高体积分数SiC_p/Al电子封装复合材料的钎焊综述（英文）

高体积分数SiC_p/Al复合材料作为电子封装材料使用日益流行,其钎焊具有重要的实际意义。近来,一些新钎料合金和工艺被开发用于高体积分数SiC_p/Al复合材料的钎焊。本文回顾了SiC_p/Al复合材料的物理力学性能和制备工艺,综述了应用于高体积分数SiC_p/Al复合材料的合金钎料、钎焊工艺及其接头微结构与性能,旨在进一步理解它们之间的关联性,以优化接头性能与可靠性。往Al-Si合金中添加Cu、Mg、Ni等合金元素有助于提高钎料合金和钎焊接头的使用性能,如可优化钎料合金的应用温度、接头界面结合和焊缝强度。而表面金属化和超声波振动两种钎焊辅助工艺可通过避免或去除复合材料表面的Al_2O_3和SiO_2氧化膜来改善合金钎料的钎焊性。最后指出,需要进一步加强对合金钎料的优化设计、表面金属化工艺以及焊料/涂层/基材体系之间的润湿性和界面行为的研究。     

高阻尼高强度铸态SiCp/Mg94Zn5Y1 复合材料的综合性能

采用铸造方法制备具有不同SiC_p含量（0.5%~2.0%，质量分数，下同）的SiC_p/Mg₉₄Zn₅Y₁复合材料，并研究了复合材料的力学性能和阻尼性能。通过扫描电子显微镜和X射线衍射仪测试复合材料的微观组织结构和物相组成。在基体中加入SiC_p之后，SiC_p均匀分布在基体中，增强体细化了复合材料的微观组织结构。SiC_p/Mg₉₄Zn₅Y₁复合材料包括α-Mg、I相（准晶相）和SiC_p相。分别使用动态热机械分析仪和AG-X试验机测试了SiC_p/Mg₉₄Zn₅Y₁复合材料的阻尼性能和力学性能。复合材料的力学性能优于Mg₉₄Zn₅Y₁合金，1.0%SiC_p/Mg₉₄Zn₅Y₁复合材料的抗压缩强度高达350 MPa；所有复合材料的阻尼性能都远高于基体合金的阻尼性能，其中0.5%SiC_p/Mg₉₄Zn₅Y₁复合材料具有最佳的阻尼性能。此外，根据功效系数法，SiC_p含量为1.0%的SiC_p/Mg₉₄Zn₅Y₁复合材料具有良好的综合性能。     

Al2O3陶瓷/AgCuTi/GH99高温合金的钎焊接头力学性能

采用AgCuTi钎料对Al₂O₃陶瓷与GH99高温合金进行了钎焊连接,研究了工艺参数(连接温度、保温时间)的变化对接头力学性能的影响,并分析了不同参数下接头的断裂位置,结果表明：保温5min时,在不同的连接温度下进行钎焊,随着连接温度的升高,接头的抗剪强度先增后减,在900℃时取得最大值,为127.24MPa,连接温度较低时,主要断裂于Al₂O₃/钎料侧,随着温度的升高,接头TiNi₃反应层增厚,因此还有部分断裂于TiNi₃反应层/钎料界面;在连接温度为900℃时,随着保温时间的延长,接头的抗剪强度逐渐降低,保温时间较短时,主要要断裂于Al₂O₃/钎料界面,保温时间过长,TiNi₃反应层延伸入钎料中部且厚度大大增加,在该反应层中产生微裂纹,造成接头强度大大降低,此时部分断裂于钎料中部及TiNi₃反应层中。     

Ti-Cu-Ni-Nb-Al-Zr-Hf非晶钎料合金真空钎焊Ti50Al50 接头的界面组织与剪切强度

在钎焊温度1140~1220 ℃、钎焊时间30 min的工艺参数下,采用Ti-9.5Cu-8Ni-8Nb-7Al-2.5Zr-1.8Hf（质量分数,%）非晶钎料成功实现了Ti₅₀Al₅₀ (at%)合金的真空钎焊连接,并研究了钎焊温度对钎焊接头的显微组织、剪切强度的影响规律。结果表明,在任何钎焊温度下获得的Ti₅₀Al₅₀钎焊接头均有3个界面反应层且每个反应层都含有α₂-Ti₃Al和Ti₂Cu(Ni) 2个物相。随着钎焊温度的增加,α₂-Ti₃Al和Ti₂Cu(Ni)在钎焊接头中的尺寸与分布发生了明显的变化,尤其是等温凝固层Ⅱ中的Ti₂Cu(Ni)相。1200 ℃下稳定存在的连续α₂-Ti₃Al层Ⅰ对母材和钎料原子的相互扩散具有阻隔壁垒作用,温度一旦超过1200 ℃,α₂-Ti₃Al相变得不稳定使得连续α₂-Ti₃Al层被打破从而失去阻隔壁垒效应。在钎缝中析出且弥散分布的α₂-Ti₃Al对焊缝中物相的形成可以起到抑制形核和细化晶粒的作用。随着钎焊温度升高,Ti₅₀Al₅₀钎焊接头平均抗剪切强度先增加后减小,在钎焊温度1180 ℃、钎焊时间30 min时钎焊接头的抗剪切强度最大,达184 MPa。剪切断口表面呈典型解理断裂特征且α₂-Ti₃Al占绝大多数。     

热处理对SiCp/Al-6%Mg复合材料微观组织及腐蚀行为影响

采用无压渗透法制备了SiC_p/Al-6%Mg复合材料,并对其进行4种热处理工艺(T1, T4, T6和退火)处理,研究了热处理工艺对SiC_p/Al-6%Mg复合材料微观组织和腐蚀行为的影响。结果表明,复合材料在4种热处理工艺下均出现了界面反应产物Si、MgA1₂O₄ 和 Mg₂Si。界面反应产物析出量(f)与热处理工艺密切相关,并呈现出如下规律：f_T1< f_T4< f_T6annealing。界面反应析出物是导致复合材料发生点蚀的主要原因,从而促进复合材料发生腐蚀。热处理工艺能影响界面反应析出量而间接影响复合材料的腐蚀速度(j_corr)：j_corr-T6> j_corr-T4> j_corr-T1。     

TiZrNiCu钎焊Si3N4-MoSi2复合陶瓷与Nb接头组织与力学性能

采用高温活性钎料TiZrNiCu对Si₃N₄-MoSi₂复合陶瓷和金属Nb进行真空钎焊试验,研究了其典型界面组织组成及形成机理,分析了钎焊温度和保温时间对钎焊接头界面组织及力学性能的影响规律。结果表明,接头典型界面结构为Nb/β-Ti/(Ti. Zr)₂(Cu, Ni)+β-Ti+(Ti, Zr)₅Si₃/TiN+(Ti, Zr)₅Si₃+MoSi₂/Si₃N₄-MoSi₂。钎焊温度和保温时间主要通过控制Si₃N₄-MoSi₂复合陶瓷母材中Si原子向钎料中扩散程度,来影响钎缝中(Ti, Zr)₅Si₃化合物的数量及分布,进而影响钎焊接头的抗剪强度。在920 ℃/10 min的工艺参数下,Si₃N₄-MoSi₂/Nb接头的室温抗剪强度最高达到112 MPa,选择最优参数条件下的Nb/Si₃N₄-MoSi₂钎焊接头在500 ℃和600 ℃条件下进行高温剪切实验,其高温抗剪强度分别达到123 MPa和131 MPa。     

空气反应钎焊ZrO2与GH3536接头组织与力学性能

采用Al₂TiO₅颗粒增强的Ag-CuO-Al₂TiO₅复合钎料,在钎焊温度为1050 ℃保温30 min工艺参数下,对ZrO₂陶瓷与GH3536合金进行了空气反应钎焊(RAB),分析了钎焊接头的界面结构及其形成机制;同时研究了接头在800 ℃氧化不同时间的组织演变规律及其对连接性能的影响。结果表明,钎焊过程中Al₂TiO₅颗粒分解产生Al₂O₃和TiO₂,TiO₂与ZrO₂陶瓷反应生成ZrTiO₄相。GH3536侧金属元素发生氧化形成尖晶石层,并分别与钎缝中的Al₂O₃、CuO反应,在钎缝中生成细密分布的NiAl₂O₄相及紧邻尖晶石层的团块状NiCuO₂相。ZrO₂/GH3536接头高温氧化1000 h后,钎缝中NiAl₂O₄呈团块状分布,Cr₂O₃薄层保持稳定;尖晶石层内部元素均匀化,厚度有明显增加。接头强度随着氧化时间的延长先降低后稳定在20 MPa。     

铝硅镁钎料真空钎焊SiC_p/Al-MMCs与可伐合金的工艺与性能研究

研究了增强相体积分数为55%的Si Cp/Al-MMCs与可伐合金的真空钎焊,分析了钎焊温度和复合材料表面镀层对接头性能的影响规律。结果表明,Al-12.0Si-1.5Mg-4.0Ti钎料在真空条件下能很好地润湿55%Si Cp/Al-MMCs和可伐合金,合适的钎焊工艺参数为:复合材料表面镀铜、真空度6.5×10-3Pa、钎焊温度590℃、保温时间30 min,接头最大剪切强度可达64.9 MPa。当钎焊温度从570℃增加到590℃时,接头的剪切强度和显微硬度都逐渐增加。复合材料表面镀铜会显著增加钎缝以及界面区域的显微硬度。复合材料表面镀层会对接头剪切强度产生影响,在590℃以下钎焊时,无镀层的复合材料和可伐合金接头的剪切强度较高。而当钎焊温度达到590℃时,表面镀铜的复合材料与可伐合金接头的剪切强度最高。     

中间层对高体积分数SiCp/Al复合材料真空钎焊的影响

采用铜箔、Al-Si-Mg及Al-Si-Mg/Cu/Al-Si-Mg(简称ACA)3种不同中间层对高体积分数45%SiC_p/Al复合材料进行真空钎焊连接研究.通过SEM,EDS及XRD等方法对钎缝的微观结构及界面组织进行了分析,研究了中间层种类对钎焊接头微观结构、界面组织以及连接强度的影响,阐明了不同中间层钎焊连接45%SiC_p/Al复合材料的界面形成过程及接头断裂机制.结果表明,ACA中间层兼具了铜和Al-Si-Mg钎料的优点,可降低钎料的液相线,增加其流动性,通过Cu原子优先在铝合金基体与其氧化膜的界面处扩散发生共晶反应,增强钎料的去膜作用,从而实现高体积分数45%SiC_p/Al复合材料的高质量连接.     

碳纤维-FeCoCrNiAl高熵合金颗粒混杂增强7075铝基复合材料的力学性能及断裂行为

为探究双相增强体对铝基复合材料拉伸性能和断裂行为的影响,采用真空热压烧结工艺在580 ℃,30 MPa条件下保温10 min制备了FeCoCrNiAl高熵合金颗粒增强7075铝基复合材料（HEA_p/Al）,Ni-Co-P镀层修饰碳纤维增强7075铝基复合材料（CF/Al）和FeCoCrNiAl高熵合金颗粒及Ni-Co-P镀层修饰碳纤维混杂增强铝基复合材料（CF-HEA_p/Al）。并对不同复合材料微观结构及拉伸性能进行分析表征及比较。结果表明：CF-HEA_p/Al复合材料的屈服强度（YS）与极限拉伸强度（UTS）随纤维含量的升高（体积分数由0至40%）呈现先增大后降低的变化,延伸率则逐渐降低。鉴于Ni-Co-P镀层修饰碳纤维与FeCoNiCrAl高熵合金颗粒的混杂强化效应, CF-HEA_p/Al复合材料的YS和UTS较HEA_p/Al与CF/Al复合材料明显提高,且其断口表现出基体韧性断裂及纤维拔出与断裂的多种失效特征。     

Effects of K2O-Li2O doping on surface and catalytic properties of Fe2O3/Cr2O3 system

The effects of K₂O and Li₂O-doping (0.5, 0.75 and 1.5 mol%) of Fe₂O₃/Cr₂O₃ system on its surface and the catalytic properties were investigated. Pure and differently doped solids were calcined in air at 400-600 °C. The formula of the un-doped calcined solid was 0.85Fe₂O₃:0.15Cr₂O₃. The techniques employed were TGA, DTA, XRD, N₂ adsorption at −196 °C and catalytic oxidation of CO oxidation by O₂ at 200-300 °C. The results revealed that DTA curves of pure mixed solids consisted of one endothermic peak and two exothermic peaks. Pure and doped mixed solids calcined at 400 °C are amorphous in nature and turned to α-Fe₂O₃ upon heating at 500 and 600 °C. K₂O and Li₂O doping conducted at 500 or 600 °C modified the degree of crystallinity and crystallite size of all phases present which consisted of a mixture of nanocrystalline α- and γ-Fe₂O₃ together with K₂FeO₄ and LiFe₅O₈ phases. However, the heavily Li₂O-doped sample consisted only of LiFe₅O₈ phase. The specific surface area of the system investigated decreased to an extent proportional to the amount of K₂O and Li₂O added. On the other hand, the catalytic activity was found to increase by increasing the amount of K₂O and Li₂O added. The maximum increase in the catalytic activity, expressed as the reaction rate constant (k) measured at 200 °C, attained 30.8% and 26.5% for K₂O and Li₂O doping, respectively. The doping process did not modify the activation energy of the catalyzed reaction but rather increased the concentration of the active sites without changing their energetic nature.     

Fe3O4/SiO2/Bi2WO6磁性复合光催化剂的制备及其光催化性能

钨酸铋(Bi₂WO₆),结构最简单的Aurivillius相化合物,是近期受到研究者关注的新型光催化材料。然而,光催化剂粉末在反应介质中难被回收,工业化应用成本较高。本文用三步方法合成了可回收的Fe₃O₄/SiO₂/Bi₂WO₆磁性复合光催化剂,通过溶剂热法合成具有磁性的Fe₃O₄,用溶胶凝胶法在Fe₃O₄表面覆盖SiO₂层,后将磁性颗粒与Bi₂WO₆纳米片相结合。光催化剂的形貌结构及性能通过XRD、SEM、PL、UV-vis进行表征测试。结果表明,直径约500 nm的Fe₃O₄微球附着在边长约500 nm的Bi₂WO₆纳米片的表面,SiO₂在两者之间起到了粘连作用。光催化剂Fe₃O₄/SiO₂/Bi₂WO₆对于罗丹明B的光降解活性较好,且有一定磁性,可以通过外加磁场将其从溶液中分离,有较大的应用潜力。     

钕的添加对V2O5-MoO3/TiO2平板式脱硝催化剂性能的影响

本研究制备了一系列不同Nd含量的V₂O₅-MoO₃-Nd₂O₃/TiO₂平板式脱硝催化剂。采用XRD、N2-吸附脱附、XPS、H2-TPR、拉曼光谱、NH3-TPD和红外光谱等表征手段对催化剂进行分析。结果表明:适量的Nd2O3(0.25%、0.5%,质量分数)可以增强V₂O₅-MoO₃/TiO₂催化剂的还原性能,增加了催化剂的Oα/(Oα+Oβ)比率,从而提升了催化剂的脱硝活性。然而,过量Nd₂O₃(0.75%、1%)的添加,会导致催化剂酸性性能的显著降低,造成催化剂脱硝性能的下降。此外,过量Nd的添加还会对催化剂的耐磨性能有负面影响。各催化剂中,VMoN d(0.5%)/Ti催化剂显示了最佳的脱硝活性。并且,该催化剂还显示了优良的抗SO₂、H₂O性能。     

废旧锂离子电池中Li, Fe和V的回收及xLiFePO4-yLi3V2(PO4)3的制备

由于LiFePO_4和Li_3V_2(PO_4)_3材料的特征相近,制备方法类似,提供了一种从废旧LiFePO_4和Li_3V_2(PO_4)_3混合电池中回收Li、Fe和V,再制备xLiFePO_4-yLi_3V_2(PO_4)_3的方法。在空气气氛中600℃热处理1h后,去除粘结剂PVDF使活性物质与集流体分离。调节Li、Fe、V和P摩尔比,球磨、锻烧,配制不同比例的xLiFePO_4-yLi_3V_2(PO_4)_3(x:y=5:1,7:1,9:1)复合电极材料。表征了其形貌、结构和电化学性能,结果表明,回收制备的复合材料将同时具备LiFePO_4和Li_3V_2(PO_4)_3两种材料的电化学性能,能显著改善LiFePO_4的倍率性能。     

Preparation and characteristic of spherical Li3V2(PO4)3

Spherical Li₃V₂(PO₄)₃ was synthesized by using N₂H₄ as reducer. The products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that single-phase, spherical and well-dispersed Li₃V₂(PO₄)₃ has been successfully synthesized in our experimental process. Electrochemical behaviors have been characterized by charge/discharge measurements. The initial discharge capacities of Li₃V₂(PO₄)₃ were 123 mAh g⁻¹ in the voltage range of 3.0–4.3 V and 132 mAh g⁻¹ in the voltage range of 3.0–4.8 V.     

Sol-gel synthesis of Bi3.25La0.75Ti3O12 nanotubes

Ferroelectric Bi_3.25La_0.75Ti₃O₁₂ (BLT) nanotubes were synthesized by sol-gel technique using nanochannel porous anodic aluminum oxide (AAO) templates, and were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). BLT nanotubes with diameter of around 240 nm and the wall thickness of about 25 nm exhibited a single orthorhombic perovskite structure and highly preferential crystal growth along the [1 1 7] orientation, which have smooth wall morphologies and well-defined diameters corresponding to the diameter of the applied template. The formation mechanism of BLT nanotubes was discussed.     

国外多孔基体氧化铝/氧化铝复合材料工程应用进展

氧化铝/氧化铝复合材料(Al2O3/Al2O3)是20世纪90年代兴起的一类连续陶瓷纤维增强陶瓷基复合材料,已经发展为与SiC/SiC、C/SiC等非氧化物陶瓷基复合材料并列的一类陶瓷基复合材料。与非氧化物陶瓷基复合材料相比,Al2O3/Al2O3具有长时抗氧化、高温耐腐蚀、低成本等独特优势,已经在航空发动机、地面燃气轮机等军民两用热结构材料领域展现出广阔的应用前景。本文从材料应用的角度出发,系统分析阐述了目前在Al2O3/Al2O3占主导地位的多孔基体Al2O3/Al2O3(P-Al2O3/Al2O3)的增韧机制、成型工艺和性能特点,重点归纳了国外近年来P-Al2O3/Al2O3的工程化应用进展及前景,最后指出了P-Al2O3/Al2O3存在的局限性并展望了未来发展方向,旨在为国内Al2O3/Al2O3体系发展提供借鉴和参考。     

Sinterability and dielectric properties of Ba0.55Sr0.4Ca0.05TiO3-CaTiSiO5-Mg2TiO4 composite ceramics

The composite ceramics of Ba_0.55Sr_0.4Ca_0.05TiO₃-CaTiSiO₅-Mg₂TiO₄ (BSCT-CTS-MT) were prepared by the conventional solid-state route. The sintering performance, phase structures, morphologies, and dielectric properties of the composite ceramics were investigated. The BSCT-CTS-MT ceramics were sintered at 1100 °C and possessed dense microstructure. The dielectric constant was tailored from 1196 to 141 as the amount of Mg₂TiO₄ increased from 0 to 50 wt%. The dielectric constant and dielectric loss of 40 wt% Ba_0.55Sr_0.4Ca_0.05TiO₃-10 wt% CaTiSiO₅-50 wt% Mg₂TiO₄ was 141 and 0.0020, respectively, and the tunability was 8.64% under a DC electric field of 8.0 kV/cm. The Curie peaks were broadened and depressed after the addition of CaTiSiO₅. The optimistic dielectric properties made it a promising candidate for the application of tunable capacitors and phase shifters.     

Synthesis and characterization of Y3Al5O12 and ZrO2-Y2O3 thermal barrier coatings by combustion spray pyrolysis

Y₃Al₅O₁₂ and ZrO₂-Y₂O₃ (8 mol% YSZ) coatings for potential application as thermal barrier coatings were prepared by combustion spray pyrolysis. Thermal cycling of as deposited coatings on stainless steel and FeCrAlY bond coat substrates was carried out at 1000 °C and 1200 °C to determine the thermal fatigue response. Structural and morphological studies on Y₃Al₅O₁₂ and 8 mol% YSZ coatings before and after thermal cycling have been carried out. It has been noted that the coatings on FeCrAlY substrates remain intact after 50 cycles between room temperature and 1200 °C, whereas the coatings on stainless steel show some minor damage such as peeling off near the periphery after 50 cycles at 1000 °C. Thermal diffusivity values of Y₃Al₅O₁₂ and 8 mol% YSZ films were measured by using photo thermal deflection spectroscopy and the values are lower than those of coatings produced by conventional techniques such as EBPVD and APS.     

Low temperature sintering and microwave dielectric properties of (Mg0.7Zn0.3)0.95Co0.05TiO3 ceramics with BaCu(B2O5) additions

The effects of BaCu(B₂O₅) additives on the sintering temperature and microwave dielectric properties of (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics were investigated. The (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics were not able to be sintered below 1000 °C. However, when BaCu(B₂O₅) were added, they were sintered below 1000 °C and had the good microwave dielectric properties. It was suggested that a liquid phase with the composition of BaCu(B₂O₅) was formed during the sintering and assisted the densification of the (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics at low temperature. BaCu(B₂O₅) powders were produced and used to reduce the sintering temperature of the (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics. Good microwave dielectric properties of Q × f = 35,000 GHz, ?_r = 18.5.0 and τ_f = −51 ppm/°C were obtained for the (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics containing 7 wt.% mol% BaCu(B₂O₅) sintered at 950 °C for 4 h.