Microstructural and mechanical properties of Al-Mg/Al2O3 nanocomposite prepared by mechanical alloying

The effect of milling time on the microstructure and mechanical properties of Al and Al-10 wt.% Mg matrix nanocomposites reinforced with 5 wt.% Al₂O₃ during mechanical alloying was investigated. Steady-state situation was occurred in Al-10Mg/5Al₂O₃ nanocomposite after 20 h, due to solution of Mg into Al matrix, while the situation was not observed in Al/5Al₂O₃ nanocomposite at the same time. For the binary Al-Mg matrix, after 10 h, the predominant phase was an Al-Mg solid solution with an average crystallite size 34 nm. Up to 10 h, the lattice strain increased to about 0.4 and 0.66% for Al and Al-Mg matrix, respectively. The increasing of lattice parameter due to dissolution of Mg atom into Al lattice during milling was significant. By milling for 10 h the dramatic increase in microhardness (155 HV) for Al-Mg matrix nanocomposite was caused by grain refinement and solid solution formation. From 10 to 20 h, slower rate of increasing in microhardness may be attributed to the completion of alloying process, and dynamic and static recovery of powders.     

Microstructural characterization and amorphous phase formation in Co40Fe22Ta8B30 powders produced by mechanical alloying

In this work, microstructural evolution and amorphous phase formation in Co₄₀Fe₂₂Ta₈B₃₀ alloy produced by mechanical alloying (MA) of the elemental powder mixture under argon gas atmosphere was investigated. Milling time had a profound effect on the phase transformation, microstructure, morphological evolution and thermal behavior of the powders. These effects were studied by the X-ray powder diffraction (XRD) in reflection mode using Cu Kα and in transmission configuration using synchrotron radiation, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The results showed that at the early stage of the milling, microstructure consisted of nanocrystalline bcc-(Fe, Co) phases and unreacted tantalum.Further milling, produced an amorphous phase, which became a dominant phase with a fraction of 96 wt% after 200 h milling. The DSC profile of 200 h milled powders demonstrated a huge and broad exothermic hump due to the structural relaxation, followed by a single exothermic peak, indicating the crystallization of the amorphous phase. Further XRD studies in transmission mode by synchrotron radiation revealed that the crystalline products were (Co, Fe)_20.82Ta_2.18B₆, (Co, Fe)₂₁ Ta₂ B₆, and (Co, Fe)₃B₂. The amorphization mechanisms were discussed in terms of severe grain refinement, atomic size effect, the concept of local topological instability and the heat of mixing of the reactants.     

Mechanical alloying and spark plasma sintering of the intermetallic compound Ti50Al50

This study investigates the microstructures and mechanical properties of Ti₅₀Al₅₀ alloys prepared via mechanical alloying (MA) starting from elemental powders. The process of the spark plasma sintering (SPS) has also been studied. It is found that the nanocrystallization process of the Ti–Al alloy proceeds and the sintering temperature can control the microstructure of alloy. The sintering of the compacts is carried out at the temperatures of 1100–1200 °C with a compaction pressure of 30 MPa and a heating rate of 30 °C min⁻¹. Specimens with high densities and approaching the equilibrium state can be obtained in short time by spark sintering than conventional sintering. Such shorter high temperature is important to prevent grain growth.     

Calorimetric and structural analysis of the new phase Al33Ni16Zr51 produced by direct synthesis and mechanical alloying

A new phase has been synthesized in the ternary phase diagram Al–Ni–Zr: its nominal composition is Al₃₃Ni₁₆Zr₅₁. For the Al₃₃Ni₁₆Zr₅₁ compound obtained by mixing the three components in suitable proportions, a study has been carried out by direct synthesis (calorimetry) and mechanical alloying in our laboratory. With the first method we know directly the enthalpy of formation of this alloy. For the amorphous alloys prepared by mechanical alloying we can determine the crystallisation enthalpy with the differential scanning calorimetry (DSC) method. So it is possible to determine a fundamental piece of information: the amorphous alloy formation enthalpy.     

Direct synthesis of MgCNi3 by mechanical alloying

MgCNi₃, an intermetallic compound with superconductivity, was synthesized from the Mg (or Mg₂Ni), Ni and graphite powders by mechanical alloying (MA). It is shown that the preliminary condition for the formation of MgCNi₃ is that Mg₂Ni must form in advance of MgCNi₃ in the MA process or be the starting component.     

ZrOCl2-Al体系熔体反应生成Al3Zr(p), Al2O3(p)/Al复合材料的反应机制

利用X射线衍射仪(XRD)和扫描电子显微镜(SEM),对ZrOCl     

Consolidation and mechanical properties of ball milled Zr50Cu50 glassy ribbons

Bulk Zr₅₀Cu₅₀ partially crystallized glassy specimens have been produced by powder metallurgy methods. Zr₅₀Cu₅₀ powder has been prepared by controlled milling of melt spun glassy ribbons and subsequently consolidated by hot pressing into bulk cylindrical samples of 10 mm diameter and 10 mm length. The consolidated material exhibits interesting mechanical properties, namely, a perfect elastic regime of 1.5%, high strength of about 1350 MPa and hardness of 4.80 GPa. However, no macroscopic ductility is visible, most likely due to the residual porosity of the consolidated specimens. These results indicate that powder metallurgy methods may become a valid alternative to casting techniques for the production of glassy and partially crystallized Zr-based alloys.     

Synthesis of TiC–Al2O3 nanocomposite powder from impure Ti chips, Al and carbon black by mechanical alloying

The possibility of providing TiC–Al₂O₃ nanocomposite as a useful composite from low-cost raw materials has been investigated. Impure Ti chips were placed in a high energy ball mill with carbon black and aluminum powder and sampled after different times. XRD analysis showed that TiC has been synthesized after 10 h of milling. It could be observed from the width of XRD patterns’ peaks that the size of produced TiC crystallites is in the order of nanometer. In order to forming of TiC–Al₂O₃ composite, heat treatment was performed in different temperatures. Investigations have revealed that formation temperature of TiC as the dominant phase decreased for the milled specimens during heat treatment, also nanocrystalline TiC–Al₂O₃ composite was formed in this situation. Furthermore milling led to increase of strain and decrease of TiC lattice parameter while during heat treatment nanocrystalline grains grow up and strain decreases.     

MoSi_2含量对MoSi_2/Al_2O_3复合涂层介电与力学性能的影响(英文)

通过喷雾干燥法制备MoSi2包覆Al2O3的壳核结构混合粉,利用该混合粉以等离子喷涂技术制备MoSi2/Al2O3复合涂层材料。研究MoSi2/Al2O3质量比涂层材料的力学和介电性能的影响。结果表明:随着MoSi2含量从0增加到45%,复合材料的抗弯强度和断裂韧性分别从198MPa和3.05MPa·m1/2增加到324MPa和4.82MPa·m1/2,随后又降到310MPa和4.67MPa·m1/2。在8.2-12.4GHz微波频率波段内,随着MoSi2含量的增加,复合材料的介电损耗增加,而介电常数的实部却呈减小趋势。这主要是由于MoSi2颗粒熔化后的凝聚及导电网络结构的形成导致电导率的增加引起的。     

Investigation of reaction between LiNH2 and H2

The reactions for LiNH₂ under a H₂ and an Ar flow were investigated, respectively. The results showed that LiNH₂ can be converted into LiH and NH₃ by reacting with H₂ under a H₂ flow condition, whereas LiNH₂ is converted into Li₂NH and NH₃ by decomposition under an Ar flow. Moreover, the reaction between LiNH₂ and H₂ can be accelerated by mixing LiNH₂ with LiH as well as doping LiNH₂ with TiCl₃. The confirmation of reaction between LiNH₂ and H₂ is helpful for the deeper insight in the systems of Li–N–H and Li–Mg–N–H for hydrogen storage materials.     

Thermoelectric properties of Fe0.98Co0.02Si2 with ZrO2 and rare-earth oxide dispersion by mechanical alloying

The n-type Co-doped β-FeSi₂ (Fe_0.98Co_0.02Si₂) with dispersion of several oxides, such as ZrO₂ or several rare-earth oxides (Y₂O₃, Nd₂O₃, Sm₂O₃ and Gd₂O₃), was synthesized by mechanical alloying and subsequent hot pressing. The effects of these oxide dispersions on the thermoelectric properties of Fe_0.98Co_0.02Si₂ were investigated. ZrO₂ was decomposed in the β phase, and the ZrSi and -FeSi phases, which are metallic phases, were formed in the samples with ZrO₂ addition. The Seebeck coefficient and the electrical resistivity were significantly decreased with increasing amount of ZrO₂, indicating that a part of the Zr atoms was substituted for Fe atoms in the β phase. In the case of the samples with rare-earth oxide addition, a decomposition of a large amount of these added oxides did not occur. However, the rare-earth oxide addition caused a slight increase in the amount of the phase. The Seebeck coefficient was significantly enhanced by the rare-earth oxide addition especially in the low temperature range. These facts indicated that a small amount of rare-earth oxides was decomposed in the β phase, and rare-earth elements were substituted for Fe atoms as a p-type dopant, resulting in the decrease in the carrier concentration. The rare-earth oxide addition was also effective in reducing the thermal conductivity.     

Complete flux jumping in nano-structured MgB2 superconductors prepared by mechanical alloying

High density nano-crystalline MgB₂ bulk superconductors with induced pinning centres were prepared from elemental precursors by a sequence of ball milling, heat treatment, and final pressing. The XRD results revealed the main phase was MgB₂ with a minor component of MgO. The magnetic moment versus temperature indicated that the transition temperature of MgB₂ samples was around 34 K, which is less than the typical transition temperature of commercial powders and also the transition temperature strongly depended on the milling time. It is well known that introduction of defects, grain boundaries and impurities act as effective flux pinning centres in MgB₂ and results in increased critical current density, J_c and decreased the transition temperature, T_c. The magnetization measurements were performed using VSM at 10 K, 20 K and 30 K, and the M–H curves indicated a complete flux jump effect, which is a severe problem for the application of superconductors. It was determined that a noticeable amount of heating (0.3 K jumps at 10 K) occurs at these jumps. In addition, it was found that the sweeping rate of magnetic field and the size of bulk sample are very effective to promote the flux jumping and whereas a low sweeping rate (12 Oe/s) avoids these “avalanches”, consistent with a kind of supercritical phenomenon: going slower allows the field gradients to stay close enough to equilibrium so that the avalanche effect is not triggered. In contrast, the sweeping rate of 100 Oe/s leads to numerous jumps.     

Nb-Cr掺杂原位合成Al2O3/TiAl复合材料的组织与性能

采用原位热压工艺,在Ti-Al-TiO2-Nb2O5体系中加入Cr2O3原位合成Al2O3/TiAl复合材料.借助X射线衍射分析、SEM分析及力学性能分析,研究了Nb-Cr掺杂复合强化Al2O3/TiAl复合材料的反应过程、微观结构及力学性能.结果表明Nb-Cr掺杂原位合成Al2O3/TiAl复合材料能够细化晶粒并通过微合金化增强增韧TiAl复合材料.     

Improvement in hydrogen sorption properties of Mg by reactive mechanical grinding with Cr2O3, Al2O3 and CeO2

We tried to improve the hydrogen sorption properties of Mg by mechanical grinding under H₂ (reactive mechanical grinding) with oxides Cr₂O₃, Al₂O₃ and CeO₂. The hydriding rates of Mg are reportedly controlled by the diffusion of hydrogen through a growing Mg hydride layer. The added oxides can help pulverization of Mg during mechanical grinding. A part of Mg is transformed into MgH₂ during reactive mechanical grinding. The Mg+10wt.%Cr₂O₃ powder has the largest transformed fraction 0.215, followed in order by Mg+10wt.%CeO₂ and Mg+10wt.%Al₂O₃. The Mg+10wt.%Cr₂O₃ powder has the largest hydriding rates at the first and fifth hydriding cycle, followed in order by Mg+10wt.%Al₂O₃ and Mg+10wt.%CeO₂. Mg+10wt.%Cr₂O₃ absorbs 5.87wt.% H at 573 K, 11 bar H₂ during 60 min at the first cycle. The Mg+10wt.%Cr₂O₃ powder has the largest dehydriding rates at the first and fifth dehydriding cycle, followed by Mg+10wt.%CeO₂ and Mg+10wt.%Al₂O₃. It desorbs 4.44 wt.% H at 573 K, 0.5 bar H₂ during 60 min at the first cycle. All the samples absorb and desorb less hydrogen at the fifth cycle than at the first cycle. It is considered that this results from the agglomeration of the particles during hydriding–dehydriding cycling. The average particle sizes of the as-milled and cycled powders increase in the order of Mg+10wt.%Cr₂O₃, Mg+10wt.%Al₂O₃ and Mg+10wt.%CeO₂. The quantities of hydrogen absorbed or desorbed for 1 h for the first and fifth cycles decrease in the order of Mg+10wt.%Cr₂O₃, Mg+10wt.%Al₂O₃ and Mg+10wt.%CeO₂. The quantities of absorbed or desorbed hydrogen increase as the average particle sizes decrease. As the particle size decreases, the diffusion distance shortens. This leads to the larger hydriding and dehydriding rates. The Cr₂O₃ in the Mg+10wt.%Cr₂O₃ powder is reduced after hydriding–dehydriding cycling. The much larger chemical affinity of Mg than Cr for oxygen leads to a reduction of Cr₂O₃ after cycling.     

Al—ZrOCl2反应体系制备ZrAl3（p）＋Al2O3（p）／Al复合材料

从Al-ZrOCl2体系利用熔体直接反应法制备了原位ZrAl3和Al2O3颗粒增强铝基复合材料。Al-Zr－O体系中原位形成的ZrAl3具有四方结构,其最大尺寸为4μm,纵横长度比小于2．0,此外,还有一定数量的亚微米级Al2O3颗粒生成,其晶体为六方结构,纵横长度比大于2．0.ZrAl3(p),Al2O3(p)/Al复合材料凝固组织,随ZrOCl2加入量的增加,生成的颗粒尺寸更小,分布更均匀,拉伸试验表明,Al-ZrOCl2体系的复合材料具有高度的强度和逆性,断口组织存在大量韧窝,韧窝中镶嵌嵌着细小颗粒,属韧性断裂。     

Hf6Ta2O17材料的合成和热膨胀性能

以HfO2、Ta2O5粉体为原料,采用固相法合成Hf6Ta2O17材料。在空气气氛下1600℃常压烧结8h制备块体试样。用X射线衍射(XRD)仪检测合成粉体的相结构,通过场发射扫描电镜(SEM)观察试样的微观形貌,用热膨胀仪检测试样的热膨胀系数(TEC)。结果表明:固相法可以制备纯净单相的Hf6Ta2O17材料和比较致密的块体试样;Hf6Ta2O17材料在20~1400℃温度范围内没有相变,其高温相稳定性优于YSZ材料;Hf6Ta2O17在1200℃的热膨胀系数为9.59×10-6/℃,与YSZ材料的热膨胀系数接近,有望用于热障涂层。     

Kinetics and formation mechanism of amorphous Fe52Nb48 alloy powder fabricated by mechanical alloying

A single phase amorphous Fe₅₂Nb₄₈ alloy has been synthesized through a solid state interdiffusion of pure polycrystalline Fe and Nb powders at room temperature, using a high-energy ball-milling technique. The mechanisms of metallic glass formation and competing crystallization processes in the mechanically deformed composite powders have been investigated by means of X-ray diffraction, Mössbauer spectroscopy, differential thermal analysis, scanning electron microscopy and transmission electron microscopy. The numerous intimate layered composite particles of the diffusion couples that formed during the first and intermediate stages of milling time (0–56 ks), are intermixed to form amorphous phase(s) upon heating to about 625 K by so-called thermally assisted solid state amorphization, TASSA. The amorphization heat of formation for binary system via the TASSA, ΔH_a, was measured directly as a function of the milling time. Comparable with the TASSA, homogeneous amorphous alloys were fabricated directly without heating the composite multilayered particles upon milling these particles for longer milling time (86 ks–144 ks). The amorphization reaction here is attributed to the mechanical driven solid state amorphization. This single amorphous phase transforms into an order phase (μ phase) upon heating at 1088 K (crystallization temperature, T_x) with enthalpy change of crystallization, ΔH_x, of −8.3 kJ mol⁻¹.     

Magnetic properties of (Fe)1−x–(Al2O3)x and (Fe50Ni50)1−x–(Al2O3)x nanocomposite magnetic media synthesized using gel like Al2O3 matrix

Composites with ferromagnetic nanoparticles, Fe and Fe₅₀Ni₅₀, dispersed in Al₂O₃ have been synthesized by a solution phase technique. The structure and magnetic properties of these composites with varying fractions of Al₂O₃ have been investigated. Both Fe and Fe₅₀Ni₅₀ nanoparticles are amorphous in the as-prepared state and become crystalline on heat treating with near equilibrium lattice parameters of 0.287 nm and 0.358 nm respectively. The interparticle distance increases with increasing Al₂O₃ from 0 wt.% to 20 wt.%. The size of Fe nanoparticles is 40 nm while the Fe₅₀Ni₅₀ nanoparticles are 20 nm in size. The Fe and Fe₅₀Ni₅₀ nanoparticles dispersed composites are found to be ferromagnetic at room temperature both in the as-prepared and heat treated conditions with clear coercive fields of 5.5–35 × 10³ A m⁻¹. The saturation magnetization increases by orders of magnitude on heat treatment, for e.g. from <1.0 emu g⁻¹ to 143.4 emu g⁻¹ for Fe–15 wt.% Al₂O₃ and 95.6 emu g⁻¹ for Fe₅₀Ni₅₀–15 wt.% Al₂O₃. The Fe-composites exhibit a Curie transition at 1000 K while the Fe₅₀Ni₅₀ composites exhibit a transition at 880 K, both temperatures close to bulk values.     

Crystallisation of oxygen-stabilised amorphous phase in a Zr50Cu50 alloy

The crystallisation of the oxygen-stabilised amorphous phase in a Zr₅₀Cu₅₀ alloy has been investigated by means of neutron diffraction and electron microscopy. The crystallisation microstructure consists of ZrO₂, Zr₂Cu and Zr₇Cu₁₀. A two-stage crystallisation mechanism is suggested: (i) primary crystallisation of Zr₂Cu and (ii) formation of nanocrystals ZrO₂ and Zr₇Cu₁₀. In (i), it is proposed, Zr₂Cu crystallises from the oxygen-stabilised amorphous phase, leaving an oxygen- and copper-enriched matrix ; Zr₂Cu rapidly grows and eventually attains a grain size of about 100 nm. In (ii), it is suggested, the residual amorphous matrix crystallises into nanocrystals ZrO₂ and Zr₇Cu₁₀ due to the sluggish growth of ZrO₂ and to the already formed ZrO₂ which acts as a growth barrier to Zr₇Cu₁₀. In this case there is no particular orientation relationship between Zr₂Cu and Zr₇Cu₁₀.