基于铜铟微纳米层常温超声辅助瞬态固相键合技术

目的 采用针状形貌铜铟微纳米层和超声能量,在常温下实现键合互连,保证互连的可靠性,从而解决传统回流焊工艺因高温引发的高热应力、信号延迟加剧等问题。方法 将镀有铜铟微纳米层的基板表面作为键合偶,对键合接触区域施加超声能量和一定压力,实现2块铜铟基板的瞬态固相键合。用扫描电子显微镜、透射电子显微镜、X射线衍射(XRD)、焊接强度测试仪等分析键合界面处的显微组织、金属间化合物及剪切强度,并对键合界面进行热处理。结果 在超声作用和较小的压力下,铜铟微锥阵列结构相互插入,形成了稳定的物理阻挡结构。键合界面处的薄铟层在超声能量作用下,其原子快速扩散转变为金属间化合物Cu2In。Cu2In是一种优质相,具有良好的塑性,有利于提高互连强度。当键合界面铟层的厚度为250 nm,键合压力为7 MPa,键合时间为1 s时,获得了相对最佳的键合质量,同时键合界面孔洞消失。热处理实验结果表明,这种固相键合技术无需额外进行热处理,就能获得良好的键合强度。结论 铜铟微纳米针锥的特殊形貌及超声波能量的引入,使键合在室温条件下即可瞬间完成,键合质量良好,可以获得较小的键合尺寸。     

Sn-1.5Ag-2Zn低银无铅焊料与取向铜界面研究

目的 高密度封装技术能减少焊盘尺寸和焊盘里面所含晶粒的数量,当多晶焊盘转为单晶焊盘时,晶粒的取向会对界面处金属间化合物的形成产生重要影响。选取具有发展前景的Sn-1.5Ag-2Zn作为焊料合金,研究焊料与单晶(111)铜基板界面反应,得到金属间化合物的生长动力学规律。方法 将Sn-1.5Ag-2Zn无铅焊料分别与单晶(111)铜基板及多晶紫铜基板在250 ℃下进行回流焊接5 min,将焊接后的样品在160 ℃下分别进行20 h,100 h,300 h,600 h热处理。用扫描电子显微镜背散射电子成像和二次电子成像、X射线衍射仪(XRD)、能谱仪等研究焊接界面处的显微组织、金属间化合物成分以及性能。结果 合金焊料与铜基板接触迅速生长出凹凸不平类似扇贝状Cu6Sn5金属间化合物层,与单晶铜表面形成的Cu6Sn5晶粒尺寸比多晶铜的大,单晶铜无晶界阻挡原子扩散,影响晶粒形核与长大。合金焊料与单晶(111)铜焊点在160 ℃下热处理20 h快速形成的Cu6Sn5生长速度是多晶铜上焊点的2倍左右。而后随热处理时间增加增长缓慢,热处理600 h后厚层Cu6Sn5由于裂纹扩散出现溃断,金属间化合物的厚度维持在3.5 µm。焊料与多晶铜焊点在热处理过程中生成的Cu5Zn8起到阻挡层的作用,阻挡焊料与铜基板接触,抑制Cu6Sn5生成,热处理300 h后Cu5Zn8破碎分解,Cu6Sn5在阻挡层消失后快速生长,厚度约为2.8 µm。结论 单晶铜上焊点金属间化合物的厚度比多晶铜上金属间化合物的厚度多0.7 µm,热处理后合金焊料与单晶铜界面形成的金属间化合物致密性更好,基本没有孔隙,而合金焊料与多晶铜界面上金属间化合物晶粒间存在明显孔隙,可以预测合金焊料与单晶铜界面的焊接质量更好。     

三维封装芯片Cu-In体系固液互扩散低温键合机理研究

芯片封装已经迈入3D封装的时代,固液互扩散键合法(Solid Liquid Inter diffusion Bonding,SLID)以其独有的优势成为芯片互连中的很有发展前景的一种方法。SLID键合采用低温钎料锡或铟,在较低温度下就可键合,并且由于焊点尺寸小,键合后全部由金属间化     

微小互连高度下的电子封装焊点微观组织

研究了互连高度分别为100,50,20,lOμm四种不同互连高度的铜／锡／铜三明治结构微焊点的微观组织变化．结果表明,随互连高度的降低,焊料层中的铜浓度也随之升高,焊点两侧生成的Cu6Sn5金属间化合物层（intermetallic compound,IMC）厚度随之降低,但其所占焊点的比例却升高．根据IMC层厚度和焊...     

Sn-Ag-Cu无铅焊料及焊点在低温下组织和性能

为保证锡银铜合金及焊点在低温环境下使用可靠性,将SnAg3.0Cu0.5合金焊料和焊点在25、4、-20和-60℃恒温环境中进行储存565 d后,考察不同温度下SnAg3.0Cu0.5无铅焊料微观组织和物相变化,对经冷储存后SnAg3.0Cu0.5/Cu焊接接头进行拉伸强度和低周疲劳测试。结果表明,焊料经低温储存后没有发生灰锡转变,合金主要由Ag3Sn和β-Sn组成,组织形貌转变为树枝状组织,排列具有一定取向,β-Sn相晶面间距变小,焊料出现低温脆性倾向;随储存温度降低,SnAg3.0Cu0.5焊料与Cu基板互连结构的断裂界面从焊料侧向铜基体方向移动,焊缝的抗拉强度随之下降;在恒幅对称应变条件下,疲劳极限-循环次数曲线的斜率随焊件储存温度降低而变大,焊接接口的抗疲劳性能变差。     

USB3.1 Type C超声辅助钎焊焊接性研究

采用自制的SnXX无铅钎料代替生产中常用的SnBi钎料,并分别采用超声波辅助钎焊技术和常规钎焊技术实现USB3.1 Type C中的铜导线和铜端子的可靠焊接互连,以阐明新型超声辅助钎焊技术在数据线连接领域内的优越性。焊后PIN位焊点锡点饱满,PIN位的前端未见未融的锡膏,焊杯界面无过多的锡珠。焊点横截面宏观形貌呈圆滑过渡,界面结合良好并形成Cu_6Sn_5化合物,无宏观缺陷,良品率较高。     

低碳铁素体钢渗氮层在3.5%NaCl溶液中腐蚀行为研究

研究了高温与低温条件下低碳铁素体钢气体渗氮后渗氮层组织形貌的区别,并分析高温渗氮过程中在渗氮层与基板界面处黑色过渡层产生的原因;同时,研究渗氮层在3.5%NaCl溶液浸泡的腐蚀行为。结果表明:高温渗氮(≥592℃)时,渗氮层中白亮层与基板处会形成20μm左右含氮马氏体过渡层,低温(592℃)时渗氮未出现该组织。在腐蚀过程中,腐蚀液易从渗氮层孔洞以及裂纹流入,使渗氮层整体脱落或者局部孔洞连接成片层状脱落。     

先进封装中铜-铜低温键合技术研究进展

Cu-Cu低温键合技术是先进封装的核心技术,相较于目前主流应用的Sn基软钎焊工艺,其互连节距更窄、导电导热能力更强、可靠性更优. 文中对应用于先进封装领域的Cu-Cu低温键合技术进行了综述,首先从工艺流程、连接机理、性能表征等方面较系统地总结了热压工艺、混合键合工艺实现Cu-Cu低温键合的研究进展与存在问题,进一步地阐述了新型纳米材料烧结工艺在实现低温连接、降低工艺要求方面的优越性,概述了纳米线、纳米多孔骨架、纳米颗粒初步实现可图形化的Cu-Cu低温键合基本原理. 结果表明,基于纳米材料烧结连接的基本原理,继续开发出宽工艺冗余、窄节距图形化、优良互连性能的Cu-Cu低温键合技术是未来先进封装的重要发展方向之一.     

纳米Ti颗粒对三维封装Sn互连材料组织与性能影响

Sn作为三维封装芯片堆叠瞬时液相键合主要互连材料之一,本文研究了纳米Ti颗粒对三维封装Sn互连材料组织和性能的影响。结果表明：微量的纳米Ti颗粒可以提高Sn膏在铜基板表面的润湿铺展面积,显著增加Sn焊点的拉伸力和剪切力,但是过量的Ti纳米颗粒会恶化焊点的力学性能。基于Ti纳米颗粒含量优化分析证实纳米Ti颗粒的最佳添加量为0.1wt.%左右。对Cu/Sn/Cu和Cu/Sn-0.1Ti/Cu三维封装模拟件进行分析,发现Cu/Sn-0.1Ti/Cu焊点界面金属间化合物的厚度明显小于Cu/Sn/Cu,证实0.1wt.%可以显著降低金属间化合物的生长速度。 基于有限元模拟,发现0.1wt.%Ti可以显著降低三维封装互连焊点的应力-应变,提高三维封装互连焊点的可靠性。     

金锡镀层在CSP气密封装中的应用及其可靠性

芯片级尺寸封装的气密性被越来越广泛的关注，为了实现CSP器件的可伐管帽与陶瓷基板之间的气密性互连，采用分层电镀沉积的方法在高温共烧陶瓷(HTCC)基板表面制备了金/锡/金镀层，利用金与锡间的共晶反应以实现管帽和基板的气密性可靠封接.文中分析了金/锡/金镀层质量、焊接工艺对Au80Sn20共晶焊料封接结果的影响.结果表明，金/锡/金镀层厚度和层间的结合力决定了Au-Sn共晶焊料的封接质量.在焊接升温过程中，锡镀层首先熔化形成“熔池”，溶解上下侧与之接触的金镀层，直至完成共晶反应；采用较短的焊接时间能够实现更好的金锡共晶封接；焊接温度为330℃、保温时间为30 s时，Au-Sn镀层共晶反应形成δ/(Au,Ni)Sn—ζ相—δ/(Au,Ni)Sn的分层共晶组织，实现了可伐管帽与HTCC基板的气密性封接.     

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.     

新型的治疗阿尔茨海默氏症药物(1-二甲基磷酰基-2,2,2-三氯)-乙基-1-醇烟酸醋对体外神经细胞的作用

目的: 观察本实验室合成的一种治疗阿尔茨海默氏症(AD)的药物(1-二甲基磷酰基-2, 2, 2 -三氯)-乙基^-1-醇烟酸醋(NMF),对体外培养的皮层神经细胞活性的影响以及对海人藻酸(KA)所致的神经损伤的保护作用。方法: 采用体外培养皮层神经元的方法,解剖分离 15 d胚胎小鼠皮层神经细胞, 接种于 96孔板,48 h 后加药并培养 72 h,以 MIT 法 观察 NMF 对小鼠皮层神经细胞活性的影响;同时将接种于 24 孔板的细胞预先给予 NMF,d 3 时加或不加KA处理后,以台盼蓝染色鉴别并计数死、活细胞,可得出细胞的存活率。结果: NMF 明显促进胎鼠皮层神经元活性,其中 NMF1、0. 1、10nmol·L^-1促进神经元活性增殖率分别高达 34.7%、37.4%、36. 7%, NMF 明显促进正常胎鼠皮层神经元存活卒,与对照组比较,10nmol·L^-1 NMF 对皮层神经元的存活率分别提高 39.3%、73.5%。 NMF能显著 对抗 KA 所致的神经元损伤,与 KA 损伤组相比, NMF0.1、10、10nmol·L^-1对损伤皮层神经元的保护率分别为 77.30%、80.10%、84.15%。结论: NMF 明 显促进胎鼠皮层神经元的洁性、提高正常皮层神经元,的存活卒,并能有效地保护KA所致的神经元损伤,提示 NMF 是一种很有潜力的治疗 AD 的药物。     

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).     

Three-Dimensional Growth of Coherent Ferrite in Austenite: A Molecular Dynamics Study

Coherent second phase often exhibits anisotropic morphology with specifi c orientations with respect to both the second and the matrix phases. As a key feature of microstructure, the morphology of the coherent particles is essential for understanding the second-phase strengthening eff ect in various industrial alloys. This letter reports anisotropic growth of coherent ferrite from austenite matrix in pure iron based on molecular dynamics simulation. We found that the ferrite grain tends to grow into an elongated plate-like shape, independent of its initial confi guration. The fi nal shape of the ferrite is closely related to the misfi t between the two phases, with the longest direction and the broad facet of the plate being, respectively, consistent with the best matching direction and the best matching plane calculated via the Burgers vector content(BVC) method. The strain energy calculation in the framework of Eshelby's inclusion theory verifi es that the simulated orientation of the coherent ferrite is energetically favorable. It is anticipated that the BVC method will be applicable in analysis of anisotropic growth and morphology of coherent second phase in other phase transformation systems.     

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.