多级时效对Al-Mg-Si(Cu)合金力学性能和显微结构的影响

本文通过透射电镜观察、差示扫描量热分析(DSC)和硬度测试等方法研究了6061铝合金在多级时效处理过程中力学性能和显微结构演变的规律.其中,T6I6热处理为先进行固溶处理,淬火后进行180℃预时效,然后在65℃中断时效,最后在180℃再次时效,120/T6I6热处理则将预时效温度改为120℃.结果表明,T6I6热处理不会明显提高合金的峰值硬度,合金强度与析出相类型、尺寸和分布有关系.120℃预时效后中断时效时继续形成GP区或β″前驱相,而180℃预时效后中断时效对显微结构的影响较小.120/T6I6的中断时效过程析出的主要是尺寸较小的GP区或β″前驱相,它们在再时效阶段不能成为析出相的形核点.T6I6在中断时效前GP区和β″前驱相基本全部析出.T6I6热处理和120/T6I6热处理均没有使峰值硬度明显增加,而且120/T6I6会拖延峰值时间.     

Cu-Cr-Zr合金时效析出相的研究

利用高分辨电子显微镜（HRTEM）及系列欠焦像出射波函数重构技术,探明了在大气环境下,Cu-Cr-Zr合金峰值时效时存在氧化物析出相。研究结果表明：Cu-Cr-Zr合金经950℃×1.5 h固溶处理、450℃时效6 h硬度达峰值;此时样品中除早期的具有花瓣状应变场衬度的共格析出相外,另一类强化相为圆盘状形貌的CuCrO2;该氧化物析出相为三方晶系,空间群为R 3 m（166）,与基体具有特定取向关系：[011]Cu//[010]CuCrO2,（111）Cu//（003）CuCrO2,惯习面为{111}Cu。     

时效温度和Ag对Al-Zn-Mg合金力学性能与微观结构的影响

本文研究了在不同时效温度条件下Ag对Al-Zn-Mg铝合金力学性能与微观结构的影响。结果表明，随着时效温度的提升，Ag对合金硬度的影响增大，合金晶界无析出带宽度明显减小。时效温度为120℃时，含Ag和不含Ag的Al-Zn-Mg铝合金均以η系列相析出为主，但含Ag合金的晶内析出相分布更为细小弥散，尺寸减小的同时径厚比增大。当时效温度升高至160℃和180℃,Ag对合金峰值硬度的提升作用显著增加。此时，Al-Zn-Mg合金主要强化相由η系列相转变为T系列相，同时尺寸明显增大，而含Ag合金中主要强化相类型与120℃时相同，仍然为η系列相，且尺寸并未明显增大。     

Al-Mg-Si-Cu合金中晶界和晶内析出相粗化规律的研究

采用显微硬度测试仪、扫描电镜和透射电镜观察及能谱分析,研究了Al-0.5Mg-1.0Si-0.8Cu(wt.%)合金的晶界析出规律和晶内析出相的粗化机制。结果表明:180℃时效处理的Al-0.5Mg-1.0Si-0.8Cu(wt.%)合金晶界处存在富Si相和Q相两类不连续分布的析出相,它们的尺寸分别约为1 mm和几十纳米;时效0.5 h时晶界处有少量富Si相,时效5 h时晶界富Si相明显增多,时效36 h时富Si相开始粗化且间距变大,再进一步时效其形貌和分布变化不大;晶界Q相与相邻晶粒铝基体的界面取向关系是:[510]Al//[1120]Q;时效36 h晶内开始出现粗化析出相,且随时效继续进行合金晶内析出大量粗化相,存在明显的晶界无析出带现象。晶内粗化析出相主要含有Si元素,呈片状、球状和棒状3种形貌。其中,棒状Si析出相是沿〈001〉Al方向生长的,且〈112〉Si//〈001〉Al,{111}Si//{010}Al。     

热处理工艺对激光增材制造铝锂合金组织及力学性能的影响

采用激光增材制造技术制备了铝锂合金板材,分析了铝锂合金在热处理过程中析出相的演变及力学性能的变化。结果表明,沉积态铝锂合金主要由α(Al)基体和TB(Al7Cu4Li)相组成,晶界处存在少量富铜相;退火后,TB相更加均匀密集地分布在晶粒内部,富铜相基本溶解,晶界处存在少量Al-Cu-Fe杂质相;固溶淬火后,TB相固溶到基体中,晶内存在少量δ′(Al3Li)相;时效后,主要弥散析出θ′(Al2Cu)和σ(Al5Cu6Mg2)相。热处理后铝锂合金的显微硬度、抗拉强度比沉积态的分别提高了47.6%和87.7%。     

固溶处理后镁铝合金时效峰值硬度时微观结构的电子显微分析

用显微维氏硬度计、金相显微镜(OM)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)研究分析了Mg-10.33wt.%Al-1.26wt.%Zn合金固溶后的时效硬化规律。实验结果表明AZ91(Mg-9wt.%Al-1wt.%Zn-0.2wt.%Mn)合金添加少量的Al后固溶强化和时效强化效果均有显著提高。实验的时效硬度曲线表明:固溶处理后的Mg-10.33wt.%Al-1.26wt.%Zn合金在473K时效10 h获得最佳时效强化效果。经过分析,进一步证实Mg-10.33wt.%Al-1.26wt.%Zn合金固溶后时效过程中单位体积内的连续析出相γ-Mg17Al12相颗粒的数目(Nv)越大,样品的显微硬度值越高。     

Ti-6Al-4Cr（Mo）合金热处理显微组织的研究

本文采用扫描电镜与透射电镜分析研究了Ti-6Al-4Cr和Ti-6Al-4Mo合金固溶和时效过程中显微组织的变化。结果表明：Ti-6Al-4Cr和Ti-6Al-4Mo合金经过相似的两相区固溶处理后,组织差别较大;两种合金经过β相区固溶后再时效,形成典型的魏氏组织,且硬度值较两相区处理的样品有很大提高;两种合金在相同热处理制度下,硬度值变化趋势相似,但前者的硬度值明显大于后者;Ti-6Al-4Cr合金在各种热处理条件下都有富Cr的固溶体区产生,经过1000℃/45min/空冷＋600℃/2h/空冷处理后,有Laves相和界面相析出。     

三级时效7 N01铝合金微观结构与力学性能关系的研究

本文针对一种有实际应用前景、经历了三级时效的7N01铝合金,采用透射电镜观察和力学性能测试,系统研究了该合金力学性能与析出相微观结构的关系。研究结果表明,该种经历了三级时效状态的7N01铝合金,相比直接人工热处理的材料,屈服强度和抗拉强度均可获得显著提高,同时不损失延伸率。透射电镜观察发现,峰值时效状态下合金的主要强化析出相为η′相和GP区。而且自然时效形成的合金元素原子集团中有GP区生成,它们在人工时效阶段可以直接转化为η′相颗粒。经三级时效处理的合金强度在一定范围内与自然时效阶段形成的GP区的多少密切相关。     

FeCrAl合金中碳化物的时效析出和钇的影响

ＴＥＭ研究表明,低碳（０．０１－０．０３ｗｔ．％Ｃ）Ｆｅ－（１５．２５）Ｃｒ－（４,５）Ａｌ合金经１２００℃固溶处理后再于４７５－５４０℃时效时,碳化物迅速在晶界、位错等昌体缺陷处析出,晶界碳化物近于连续,晶界两侧形成析出带,析出相的衍谱与Ｃｒ２３Ｃ６和Ｃｒ７Ｃ３基本吻合,在含０．４ｗｔ．％Ｙ的ＦｅＣｒＡｌ合金中,含２相的衍射谱与六方α－Ｆｅ１７Ｙ２相的谱吻合,该相俘获碳原子的作用使合金在时效时不     

激光增材制造铝锂合金的热处理组织及T_B相析出

采用激光增材制造技术制备了铝锂合金,分析了沉积态铝锂合金的显微组织,优化得到了沉积态铝锂合金的双级均匀化退火和固溶热处理工艺参数,并探讨了TB相的时效析出行为。结果表明,经过双级均匀化退火及固溶热处理后,铝锂合金晶界和晶内析出的低熔点富铜相数量减少,铝锂合金的成分均匀性得到提高。当时效温度为400℃时,铝锂合金中析出的TB相数量达到最大;随着时效温度的继续升高,TB相数量逐渐减少。铝锂合金的显微硬度随着TB相含量的增加先减小后增大。     

时效对Sn3.0Cu0.15Ni/Cu界面组织的影响

研究了150℃时效0,200,500h对Sn3.0Cu0.15Ni/Cu界面组织结构的影响.结果表明:界面金属间化合物层由Cu6Sn5层和Cu3Sn层组成,质量分数为0.15％的Ni的加入会使IMC层最初变厚,但在时效过程中,热稳定性强的界面化合物(Cu,Ni)6Sn5的生成,会抑制Cu3Sn化合物层的生长;同时Ni的加入会降低Cu6Sn5颗粒的长大速度,并且随着时效时间的延长,Cu6Sn5颗粒的形貌呈多面体结构.     

Sn3.8Ag0.7Cu和Sn37Pb焊点界面显微结构研究

利用扫描电子显微镜（SEM）和透射电子显微镜（TEM）研究了Sn3.8Ag0.7Cu（Sn37Pb）/Cu焊点在时效过程中的界面金属间化合物（IMC）形貌和成份。结果表明：150℃高温时效50、100、200、500h后,Sn3.8Ag0.7Cu（Sn37Pb）/Cu焊点界面IMC尺寸和厚度增加明显,IMC颗粒间的沟槽越来越小。50h时效后界面出现双层IMC结构,靠近焊料的上层为Cu6Sn5,邻近基板的下层为Cu3Sn。之后利用透射电镜观察了Sn37Pb/Ni和Sn3.8Ag0.7Cu/Ni样品焊点界面,结果显示,焊点界面清晰,IMC晶粒明显。     

Intermetallic reactions in Sn3Ag0.5Cu and Sn3Ag0.5Cu0.06Ni0.01Ge solder BGA packages with Au/Ni surface finishes

The intermetallic compounds (IMCs) formed during the reflow and aging of Sn3Ag0.5Cu and Sn3Ag0.5Cu0.06Ni0.01Ge solder BGA packages with Au/Ni surface finishes were investigated. After reflow, the thickness of (Cu, Ni, Au)₆Sn₅ interfacial IMCs in Sn3Ag0.5Cu0.06Ni0.01Ge was similar to that in the Sn3Ag0.5Cu specimen. The interiors of the solder balls in both packages contained Ag₃Sn precipitates and brick-shaped AuSn₄ IMCs. After aging at 150°C, the growth thickness of the interfacial (Ni, Cu, Au)₃Sn₄ intermetallic layers and the consumption of the Ni surface-finished layer on Cu the pads in Sn3Ag0.5Cu0.06Ni0.01Ge solder joints were both slightly less than those in Sn3Ag0.5Cu. In addition, a coarsening phenomenon for AuSn₄ IMCs could be observed in the solder matrix of Sn3Ag0.5Cu, yet this phenomenon did not occur in the case of Sn3Ag0.5Cu0.06Ni0.01Ge. Ball shear tests revealed that the reflowed Sn3Ag0.5Cu0.06Ni0.01Ge packages possessed bonding strengths similar to those of the Sn3Ag0.5Cu. However, aging treatment caused the ball shear strength in the Sn3Ag0.5Cu packages to degrade more than that in the Sn3Ag0.5Cu0.06Ni0.01Ge packages.     

Effects of Minor Additions of Zn on Interfacial Reactions of Sn-Ag-Cu and Sn-Cu Solders with Various Cu Substrates during Thermal Aging

The effects of Zn additions to Sn-0.7Cu and Sn-3.8Ag-0.7Cu (all in wt.% unless specified otherwise) Pb-free solders on the interfacial reactions with Cu substrates were investigated. The study was focused on the intermetallic compound (IMC) growth, Cu consumption and void formation as a function of thermal aging and solder composition. Four different kinds of Cu substrates (high-purity Cu, oxygen-free Cu, vacuum-sputtered Cu, and electroplated Cu) were prepared to compare their interfacial reaction behaviors with Zn-added solders. Thermal aging was performed at 150°C for up to 1000 h to accelerate the interfacial reactions between solders and Cu substrates. Growth of IMCs (Cu₆Sn₅ and Cu₃Sn) in Zn-added solders was slower than those without Zn additions. The growth of the Cu₃Sn phase, in particular, was drastically reduced in the Zn-added solders on all four Cu substrates. On an electroplated Cu substrate, numerous voids were observed in the Cu₃Sn phase for Sn-Cu and Sn-Ag-Cu solders aged at 150°C for 1000 h. However, these voids were largely eliminated in the Zn-added solders. On the other three Cu substrates, the conditions which produce a high density of voids were not found after aging both solders with and without Zn. The Cu consumption with Zn-added solders was also significantly lower. The beneficial effects of Zn additions on interfacial reaction behaviors are reported, and the corresponding mechanisms in suppressing void formation and Cu consumption due to Zn additions will be discussed.     

Sn-3.0Ag-0.5Cu/Ni/Cu微焊点剪切强度与断口的研究

用直径为200~500μm的Sn-3.0Ag-0.5Cu无铅焊球分别在Ni和Cu焊盘上制作焊点,并对焊后和时效200h后的焊点进行剪切测试,并采用SEM观察剪切断口形貌。结果表明,焊后和时效200 h后焊点接头的剪切强度都随焊球尺寸增大而减小。焊后断口处韧窝形状为抛物线型,断裂方式为韧性断裂;随着焊球尺寸的增大,剪切断口处的韧窝数量增多,韧窝的变小变浅。时效200 h后,韧窝变浅,趋于平坦,韧窝数量也明显减少,材料的韧性下降,脆性增加,断裂方式由韧性向脆性发生转变。     

Intermetallic reactions in reflowed and aged Sn-9Zn solder ball grid array packages with Au/Ni/Cu and Ag/Cu pads

During the reflowing of Sn-9Zn solder ball grid array (BGA) packages with Au/Ni/Cu and Ag/Cu pads, the surface-finished Au and Ag film dissolved rapidly and reacted with the Sn-9Zn solder to form a γ₃-AuZn₄/γ-Au₇Zn₁₈ intermetallic double layer and ε-AgZn₆ intermetallic scallops, respectively. The growth of γ₃-AuZn₄ is prompted by further aging at 100°C through the reaction of γ-Au₇Zn₁₈ with the Zn atoms dissolved from the Zn-rich precipitates embedded in the β-Sn matrix of Sn-9Zn solder BGA with Au/Ni/Cu pads. No intermetallic compounds can be observed at the solder/pad interface of the Sn-9Zn BGA specimens aged at 100°C. However, after aging at 150°C, a Ni₄Zn₂₁ intermetallic layer is formed at the interface between Sn-9Zn solder and Ni/Cu pads. Aging the immersion Ag packages at 100°C and 150°C caused a γ-Cu₅Zn₈ intermetallic layer to appear between ε-AgZn₆ intermetallics and the Cu pad. The scallop-shaped ε-AgZn₆ intermetallics were found to detach from the γ-Cu₅Zn₈ layer and float into the solder ball. Accompanied with the intermetallic reactions during the aging process of reflowed Sn-9Zn solder BGA packages with Au/Ni/Cu and Ag/Cu pads, their ball shear strengths degrade from 8.6 N and 4.8 N to about 7.2 N and 2.9 N, respectively.     

elemental redistribution and interfacial reaction mechanism for the flip chip Sn-3.0Ag-(0.5 or 1.5)Cu solder bump with Al/Ni(V)/Cu under-Bump metallization during aging

In flip chip technology, Al/Ni(V)/Cu under-bump metallization (UBM) is currently applicable for Pb-free solder, and Sn−Ag−Cu solder is a promising candidate to replace the conventional Sn−Pb solder. In this study, Sn-3.0Ag-(0.5 or 1.5)Cu solder bumps with Al/Ni(V)/Cu UBM after assembly and aging at 150°C were employed to investigate the elemental redistribution, and reaction mechanism between solders and UBMs. During assembly, the Cu layer in the Sn-3.0Ag-0.5Cu joint was completely dissolved into solders, while Ni(V) layer was dissolved and reacted with solders to form (Cu_1−y,Ni_y)₆Sn₅ intermetallic compound (IMC). The (Cu_1−y,Ni_y)₆Sn₅ IMC gradually grew with the rate constant of 4.63 × 10⁻⁸ cm/sec^0.5 before 500 h aging had passed. After 500 h aging, the (Cu_1−y,Ni_y)₆Sn₅ IMC dissolved with aging time. In contrast, for the Sn-3.0Ag-1.5Cu joint, only fractions of Cu layer were dissolved during assembly, and the remaining Cu layer reacted with solders to form Cu₆Sn₅ IMC. It was revealed that Ni in the Ni(V) layer was incorporated into the Cu₆Sn₅ IMC through slow solid-state diffusion, with most of the Ni(V) layer preserved. During the period of 2,000 h aging, the growth rate constant of (Cu_1−y,Ni_y)₆Sn₅ IMC was down to 1.74 × 10⁻⁸ cm/sec^0.5 in, the Sn-3.0Ag-1.5Cu joints. On the basis of metallurgical interaction, IMC morphology evolution, growth behavior of IMC, and Sn−Ag−Cu ternary isotherm, the interfacial reaction mechanism between Sn-3.0Ag-(0.5 or 1.5)Cu solder bump and Al/Ni(V)/Cu UBM was discussed and proposed.     

Cr/Cu/Al/Cr薄膜电极的防氧化性能

采用Al作为Cu导电层的主要防氧化保护层,在普通浮法玻璃上利用磁控溅射和湿法刻蚀技术制备Cr/Cu/Al/Cr复合薄膜及其电极,研究不同的热处理温度对复合薄膜及其电极的结构、表面形貌和导电性能的影响。由于有Al层作为保护层,在热处理过程中,Al先与穿过Cr保护层的氧进行反应,从而可以更有效地保护Cu膜层在较高的温度下不被氧化,所制备的薄膜在经过600℃的热处理之后仍然具有较好的导电性能。而对于Cr/Cu/Al/Cr电极,侧面裸露的金属层在热处理过程中的氧化是其导电性能逐渐下降的主要原因,退火温度超过500℃之后,电极侧面裸露部分的氧化范围不断往电极的中间扩散,导致了薄膜电极导电性能显著恶化。虽然如此,Cr/Cu/Al/Cr薄膜电极在430℃附近仍然具有较好的导电性能,电阻率为7.3×10-8Ω.m,符合FED薄膜电极的要求。以此薄膜电极构建FED显示屏,通过发光亮度均匀性的测试验证了Cr/Cu/Al/Cr电极的抗氧化性。     

Reliability of Cu nanoparticle joint for high temperature power electronics

Power cycle reliability of Cu nanoparticle joint has been studied for high temperature operation of power devices. Al₂O₃ heater chips and Cu–65 wt% Mo baseplates were joined by Cu nanoparticles and Sn–0.7Cu and power cycle tests of 65/200 °C and 65/250 °C were carried out on the joints. The Cu nanoparticles were prepared by reducing Cu carbonate in ethylene glycol with dodecanoic acid + dodecyl amine (C12) and decanoic acid and decyl amine (C10) as capping agents. A power cycle test of 65/200 °C did not inflict severe damage on the Cu nanoparticle joints so that there were not many cracks formed after 3000 cycles. Vertical cracks were formed in the C12 Cu nanoparticle joint after 3000 cycles of 65/250 °C test, however the maximum temperature during the power cycle test did not change at all because vertical cracks did not have an effect on preventing heat flow. On the contrary, lateral cracks were completely formed in the Sn–0.7Cu soldered joint after 200 cycles of 65/200 °C test and in the C10 Cu nanoparticle joint after 360 cycles of 65/250 °C test. In these experiments, the maximum temperatures were rapidly increased because heat conduction was prevented across the formed lateral cracks.     

Interfacial Reaction Between Cu Substrates and Zn-Al Base High-Temperature Pb-Free Solders

Chemical reactions between Cu substrates and Zn-Al high-temperature solder alloys, Zn-4Al and Zn-4Al-1Cu (mass%), at temperatures ranging from 420°C to 530°C were experimentally investigated by a scanning electron microscope using backscattered electrons (SEM-BSE) and an electron probe microanalyzer (EPMA). Intermediate phases (IMPs), β(A2) or β′(B2), γ(D8₂), and ε(A3) phases formed and grew during the soldering and aging treatments. The consumption rate of the IMP for Cu substrates is described by the square root of t in both the alloys, while the additional Cu in the molten Zn-Al alloy slightly suppresses the consumption of Cu substrates. The growth of IMPs during soldering treatment is controlled by the volume diffusion of constituent elements, and its activation energy increases in the order of Q _ε < Q _γ < Q _β. In view of the aging process, the growth of IMPs is considered to be controlled by the volume diffusion. In particular, the layer thickness of γ rapidly grows over 200°C, although the thickness of the β layer grows very slowly.