NiCoCrAlYHf涂层与一种Ni基单晶高温合金循环氧化行为研究

在第三代Ni基单晶高温合金上制备NiCoCrAlYHf(HY5)高温抗氧化涂层,采用扫描电镜(SEM),能谱分析(EDS)和X射线衍射(XRD)等手段,对涂层表面及界面进行组织形貌观察和相结构分析,研究涂层试样的循环氧化动力学和元素互扩散行为。结果表明:采用真空电弧镀(AIP)方法制备的HY5涂层,提高了单晶高温合金的循环抗氧化能力;在1100℃大气环境中扩散600h后,涂覆HY5涂层的单晶高温合金基体中形成了互扩散区IDZ,互扩散主要由Cr,Ni元素从基体向高温抗氧化涂层的外扩散以及Al元素从高温抗氧化涂层向基体的内扩散构成;在涂层下方60μm左右有拓扑密堆相TCP析出,并形成二次反应区SRZ。     

纯钛材表面电弧喷涂铝层的高温抗氧化性能及机制

为了提高钛材的高温抗氧化性能,采用电弧喷涂方法在纯钛材表面制备了铝涂层,并对其进行800℃,64 h的连续氧化,从铝涂层的微观组织变化,探讨了其高温抗氧化机制。结果表明:电弧喷涂铝涂层可以显著提高纯钛材的高温抗氧化性能;在加热过程中,电弧喷涂的铝涂层发生熔化、扩散,形成了以Al3Ti相为主的扩散层,该富铝相提供充足的铝元素,在涂层表面形成连续的Al2O3,从而对纯钛基体提供有效的高温氧化防护作用。     

冷喷涂CoNiCrAlY涂层在Na_2SO_4熔盐中的热腐蚀行为

利用冷喷涂技术制备CoNiCrAlY涂层,并对涂层进行了真空预氧化处理。结合X射线衍射,扫描电镜,能谱分析等方法研究预氧化处理前后的CoNiCrAlY涂层在900℃的Na2SO4熔盐中的热腐蚀行为。结果表明:冷喷涂CoNiCrAlY涂层含氧量为0.12%(质量分数),孔隙率小于0.28%(体积分数)。真空预氧化处理在涂层表面生成厚约0.26μm连续、致密的α-Al_2O_3氧化膜;喷涂态涂层和预氧化涂层在热腐蚀150h后表面均生成了以α-Al_2O_3为主的致密连续氧化膜,保护了基体免受腐蚀破坏;真空预氧化处理有效减缓了S和O等元素向涂层内扩散的速率,从而提高了涂层的抗Na2SO4熔盐热腐蚀性能;高温热腐蚀对涂层的破坏作用远大于高温氧化。在相同温度下,涂层在单一Na2SO4熔盐中腐蚀时,Al的消耗速率约为高温氧化时的2倍。     

K4104镍基高温合金Al-Si涂层高温氧化过程中的元素扩散分析

采用无机盐料浆法在K4104镍基高温合金表面制备Al-Si涂层。依据GB/T13303-91《钢的抗氧化性能测定方法》标准,采用静态增重法对有涂层试样和无涂层试样进行了1000℃×200h抗高温氧化性能试验,并绘制了氧化动力学曲线。用带能谱扫描电镜对氧化膜的表面形貌和截面组织进行分析,研究有无涂层试样在高温氧化过程中的元素扩散。结果表明:Al-Si涂层和基体合金之间在高温氧化过程中的互扩散形成了厚度为120~140um的渗层。随着氧化时间的延长,外层铝含量逐渐降低,但仍能保持稳定的β-NiAl相。Si在扩散作用下形成内高外低的分布形式,形成的Cr3Si和富Si的M6C相有利于阻止涂层和基体元素之间的互扩散,降低化合物层的形成速度,体现了Al-Si涂层良好的抗高温氧化能力。     

发动机用TiAl表面双辉等离子制备W-Mo合金层及其高温氧化行为

目前采用双辉等离子表面合金化技术在TiAl合金表面制备W-Mo涂层的研究不多。通过SEM与XRD等测试手段,研究双辉等离子表面合金化技术在TiAl基体表面制得的W-Mo合金涂层在780℃温度下的氧化行为。研究结果表明:W-Mo改性合金在初期氧化阶段快速氧化增重,经过100 h氧化后,试样增重5.2 mg/cm2,有效改善了TiAl基体的高温抗氧化性能。W-Mo合金涂层对氧气扩散起到阻碍作用,使TiAl基体抗高温氧化性能获得显著提升。氧化处理后合金涂层表面未发生改变,形成了致密、均匀的氧化膜层。TiAl基体经100 h氧化后表面氧化膜主要是一种柱状晶结构,TiAl基体氧化产物包括金红石型TiO2以及刚玉2种成分。     

合金元素在MCrAlY涂层中的行为

采用电弧离子镀在新型r-Ni3Al基高温合金IC－6上沉积Ni-Cr-Al-Y和Ni-Co-Al-Y涂层,研究了元素对MCrALY涂层性能及元素行为的影响,结果表明,在沉积过程中,合金中的Al和Mo元素抑制了Cr从涂层向基体扩散,使涂层中的Cr维持在较高浓度,真空扩散处理时,涂层和基体之间发生互扩散,使涂层－基体元素浓度呈梯度分布,减小了涂层和基体热膨胀系数的差别,同时涂层的相结构也发生变化,r-Ni3Al和r-Ni仍是涂层的主要相,但是由于Cr原子的取代作用致使晶格常数a0发生变化,等温氧化实验表明,Ni-Cr-Al-Y和Ni-Co-Cr-Y涂层氧化规律遵循抛物线规律,900℃静态空气等温氧化时,Ni-Cr-Al-Y涂层中加入Co对其抗氧化性能的影响不大,1000℃静态空气等温氧化时,Ni-Cr-Al-Y涂层中加入Co后,降低了其抗氧化性。     

钼网表面MoSi2涂层的制备及其1500℃高温氧化性能

钼网被广泛用作高温催化剂载体,但关于其高温防护涂层的制备及失效机制却鲜有报道.用包埋渗硅方法在钼网表面制备了MoSi2高温抗氧化涂层,并在静态大气环境中开展了1500℃恒温氧化试验.利用X射线衍射仪(XRD)、扫描电镜(SEM)、能谱分析(EDS)等对氧化前后涂层的微观形貌和组织结构进行了表征.结果表明:1500℃氧化2h,MoSi2涂层中的Si元素会发生选择性氧化,在涂层表面形成一层连续的、具有“自愈合”功能的熔融态SiO2保护膜,阻挡氧向基体一侧的扩散,展现出了良好的高温抗氧化性能;高温条件下,涂层中的Si元素会和钼基体发生界面扩散反应生成抗氧化性能差的Mo5Si3,同时MoSi2不断地和氧发生反应生成Mo5Si3和SiO2,当涂层中的MoSi2完全转化为Mo5Si3,涂层将快速氧化失效.     

钼网表面MoSi_2涂层的制备及其1500℃高温抗氧化性能

钼网被广泛用作高温催化剂载体,但关于其高温防护涂层的制备及失效机制却鲜有报道。用包埋渗硅方法在钼网表面制备了MoSi_2高温抗氧化涂层,并在静态大气环境中开展了1 500℃恒温氧化试验。利用X射线衍射仪(XRD)、扫描电镜(SEM)、能谱分析(EDS)等对氧化前后涂层的微观形貌和组织结构进行了表征。结果表明:1 500℃氧化2 h,MoSi_2涂层中的Si元素会发生选择性氧化,在涂层表面形成一层连续的、具有"自愈合"功能的熔融态SiO_2保护膜,阻挡氧向基体一侧的扩散,展现出了良好的高温抗氧化性能;高温条件下,涂层中的Si元素会和钼基体发生界面扩散反应生成抗氧化性能差的Mo_5Si_3,同时MoSi_2不断地和氧发生反应生成Mo_5Si_3和SiO_2,当涂层中的MoSi_2完全转化为Mo_5Si_3,涂层将快速氧化失效。     

致密化处理对冷喷涂NiAl涂层的高温氧化行为的影响

通过机械合金化及冷喷涂在镍基高温合金(IN738)基体上制备Ni/Al复合涂层。在保护气氛Ar中热扩散制备NiAl金属间化合物涂层。为了研究致密化对NiAl涂层的抗氧化性能的影响,对NiAl金属间化合物涂层及经过喷丸工艺和在1080℃下10h的热处理获得的NiAl致密化涂层进行了等温氧化试验。将试样在1020℃下分别进行1h、10h和200h的氧化,采用X射线衍射仪和扫描电子显微镜分析了高温氧化后涂层的组织结构。结果表明,NiAl涂层高温氧化过程中涂层表面氧化膜剥落情况比较严重,1020℃高温氧化10h时有明显的氧化膜剥落现象,但涂层内部氧化随高温氧化的时间变化不大。致密化处理后NiAl涂层没有发生明显的氧化,并表现出了很好的抗氧化性能,在1020℃高温氧化200h后,涂层内部仍然没有发生明显的氧化。     

电弧离子镀TiC扩散障结构及抗高温氧化性能研究

采用电弧离子镀技术(AIP)在NiCrAlY涂层与镍基高温合金(DD3合金)之间沉积TiC薄膜作为扩散障层,研究了TiC对NiCrAlY涂层与基体的元素互扩散的阻碍作用和对涂层氧化动力曲线的影响。对于添加扩散障层前后的试样,进行循环抗氧化试验来评价其抗高温氧化性能,并用扫描电镜(SEM)分析氧化前后试样微观形貌和成分,用X-射线衍射仪分析涂层的相结构。试验结果表明:TiC有效阻滞DD3基体与涂层之间的元素互扩散,提高了NiCrAlY涂层和DD3合金的抗高温氧化性能。     

Effect of annealing titanium on in vitro bioactivity

In order to modify titanium surfaces for various biological applications, bioactive and pure titanium oxide thin films were coated on the titanium by thermal oxidation technique. The commercially pure titanium discs after polishing were heated at 500, 550, 600, 650 and 700 °C, respectively, for 10 min in air or in argon. To evaluate the ability of calcium phosphate formation, samples after annealing were soaked in the Eagle's minimum essential medium solution. Surface morphology and chemical composition of the samples before or after immersion were characterized by field emission – scanning electron microscopy and energy dispersive X-ray spectrometry.     

Formation of Hydroxyapatite Coatings on Titanium by Plasma-Electrolytic Oxidation in Alkaline Electrolytes

Materials Science - We study the influence of the voltage (100–180 V) of plasma-electrolytic oxidation on the formation of hydroxyapatite coatings on VT1-0 commercially pure titanium in...     

Influence of the Parameters of Plasma-Electrolytic Oxidation on the Formation of Calcium-Phosphate Coatings on Titanium

Materials Science - We study the dependence of formation of calcium-phosphate coatings on commercially pure VT1-0 titanium on the parameters of plasma-electrolytic oxidation: deposition voltage...     

H_2O和Y(O)对NiCoCrAl热障涂层高温氧化的影响

分别利用真空等离子沉积和超音速火焰喷涂技术制备含有Y和含Y氧化物的NiCoCrAl涂层,用差热分析和光学及电子显微镜研究两种涂层在Ar-16.7%O_2,Ar-3.3%H_2O和Ar-0.2%H_2-0.9%H_2O气氛中1100℃时的氧化动力学和断面微观结构,通过第一性原理计算对比在不同气氛中含Y氧化物对涂层氧化的影响机理。结果表明:对于NiCoCrAl+Y涂层,Y倾向于向界面扩散并在界面富集导致Al_2O_3膜生成更多有利于内氧化的孔洞,水蒸气更会对内氧化产生促进作用。而对于NiCoCrAl+Y(O)涂层,由于Y在涂层制备过程中被氧钉扎,导致NiCoCrAl+Y(O)涂层在上述气氛中生成了平直而均匀的Al_2O_3层,不同气氛对其氧化行为影响较小。上述研究进一步揭示NiCoCrAl涂层中活性元素Y的存在状态和氧化气氛中的水蒸气对氧化铝组织结构和生长速率有重要影响。     

The recrystallization and thermal oxidation behavior of CP-titanium

In this study, the effect of cold working on the recrystallization and thermal oxidation behaviours of Grade 2 quality commercial purity titanium (CP-Ti) were examined. Recrystallization tests were carried out on the 23%, 35% and 50% cold worked samples at various temperatures in between 550 and 700 °C. Thermal oxidation of the cold worked samples was conducted at 600 and 650 °C. Recrystallization activation energy was calculated as 66–88 kJ/mol. Since thermal oxidation progresses by oxide layer growth and diffusion of oxygen into the substrate (oxygen diffusion zone formation), oxygen diffusion zone formation activation energies of 149–170 kJ/mol were calculated for the examined cold work ratios. These results indicate that when a cold worked CP-Ti was subjected to thermal oxidation treatment to improve its surface hardness and wear resistance, it loses its bulk hardness due to recrystallization.     

Plasma-assisted deposition of metal and metal oxide coatings

A combination of physical vapour deposition and plasma-assisted chemical vapour deposition techniques were used to deposit Cu-, Ni- and Sn-rich SnO/SnO2 coatings on metal and ceramic substrates. Cu and Ni were deposited on Al alloy 6061 substrates and Ni deposition was also performed on glass microscope slides and commercially pure alumina substrates. Sn-rich SnO/SnO2, on the other hand, was coated on stainless steel and pure Cu substrates. A direct-current plasma system was used to deposit the pure metals in vacuum with a resistively heated tungsten boat that was coated with alumina. All samples were sputtered for 20 min in an argon:hydrogen (1:1) atmosphere at a pressure of 300 mTorr. To reduce contamination and oxidation of both substrates and deposited layers, Cu and Ni coatings were made with argon:hydrogen (2:1) carrier gas. Sn-rich tin oxide coatings were deposited in a pure argon atmosphere (no hydrogen) to allow for the oxidation of Sn deposits on the stainless steel and copper substrates. Investigations of coated surfaces by scanning electron microscopy and X-ray diffraction showed coatings to be smooth, continuous and pure. Deposition rates showed this application to provide a very high rate when compared with chemical vapour deposition and metal–organic chemical vapour deposition techniques. Scratch tests results prove good attachment of the coatings to their respective substrates. © 1998 Chapman & Hall     

Thin films of calcium phosphate and titanium dioxide by a sol-gel route: a new method for coating medical implants

Titanium is a commonly used biomaterial for dental and orthopaedic applications. To increase its ability to bond with bone, some attempts were made to coat its surface with calcium phosphate (CaP). This paper describes a new type of coating. Instead of a pure CaP layer, a mixing of titanium dioxide (TiO₂) and CaP is fabricated and deposited as a coating. These layers are deposited by a sol-gel route on pure titanium substrates using various pre-treatments. The method consists of mixing a solution of tetrabutyl ortho-titanate or a sol of titanium dioxide with a solution of calcium nitrate and phosphorous esters. This composite is deposited on to commercially pure titanium plates, mechanically polished or blasted with pure crystalline aluminum oxide, using the spin-coating technique. These coatings are then fired at 650 or 850°C for various times. The samples are characterized by X-ray diffraction for their crystallinity, X-ray photoelectron spectroscopy for their surface chemical composition and scanning electron microscopy for their topography. Samples treated at 850°C present a well-pronounced crystallinity, and a high chemical purity at the surface. The topography is strongly related to the viscosity of the precursor and the substrate pre-treatment. Possibilities to structure the outermost layer are presented. © 1999 Kluwer Academic Publishers     

钛表面的氧化对钛瓷结合强度的影响

研究了钛表面氧化对钛/瓷结合强度的影响, 并采用溶胶凝胶技术在钛表面制备SnO_x中间层, 研究SnO_x层对钛/瓷结合强度的影响. 结果表明：空气炉中800℃氧化3min后, 钛/瓷结合强度明显下降; 烤瓷炉中预氧化3min, 钛/瓷结合强度无明显变化. 热处理使钛表面生成一层金红石型氧化层, 钛/瓷剥脱主要发生在金红石氧化层与钛之间. 采用溶胶-凝胶法经300℃处理后在钛表面制得的SnO_x涂层, 可有效隔绝氧向Ti表面的扩散, 防止钛表面的过度氧化, 提高了钛/瓷结合强度. 经SnO_x涂层处理后, 钛/瓷剥脱主要发生在SnO_x涂层内.     

A study of the physical,chemical and biological properties of TiO2 coatings produced by micro-arc oxidation in a Ca–P-based electrolyte

In this work, a porous and homogeneous titanium dioxide layer was grown on commercially pure titanium substrate using a micro-arc oxidation (MAO) process and Ca–P-based electrolyte. The structure and morphology of the TiO₂ coatings were characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy, and profilometry. The chemical properties were studied using electron dispersive X-ray spectroscopy (SEM–EDS) and X-ray photoelectron spectroscopy. The wettability of the coating was evaluated using contact angle measurements. During the MAO process, Ca and P ions were incorporated into the oxide layer. The TiO₂ coating was composed of a mixture of crystalline and amorphous structures. The crystalline part of the sample consisted of a major anatase phase and a minor rutile phase. A cross-sectional image of the coating–substrate interface reveals the presence of voids elongated along the interface. An osteoblast culture was performed to verify the cytocompatibility of the anodized surface. The results of the cytotoxicity tests show satisfactory cell viability of the titanium dioxide films produced in this study.     

TA2纯钛微弧氧化陶瓷膜层的颜色和性能

在添加乙酸铜、乙酸镁的磷酸-氟锆酸钾电解液中对纯钛TA2基体进行微弧氧化处理,制备出颜色均匀的浅棕色陶瓷膜层。通过X射线衍射分析(XRD)、扫描电子显微分析(SEM)及附带的能谱(EDS),研究了陶瓷膜的表面和截面形貌、元素分布、相组成;用分光光度计测量了膜层的颜色,根据热震试验和三点弯曲法评价了膜层与基体的结合强度。结果表明:随着微弧氧化时间的延长,膜层中铜镁元素的含量增加,膜层的颜色随之发生变化,膜层与基体的结合强度降低。热震实验结果表明,膜层与基体有较高的结合强度。