Electrical conductivity changes of bulk tin and Sn-3.0Ag-0.5Cu in bulk and in joints during isothermal aging

The changes of electrical conductivity （resistance） between Sn-3.0Ag-0.5Cu solder joints and printed circuit board （PCB） assembly during aging at 125℃ were investigated by the four-point probe technique. The microstructural characterizations of interfacial layers between the solder matrix and the substrate were examined by optical microscopy and scanning electronic microscopy. Different types of specimens were designed to consider several factors. The experimental results indicate that electrical conductivities （resistances） and residual shear strengths of the solder joint specimens significantly decrease after 1000 h during isothermal aging. Microcracks generate in the solder matrix at the first 250 h. Besides, the evolutions of microstructural characterizations at the interface and the matrix of solder joints were noted in this research.

Effect of electromigration and isothermal aging on interfacial microstructure and tensile fracture behavior of SAC305/Cu solder joint

The Cu/Sn-3. OAg-0.5Cu/Cu butting solder joints were fabricated to investigate the evolution of the interfacial intertnetaUic compound （ IMC ） and the degradation of the tensile strength of solder joints under the effect of electromigration （ EM） and aging processes. Scanning electron microscopy（SEM） results indicated that the Cu6Sn5 interfacial IMC presented obvious asymmetrical growth with the increase of EM time under current density of l. 78 × 10^4 A/cm^2 at 100 ℃ , and the growth of anodic IMC presented a parabolic relationship with time while the cathodic IMC got thinner gradually. However, as for aging samples at 100℃ without current stressing, the Cu6Sn5 IMC presented a symmetrical growth with a slower rate than the anodic IMC of EM samples. The tensile results indicated that the tensile strength of the solder joints under current stress declined more drastic with time than the aging samples, and the fracture mode transformed from ductile fracture to brittle fracture quickly while the fracture mode of aging samples transformed from cup-cone shaped fracture to microporous gathering fracture in a slow way.

Influence of isothermal aging onσprecipitation in super duplex stainless steel

The time-temperature-transformation （TTT） curve of the 00Cr25Ni7Mo4N duplex stainless steel was obtained with a Formastor-digital thermal dilatometer, and the influence of isothermal aging on o precipitation was studied by metallographic observation, X-ray diffraction （XRD）, and transmission electron microscopy （TEM）. The results show that the decomposition of ferrite phase is accompanied by the formation of σ phase at 750-1000℃, especially in the range of 800-900℃. The longer the aging time, the higher the amount of o precipi- tation. The area fxaction of various phases remains at a certain value upon the completion of ferrite deformation. The temperature of 850℃ is the most sensitive transaction temperature, the incubation time for the formation of o precipitation is less than 1 min, and aging for 20 min leads to the complete transformation of ferrite. The o phase is formed preferentially at the α/α/γjunction, and then grows along the α/α boundary in the matrix.

Isothermal Aging Kinetics in CuZnAl Shape Memory Alloy

Isothermal aging behaviours of a CuZnAl shape memory alloy have been investigated by means of dilatometry.The length of the specimens during isothermal aging from 190 to 280℃ increases with the aging time at each temperature.The isothermal aging kinetics fits in Avrami equation and the time exponent n decreases with the increase in aging temperature.The apparent activation energy for the isothermal aging process was measured to be 109.0kJ/mol,which is about equal to that of a relaxation internal friction peak at about 200℃ (f≈1 Hz) in the alloy.

Influence of long-term isothermal aging on microstructure and creep rupture properties of Ni-base superalloy M4706

After a standard heat treatment,the microstructural evolution with time during isothermal aging at 850°C and its effect on the creep rupture properties of the Ni-base superalloy M4706 at 870°C and 370 MPa are investigated.It is found that as the aging time increases from 0 to 5000 h,the average diameter of coarseγ′increases from 241 to 484 nm,and the distribution of the carbides at grain boundaries changes from discontinuous to continuous.Moreover,experimental observations on the microstructures of all the crept specimens reveal that dislocation bypassing controls the creep deformation.Thus,it is concluded that the transitions in the microstructures result in the degeneration of the creep rupture properties of the experimental alloy with aging time.

Microstructure and Shear Properties Evolution of Minor Fe-Doped SAC/Cu Substrate Solder Joint under Isothermal Aging

Different amounts of Fe(0.005,0.01,0.03,0.05,and 0.07 wt%)were added to SAC305 to study the shear behavior damage of Fe-doped SAC solder joints under thermal loading(170℃,holding time of 0,250,500,and 750 h).The results show that during isothermal aging at 170℃,the average shear force of all solder joints decreases with increasing aging time,while the average fracture energy first increases and then decreases,reaching a maximum at 500 h.Minor Fe doping could both increase shear forces and related fracture energy,with the optimum Fe doping amount being 0.03 wt%within the entire aging range.This is because the doping Fe reduces the undercooling of the SAC305 alloy,resulting in the microstructure refining of solder joints.This in turn causes the microstructure changing from network structure(SAC305 joint:eutectic network+β-Sn)to a single matrix structure(0.03Fe-doped SAC305 joint:β-Sn matrix+small compound particles).Specifically,Fe atoms can replace some Cu in Cu_(6)Sn_(5)(both inside the solder joint and at the interface),and then form(Cu,Fe)_(6)Sn_(5) compounds,resulting in an increase in the elastic modulus and nanohardness of the compounds.Moreover,the growth of Cu_(6)Sn_(5) and Cu_(3)Sn intermetallic compounds(IMC)layer are inhibited by Fe doping even after the aging time prolonging,and Fe aggregates near the interface compound to form FeSn_(2).This study is of great significance for controlling the growth of interfacial compounds,stabilizing the microstructures,and providing strengthening strategy for solder joint alloy design.

In-situ isothermal aging TEM analysis of a micro Cu/ENIG/Sn solder joint for flexible interconnects

Sn/ENIG has recently been used in flexible interconnects to form a more stable micron-sized metallurgical joint,due to high power capability which causes solder joints to heat up to 200℃.However,Cu_(6)Sn_(5)which is critical for a microelectronic interconnection,will go through a phase transition at temperatures between 186 and 189℃.This research conducted an in-situ TEM study of a micro Cu/ENIG/Sn solder joint under isothermal aging test and proposed a model to illustrate the mechanism of the microstructural evolution.The results showed that part of the Sn solder reacted with Cu diffused from the electrode to formη´-Cu_(6)Sn_(5)during the ultrasonic bonding process,while the rest of Sn was left and enriched in a region in the solder joint.But the enriched Sn quickly diffused to both sides when the temperature reached 100℃,reacting with the ENIG coating and Cu to form(Ni_(x)Cu_(1-x))_(3)Sn_(4),AuSn_(4),and Cu_(6)Sn_(5)IMCs.After entering the heat preservation process,the diffusion of Cu from the electrode to the joint became more intense,resulting in the formation of Cu_(3)Sn.The scallop-type Cu_(6)Sn_(5)and the seahorse-type Cu_(3)Sn constituted a typical two-layered structure in the solder joint.Most importantly,the transition betweenηandη’was captured near the phase transition temperature for Cu_(6)Sn_(5)during both the heating and cooling process,which was accompanied by a volume shifting,and the transition process was further studied.This research is expected to serve as a reference for the service of micro Cu/ENIG/Sn solder joints in the electronic industry.

Microstructure and shear properties evolution of Mn-doped SAC solder joint under isothermal aging

The effects of Mn addition(0.005,0.01,0.03,0.05,and 0.07 wt.%)on microstructure,shear mechanical behavior,and interfacial thermal stabilities of SAC305 joints were investigated under isothermal aging temperatures of 170 C with different aging time(0,250,500,and 750 h).It is found that Mn addition can increase fracture energy of joints without decreasing the shear strength.And the microstructures have transformed from the eutectic net-like structure in SAC305 solder joints into the structures based onβ-Sn matrix with intermetallic compounds(IMCs)distributed.By doping 0.07 wt.%Mn,the Cu_(6)Sn_(5) growth along the SAC305/Cu interface during thermal aging can be inhibited to some extent.During isothermal aging at 170°C,the maximum shear force of solder joint decreases continuously with aging time increasing,while the fracture energy rises first and then decreases,reaching the maximum at 500 h compared by that with the microstructure homogenization.Cu_(3)Sn growth between Cu_(3)Sn_(5)/Cu interface has been retarded most at the aging time of 250 h with 0.07 wt.%Mn-doped joints.With the aging time prolonging,the inhibition effect of Mn on CusSn IMC layer becomes worse.The strengthening effect of Mn can be explained by precipitation strengthening,and its mechanical behavior can be predicted by particle strengthening model proposed by Orowan.

Microstructures and mechanical properties of homogenization and isothermal aging Mg–Gd–Er–Zn–Zr alloy

The effects of homogenization and isothermal aging treatment on the mechanical properties of Mg-12Gd- 2Er-1Zn-0.6Zr （wt%） alloy were investigated. The precipitated long-period stacking order （LPSO） structure and the aging precipitation sequence of the conditioned alloys were observed and analyzed, respectively. The results indicate that the 14H-LPSO structure occurs after the homogenization treatment and the 131 phase forms after the isothermal aging process. These two independent processes could be controlled by the precipitation temperature range. The significant increase in the elongation of the as-cast alloy after homogenization treatment is attributed to the disappearance of the coarse primary Mgs（Gd, Er, Zn） phase and the presence of the 14H-LPSO structure. The precipitation sequence of the investigated alloy is α-Mg（SSS）/β″（D019）/β′（cbco）/β. Furthermore, the yield tensile strength （YTS） and ultimate tensile strength （UTS） values of the isothermal aging alloy have a great improvement, which could be attributed to the high density of the precipitated β′ phase.

Effects of Isothermal Aging on Microstructure and Mechanical Property of Low-Carbon RAFM Steel

In order to investigate the microstructure and mechanical property evolution of low-carbon reduced activation ferritic/martensitic(RAFM)steel during isothermal aging,the normalized and tempered specimens were aged at 600℃for 500,1000,and 3000 h,respectively.The microstructural evolution with aging time was analyzed,including the precipitation and growth of M23C6 and MX-type carbides as well as the formation of Laves phase.The results indicate that the coarsening of M23C6 is more obvious than that of MX with increase in aging time.During the long-term thermal exposure,the Fe2 W Laves phase precipitates adjacent to M23C6 along the prior austenite grain boundaries and packet boundaries.Lower carbon content can delay the precipitation of Laves phase compared to the steel containing higher carbon.In addition,the Laves phase precipitated along boundaries can provide the precipitation strengthening,slightly increasing the tensile strength of low-carbon RAFM steel after aging for 3000 h.

Sn-9Zn-2Cu钎料合金等温时效组织及显微硬度

对Sn-9Zn-2Cu钎料合金进行了不同时长的等温时效处理,分析了合金显微组织演化,并测试了合金显微硬度。结果表明:铸态合金显微组织由β-Sn相基体、针状α-Zn相、不规则γ-Cu5Zn8相组成,合金显微硬度为16.62HV;随时效时间由24 h增至120 h,合金中的γ-Cu5Zn8相含量逐渐增多,相邻γ-Cu5Zn8相相连且形貌由不规则向树枝状转变,针状α-Zn相变短,且形貌逐渐转变为细小球状,合金显微硬度分别降至16.31HV和15.1HV;当时效时间延长至240 h和360 h时,合金显微组织无明显变化,显微硬度约为15.1HV;但当时效时间达到720 h,γ-Cu5Zn8相明显粗化,合金显微硬度降至14.09HV。

Cr对Al-Cu-Mg-Ag合金动态再结晶行为和力学性能的影响

借助光学显微镜(OM),X射线衍射仪(XRD),场发射扫描电镜(SEM-EDS)和透射电镜(TEM)研究Cr对Al-CuMg-Ag合金铸态组织和双级均匀化后弥散相分布、尺寸和数量密度的影响,并采用高通量等温压缩实验研究不同等效应变下Cr对Al-Cu-Mg-Ag合金动态再结晶行为的影响。结果表明:均匀化阶段除析出棒状T-Al_(20)Cu_(2)Mn_(3)弥散相外,还出现平均直径和数量密度分别为67.4 nm和4.7μm^(-2)的球状Al7(Cr, Mn)弥散相,Cr与Mn相反的平衡分配系数(K_(Mn)<1_(vs) K_(Cr)>1)将无弥散相析出面积分数从29.5%降至13.8%,棒状的T-Al_(20)Cu_(2)Mn_(3)弥散相平均长度从275.4 nm减小至147.3 nm,数量密度从3.5μm^(-2)增至10.4μm^(-2)。EBSD和拉伸实验结果表明,Al7(Cr, Mn)弥散相对位错运动阻碍作用减少热压缩过程中小角度晶界向大角度晶界的转变,抑制动态再结晶。Cr的添加提高Al-Cu-Mg-Ag合金不同温度下的力学性能,在25,250,300℃下Al_(7)(Cr,Mn)弥散相对合金屈服强度的贡献值分别为21.9,16.2 MPa和15.3 MPa。

Precipitates in an isothermally aged Fe-18Cr-12Mn-0.04C-0.48N high-nitrogen austenitic stainless steel

Vertical section of Fe-18Cr-12Mn-0.04C-N system phase diagram varying with nitrogen content at 1×105 Pa was calculated using Thermo-Calc software and thermodynamic database.The morphology and crystallography information of precipitates in Fe-18Cr-12Mn-0.04C-0.48N high-nitrogen austenitic stainless steel during isothermal aging at 800 ℃ after austenization was investigated using optical microscopy(OM),and transmission electron microscopy(TEM) with energy distribution spectrum(EDS).The experimental results show that three precipitates,(Cr,Fe,Mn)2(N,C),(Cr,Fe,Mn)23(C,N)6 and σ phase exist in this steel,which is consistent with the thermodynamic calculation,indicating that thermodynamic calculation can provide instructions for alloy composition design,heat treatment and prediction of precipitation sequence in Fe-18Cr-12Mn-0.04C-N system.

基于IRC法和局部放电法的车载高压电缆绝缘状态评估

为准确评估乙丙橡胶(EPDM)车载电缆的绝缘老化状态,引用了等温松弛电流(IRC)法和局部放电(PD)法,分别讨论了老化因子、局部放电特征信息与电缆老化状态之间的映射关系,结果表明:随着车载电缆运行里程的增加,老化因子、局部放电量、放电次数和放电电流均呈现规律性增长趋势,多种老化应力协同作用是造成车载电缆绝缘劣化的主要原因,绝缘材料内部陷阱的增多和加深是车载电缆老化的微观表现。协同等温松弛电流法和局部放电法对车载电缆绝缘状态的评估具有有效性和可行性,通过建立微观陷阱分布特性与宏观局部放电特性之间的联系,分析可得:深陷阱捕获电荷的能力较强,电荷极易集聚,局部放电容易发生,因此基于IRC法和局部放电法对车载电缆绝缘状态进行评估具有一定的价值意义,可指导高速动车组电网规划及电缆检修工作。

煤炭地下气化渗透反应墙构建材料的吸附和渗流特性研究

煤炭地下气化(UCG)带来的地下水污染风险是限制其推广发展的主要问题之一。渗透反应墙(PRB)修复技术是地下水原位修复的主要研究热点,而PRB材料特性是影响其正常运行的关键。本文首先探究了砂、有机膨润土、活性炭对UCG特征有机污染物苯酚的吸附特性,在此基础上,采用自建的渗流实验系统研究了砂、有机膨润土、活性炭及其混合物的吸附和渗透特性对净化污染水的综合影响效果。结果表明:(1)有机膨润土对溶液中苯酚的吸附速率较快,可在10 min之内达到吸附平衡,但吸附容量较小(1.98 mg/g);活性炭对溶液中苯酚的吸附速率较慢,但吸附容量较大(2.22 mg/g)。(2)有机膨润土对苯酚的等温吸附可用Freundlich模型描述,模型参数k_(F)=0.040,n=1.207;活性炭对苯酚的等温吸附可用Langmuir模型描述,模型参数S_(max)=2.44 mg/g,k_(L)=0.125 L/mg。(3)砂和活性炭的渗透系数分别为1.006×10^(-3) m/s和4.761×10^(-2) m/s,砂与活性炭或有机膨润土混合可有效调节混合材料的渗透性,当砂与有机膨润土质量比由1∶1增大到3∶1时,其混合材料的渗透系数由2.624×10^(-6)增大至3.468×10^(-5) m/s;而砂与活性炭质量比由1∶1增大到3∶1时,其混合材料的渗透系数由1.379×10^(-3)减小至1.301×10^(-4) m/s。

时效工艺对Al-Zn-Mg-Cu挤压棒材组织和性能的影响

研究了时效工艺对Al-Zn-Mg-Cu挤压棒材组织和性能的影响。结果表明,合金经双级+再时效、回归再时效和非等温时效处理后,均获得了优于T73时效处理的抗晶间腐蚀性能,最大腐蚀深度由70μm分别降至19、48和30μm。合金经过双级+再时效处理后,获得了与回归再时效和非等温时效处理样品相近的抗拉强度和屈服强度,而抗晶间腐蚀性能明显优于回归再时效和非等温时效。合金经T73、双级+再时效、回归再时效和非等温时效处理后,晶界析出相平均尺寸分别为27.7、39.2、31.6和25.5 nm,基体沉淀相平均尺寸分别为8.1、10.2、10.9和11.0 nm。

非等温回归再时效工艺对7055铝合金组织与性能的影响

文章以7055铝合金为研究对象,通过TEM、力学性能测试、耐腐蚀性能测试等实验手段,探究非等温回归过程中升温速率对合金组织与性能的影响规律,回归升温速率设为40℃/h、60℃/h、600℃/h,升温截止温度为180℃。结果表明,当非等温回归再时效工艺为(120℃×24 h)+(60℃/h→180℃)+(120℃×24 h)时,7055铝合金获得了高于T6态的强度,抗拉强度680 MPa,屈服强度641 MPa,延伸率14%。60℃/h升温速率下回归再时效后,晶内析出相细小弥散分布,晶界析出相断续排列,晶界无沉淀析出带(PFZ)明显,剥落腐蚀性能评级为EA,耐腐蚀性能优异。

Optimizing temperature coefficient of Sm_(2)Co_(17)-type magnets through adjusting the isothermal aging process

The high-temperature magnetic perfo rmance and micro structure of Sm_(1-x)Gd_(x)(Co_(bal)Fe_(0.09)Cu_(0.09)Zr_(0.025))_(7.2)(x=0.3,0.5) magnets were investigated.With the isothermal aging time decreasing from 11 to 3 h,the temperature coefficient of intrinsic coercivity in the temperature range of 25-500℃,β_(25-500℃),was optimized from -0,167%/℃ to-0.112%/℃ for x=0.3 magnets.The noticeable enhancement(~33%) of temperature stability is correlated with the increased content of 1:5H cell boundary phase and its relatively high Curie temperature as well.However,for the x=0.5 magnet,it is found that the presence of Sm_(5)Co_(19) phases and wider nanotwin variants hinder the formation of 1:5H cell boundary phase.The insufficient 1:5H is not beneficial to the proper redistribution of Cu in cell boundary,making the x=0.5 magnet difficult to achieve higher temperature stability.Consequently,the approach of adjusting the isothermal aging process can offer guidance for attaining superior magnetic performance in the temperature range from 25 to 500℃ for Gd-substituted Sm_(2)Co_(17)-type magnets.

高银系Sn-Ag-Cu/Cu界面金属间化合物生长行为

【目的】为研究高银系(Ag质量分数大于3.0%)Sn-Ag-Cu在固相时效过程中的界面反应和生长动力学。【方法】高温条件下不同银含量对界面结构和界面生长的影响,为了确定焊点的长期可靠性,在150℃下进行了0 h,100 h,300 h,500 h的热加速老化试验。用SEM与EDS进行了IMC表面形貌、厚度和元素组成。【结果】研究结果表明,随着银含量的增加,Cu_(6)Sn_(5)的生长受到不同程度抑制。在等温时效过程中,金属间化合物(IMC,Cu_(6)Sn_(5)+Cu_(3)Sn)的生长动力学是一个扩散控制过程,Cu_(6)Sn_(5)逐渐生长为Cu_(3)Sn;在后期的老化阶段,扇贝状的形状消失,表明生长机制发生了变化,变化为向垂直于界面方向的稳定生长;通过有限元技术,得出在服役过程中,热应力主要集中于Cu_(3)Sn与Cu基板交界处;随着时效时间的增加,焊点等效蠕变应变上升,可靠性逐渐降低;利用阿仑尼乌斯公式计算了金属间化合物IMC(Cu_(6)Sn_(5)+Cu_(3)Sn)在界面Sn-3.0Ag-0.7Cu/Cu,Sn-3.4Ag-0.7Cu/Cu,Sn-3.8Ag-0.7Cu/Cu的表观活化能分别为67.13 kJ/mol,70.50 kJ/mol,69.54 kJ/mol。【结论】根据试验与数值模拟计算相结合的研究手段,得到Sn-3.4Ag-0.7Cu款无铅焊料在高温服役过程中比其他焊料更能满足电子元件的要求。

非等温时效对含银Al-Mg-Si合金多层摩擦表面显微组织和腐蚀行为的影响

研究非等温时效对添加不同银含量Al-Mg-Si合金多层摩擦表面显微组织和腐蚀行为的影响。通过在耗材棒横截面上钻孔的方式添加4%、8%和13%(质量分数)的银。采用光学显微镜和电子显微镜研究涂层的显微组织,采用显微硬度和拉伸实验研究涂层的力学性能,采用电化学测试研究样品的耐腐蚀性。结果表明,随着银添加量从4%(质量分数)增加到13%(质量分数),摩擦堆焊表面层的晶粒尺寸从(1.5±0.3)μm减小到(1.0±0.3)μm。铝基体中的溶质银能够加速Al-Mg-Si合金的析出动力学。经非等温时效处理后,含银涂层的屈服强度和抗拉强度分别比不含银涂层高50.6%和43.5%。经非等温时效处理后,材料的腐蚀电流密度降低,含银和不含银样品的耐腐蚀性均提高,含银涂层的耐蚀性比无银镀层提高了96.5%。