Al2O3/Ti生物相容连接接头微观组织及力学性能

文中对Al₂O₃陶瓷和金属Ti表面磁控溅射Mo和Ti金属层,以纯Au箔钎料,研究连接工艺及Ti金属化层厚度对连接接头微观组织和力学性能的影响.结果表明,焊缝主要由Au钎料和（Au,Mo） ss构成,（Au,Mo） ss中含有少量（Ti,Mo） ss和TixAuy金属间化合物.另外,在Al₂O₃/钎料界面处及焊缝中存在少量呈条状分布的TiO₂和Ti_xAl_y金属间化合物.连接工艺及Ti金属化层厚度主要影响各物相的数量及分布状态,通过影响焊缝中固溶体的分布均匀性及金属间化合物的数量而影响接头抗剪强度.当连接温度为1 080℃、保温时间为5 min、Ti金属化层厚度为0.2 μm时,接头的抗剪强度达到最大值138 MPa.     

采用Au基钎料真空钎焊Al2O3陶瓷

首先选用AgCuTi活性钎料在880℃/10 min参数下对A1₂O₃陶瓷表面进行金属化处理,之后尽量去除金属化层中的AgCu共晶组织,然后选用两种Au基高温钎料在980℃/10 min参数下对金属化后的A1₂O₃进行了钎焊连接.结果表明,在Al₂O₃/Au-Ni/Al₂O₃接头中靠近Al₂O₃母材的界面处生成一层薄薄的扩散反应层,该反应层主要由TiO₂和Al₂O₃组成;在Al₂O₃/Au-Cu/Al₂O₃接头中同样存在扩散反应层,与前者不同的是,接头中检测到Ti-Au相的存在.分别对Au-Ni和Au-Cu两种钎料获得的Al₂O₃接头进行了抗剪强度测试,前者对应接头强度为95.5 MPa,后者对应接头强度达到102.3 MPa.     

表面活化Al2O3陶瓷与5005铝合金真空钎焊

采用Al-Si钎料对经过Ag-Cu-Ti粉末活性金属化处理的Al₂O₃陶瓷与5005铝合金进行了真空钎焊,研究了钎焊接头的典型界面组织,分析了钎焊温度对接头界面结构特征及力学性能的影响. 结果表明,接头典型界面结构为5005铝合金/α-Al+θ-Al₂Cu+ξ-Ag₂Al/ξ-Ag₂Al+θ-Al₂Cu+Al₃Ti/Ti₃Cu₃O/Al₂O₃陶瓷. 钎焊过程中,Al-Si钎料与活性元素Ti及铝合金母材发生冶金反应,实现对两侧母材的连接. 随着钎焊温度的升高,陶瓷侧Ti₃Cu₃O活化反应层的厚度逐渐变薄,溶解进钎缝中的Ag和Cu与Al反应加剧,生成ξ-Ag₂Al+θ-Al₂Cu金属间化合物的数量增多,铝合金的晶间渗入明显;随钎焊温度的升高,接头抗剪强度先增加后降低,当钎焊温度为610 ℃时,接头强度最高达到15 MPa.     

填充泡沫Ti/AlSiMg的SiC陶瓷钎焊接头的组织与性能

为丰富SiC陶瓷钎焊所用钎料的设计思路,提出了一种泡沫Ti/AlSiMg新型复合钎料,通过Ti元素的溶入提高钎料与SiC陶瓷之间的界面结合力,利用泡沫Ti与Al基钎料之间的界面反应获得原位增强的钎缝,从而提升接头力学性能. 采用钎焊温度700 ℃、保温时间60 min和焊接压力10 MPa进行SiC陶瓷真空钎焊,利用光学显微镜、扫描电镜、能谱分析、X射线衍射、电子探针和万能试验机对接头组织、成分和性能进行分析,探索泡沫Ti/AlSiMg复合钎料在SiC陶瓷钎焊中的可用性. 结果表明,填充泡沫Ti/AlSiMg复合钎料所得接头结构为SiC/Al/Ti(Al,Si)₃/Ti(Al,Si)₃原位增强Ti基钎缝/ Ti(Al,Si)₃/Al/SiC,断裂发生在铝合金界面层和SiC陶瓷之间,Ti元素的溶入提高了铝合金界面层与SiC陶瓷之间的界面结合力,接头抗剪强度达111 MPa.     

采用Cu-Ti钎料高温连接Si3N4陶瓷

采用Cu80Ti20钎料在1413~1493 K的温度,保温时间5~15 min的工艺条件下分别进行了Si₃N₄陶瓷的高温活性钎焊,在所选工艺条件下均成功得到了无明显缺陷和裂纹的钎焊接头,通过对接头组织和成分的分析,接头的组成为Si₃N₄陶瓷/TiN界面反应层/Cu-Ti化合物+Ti5Si3/TiN界面反应层/Si₃N₄陶瓷.在1413 K保温10min条件下,固溶体中的Ti元素扩散至钎缝与母材的界面并发生反应,形成了致密连续的厚度约为1 μm的反应层.获得了钎焊温度、保温时间、钎缝宽度及界面层厚度等对接头强度的影响规律,在试验中所采用的工艺参数条件下,接头抗剪强度达到了105 MPa.     

DD3高温合金与Ti3AlC2陶瓷的真空钎焊

通过对比试验优选出了合适钎料,并进行了后续钎焊试验.在钎焊温度800~900℃,保温时间为10 min的条件下,采用Ag-Cu-Ti钎料实现了DD3镍基高温合金与Ti₃AlC₂陶瓷的真空钎焊连接.利用扫描电镜、能谱仪、XRD等对接头的界面结构进行了分析.结果表明,接头的典型界面结构为DD3/AlNi/Al₃(Ni,Cu)₅+Al(Ni,Cu)+Ag_ss/(Al,Ti)₃(Ni,Cu)₅/Al₄Cu₉+AlNi₂Ti+Ag_ss/TiAg/Ti₃AlC₂.接头的力学性能测试表明,在钎焊温度为850℃,保温时间为10 min的条件下,接头的最高抗剪强度可达135.9 MPa,断裂发生在靠近钎缝的Ti₃AlC₂陶瓷侧.降低和提高钎焊温度对接头界面组织影响不大,但接头强度有一定程度下降.     

Ag-Cu+WC复合钎料钎焊ZrO2陶瓷和TC4合金

采用新型Ag-Cu+WC复合钎料进行ZrO₂陶瓷和TC4合金钎焊连接,探究了接头界面组织及形成机制,分析了钎焊温度对接头界面结构和力学性能的影响. 结果表明,接头界面典型结构为ZrO₂/TiO+Cu₃Ti₃O/TiCu+TiC+W+Ag_(s,s)+Cu_(s,s)/TiCu₂/TiCu/Ti₂Cu/TC4. 钎焊过程中,WC颗粒与Ti发生反应,原位生成TiC和W增强相,为Ti-Cu金属间化合物、Ag基和Cu基固溶体提供了形核质点,同时抑制了脆性Ti-Cu金属间化合物的生长,优化了接头的微观组织和力学性能. 随钎焊温度的升高,接头反应层的厚度逐渐增加,WC颗粒与Ti的反应程度增强. 当钎焊温度890 ℃、保温10 min时,复合钎料所得接头抗剪强度达到最高值82.1 MPa,对比Ag-Cu钎料所得接头抗剪强度提高了57.3%.     

采用Ag-Cu-In-Ti钎料真空钎焊SiO2f/SiO2复合陶瓷与铌

设计了Ag-(15~26)Cu-(13~20)In-(3.1~6.9)Ti活性钎料,分别在780℃/20 min,780℃/40 min和800℃/10 min三种参数下实现了SiO_2f/SiO₂复合材料与铌的连接,分析了接头微观组织,测试了接头室温抗剪强度.其中800℃/10 min钎焊参数下的接头平均抗剪强度最高,达到21.6 MPa;微观分析结果表明,接头中靠近SiO_2f/SiO₂母材界面处形成了厚度约为2μm的连续扩散反应层,靠近铌的界面钎料与母材也形成了良好的结合.该钎焊参数下接头界面物相依次为:SiO_2f/SiO₂→TiO+TiSi₂→TiO+Cu₃Ti→Ag(s, s)+Ag₃In+Cu(s, s)→Nb.     

Al2O3陶瓷/AlSiMg/1A95铝合金间接钎焊接头组织与性能的研究

采用Al-Si-Mg钎料制备了表面Mo-Mn化后镀Ni的Al_2O_3陶瓷与1A95铝合金真空钎焊接头,研究了钎焊温度和保温时间对钎焊接头组织和剪切性能的影响,并分析了接头的界面微观组织及断口形貌。研究表明,最佳钎焊工艺为580℃×20 min,接头的抗剪强度达到74 MPa,此时接头界面结构为Al_2O_3/Mo-Mn/Al_3Ni/α-Al/1A95。随着钎焊温度的升高,界面处Al_3Ni化合物厚度增加;随着保温时间的延长,界面处产生了Al_(12)Mo化合物覆盖在Al_3Ni化合物上方。接头的断裂形式均为脆性断裂:当钎焊温度较低保温时间较短时,断裂主要发生在靠近铝合金与钎料层的界面处。最佳工艺条件下,断裂一部分发生在钎料和镀镍层的反应区内,一部分发生在靠近铝合金与钎料层的界面处。随着钎焊温度或保温时间进一步提高,断裂主要发生在钎料和镀镍层的反应区内。     

5005铝合金与1Cr18Ni9Ti的真空钎焊分析

采用Al-Si-Mg钎料成功实现了5005铝合金与1Cr18Ni9Ti不锈钢的真空钎焊,借助扫描电镜、能谱分析仪和X射线衍射仪对焊后接头界面组织进行分析,同时对接头抗剪强度进行测试.结果表明,焊后接头界面结构从1Cr18Ni9Ti不锈钢侧到5005铝合金侧的界面组织依次为FeAl,FeAl₃,Fe_mAl_n+αAl.随着钎焊温度的升高或保温时间的延长,接头抗剪强度均呈现先升高后降低的变化趋势.当钎焊温度为580℃,保温时间为15 min时,接头抗剪强度达到最大值49 MPa.接头断裂形式受钎焊温度的影响,当钎焊温度较低时,接头断裂于铝合金侧氧化膜层及Fe_mAl_n+αAl反应层;温度升高至580℃时,接头断裂于Fe_mAl_n+αAl反应层中,接头抗剪强度最高.     

Vacuum brazing of TZM alloy to ZrC particle reinforced W composite using Ti-28Ni eutectic brazing alloy

Reliable brazing of TZM alloy and ZrC particle reinforced (ZrC_p) W composite was achieved in this study by using Ti-28Ni eutectic brazing alloy. The typical interfacial microstructure of TZM/Ti-28Ni/ZrC_p-W brazed joint consisted of a Ti solid solution (Ti(s, s)) layer, a continuous Ti₂Ni layer and a diffusion layer mainly composed of W particles and (Ti, Zr)C particles. With an increase of brazing temperature, more ZrC particles and W particles entered the molten brazing alloy, which broadened the brazing seam and diminished the Ti₂Ni layer, resulting in the disappearance of the Ti₂Ni layer eventually. Meanwhile, more Ti(s, s) stripes were observed on the TZM side. The presence of continuous Ti₂Ni intermetallic phase and Ti(s, s) stripes structure in joints deteriorated the joining properties, which resulted in the formation of brittle fracture under shear test. In addition, the fracture path was related to the brazing temperature, and cracks initiate and propagate in the continuous Ti₂Ni layer at lower temperatures. However, the fracture path tended to be located at the TZM substrate close to the interface between TZM and the brazing seam when the brazing temperature exceeded 1040 °C. The optimal room temperature shear strength reached 120.5 MPa when brazed at 1040 °C for 10 min and the fracture surface exhibited cleavage fracture characteristics, and the shear strength at high temperature of 800 °C for the specimens with highest shear strength at room temperature reached 77.5 MPa.     

Ti活度对Al2O3/AgCuTi/Fe-Ni-Co钎焊接头机械性能和微观组织结构的影响

采用AgCuTi钎料实现了Al₂O₃陶瓷与Fe-Co-Ni合金的钎焊连接,并调查了不同钛含量的钎料对Al₂O₃/AgCuTi/Fe-Ni-Co钎焊接头机械性能和微观组织结构的影响。扫描电子显微镜(SEM), X射线能量色散光谱仪(EDS), X射线衍射仪(XRD)及电子万能试验机用于分析钎焊接头的机械性能和微观组织结构,结果表明:钛含量的增加明显提高AgCuTi钎料与Al₂O₃陶瓷的相互作用,在Al₂O₃/Ag-Cu-Ti界面生成一层由Ti-Al 和 Ti-O化合物组成的反应层。Al₂O₃/AgCuTi/Fe-Ni-Co钎焊接头的抗拉强度随钛含量的增加而增加,当钛含量提高到8wt.%时,抗拉强度达到最大值78Mpa。通过微观组织结构分析发现,采用AgCu4Ti在890℃保温5min的条件下可以获得较好的钎焊接头,典型接头的微观组织结构为Al₂O₃/TiAl+Ti₃O₅/NiTi+Cu₃Ti+Ag(s,s)/Ag(s,s)+Cu(s,s)+(Cu,Ni)/Fe-Ni-Co。采用AgCu8Ti获得的钎焊接头的界面反应层与AgCu4Ti差异不大,但反应层稍微增厚,并伴有TiO和Ti3Al在Al₂O₃/Ag-Cu-Ti界面生成。     

Interfacial microstructure and mechanical properties of GH99 superalloy and Nb brazed joint using Cu75Pt25 filler

Cu75Pt25 brazing filler was applied to brazing GH99 superalloy to Nb, and the sound joints were obtained by adjusting brazing parameters. The typical interfacial microstructure of the brazed joint was Nb/Nb₇Ni₆+NbNi₃/ Ni(s,s)+Cr-rich NbNi₃+(NbCr₂+NbNi₃)/GH99. The effects of brazing temperature and holding time on the interfacial microstructure of GH99/Cu75Pt25/Nb joints were studied. The results showed that the solution and diffusion of Ni atoms from GH99 substrate into brazing seam played a critical role in the interfacial microstructure evolution. As the brazing temperature rose, the Nb–Ni reaction layer was formed instead of the initial Nb₃Pt layer, and the thickness increased firstly and then remained constant. The highest shear strength of the joint reached 152 MPa when brazed at 1150 °C for 15 min. All of the joints presented a brittle fracture mode during shear test, and the fracture location changed from Nb₃Pt layer to Nb–Ni compounds layer.     

Brazing of TiBw/TC4 composite and Ti60 alloy using TiZrNiCu amorphous filler alloy

TiB_w/TC4 composite was brazed to Ti60 alloy successfully using TiZrNiCu amorphous filler alloy, and the interfacial microstructures and mechanical properties were characterized by SEM, EDX, XRD and universal tensile testing machine. The typical interfacial microstructure was TiB_w/TC4 composite/β-Ti + TiB whiskers/(Ti, Zr)₂(Ni, Cu) intermetallic layer/β-Ti/Ti60 alloy when being brazed at 940 °C for 10 min. The interfacial microstructure evolution was influenced strongly by the diffusion and reaction between molten fillers and the substrates. Increasing brazing temperature decreased the thickness of brittle (Ti, Zr)₂(Ni, Cu) intermetallic layer, which disappeared finally when the brazing temperature exceeded 1020 °C. Fracture analyses indicated that cracks were initialized in the brittle intermetallic layer when (Ti, Zr)₂(Ni, Cu) phase existed in the brazing seam. The maximum average shear strength of joints reached 368.6 MPa when brazing was conducted at 1020 °C. Further increasing brazing temperature to 1060 °C, the shear strength was decreased due to the formation of coarse lamellar (α+β)-Ti structure.     

Al_2O_3-TiC复合陶瓷与Q235钢扩散连接界面组织结构

采用Ti/Cu/Ti复合中间层通过液相扩散连接技术实现了Al2O3-TiC复合陶瓷与Q235低碳钢的扩散连接.采用扫描电镜、电子探针及X射线衍射等测试手段对Al2O3-TiC/Q235扩散连接接头的显微组织、断口形貌及相组成进行了分析.结果表明,Al2O3-TiC/Q235界面结合紧密,没有显微孔洞、裂纹及未连接区域;Al2O3-TiC/Q235界面附近有各种各样的新相生成,如TiO,Ti3Al,Cu2Ti4O及Cu3Ti3O,所生成的TiO相及复杂结构氧化物Cu3Ti3O和Cu2Ti4O都具有金属特性,对于促进Al2O3-TiC/Q235的可靠连接起到重要作用;接头抗剪强度达143MPa,断口表现为脆性断裂特征,Al2O3-TiC/Q235接头断在界面附近的Al2O3-TiC内.     

Influence of B2O3 additives on microstructure and electrical properties of ZnO-Bi2O3-Sb2O3-based varistors

B₂O₃-doped ZnO-Bi₂O₃-Sb₂O₃-based varistors were fabricated by conventional ceramic technique. The microstructure and electrical properties were investigated by SEM, XRD and electrical measurements. With the addition of B₂O₃, the liquid-assisted sintering based on Bi₂O₃ was improved, and the Bi₂O₃-B₂O₃ glass and Zn₃(BO₃)₂ phase were formed on the grain boundaries. The doping of B₂O₃ markedly improved the varistor performance of the ZnO-Bi₂O₃-Sb₂O₃-based varistors. The nonlinear coefficient of the sample with 3.5 mol% B₂O₃ sintered at 1100 °C reached 56 and the leakage current was only 0.3 μA.     

工艺参数对Al2O3/TC4合金接头界面组织及力学性能的影响

采用Cu＋B钎料分别在钎焊温度890～970℃,保温时间为10min;钎焊温度为930℃,保温时间0～30min条件下,钎焊A120,陶瓷与TCA合金．利用SEM,EDS和压剪试验研究接头界面组织及力学性能．结果表明,随钎焊温度升高或保温时间的延长,Ti2（Cu,Al）2O层增厚,紧邻其侧生成连续并增厚的Ti2（Cu,Al）,Ti2（Cu,Al）含量增加;Ti＋Ti2（Cu,Al）含量增加,尺寸变大,分布范围逐渐变宽并向TC4合金侧迁移,TCA合金侧过共析组织区变宽．钎焊温度低于950℃时,TiB晶须主要分布在Ti2Cu晶界处的AlCu2Ti上;当钎焊温度高于950℃时,AlCu2Ti相逐渐消失,TiB晶须主要分布于Ti2Cu上．当保温时间为10min,钎焊温度为950℃时,接头最大强度为96MPa;而当钎焊温度为930℃,保温时间为20min时,接头最大强度为83MPa．关键词：Al2O3陶瓷;TC4合金;钎焊参数;界面组织;抗剪强度     

Interfacial Behavior and Its Effect on Mechanical Properties of C<Subscript>f</Subscript>/SiC Composite/TiAl6V4 Joint Brazed with TiZrCuNi

In order to characterize the interfacial behavior of brazed joints and offer theoretical basis for the applications of TiZrCuNi-based composite fillers, C_f/SiC composite and TC4 were brazed by TiZrCuNi filler, and the microstructures of joints versus temperature and versus holding time were systematically studied in this paper. The mechanical properties of brazed joints were measured and analyzed. The results showed that Ti(Zr)C, Ti₅Si₃, Ti₂Cu, TiNi, TiZrCu₂, Ti₂(Cu,Ni) and Ti(s,s) were the predominant compounds in the joints. Brazing temperature had a distinct effect on the microstructures of joints: with the increase of brazing temperature, the structure of brazed joints was reduced from four parts to three parts, and the wavy reaction layer became continuous and much thicker. While holding time had a similar but weaker effect on microstructures: with the extension of holding time, the reaction layer became thicker, but it was difficult to induce the decrease in the structural parts of joint. The thickness of reaction layer determined the mechanical properties of joints. The results were beneficial for the selection of reinforced phases and the design of composite fillers to obtain better mechanical performances. When the brazing temperature was 940 °C and the holding time was 25 min, the maximum shear strength of brazed joints attained a value of 143.2 MPa.