Cu和Ni对铁基合金玻璃形成能力及热稳定性的影响

利用X射线衍射（XRD）和差热分析（DSC）方法研究了Cu和Ni元素对Fe-（Al，Ga）-（P，C，Si，B）系合金非晶形成能力及热稳定性的影响。结果表明，含有少量Cu（小于2％，摩尔分数）的合金仍保持非晶态。由于Fe-Cu、Cu-Al之间的复杂作用影响了合金玻璃形成能力，使Al／Cu比值成为重要因素。而Ni含量小于4％（摩尔分数）时，则有利于合金的玻璃形成能力的提高和热稳定性的增加。     

热处理对两种铜膜结合强度的影响

采用PVD和CVD技术制备Cu/TiN/PI试样，研究表明，TiN薄膜可以有效地阻挡Cu向PI基板内部扩散，CVD工艺制备的Cu膜内部残余应力很小，Cu膜有相对高的结合强度；而PVD制备的Cu膜，在有TiN阻挡层存在的情况下，Cu膜内存在拉应力，拉应力降低了Cu膜结合强度，300℃退火可以消除膜内残余应力，结合强度提高。     

Thermal performance of sputtered Cu films containing insoluble Zr and Cr for advanced barrierless Cu metallization

Pure Cu films and Cu alloy films containing insoluble substances(Zr and Cr)were deposited on Si(100)substrates,in the presence of interfacial native suboxide(SiOx),by magnetron sputtering.Samples were vacuum annealed between 300℃and 500 ℃to investigate effects of Zr and Cr additions on the thermal performance of Cu films.After annealing,copper silicides were found in the Cu(Zr)films,while no detectable silicides were observed in Cu and Cu(Cr)films.Upon annealing,Zr accelerated the diffusion and reaction between the film and the substrate,and lowered the thermal stability of Cu(Zr)alloy films on Si substrates,which was ascribed to the‘purifying effect’of Zr on the Si substrates.Whereas,Cr prohibited the agglomeration of Cu films at 500℃and decreased the surface roughness.As a result,the diffusion of Cu in Si substrates for Cu(Cr)films was effectively inhibited.In contrast to the high resistivity of Cu(Zr)films,the final resistivity of about 2.76μΩ·cm was achieved for the Cu(Cr)film.These results indicate that Cu(Cr)films have higher thermal stability than Cu(Zr)films on Si substrates and are preferable in the advanced barrierless Cu metallization.     

纳米多孔铜制备及其电化学性能研究

通过真空熔炼和快速凝固技术制备了Cu-55Al(at%)合金铸锭和快淬薄带,用稀盐酸浸泡法对所得合金进行了化学脱合金。采用XRD、SEM和TEM等方法对脱合金前后的相组成及微观形貌进行了表征。结果表明,合金原始物相均由AlCu和Al2Cu相组成,快淬薄带中Al2Cu相含量更高。二者经脱合金后均能获得三维无序网状多孔铜,孔带平均尺寸分别为83、58 nm。此外,块体多孔铜中虽有少量Al残余,但孔带光滑完整。而合金薄带虽然能够完全脱Al,但孔带表面粗糙,并含有少量的Cu2O。电化学测试表明,多孔铜在碱性条件下电氧化甲醇的电流密度较光滑铜电极提高了25倍,同时还表现出优良的电容性能。     

Annealing effects on microstructure and properties of Ta-Al thin film resistors

The Ta-Al thin film resistor has been used as a heating element of the thermal bubble inkjet printhead with several millions of thermal cycle operations between room temperature and about 350 °C. In this paper, the thermal stability of Ta-Al alloy films was investigated by the variation of phase transformation, microstructure and resistivity at annealing temperatures of 450-650 °C for 1 h. Three kinds of Ta-Al films were prepared with average Ta/Al atomic composition ratios of about 2/1, 1/1 and 1/2, respectively. The Ta-Al film with composition ratio of about 1/1 exhibits amorphous-like microstructure with nanocrystalline grains embedded in an amorphous matrix. The thermal stability is strongly related to the composition and microstructure in Ta-Al alloy. The best thermal stability of Ta-Al films occurs in Ta-rich alloy up to 650 °C and the worst occurs in Al-rich alloy with phase transformation as low as 450 °C. The amorphous-like Ta-Al alloy is stable up to 550 °C, but then exhibits polycrystalline multiphase formation at 650 °C. The resistivity of Ta-Al films is also related to the annealing temperature. The resistivity of Ta-rich Ta-Al film increases to about 13.5% from as-deposited to after annealing at 450 °C while that is doubled in the Al-rich Ta-Al film. In contrast, the resistivity of the amorphous-like Ta-Al film increased by about 6.1% at 450 °C and then remains nearly stable at 1.5% variation on annealing at 450-550 °C. The as-deposited amorphous-like Ta-Al film has the merits of high resistivity, smooth morphology and good thermal stability at annealing temperatures of up to 550 °C. These attributes are beneficial for the thermal bubble inkjet application with thermal cycling at maximum temperatures below 400 °C.     

Corrosion behavior of Cu during graphene growth by CVD

The corrosion performance of Cu samples may be affected by annealing at high temperatures during graphene growth via the chemical vapor deposition method. In this study, multiple graphene films were deposited on Cu and characterized by Raman spectroscopy and transmission electron microscopy. The corrosion behavior of Cu immersed in 3.5 wt.% NaCl solution was investigated using electrochemical impedance spectroscopy. The Cu morphology was observed by optical microscopy and scanning electron microscopy. Results indicated that annealing affects the corrosion process of Cu. The presence of graphene films on the Cu substrate improved the corrosion performance of the material for a short period of time.     

并联导热结构的金刚石/铜基复合材料的制备

为提高金刚石/铜基复合材料的导热性能,在芯材表面预先化学气相沉积(CVD)高质量金刚石膜,获得柱状金刚石棒,再将其垂直排列,填充铜粉后真空热压烧结,制备并联结构的金刚石/铜基复合材料。分别采用激光拉曼光谱(Raman)与扫描电子显微镜(SEM)对CVD金刚石膜的生长进行分析,并通过数值分析讨论复合材料的热性能。结果表明:金刚石/铜基复合材料结构致密,密度为9.51g/cm3;CVD金刚石膜构成连续的导热通道,产生并联式导热,复合材料的热导率为392.78 W/(m·K)。     

Reaction thermodynamics and kinetics on in-situ Al2O3/Cu composites

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加热温度对淬火态Cu-Al合金电阻率的影响

采用电阻率测试仪研究了加热温度对淬火态Cu-Al合金电阻率的影响。结果表明,在25~380℃范围内,Cu-Al合金的电阻率随着温度的升高而增大;当温度从380℃升至473℃时,合金的电阻率变化不大,而随着温度的进一步升高电阻率再次增大。对上述合金电阻率随加热温度的变化进行了初步分析。     

Enhancement of the orientation and adhesion of Al films on LiNbO3 with Ni underlayer

1 Introduction Al films are widely used in surface acoustic wave (SAW) devices for mobile communication systems. In the SAW devices, the input electrical signals are transformed to SAW signals propagating on a piezoelectric substrate by interdigital elect…     

Layer Thickness-Dependent Hardness and Strain Rate Sensitivity of Cu–Al/Al Nanostructured Multilayers

Cu–Al/Al nanostructured metallic multilayers with Al layer thickness hAlvarying from 5 to 100 nm were prepared, and their mechanical properties and deformation behaviors were studied by nanoindentation testing. The results showed that the hardness increased drastically with decreasing hAldown to about 20 nm, whereafter the hardness reached a plateau that approaches the hardness of the alloyed Cu–Al monolithic thin films. The strain rate sensitivity(SRS, m),however, decreased monotonically with reducing hAl. The layer thickness-dependent strengthening mechanisms were discussed, and it was revealed that the alloyed Cu–Al nanolayers dominated at hAlB 20 nm, while the crystalline Al nanolayers dominated at hAl[ 20 nm. The plastic deformation was mainly related to the ductile Al nanolayers, which was responsible for the monotonic evolution of SRS with hAl. In addition, the hAl-dependent hardness and SRS were quantitatively modeled in light of the strengthening mechanisms at different length scales.     

热处理对铜铝低温钎焊的影响

研究了热处理温度和保温时间对低温钎焊Al/Sn-Bi/Cu接头强度的影响,采用光学显微镜和扫描电镜对接头界面显微组织和断口表面形貌进行了分析。结果表明,随着热处理温度的增加,焊接件的剪切强度表现出增加的趋势。随着热处理时间的增加,Al/Sn-Bi/Cu接头的剪切强度呈现出先增大后减小的趋势。钎焊时铜铝元素进入到钎焊层当中,主要以Cu-Al固溶体的形式存在,并随着热处理时间延长而聚集。热处理使钎缝内粗大的脆性Sn-Bi共晶组织变得细小且覆盖面积减小,从而增加接头强度,Cu-Al固溶体聚集和生长会降低接头强度。     

Role of Al2O3 layer in oxidation resistance of Cu-Al dilute alloys pre-annealed in H2 atmospheres

Copper was alloyed with small amounts of Al (0.2, 0.5, 1.0 and 2.0 mass%) to improve the oxidation resistance. Copper (6 N) and the Cu-Al alloys were oxidized at 773-1173 K in 0.1 MPa oxygen atmosphere after hydrogen annealing at 873 K. Continuous very thin Al₂O₃ layers were formed on the surface of all Cu-Al dilute alloys during the hydrogen annealing. Oxidation resistance of Cu-Al alloys was improved especially for Cu-2.0Al at 773-973 K, while it decreases on increasing the oxidation temperature. Cu-Al alloys followed the parabolic rate law at 1173 K, but most of other cases do not at and below 1073 K. Oxidation resistance for Cu-Al alloys was found relevant to the maintenance of the thin Al₂O₃ layer at the Cu₂O/Cu-Al alloy interface.     

Microstructure and thermal expansion of copper-based amorphous alloys during structural relaxation

(Cu43Zr48Al9)98Y2 amorphous alloy bar was prepared by the arc melting copper mold absorption casting method,and then,the amorphous alloy was annealed at different temperatures for different times.The influence of heating rate on thermal expansion and thermal stability was studied by thermomechanical analysis(TMA),and the microstructure evolution of the amorphous alloy during structural relaxation and crystallization was studied by XRD and TEM.Results show that the structural evolution behavior of the(Cu43Zr48Al9)98Y2 amorphous alloy can be divided into five different stages(structural relaxation preparation stage,structural relaxation stage,first crystallization stage,second crystallization stage,and grain growth stage).When the heating rate is 20 K/min,the amorphous alloy has the smallest thermal expansion coefficient and the best thermal stability.The width of the supercooled liquid region is 66.42 K.Samples with different relaxation states were prepared by annealing at the heating rate of 20 K/min.The structural evolution of amorphous alloys with different relaxation states is as follows:amorphous→CuZr2+AlCu2Zr7→CuZr2+AlCu2Zr7+CuZr(B2)+CuZr(M)+Cu10Zr7→CuZr2+AlCu2Zr7+CuZr(B2)+CuZr(M).After annealing at 706 K and 726 K(in the supercooled liquid region)for 1.5 h,the amorphous-nanocrystalline composites were obtained.When the annealing temperature is 706 K,the crystallization process of the sample is as follows:amorphous→Cu10Zr7→Cu10Zr7+CuZr,and for the sample at 726 K,it is as follows:amorphous→CuZr2+AlCu2Zr7+Cu10Zr7→Cu10Zr7+CuZr2→CuZr2+CuZr(B2)+Cu10Zr7.     

泡沫铜表面改性对化学气相沉积高质量泡沫金刚石的影响

目的选择合适的过渡层材料改善三维连通泡沫铜衬底与金刚石之间的结合性,制备出三维连通结构的泡沫金刚石。方法选择三维连通的泡沫铜作为衬底,使用磁控溅射技术在其表面沉积Ti、Cr过渡层,然后通过热丝化学气相沉积技术(HFCVD)在表面改性后的泡沫铜衬底上沉积金刚石涂层。通过扫描电子显微镜(SEM)、能谱分析仪(EDS)、拉曼光谱仪及红外热成像仪等仪器,对样品的表面/截面形貌、成分结构及热扩散性能进行检测与分析。结果经过Ti、Cr过渡层改性后,泡沫铜表面均能沉积出连续致密的高质量金刚石涂层,在相同的CVD沉积参数下,Cr过渡层泡沫金刚石(Cu-Cr/Dia)的晶粒尺寸更大(~5μm),晶粒质量更高,且膜层厚度大于Ti过渡层泡沫金刚石(Cu-Ti/Dia),Cu-Ti/Dia与铜衬底的结合性要优于Cu-Cr/Dia。Cu-Cr/Dia和Cu-Ti/Dia的热扩散性能均优于泡沫铜,其中Cu-Cr/Dia的热扩散能力略高于Cu-Ti/Dia。结论镀覆Ti、Cr过渡层有效增强了金刚石与泡沫铜衬底之间的界面结合,成功制备了三维连通结构的泡沫金刚石。     

Correlation between liquid structure and γ2-phase precipitation of Cu-Al-Ni shape memory alloys

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电弧离子镀方法制备的Ti/TiN多层膜的结构与耐腐蚀性能

采用电弧离子镀技术,通过周期性变换环境气氛,在7075Al合金上制备了Ti/TiN多层膜,并研究调制周期对多层膜的结构组成和腐蚀性能的影响。结果表明:多层膜与铝合金衬底界面结合较好,基本没有孔洞等缺陷。多层膜具有明显的层状特征,层间界面清晰。多层膜中TiN与单层中TiN薄膜有着相同的晶体结构,并存在(111)择优取向,每个调制周期内的TiN层都呈柱状生长。随着调制周期变小,多层膜阳极极化曲线的腐蚀电位增加,交流阻抗谱的阻抗值增大,容抗弧的半径也增大,即膜层的耐腐蚀性增加。多层膜调制周期的减小使得薄膜中含有的层界面增多,而贯穿至衬底表面的针孔等缺陷的数量将减少,这样,腐蚀性介质经过针孔等缺陷与衬底接触的机会变少,这将使薄膜的抗腐蚀能力得到改善。     

Reliability of anodic vacuum arc in depositing thermoelectric alloy thin films

Inductively coupled plasma optical emission spectrometry (ICP-OES) was applied for the analysis of major and minor elements of thermoelectric alloys (Constantan, Chromel and Alumel) and their thin films deposited using anodic vacuum arc (AVA) plasma deposition technique. Digestion of samples was done in aqua regia. The minor and trace elements were determined without matrix separation. The precision for all the constituents was <3%. The changes in the composition of these alloy films were studied as a function of number of deposition cycles and also with various positions of the samples on the substrate holder. Due to the difference in the evaporation rates of the alloy constituents and the interaction of Ni with the refractory basket, the AVA deposited films showed varying compositions in the initial cycles of deposition. However, a good agreement was obtained among the samples deposited on various positions of the substrate holder, suggesting a uniform plasma flux in the system. Films deposited using Constantan wires were much enriched with Cu. By depositing bilayers of Cu and Ni, followed by post annealing, we were able to produce films in which the Cu and Ni concentrations were similar to that of Constantan. A deviation of ∼15% was observed among 10 Cu films of thickness ∼300 nm deposited using this technique. AVA deposited films of Chromel and Alumel having Ni (≥90%) could be developed without much alteration in their composition.     

Relationship between the growth rate and Al incorporation of AlGaN by metalorganic chemical vapor deposition

The growth rate and its relationship with growth conditions of AlGaN alloy films by metalorganic chemical vapor deposition (MOCVD) are investigated. It is found that both parasitic reaction and competitive adsorption play important roles in determining the growth rate and Al incorporation in AlGaN. Low reactor pressure can weaken parasitic reactions, thus increasing the Al composition. In addition, a decrease of absolute amount of Ga atoms arriving on the substrate may lead to a lower Ga competitive power, and then a higher Al content in AlGaN film.     

Fe和Cu对6061再生铝合金凝固行为和热裂倾向的影响

利用双电偶热分析和约束杆模具热裂评价法,研究了Fe和Cu杂质元素对6061再生铝合金凝固特性和热裂倾向(HTS)的影响.结果表明,随着Fe和Cu元素含量的增加,再生铝合金的热裂倾向逐渐增大.Fe元素主要影响再生铝合金初期凝固行为,提高Al13Fe4富铁相的形核温度和含量,促使凝固过程中枝晶搭接完成,阻碍液相流动补缩.C...