高压下Zr70Cu30非晶合金的热稳定性和晶化相的变化

 用电阻测量及X射线衍射法研究了非晶Zr₇₀Cu₃₀合金在常压和高压下热稳定性以及晶化相的变化。结果表明压力提高了这种非晶合金的晶化温度并明显地改变了合金中的相平衡关系。在2 GPa压力下，平衡相为Cu₁₀Zr₇和α-Zr的混合物，而常压下为CuZr₂和少量α-Zr的混合物。     

非晶Fe78Si9B13合金在高压下的晶化

 本文研究了压力对Fe₇₈Si₉B₁₃非晶合金晶化温度的影响。给出了常压及7.5 GPa压力下的时间－温度－相变图。结果指出：晶化温度不仅与压力的大小有关，而且还与热处理的时间因素有关。此外，高压下bcc-Fe(Si)相结晶区域明显变大。     

高压下Al65Co20Mn15合金准晶相得截获及其稳定性的研究

 本文利用高压熔态淬火方法，对Al₆₅Co₂₀Mn₁₅合金进行了研究。首次发现在4.4 GPa压力下淬火的样品中有准晶T相形成。使用电子衍射和X射线衍射对准晶态进行了鉴别。用高温X射线衍射进行了热稳定性研究，发现Al₆₅Co₂₀Mn₁₅合金中准晶T相得晶化温度约为600 ℃。     

高温高压下SrB4O7：Eu2+玻璃的晶化

 利用X射线衍射和Eu²⁺发射光谱方法研究了非晶玻璃SrB₄O₇在高温高压下的晶化。结果表明：在5.0 GPa压力下，200 ℃仍为玻璃态，只有几个强度极低的小峰，表明有晶化的迹象；600 ℃时已基本晶化，但为SrB₄O₇正交相与SrB₄O₇高压立方相二相共存；当温度提高到1 000 ℃时，晶化成了近单相的与常压SrB₄O₇粉末晶体相同的正交结构。伴随晶化度的加强，Eu²⁺发射强度增强，与Ｘ射线衍射结果相一致。     

非晶La80Al20晶化相的超导电性

 本文把非晶La₈₀Al₂₀在真空中、不同温度及其时间条件下进行退火，以及在6 GPa不同温度退火40 min，并对退火样品的相结构及超导性进行了研究。发现真空中，250 ℃退火的样品晶化成了T>4.2 K、不超导的单相四方La₄Al；300 ℃及450 ℃退火的样品晶化成La₃Al、α-La、β-La及一些未知杂相，这些多相混合物的T_C<6.0 K。在6 GPa 300 ℃及以下温度退火的样品，晶化成单相六角La₄Al，其晶格常数与六角La₃Al的完全相同，这些样品的T_C>5.1 K；6 GPa、350 ℃及以上温度退火的样品，晶化成La₃Al相及新未知相H，新相H的T_C约为6.3 K。     

静高压下Al80Mn14Si6合金准晶相形成的研究

 本文首次研究了Al₈₀Mn₁₄Si₆合金在静高压下准晶相得形成。利用静高压熔态淬火方法，在压力2.8和3.1 GPa下得到淬火的Al-Mn-Si样品。电子和X射线衍射实验表明，高压淬火样品中含有准晶二十面体相和非晶相。X射线衍射实验还表明，高压淬火样品经350 ℃退火一小时基本上没有发生变化；而经过500 ℃退火一小时后，准晶相晶化为α-Al₇₃Si₁₀Mn₁₇相。另外，电子衍射实验表明，高压淬火后样品中还存在其它中间亚稳相。本文还讨论了静高压熔态淬火方法的适用性。     

静高压下非晶(Fe0.99,Mo0.01)78Si9B13合金晶化过程的热力学研究

 在600~930 K，常压到7 GPa的范围内，对非晶(Fe_0.99,Mo_0.01)₇₈Si₉B₁₃合金等温等压退火30 min。实验表明：其晶化产物α-Fe(Mo, Si)、Fe₃B和Fe₂B相的析出与所加压力密切相关。压力使非晶(Fe_0.99,Mo_0.01)₇₈Si₉B₁₃合金的晶化温度和亚稳Fe₃B相的析出温度下降，在一定的压力和温度下，亚稳Fe₃B相将向稳定Fe₂B相转变，其转变温度随压力而变化。还对非晶(Fe_0.99,Mo_0.01)₇₈Si₉B₁₃合金的晶化和亚稳Fe₃B到稳定Fe₂B转变的热力学机制进行了讨论，并给出Fe₃B向Fe₂B的相转变方程。     

TiN/TiB2纳米复合材料的合成与性能

 结合高能球磨和高温高压实验技术,制备了块体TiN/TiB₂纳米复合材料。通过X射线衍射和拉曼光谱对材料的微观结构进行了研究。结果表明,采用金属Ti和六方BN为原料,在球磨过程和高温高压实验过程中,TiN先于TiB₂形成,球磨70 h后有少量的纳米晶TiN开始形成。在高温高压实验中,在样品腔的合成温度低于1 300 ℃时,没有TiB₂出现;当温度达到1 300 ℃后,合成出了TiN和TiB₂的复合材料。对所合成的块状材料的热膨胀性和导电性能进行了测试。     

与Al发生扩散反应的非晶(Fe0.99Mo0.01)78Si9B13晶化

 高压下与Al发生扩散反应的非晶(Fe_0.99Mo_0.01)₇₈Si₉B₁₃（FMSB）的晶化产物与纯FMSB的不同。与Al反应的FMSB非晶在3.0~5.0 GPa、780~900 K热处理时,晶化为α-Fe(Al)和次亚稳非晶合金;在这一压力范围以外,720~900 K热处理时,晶化为α-Fe(Si)、Fe₃B或Fe₂B。与Al发生反应的FMSB非晶可能通过与Al的扩散反应在Al/FMSB界面开始晶化。压力和温度对晶化过程的影响主要是由于α-Fe固溶体的Gibbs自由能随压力、温度和Al含量的变化。     

Fe40Ni40P12B8非晶合金的冲击晶化实验研究

 本文研究了Fe₄₀Ni₄₀P₁₂B₈非晶合金冲击波加载下的晶化行为，冲击波由二级轻气炮发射的告诉弹丸撞击靶产生。实验结果表明：Fe₄₀Ni₄₀P₁₂B₈非晶合金在冲击波加载下，晶化可在加载时间（微秒量级）内发生；晶化的阈值压力在30~50 GPa之间，相应的冲击温度约为510~800 K，晶化析出相与冲击压力有关，低压下析出相是面心立方γ-(Fe, Ni)固溶体和Fe₃(P_0.37B_0.63)化合物，高压下（大于60 GPa）析出相除了面心立方γ-(Fe, Ni)固溶体和Fe₃(P_0.37B_0.63)化合物之外，还包括(Fe, Ni)₃P化合物。     

One step ultrafast mechanosynthesis of nanocrystalline cubic Ti0.9Al0.1B and its microstructure evolution

Nanocrystalline single phase cubic Ti_0.9Al_0.1B has been prepared at room temperature in a minimum duration of 4 h by mechanical alloying the stoichiometric mixture of Ti, Al and B powders in a high energy planetary ball mill under argon atmosphere. The Rietveld's structure refinement of X-ray diffraction data reveals that cubic Ti–Al–B phase is initiated just after 1 h of milling and at the same time α-Ti (hcp) phase partially transforms to metastable β-Ti (bcc) phase. In the course of milling, ordered Ti–Al–B lattice gradually transforms to a distorted state and the degree of distortion increases with milling time up to 15 h. The formation of cubic Ti_0.9Al_0.1B is also confirmed from the selected area electron diffraction (SAED) pattern. Microstructure characterization by high resolution transmission electron microscopy (HRTEM) reveals that Ti–Al–B nanoparticles are isotropic in nature with average particle size ~4.5 nm and is in good agreement with the value obtained from the Rietveld analysis of X-ray diffraction data.     

Interfacial reaction of intermetallic compounds of ultrasonic-assisted brazed joints between dissimilar alloys of Ti6Al4V and Al4Cu1Mg

Ultrasonic-assisted brazing of Al4Cu1Mg and Ti6Al4V using Zn-based filler metal (without and with Si) has been investigated. Before brazing, the Ti6Al4V samples were pre-treated by hot-dip aluminizing and ultrasonic dipping in a molten filler metal bath in order to control the formation of intermetallic compounds between the Ti6Al4V samples and the filler metal. The results show that the TiAl(3) phase was formed in the interface between the Ti6Al4V substrate and the aluminized coating. For the Zn-based filler metal without Si, the Ti6Al4V interfacial area of the brazed joint did not change under the effect of the ultrasonic wave, and only consisted of the TiAl(3) phase. For the Zn-based filler metal with Si, the TiAl(3) phase disappeared and a Ti(7)Al(5)Si(12) phase was formed at the interfacial area of the brazed joints under the effect of the ultrasonic wave. Due to the TiAl(3) phase completely changing to a Ti(7)Al(5)Si(12) phase, the morphology of the intermetallic compounds changed from a block-like shape into a lamellar-like structure. The highest shear strength of 138MPa was obtained from the brazed joint free of the block-like TiAl(3) phase.     

Ball milling of Fe40Ni40P20-xSix (x = 6, 10 and 14): production and characterization

Progress in the ball milling amorphization of elemental powders with the overall composition Fe₄₀Ni₄₀P_{20 ? x}Si_x (X = 6, 10 and 14) and thermally induced crystallization of obtained alloys were characterized by differential scanning calorimetry, X-ray diffraction and transmission Mössbauer spectroscopy (TMS). Diffusion of Si into Fe and Ni alloys promotes the formation of the amorphous phase, via previous formation of (Fe, Ni) phosphides. After milling for 32–64 h, most of the powders are amorphous but bcc Fe(Si) crystallites remain (about 5% in volume). TMS results indicate that homogenization of the amorphous phase occurs by interdiffusion of Ni and Fe in Fe(Si,P)-rich and Ni(Si,P)-rich zones respectively. Annealing induces structural relaxation of stresses induced by milling, growth of bcc Fe(Si) crystallites, precipitation of bcc Fe(Si) and fcc Ni–Fe, and minor phases of Ni-rich silicides and (Fe, Ni) phosphides. The main ferromagnetic phase is bcc Fe(Si) for Fe₄₀Ni₄₀P₁₀Si₁₀ powders obtained after milling for 32 h. However, it is fcc Fe–Ni for the same alloy after milling for 64 h. In the later powders, as well as for alloys with x = 6 and 14 milled for 32 h, the fcc Fe–Ni shows the Invar magnetic collapse.     

Investigation of formation mechanism of Ti3SiC2 by high pressure and high-temperature synthesis

ABSTRACT

In this paper, synthesis of titanium silicon carbide (Ti₃SiC₂) under high pressure and high-temperature condition has been investigated by using the reactant systems Ti/Si/C, Ti/SiC/TiC, Ti/SiC/C and Ti/TiC/Si. Results reveal that Ti/TiC/Si is unsuited to the synthesis of Ti₃SiC₂ under a high pressure of 2.0?GPa, while an elemental mixture of Ti/Si/C is applicable. By the addition of Al, Ti₃SiC₂ with 95.8?wt% purity was obtained from elemental mixture with a large excess of silicon. The optimum experimental parameters were determined as Ti/Si/Al/C having the molar ratio of 3:1.5:0.5:1.9, holding at 2.0?GPa and 1300?°C for 60?min.     

Mechanochemical Reactions in Fe2O3–M (M: Al, Ti)

The production of metal–ceramic nanodispersion by mechanical milling of powders through the displacement reaction Fe₂O₃+M→Fe+M-oxide (with M: Al, Ti) was studied. The reaction progress with milling time was followed by recording the temperature and pressure during the process. The samples were characterized by X-ray diffraction and Mössbauer spectroscopy at the intermediate and final stages. In both cases self-sustained reactions were observed with different activation times. The results confirm that mechanical work at room temperature yields the reduction of hematite by Ti and Al. The final oxides were identified as Ti₂O₃ and Al₂O₃, respectively. The dependence of the intermediate and final stages on the milling conditions and the starting composition will be discussed.     

Interaction behaviors at the interface between liquid Al–Si and solid Ti–6Al–4V in ultrasonic-assisted brazing in air

Power ultrasonic vibration (20 kHz, 6 μm) was applied to assist the interaction between a liquid Al–Si alloy and solid Ti–6Al–4V substrate in air. The interaction behaviors, including breakage of the oxide film on the Ti–6Al–4V surface, chemical dissolution of solid Ti–6Al–4V, and interfacial chemical reactions, were investigated. Experimental results showed that numerous 2–20 μm diameter-sized pits formed on the Ti–6Al–4V surface. Propagation of ultrasonic waves in the liquid Al–Si alloy resulted in ultrasonic cavitation. When this cavitation occurred at or near the liquid/solid interface, many complex effects were generated at the small zones during the bubble implosion, including micro-jets, hot spots, and acoustic streaming. The breakage behavior of oxide films on the solid Ti–6Al–4V substrate, excessive chemical dissolution of solid Ti–6Al–4V into liquid Al–Si, abnormal interfacial chemical reactions at the interface, and phase transformation between the intermetallic compounds could be wholly ascribed to these ultrasonic effects. An effective bond between Al–Si and Ti–6Al–4V can be produced by ultrasonic-assisted brazing in air.     

Study of the gradual interface between hydroxyapatite thin films PLD grown onto Ti-controlled sublayers

Hydroxyapatite thin films were grown on layered structures by Pulsed Laser Deposition with the goal of investigating the interface of the ceramic film with the substrate. The latter consisted of Si/TiN/Ti sandwich structures. This multilayer substrate was also prepared by laser ablation earlier in the same experimental session.This particular type of structure was chosen in order to induce the in situ growth of hydroxyapatite directly onto freshly deposited Ti. We tried this way to avoid previous direct Ti exposure to air, hence its oxidation. The subsequent depositions of multilayers were performed with the aid of a carousel multi-target system mounted inside the irradiation chamber. This allowed for selecting in order the respective TiN, Ti and HA targets without opening the chamber between individual depositions.X-ray diffractometry, transmission electron microscopy and selected area electron diffractometry studies revealed the formation at the interface of a transition complex phase, 2 to 25 nm thick, consisting of a mixture of TiO₂ and CaP phase. The specific growth of TiN and Ti phases was also investigated.     

Effects of Raw Material Content on Efficiency of TiN Synthesized by Reactive Ball Milling Ti and Urea

Ti and urea mixed according to the molar ratios of 2：1, 3：1 and 4：1 axe milled under the same condition. The structures of the as-synthesized powders are analyzed by an x-ray diffractometer （XRD）. The decomposed temperature of the urea and the products decomposed are characterized by differential scanning calorimetry （DSC） and thermogravimetry analysis-Fourier transform infrared （TG-FTIR） spectrometry. The results show that the reaction progress is a diffusion reaction. The efficiency of TiN synthesized by reactive ball milling can be increased by increasing the content of Ti. The reactive ball milling time decreases from more than 90 h to 40 h correspond- ing to the content ratio between Ti and urea increasing from 2：1 to 4：1. Ammonia gas （NH3） and cyanic acid （HNCO）, the decomposed products of urea, react with the refined Ti to form TiN. The grain refinement of Ti has a significant effect on the efficiency of reactive ball milling.     

Silica-based composite and mixed-oxide nanoparticles from atmospheric pressure flame synthesis

Binary TiO₂/SiO₂ and SnO₂/SiO₂ nanoparticles have been synthesized by feeding evaporated precursor mixtures into an atmospheric pressure diffusion flame. Particles with controlled Si:Ti and Si:Sn ratios were produced at various flow rates of oxygen and the resulting powders were characterized by BET (Brunauer–Emmett–Teller) surface area analysis, XRD, TEM and Raman spectroscopy. In the Si–O–Ti system, mixed oxide composite particles exhibiting anatase segregation formed when the Si:Ti ratio exceeded 9.8:1, while at lower concentrations only mixed oxide single phase particles were found. Arrangement of the species and phases within the particles correspond to an intermediate equilibrium state at elevated temperature. This can be explained by rapid quenching of the particles in the flame and is in accordance with liquid phase solubility data of Ti in SiO₂. In contrast, only composite particles formed in the Sn–O–Si system, with SnO₂ nanoparticles predominantly found adhering to the surface of SiO₂ substrate nanoparticles. Differences in the arrangement of phases and constituents within the particles were observed at constant precursor mixture concentration and the size of the resultant segregated phase was influenced by varying the flow rate of the oxidant. The above effect is due to the variation of the residence time and quenching rate experienced by the binary oxide nanoparticles when varying the oxygen flow rate and shows the flexibility of diffusion flame aerosol reactors.     

非晶FeMoSiB合金机械晶化的动力学机制

 研究了非晶(Fe_0.99Mo_0.01)₇₈Si₉B₁₃（FMSB）合金的机械晶化过程和机制,并讨论了局域高压的作用。结果表明：非晶FMSB合金的晶化过程及其产物与球磨强度和球磨时间有密切关系,在低能球磨FMSB非晶过程中,晶化相只有α-Fe(Mo,Si)固溶体,而在高能球磨过程中,除了α-Fe(Mo,Si)固溶体结晶相之外,还分别有(Fe,Mo)₃B和Fe₂B相析出。其晶化机制可归因于由碰撞引起的局域高压和局域高温共同作用的结果。实验结果还表明,机械球磨不仅对非晶FMSB的常压热晶化温度有重要影响,而且对其热晶化结果亦有重要影响。