Effects of various fillers on sintering,microstructures and properties of Ca-Ba-Al-B-Si-O glass/ceramic composites简

Low-temperature sintering and properties of LTCC （low temperature co-fired ceramics） materials based on CaO-BaO-Al2O3-B2O3-SiO2 glass and various fillers such as Al2O3, silica glass, christobalite, AlN, ZrO2, MgO-SiO2, TiO2 were investigated. The results show that densification, crystallization, microstructures and dielectric properties of the composites are found to strongly depend on the type of filler. The densification process of glass/ceramic composites with various fillers is mainly from 600 ℃ to 925 ℃, and the initial compacting temperature of samples is 600 ℃. The initial rapid densification of samples starts at its glass softening temperature. LTCC compositions containing Al2O3, silica glass, AlN and MgO-SiO2 fillers start to have the crystallization peaks at 890, 903, 869 and 844 ℃, respectively. The crystallization peaks are believed as correlated to the crystallization of CaAl2SiO8, β-SiO2, Ca2Al2SiO7 and β-SiO2. The composite ceramic with Al2O3, silica glass and TiO2 ceramic have a better dense structure and better smooth fracture surface. Sample for Al2O3 has the lowest dielectric loss tanδ value of 0.00091, whereas the sample for MgO.SiO, has the highest dielectric loss tanδ value of 0.02576. The sample for TiO2 has the highest dielectric constant value of 14.46, whereas the sample for AIN has the lowest dielectric constant value of 4.61.     

Al2O3对3Ti/Si/2C体系自蔓延高温合成Ti3SiC2的影响

以3Ti/Si/2C粉体为原料,通过自蔓延高温合成技术合成了Ti3SiC2材料。研究了Al2O3助剂对自蔓延高温合成Ti3SiC2的影响。研究结果表明,3Ti/Si/2C粉体会发生自蔓延反应,产物的组成相为TiC、Ti3SiC2和Ti5Si3,产物中Ti3SiC2含量约为23%。添加适量的细粒度Al2O3可显著促进反应合成Ti3SiC2,3Ti/Si/2C/0.1Al2O3原料反应后得到的产物中Ti3SiC2含量达64%。     

Electric field assisted solid-state interfacial joining of TaC-HfC ceramics without filler

The application of ultra-high-temperature ceramics (UHTCs) demands effective ways of joining in overcoming the problems associated with the fabrication of complex-shaped components. In this study, we choose to investigate a new method of rapidly joining pre-sintered TaC and HfC ceramics without any filler material using the spark plasma sintering (SPS) technique. A well-bonded TaC–HfC interface was observed with no apparent cracking and porosity at the joint. The joining mechanisms were predominantly driven by solid-state diffusion and localized plastic deformation. The nanomechanical properties of the TaC-HfC joint are better than the HfC while comparable to that of the TaC. High-load indentation (up to 200 N) results suggest that the TaC–HfC interface is stronger than the parent UHTCs with no crack propagating at the interface. Upon comparison with the parent UHTCs, the damaged area and the average crack length at the interface, reduced up to ~94% and ~56%, respectively. This study shows that the SPS technique can also apply to joining other UHTCs without any filler, resulting in the new field of developing complex components for the thermal protection system (TPS).     

Sintering parameter optimization of Tb3Al5O12 magneto-optical ceramics by vacuum sintering and HIP post-treatment

Transparent terbium aluminum garnet (TAG) ceramics were achieved by the vacuum sintering plus HIP post-treating from the coprecipitated TAG nanoparticles. The influences of vacuum sintering temperature and sintering aid TEOS on the optical quality of the TAG ceramics were studied. The results show that with the increase of sintering temperature, the optical quality of TAG ceramics is improved gradually, and the in-line transmittance of the TAG ceramics treated at 1720°C for 20 hours under vacuum and then HIP post-treated at 1700°C for 3 hours under 200 MPa argon gas is 81.6% at 1064 nm. The sintering additive TEOS can improve the optical quality of TAG ceramics and inhibit the valence state change of Tb³⁺ ions to Tb⁴⁺ during the annealing process. The Verdet constant of the TAG ceramics at 632.8 nm is about −178 rad·T⁻¹·m⁻¹ at room temperature, which is 1.3 times that of the commercial TGG crystals (−134 rad·T⁻¹·m⁻¹).     

Cold sintering of diatomaceous earth

Diatomite, a natural silicate-based sedimentary rock, was densified by cold sintering at room temperature and 150°C under various pressures (100, 200, and 300 MPa) and using different NaOH water solutions (0–3 M). The relative density of cold sintered diatomite can be as high as 90%, a condition that can be achieved by conventional firing only at 1200–1300°C. The cold sintered materials maintain the same mineralogical composition of the starting powder (quartz, glass, and illite) and are constituted by well-deformed and flattened grains oriented orthogonally to the applied pressure. Conversely, an evident phase evolution takes place upon conventional firing with the formation of cristobalite and mullite. The bending strength of cold sintered artifacts can exceed 40 MPa and increases to ≈80 MPa after post-annealing at 800°C, such mechanical strength is much larger than that of conventionally pressed samples sintered at 800°C, which is only ≈1 MPa.     

Effect of AlN addition on the electrical resistivity of pressureless sintered SiC ceramics with B4C and C

The effect of 0–12 wt% AlN addition on the electrical resistivity of SiC ceramics pressureless sintered with 0.7 wt% B₄C and 2.5 wt% C additives was investigated. The elemental analysis of SiC grains revealed a codoping of Al and N in the SiC lattice with a higher N concentration with 1 wt% AlN addition and a higher Al concentration with 12 wt% AlN addition. The electrical resistivity decreased by four orders of magnitude (1.7 × 10⁵ → 8.3 × 10¹ Ω cm) with 1 wt% AlN addition due to the increased carrier density (1.7 × 10¹⁰ → 2.3 × 10¹⁵ cm⁻³) caused by excess N-derived donors. However, subsequent AlN addition (4 → 12 wt%) led to an increase (2.9 × 10³ → 1.2 × 10⁴ Ω‧cm) in electrical resistivity due to (1) increased Al dopants which act as deep acceptors for trapping N-derived carriers causing a decrease in carrier density (2.3 × 10¹⁵ → 5.9 × 10¹³ cm⁻³), (2) the formation of electrically insulating SiC-AlN solid solution, and (3) the presence of electrically insulating AlN grains at the grain boundaries.     

Relation between crystal structure and lattice oxygen content of sintered reaction-bonded silicon nitride

When reaction-bonded silicon nitride containing MgO/Y₂O₃ additives is sintered at three different temperatures to form sintered reaction-bonded silicon nitride (SRBSN), the thermal conductivity increases with sintering temperature. The β-Si₃N₄ (silicon nitride) crystals of SRBSN ceramics were synthesized and characterized to investigate the relation between the crystal structure and the lattice oxygen content. The hot-gas extraction measurement result and the crystal structure obtained using Rietveld analysis suggested that the unit cell size of the β-Si₃N₄ crystal increases with the decrease in the lattice oxygen content. This result is reasonable considering that the lattice oxygen with the smaller covalent radius substitutes nitrogen with the larger one in the β-Si₃N₄ crystals. The lattice oxygen content decreased with increasing sintering temperature which also correlated with increase in thermal conductivity. Moreover, it is noteworthy from the viewpoint that it may be possible to apply the lattice constant analysis for the nondestructive and simple measurement of the lattice oxygen content that deteriorates the thermal conductivity of the β-Si₃N₄ ceramics.     

Characterization of PA-12 specimens fabricated by projection sintering at various sintering parameters

Large area projection sintering (LAPS) promises to be a new method in the field of additive manufacturing. Developed in the Mechanical Engineering Department, University of South Florida, LAPS uses long exposure times over a broad area of powder to fuse into dense, reproducible materials. In contrast, LS, a common powder-based additive manufacturing, uses a focused beam of light scanned quickly over the material. Local regions of concentrated high-energy bursts of light lead to higher peak temperatures and differing cooling dynamics and overall crystallinity. The mechanical properties of laser sintered specimens suffer because of uneven particle fusion. LAPS offers the capacity to fine-tune fusion properties through enhanced thermodynamic control of the heating and cooling profiles for sintering. Further research is required to identify the relationship between LAPS build settings and part properties to enable the fabrication of custom parts with desired properties. This study examines the influence of LAPS sintering parameters on chemical structures, crystallinity, mechanical, and thermal properties of polyamide-12 specimens using powder X-ray diffraction, Fourier transform infrared spectroscopy, differential scanning calorimetry, small-angle X-ray scattering, scanning electron microscopy, and microhardness testing. It was observed that higher crystallinity was imparted to specimens that were sintered for a shorter time and vice versa.     

Near-zero-shrinkage Al2O3 ceramic foams with coral-like and hollow-sphere structures via selective laser sintering and reaction bonding

The large shrinkage that ceramics undergo during sintering is a severe challenge for high-performance porous ceramics. In this study, we report a powder-based selective laser sintering (SLS) approach to prepare Al₂O₃ ceramic foams with near-zero shrinkage, high porosity, and outstanding strength. The ceramic foams consist of specific coral-like and hollow-sphere structures derived from the raw Al₂O₃/Al composite powders via reaction bonding (RB). A near-zero shrinkage of 0.91 ± 0.15 % and a high porosity of 73.7 ± 0.2 % can be achieved based on the Kirkendall effect during the oxidation of Al particles. Meanwhile, the reinforced sintering necks and robust bond-bridge connections between hollow-sphere and coral-like structures result in a remarkable bending strength of 7.37 ± 0.37 MPa. This measured strength is more than six times higher than other fabricated samples from spherical Al₂O₃ powders, and the comprehensive performance of ceramic foams prepared by this novel SLS/RB strategy is exceptionally remarkable versus that via conventional forming methods.     

工艺参数对选择性激光烧结PS/SBS/纳米CaCO3制件弯曲强度影响

针对聚苯乙烯(PS)粉末选择性激光烧结(SLS)成型件强度较低的问题,采用机械混合法制备了PS/苯乙烯–丁二烯–苯乙烯嵌段共聚物(SBS)/纳米CaCO₃复合粉末,通过单因素实验分析了SLS工艺参数对成型件弯曲强度的影响,并通过正交试验和极差分析获得了最优工艺参数组合。实验结果表明,烧结件的弯曲强度随着激光功率的增大而升高,随着扫描速度、扫描间距和分层厚度的增大而降低;激光功率对PS/SBS/纳米CaCO₃复合粉末烧结件弯曲强度的影响最大,分层厚度对弯曲强度的影响最小,扫描速度和扫描间距的影响介于两者之间;最佳工艺参数组合为:激光功率27 W,扫描速度1300 mm/s,扫描间距0.24 mm,单层厚度0.22 mm。在此工艺参数组合下PS/SBS/纳米CaCO₃复合粉末烧结件的弯曲强度为13.38 MPa;改性纳米CaCO₃与PS和SBS的相容性较好,能有效起到增强的作用。