磁控溅射沉积Cu-Nb薄膜的特征及热退火的影响

用磁控共溅射法制备含铌1.16%～27.04%(原子分数)的Cu-Nb合金薄膜,运用EDX,XRD,SEM,TEM,显微硬度仪和电阻仪对沉积态和热退火态薄膜的成分、结构和性能进行了研究.结果表明,Nb添加显著影响Cu-Nb合金薄膜微结构,使Cu-Nb薄膜晶粒细化,含铌1.82%～15.75%的Cu-Nb膜呈纳米晶结构,存在Nb在Cu中的fec Cu(Nb)非平衡亚稳过饱和同溶体,固溶度随薄膜Nb浓度增加而上升,最大值为8.33%Nb.随Nb含量增加,薄膜中微晶体尺寸减小,Cu-27.04%Nb膜微结构演变至非晶态.与纯Cu膜对比表明,Nb添加显著提高沉积态Cu-Nb薄膜显微硬度和电阻率,总体上二者随膜Nb含量上升而增高.Nb含量高于4.05%时显微硬度增幅趋缓,非晶Cu-Nb膜硬度低于晶态膜,电阻卒则随铌含量上升而持续增加.经200,400及650℃退火1h后,Cu-Nb膜显微硬度降低、电阻率下降,降幅与退火温度呈正相关.XRD和SEM显示,650℃退火后晶态Cu-Nb膜基体相发生晶粒长大,并出现亚微米级富Cu第二相,非晶Cu-27.04%Nb膜则观察到晶化转变和随后的晶粒生长.Nb添加引起晶粒细化效应以及退火中基体相晶粒度增大是Cu-Nb薄膜微观结构和性能形成及演变的主要原因.     

Cu-W、Cu-Mo薄膜的微观结构及显微硬度分析

采用磁控共溅射方法分别制备了含有W和Mo两种不同成分的铜系薄膜,用EDX、XRD、SEM和纳米压痕仪对薄膜成份、结构、形貌和显微硬度进行了分析。结果表明,制备出的Cu—W和Cu-Mo薄膜均呈晶态结构,Cu-W和Cu—Mo形成了均匀的固溶体;经650℃热处理1h后,Cu—W和Cu—Mo薄膜中晶粒长大,有富w和富Mo相从基体Cu相中弥散析出;Cu-W薄膜的显微硬度随W成分的增加先增加后降低;Cu—Mo薄膜的显微硬度随Mo成分的增加而持续升高,薄膜退火态的显微硬度低于沉积态。分析认为,以上结果的产生均因添加W、Mo所引起的晶粒细化效应和薄膜的热稳定性较差所致。     

球磨法制备Mg-Cu非晶态合金粉末

本文研究了Mg—Cu二元相图的三个共晶点成分配方和两个化合物成分配方在球磨条件下非晶态合金的形成能力。XRD结果显示：除一个共晶点成分配方外，其它所有成分配方都能形成非晶态合金；非晶形成能力由大到小依次为MgCu2(化合物)，Mg58Cu42(共晶点)，Mg2Cu(化合物)，Mg85Cu15(共晶点)，Mg22Cu78(共晶点)。显然，作为选择非晶态合金成分的判据来说，Schwarz与Johnson的两个条件准则比Davies的共晶线准则更加合适。非晶形成的过程是：首先发生Mg在Cu中的固溶，随后形成过饱和固溶体，最后过饱和固溶体失稳形成非晶态合金。     

在线淬火工艺与微量元素对6008铝合金吸能盒性能的影响

研究了在线淬火方式及微量合金元素Mn对6008铝合金吸能盒组织与性能的影响。结果表明:型材强度随着淬火冷却速率的提高而明显提高,延伸率也有所增加。穿水冷却改善了型材的力学性能与压溃效果,主要原因是穿水冷却可以有效避免淬火过程中过饱和固溶体脱溶,确保了Mg、Si元素的过饱和固溶度。Mn元素的含量从0.3%增加到0.5%时,晶粒尺寸明显减小,力学性能和压溃性能明显提高。     

Al-Er合金中Al3Er相的形成及演化

采用金属型水冷模铸造制备了不同含铒量的Al-Er二元合金,通过对铸态及均匀化处理后实验合金的金相观察、电子探针(EPMA)以及透射电镜分析,研究了对不同含量的Er在AI-Er合金中的存在形式及固溶Er在纯铝中的固溶度.结果表明,在本实验条件下铒元素以过饱和固溶体形式存在于α-Al中和以Al3Er化合物的形式分布在晶界上,另外Er在铝基体的最大固溶度为O.1%(质量分数).     

W纤维增强高Cu含量W-Cu复合材料的研究

选用0.13mm的W纤维编织成纤维毡,通过控制压制压力制备一系列孔隙度不同的W骨架,用高温熔渗得到Cu-W基复合材料。采用金相观察、物理和力学性能测试等试验手段,研究其显微组织、密度、硬度和电学性能。结果表明:用螺旋状W纤维织得的纤维毡,熔渗可得到较宽范围Cu含量的W纤维增强Cu基复合材料,W纤维均匀地分布在Cu基体内;W-Cu合金的相对密度达到98%以上,硬度超过86HB,电导率最高达到78.4%IACS。     

钨粉/锆基非晶复合材料制备工艺研究

研究了钨粉/锆基非晶复合材料的制备工艺。将高纯度的W、Ti、Ni粉混合均匀并压缩成块,与Cu、Be、Zr块一同放入铜坩埚中,通过电弧熔炼铜模铸造的方法制备出钨粉/锆基非晶复合材料。对该非晶复合材料进行金相组织观察、成分分析、力学性能测试,并对试样的断口进行SEM观察,发现由于钨粉和液态金属的接触面积增加,作用接触时间增长,使非晶复合材料中有晶态相产生,其压缩强度要低于非晶合金。     

停放时间对Al-Mg-Si合金挤压棒材组织与性能的影响

通过光学显微镜、X射线衍射技术、透射电子显微镜、硬度和单轴拉伸等分析测试技术,研究了停放时间对AlMg-Si合金挤压棒材显微组织和性能的影响。研究结果表明,当合金经过固溶淬火后,立即进行人工时效,合金析出序列为过饱和固溶体→β'相,基体强化相主要为棒状过渡β'相;合金固溶后,当经过不同停放时间后,再进行人工时效,合金析出序列为过饱和固溶体→β″相,基体强化相主要为针状亚稳β″相,且β″相的数量随着停放时间延长而逐渐增多,当停放时间超过6h后趋于稳定,因此最佳的停放时间为6h。     

机械合金化制备Zr_(50)Al_(15)Ni_(10)Cu_(25)非晶合金粉末的非晶化机制

用Zr,Al,Ni和Cu的元素粉末,采用机械合金化的方法在转速为400 r/min、球料质量比20:1的条件下制备具有非晶结构的Zr50Al15 Ni10Cu25粉末,研究其非晶化机制。用X射线衍和扫描电镜分析粉末的结构、晶粒尺寸和形貌。结果表明:在球磨8 h后可使Zr50Al15 Ni10Cu25混合粉末非晶化,晶粒尺寸约80 nm;球磨过程中并没有出现任何过饱和固溶体或者中间合金相,非晶化过程是由于球磨过程中球磨罐和磨球对粉末的不断冲击、剪切、摩擦和挤压,使混合粉末中的晶粒极度细化而直接转变为非晶态颗粒,得到非晶粉末。     

Laves相Cr2Nb元素混合粉末的机械合金化

对Laves相Cr2Nb化学配比成分的元素混合粉末的机械合金化行为进行了研究.结果表明,在机械合金化过程中,Cr、Nb元素混合粉末首先变成复合粉末,复合粉末中的成分逐渐均匀并演变成过饱和固溶体.机械合金化40h后过饱和固溶体发生部分非晶化.粉末颗粒尺寸在机械合金化初期的5h内粗化,随后逐渐细化,50h后细至亚微米级.在50h的机械合金化过程中始终未发现Laves相Cr2Nb的合成.但15h的机械合金化粉末在900℃的较低温度下通过固相热反应合成出了Laves相Cr2Nb,而未球磨的原始粉末在此温度下未能合成.这说明机械合金化虽然没有直接合成出Laves相Cr2Nb,但产生了活化Laves相高温反应合成的效果,使合成反应温度显著降低.     

Effect of Mn on the Microstructure and Magnetic Properties in Cu-Fe-Co Alloys

An attempt was made to study the effect of Mn addition on the formation of supersaturated solid solution of Co and Fe in Cu during ball milling and precipitation of the solute-rich phases during subsequent annealing of the ball-milled product. It is demonstrated that the addition of Mn in the ternary CuFeCo powder blend enhances the metastable solubility of Fe and Co in Cu and facilitates the formation of the nanocrystalline supersaturated single-phase solid solution. Field emission–scanning electron microscopy (FE-SEM) also revealed notable influence of Mn on the morphological evolution of the ball-milled and annealed alloy powders. X-ray diffraction (XRD) analysis revealed that the FeCo phase having the bcc Bravais lattice forms after annealing at and above 620 K (350 °C) in both alloys. Estimation of magnetic properties showed that Mn addition in the CuFeCo alloy improved the coercivity, remanence, and magnetic saturation.     

Microstructure investigations of ball milled materials

HREM and FEG TEM were emphasized and extensively used to follow the most subtle changes in the structure and composition of ball-milled Cu, Fe-Cu, and thermally decomposed Fe60Cu40. Some significant results are obtained and summarized as follows: HREM shows that the deformation of ball-milled copper proceeds mainly by twinning and shear bands (SBs) formation. The nano-grains formed during ball milling (BM) contain a high density of dislocations. The grain boundaries (GBs) of nanocrystalline (NC) Cu prepared by BM are ordered, curved, and strained, but disordering, lattice distortion, and nanovoids in local regions were frequently observed. Nanoscale composition analysis on mechanically alloyed Fe16Cu84 shows that the average Fe content in both the interior of grains and the GBs is close to the designed composition, which proves that a supersaturated solid solution has really formed. However, the Fe content is rather inhomogeneous between the larger and smaller grains, which infers the inhomogeneous mixing of Fe and Cu during mechanical alloying (MA). NC structure and the mechanical force-enhanced fast diffusion are the reasons of the formation of supersaturated solid solutions in immiscible systems with positive enthalpy of mixing. HREM observations carried out with the thermally decomposed Fe60Cu40 solid solution show that the Nishiyama (N-W) or Kurdyumov-Sachs (K-S) orientation relationships exist between alpha-Fe and Cu. Energy dispersive X-ray spectra (EDXS) results show that the Cu content in these alpha-Fe grains reaches as high as 9.5 at.% even after heating to 1,400 degrees C, which is even higher than the maximum solubility of Cu in gamma-Fe at 1,094 degrees C.     

Study of aged Mg-Sm alloys subjected to severe plastic deformation

The effect of severe plastic deformation by high-pressure torsion on the structure and properties of aged magnesium alloys containing 2.8–5.5 wt % Sm (the maximum solubility of samarium in solid magnesium is 5.8 wt %) are studied. The severe plastic deformation leads to substantial strengthening caused by the formation of a submicrocrystalline structure along with strengthening caused by the decomposition of a supersaturated magnesium-based solid solution.     

Microstructural characterization of rapidly solidified Al-Ta alloys

Two Al-rich Al-Ta alloys containing by weight 3 and 6 pct Ta have been rapidly solidified from the melt using the ‘gun’ technique. The microstructures and the crystal structures of the phases in the as-solidified as well as those formed on subsequent decomposition of the supersaturated solid solution have been characterized. A supersaturated solid solution was obtained in both the alloys in the as-solidified condition indicating a solid solubility extension of Ta in Al to almost 6 wt pct. The supersaturated solid solutions formed in both the alloys have been found to be quite stable up to 673 K (for 1 hour). Annealing at higher temperatures resulted in the formation of rod-shaped precipitates inside the grains and massive precipitates along grain boundaries. The rod-shaped precipitates arranged in a regular pattern constitute a new metastable intermediate phase Al₇Ta having an ordered structure. The massive precipitates which form along grain boundaries constitute the equilibrium Al₃Ta phase with a tetragonal crystal structure. The transformation behavior and the morphology of the transformation products are detailed in this paper.     

Metastable crystalline and amorphous structures formed in the Cu-W system by vapor deposition

The possibility of producing nonequilibrium amorphous and crystalline phases in the Cu-W system is of interest because, under equilibrium conditions, no mutual solubility is expected between Cu and W. Triode sputtered coatings (45 to 150 μm thick, produced at deposition rates between 20 and 150 Å/s) consisted of amorphous and metastable crystalline phases. The latter remained decomposition-resistant on heating to various temperatures between 340 °C and 600 °C (the maximum temperature of exposure). The amorphous phase in such coatings crystallized on heating into a metastable body-centered cubic (bcc) phase, and the crystallization temperatureT _x was found to decrease across the phase diagram from 450 °C to 340 °C as the percentage of W increased from 26 to 60 at. pct. Samples containing amorphous phase regions, when subjected to heating between 150 °C and 250 °C, showed an unusual rapid precipitation of Cu at the sample surface, indicating an easy diffusion of the Cu component. This occurred without crystallization of the remaining slightly tungsten-enriched amorphous matrix. Microhardness measurements in sputtered two-phase amorphous and bcc regions have shown that in alloys of the same composition, the amorphous phase was always softer than the bcc solid solution phase. X-ray, microprobe, and optical evidence suggests that the amorphous films deposited at very low temperatures(i.e., at liquid N₂) may subsequently undergo a phase separation upon heating to room temperature and prior to crystallization. Earlier work and present studies of vapordeposited alloys in this system confirm that the observed phases and microstructures can be related to free energy trends estimated from thermodynamic considerations and to specific deposition parameters, such as the substrate temperature and the deposition rates, which influence the kinetics.     

二元互不溶体系合金机械合金化的热力学研究进展

二元互不溶体系合金在机械合金化的非平衡态过程中能够形成过饱和固溶体、非晶和纳米相复合结构等亚稳相,并表现出与其微米尺度结构合金所不同的性能。综述了Alonso热力学模型和机械合金化在二元互不溶体系合金中制备亚稳相的热力学计算。     

Formation of amorphous and metastable extended solid solutions in Cu-Ti alloys using the triode sputtering technique

The triode sputtering technique and a split Cu-Ti target arrangement have been used to produce metastable extended solid solutions and amorphous phases in the Cu-Ti system. Metastable extension of the solid solubility of Ti in Cu-based fcc solid solution of up to 30 at. pct was observed; nearly 20 at. pct of Cu was incorporated metastably into the hcp solid solution based on Ti. Amorphous phase formation was observed in alloys containing approximately between 26 and 84 at. pct Ti. Amorphous deposits were as thick as 250 μm, without the presence of detectable crystalline phases. Interatomic spacings in both crystalline and amorphous alloys were found to follow an approximately linear trend with composition. Microhardness measurements indicated a very substantial increase in hardness in all alloys when compared with an extrapolated linear trend between pure Cu and Ti.     

STUDIES OF THE BINDER PHASE IN WC-Co CEMENTED CARBIDES HEAT-TREATED AT 650°C

Abstract

The binder phase of WC-Co cemented carbide is a Co-rich alloy in which tungsten and carbon are in solid solution. The binder phase is supersaturated with respect to tungsten even after slow cooling from the sintering temperature. In this study the binder phase contained 6% W in solid solution before heat-treatment at 650°C (923 K). Transmission electron microscopy on thin foils of binder phase showed that a finely dispersed. phase, α′, precipitated in the cubic binder phase. After long ageing times Co₃W could be identified by X-ray diffraction methods. As no discontinuous , ‘cells’ of Co₃W and ?-Co could be observed, the following reaction is suggested.

α-Co(W, C)→α-Co+α′→α-Co (C)+Co₃W (needles)

The precipitation of α′ was accompanied by an increase in hardness and a decrease in transverse rupture strength. The effects observed are consistent with those found during annealing of Co-rich cobalt-tungsten-carbon alloys (> 85% Co).     

Tribological and Mechanical Properties of Al(Cu)/MWCNT Nanocomposite Prepared by Mechanical Alloying and Hot Extrusion

The bulk Al–Cu-multiwall carbon nanotube (MWCNT) nanocomposite was prepared using mechanical alloying (MA) and hot extrusion processes. Al–4 wt % Cu powder mixture was first milled for 20 h to form the nanostructured Al(Cu) solid solution. The MWCNT was then added to the Al(Cu) powder mixture and further milled for 5 h. X-Ray Diffraction (XRD) and Differential Thermal Analysis (DTA) were performed to study the phase transformations during mechanical alloying and hot extrusion. Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) were also employed to study the samples microstructure. Mechanical properties of the bulk Al(Cu)/CNT nanocomposite were also studied using room and high temperature compression and wear tests. The results showed that after 20 h of mechanical alloying, a supersaturated Al(Cu) solid solution with the average grain size of 25 nm was achieved. Homogenous distribution of CNTs in the Al(Cu) supersaturated matrix was obtained. CNTs retained their tubular structure after 5 h milling time. Hot extrusion process at 550°C also led to the formation of bulk samples with nearly full density. The average yield and compressive strength of the Al(Cu)/CNT nanocomposite were found to be around 450 and 590 MPa at room temperature. The bulk nanocomposite showed suitable thermal stability by keeping its strength up to 300°C.