成型温度对PBX装药内部质量及性能的影响

针对压制成型的PBX炸药装药，选择CT无损检测、巴西实验和扫描电镜检测等技术，对比研究了室温和加热两种温度下压制成型的炸药装药内部质量、静态力学性能和细观破坏形式。结果表明，加热压制有利于改善炸药装药的内部质量，可避免产生初始损伤，且提高了装药的力学性能。细观尺度上，室温压制成型的装药主要发生界面脱黏破坏，加热压制成型装药的主要破坏形式是穿晶断裂。     

Profiling hot isostatically pressed canister–wasteform interaction for Pu-bearing zirconolite-rich wasteforms

Zirconolite-rich full ceramic wasteforms designed to immobilize Pu-bearing wastes were produced via hot isostatic pressing (HIP) using stainless steel (SS) and nickel (Ni) HIP canisters. A detailed profiling of the elemental compositions of the major and minor phases over the canister–wasteform interaction zone was performed using scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM-EDS) characterization. Bulk sample analyses from regions near the center of the HIP canister were also conducted for both samples using X-ray diffraction and SEM-EDS. The sample with the Ni HIP canister showed almost no interaction zone with only minor diffusion of Ni from the inner wall of the canister into the near-surface region of the wasteform. The sample with the SS HIP canister showed ∼100–120 μm of interaction zone dominated by high-temperature Cr diffusion from canister materials to the wasteform with the Cr predominantly incorporated into the durable zirconolite phase. We also examined, for the first time, changes to the HIP canister wall thickness caused by HIPing and demonstrated that no canister wall thinning occurred. Instead, in the areas examined, the canister wall thickness was observed to increase (up to ∼20%) due to the compression occurring during the HIP cycle. Further, only sparse formation of (Cr, Mn)-rich oxide particles were noted within the HIP canister inner wall area immediately adjacent to the ceramic material, with no evidence for reverse diffusion of ceramic materials. Though the HIP canister–wasteform interaction extends to ∼120 μm when using an SS HIP canister for the system investigated, this translates to <<1 vol.% for an industrial scale HIPed wasteform. Importantly, the HIP canister–wasteform interactions did not produce any obviously less durable phases in the wasteform or had any detrimental impact on the HIP canister properties.     

Effect of organic solvent on the cold sintering processing of SrFe12O19 platelet-based permanent magnets

In this work we have investigated the effect of the solvent during the processing of SrFe₁₂O₁₉ platelet-based permanent magnets by cold sintering process (CSP) plus a post-thermal treatment. Several organic solvents: glacial acetic acid, oleic acid and oleylamine have been analyzed, optimizing the CSP temperatures at 190?270 °C, under pressures of 375?670 MPa and 6?50 wt% of solvent. Modifications in the morphological and structural properties are identified depending on the solvent, which impacts on the magnetic response. Independently of the solvent, the mechanical integrity of ferrite magnets obtained by CSP is improved by a post-annealing at 1100 °C for 2 h, resulting in relative densities around 92 % with an average grain size of 1 μm and a fraction of SrFe₁₂O₁₉ phase >91 %. H_C ≥ 2.1 kOe and M_S of 73 emu/g are obtained in the final sintered ceramic magnets, exhibiting the highest H_C value of 2.8 kOe for the magnet sintered using glacial acetic acid.     

(Cu1/3Nb2/3)4+ ionic substituting effects,low-temperature sintering behaviors,and improved temperature stability of Ba3Nb4Ti4O21 microwave dielectric ceramics

In this study, (Cu_1/3Nb_2/3)⁴⁺ complex cation and BaO–ZnO–B₂O₃ glass frit were adopted to solve the high sintering temperature and poor temperature stability of Ba₃Nb₄Ti₄O₂₁ ceramics. It is shown that pure Ba₃Nb₄Ti₄O₂₁ phase was formed when Ti site was partially replaced by (Cu_1/3Nb_2/3)⁴⁺ cation. The increasing number of dopants decreases the dielectric polarizability, correspondingly, the dielectric constant and temperature coefficient of the resonance frequency values are reduced consistently. The variation of the Q × f value is determined by internal ionic packing fraction and external sintering densification. The (Cu_1/3Nb_2/3)⁴⁺ cation effectively decreases the suitable sintering temperature from 1200 to 1050 °C while greatly improving the temperature stability. BaO–ZnO–B₂O₃ glass was used to further improve the low-temperature sintering characteristics of Ba₃Nb₄Ti₄O₂₁ ceramics. It is proven that the addition of glass frits effectively decreases the temperature to 925 °C with combinational excellent microwave dielectric properties: ε_r ～55.6, Q × f ～5700 GHz, τ_f ～3 ppm/^°C, making the Ba₃Nb₄Ti₄O₂₁ ceramics promising in the applications of low-temperature cofired ceramic technology.     

Fabrication and upconversion luminescence properties of Er:SrF2 transparent ceramics compared with Er:CaF2

SrF₂ transparent ceramic is a promising upconversion material due to the low phonon energy. The effect of different sintering temperatures on Er:SrF₂ transparent ceramics was investigated. The suitable sintering temperature for Er:SrF₂ transparent ceramics was 900 °C by hot-pressed sintering in this study. High quality of Er:SrF₂ transparent ceramics with different doping concentrations were obtained. The upconversion luminescence spectra and decay behavior were compared between Er:SrF₂ and Er:CaF₂ transparent ceramics with different Er³⁺ doping concentration. The green emission of 5 at.% Er:SrF₂ ceramic was much stronger than that of 5 at.% Er:CaF₂ ceramic, while the red emission of Er:SrF₂ ceramic was almost the same as that of Er:CaF₂ ceramic. The upconversion luminescence lifetime of Er:SrF₂ transparent ceramics was longer than that of Er:CaF₂.All the results indicated Er:SrF₂ transparent ceramics was a candidate for green fluorescent upconversion materials.     

Moderate temperature sintering of BaZr0.8Y0.2O3-δ protonic ceramics by A novel cold sintering pretreatment

The state-of-the-art protonic ceramic conductor BaZr_0.8Y_0.2O_3-δ (BZY20) requires an extremely high sintering temperature (≥1700 °C) to achieve the desired relative density and microstructure necessary to function as a proton conducting electrolyte. In this work, we developed a cold sintering pretreatment assisted moderate-temperature sintering method for the fabrication of high-quality pure BZY20 pellets. BZY20 pellets with high relative density of ~94% were fabricated with a final sintering temperature of 1500 °C (200 °C lower than the traditional sintering temperature). A comparison with BZY20 control samples indicated that the proper amount of BaCO₃ introduced on the BZY20 particle surface and the high green density achieved by cold sintering pretreatment were the main drivers for lowering the sintering temperature. The electrical conductivity measurement by electrochemical impedance spectroscopy showed that the as-prepared BZY20 pellets have a proton conductivity comparable to the state-of-the-art values. The cold sintering pretreatment outlined in this work has the potential to lower the sintering temperatures for similar types of protonic ceramic materials under consideration for a wide range of energy conversion and storage applications.     

Cold sintered,temperature-stable CaSnSiO5-K2MoO4 composite microwave ceramics and its prototype microstrip patch antenna

Dense (1-x)wt%CaSnSiO₅-xwt%K₂MoO₄ (CSSO-KMO) composite ceramics were fabricated by the cold sintering process at 180 °C under 400 MPa for 60 min. X-ray diffraction, Energy dispersive X-ray and Raman spectroscopy confirmed that CSSO and KMO coexisted without intermediate phases. As KMO weight fraction increased, relative permittivity (ε_r) and temperature coefficient of resonant frequency (τ_f) decreased and the microwave quality factor (Q×f, where f is resonant frequency) increased. Near-zero τ_f (-0.5 ppm/°C) was obtained for 65 wt%CSSO-35 wt%KMO with ε_r ～ 9.2 and Q×f ～ 6240 GHz. No chemical reaction between ceramic composites and silver was observed, demonstrating potential for cofiring with Ag-paste. A prototype antenna was fabricated from 65 wt%CSSO-35 wt%KMO composite ceramic with a bandwidth of 144 MHz @ -10 dB, a gain of 5.7 dBi and a total efficiency of 88.4 % at 5.2 GHz, suitable for 5 G mobile communication systems.     

Dense and core-rim structured B4C-TiB2 ceramics with Mo-Co-WC additive

B₄C-TiB₂ ceramics (TiB₂ ranging 5~70 vol%) with Mo-Co-WC as the sintering additive were prepared by spark plasma sintering. In comparison with B₄C-TiB₂ without additive, the enhanced densification was evident in the sintered specimen with Mo-Co-WC additive. Core-rim structured grain was observed around TiB₂ grains. The interface of the rim between TiB₂ and B₄C phases demonstrated different feature: the inner borderline of the rim exhibited a smooth feature, whereas a sharp curved grain boundary was observed between the rim and the B₄C grain. The formation mechanism is discussed: the epitaxial growth of (Ti,Mo,W)B₂ rim around the TiB₂ core may occur as a result of the solid solution and dissolution-precipitation between TiB₂ phase and the sintering additive. It was revealed that the fracture toughness increased as the content of TiB₂ content increased, alongside the decreased hardness. B₄C-30 vol% TiB₂ specimen demonstrated the optimal combination of mechanical properties, reaching Vickers hardness of 24.3 GPa and fracture toughness of 3.33 MPa·m^1/2.     

Chromium-promoted preparation of forsterite refractory materials from ferronickel slag by microwave sintering

The chromium-promoted preparation of forsterite refractory materials from ferronickel slag was investigated by microwave sintering of the slag with the additions of sintered magnesia and 0–10 wt% chromium oxide (Cr₂O₃). The thermodynamic calculations revealed that the addition of Cr₂O₃ can promote the formations of spinel and liquid phase and maintain high content of forsterite below 1500 °C. The experimental results showed that there existed a stronger promoting effect of Cr₂O₃ additive on the properties of refractory materials in the microwave field than that in conventional sintering. It was attributed to the preferential formation and growth of spinel with stronger microwave absorption than other phases (e.g., enstatite), the existence of more forsterite, and the enhanced densification in association with the presence of more liquid phase at the same temperature. By microwave sintering of the mixture of ferronickel slag, 25 wt% sintered magnesia, and 4 wt% Cr₂O₃ at 1350 °C for 20 min, a superior refractory material with refractoriness of 1801 °C, thermal shock resistance of 6 times, bulk density of 2.97 g/cm³, apparent porosity of 1.4%, and compressive strength of 197 MPa was obtained. Compared with that prepared by conventional sintering at 1350 °C for 2 h, the refractoriness and thermal shock resistance were increased by 175 °C and 100%, respectively. The present study provided a novel method for preparing high-quality refractory materials from ferronickel slag and relevant industrial wastes.     

Achieving fabrication of highly transparent Y2O3 ceramics via air pre-sintering by deionization treatment of suspension

An easy albeit quite effective deionization suspension treatment was adopted to alleviate the detrimental effects related to the hydrolysis of Y₂O₃ in an aqueous medium. Fabrication of highly transparent Y₂O₃ ceramics with a fine grain size via air pre-sintering and post–hot isostatic pressing (HIP) treatment without using any sintering additive was achieved using the treated suspensions. The hydrolysis issue of Y₂O₃ powder in an aqueous medium was effectively alleviated by using deionization treatment, and a well-dispersed suspension with a low concentration of dissolved Y³⁺ species was obtained. The dispersed suspensions were consolidated by the centrifugal casting method, and the green bodies derived from the suspension of 35.0 vol% solid loading showed an improved homogeneity with a relative density of 52.1%. Fully dense Y₂O₃ transparent ceramic with high transparency was obtained by pre-sintering consolidated green compacts at a low temperature of 1400°C for 16 h in air followed by a post-HIP treatment at 1550°C for 2 h under 200 MPa pressure. The sample had a fine average grain size of 690 nm. The in-line transmittance of the sample reached 83.3% and 81.8% at 1100 nm and 800 nm, respectively, very close to the theoretical values of Y₂O₃.