激光沉积修复GH4169合金热处理的组织及性能

激光沉积修复GH4169合金强度与塑性仅达到铸件标准Q/5B 453-1995,热处理是改善其力学性能的重要手段。研究了不同热处理工艺对激光沉积修复GH4169合金显微组织和拉伸性能的影响规律,结果表明:激光沉积修复GH4169合金试样经直接时效热处理后,与沉积态相比,枝晶间的Laves相少量熔解,拉伸强度提高,与锻件标准Q/3B 548-1996(高强)相当,而塑性略有下降;且随着时效时间的延长,试样拉伸强度与塑性没有提高。修复试样经固溶处理后,Laves相部分熔解,并在其周围析出大量针状δ相,拉伸强度达到锻件标准,断后伸长率比沉积态提高21%;修复试样经均匀化处理后,Laves相基本熔解,在晶界及晶内均析出了δ相,拉伸强度接近锻件标准,断后伸长率超过了锻件标准27.1%。试验表明合适的热处理能有效提高激光沉积修复GH4169合金的强度与塑性。     

热等静压处理对选区激光熔化GH3536微观结构及拉伸性能的影响

利用选区激光熔化技术制备GH3536试样,研究了热等静压处理前、后选区激光熔化GH3536微观结构演变对力学性能各向异性的影响。利用扫描电镜、电子背向散射衍射和拉伸试验等方法对沉积态和热等静压态试样进行了微观组织、晶体织构和力学性能表征分析。研究结果表明,与传统工艺相比沉积态试样形成了超细晶组织且拉伸性能较高。X-Y面中的等轴晶存在〈001〉和〈101〉择优取向;Y-Z面中外延生长的柱状晶结构的〈001〉晶向近似与增材方向平行。受晶粒尺寸及织构强度的影响,相对于纵向试样,横向试样的屈服和抗拉强度更高,但其延展性偏低,在断口中观察到脆性断裂特征及未熔合缺陷。经热等静压处理后,柱状晶粒发生等轴化转变,晶粒取向随机分布,碳化物沿晶界析出,裂纹愈合,但是试样拉伸强度降低,塑性升高,并且各向异性消失。     

激光沉积Ti65钛合金的显微组织与各向异性研究

采用激光沉积制造技术制备了Ti65钛合金试样，并对其进行了退火热处理，分析了试样不同截面/方向的显微组织和力学性能。结果表明：激光沉积Ti65试样沿沉积方向形成了粗大的柱状晶和平行分布的层带结构，层带中的α板条粗化明显；垂直于沉积方向的截面呈等轴晶结构；不同截面的显微组织均为片层组织。退火后，不同截面的晶界断续，α板条粗化，显微组织均为网篮组织，显微组织的各向异性不明显。沉积态试样沿沉积方向和垂直于沉积方向的抗拉强度分别为1015 MPa和1055 MPa，伸长率分别为11.4%和8.4%；退火后，沿沉积方向和垂直于沉积方向的抗拉强度分别为1025 MPa和1079 MPa，伸长率分别为12.7%和10.5%。沉积态试样沿沉积方向的显微硬度比垂直于沉积方向低约20 HV0.2；退火后，不同方向的显微硬度接近并约为400 HV0.2。退火后激光沉积Ti65综合力学性能的各向异性趋于弱化。     

激光成形修复Ti60合金组织与性能研究

利用金相分析、维氏硬度、X射线衍射、室温和高温(600℃)静载拉伸等方法,对整体叶盘候选材料Ti60合金进行激光成形修复组织与性能的研究.研究发现:激光成形修复后,修复区与锻件基体形成致密的冶金结合,热影响区的组织从锻件的双态组织逐步过渡到激光修复区的魏氏组织.激光成形沉积态修复区的硬度高于锻件基体,热影响区的硬度处于两者之间,经过退火(650℃,2h/空冷),激光修复区硬度减小;激光修复结合面测试试样室温和600℃高温拉伸测试都断裂在锻件基体;不同修复体积(10%,20%、50%和80%)的试样室温和高温(600℃)强度高于锻造态,室温塑性比锻造态低,而高温塑性与锻造态相当.     

SLM成形TC4钛合金高温拉伸力学性能及断裂机制分析

研究了选区激光熔化(SLM)成形TC4钛合金室温拉伸及高温拉伸力学性能和微观组织,以及高温拉伸断口形貌和气孔形成原因.结果表明:SLM成形TC4钛合金沉积态试样性能呈现强度高而塑性低的特点;经过800℃、4 h真空退火处理后,室温拉伸力学性能达到同牌号锻件水平.在400℃、500℃和600℃高温拉伸条件下,沉积态试样高...     

热处理对激光选区熔化成形316不锈钢组织与拉伸性能的影响

研究了激光选区熔化成形316不锈钢沉积态、400℃/3 h退火态、900℃/3 h退火态以及热等静压态(HIP)的组织与拉伸性能。结果表明,沉积态组织主要由呈外延生长的柱状晶组成。沉积态试样经400℃/3 h退火后,组织变化不明显,横向和纵向的强度略有提高,纵向延伸率明显提高,横向延伸率有所降低;经900℃/3 h退火后,粗大柱状晶分裂为较为细长的柱状晶,横向和纵向延伸率在强度有所降低的情况下得到了明显提高,拉伸强度与延伸率达到锻件水平;经热等静压后,粗大柱状晶分裂为细小的柱状晶,有等轴化的趋势,横向和纵向的强度有明显的降低,横向延伸率略有升高,纵向延伸率显著提高,拉伸强度与延伸率达到锻件水平;4种状态相比较,900℃/3 h退火态的拉伸强度和延伸率匹配度最佳。     

选区激光熔化Hastelloy-X合金组织演变及拉伸性能

采用选区激光熔化技术加工哈氏合金试样并进行后处理,分别分析了沉积态、热处理态、热处理+热等静压态试样的宏观/微观组织特征,并测试了室温/高温拉伸性能。结果表明,沉积态试样横向/纵向均出现微裂纹,但未出现析出物。热处理后,横向组织为等轴晶,纵向组织为交错分布的细柱状晶和粗柱状晶,这些晶粒内部存在两种形态差异显著的析出物。热等静压处理后,晶粒显著长大,析出物分布均匀化,试样的室温拉伸性能达到锻件标准;相比于纵向拉伸性能,横向拉伸性能具有高强度低塑性的特征。     

激光沉积修复BT20合金试验研究

采用激光沉积技术对BT20钛合金锻件加工超差及服役损伤进行修复,对修复过程中气孔和熔合不良等缺陷的形成进行了原因分析,并采用了优化工艺参数,对激光熔池施加超声外场等手段,获得无缺陷的修复试样。考察了试样的微观组织和主要合金元素的分布,测量了激光沉积层的显微硬度。结果表明:优化工艺参数后得到的修复组织和基体形成致密的冶金结合,而施加超声外场使修复区的气孔率明显下降;修复试样整体无合金元素的偏析,显微硬度分布从基材到修复区呈递增趋势。     

高沉积率激光熔覆沉积GH4169合金的微观组织与拉伸性能

采用高沉积率激光熔覆沉积技术制备了GH4169合金试样,研究了沉积率为2.2kg/h时GH4169合金的微观组织和拉伸断裂机制。结果表明:高沉积率激光熔覆沉积GH4169合金沉积态试样的析出相主要包括Laves相、针状δ相及不均匀分布的γ″和γ′强化相。拉伸测试结果表明,沉积态GH4169高温合金的塑性和强度均低于锻件标准。     

热等静压对激光直接沉积TB6钛合金组织和拉伸性能的影响

为揭示激光直接沉积TB6钛合金的组织与性能相关性,研究了其沉积态和沉积/热等静压态的组织特征和拉伸性能.结果表明:激光直接沉积TB6钛合金的沉积态组织为等轴晶,其拉伸断口为沿晶/穿晶混合断裂方式:激光直接沉积TB6钛合金的沉积/热等静压组织仍为等轴晶,但晶内析出针/束状a相,其拉伸断口为穿晶断裂方式并存在大量韧窝:热等静压导致激光直接沉积TB6钛合金的拉伸强度降低约200MPa,而塑性提高1倍.该结果表明热等静压工艺可以有效调控激光直接沉积TB6钛合金的组织及性能.     

激光熔化沉积Ti60合金、TiCp/Ti60复合材料的高温拉伸持久寿命及断裂过程

通过激光熔化沉积工艺制备出Ti60合金和质量分数为5%的TiCp/Ti60复合材料,分析比较了两种材料的微观组织及高温(600 ℃)拉伸持久性能。结果表明,所沉积TiCp/Ti60复合材料中初生TiC呈树枝晶分布于原始β晶界,共晶TiC呈颗粒状分布于α -Ti板条间,TiC的存在导致基体组织细化。TiCp/Ti60复合材料较基体合金具有更加优异的高温(600 ℃)拉伸持久寿命,其高温拉伸持久断裂过程为：增强体与基体界面脱粘、α -Ti/β -Ti的界面处微孔形核、长大、横向扩展及连接,最终导致复合材料的失效。     

Ultra-Shallow junctions in silicon using amorphous and polycrystalline silicon solid diffusion sources

The inter-dependence of diffusion behavior and grain microstructure in amorphous silicon/polysilicon-on-single crystal silicon systems has been studied for rapid thermal and furnace annealing for P and BF₂ implants. It is found that the changes of microstructure during annealing play a major role in determining the diffusion profiles in the substrate as well as in the polysilicon layer. For P doping, a drive-in diffusion results in a much larger grain microstructure for as-deposited amorphous silicon than for as-deposited polysilicon, which leads to the formation of shallower junctions in the substrate for the first case. For B doping, there is little difference in the final microstructure and junction depth between the two cases. The P and B junctions formed in the substrate are found to be laterally very uniform in spite of expected doping inhomogeneities due to polysilicon grain boundaries both for as-deposited amorphous silicon diffusion sources and for as-deposited polysilicon diffusion sources.     

Analysis of the stress and interfacial reactions in Pt/Ti/SiO2/Si for use with ferroelectric thin films

The microstructure of the Pt/Ti/SiO₂/Si structure has been investigated by scanning and transmission electron microscopy. Pt films of 100 nm thickness deposited by sputtering or evaporation onto unheated substrates gave complete coverage of the underlying Ti layer and showed a granular and faceted structure with grains ∼20 nm in diameter. They did not exhibit hillocks or surface TiO_x formation. X-ray diffraction was used to examine the film stress through use of the sin²ψ method with bulk values for the elastic constants (v=0.39, E=162 GPa). The as-deposited sputtered film had a compressive stress of ∼540 MPa, while the evaporated films had tensile stresses of ∼630 MPa. The films then received a 400°C rapid thermal anneal (RTA) for 90 s and a subsequent RTA of 650°C for 30s. Further investigation of the film stresses and microstructure were made after each annealing step. After the low temperature anneal, the film stress for the sputtered film became tensile. Plan-view sections examined by transmission electron microscopy (TEM) showed that the as-deposited sputtered films were dense but became porous after annealing. Initially, the evaporated films had a less dense microstructure, but were more stable with annealing. Little change in the stress for the evaporated film was observed after this initial low temperature annealing step. Additional annealing of the evaporated and sputtered samples caused complete consumption of the Ti layer including some TiO_x formation from the underlying SiO₂ layer and marked interaction with the Pt; however, little change in the stress was found. The surface of the Pt film revealed larger grains, but otherwise remained unaffected. The underlying phase changes were minimized once the Ti layer had reacted with the Pt. Due to the ratio of the layers, Pt:Ti of 2:1, the surface of the Pt was unaffected.     

Creep deformation of grain boundary in a highly crystalline SiC fibre

Silicon carbide (SiC) matrix composites reinforced by SiC fibres (SiC/SiC composites) are currently being considered as alternative materials in high Ni alloys for high-temperature applications, such as aerospace components, gas-turbine energy-conversion systems and nuclear fusion reactors, because of their high specific strength and fracture toughness at elevated temperatures compared with monolithic SiC ceramics. It is important to evaluate the creep properties of SiC fibres under tensile loading in order to determine their usefulness as structural components. However, it would be hard to evaluate creep properties by monoaxial tensile properties when we have little knowledge on the microstructure of crept specimens, especially at the grain boundary. Recently, a simple fibre bend stress relaxation (BSR) test was introduced by Morscher and DiCarlo to address this problem. Interpretation of the fracture mechanism at the grain boundary is also essential to allow improvement of the mechanical properties. In this paper, effects of stress applied by BSR test on microstructural evolution in advanced SiC fibres, such as Tyranno-SA including small amounts of Al, are described and discussed along with the results of microstructure analysis on an atomic scale by using advanced microscopy.     

激光立体成形17-4 PH不锈钢组织性能研究

对激光立体成形17-4 PH(0Cr17Ni4Cu4Nb)沉淀硬化不锈钢沉积区热处理前后的组织和常规力学性能进行了研究。光学显微镜(OM)、扫描电子显微镜(SEM)和X射线衍射(XRD)结果表明,沉积态组织主要由板条状马氏体和分布于其上和板条间少量的第二相强化质点组成。根据合金特性,推测马氏体基体上弥散析出的第二相强化质点应该为M7C3及NbC型碳化物等。靠近基材处的沉积态组织以细长的板条状淬火马氏体为主;远离基材的沉积态组织则变成粗大的板条状马氏体。沉积态试样经过固溶时效处理后,组织变为细小均匀的板条状回火马氏体,并且基体上析出了更多的第二相强化质点,这类强化质点推测应为NbC型以及M7C3,M23C6型碳化物。成形件经过热处理后,强度、硬度略微提高,而塑性则显著增加。并且其抗拉强度和塑性均高于锻棒标准,屈服强度则略低于锻棒标准。热处理前后成形件拉伸断裂均属于韧性断裂,其中M7C3型碳化物等形成的第二相质点是微观空穴和韧窝形成之源。     

溅射法制备高取向Pt薄膜的工艺研究

采用射频磁控溅射工艺在SiO2／Si衬底上成功制备了适用于pZT铁电薄膜底电极的180nm厚、沿(111)晶向强烈取向的Pt薄膜。厚约50nm的Ti膜被用作过渡层，以增强Pt薄膜与衬底之间的黏着性。实验表明，在Pt薄膜的制备过程中，较高的衬底温度有利于薄膜晶化，促使Pt薄膜沿(111)晶向择优取向生长。而在薄膜沉积后加入适当的热处理工艺，能有效地提高Pt薄膜的择优取向性，同样可以得到沿(111)晶向强烈取向的Pt薄膜。原子力显微镜分析表明，制得的薄膜结构相对致密，结晶状况良好，晶粒尺寸约为50nm。     

The microstructure,mechanical stress,texture, and electromigration behavior of Al-Pd alloys

As the minimum feature size of interconnect lines decreases below 0.5 urn, the need to control the line microstructure becomes increasingly important. The alloy content, deposition process, fabrication method, and thermal history all determine the microstructure of an interconnect, which, in turn, affects its performance and reliability. The motivation for this work was to characterize the microstructure of various sputtered Al-Pd alloys (Al-0.3wt.%Pd, Al-2Cu-0.3Pd, and Al-0.3Nb-0.3Pd) vs sputtered Al-Cu control samples (Al-0.5Cu and Al-2Cu) and to assess the role of grain size, mechanical stress, and crystallographic texture on the electromigration behavior of submicrometer wide lines. The grain size, mechanical stress, and texture of blanket films were measured as a function of annealing. The as-deposited film stress was tensile and followed a similar stress history on heating for all of the films; on cooling, however, significant differences were observed between the Al-Pd and Al-Cu films in the shape of their stress-temperature-curves. A strong (111) crystallographic texture was typically found for Al-Cu films deposited on SiO₂. A stronger (111) texture resulted when Al-Cu was deposited on 25 nm titanium. Al-0.3Pd films, however, exhibited either a weak (111) or (220) texture when deposited on SiO₂, which reverted to a strong (111) texture when deposited on 25 nm titanium. The electromigration lifetimes of passivated, ≈0.7 μm wide lines at 250°C and 2.5 × 10⁶ A/cm² for both single and multi-level samples (separated with W studs) are reported. The electromigration behavior of Al-0.3Pd was found to be less dependent on film microstructure than on the annealing atmosphere used, i.e. forming gas (90% N₂-10%H₂) annealed Al-0.3Pd films were superior to all of the alloys investigated, while annealing in only N₂ resulted in poor lifetimes.     

热处理对脉冲激光沉积羟基磷灰石薄膜组织和性能的影响

利用脉冲激光沉积技术在Ti6Al4V(TC4)合金表面制备了羟基磷灰石(HA)薄膜,研究了退火温度对薄膜组织和性能的影响。采用扫描电子显微镜(SEM)、能谱仪(EDS)、X射线衍射(XRD)和傅里叶红外光谱(FTIR)等分析手段对热处理前后薄膜的表面形貌、成分和组织结构进行了分析;采用轮廓仪、接触角测量仪分别对热处理前后薄膜的表面粗糙度和润湿性进行了测量。实验结果表明,利用脉冲激光沉积技术制备的HA薄膜致密、无缺陷,主要由非晶相组成。热处理后的薄膜结晶度提高、表面粗糙度增大,Ca/P比更接近于HA,具有更好的表面亲水性。但是过高的热处理温度(700℃)会导致薄膜中微裂纹的出现。     

退火工艺对La-Nb共掺杂Bi_4Ti_3O_(12)薄膜结构的影响

采用sol-gel法制备了Si基Bi3.25La0.75Ti2.94Nb0.06O12.03(BLTN)铁电薄膜,研究了退火温度、升温速率和退火时间对BLTN薄膜微观结构的影响。结果表明:制备的BLTN薄膜具有单一的钙钛矿结构,且为随机取向,表面平整致密;退火温度由550℃升高到750℃时,薄膜的衍射峰强度增强,晶粒尺寸由65 nm增大到110 nm;退火升温速率由10℃/min提高为20℃/min时,薄膜的晶化程度降低;退火时间对薄膜的晶相结构影响不大,但时间超过30 min会造成薄膜表面孔洞增多、致密性下降。     

The process window of a-Si/Ti bilayer metallization for anoxidation-resistant and self-aligned TiSi2 process

The dependences of both oxidation-resistant and self-aligned silicidation properties on the thicknesses of top amorphous-Si (a-Si) and Ti metal in an a-Si/Ti bilayer process are presented. It is shown that a thin silicide layer formed during the reaction between a-Si and Ti films becomes a stable oxidation and nitridation barrier for oxygen- and nitrogen-related impurities. Moreover, the formation sequence of the silicide phase depends not only on the annealing temperature but also on the thickness of the Ti film. In addition, the preferential orientation of the silicide phase after annealing at high temperature also shows a strong dependence on the thickness of Ti film, which is attributed to the difference of the grain size in the polycrystalline silicide film. The allowed process window for the a-Si thickness can be determined experimentally and a reproducible and homogeneous self-aligned TiSi₂ film can be easily obtained by using the a-Si/Ti bilayer process in salicide applications despite high-level contaminations of oxygen impurities in both the as-deposited Ti film and the annealing ambient