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1.
We have successfully developed transparent polycrystalline Gd2Hf2O7 ceramics with high in‐line transparency. A sol–gel process was used to synthesize the Gd2Hf2O7 powder. Simultaneous thermal gravimetric analysis and differential thermal analysis (TGA/DTA) was used to identify the decomposition sequence as a function of temperature for the as‐synthesized sol–gel powders. The calcined powder is single phase and was formed with an estimated average particle size of 120 nm. Crystallization was confirmed by x‐ray diffraction (XRD) and a single phase was achieved by calcining at 1000°C. The calcined powders were hot‐pressed at 1500°C to achieve >95% theoretical density with closed pore structure followed by a hot isostatic pressing at 1500°C at 207 MPa to achieve a fully dense structure. Microstructural characterization shows a uniform grain size distribution with an average grain size of about 11 μm. In‐line transmission measurements revealed high transparency in the red and infrared. Dielectric properties remain stable with relative permittivity values around 180 and loss tangents less than 0.005 up to 350°C. Thermal conductivity was measured to be ~1.8 W/m°K at room temperature, decreasing to ~1.5 W/m°K by 500°C.  相似文献   

2.
A glucose sol–gel combustion method has been developed to synthesize composite nanopowders with equal volume fractions of Y2O3 and MgO. The synthesis involves the generation of precursor foam containing Y3+ and Mg2+ cations via the chemical and thermal degradation of glucose molecules in aqueous solutions. Subsequent calcination of the foam gave the composite nanopowders uniform composition and surface areas of 44–62 m2/g depending on the relative amount of glucose. Then the nanopowder with an average particle size of 19 nm was consolidated by the hot‐pressing technique with different sintering temperatures. The fabricated nanocomposite is mid‐infrared transparent as the result of fine grains, narrow grain size distribution, and uniform phase domains. The transmittance increases with increase in the sintering temperature and reaches 83.5% at 3–5 μm mid‐infrared wave range once the temperature reaches 1350°C, which is close to the theoretical value of 85%. And it is noteworthy that the cutoff wavelength reaches 9.6 μm, which is superior to those of spinel, AlON, and sapphire. And the Vickers hardness of the sample reaches 10.0 ± 0.1 GPa, which is significantly higher than those of the coarse grained single‐phase MgO and Y2O3. The results indicate that the glucose sol–gel combustion and hot‐pressing technique is an effective method to fabricate infrared transparent Y2O3–MgO nanocomposites.  相似文献   

3.
Transparent polycrystalline Gd3TaO7 ceramics were successfully developed. A sol‐gel process was used to synthesize Gd3TaO7 powder with a uniform composition and an estimated average particle size of 100 nm. Simultaneous thermal gravimetric analysis and differential thermal analysis (TGA/DTA) was used to identify the decomposition sequence as a function of temperature for the as‐synthesized sol‐gel powders. Crystallization was confirmed by X‐ray diffraction (XRD) and a single phase was achieved by calcining at 1000°C. The calcined powders were hot‐pressed at 1400°C to achieve >96% theoretical density with closed pore structure followed by a hot isostatic pressing at 1400°C at 207 MPa to achieve a fully dense structure. Microstructural characterization shows a uniform grain size distribution with an average grain size of about 7 μm. In‐line transmission measurements revealed high transparency in the red and infrared. Thermal conductivity was measured to be >1.6 W/mK at room temperature, decreasing to ~1.3 W/mK by 500°C. Dielectric properties remain stable with relative permittivity values just above 200 and loss tangents <0.005 up to 350°C.  相似文献   

4.
A novel composite ceramic, composed of equal-volumetric Zr-stabilized Gd2O3 and MgO phases, was prepared to be transparent in mid-wave infrared range. Zr stabilized Gd2O3 is proved to have a lower lattice parameter (10.7516 Å) using XRD refinement. Pressureless sintering behavior of Gd2O3-MgO with/without 2 at% Zr-doping (naming ZGM and GM) was studied via the real-time observation technique. The shrinkage of ZGM green body proceeds steadily up to 1400 °C while that of the undoped one shrinks sharply at 1250 °C due to Gd2O3 phase transition. The segregation of Zr element along the grain boundaries of Zr-Gd2O3 creates a synergized effect on the grain refinement with pinning effect. Dense ZGM ceramics exhibit superior transmittance of 78.3 %‐85.6 % at 3–5 µm, which show good consistency with the calculated values. The refractive index of Zr- Gd2O3 varies from 1.87 at 3 µm to 1.80 at 5 µm, which is smaller than those of monoclinic Gd2O3.  相似文献   

5.
To decrease the sintering temperature of MgO‐Y2O3 composites to avoid undesired grain coarsening, high reactive MgO‐Y2O3 nanopowders were synthesized via microwave combustion method. The degree of combustion was enhanced effectively by adding an extra oxidant ammonium nitrate. The as‐synthesized MgO‐Y2O3 nanopowders, ~18 nm in size, showed high specific surface area of 64.55 m2/g and low agglomeration. Relative density of 98% was obtained when sintered at a low sintering temperature of 1350°C. The high reactivity can be attributed to the lower activation energy Q (131.13 kJ/mol), compared with samples without extra oxidant (192.97 kJ/mol).  相似文献   

6.
The transition from the cubic to monoclinic phase of Gd2O3 at high temperatures poses a significant challenge to the preparation of transparent Gd2O3 materials. In this work, we presented a straightforward yet effective method for fabricating transparent Gd2O3 ceramics. Via ZrO2 stabilization effect for phase structure, highly transparent Gd2O3 ceramics were successfully fabricated by vacuum sintering at 1850 °C for 8 h. The effect of different Zr (0 ∼ 13 at%) concentrations on phase transition, grain growth, fracture mode and optical properties of Gd2O3 transparent ceramics was investigated. As the Zr content increases, the transition from the cubic (C) to monoclinic (M) phase is effectively suppressed, which is crucial for achieving Gd2O3 transparent ceramics. Moreover, the results indicate that the addition of ZrO2 has a significant effect on grain growth by not only impeding the migration of grain boundaries but also affecting the phase composition. In addition, the 11 at% Zr-doped Gd2O3 ceramic exhibits the best optical properties, of which transmittance is about 76% at 850 nm and about 80% in the 2.5 µm ∼ 6 µm mid-infrared range. This work provides an illustrative example for the development of other ceramics with phase transition. The obtained Zr-doped Gd2O3 transparent ceramics with high optical quality are potential candidates for optical window, scintillator host and mid-infrared transmission materials.  相似文献   

7.
This work attempts to obtain Dy3+‐doped SiO2–Gd2O3 by sol–gel process, with a molar ratio of 70Si4+–30Gd3+ and Dy3+ concentrations of 0.1, 0.3, 0.5, and 1 mol%. Heat treatment at temperatures of 1000°C, 1100°C, 1200°C, and 1300°C have been performed. From XRD, the Gd2O3 cubic phase was observed at 1000°C and 1100°C, at 1200°C also were observed Gd2O3 monoclinic phase, predominant at 1300°C. The band‐gap values vary between 4.4 and 5.3 eV, showing dependence on the crystalline phase. Under UV excitation, emission spectra show bands assigned to the Dy3+ transitions: 4F9/26H15/2 (484 nm), 4F9/26H13/2 (572 nm), and 4F9/26H11/2 (668 nm). The excitation at 275 nm has shown more effective. The ratio between the most intense emission bands (yellow/blue) show values around 0.84 and 1.63. CIE chromaticity diagrams show color coordinates at blue, yellow, and white regions, as a function of Dy3+ concentration and heat treatment. The lifetime values of excited state 4F9/2 were around 0.20 and 0.69 ms. The morphology of particles changed from spherical to coral‐like shape as a function of heat treatment are observed. The sol–gel process showed to be an interesting route to obtain Dy3+‐doped binary system materials.  相似文献   

8.
New phase diagram data and a thermodynamic assessment of the CeO‐Gd2O3‐CoO system using the CALPHAD approach are presented. This information is needed to understand the surprisingly low sintering temperature (950°C–1050°C) of CeO2‐based materials doped with small amounts of transition metal oxide (e.g., CoO). Experimental phase equilibria between 1100°C and 1300°C are reported based on the analysis of annealed and molten samples. No isolated compound exists in the ternary. At 1300°C the Co solubility in the ternary compounds Ce1?x?yGdxCoyO2?x/2?y (fluorite) is 2.7 mol% and is less than 1 mol% in the Gd2?xCexO3+x/2 (bixbyite). The Ce solubility in the perovskite GdCoO3?δ was found to be 1 mol%. The lowest temperature eutectic melt in the ternary has a composition of 57.2 mol% Co and 41.1 mol% Gd melting at an onset temperature of 1303 ± 5°C, which is close to the binary eutectic in the Gd2O3‐CoO system at 60 ± 2 mol% Co and 1348 ± 1°C.  相似文献   

9.
Thin Gd2O3 films with a thickness of about 150 nm were deposited by pulsed layer deposition on polycrystalline CeO2 substrates to study the structural evolution of the Ce1−xGdxO2−x/2 system with respect to phase formation and cation interdiffusion in the temperature range between 986 °C and 1270 °C. Transmission electron microscopy combined with quantitative energy dispersive X-ray spectroscopy was applied to study the microstructure and to obtain composition profiles across the Gd2O3/CeO2-interface. Gd2O3 was observed to occur in the bixbyite structure up to 1175 °C. The fluorite and the bixbyite phase are found at intermediate compositions without any indication for a miscibility gap. Interdiffusion coefficients were obtained from Gd2O3/CeO2-concentration profiles on the basis of the diffusion-couple solution of the diffusion equation. The activation enthalpy and frequency factor of the diffusion coefficient were derived assuming an Arrhenius-type behavior in the investigated temperature range.  相似文献   

10.
Magnesium aluminate spinel solid solutions with the alumina‐rich compositions MgO·2Al2O3 and MgO·2.5Al2O3 have been prepared as polycrystalline ceramics with average in‐line transmissions at 550 nm of 85.5 ± 0.3% and 80.9 ± 0.4%, respectively. Starting powders are prepared from combinations of high purity Mg(OH)2 and γ‐Al2O3 thoroughly mixed in an aqueous slurry, and the solids are collected, dried, calcined, mixed with LiF sintering aid, and sieved. The optimum amount of LiF added varies with the alumina composition of the spinel solid solution. The powders are sintered into dense ceramics by hot pressing at 1600°C under vacuum and 20 MPa uniaxial load followed by hot isostatic pressing at 1850°C under 200 MPa in Ar. Both compositions exhibit exaggerated grain growth with average sizes well over 500 μm. Knoop hardness measurements are 11.2 ± 0.3 GPa for MgO·2Al2O3 and 11.0 ± 0.4 GPa for MgO·2.5Al2O3.  相似文献   

11.
Nanocrystals with orange‐reddish luminescence based on the pyrochlore‐type complete solid solutions with cube‐like morphology in the Eu2Sn2O7–Gd2Sn2O7 system were directly formed from the precursor solutions of SnCl4, GdCl3, and EuCl3 under weakly basic hydrothermal conditions at temperatures higher than 180°C for 5 h. The crystallite of Gd2Sn2O7 pyrochlore gradually grew from 10 to 37 nm as the hydrothermal treatment temperature rose from 180°C to 240°C. The lattice parameter of cubic phase linearly increased with increased europium concentration according to the Vegard's law. The characteristic orange‐reddish photoluminescence spectra of Gd2Sn2O7:Eu3+ cubelike nanocrystals with crystallite size from 34 to 37 nm that were formed at 240°C for 5 h were attributed to the most sharp orange (586 nm) luminescence with high intensity and quite broad red (610–630 nm) emission with weak intensity, according to the 5D07F1 and 5D07F2 transitions of Eu3+, respectively. At a composition of (Eu0.09Gd0.91)2Sn2O7, the intensity of orange emission reached the maximum. The Red‐to‐Orange (5D07F2/5D07F1) (R/O) emission intensity ratio was in the low range from 0.10 to 0.14, which was a characteristic of Gd2Sn2O7:Eu3+.  相似文献   

12.
A sol–gel combustion method has been used to synthesize Y2O3–50 vol%MgO composite nanopowders. Solutions of the precursor nitrates were mixed with citric acid and ethylene glycol, heated from 200°C to a predetermined temperature gradually, giving nanocrystalline ceramic powders. The influence of the ratio of yttrium nitrate to the whole precursor mixture and the holding temperature on the properties of the composite nanopowder was investigated using a combination of thermal analysis, X‐ray diffraction, specific surface area analysis, and scanning electron microscopy techniques. When the ratio of yttrium nitrate to the whole precursor mixture reaches 22.5 mol%, the average particle size of synthesized composite nanopowder is 13 nm and the specific surface area is 45.9 m2/g. Then the synthesized Y2O3–MgO composite nanopowder was consolidated by the hot‐pressing technique at 1200°C with different dwell time. As a result, the nanocomposite ceramic prepared with a dwell time of 60 min got the highest transmittance of 75% at 5 μm wavelength. The cut‐off wavelength of Y2O3–MgO nanocomposite ceramic reaches 9.8 μm, which is superior to other mid‐IR transparent materials. In addition, the fabricated sample is more or less transparent in visible wavelengths and the transmittance at 0.8 μm is as high as 14.5%.  相似文献   

13.
《Ceramics International》2023,49(4):5770-5775
In this work, MgAl2O4: Cr3+ transparent ceramics have been synthesized by the hot press sintering techniques, and the effect of the sintering aid Gd2O3 and its content on the densification, microstructure, and optical, photoluminescence was studied and discussed. The relative density reached 99.29% with 0.8 wt% Gd2O3 as a sintering aid, and the optical transmittance at 686 nm and 1446 nm were approximately 76%. As Gd2O3 content continued to increase, the grain size of the ceramics became smaller and uniform, accompanied by some pores with the size of ~1 μm. The ceramics with 4.0 wt% Gd2O3 showed a higher transmittance, of 82% at 1446 nm. Additionally, Gd2O3 was helpful for Cr3+ in the sites of octahedral symmetry, which increased the quantum yield. The quantum yield of MgAl2O4: Cr3+ with 0.8 wt% Gd2O3 was about 0.175, which was 36% higher than that of ceramic without Gd2O3. In short, the sintering aid Gd2O3 not only contributed to improving the densification, homogenizing the grain size, and heightening the optical transmittance but also enhanced the quantum yield of Cr3+.  相似文献   

14.
(Gd1−xYbx)2Zr2O7 compounds were synthesized by solid reaction. Yb2O3 doped Gd2Zr2O7 exhibited lower thermal conductivities and higher thermal expansion coefficients (TECs) than Gd2Zr2O7. The TECs of (Gd1−xYbx)2Zr2O7 ceramics increased with increasing Yb2O3 contents. (Gd0.9Yb0.1)2Zr2O7 (GYbZ) ceramic exhibited the lowest thermal conductivity among all the ceramics studied, within the range of 0.8–1.1 W/mK (20–1600 °C). The Young's modulus of GYbZ bulk is 265.6 ± 11 GPa. GYbZ/YSZ double-ceramic-layer thermal barrier coatings (TBCs) were prepared by electron beam physical vapor deposition (EB-PVD). The coatings had an average life of more than 3700 cycles during flame shock test with a coating surface temperature of ∼1350 °C. Spallation failure of the TBC occurred by delamination cracking within GYbZ layer, which was a result of high temperature gradient in the GYbZ layer and low fracture toughness of GYbZ material.  相似文献   

15.
《Ceramics International》2022,48(21):31326-31333
The present work describes a multi-stage processing method for the hydrothermal synthesis of gadolinium oxide (Gd2O3) nanoparticles and subsequent surface modification with iron oxide (Fe3O4) and dextrose. To prepare gadolinium oxide nanoparticles, gadolinium chloride was reacted with sodium hydroxide, and the resulting precipitate was autoclaved. Subsequently, the product was calcined. Afterward, Gd2O3 nanoparticles were coated with a Fe3O4 nanolayer synthesized via coprecipitation, and the resulting core-shell nanocomposites were encapsulated in a dextrose capping agent for enhanced biocompatibility. The effect of various Gd2O3 synthesis parameters on particle size, structure, and magnetic properties was then investigated. These parameters included preliminary precipitation temperature (25, 90 °C) and stirring speed (400, 1000 rpm), hydrothermal temperature (150 and 180 °C) and pressure (5 and 10 bar), and final calcination temperature (600 and 1000 °C). For the investigation of nanocomposites, X-ray diffraction (XRD), scanning and transmission electron microscopy, dynamic laser scattering (DLS), Fourier-Transform infrared spectroscopy (FTIR), and magnetometry (VSM) techniques were used, while the viability of colloidal samples was determined using the MTT-assay method. The results indicated that increasing the steering speed and temperature of the precipitation process and raising the calcination temperature reduced the size of Gd2O3 nanoparticles. Autoclave dehydration had no discernible effect on Gd2O3 nanoparticles. TEM and SEM images confirmed the core/shell structure of Gd2O3/Fe3O4. The shell thickness of 74–95 nm core nanoparticles was in the range of 30–40 nm. With a saturation magnetization of 3.4 emu/g, the nanoparticles exhibited paramagnetic behavior. The 48-h MTT assay demonstrated excellent biocompatibility up to 285 μg solid concentrations containing 24.5 μg [Fe] and 91.2 μg [Gd], with viability remaining greater than 50% at 400 μg solid concentration.  相似文献   

16.
Highly transparent (Y0.95?xGdxEu0.05)2O3 (= 0.15–0.55) ceramics have been fabricated by vacuum sintering at the relatively low temperature of 1700°C for 4 h with the in‐line transmittances of 73.6%–79.5% at the Eu3+ emission wavelength of 613 nm (~91.9%–99.3% of the theoretical transmittance of Y1.34Gd0.6Eu0.06O3 single crystal), whereas the = 0.65 ceramic undergoes a phase transformation at 1650°C and has a transparency of 53.4% at the lower sintering temperature of 1625°C. The effects of Gd3+ substitution for Y3+ on the particle characteristics, sintering kinetics, and optical performances of the materials were systematically studied. The results show that (1) calcining the layered rare‐earth hydroxide precursors of the ternary Y–Gd–Eu system yielded rounded oxide particles with greatly reduced hard agglomeration and the particle/crystallite size slightly decreases along with increasing Gd3+ incorporation; (2) in the temperature range 1100°C–1480°C, the sintering kinetics of (Y0.95?xGdxEu0.05)2O3 is mainly controlled by grain‐boundary diffusion with similar activation energies of ~230 kJ/mol; (3) Gd3+ addition promotes grain growth and densification in the temperature range 1100°C–1400°C; (4) the bandgap energies of the (Y0.95?xGdxEu0.05)2O3 ceramics generally decrease with increasing x; however, they are much lower than those of the oxide powders; (5) both the oxide powders and the transparent ceramics exhibit the typical red emission of Eu3+ at ~613 nm (the 5D07F2 transition) under charge transfer (CT) excitation. Gd3+ incorporation enhances the photoluminescence and shortens the fluorescence lifetime of Eu3+.  相似文献   

17.
《Ceramics International》2022,48(12):16839-16844
In this work, the effects of starting oxide powders with different-scale particle sizes on the synthesis of gadolinium zirconate pyrochlore (Gd2Zr2O7, GZO) and its physical properties were studied. Micron Gd2O3 (μG), micron ZrO2 (μZ), nano Gd2O3 (nG), and nano ZrO2 (nZ) powders were used. GZO ceramics were prepared by employing solid-state reactive sintering at 1300 °C, 1400 °C, 1500 °C and 1600 °C with mixed powders of different sizes (μGμZ, μGnZ, nGμZ and nGnZ). X-ray diffraction and Raman analyses of the ceramics revealed that nG has a more significant impact on the crystallization process than nZ. All ceramics synthesized with different sized oxide powders crystallized into pyrochlore phases except for those synthesized with μGnZ mixed powders, which resulted in a fluorite phase. The results indicated that decreasing the particle size of only ZrO2 to synthesize pyrochlore-phase Gd2Zr2O7 with high crystallinity may not be effective. Samples obtained at 1500 °C were further analyzed. Scanning electron microscopy results revealed that all four ceramics have a non-homogeneous grain size and that the average grain size ranges from 5.40 to 8.30 μm. In addition, the density and Vickers hardness measurements showed that the use of nanopowders significantly improves the mechanical properties.  相似文献   

18.
《Ceramics International》2015,41(8):9692-9700
Spark plasma sintering followed by hot isostatic pressing was applied for preparation of polycrystalline alumina with submicron grain size. The effect of additives known to influence both densification and grain growth of alumina, such as MgO, ZrO2 and Y2O3 on microstructure development was studied. In the reference undoped alumina the SPS resulted in some microstructure refinement in comparison to conventionally sintered materials. Relative density >99% was achieved at temperatures >1200 °C, but high temperatures led to rapid grain growth. Addition of 500 ppm of MgO, ZrO2 and Y2O3 led, under the same sintering conditions, to microstructure refinement, but inhibited densification. Doped materials with mean grain size <400 nm were prepared, but the relative density did not exceed 97.9%. Subsequent hot isostatic pressing (HIP) at 1200 and 1250 °C led to quick attainment of full density followed by rapid grain growth. The temperature of 1250 °C was required for complete densification of Y2O3 and ZrO2-doped polycrystalline alumina by HIP (relative density >99.8%), and resulted in fully dense opaque materials with mean grain size<500 nm.  相似文献   

19.
《Ceramics International》2022,48(18):26387-26392
In this study, nano-grained Gd2Zr2O7 (NGZO) ceramic with a high relative density was prepared by a novel cold sintering process (CSP) assisted by microwave sintering (CSP-MS). The CSP with water as the liquid phase at 280 °C yielded nano-grained ceramic with a relative density of 71.5%. NGZO with a high relative density of 97.1% and average grain size of 73 nm was obtained by subsequent microwave sintering of the cold-sintered sample at 1300 °C. Therefore, CSP-MS is feasible in preparing dense NGZO ceramics with small grain sizes at relatively low sintering temperatures.  相似文献   

20.
O'-Sialon/Si3N4 composite ceramics for solar absorber were prepared in situ through pressureless sintering from Si3N4 and low pure Al2O3 with different rare-earth oxides (i.e., Yb2O3 and Gd2O3). This study investigates the effects of Yb2O3 and Gd2O3 on phase composition, microstructure, densification, oxidation resistance and solar absorptance. The results revealed that Yb2O3 and Gd2O3, which were applied as flux materials, significantly reduced the sintering temperature and improved the densification, oxidation resistance of the composite ceramics. Moreover, the introduction of the two sintering aids promoted the formation of O'-Sialon through the liquid-phase sintering mechanism. The samples doped with Gd2O3 exhibited more O'-Sialon content, lower porosity, and better oxidation resistance compared with those doped with Yb2O3. Especially, sample A2 (6 wt% Gd2O3 additional) sintered at 1600 °C exhibited the best comprehensive properties for 10.10% water absorption, 23.29% porosity, 105.57 MPa bending strength, 75.16% solar absorption. Dense oxide layers were generated on sample surfaces after oxidation at 1300 °C, which protected the ceramics samples from further oxidation. However, the two additives had characteristic reflection peaks in the ultraviolet–visible region (300–400 nm) and were also blamed for high reflectivity in the near–infrared region, which resulted in the decrease in absorption.  相似文献   

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