Fabrication of homogenous dispersion TiB<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites

In order to get a homogenous mixture and compact of TiB2-Al2O3, hybridization as a surface modification method was used to prepare nano-scale Al2O3 coated TiB2 particles. PE-wax particles were first coated onto TiB2 particles by hybridization, and then the nano-scale Al2O3 particles were coated onto the surface of TiB2 coated by PE-wax particles again. SEM, TEM and EDS were used to characterize the microstructure of as-received core/shell particles and its compacts. The experimental results show that a particle-scale homogenous dispersion of TiB2 and Al2O3 can be formed not only in mixed powder but also in dewaxed compacts. The compacts then were sintered by gas-pressing sintering (GPS). Finial products show improved mechanic properties comparing with reference samples fabricated by normal ways.     

Microstructure and mechanical properties of TiB<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites

Effects of Al2O3 and Ni as the additives on the sinterability, microstructure and mechanical properties were systematic studied. The experimental results show that only a relative density about 96.2% of hot-pressing TiB2-30%Al2O3 can be attained due to the plate-like TiB2 particle and its random orientation and excessive Al2O3 grain growth. When sintering temperature is higher than 1 700 ℃, TiB2 grain growth can be found, which obvious improves flexural strength of TiB2 matrix but decreases toughness. It seems that mechanical properties of TiB2-Al2O3 composites are mainly depended on relative density besides grain growth. otherwise, they will be determined by relative density and TiB2 matrix strength together. Anyway, Al2O3 addition can weaken the grain boundary and thus improve the toughness of the materials. A flexural strength of 529 MPa, Vickers hardness of 24.8 GPa and indentation toughness of 4.56 MPa·m1/2 can be achieved inTiB2-30vol% Al2O3.     

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.     

Synthesis of Ti3SiC2/TiB2 Composite by In-situ Hot Pressing （HP） Method

Ti3SiC2/TiB2 composite was successfully obtained by hot pressing Ti/TiC/Si/B4C power mixtures.Volume fraction of TiB2 in Ti3SiC2/TiB2 composite can not exceed 10%.Incorporation of excessive TiB2 will affect the reactions process.TiC and Ti5Si3 were two important intermediate phases during the whole reactions.The microstructure characteristics of the Ti3SiC2/TiB2 composites were analyzed using scanning electron microscopy （SEM） and transmission electron microscopy （TEM）.The experimental results show that the grains of Ti3SiC2/TiB2 composite are structured in a layered form,and the formation of TiB2 particles as reinforcements with elongated or equiaxed shape distributes in Ti3SiC2 matrix.     

Influence of TiX (<Emphasis Type="Italic">X</Emphasis>=B<Subscript>2</Subscript> or N) addition on the interfacial microstructure features of CBN grains and AgCuTi composite filler

Joining experiments of CBN grains to AISI 1045 steel were conducted using Ag-Cu-Ti composite fillers containing TiX (X=B₂ or N) particles at 920 °C for 5 min. The influences of TiB₂ and TiN particles on the interfacial microstructure features between CBN and filler were investigated comparatively. The experimental results show that TiN particles are more effective than TiB₂ ones to control the interfacial reaction and particularly the resultants. Thermodynamic analysis reveals that the varied interfacial reaction induced by the addition of TiB₂ and TiN particles is mainly atttributed to the activity change of the B and Ti elements in the brazing reaction system.     

Dielectric Properties of B2O3 Doped MgTiO3-CaTiO3 System Ceramics

The dielectric ceramics with a main crystal phase of MGTiO3 and additional crystal phase of CaTiO3 were prepared by the conventional electronic ceramics technology .the strucures of MgTiO3 are ilmenitetype,and belong to hexagonal syngony.the ratio of MgTiO3 to Ca TiO3 doping on the dielectric properties of MGTiO3-CaTiO3(MCT)ceranics were inrestigated.the addition of B2O3 decreases the sintering temperatnre and results in rapid desification without obrious negative effect on the Q values of the system(Q=1/tan ).B2O3 exists as liquid phase in the sintering process,promoting the reactions as a singering agent.     

Fabrication and plasma arc thermal shock resistance of HfB2-based ultra high temperature ceramics

Two hafnium diboride based ceramic matrix composites containing 20% (volume fraction) SiC particle and with or without AlN as sintering additives were fabricated by hot-pressed sintering. The mechanical properties and microstructures of these two composites were tested and the thermal shock resistances were evaluated by plasma arc heater. The results indicate that the composite with AlN as sintering additive has a denser and finer microstructure than composite without sintering additive, and the mechanical properties, thermal shock resistance of the composite with AlN as sintering additive are also higher than those of the composite without AlN. Microstructure analysis on the cross-section of two composites after thermal shock tests indicates that a compact oxidation scale contains HfO₂ and Al₂O₃ liquid phase is found on the surface of composite with AlN, which could fill the voids and cracks of surface and improve the thermal shock resistance of composite.     

Graded materials of (TiB<Subscript>2</Subscript>)<Subscript>p</Subscript>Ni with nickel substrate prepared by field-activated pressure-assisted synthesis process

The preparation of functionally graded materials (FGMs) of (TiB₂)_pNi with an intermetallic compound media layer of Ni₃Al and a substrate of nickel by field-activated pressure-assisted synthesis process (FAPAS) was investigated. Ni₃Al was chosen as a layer of FGM for the first time due to its great deal of heat released during its synthesis from nickel and aluminium powder. The microstructure, phase composition of layers, micro-hardness and elemental concentration profiles across interfaces were characterized. The significant inter-diffusion of elements between layers showed the formation of good bonds. The measured micro-hardness values of the sample increased monotonically to more than 3 500 HK over a distance of 2 mm from the nickel substrate to the surface layer (TiB₂)_pNi. The results of this investigation demonstrate the feasibility of the FAPAS process for rapid formation of FGMs with good diffusion bonds.     

Thermal Wave Effect and Sintering Activation Energy at the Initial Stage of Field Assisted Sintering Process for Non-conductive Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Powders

The effect of thermal wave at the initial stage for non-conductive Al₂O₃ powders compact in field assisted sintering technique (FAST) was investigated. The Lord and Shulman type generalized thermoselastic theory was introduced to describe the influence of thermal-mechanical interaction, as well as the heat transport and thermal focusing caused by thermal wave propagation. The expression of vacancy concentration difference of the particles was deduced by considering transient thermal stress. Subsequently, the relationship between activation energy and vacancy concentration difference was obtained. The mechanism of surface diffusion, volume diffusion, simultaneous surface and volume diffusion was analyzed. The numerical simulations indicate that low sintering temperature can obtain high local temperature by the superposition effect of thermal wave. Vacancy concentration differences were improved during FAST compared with hot-pressure and pressureless sintering, thereby decreasing the sintering time. By contrast, the activation energy declined with the decrease of vacancy concentration difference in the neck growth process.     

Self-assembled SnO<Subscript>2</Subscript> colloidal particles and their gas sensing performance to H<Subscript>2</Subscript>, C<Subscript>2</Subscript>H<Subscript>5</Subscript>OH and LPG

Using organo-tin Sn(OC4H9)4 as precursor, sodium dodecyl sulfonate (SDS) and SDS-gelatin (SDS-G) complex as template, two tin dioxide colloidal particles were prepared by a self-assembly method. Both SnO2 products were respectively labelled SnO2-B particles with SDS and SnO2-C particles with SDS-G, which are applied in fabricating SnO2 gas sensors corresponding to SnO2-B’ and SnO2-C’ sensors. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermo-gravimetry and different thermal analysis (TG/DTA) were used for characterizations. The experimental results show that SnO2-B colloidal particles are composed of mesoporous piece-like particles, while SnO2-C particles mainly consist of spherical particles. Gas sensing measurements show that SnO2-B’ sensor performs the best sensing response to all target gases, including H2, C2H5OH and liquid petroleum gas (LPG). In particular, the sensing response of SnO2-B’ sensor is achieved at 32 in H2 atmosphere at the concentration of 1000×10-6 M. The gas sensing mechanism was purposely discussed from the electron transfer process and the microstructures of the as-prepared SnO2 products. It is found that serious agglomerations in SnO2-B’ particles facilitate the high gas sensing performance of SnO2-B’ sensor, while mesoporous structures in SnO2-C’ particles decrease the gas sensing response of SnO2-C’ sensor.     

Preparation and microstructure of spinel zinc ferrite ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> by Co-precipitation method

Spinel zinc ferrites ZnFe₂O₄, prepared by co-precipitation method using the zinc nitrate Zn(NO₃)₂·6H₂O and ferric nitrate Fe(NO₃)₃·2H₂O as the raw materials, were characterized by the thermo gravimetric analysis (TG) and differential scanning calorimeter (DSC), X-ray diffraction (XRD) and scanning electron microscope (SEM). The influence of synthesis conditions, such as Zn/Fe molar ratio, pH value, the sintering temperature and time, on the microstructures was detailedly investigated. The relationships between the microstructures and the synthesis conditions were discussed. The results show that the pure spinel zinc ferrites ZnFe₂O₄ are formed when the Zn/Fe molar ratio is 1.05:2 at pH=8.5 or Zn/Fe molar ratio is 1:2 at Ph=9-10, and the precursors are sintered at 1100 °C for 4 h. Especially no other phases are observed when the Zn/Fe molar ratio is 1:2 at pH=10 and the precursor is sintered above 700 for 4 °C h. The higher sintering temperature and longer sintering time contribute to grain growth.     

Effect of MnO<Subscript>2</Subscript> on properties of SiC-mullite composite ceramics for solar sensible thermal storage

For improving the properties of SiC-mullite composite ceramics used for solar sensible thermal storage, MnO₂ was introduced as sintering additive when preparing. The composite ceramics were synthesized by using SiC, andalusite, α-Al₂O₃ as the starting materials with non-contact graphite-buried sintering method. Phase composition and microstructure of the composites were investigated by XRD and SEM, and the effect of MnO₂ on the properties of SiC composites was studied. Results indicated that samples SM1 with 0.2 wt% MnO₂ addition achieved the optimum properties: bending strength of 70.96 MPa, heat capacity of 1.02 J·(g·K)^-1, thermal conductivity of 9.05 W·(m·K)^-1. Proper addition of MnO₂ was found to weaken the volume effect of the composites and improve the thermal shock resistance with an increased rate of 27.84% for bending strength after 30 cycles of thermal shock (air cooling from 1 100 °C to RT).     

Effect of ZnO-B<Subscript>2</Subscript>O<Subscript>3</Subscript> glass addition on the microwave dielectric properties of BaO-Nd<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiO<Subscript>2</Subscript>-Bi<Subscript>2</Subscript>O<Subscript>3</Subscript> system

The effect of ZnO-B₂O₃(ZB) glass addition on the sintering behavior, microstructures and microwave dielectric properties of BaO-Nd₂O₃-TiO₂-Bi₂O₃ (BNTB) system was investigated with the aid of X-ray diffraction, scanning electron microscopy and capacitance meter. It is found that the ZB glass addition, acting as a sintering aid, can effectively lower the sintering temperature of BNTB system to 850 °C. The dielectric constant of BNTB-ZB ceramics increases with the increase of soaking time and the value of dielectric loss decreased with increasing soak time. The optical dielectric properties at 1 GHz of ɛ=74, tan δ=4×10⁻⁴, and TCC=25 ppm/°c were obtained for the BNTB system doped with 25 wt% ZB glass sintered at 850 °C for 2 h, representing that the BNTB-ZB ceramics could be promising for multilayer low temperature co-fired ceramics applications.     

Microwave sintering of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-ZrO<Subscript>2</Subscript>-WC-Co cermets

Composite powders of nanocrystalline WC-10Co (15wt%),Y2O3 (8mol%) stabilized nanocrystalline ZrO2 (30wt%),industrial cobalt powder (4.5wt%) and submicron Al2O3 (55wt%) composite powders were fabricated by high-energy ball-milling process.The nanocomposite powders were consolidated by microwave sintering process at temperature ranged 1300℃-1550℃ for 15min,respectively.The optimum consolidation conditions,such as temperature,were researched during microwave sintering process.Vickers Hardness of the consolidated cermets was measured by using a Vickers indentation test,and density of specimens was also determined by Archimedes’ principle.Microwave sintering process could not only increase the density of Al2O3-ZrO2-WC-Co cermets and reduce the porosity,but also inhibit abnormal grain growth.     

Manufacture Process of 8Y2O3 Stabilized ZrO2 from Nano Powders

The manufacture process of 8 mol% Y2O3 stabilized ZrO2 ( YSZ ) from nano powders, including the forming and sintering stages, was studied. During the forming process of YSZ powders, the relative density of YSZ increases lineally with the forming press, and the sintering linear shrinkage of YSZ to the forming press compiles to the parabola trend. When the forming press exceeding 500MPa, the samples with lower shrinkage and high density were obtained. The sintering temperature of YSZ decreases greatly because of the small size and high active surface of YSZ powders. As a result, the beginning sintering temperature of YSZ made in the experiment is as low as 825℃, and the end sintering temperature is 1300-1350℃ . The relative density of YSZ ceramic by solid sintering at 1300-1350℃ is more than 97% , with little and small pores in the uniform microstructure.     

Mechanism and kinetic model of <Emphasis Type="Italic">in-situ</Emphasis> TiB<Subscript>2</Subscript>/7055Al nanocomposites synthesized under high intensity ultrasonic field

In-situ TiB2/7055Al nanocomposites are fabricated by in situ melt chemical reaction from 7055Al-K2TiF6-KBF4 system under high intensity ultrasonic field,and the mechanism and kinetic model of in-situ melt chemical reaction are investigated.X-ray diffraction (XRD) and scanning electron microscope (SEM) analyses indicate that the sizes of in-situ TiB2 nanoparticles are in the range of 80-120 nm.The results of ice-water quenched samples show that the whole process contains four stages,and the overall in-situ reaction time is 10 minutes.The in situ synthesis process is controlled mainly by chemical reaction in earlier stage (former 3 minutes),and by the particulate diffusing in later stage.The mechanism of key reaction between Al3Ti and AlB2 under high intensity ultrasonic in the 7055Al-K2TiF6-KBF4 system is the reaction-diffusion-crack-rediffusion.Furthermore,the reactive kinetic models in 7055Al-K2TiF6-KBF4 system are established.     

Effect of aluminum addition on microstructure and properties of SiO<Subscript>2</Subscript>-B<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-CaO vitrified bond

Influence of aluminum addition on the structures and properties of SiO₂-B₂O₃-Al₂O₃-CaO vitrified bond at low sintering temperature and high strength was discussed. FTIR and XRD analyses were used to characterize the structures of the basic vitrified bond with different contents of aluminum. The bending strength and the thermal expansion coefficients were also tested. Meanwhile, the microstructures of composite specimens at sintering temperature of 660 °C were observed by scanning electron microscope (SEM). The experimental results showed that the properties of vitrified bond with 1wt% aluminum were improved significantly, where the bending strength, Rockwell hardness, and thermal expansion coefficient of the vitrified bond reached 132 MPa, 63 HRB, and 6.73×10^-6 °C^-1, respectively.     

Two-step synthesis of TiC<Subscript>0.7</Subscript>N<Subscript>0.3</Subscript>@WC-MoC<Subscript>2</Subscript> core-shell microspheres and fabrication of TiC<Subscript>0.7</Subscript>N<Subscript>0.3</Subscript>@WC-MoC<Subscript>2</Subscript>-based cermets by SPS

The precursor with TiC0.7N0.3@WO3-MO3 microspheres were prepared by a novel method from the WO3-MoO3 sol dipping. Subsequently, TiC0.7N0.3@WC-MoC2 core-shell structural microspheres were successfully obtained by carburizing the precursor at 900 °C in a flowing mixture of CH4 (20 ml·min-1) and H2 (200 ml·min-1) for 2 h. Then TiC0.7N0.3@WC-MoC2-15Co cermets were prepared utilizing the core-shell powders by spark plasma sintering (SPS). Powders of the precursors with TiC0.7N0.3@WO3-MO3 microspheres, TiC0.7N0.3@WC-MoC2 microspheres and TiC0.7N0.3@WC-MoC2-15Co cermets were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The obtained TiC0.7N0.3@WC-MoC2 microspheres have a dense WC-MoC2 coatings shell. The thickness of the shell could be easily controlled by adjusting the number of sol dipping cycles. It was found that the TiC0.7N0.3@WC-MoC2 microspheres were more beneficial to fabricate the "core-rim" structures by SPS.     

Effect of Grain Size of CaCO3 and SiO2 on the Formation of C3S Under Different Conditions

The effect of grain size of CaCO3 and SiO2 on the formation of C3S under various conditions, such as rapid heating rate（800 ℃/min）, normal heating rate（30 ℃/min） and in the presence or absence of ZnO, was studied. The results show that the decomposition temperature of CaCO3, the temperature of appearance of liquid phase and the f-CaO content descend when the grain size of CaCO3 and SiO2 becomes smaller, which attributes to the reactive activity enhancement of powders due to the decrease of the particle size. When the grain size of CaCO3 and SiO2 is below 1 μm, the rate of the formation of C3S is greatly raised. A rapid sintering rate and the presence of ZnO have an important effect on the formation of C3S and can lower the temperature of the formation of C3S by about 50 ℃.