CNPcomposites were much finer than that of the unreinforced pure nickel,which was considered to be due to the composite ball milling process.In all cases,the Ni–Si CNPcomposites showed higher strengths and hardness values than the unreinforced pure nickel,likely due to a combination of dispersion strengthening(Orowan effects) and particle strengthening(Hall–Petch effects).For the Ni–Si CNPcomposites,the strength increased initially and then decreased as a function of Si CNPcontent,whereas their elongation percentages decreased linearly.Compared to all materials tested,the Ni–Si CNPcomposite containing 1.5% Si C was found more superior considering both their strength and plastic properties.     

Directional Growth of Tin Crystals Controlled by Combined Solute Concentration Gradient Field and Static Magnetic Field

A new method was introduced to achieve directional growth of Sn crystals. Microstructures in liquid(Pb)/liquid(Sn) diffusion couples were investigated under various static magnetic fields. Results show that the β-Sn crystals mainly reveal an irregular dendritic morphology without or with a relatively low static magnetic field(B0.3 T). When the magnetic field is increased to 0.5 T, the β-Sn dendrites close to the final stage of growth begin to show some directional character. With a further increase in the magnetic field to a higher level(0.8–5 T), the β-Sn dendrites have an enhanced directional growth character, but the dendrites show a certain deflection. As the magnetic field is increased to 12 T, the directional growth of the β-Sn dendrites in the center of the couple is severely destroyed. The mechanism of the directional growth of the β-Sn crystals and the deflection of the β-Sn crystals with the application of static magnetic field was tentatively discussed.     

电化学噪声数据处理方法概述

综述了常见的电化学噪声数据处理方法,介绍了直流趋势剔除、统计分析、快速傅立叶变换(FFT)法计算功率谱密度(PSD)以及小波变换处理电化学噪声信号的基本过程,并阐释了各种数学处理及所得参数的物理意义。