Microstructures and mechanism of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/Al composites fabricated by the reaction between SiO<Subscript>2</Subscript> and molten aluminum

Al₂ O₃/Al composite was fabricated by the reaction between SiO₂ and molten aluminum. The microstructures of the composite obtained under different reaction conditions were analyzed. The formation mechanism of the composite microstructure was discussed. Results show that the reaction kinetics is influenced remarkably by the reaction temperature, reaction time and the quantity of SiO₂. The morphologies of Al₂O₃ have different features, depending on the reaction temperature. The composite has equaxed Al₂O₃ grains when materials reacted below 1200°C, and the composite is composed of a large number of fine Al₂O₃ grains and aluninum. The composite has a frame-shaped Al₂O₃ microstructure at the reaction temperature of above 1250°C. CHENG Xiao-min: Born in 1964 Funded by the National Natural Science Foundation of China (No. 91522)     

Self-Propagating High-Temperature Reduetive Synthesis of TiB2-Al2O3 Composite Powders

TiB2-Al2O3 composite powders were produced by self-propagating high-temperature synthesis（SHS） method with reductive process from B2O3-TiO2-AI system. X-ray diffraction（XRD） and scanning electron microscopy（SEM） analyses show the presence of TiB2 and Al2O3 only in the composite powders produced by SHS. The powders are uniform and free-agglomerate. Transmission electron microscopy （TEM） and high resolution electron microscopy （HREM） observation of microstructure of the composite powders indicate that the interfaces of the TiB2-Al2O3 bond well, without any interfacial reaction products. It is proposed that the good interfacial bonding of the composite powders can be resulted from the TiB2 particles crystallizing and growing on the Al2O3 particles surface with surface defects acting as nucleation centers.     

Effect of matrix composition on physical properties of Al<Subscript>3</Subscript>CON in-situ reaction reinforced corundum composite

60% white corundum used for aggregate, 5% aluminium powder for fixed additions and 35% various additives for matrix were prepared for specimens 1#,2#,3#. They were mixed uniformly with the suitable resin as a binder and pressed under pressure of 315 ton forging press, then dried at 200℃ for 24 h. Effects of various additives on 1500 ℃×2 h creep properties of Al3CON reinforced corundum composite were researched. The experimenal results show that creep coefficients of specimens 1#,2#,3# at 1500 ℃×2 h are 1.4×10^- 4, -9.4×10^-4, -22.6×10^-4, respectively. Crushing strength of the slide plate added with suitable additive A after fired at 1500 ℃ ×3 h reaches to 225 MPa, the creep rate is positive all the time from 0% to 0.014% at 1500 ℃ for 2 h. The microstructure result analysis shows that reinforced phases of Al3CON fiber composite have been formed after fired with Al powder in coke at high temperatures for specimen 1#, and the strength of the composite is increased. The hot modulus of rupture is up to 59 MPa at 1400 ℃ and the RUL is obviously higher than that at 1700 ℃. Its service life is two times as that of Al2O3-C slide plate when used in the process of pouring steel. The mechanism of creep rate resistance of the composites can be discovered by means of SEM and EDAX analysis. It is concluded that the active Al3CON and Al2O3 multiphases that were formed by N2 in gas, C, Al and Al2O3 inside the matrix of the composites during in-situ reaction,which gives the composites outstanding creep rate resistance for the dense zone resuiting from Al3CON oxidation that inhibits contraction at the high temperature. Besides, the matrix will turn into the multiphase with high refractoriness, N content and its Al3CON reinforced fiber will further increase accordingly. In addition, Al3CON formed by Al2O3 and C, Al in the matrix with N2 in gas will inhibit the creep rate and also greatly improve the creep rate resistance of the composites.     

复合活性钎料钎焊Cu与Al2O3的接头组织及性能

为改善紫铜与Al_2O_3陶瓷的连接强度,采用纳米-Al_2O_3增强的AgCuTi复合钎料(Ag Cu Tip)对紫铜与Al_2O_3陶瓷进行了真空钎焊.采用扫描电镜、能谱分析以及剪切试验对钎焊接头微观组织及力学性能进行了分析.钎焊接头典型界面组织为紫铜/扩散层/铜基固溶体+银基固溶体+Ti_2Cu+Ti_3(Cu,Al)3O/Al_2O_3.纳米-Al_2O_3的添加抑制了Al_2O_3侧反应层的生长,并促进钎缝中形成弥散分布的Ti_2Cu相.随着保温时间的延长,铜侧扩散层和Ti_3(Cu,Al)_3O反应层的厚度逐渐增大.保温时间为20 min时,铜母材向钎料过度溶解,降低了接头性能.当钎焊温度为880°C,保温10 min时,接头抗剪强度最高为82 MPa.纳米颗粒的加入细化了钎缝组织并降低了母材与钎缝热膨胀系数的不匹配,因此提高了接头的连接性能.保温时间可影响界面组织及反应层的厚度,进而影响接头的连接强度.     

Microstructure and mechanical properties of submicron-grained NiAl-Al2O3 composite prepared by pulse current auxiliary sintering

Dense and submicron-grained NiAl-Al2O3 composite was fabricated by pulse current auxiliary sintering(PCAS).Its microstructure was analyzed by XRD,SEM and TEM,and its mechanical behavior was evaluated through compression test and fracture toughness test.The average grain sizes of NiAl and Al2O3 are about 200 nm and 100 nm respectively.The Al2O3 particles dispersed in NiAl matrix,forming intergranular structure and intragranular structure.During sintering,Al2O3 particles were remarkably spherized due to the unique sintering mechanism of PCAS,which is beneficial to the improvement of toughness.The NiAl-Al2O3 composite exhibits high compressive yield strength,whether at room temperature or elevated temperature.Its room-temperature(23 ℃) and elevated-temperature(1 200 ℃) compressive yield strength are up to 2 050 MPa and 140 MPa,respectively.Meanwhile,its fracture toughness is significantly enhanced,which is up to 8.2 MPa?m1/2.It is suggested that the main strengthening-toughening mechanisms are grain refinement strengthening and Al2O3 dispersion strengthening.The fracture of larger NiAl grain is the transgranular cleavage and this is induced by crack tip deflection and grain boundary weakening which are caused by intergranular and intragranular Al2O3 particles,respectively.     

铝热法合成NiAl／Al2O3复合材料

以铝粉和NiO粉为原料,采用铝热法合成了NiAl／Al2O3复合材料。通过X射线衍射分析仪（XRD）,扫描电子显微镜（SEM）并结合差示扫描量热仪（DSC）对其相组成、微结构和反应过程进行了分析。实验结果表明：850℃Al／NiO体系铝热反应被点燃,并自蔓延发生于整个反应系统;950℃保温40min,Al／Ni0体系铝热反应生成相互交织网状结构的NiAl／Al2O3复合材料。     

The influence of mo additive on the microstructure and property of Ti/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composite

The influence of Mo on the microstructure, bending strength and HV of Ti/Al₂O₃ composite was studied, and the influence mechanism was analyzed. The results indicate that after the addition of Mo, the composite organization is finer and phases distribution is better-proportioned which make the microstructure denser, the bending strength and HV of composite are also increased to a degree. But the bending strength increases first then decreases with the increasing of Mo content, so the appropriate Mo content for the Ti/Al₂O₃ composite is to be further confirmed. WANG Zhi: Born in 1962 Funded by Natural Science Foundation of China (No. 50232020) and Natural Science Foundation of Shandong Province (No. 2002F21)     

Preparation of LiFePO4 for lithium ion battery using Fe2P2O7 as precursor

In order to obtain a new precursor for LiFePO4, Fe2P2O7 with high purity was prepared through solid phase reaction at 650 ℃ using starting materials of FeC2O4 and NH4H2PO4 in an argon atmosphere. Using the as-prepared Fe2P2O7, Li2CO3 and glucose as raw materials, pure LiFePO4 and LiFePO4/C composite materials were respectively synthesized by solid state reaction at 700 ℃ in an argon atmosphere. X-ray diffractometry and scanning electron microscopy（SEM） were employed to characterize the as-prepared Fe2P2O7, LiFePO4 and LiFePO4/C. The as-prepared Fe2P2O7 crystallizes in the Cl space group and belongs to β-Fe2P2O7 for crystal phase. The particle size distribution of Fe2P2O7 observed by SEM is 0.4-3.0 μm. During the Li^＋ ion chemical intercalation, radical P2O7^4- is disrupted into two PO4^3- ions in the presence of O^2-, thus providing a feasible technique to dispose this poor dissolvable pyrophosphate. LiFePO4/C composite exhibits initial charge and discharge capacities of 154 and 132 mA·h/g, respectively.     

Preparation of Al2O3-SiO2-TiO2-ZrO2 Composite Ceramic Membranes by Sol-Gel Method

Al2O3-SiO2- TiO2-ZrO2 supported membranes were prepared by Sol-Gel method. These composite ceramic membranes are level, even and no macro crack. There exist several crystalline phases such as Al2O3, TiO2 ( anatase ), Al2 SiO5 , and ZrO2 in these membranes. Changing the molar ratio of Al:Si: Ti : Zr ,the kinds and content of crystal phases of composite membranes could be different, which may lend to a variety of microstructure of membranes. The surface nanoscale topography and microstructure of membranes were investigated by XRD, SEM, AFM, EPMA. The effects of additives and heat treatments on the surface nanoscale topography and microstracture of composite ceramic membranes were also analyzed.     

Effect of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> content on residual stress and properties of CAS glass-ceramics

The structure and properties of the glass-ceramics were tested with X-ray diffraction testing instrument,correlative software,and other modern testing means.Then the effect of Al2O3 content on internal stresses in CaO-Al2O3-SiO2 glass-ceramics was studied deeply.In order to study the relationship of Al2O3 to the residual stress of CaO-Al2O3-SiO2 glass-ceramics,X-ray diffraction ＂sin2ψ＂ was used.The means utilized the x radial incidence produced from cathode radial tube,and took the space between crystals as measurement of strain.When the stresses produced,the space between crystals changed and the diffraction peak moved during Bragg diffraction.The magnitude of movement is related to the stresses.The experimental results show the residual stress is considerably high and Al2O3 can influence the mechanical properties of this material hugely.     

Effect of Nb on the mechanical properties of Ti/Al2O3 composite

Ti/Al₂O₃ composite with improved mechanical properties was synthesized by the spark plasma sintering. The effect of Nb on the microstructure of the composite was analyzed by TEM, SEM and so on. The experimental results indicate that the bending strength, fracture toughness, micro-hardness and relative density of the composite are 897.29MPa, 17.38MPa·m^1/2, 17.13GPa and 99.24% respectively when adding 1.5vol Nb. The bending strength is improved by reason of forming dislocation ring and transfering fracture mode from integranular to mixture fracture of intergranular and transgranular. The crack propagating is mainly the deflection bridging. It indicates a reduction of crack driving force and an increase in crack growth resistance, which results in toughness enhanced. Funded by the National Natural Science Foundation of China (No. 50232020) and the Natural Science Foundation of Shandong Province (No. 2002F21)     

Microstructures and Properties of SiC／Al2O3 ／Al- Si Composites Prepared by Reactive Penetration

The composition, microstructures and properties of SiC/Al2O3/Al-Si composites formed by reactive penetration of the molten aluminum into the preforms of SiO2 and SiC were investigated. The composition of the composites was measured by X-ray diffraction ( XRD ). The microstructures of the composites were also measured by scanning electron microscopy (SEM) and optical microscopy. In addition, the factors affecting the properties of the composites were discussed. The experiments show that the mechanical properties of the composites depend on their relative densities and the sizes of the fillers“ SiC gains“. The denser the SiC/Al2O3/Al-Si composites, the higher their bending strength. As the filler “SiC gains“ become fine, the bending strength of the composites increases.     

High-temperature oxidation behavior of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/TiAl matrix composite in air

The oxidation behavior of Al₂O₃/TiAl in situ composites fabricated by hot-pressing technology was investigated at 900° in static air. The results indicate that the mass gains of the composites samples decrease gradually with increasing Nb₂O₅ content and the inert Al₂O₃ dispersoids effectively increase the oxidation resistance of the composites. The higher the Al₂O₃ dispersoids content, the more pronounced the effect. The primary oxidation precesses obey approximately the linear laws, and the cyclic oxidation precesses follow the parabolic laws. The oxidized sample containing Ti₂AlN and TiAl phases in the scales exhibits excellent oxidation resistance. The oxide scale formed after exposure at 900°C for 120 h is multiple-layered, consisting mainly of an outer TiO₂ layer, an intermediate Al₂O₃ layer, and an inner TiO₂+Al₂O₃ mixed layer. From the outer layer to the inner layer, TiO₂+Al₂O₃ mixed layer presents the transit of Al-rich oxide to Ti-rich oxide mixed layer. Near the substrate, cross-section micrograph shows a relatively loose layer, and micro- and macro-pores remain on this layer, which is a transition layer and transferres from Al₂O₃+TiO₂ scale to substrate. The thickness of oxide layer is about 20 μm. It is also found that continuous protective alumina scales can not be observed on the surface of oxidation scales. Ti ions diffuse outwardly to form the outer TiO₂ layer, while oxygen ions transport inwardly to form the inner TiO₂+Al₂O₃ mixed layer. Under long-time intensive oxidation exposure, the internal Al₂O₃ scale has a good adhesiveness with the outer TiO₂ scale. No obvious spallation of the oxide scales occurs. The increased oxidation resistance by the presence of in situ Al₂O₃ particulates is attributed to the enhanced alumina-forming tendency and thin and dense scale formation. Al₂O₃ particulates enhance the potential barrier of Ti ions from M/MO interface to O/MO interface, thereby the TiO₂ growth rate decreases, which is also beneficial to improve the oxidation resistance. Moreover, the multi-structure of the TiO₂+Al₂O₃ mixed layer decreases the indiffusion of oxygen ions and also avails to improve the high temperature oxidation resistance of the as-sintered composites. Supported by the Special Program for Education Bureau of Shaanxi Province, China (Grant No. 08JK240) and Scientific Research Startup Program for Introduced Talents of Shaanxi University of Technology, China (Grant No. SLGQD0751)     

Modification of LiCo1/3Ni1/3Mn1/3O2 cathode material by CeO2-coating

LiCo_1/3Ni_1/3Mn_1/3O₂ was coated by a layer of 1.0 wt% CeO₂ via sol-gel method. The bared and coated LiMn_1/3Co_1/3Ni_1/3O₂ was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammogram (CV) and galvanotactic charge-discharge test. The results show that the coating layer has no effect on the crystal structure, only coating on the surface; the 1.0 wt% CeO₂-coated LiCo_1/3Ni_1/3Mn_1/3O₂ exhibits better discharge capacity and cycling performance than the bared LiCo_1/3Ni_1/3Mn_1/3O₂. The discharge capacity of 1.0 wt% CeO₂-coated cathode is 182.5 mAh·g⁻¹ at a current density of 20 mA·g⁻¹, in contrast to 165.8 mAh·g⁻¹of the bared sample. The discharge capacity retention of 1.0 wt% CeO₂-coated sample after 12 cycles reaches 93.2%, in comparison with 86.6% of the bared sample. CV results show that the CeO₂ coating could suppress phase transitions and prevent the surface of cathode material from direct contact with the electrolyte, thus enhance the electrochemical performance of the coated material.     

Study on the isothermal oxidation behavior in air of Ti3AlC2 sintered by hot pressing

The isothermal oxidation behavior at 900–1300°C for 20 h in air of bulk Ti₃AlC₂ with 2.8 wt% TiC sintered by means of hot pressing was investigated in the work. The isothermal oxidation behavior generally followed a parabolic rate law. The parabolic rate constants increased from 1.39×10⁻¹⁰ kg²·m⁻⁴·s⁻¹ at 900°C to 5.56×10⁻⁹ kg²·m⁻⁴·s⁻¹ at 1300°C. The calculated activation energy was 136.45 kJ/mol. It was demonstrated that Ti₃AlC₂ had excellent oxidation resistance due to the continuous, dense and adhesive protect scales consisted of a mass of α-Al₂O₃ and a little of TiO₂ and/or Al₂TiO₅. In principle, the oxide scale was grown by the inward diffusion of O²⁻ and the outward diffusion of Ti⁴⁺ and Al³⁺. The rapid outward diffusion of cations usually resulted in the formation of cracks, gaps, and holes.     

Kinetics of Fe3O4 formation by air oxidation

The kinetics of Fe₃O₄ formation by air oxidation of slightly acidic suspension of Fe(OH)₂ was studied. The effects of initial concentration of Fe(II), temperature, partial pressure of oxygen, air flow rate and stirring rate on the oxidation rate were investigated. The results show that Fe₃O₄ formation is composed of two-step reaction, the first step is the formation of Fe(OH) ₂ ⁺ by oxidation of Fe(OH)⁺ complex ions, the second step is the formation of magnetite by dehydration and deprotonation of Fe(OH)⁺ and Fe(OH) ₂ ⁺ . The oxidation reaction is zero-order with respect to the concentration of Fe(II) and around 0.5-order with respect to partial pressure of oxygen, and oxygen transfer process is rate-limiting step of oxidation reaction with apparent activation energy of 2.74 kJ · mol⁻¹.     

Luminescent properties of BaO-La2O3-B2O3 glasses with dopant

The luminescent properties of glasses synthesized in air atmosphere by conventional high temperature process were stud{ed. The emissions spectra of Eu^2 and Eu^3 were observed in BaO-La2O3-B2O3-Eu2O3 glasses.The results show that the broad emission peaks at 430 nm correspond to 5d→4f emission transition of Eu^2 , the sharp emission peaks at 592, 616, 650 and 250 nm correspond to 5^D0→1Fj(j=1--4) emission transition of Eu^3 ,respectively, which indicates that the BaO-La2O3a-B2O3-Eu2O3 glass can convert ultraviolet and green omponents of sunlight into blue and red light so as to increase the intensity of blue and red light, respectively. The luminescent in--tensity of Eu^2 increases with increasing the molar ratio of Tb^3 in BaO-La2O3-B2O3-Eu2O3a-Tb4O3 glasses, whereas the luminescent intensity of Eua^3 decreases. So the luminescent intensity of Eu(Ⅲ,Ⅱ) is influenced by Tb^3 .These phenomena can be explained by electron transfer mechanism; Eu^3 (4f6) Tb^3 (4f^8)→Eu^2 (4f′) Tb^4 (4f′). Taking advantage of the luminescent properties of BaO-La2O3-B2O3-Eu2O3 glasses, light-conversion glass for agriculture can be produced.     

Modification of nano-TiO2 by Al2O3 in-situ coating

A novel technology of in-situ coating Al₂O₃ on the surface of H₄TiO₄ was developed to prevent the aggregation of nano-TiO₂ powders and improve the dispersibility and thermal stability in the way of forming a uniform coating layer. The heterogeneous nucleation was conducted to prepare the precursor of nano-TiO₂ and then Al₂O₃ was coated on the surface of precursor. The effects of Al₂O₃ in-situ coating on the properties of nano-TiO₂ were investigated. The results show that H₄TiO₄ can be dispersed well under alkaline condition (pH 8.5) and the heterogeneous nucleation can be controlled easily. The optimized uniform coating layer is obtained by adding 5% (mass fraction) and 10% of Al₂O₃ and the aggregation of nano-TiO₂ powders is effectively inhibited and the dispersibility is obviously improved. The crystal sizes of TiO₂ powders are 12.3, 11.4 and 8.7 nm after coating 0,5% and 10% of Al₂O₃ respectively. Al₂O₃ on the surface of particulates in amorphous phase could increase the thermal stability of nano-particles after calcined at 550 °C. Foundation item: Project(04GK2007) supported by Hunan Industrial Key Project of Science and Technology     

Synthesis and characterization of high-voltage cathode material LiNi0.5Mn1.5O4 by one-step solid-state reaction

LiNi_0.5Mn_1.5O₄ was prepared under various conditions by one-step solid-state reaction in air and its properties were investigated by X-ray diffractormetry (XRD), scanning electron microscopy (SEM) and electrochemical measurement. XRD patterns show that LiNi_0.5Mn_1.5O₄ synthesized under various conditions has cubic spinel structure. SEM images exhibit that the particle size increases with increasing calcination temperature and time. Electrochemical test shows that the LiNi_0.5Mn_1.5O₄ calcined at 700 °C for 24 h delivers up to 143 mA · h/g, and the capacity retains 132 mA · h/g after 30 cycles. Foundation item: Project (76600) supported by Postdoctoral Science Foundation of Central South University     

Study of GaN MOS-HEMT using ultrathin Al2O3 dielectric grown by atomic layer deposition

We report on a GaN metal-oxide-semiconductor high electron mobility transistor (MOS-HEMT) using atomic-layer deposited (ALD) Al₂O₃ as the gate dielectric. Through further decreasing the thickness of the gate oxide to 3.5 nm and optimizing the device fabrication process, a device with maximum transconductance of 150 mS/mm was produced. The drain current of this 0.8 μm gate-length MOS-HEMT could reach 800 mA/mm at +3.0 V gate bias. Compared to a conventional AlGaN/GaN HEMT of similar design, better interface property, lower leakage current, and smaller capacitance-voltage (C-V) hysteresis were obtained, and the superiority of this MOS-HEMT device structure with ALD Al₂O₃ gate dielectric was exhibited. Supported by the National Natural Science Foundation of China (Grant No. 60736033) and the National Basic Research Program of China (“973“) (Grant No. 51327020301)