One-step hydrothermal synthesis of yttria-stabilized tetragonal zirconia polycrystalline nanopowders for blue-colored zirconia-cobalt aluminate spinel composite ceramics

A novel approach for the preparation of blue-color giving zirconia nanopowders by doping of 3?mol% Y₂O₃ through simple one-step hydrothermal process is proposed. A blue-color giving yttria-stabilized tetragonal zirconia polycrystalline (Y-TZP) powders were prepared by urea-based solution, zirconium acetate, CoCl₂·6H₂O and AlCl₃ precursors in hydrothermal vessel at 24?h, 150?°C and 20 bars. Based on the results, the synthesized blue-color giving Y-TZP nanopowders have entirely tetragonal structure as mono phase with 3.8?±?0.2?nm average grain size and (Y, Co, Al)_xZrO₂; x?≤?0.03?at. with chemical composition. Thermal treatment was also applied to synthesized Y-TZP powders at 1200?°C and 1450?°C to observe the color evolution. Only sharp blue was obtained in Y-TZP powders resulting the development of zirconia-cobalt aluminate spinel (ZrO₂-CoAl₂O₄) composite ceramic structure for both temperatures after heat-treatment. Herein, not only formation of CoAl₂O₄ but also incorporation of cobalt (Co) and aluminum (Al) into the Y-TZP grains plays a critical role on evolving of blue color. This synthesized Y-TZP nanopowders can be a good candidate for one-step production of blue-color sintered ZrO₂-CoAl₂O₄ spinel composite ceramics in numerous ceramic applications due to their superior structural and functional properties.     

Erbium-doped LAS glass ceramics prepared by spark plasma sintering (SPS)

Dense nanocrystalline glass ceramics of the Li₂O–Al₂O₃–SiO₂ (LAS) system were obtained by spark plasma sintering (SPS) of powders prepared by sol–gel method. The low thermal expansion LAS glass ceramic was chosen as host matrix for erbium ions. ZrO₂ was added both as a nucleating agent and as a possible good environment for the rare earth. The developed crystalline phases were analysed by X-ray diffraction (XRD) and the amorphous phase was quantified. Scanning and transmission electron microscopy (SEM, TEM) was used to investigate the microstructure. A different behaviour during the crystallisation process was observed between the sample prepared through the sintering of powders and the glass produced by the melting technique. A photoluminescence characterisation was also performed.     

The Effects of pH and Alkaline Earth Ions on the Formation of Nanosized Zirconia Phases Under Hydrothermal Conditions

The phase composition and crystallite size of zirconia formed under hydrothermal conditions is strongly dependent on crystallization conditions, in particular, pH and a mineralizer. Monoclinic ZrO₂ formed easily in the strong acid and basic media. When pH<1 or >14, monoclinic ZrO₂ was exclusively obtained and its crystallite size increased with increasing pH. In the range of pH 1–14, products of hydrothermal reaction are a mixture of monoclinic and tetragonal ZrO₂. The effects of Mg²⁺, Ca²⁺ and Sr²⁺ ions on the formation of zirconia under hydrothermal conditions were investigated. The presence of these bivalent M²⁺ ions was in favour of the formation of tetragonal (or cubic) ZrO₂. The nanosized ZrO₂ crystallites of cubic and tetragonal symmetry were obtained at pH 10, 220°C for 2 h and in the case of Ca²⁺ and Sr²⁺ as mineralizer, respectively.     

Structural and luminescence properties of silica powders and transparent glass‐ceramics containing LaF3:Eu3+ nanocrystals

In this work, silica powders and transparent glass‐ceramic materials containing LaF₃:Eu³⁺ nanocrystals were synthesized using the low‐temperature sol‐gel technique. Prepared samples were characterized by TG/DSC analysis as well as X‐ray diffraction and IR spectroscopy. The transformation from liquid sols toward bulk powders and xerogels was also examined and analyzed. The optical behavior of prepared Eu³⁺‐doped sol‐gel samples were evaluated based on photoluminescence excitation (PLE: λ_em = 611 nm) and emission (PL: λ_exc = 393 nm, λ_exc = 397 nm) spectra as well as luminescence decay analysis. The series of luminescence lines located within reddish‐orange spectral scope were registered and identified as the intra‐configurational 4f⁶‐4f⁶ transitions originated from Eu³⁺ optically active ions (⁵D₀ → ⁷F_J, J = 0‐4). Moreover, the R/O‐ratio was also calculated to estimate the symmetry in local framework around Eu³⁺ ions. The luminescence spectra and double‐exponential character of decay curves recorded for fabricated nanocrystalline sol‐gel samples (τ₁(⁵D₀) = 2.07 ms, τ₂(⁵D₀) = 8.07 ms and τ₁(⁵D₀) = 0.79 ms, τ₂(⁵D₀) = 9.76 ms for powders and glass‐ceramics, respectively) indicated the successful migration of optically active Eu³⁺ ions from amorphous silica framework to low phonon energy LaF₃ nanocrystal phase.     

Color tunable up-conversion emission of ZrO2:Yb3+, Er3+ thin films prepared by chemical solution deposition

The color-tunable up-conversion (UC) emission was observed in ZrO₂:Yb³⁺, Er³⁺ thin films synthesized on fused silica substrates using a chemical solution deposition method. The crystal structure, surface morphology image and optical transmittance of ZrO₂:Yb³⁺, Er³⁺ thin films were detected in the matter of Yb³⁺/Er³⁺ doping content. Under excitation by 980?nm infrared light, intense UC emission can be obtained from ZrO₂:Yb³⁺, Er³⁺ thin films. Photoluminescence study shows that there are two emission bands centered at 548?nm and 660?nm in the UC luminescence spectra, which can be owing to (²H_11/2,⁴S_3/2)→⁴I_15/2 and ⁴F_9/2→⁴I_15/2 transitions of Er³⁺ ions, respectively. In addition, the color coordinate of UC emission between green-red can be tuned by properly adjusting the dopant concentration, because the composition of Yb³⁺/Er³⁺ affect the red/green ratio via the process of cross relaxation and energy back transfer. Our study suggests that ZrO₂:Yb³⁺, Er³⁺ thin films can be considered as promising materials for new photoluminescence devices.     

Preparation and properties of Eu and Dy co-doped strontium aluminate long afterglow nanomaterials

The long afterglow nanomaterials of strontium aluminate co-doped by Eu and Dy have been synthesized by co-precipitation combined hydrothermal method. The effects of hydrothermal time, calcination time, pH value, the amount of aluminum nitrate, activator, co-activator and flux H₃BO₃ on the fluorescence properties of the product were investigated by means of single factor optimization experiment. Then the orthogonal experiment was employed to obtain the optimal synthesis conditions that are as follows: n_Dy/n_Eu = 2.5, t_c = 2.5?h, n_Eu/n_Sr = 0.02, t_h = 8?h. Subsequently, the optimal synthesis conditions were verified by three repeated experiments, and the obtained products were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and fluorescence spectrometer. The results showed that the synthesized target products all were the mixed crystal phase of SrAl₂O₄ and Sr₄Al_l4O₂₅. The particles presented regular spherical-like with size ~ 100?nm. The dopants Eu and Dy were confirmed existed in the SrAl₂O₄ powders. The fluorescence and afterglow data of the target products were better than that in the orthogonal experiment scheme. The primary emission spectra band was in the range of 400–600?nm with characteristic peak located at ~ 460?nm corresponding to the transitions of Eu²⁺ ions from 4f⁶5d→4f⁷, and the blue light can be observed by naked eyes. The similar fast-decaying and slow-decaying processes were displayed in all the afterglow curves, and the initial afterglow brightness of the target product is apparently higher than that of products synthesized by the orthogonal experiment. The synthesized target products, which show excellent long afterglow performance, present a great application prospects in the aspects of ceramics, plastics, arts and crafts, ink and coating.     

Enhanced Activation Energy of Crystallization of Pure Zirconia Nanopowders Prepared via an Efficient Way of Synthesis Using NaBH4

An efficient way through borohydride synthesis route using NaBH₄ was performed to prepare pure zirconia nanopowders via three different conditions such as gelation, precipitation, and constant pH. Zirconia powders prepared through constant pH route show highest activation energy of crystallization (E_a = 260 kJ/mol) or higher exothermic peak temperature (717°C), when compared with gelation or precipitation route due to its controlled growth of smaller crystallites. The released huge amount of H₂ gas bubbles during borohydride synthesis via constant pH route play a major role for formation of loose smaller crystallites and thus enhances the activation energy of crystallization of pure zirconia. So, the as‐prepared zirconia powders prepared through constant pH route remain amorphous up to 600°C and pure t‐ZrO₂ (~20 nm) was stable up to 800°C.     

Photoluminescence properties of Eu3+-doped stalk-like Al2O3 via a hydrothermal route followed by heat treatment

ABSTRACT

Uniform Al₂O₃:Eu³⁺ samples were successfully fabricated via a hydrothermal method and subsequent thermal decomposition of Eu³⁺-doped precursors. The sample characterisations were carried out by means of X-ray diffraction (XRD), scanning electron microscope (SEM) and photoluminescence spectra. XRD results revealed Eu³⁺-doped samples were a pure γ-Al₂O₃ phase after being calcined at 1173?K. SEM results showed that these Eu³⁺-doped Al₂O₃ samples were stalk-like, with an average length of 1.5?μm. Upon excitation at 394?nm, the orange–red emission bands, having wavelengths longer than 580?nm, were to be from ⁵D₀→⁷F_J (J?=?1, 2) transitions. The asymmetry ratio of (⁵D₀→⁷F₂)/(⁵D₀→⁷F₁) intensity is about 0.54, 2.76, 3.29, 2.86, 3.36, 3.13 for Eu³⁺ concentrations of 0.1, 0.4, 0.7, 1.0, 1.5 and 2.0?mol-%, respectively. The optimal doping concentration of Eu³⁺ ions in Al₂O₃ is 1.5?mol-%. According to Dexter's theory, the critical distance between Eu³⁺ ions for energy transfer was determined to be 14?Å.     

Synthesis and characterization of the crystalline powders on the basis of Lu2O3:Eu3+spherical submicron-sized particles

This study is devoted to the preparation of the crystalline powders on the basis of non-agglomerated monodisperse Lu₂O₃:Eu³⁺ spherical particles with the diameters in the range of 50–250 nm by the soft chemistry co-precipitation route. The influence of the synthesis parameters on control morphology, particles size and agglomeration in the final Lu₂O₃:Eu³⁺ powder was considered. Lu₂O₃:Eu³⁺ crystalline powders were characterized by means of electron microscopy methods (TEM, SEM), FT-IR spectroscopy, thermal analysis (TG-DTA) and X-ray diffractometry. The mechanisms of the precursor decomposition and crystallization at the temperatures ranging from 60 to 900 °C were discussed. It was shown that the powders obtained were characterized by the effective luminescence under X-ray excitation in λ = 575–725 nm spectral region corresponding to ⁵D₀ → ⁷F_J transitions (J = 0–4) of Eu³⁺ ions with a maximum at 612 nm and the luminescence intensity strongly depends on annealing temperature. The relative densities of the green-bodies on the basis of Lu₂O₃:Eu³⁺ powders were estimated and the sintering of compacts at the temperatures up to 1500 °C was studied.     

Structural and Optical Properties of Tunable Warm‐White Light‐Emitting ZrO2:Dy3+–Eu3+ Nanocrystals

A series of Dy³⁺–Eu³⁺‐codoped ZrO₂ nanocrystals with tetragonal and cubic symmetry was synthesized via a wet chemical reaction. When the Eu³⁺‐doping content was fixed, the crystal structure could be stabilized from the mixed phase to single cubic phase by simply adjusting the content of Dy³⁺. The cubic ZrO₂:Dy³⁺–Eu³⁺ nanoparticles exhibited spherical and nonagglomerated morphology. The effective phonon energy of cubic ZrO₂:5%Dy³⁺–5%Eu³⁺ was calculated to be 445 cm^?1, which is lower than the previously reported results. Extensive luminescence studies of ZrO₂:Dy³⁺–Eu³⁺ as a function of Dy³⁺ content demonstrated that the dopant concentration and its site symmetry play an important role in the emissive properties. Under 352 nm excitation, the increment of Dy³⁺ concentration in ZrO₂:Dy³⁺–Eu³⁺ led to an increase in orange (590 nm) and red (610 nm) emissions of Eu³⁺ ions, which are attributed to the ⁵D₀→⁷F_J(J = 1, 2) transitions of Eu³⁺ ions. This increment is possibly due to the efficient energy transfer (ET) ⁴F_9/2:Dy³⁺→⁵D₀:Eu³⁺. The phosphors can generates light from yellow through near white and eventually to warm white by properly tuning the concentration of Dy³⁺ ions through the ET and change in site symmetry. These phosphors may be promising as warm‐white‐/yellow‐emitting phosphors.     

Synthesis,microstructure and optical characterization of zirconium oxide nanostructures

Zirconium oxide (ZrO₂) nanostructures were synthesized by hydrothermal route. Surface morphology analysis depicts the formation of the nanobars and hexagonal-shaped nanodiscs at different synthesis conditions. The structural analysis confirms that the as-synthesized ZrO₂ product is of pure monoclinic phase (m-ZrO₂) with crystallite size of about 25 nm. The product consists of monodispersed nanoparticles of uniform composition, high purity, and crystallinity. The Raman spectra are quantitatively analyzed and the observed peaks are attributed to various vibration modes of the m-ZrO₂. The UV–vis absorption spectrum showed a strong absorption peak at about 292 nm and the estimated optical band gap was around 3.57 eV. Photoluminescence (PL) spectrum of ZrO₂ nanostructure showed a strong and broad emission peak at around 410 nm at room temperature, which can be attributed to the ionized oxygen vacancy in the material.     

Luminescent properties of MgAl2O4 ceramics doped with rare earth ions fabricated by spark plasma sintering technique

MgAl₂O₄ ceramics doped with rare earth ions (Eu²⁺ and Ce³⁺ ions) were fabricated by spark plasma sintering technique. A complex characterization of the crystalline and defect structure of the ceramic by XRD was carried out. Absorption, excitation, photo- and cathodoluminescence spectra were studied. The photoluminescence spectrum shifts to the blue region with a maximum at λ_em =?475?nm for the MAS:0.1Ce ceramics. The nature of this luminescence can be caused by the radiative transitions in the cerium ion 5d–4f. The emission spectrum of MAS:0.1Eu has a “green” band emission in range of 400–700?nm centered around 500?nm, which can be ascribed to the allowed 4f⁶5d¹→4f⁷ (5d–4f) transition of Eu²⁺. In the millisecond time range, simultaneously with the emission of the complex host centers, the impurity luminescence bands of the chromium ion are recorded. It was shown that cathodoluminescence spectra in nanosecond time range can be decomposed into several emission bands at 2.72, 3.01, 3.37, 3.63–3.82?eV caused by F-type centers. It was demonstrated that the Eu²⁺ and Ce³⁺ ions lead to change the intensity ratio of the luminescence bands. The luminescence decay kinetics of synthesized spinel ceramics in nano- and millisecond time range were investigated in detail.     

Re-passivation current of amorphous Zr65Al7.5Ni10Cu17.5 alloy in a Hanks’ balanced solution

To evaluate the repassivation behavior of amorphous phase with chemical and structural homogeneity, time transient of re-passivation current density was measured on amorphous Zr₆₅Al_7.5Ni₁₀Cu_17.5 alloy and crystalline pure Zr with a momentary fracture of a ribbon shaped specimen in an artificial body fluid. Current density abruptly increased to a peak, J_peak, and exponentially decreased to the constant value, J_∞, J_peak and J_∞ on the amorphous specimen were smaller than those on the crystalline specimen, indicating that the amorphous phase would show the smaller dissolution rate from bare metal surface and from a re-passive film than the crystalline specimen, respectively. On the other hand, decrease rate of the current density on the amorphous specimen was smaller than that on the crystalline specimen, indicating the regeneration of passive film on the amorphous specimen was delayed probably because the amount of metal ions dissolved at the initial stage, i.e. the source of re-passive film, was smaller on the amorphous specimen. Consequently, the total charge for the re-passivation of the amorphous specimen was smaller than that of the crystalline specimen, supposing that the amount of dissolved metal ions during re-passivation was smaller on the amorphous specimen than the crystalline specimen.     

Growth and characterization of the Al-doped and Al–Sn co-doped ZnO nanostructures

In the present work, well-dispersed structures of spherical-like pure ZnO, Al doped ZnO (AZO) and Al, Sn co-doped ZnO (ATZO) nanocrystals were successfully synthesized by using zinc acetate dihydrate as the starting material and also the low temperature hydrothermal process without any additional surfactant or catalytic agent. The ZnO structures were characterized by X-ray diffraction (XRD), and transmission electron microscopy (TEM). The XRD results revealed that ZnO powders have a hexagonal crystal structure and the TEM indicated that the nanoparticles self-aggregate. An X-ray photoelectron spectroscopy (XPS) study confirmed the substitution of Zn²⁺ by Sn and Al ions. Optical properties of the ZnO structures were investigated by Raman spectroscopy and room-temperature photoluminescence (PL) spectroscopy. The Raman spectroscopy results demonstrated that the doped ZnO nanoparticles had a higher crystalline quality than that of pure ZnO. Room-temperature PL spectra of these structures showed a strong UV emission peak and a relative weak green emission peak, and the UV peak of the doped ZnO nanoparticles was blue-shifted with respect to that of the undoped ZnO nanoparticles.     

Upconversion emission of ZrO2 nanoparticles doped with erbium (Er3+) and ytterbium (Yb3+), synthesized by hydrothermal route

This paper reports the luminescent response upconversion of zirconium oxide (ZrO₂) nanoparticles doped with erbium (Er³⁺) and ytterbium (Yb³⁺) ions, synthesized by hydrothermal route. X ray diffraction (DRX) showed that the synthesized material presents the face centered cubic (FCC) structure. High resolution transmission electron microscopy (HRTEM) showed the presence of crystals size smaller than 10 nm. The photoluminescent analysis allowed to observe an intense upconversion luminescence emission of the samples doped with both ions Er³⁺ and Yb³⁺, when these are excited with 910 nm laser source, showing the electronic transitions ⁴F_9/2 → ⁴I_5/2; ²H_11/2 → ⁴I_5/2; ⁴S_3/2 → ⁴I_15/2 of Er³⁺. Two decay times were observed, whose behavior can be associated to the average distance between erbium ions within the nanocrystals.     

Synthesis and structural,optical, photocatalytic,and electrochemical properties of undoped and yttrium-doped tetragonal ZrO2 nanoparticles

Template-free undoped and yttrium-doped tetragonal ZrO₂ nanoparticles were successfully synthesized using a hydrothermal technique, and their structural, morphological, optical, and electrochemical properties were characterized. The photocatalytic activity for the dye degradation of the Rhodamine B (RhB) was also studied under UV light irradiation. The tetragonal crystal phase of the nanoparticles was confirmed by XRD analysis. The observed peak shift in XRD patterns confirmed the incorporation of dopant into host lattice. The Yttrium-doped ZrO₂ nanoparticles showed a higher specific surface area and smaller optical band gap (191.5?m²/g and 3.66?eV) than the pristine ZrO₂ nanoparticles (108.6?m²/g and 4.94?eV). The yttrium-doped ZrO₂ nanoparticles exhibited greater photocatalytic activity (~98%) than the pure ZrO₂ nanoparticles within 40?min, due to their high specific surface area and reduced photogenerated charge carrier recombination rate. The Nyquist plot of yttrium-doped sample exhibited lower charge transfer resistance than that of the undoped sample. The photocurrent of the doped sample (28.6?mA/cm²) was ~9 times higher than that of pristine ZrO₂ sample (3.2?mA/cm²). The doped sample showed stable and higher photocurrent density up to 520?s under light illumination.     

Sol-gel synthesis and luminescence properties of Ba2SiO4:Sm3+ nanostructured phosphors

Ba₂SiO₄:Sm³⁺ nanostructure phosphors have been synthesized by a simple sol-gel method. Phase evaluation, structural characteristics and photoluminescence properties of the synthesized Ba₂SiO₄:Sm³⁺ powders were studied using field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric and differential thermal analysis (TG-DTA), Fourier transform infrared spectroscopy (FTIR), and photoluminescence spectroscopy (PL). X-ray diffraction results showed that all synthesized samples were single-phase barium silicate (Ba₂SiO₄) and samarium (Sm) ions were incorporated into the lattice of Ba₂SiO₄. Adding samarium to barium silicate changed the microstructure from vermicular to spherical structures. The Photoluminescence spectrum of Ba₂SiO₄:Sm³⁺ phosphors exhibited characteristic emission peaks at 562?nm which is due to the ⁴G_{5/2 →}⁶H_7/2 transition of samarium ions and corresponds to the orange region. The results showed that the barium silicate activated with 0.08?mol samarium exhibited the highest PL intensity.     

Effect of silica coating on the structural and luminescent properties of Sm3+/Yb3+ or Tm3+/Yb3+ co-doped TiO2 nanoparticles

The luminescent characteristics of spherical titanium dioxide (TiO₂) nanoparticles (NP's) doped with Sm³⁺/Yb³⁺ and Tm³⁺/Yb³⁺ with and without a silica coating were analyzed. These nanoparticles were synthesized using the spray pyrolysis technique and coated with silica through a wet chemical process. The Sm³⁺/Tm³⁺ and Yb³⁺ doping induces a triphasic poly-crystalline structure of rutile and anatase TiO₂ and a Sm₂Ti₂O₇/Tm₂Ti₂O₇ cubic phase. A Williamson-Hall analysis was used to monitor the tensions of the NP's crystallites at the various doping concentrations and with addition of the silica shell. The luminescent spectra presented the characteristic emission peaks for the electronic energy levels transitions of the Sm³⁺/Tm³⁺ and Yb³⁺ ions. The Sm³⁺/Yb³⁺ co-doped NP's showed a maximum emission peak in the visible region at 612 nm, associated with ⁴G_5/2 → ⁶H_7/2 transitions of the Sm³⁺ ions. The IR emission peak at 973 nm (²F_5/2 → ²F_7/2) pertaining to Yb³⁺. For the combination of Tm³⁺/Yb³⁺, two emissions associated with Tm³⁺ ions were observed at 440 nm (¹D₂ → ³F₄) and 806 nm (³H₄ → ³H₆). The emission at 973 nm (²F_5/2 → ²F_7/2) is correlated to the Yb³⁺ ions. Silica coating of the NP's resulted in luminescence emission intensity increase of about 4 times.     

Structure and luminescence properties of Eu3+ doped TiO2 nanocrystals and prolate nanospheroids synthesized by the hydrothermal processing

We report on a new approach to the synthesis of Eu³⁺ doped TiO₂ nanocrystals and prolate nanospheroids. They were synthesized by shape transformation of hydrothermally treated titania nanotubes at different pH and in the presence of Eu³⁺ ions. The use of nanotubes as a precursor to the synthesis of Eu³⁺ doped TiO₂ nanocrystals and prolate nanospheroids opens the possibility of overcoming the problems related to molecular precursors. The shapes and sizes of the nanotubes, Eu³⁺ doped TiO₂ nanocrystals and prolate nanospheroids were characterized by transmission electron microscopy (TEM) technique. Crystal structures of the resultant powders were investigated by X-ray diffraction (XRD) analysis. The percentage ratio of Eu³⁺ to Ti⁴⁺ ions in doped nanocrystals was determined using inductively coupled plasma atomic emission spectroscopy. The optical characterization was done by using fluorescence and ultraviolet-visible reflection spectroscopies. An average size of faceted Eu³⁺ doped TiO₂ nanocrystals was 13 nm. The lateral dimensions of Eu³⁺ doped TiO₂ prolate nanospheroids varied from 14 to 20 nm, while the length varied from 40 to 80 nm, depending on precursor concentrations. The XRD patterns revealed the homogeneous anatase crystal phase of Eu³⁺ doped TiO₂ nanocrystals and prolate nanospheroids independently of the amount of dopant. A postsynthetic treatment (filtration or dialysis) was applied on the dispersions of the doped nanoparticles in order to study the influence of the dopant position on photoluminescence (PL) spectra. In the red spectral region, room temperature PL signals associated with ⁵D₀ → ⁷F_J (J = 1–4) transitions of Eu³⁺ were observed in all samples. The increased contribution of dopants from the interior region of dialyzed nanocrystals to photoluminescence was confirmed by the increase of R value.     

Effect of the carbonate environment on morphology and sintering behaviour of variously co-doped (Ca,Sr, Er,Pr) Samarium-doped Ceria in co-precipitation/hydrothermal synthesis

Variously co-doped Samaria-20?mol% doped ceria (SDC20) nanopowders were synthesized through a combined co-precipitation/hydrothermal treatment method under different carbonate environments. Urea and ammonium carbonate were used as both precipitating and mineralizing agent. In all cases, the adopted powder composition was Ce_0.8Sm_0.16 ×_0.04O_1.9-δ, where X was either Ca, Sr, Er or Pr and δ is 0 for trivalent cations (i.e. Er and Pr) or 0.02 for divalent cations (i.e. Ca and Sr). The effects of different synthesis parameters on powders morphology and crystalline phases have been pointed out. Differently synthesized powders underwent structural and morphological transformations during the hydrothermal treatment leading to different crystalline precursors for the desired co-doped ceria nanopowders, i.e. crystallized into the fluorite-like cubic structure after a calcination step at 700?°C for 1?h. The final properties of the calcined powders are strongly related to the corresponding parent powder features, consequently determining different sintering behaviours in the various pellets. In particular, except for Er/Sm co-doped ceria, all samples synthesized with ammonium carbonate as precipitating/mineralizing agent exhibited excellent sintering behaviour, with remarkable values of relative density (higher than 97% and up to 99.4%) and an almost ideal microstructure. Definitely, the present work gives several guidelines in terms of synthesis parameters and conditions to produce, with a relatively simple and cheap process, highly reactive co-doped ceria nanopowders with tuned properties and suitable as electrolytes for intermediate temperature solid oxide fuel cells (IT-SOFCs).