Low‐Temperature Eutectic Synthesis of PtTe2 with Weak Antilocalization and Controlled Layer Thinning

Metallic transition metal dichalcogenides (TMDs) have exhibited various exotic physical properties and hold the promise of novel optoelectronic and topological devices applications. However, the synthesis of metallic TMDs is based on gas‐phase methods and requires high‐temperature condition. As an alternative to the gas‐phase synthetic approach, lower temperature eutectic liquid‐phase synthesis presents a very promising approach with the potential for larger‐scale and controllable growth of high‐quality thin metallic TMD single crystals. Here, the first realization of low‐temperature eutectic liquid‐phase synthesis of type‐II Dirac semimetal PtTe₂ single crystals with thickness ranging from 2 to 200 nm is presented. The electrical measurement of synthesized PtTe₂ reveals a record‐high conductivity of as high as 3.3 × 10⁶ S m⁻¹ at room temperature. Besides, the weak antilocalization behavior is identified experimentally in the type‐II Dirac semimetal PtTe₂ for the first time. Furthermore, a simple and general strategy is developed to obtain atomically thin PtTe₂ crystal by thinning as‐synthesized bulk samples, which can still retain highly crystalline and exhibits excellent electrical conductivity. The results of controllable and scalable low‐temperature eutectic liquid‐phase synthesis and layer‐by‐layer thinning of high‐quality thin PtTe₂ single crystals offer a simple and general approach for obtaining different thickness metallic TMDs with high melting‐point transition metal.     

低熔点高Δn值双环向列相液晶的合成研究

为了获得低熔点、折射率各向异性(Δn)大的快速响应向列相液晶材料,高Δn值的液晶混合体系中需要加入熔点在50℃以下、Δn大于0.35的双环类液晶组分,以使快速响应向列相液晶材料满足室温工作的要求。本文合成了异硫氰基含氟二苯乙炔类液晶化合物;一方面由于在分子苯环侧位引入F原子,减小分子间作用力,使化合物的熔点下降;另一方面在两个苯环间引入三键、分子末端接入异硫氰基极性基团,增加了分子的共轭性,提高了目标化合物的Δn值。获得了熔点分别为31℃和50℃、Δn为0.39和0.40,这两种低熔点化合物与目前已具有的毫秒级快速响应向列相液晶化合物混合,可使其熔点低至10℃以下。     

High performance room temperature nematic liquid crystals based on laterally fluorinated isothiocyanato-tolanes

High birefringence and low viscosity isothiocyanates liquid crystal single compounds and eutectic mixtures, based solely on laterally fluorinated aromatic rigid core structures, are reported. Extraordinarily high values of figure-of-merit were observed at room temperature and also elevated temperatures for the nematic mixtures we formulated. Potential applications of such mixtures for laser beam steering at /spl lambda/=1.55 /spl mu/m using optical phased arrays are emphasized.     

A new COG technique using low temperature solder bumps for LCD driver IC packaging applications

A new chip on glass (COG) technique using flip chip solder joining technology has been developed for excellent resolution and high quality liquid crystal display (LCD) panels. The flip chip solder joining technology has several advantages over the anisotropic conductive film (ACF) bonding technology: finer pitch capability, better electrical performance, and easier reworkability. Conventional solders such as eutectic Pb-Sn and Pb-5Sn require high temperature processing which can lead to degradation of the liquid crystal or the color filter in LCD modules. Thus it is desirable to develop a low temperature process below 160/spl deg/C using solders with low melting temperatures for this application. In our case, we used eutectic 58 wt%Bi-42 wt%Sn solder for this purpose. Using the eutectic Bi-Sn solder bumps of 50-80/spl mu/m pitch sizes, an ultrafine interconnection between the IC and glass substrate was successfully made at or below 160/spl deg/C. The average contact resistance of the Bi-Sn solder joints was 19m/spl Omega/ per bump, which is much lower than the contact resistance of conventional ACF bonding technologies. The contact resistance of the underfilled Bi-Sn solder joints did not change during a hot humidity test. We demonstrate that the COG technique using low temperature solder joints can be applied to advanced LCDs that lead to require excellent quality, high resolution, and low power consumption.     

Development of a solder material process to relieve the plastic constraint associated with thin joints

High aspect ratio (large diameter/thickness) solder joints which are plastically constrained develop large hydrostatic stresses (Friction Hill) greatly in excess of their yield strength. Because the local high triaxial stresses arising from the Friction Hill prevent homogeneous yielding and, in a strain controlled system, will localize plastic deformation within the regions near free surfaces, abrupt brittle fracture through an intermetallic or along an interface can occur. In such situations, the service life of the joint during fatigue situations such as thermal cycling will be greatly reduced. The prevention of triaxial stress build up within such a strain controlled environment which can occur in, for example, leadless chip carrier solder joints requires a distribution of internal free surfaces within the joint. The solder system developed in this study is a thin porous metal film with a regular distribution of pores. The solder material is formed from the usual components, tin and lead. Small lead or tin particles are coated with a thin film of the other component, mixed with flux paste, and the temperature is raised to just above the eutectic temperature. Solid state diffusion occurs across the lead-tin interface until its composition reaches the melting point. The particles then are interconnected by a thin near eutectic liquid film. Additional metal from the solid particle dissolves into the liquid increasing its position and, thus its melting point. Diffusion into the liquid continues until it solidifies isothermally. This forms an interconnecting network of solder “mini-elements” with a dense pore structure.     

Reaction of solder with Ni/Au metallization for electronic packagesduring reflow soldering

Gold over Ni is one of the most common surface finishes for Cu soldering pads in ball-grid-array (BGA) and other electronic packages. The Au layer is for oxidation protection, and the Ni layer serves as a solderable diffusion barrier. In this study, eutectic Pb-Sn solder-balls were reflowed on the Au/Ni/Cu pads, and the chemical interactions between the solder and the surface finish were studied. Quenched-in microstructures at different stages of the reflow were carefully examined using the scanning electron microscopy. It was found that the solder melted locally along the solder/pad interface at the very early stages of the reflow before the whole solder ball had reached the Pb-Sn eutectic temperature. This was because a ternary eutectic reaction L=(Pb)+(Sn)+AuSn₄ occurred at 177°C, six degrees below the Pb-Sn eutectic temperature. Four distinct stages were identified for the reflow process. The four stages are: (1) partial melting of solder balls and the initial reaction of Au with Sn; (2) complete reaction of An with Sn; (3) separation of (Au_xNi_1-x)Sn₄ from the pad; (4) complete melting of solder balls and the reaction of Ni with Sn. After a typical reflow, with a 225°C peak reflow temperature and 115 s reflow time, all the An and Au-bearing intermetallic compounds left the interface and the only intermetallic compound at the interface was Ni₃Sn₄ with a thickness of about 2 μm     

激光快速成形Rene 80高温合金组织及裂纹形成机理

研究了激光快速成形(LRF)Rene 80高温合金厚壁件的凝固组织和裂纹的形成机理。结果表明,激光快速成形Rene 80高温合金的凝固组织为与沉积高度方向平行的定向凝固枝晶组织,由于凝固偏析,MC型碳化物和γ-γ′共晶组织分布于定向凝固组织的枝晶间区域。激光快速成形Rene 80高温合金厚壁件含有许多长度大于10mm,扩展方向与沉积高度方向平行的宏观裂纹。分析表明,这些裂纹为液化裂纹,其形成原因为:激光快速成形时,紧邻激光熔池的热影响区(HAZ)内沿晶界分布的低熔点γ-γ′共晶组织发生熔化,形成热影响区内沿晶界扩展的晶界液相,在热影响区冷却过程中,由于热影响区内固相的收缩应力作用,沿晶界扩展的固-液界面被撕开,从而导致液化裂纹的产生。     

Microstructure and mechanical properties of Pb-free solder alloys for low-cost electronic assembly: A review

Lead-free solders, including Sn-58Bi, Sn-52In, and Sn-3.5Ag, are potential replacements for Sn-37Pb solder in low-cost electronic assembly. This paper reviews the literature on the microstructure and mechanical properties of these alloys. Because of the processing and testing conditions, many of the data are not predictive for electronic assembly applications. However, eutectic Sn-Bi seems to have properties approaching those of eutectic Sn-Pb under most conditions, while eutectic Sn-In seems far inferior in most respects. Eutectic Sn-Ag has many promising characteristics, but its relatively high melting temperature may preclude its use for this type of application.     

Forming high temperature solder joints through liquid phase sintering of solder paste

Eutectic lead-tin has been the solder of choice throughout the history of the electronics industry. Alternatives to this material are now being considered because of environmental concerns, as well as the strength and temperature limitations of eutectic lead-tin. Identifying and using these alternative materials poses significant challenges, many of which we believe can be addressed if one forms solder joints through liquid phase enhanced sintering. First, most alternative solder materials have significantly higher melting temperatures (than eutectic lead-tin), and their use would require the replacement of much of the manufacturing infrastructure. In this work joints with shear stresses approaching that of eutectic lead-tin solder were formed by sintering a eutectic tin-sliver solder paste (T_m=221°C) doped with 3 v/o eutectic Sn-Bi powder at 210°C for 30 min. Second, to date the industry has limited its consideration to eutectic or near-eutectic alloys because of the concern of forming cold solder joints. In this work joints have been prepared by sintering solder pastes with a wide thermal range at temperatures just above the solidus, where a small amount of liquid will form and therefore enhance the rate of sintering, which have shear strengths of 6 MPa or higher. These findings indicate that it may be worthwhile to investigate developing a sinterable solder paste, which can be used to prepare surface mount assemblies.     

Experimental characterization of the mechanical behavior of two solder alloys for high temperature power electronics applications

An experimental investigation of two potential candidate materials for the diamond die attachment is presented in this framework. These efforts are motivated by the need of developing a power electronic packaging for the diamond chip. The performance of the designed packaging relies particularly on the specific choice of the solder alloys for the die/substrate junction. To implement a high temperature junction, AuGe and AlSi eutectic alloys were chosen as die attachment and characterized experimentally. The choice of the AlSi alloy is motivated by its high melting temperature T_m (577 °C), its practical elaboration process and the restrictions of hazardous substances (RoHS) inter alia. The AuGe eutectic solder alloy has a melting temperature (356 °C) and it is investigated here for comparison purposes with AlSi. The paper presents experimental results such as SEM observations of failure facies which are obtained from mechanical shear as well as cyclic nano-indentation results for the mechanical hardening/softening evaluation under cyclic loading paths.     

Catalytic Metal Foam by Chemical Melting and Sintering of Liquid Metal Nanoparticles

Metal foams are highly sought‐after porous structures for heterogeneous catalysis, which are fabricated by templating, injecting gas, or admixing blowing agents into a metallic melt at high temperatures. They also require additional catalytic material coating. Here, a low‐melting‐point liquid metal is devised for the single‐step formation of catalytic foams in mild aqueous environments. A hybrid catalytic foam fabrication process is presented via simultaneous chemical foaming, melting, and sintering reaction of liquid metal nanoparticles. As a model, nanoparticles of tertiary low‐melting‐point eutectic alloy of indium, bismuth, and tin (Field's metal) are processed with sodium hydrogen carbonate, an environmentally benign blowing agent. The competing endothermic foaming and exothermic sintering reactions are triggered by an aqueous acidic bath. The overall foaming process occurs at a localized temperature above 200 °C, producing submicron‐ to micron‐sized open‐cell pore foams with conductive cores and semiconducting surface decorations. The catalytic properties of the metal foams are explored for a range of applications including photo‐electrocatalysis, bacteria electrofiltration, and CO₂ electroconversion. In particular, the Field's metal‐based foams show exceptional CO₂ electrochemical conversion performance at low applied voltages. The facile process presented here can be extended to other low‐temperature post transition and transition metal alloys.     

含氟三苯二炔类液晶化合物合成及其性质研究

目前,越来越多的液晶应用要求向列相液晶材料具有高双折射率性能。本文合成了5个高双折射率含氟三苯二炔类液晶化合物(Ⅳ),经过IR,1 H NMR,13 C NMR谱图鉴定,这些化合物的分子结构完全正确;通过DSC和POM对其液晶相态测试的实验结果表明该类液晶化合物具有较低的熔点和相对较宽的向列相温度范围(达到100℃左右);对其折光率测试结果表明这些液晶化合物的双折射率(Δn)值在0.47以上,改善液晶光学性能。     

Interconnections based on Bi-coated SnAg solder balls

To decrease the bonding temperature required for eutectic SnAg solder, SnAg solder bumps were chemically coated with a pure Bi layer. During heating, a low melting eutectic forms between the Bi coating and the SnAg, enabling bonding at temperatures below the melting points of either pure Bi or SnAg solder. As the composition of the molten solder changes toward more dilute Bi concentrations, the melting point in the joint region increases and the joint solidifies. After solidification the joints will no longer melt at the original bonding temperature. Bi-coated SnAg solder balls were joined to metallized substrates at temperatures ranging from 180°C to 250°C. The microstructure at the joint interface was characterized by the SEM/EDS technique. As expected, at 180°C the Bi-coated SnAg solder balls melted only locally at the interfacial regions between the ball and the substrate and so retained their spherical shape during bonding. After solidification there were a lot of small Bi precipitates in the joint region. At higher temperatures, the wetting was evidently better, and there were less Bi precipitates, because the melt was more dilute in bismuth. In all cases, Bi formed relatively small, equi-axed precipitates instead of the eutectic structure found in eutectic Sn-Bi solder joints     

进口AuSn20焊料环特性及焊缝化合物分析

AuSn20焊料环是高可靠密封工艺中一种常用的密封材料,采用差示扫描量热法对进口AuSn20焊料环进行熔化和凝固温度的检测,探明其熔化温度为280℃,凝固温度为277℃,AuSn20焊料环纯度很高几乎无杂质.通过对进口和国产AuSn20焊料环的表面状态形貌进行对比,发现均为AuSn和Au5Sn的均匀分布状态,未见明显区...     

Local melting induced by electromigration in flip-chip solder joints

A new electromigration failure mechanism in flip-chip solder joints is reported. The solder joints failed by local melting of a PbSn eutectic solder. Local melting occurred due to a sequence of events induced by the microstructure changes in the flip-chip solder joint. The formation of a depression in the current-crowding region of a solder joint induced the local electrical resistance to increase. The rising local resistance resulted in a larger Joule heating, which, in turn, raised the local temperature. When the local temperature rose above the eutectic temperature of the PbSn solder, the solder joint melted and consequently failed. The results of this study suggest that a dynamic, coupled simulation that takes into account the microstructure evolution, current density distribution, and temperature distribution may be needed to fully solve this problem.     

Determination of Average Failure Time and Microstructural Analysis of Sn-Ag-Bi-In Solder Under Electromigration

Despite the extensive use of Sn-Ag-Cu as a Pb-free solder alloy, its melting point is significantly higher than that of eutectic Sn-Pb solder. Sn-Ag-Bi-In solder is an alternative Pb-free solder, with a melting temperature close to that of eutectic Sn-Pb. This study elucidates the electromigration behavior of Sn-Ag-Bi-In solder and then compares the results with those of the Sn-Ag-Bi system. The behavior of Pb-free Sn-Ag-Bi-In solder strips under electromigration is examined by preparing them in Si (001) U-grooves. The samples are then tested under various temperatures and current densities. Although the compounds thicken near both electrodes with current stressing, the thickness at the anode exceeds that at the cathode. Experimental results of the average failure time indicate that Sn-Ag-Bi-In solder has a longer lifetime than does Sn-Ag-Bi, which is attributed to the ζ phase. Additionally, the ζ phase dissolved by the current in the early stage replenishes the outgoing atomic flux. These atomic fluxes also enhance the growth of abnormally large particles in the middle of the strips. Field-emission electron probe microanalysis (FE-EPMA) results indicate that the amount of indium is reduced after the ζ phase near the cathode is exhausted for extended current stressing time.     

Low temperature FIB cross section: Application to indium micro bumps

This paper presents the interest of low temperature FIB cross section on indium micro bump. Experimental setup and results which demonstrate the interest of cooling the sample are detailed. We will explain the artefacts observed during FIB milling at room temperature. The Ga ions interact with indium to create locally an eutectic alloy, with melting point below room temperature. Inside the vacuum chamber, this eutectic alloys sublimates quickly and voids appear in the cross section. Cooling the sample with cryogenic stage enables to perform “clean” cross section without these artefacts.     

选区激光熔化成形Al-Si合金及其裂纹形成机制研究

为了得到性能良好的Al-Si合金零件,对选区激光熔化成形Al-Si合金的成形特性以及成形试样中裂纹进行了研究,得到了成形样致密度和工艺参量的关系以及裂纹的形成机制。在合适的工艺区间内,随着激光能量密度的增大,致密度先上升后下降;大部分试样底部存在沿熔覆层扩展的冷裂纹;其形成机制是Al-Si合金粉末成形过程中,生成大量共晶Si相,使材料的抗裂性能不足以抵抗成形过程中的高温度梯度导致的残余应力所致。结果表明,通过调整成形工艺参量,可以得到无裂纹的性能良好的成型零件。     

乙炔桥键四环异硫氰酸酯液晶化合物的合成及性能

为了研究液晶材料结构与性能的关系,本文以含乙炔桥键的四环异硫氰酸酯化合物为研究对象,芳基硼酸和3-氟-4-溴碘苯为起始原料,经6步反应合成了12种目标化合物,LC纯度大于99%,采用核磁共振、红外光谱对其结构进行了表征。采用DSC和POM对目标化合物的介晶性进行了研究,采用外推法对其双折射率和介电各向异性值进行了测试。结果表明:目标化合物具有300℃以上高清亮点、150℃以上向列相温度区间、0.40~0.51的双折射率以及大于17的介电各向异性值。对于同一系列化合物,随着末端烷基链的增长,化合物熔点降低,但呈现近晶相的趋势增加。在Y、Z位引入侧向氟取代基,熔点和清亮点均降低;X位再引入侧向氟取代基,熔点上升、清亮点下降。用环己烷替代左边第一个苯环,化合物熔点降低、向列相温度区间变宽。引入侧向氟取代基使双折射率下降0.008~0.036。目标化合物有利于提高混合液晶配方的双折射率、清亮点和降低阈值电压。     

Synthesis of SnAgCu nanoparticles with low melting point by the chemical reduction method

SnAgCu alloy with low melting point and good soldering property is a good candidate for the Sn/Pb eutectic. In this paper, SnAgCu nanoparticles were synthesized by a chemical reduction method. The particle size and the melting point are controlled by modifying the process parameters, including reaction temperature, surfactant concentration and dropping speed of precursor. The lowest melting onset temperature is observed at 199.1 °C, which is 18 °C lower than that of commercially available SnAgCu solder alloy. The tensile strength of the as-synthesized reaches 34.3 MPa, which reveals a good solderability property.