冷喷涂SiC/Al纳米复合涂层的组织结构与性能

为制备基体相晶粒细小、增强相均匀分布的SiC/Al纳米复合涂层,以Al、SiC为原料,采用高能球磨法获得SiC颗粒弥散分布的纳米晶Al基复合材料粉末,利用冷喷涂技术低温成型制备了SiC/Al纳米复合涂层,分析了SiC含量对复合涂层相结构、晶粒尺寸、微观结构、硬度及磨损性能的影响规律。结果表明：冷喷涂可实现球磨纳米晶复合粉末结构的原位移植,所制备SiC/Al纳米复合涂层组织致密,微米及亚微米级SiC弥散分布在纳米晶Al（约80 nm）基体之上;SiC颗粒对Al基体有明显强化作用,冷喷涂SiC/Al纳米复合涂层的硬度随SiC体积分数的增加而显著增加,50% SiC/Al纳米复合涂层的硬度高达515 HV_0.3,约为Al块材的13倍;冷喷涂SiC/Al纳米复合涂层的耐磨损性能随着SiC含量增加而显著提高,涂层磨损失效机制为磨粒对基体的切削犁沟变形。     

湿度对纳米铝粉活性影响的研究

研究了存储环境湿度对纳米铝粉活性的影响,并对其变化机理进行了较深入的探讨.结果表明,环境湿度对纳米铝粉的活性影响十分明显：在相同存储时间内,随着环境湿度的增加,纳米铝粉的热焓和活性铝含量显著减少;原始纳米铝粉是被一层3 nm厚非晶态氧化铝包覆的壳层结构,在不同湿度条件下放置8周后,壳层厚度将逐渐增加至5 nm,随后不再继续增加.但在高湿度条件下,纳米铝粉颗粒芯部发现了类似壳层的非晶态结构,表明氧化行为仍在通过其它途径进入到了纳米铝粉的芯部.同时,在对纳米铝粉DSC-TG分析中还发现存在两次氧化现象.     

STRUCTURE AND SURFACE CONDITION OF ULTRAFINE AI PARTICLES

The crystal habit,crystalline structure,surface condition and composition of the ultrafine Alparticles prepared by inert gas evaporation method were studied in detail by means of highresolution transmission electron microscope,X-ray diffraction and X-ray photo-electronspectrum.The results indicate that the ultrafine Al particles prepared in high pure inert gasare of clear crystal habits,single crystal in a large majority and fcc crystalline structure witha_0=0.405 nm.It is also found on the surface of the Al particles that there is a layer of amor-phous Al_2O_3 with 2 nm average thickness,which could protect the particles against oxidizingfurther.Therefore,the ultrafine Al particles prepared by the inert gas evaporation method arevery stable in atmosphere.     

沉积偏压对AlCrTiN纳米复合涂层力学与抗高温氧化性能的影响

沉积偏压对涂层的结构与性能具有重要影响,为研究其对AlCrTiN纳米复合涂层成分、组织结构、力学与抗高温氧化性能的影响规律,采用磁控溅射技术,改变沉积偏压(-30、-60、-90、-120 V)制备四种AlCrTiN纳米复合涂层。利用X射线衍射仪、扫描电子显微镜、纳米压痕仪等仪器表征涂层的组织结构、成分、力学性能和抗高温氧化性能。研究结果表明：不同偏压下制备的AlCrTiN纳米复合涂层均为NaCl型fcc-(Al,Cr,Ti)N相结构。随着沉积偏压增大,涂层由沿(111)晶面择优生长转变为无明显的择优生长取向,晶粒尺寸降低,残余应力和硬度增大。偏压为-90 V与-120 V时,涂层表面更加致密,具有更高的硬度和弹性模量。在800℃与900℃氧化1 h后,所有涂层表面均生成一层连续致密的Al₂O₃膜。随着沉积偏压增加,氧化膜厚度逐渐降低,表明抗高温氧化性能逐渐增强,这是因为高偏压下涂层组织更致密,且晶粒更细小。研究成果对AlCrTiN纳米复合涂层的综合性能提升与工程化应用具有一定指导意义。     

OXIDATION RESISTANCE OF NANOCRYSTAL ODS ALUMINIDE COATINGS PRODUCED BY PACK ALUMINIZING PROCESS ASSISTED BY BALL PEENING

Nanocrystal ODS （oxide dispersion strengthening） aluminide coatings were produced on a stainless steel and nickel-based superalloy by the pock aluminizing process assisted by ball peening, Pure Al powders and 1% of ultra-fine Y2O3 powders were mixed by ball milling. The ultra-fine Y2O3 powders were dispersed in Al particles. Ball peening welded the Al particles onto the substrate and accelerated the formation of aluminide coating. Nanocrystal ODS aluminide coatings were produced by the outward growth at a much low temperature （below 600℃） in a short treatment time. The effects of the operation temperature and treatment time on the formation of the coatings were analyzed. SEM （scanning electron microscope）, AFM （atomic force microscope）, EDS （energy dispersive X-ray spectroscopy）, XRF （X-ray fluorescence spectrometer） and XRD （X-ray diffraction） methods were applied to investigate the microstructure of the coatings. High-temperature oxidation tests were carried out to evaluate the oxidation resistance of the ODS aluminide coatings.     

Influence of NH4Cl Powder Addition for Fabrication of Aluminum Nitride Coating in Reactive Atmospheric Plasma Spray Process

Reactive plasma spray is the key to fabricating aluminum nitride (AlN) thermally sprayed coatings. It was possible to fabricate AlN/Al composite coatings using atmospheric plasma spray process through plasma nitriding of Al powders (Al 30 ??m). The nitriding reaction and the AlN content could be improved by controlling the spray distance and the feedstock powder particle size. Increasing the spray distance and/or using smaller particle size of Al powders improved the in-flight nitriding reaction. However, it was difficult to fabricate thick and dense AlN coatings with an increase in the spray distance and/or when using fine particles. Thus, the coatings thickness was suppressed because of the complete nitriding of some particles (formation of AlN particles) during flight, which prevents the particle deposition. Furthermore, the excessive vaporization of Al fine particles (due to increased particle temperature) decreased the deposition efficiency. To fabricate thick AlN coatings in the reactive plasma spray process, improving the nitriding reaction of the large Al particles at short spray distance is required to decrease the vaporization of Al particles during flight. This study investigated the influence of adding ammonium chloride (NH₄Cl) powders on the nitriding process of large Al powders and on the microstructure of the fabricated coatings. It was possible to fabricate thick AlN coatings at 100 mm spray distance with small addition of NH₄Cl powders to the Al feedstock powders (30 ??m). Addition of NH₄Cl to the starting Al powders promoted the formation of AlN through changing the reaction path to vapor-phase nitridation chlorination-nitridation sequences as confirmed by the thermodynamic analysis of possible intermediate reactions. This changes the nitriding reaction to a mild way, so it is more controlled with no explosive mode and with relatively low heating rates. Thus, NH₄Cl acts as a catalyst, nitrogen source, and diluent agent. Furthermore, the evolved gases from the sublimation or decomposition of NH₄Cl can prevent the Al particles coalescing after melting.     

Characterization of Silicon Nanoparticles Formed from a Fluidized Bed Reactor and Their Incorporation onto Metal-Coated Carbon Fibers

Enhancing the light trapping using nonwoven arrays of fibers has the potential to improve the photocurrent of silicon solar cells. In this work, amorphous and crystalline Si nanopowders (30–300 nm) were embedded in carbon fibers and fixed in place with electrodeposited nickel. Scanning and transmission electron microscopy techniques have been used to study the morphology of the Si particles and their interactions with the coatings. Two types of nanoparticles are identified, homogeneous nucleated particles (amorphous particles with some crystalline regions) and attrition particles (mostly crystalline products formed from fracture of particles as they grow in a fluidized bed reactor). Using the Brunauer–Emmett–Teller (BET) technique, the surface area and the pore diameter of these agglomerated Si nanoparticles were calculated to be 6.4 m²/g and 9.8 nm, respectively. After embedding the Si particles into the carbon matrix with the metal coatings, the electrical resistivity decreases, suggesting it is possible to enhance the light extraction of silicon solar cells using Si nanoparticles.     

ZrCuAlSi大块非晶合金变温晶化行为

利用铜模吸铸法制备Zr46.3Cu43.3Al8.9Si1.5(at%)大块非晶合金,利用示差扫描量热(DSC)仪研究合金连续升温过程中的晶化行为,利用Kissinger方法计算其特征温度表观激活能,利用Doyle方法计算其局域激活能。结果表明,Zr46.3Cu43.3Al8.9Si1.5大块非晶合金具有良好的热稳定性。利用Kissinger方法计算得到其玻璃转变激活能Eg为395.4kJ/mol、晶化起始激活能Ex为343.2kJ/mol、晶化峰的激活能Ep为343.0kJ/mol。Doyle方法计算其局域激活能表明,其晶化过程中,激活能明显越过一能量势垒后,再呈现逐渐减小的趋势。     

Study on Nano structured WC Co Composite Powders Made by Mechanical Milling

１ＩｎｔｒｏｄｕｃｔｉｏｎＷＣＣｏｃｏｍｐｏｓｉｔｅｐｏｗｄｅｒｓａｒｅｔｈｅｍａｉｎｒａｗｍａｔｅｒｉａｌｓｆｏｒｐｒｏｄｕｃｉｎｇｃｅｍｅｎｔｅｄｃａｒｂｉｄｅｃｕｔｉｎｇｔｏｏｌｓ．Ｉｎｏｒｄｅｒｔｏｉｍｐｒｏｖｅｔｈｅｉｒｔｏｕｇｈｎｅ...     

表面钝化纳米铝粉的制备及氧化机理分析

采用高频感应线圈加热,以蒸发-冷凝法制备了纳米铝粉,用空气进行钝化处理,得到有钝化层保护的纳米铝粉.使用透射电镜、场发射扫描电镜、X射线衍射、差热分析DTA等测试手段,研究了表面钝化处理对纳米铝粉抗氧化性能的影响.结果表明:经过表面钝化处理的纳米铝粉粒径范围为15～60nm,纳米铝粉表面包覆了3～5nm厚的氧化铝膜,形成明显的核/壳结构,具有较好的抗氧化性能,这对于纳米铝粉的存储、活性保护机理的探讨有一定的意义.     

Nanopowder deposition by supersonic rectangular jet impingement

With a view toward developing the next generation of coatings using nanopowders, a cold gas dynamic spray (CGDS) technique has been investigated. In this method, a powder feeder is used to inject nanopowder agglomerates into a supersonic rectangular jet, with a design Mach number of 3.2. The powder particles gain speeds of up to 700 m/s through momentum transfer from the jet and bond to the substrate surface due to kinetic energy dissipation. Coatings of copper and nano-WC/10% Co on steel and aluminum substrates (3 to 5 μm in thickness) have been produced. The benefit of this process is that the material does not undergo any chemical changes during coating formation. To improve the quality of the coatings produced, the flapping motions produced by supersonic jet impingement were studied. Powder particle velocities and the jet impingement flow field were quantified using particle image velocimetry (PIV).     

Microstructural evolution during deformation of tin dioxide nanoparticles in a comminution process

Nanoparticles can be produced by wet grinding in stirred media mills if agglomeration is prevented by stabilization of the particles. Since the fracture mechanisms at the lower nanoscale are not yet understood, we studied the evolution of the microstructure within tin dioxide particles. Electrostatic stabilization allows the formation of tin dioxide with a mean particle size of 25 nm as measured by dynamic light scattering. High-resolution transmission electron microscopy (HRTEM) images show particles well below 10 nm and mean crystallite sizes of 9 nm were obtained from X-ray diffraction by applying the Rietveld refinement method. Additionally, TEM and HRTEM analyses were conducted to gain detailed insight into the microstructural effects governing the grinding process. Microscopy revealed surprisingly rich phenomena including the formation of shear bands, twinning and stacking faults that directly affect the grinding behavior. Interestingly the ceramic nanoparticles showed not only fracture patterns expected from brittle fracture but also many traces of plastic deformation. For comparison the uniaxial compression of particles up to 30 nm in diameter was simulated using molecular dynamics. The simulated particles shared microstructural details with the real samples, most importantly the shear bands which lead to significant plastic deformation. The internal microstructure produced during multiple particle stressing events in the mill and also observed in the simulations is directly linked to the fracture mechanism and the experimentally observed grinding limit.     

7055铝合金挤压材黑线缺陷分析

利用高倍组织观察,结合能谱分析,对7055铝合金挤压材阳极氧化后的“黑线”缺陷进行了分析。结果表明:“黑线”区域为AlZr聚集导致。通过严格控制原料质量,改善AlZr中间合金组织;在合金成分范围内,适当降低Zr元素的含量;熔炼过程中适当提高加热温度及时间,使Al₃Zr粒子熔解等手段,可消除“黑线”缺陷。     

原位自生TiB2/Al复合材料的组织与力学性能

采用钛盐与硼盐反应法成功制备原位自生TiB2/纯Al复合材料。利用扫描电子显微镜、透射电子显微镜和拉伸试验机研究不同粒子含量(质量分数为1%、2%和3%)对复合材料组织和力学性能的影响。结果表明:原位生成的TiB2粒子有矩形、近圆形和六边形三种形貌,尺寸为200~500 nm;粒子与Al基体界面洁净无反应层。随着粒子含量的增加,复合材料的强度随之升高,而伸长率则随之降低;当TiB2含量为3%时,屈服强度和抗拉强度分别达到78.1 MPa和102 MPa,相比于纯Al分别提高58%和43%,而伸长率降至32.5%,下降了24%。断口分析表明:随着TiB2粒子含量的增加,粒子团聚机率增加,在拉伸过程中,裂纹在粒子团聚处萌生并扩展,导致材料的塑性降低。     

Über die Vorbereitung von Metallgegenständen für das elektrophoretische Lackieren

Pretreatment of metal parts for electrocoating Electrocoating requires very careful pretreatment because surface defects and contaminations may have a very negative influence on coating quality (surface structure remains visible, decoloration of bright colors, in particular yellowing). Adhesion and corrosion resistance of the coatings are improved by phosphate coatings (on Fe, Al, Zn); Zn phosphate coats are most suitable on Fe and Zn, and Al phosphate coatings on Al. Coating thickness, however, must not be excessive. The accelerators added to the phosphating baths have a very pronounced bearing and should therefore be carefully selected. The phosphate coatings are partially (by 10%) dissolved in the electrophoretically applied coating.     

High-Resolution TEM of Precipitates and Interfaces

The advent of medium and high-voltage transmission electron microscopes (TEM) with point-to-point resolutions below 0.2 nm makes it possible to study precipitates and interfaces in metals at the atomic level. Understanding these structures at the atomic level is critical to understand microstructural development and the resulting physical and mechanical properties of metals. One area of transformation interfaces in metals that has recently been investigated by high-resolution transmission election microscopy (HRTEM) is the structure of metastable aging precipitates and their interphase boundaries in Al alloys.^1,2 The presence of these precipitates is largely responsible for the high strengths of many Al alloys. The low atomic number of Al alloys makes them ideally suited for study by HRTEM. The results from HRTEM investigations of percipitates and transformation interfaces in Al-2%Li-1%Cu and Al-15%Ag (wt.%) alloys illustrate the wealth of information that HRTEM can provide about the internal and interphase boundary structures of microscopic aging precipitates in metals. Currently, it is not possible to obtain such detailed structural information by any other technique.     

Effects of Ti_(0.5)Al_(0.5)N coatings on the protecting against oxidation for titanium alloys

Ti0.5Al0.5N coatings were deposited on TC11(Ti-6.5Al-3.5Mo-1.5Zr-0.3Si) and silicon substrates using a cathode arc ion-plating system.The microstructure, composition, phase structure, and oxidation-resistance of the alloys and nitride coatings were investigated by scanning electron microscopy, X-ray diffraction, transmission electron microscopy, Auger electron spectroscopy, and thermal analyzer.The results show that the oxidation resistance of the titanium alloy is relatively limited;the compound structures of Ti mixed with Al oxides are formed during the heating process.The phases of the Ti0.5Al0.5N coatings are composed of a TiN solid solution phase.The oxidation kinetics obeys the parabolic law.During the oxidation process, the selective oxidation of Al occurs, thus protecting the underlying coating and substrate.     

Preparation of Nanocomposite GDC/LSCF Cathode Material for IT-SOFC by Induction Plasma Spraying

Homogeneous mixtures of Ce_0.8Gd_0.2O_1.9 (GDC) and La_0.6Sr_0.4Co_0.2Fe_0.8O₃ (LSCF) nanopowders were successfully synthesized using induction plasma by axial injection of a solution. The resulting nanocomposite powders consisted of two kinds of nanopowders with different mass ratio of GDC/LSCF, such as 3/7 and 6/4. The morphological features, crystallinity, and the phases of the synthesized powders were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), local energy-dispersive x-ray spectroscopy (EDS) analysis, and x-ray diffraction (XRD). The nanopowders are almost globular in shape with a diameter smaller than 100 nm and their BET specific areas are around 20 m² g^?1. The GDC and LSCF phases are well distributed in the nanopowders. In addition, suspensions, made with the as-synthesized composite nanopowders and ethanol, were used to deposit cathode coatings using suspension plasma spray (SPS). Micro-nanostructures of the coatings are discussed. The coatings are homogeneous and porous (51% porosity) with cauliflower structures.     

Effect of Substrate Temperature on CaHPO4 Coating on HT-C/C Composites Prepared by Ultrasonic Induction Heating Method

采用超声感应加热法在H2O2水热处理C/C复合材料表面沉积了CaHPO4涂层,借助SEM、XRD、FTIR、EDS等手段,研究了衬底温度对涂层的微观结构的影响,并通过划痕测试评价涂层与C/C基体之间的结合强度,同时运用分析天平测量质量以研究涂层的沉积动力学。结果显示,所制得的CaHPO4涂层钙磷比为1.2左右,晶格中出现碳离子。涂层形貌无明显变化,但是伴随温度的升高,涂层致密度降低。涂层与基体之间的结合强度随温度升高而增强,但内聚强度随温度升高而减弱。CaHPO4涂层的感应加热沉积过程受表面化学反应控制,沉积活化能为46.7 kJ/mol。     

The influence of coating compliance on the delamination of thermal barrier coatings

Low relative density yttria stabilized zirconia (YSZ) thermal barrier coatings have been deposited on NiCoCrAlY over-lay bond-coated Hastelloy-X substrates by an electron beam-directed vapor deposition (EB-DVD) method. The coatings have been applied to both roughened and smooth bond coat surfaces. During thermal cycling, those deposited on roughened surfaces spalled by delamination with the failure located in the YSZ layer close to the thermally-grown oxide (TGO). The cracks were initiated at “corn kernel” defects in the YSZ layer by a bond coat rumpling mechanism. Coatings applied to smooth bond coat surfaces had much longer (factor of two) spallation lifetimes and delamination occurred at the bond coat/TGO interface by the nucleation and coalescence of interfacial voids. In both cases, the delamination lifetime decreased with coating density and significantly exceeded the lifetimes of higher density coatings made by conventional electron beam deposition methods. The enhanced life of the more porous coatings is consistent with an increased compliance. This reduces the YSZ layers stored strain energy contribution to the driving force for interface delamination.