Optimal Calcination Research Articles

Effect of magnesium and zinc on phase formation of pyrochlore-type Bi2Mg(Zn)1-хMxTa2O9.5-Δ (M-Cr, Fe) ceramics

New pyrochlores (sp. gr. Fd-3m) of Bi2Mg(Zn)1-хMхTa2O9.5-Δ (M − Cr, Fe) composition were obtained for the first time by the method of solid-phase synthesis. The process of phase formation of pyrochlores in the temperature range 650–1050°С was studied. It has been established that the precursor of the pyrochlore phase in all cases is orthorhombic bismuth orthotantalate BiTaO4. The pyrochlore phase synthesis reaction proceeds predominantly at temperatures above 850–900°С. The influence of magnesium and zinc on the course of pyrochlore synthesis was revealed. For chromium pyrochlores, the formation of intermediate phases such as Bi6Cr2O15, Bi16CrO27 was established; for iron-containing pyrochlores, Bi25FeO40 was identified as an intermediate phase. For all systems, the change in the parameter of the pyrochlore cell constant depending on the synthesis temperature was analyzed. The samples are characterized by a porous dendritic microstructure. The calcination temperature did not significantly affect the microstructure of the samples. The porosity of the samples was estimated. The optimal calcination temperature for obtaining phase-clean pyrochlores can be considered 1050°С.

Preparation of nanoscale LaXO3 (X=Co, Mn, Ni) by rheological phase method for oxygen reduction reaction

The rheological phase method(RPM) is a simple and environmentally friendly synthesis method. In this work, nanoscale LaXO3 (X = Co, Mn, Ni) series catalysts have been synthesized by RPM and their oxygen reduction reaction (ORR) have been investigated. The optimal calcination temperature of the RPM is lower than that of the solid-phase method, and the catalytic activity of the catalyst is also higher than that of solid-phase method, mainly because the products prepared by RPM have a nanoscale porous structure and a small amount of residual carbon. By comparing the differences among LaCoO3, LaMnO3, and LaNiO3, the results show that the ORR activity of the catalyst is the strongest when the b-site element is Mn, and the calculated electron transfer number is 3.99, which is close to 4 electrons, indicating that the by-product generation is relatively small, and the kinetic current density reach 6.63 mA cm−2. Both were higher than of LaCoO3 and LaNiO3. This work is expected to provide a new green synthesis method for non-noble metal catalyst perovskite oxygen reduction catalyst of LaCoO3, LaMnO3, and LaNiO3.

Preparation and decarburization characteristics of SiO2-Al2O3 composite aerogel modified by potassium carbonate

In this paper, the preparation of potassium carbonate modified SiO2-Al2O3 composite aerogel, the carbonation characteristics of K2CO3 and the decarburization characteristics of regeneration cycle were studied. The influence of loading rate on CO2 adsorption was studied by using a fixed bed reactor, and the microstructure of the samples was analyzed by combining SEM and BET. The results show that during the alkali fusion sintering of Na2CO3, the Si-O-Si and Si-O-Al bonds break, the crystal structure is destroyed, and the covalent bond of mullite is transformed into the ionic bond of nepheline. Through orthogonal test, taking the specific surface area of aerogel as the measurement index, the optimal calcination conditions are determined as follows: 900 ℃, reaction for 60 min, Na2CO3 addition ratio of 0.5. The more K2CO3 is loaded, the less the corresponding active sites on the surface of the carrier. When the loading is 30%, the maximum CO2 adsorption capacity is 2.86 mmol·g–1. Excess K2CO3 will plug the pore structure, destroy the diffusion of CO2, and reduce the diffusion and utilization efficiency. The percentage of mesoporous pore volume decreased from 94.21% to 89.32%, indicating that the active component K2CO3 was mainly filled in the mesoporous. After 10 cycle regeneration tests, the CO2 adsorption capacity of the adsorbent decreased by 10.49%. The pore structure of the adsorbent was stable and the decarburization performance was excellent.

Balanced Crystallinity and Nanostructure for SnS2 Nanosheets through Optimized Calcination Temperature toward Enhanced Pseudocapacitive Na+ Storage.

Sodium ion batteries (SIBs) are expected to take the place of lithium ion batteries (LIBs) as next-generation electrochemical energy storage devices due to the cost advantages they offer. However, due to the larger ion radius, the reaction kinetics of Na+ in anode materials is sluggish. SnS2 is an attractive anode material for SIBs due to its large interlayer spacing and alloying reactions with high capacity. Calcination is usually employed to improve the crystallinity of SnS2, which could affect the Na+ reaction kinetics, especially the pseudocapacitive storage. However, excessively high temperature could damage the well-designed nanostructure of SnS2. In this work, we uniformly grow SnS2 nanosheets on a Zn-, N-, and S-doped carbon skeleton (SnS2@ZnNS). To explore the optimal calcination temperature, SnS2@ZnNS is calcined at three typical temperatures (300, 350, and 400 °C), and the electrochemical performance and Na+ storage kinetics are investigated specifically. The results show that the sample calcined at 350 °C exhibited the best rate capacity and cycle performance, and the reaction kinetics analysis shows that the same sample exhibited a stronger pseudocapacitive response than the other two samples. This improved Na+ storage capability can be attributed to the enhanced crystallinity and the intact nanostructure.

Nanostructured magnetite-ceria-based composite: Synthesis, calcination, properties, and applications

Magnetite and magnetite/ceria composites prepared by chemical procedures in various mutual ratios were exposed to calcination treatment in a temperature interval between 473 K and 1073 K. A combination of several experimental methods has provided detailed structural, phase, and magnetic properties utilisable for selection of optimal compositions and calcination conditions from the viewpoint of degradation ability tested using parathion methyl and paraoxon. It was shown that the ceria content, selected between 5 wt% and 50 wt%, influences magnetic properties. Its optimal amount was determined to be above 20 wt% and the calcination temperature of 773 K when the highest rate constant, slightly above 0.06 min−1, was obtained for parathion methyl in acetonitrile using a degradation test.

Improvement of sulfur and water resistance with Fe-modified S-MnCoCe/Ti/Si catalyst for low-temperature selective catalytic reduction of NO with NH3.

The low-temperature SCR of NOx by NH3 is restricted in application since the catalysts is easily poisoned by sulfur and water. The Fe modified Mn-Co-Ce/TiO2/SiO2 catalysts synthesized via impregnation method and sulfating were evaluated for low-temperature NH3-SCR in the presence of SO2 and H2O. The calcination temperature and loading amounts of Mn, Fe, Co and Ce were optimized. Adding of Fe into S-MnCoCe/Ti/Si played an important role in resistance to sulfur and water poisoning. The optimal calcination temperature was 380°C and the optical mass loading of the catalyst was 10% of Mn, 10% of Fe, 1% of Co and 4% of Ce. The optimal S-MnFeCoCe/Ti/Si catalyst maintained high NOx conversion of 93% at reaction temperature of 160°C in the presence of 50ppm SO2 and 10vol% H2O. The catalytic activity did not continue to fall after two times of repeated used in the temperature range of 100-200°C, indicating its excellent sulfur and water durability and stability in the presence of SO2 and H2O. The interaction between MnOx and FeOx enhanced sulfur and water durability rather than other bi-metal interactions. Furthermore, the mechanism of Fe improving resistance to SO2 and H2O was discussed.

Effect of the calcination temperature on SnO2-MoO3 crystal structure and catalytic activity in desulfurization of model diesel

Fuel’s sulfur content should be controlled to prolong catalytic converters and infrastructure life and improve air quality and human health. Catalytic sulphur oxidation is widely used for fuel refining. In this work, a novel SnO2-MoO3 catalyst was synthesized by the inverse sol–gel method for oxidative desulfurization of dibenzothiophene (DBT). The catalyst was characterized by thermogravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), N2 adsorption–desorption, and Fourier-transformed infrared spectroscopy (FTIR). Calcination temperatures 150–650 °C significantly affected the catalyst’s thermal stability, textural properties, and catalytic efficiency. The optimal calcination temperature of 450 °C resulted in a 99.6 % conversion of the DBT to dibenzothiophene sulfone. Kinetic investigations revealed a pseudo-first-order reaction with a 36 ± 4 kJmol−1 activation energy. The catalyst demonstrated excellent catalytic activity and reusability and thus has huge potential in industrial catalytic desulfurization. This catalyst promises improved air quality, public health, long catalytic converter life, and reduced infrastructure degradation.

Preparation and 3D printing building application of sulfoaluminate cementitious material using industrial solid waste

The iron and steel industry , the power industry, and the mining industry each produce large volumes of industrial solid waste. These industrial solid waste are dumped in huge volumes over a wide geographical distribution , causing far-reaching environmental harm in China. To date, the preparation of eco-friendly construction materials from industrial solid waste is one of the feasible large-scale utilization methods. This paper studied the preparation of different types of environmentally benign novel green sulfoaluminate cementitious materials with different contents of Ca 4 Al 6 SO 16 and Ca 2 SiO 4 by using stone tailing, coal gangue , secondary aluminum slag, and desulfurization gypsum . Moreover, the prepared solid-waste-based sulfoaluminate cementitious material (SCM) was used to further prepare 3D printing material. The results show that the optimal calcination conditions are 1260–1290 °C for about 1 h, and the main mineral phases in the clinker system are Ca 4 Al 6 SO 16 , Ca 2 SiO 4 , and Ca 4 Al 2 Fe 2 O 10 . The compressive strengths of hydrated specimens reached 40, 61, and 86 MPa after curing for 1d, 3d, 28 d, respectively, and the main mineral phases of the hydration product were ettringite , alumina gel, and silica gel . After improving its properties by using a suitable accelerant and retardant , the SCM showed advantages of a controlled setting time in the range of 15–80 min, rapid hardening, and rapid attainment of mechanical strength. The compressive strength of hydrated specimens reached 15–20 MPa after curing for 2 h, and the modified SCM proved to be eminently suitable for 3D printing applications. These results provided not only a sustainable mode for 3D printing construction materials and development, but also an innovative strategy for full utilization of industrial solid waste. • A new synthetic method to prepare eco-friendly 3D printing building materials is described. • The novel technological process of SCM from hazardous and industrial solid wastes was proposed. • Effect of raw mix composition and sintering temperature on properties of SCM was analyzed.

Performance of cement-based materials containing calcined coal gangue with different calcination regimes

The storage of coal gangue (CG) takes up a lot of lands and pollutes the environment. Calcined CG has the potential to be used as supplementary cementitious material. In this paper, the CG from Yibin, Sichuan province of China were treated with different calcined temperature, holding times and cooling modes, and the microtopography, phase composition and pozzolanic reactivity of calcined CG were studied. Meanwhile, the fluidity, mechanical properties, hydration products, and pore structure of cement paste and mortar with different calcined CG were analyzed. The apparent color of coal gangue under different treatment methods has also been studied to promote its better application for a wider range in cement-based materials. Results showed that there exists an optimal calcination condition of calcined CG at 800 °C and holding time of 2 h. Rapid cooling and slow cooling reduced the activity of calcined CG. Calcined CG powder would reduce the fluidity of cement mortar. However, proper calcination temperature and sufficient holding time could eliminate it to some extent. It was also found that calcination temperature has a greater impact on the early age reactivity of CG when compared to different temperature treated CG powder, C8T2 sample has the best early activity. Compared to rapid cooling, slow cooling and water-cooling mode, room temperature cooling would result in higher reactive CG. CG powder after proper thermal treatment could refine the pore structure of the hardened cement paste in the later age (28 days), reduce the harmful pores content (>100 nm), and increase harmless pores content (<100 nm) in hardened cement paste. It was found that the CG powder of calcined at 800 °C for 2 h, cooling in water and room temperature might be more suitable as the supplementary cementing material combined the apparent color, pozzolanic reactivity, and preparation process.

Asphaltene adsorption on MgO, CaO, SiO2, and Al2O3 nanoparticles synthesized via the Pechini-type Sol−Gel method

Basic, amphoteric, and acidic metal oxide nanoparticles including MgO, CaO, SiO2 and Al2O3 were synthesized via the Pechini-type sol–gel process and evaluated for adsorption of two types of asphaltenes (Ap1, Ap2) extracted from two different Iranian crude oils. The adsorbents were characterized by the N2 adsorption–desorption, XRD, FE-SEM, TEM, and EDS and the asphaltene samples were examined using FTIR analysis. The effects of citric acid to metal precursor molar ratio (M), calcination temperature, type of adsorbent, textural properties, adsorption temperature, and regeneration on the adsorbent performance were investigated. The SiO2 nanoparticle with the highest specific surface area and an amphoteric character was an excellent adsorbent capable of removing more than 70% of asphaltene from a model oil with initial asphaltene concentration of 3000 ppm. However, CaO exhibited the highest specific adsorption capacity, indicating that basic sites were active centers for asphaltene adsorption. It was demonstrated that with increasing the calcination temperature, the crystallite sizes of MgO and SiO2 increased and their BET surface areas decreased. The maximum asphaltene adsorption capacities of MgO and SiO2 nanoparticles were obtained at optimal calcination temperatures of 600 °C and 500 °C, respectively. Moreover, the optimum M value for the synthesis of MgO nanoparticle, in terms of asphaltene adsorption capacity, was M = 1, while it was M = 2 (for Ap1) and M = 1 (for Ap2) for SiO2. The adsorption isotherms were best fitted by the Jovanovic model. Moreover, kinetic data for the best adsorbents (MgO and SiO2) were in maximum agreement with the Elovich model. The adsorbents could be easily regenerated by calcination at 600 °C.

Effect of poly(N-vinylpyrrolidone) ligand on catalytic activities of Au nanoparticles supported on Nb2O5 for CO oxidation and furfural oxidation

The development of green preparation methods for acidic metal oxide supported gold catalysts is of great importance for the extensive use of gold catalysts as well as for a comprehensive understanding of gold catalysts. In this study, poly(N-vinylpyrrolidone) (PVP) was used as the stabilizer of gold colloids to deposit gold nanoparticles on an acidic metal oxide, Nb2O5. The effects of the PVP ligand on the preparation of Au(-PVP)/Nb2O5 and on the catalytic activities for gas-phase CO oxidation and liquid-phase furfural oxidation were investigated. As removing more ligand PVP of Au(-PVP)/Nb2O5, the catalytic activities for both CO oxidation and furfural oxidation increased. The optimal calcination temperature for Au(-PVP)/Nb2O5 was determined to be 400 °C, and calcination at that temperature gave gold nanoparticles with an average size of 6.4 ± 2.5 nm and of the support of Nb2O5 remained as the original crystalline structure. The temperature for 50% CO conversion (T50%) of Au(-PVP)/Nb2O5 (calcined at 400 °C) was 81 °C. In addition, Au(-PVP)/Nb2O5 (calcined at 400 °C) presented 43% furfural conversion with 100% selectivity of furoic acid under a mild conditions (0.5 MPa O2, 40 °C) in the batch system. These results suggested that Au(-PVP)/Nb2O5 is a good catalyst for both gas-phase and liquid-phase reactions.

Study of performances and microstructures of mortar with calcined low-grade clay

This paper studied the effect of calcination temperatures (600–900 °C) on physical characteristics and microstructure changes of low-grade clay containing 14.6% kaolinite and 17.8% 2:1 clay mineral. The pozzolanic activity of calcined low-grade clay as a supplementary cementitious material was evaluated using strength activity index and relative strength index. The results show that the kaolinite transformed from crystalline phase to amorphous metakaolin phase at 600 °C, while the particle size of clay first increases and then decreases. The optimal calcination temperature is found between 700 and 800 °C, whereas the optimal cement replacement level is 10–20 wt%.

Fabrication of B4C ultrafiltration membranes on SiC supports

The fabrication of B4C ultrafiltration membranes is described. Firstly, a semi-dilute B4C slurry was environmentally-friendly prepared by aqueous colloidal processing, optimizing its dispersion by sonication, and used to deposit B4C membranes onto SiC macro-porous supports by dip-coating. Secondly, the resulting green membranes were characterised microstructurally by scanning electron microscopy (SEM), and pressureless sintered within the intermediate sintering regime. Thirdly, the sintered membranes were calcined in air to clean them from possible free carbon in the smallest pores, with the optimal calcination conditions having been identified by thermogravimetry coupled with mass spectrometry. Next, the calcined, sintered membranes were characterised microstructurally by SEM, tested mechanically against scratching, and characterised texturally by capillary flow porometry, thus identifying the optimal among them. Lastly, as a complement to the fabrication study, the filtration permeability of the optimal membrane was evaluated using deionized water. This work thus paves the way towards the fabrication of ceramic membranes based on B4C, lighter and potentially more durable than others, for filtration applications.

MgO Catalysts for FAME Synthesis Prepared Using PEG Surfactant during Precipitation and Calcination

To develop a method for the preparation of MgO nanoparticles, precatalyst synthesis from magnesium nitrate with ammonia and calcination was performed in presence of PEG in air. Without PEG, the catalysts are inactive. The conversion to hydroxide was performed using a PEG/MgO molar ratio of 1, but, before the calcination, excess of PEG was either saved (PEG1) or increased to 2, 3, or 4 (PEG 2–4). Catalysts were calcined at 400–660 °C and characterized using XRD, N2 adsorption-desorption, TGA, FTIR, and SEM. The FAME yield in the reactions with methanol depend on the PEG ratio used and the calcination temperature. The optimal calcination temperature and highest FAME yield in the 6 h reactions for catalysts PEG1, PEG2, PEG3 and PEG4 were 400 °C, 74%; 500 °C, 80%; 500 °C, 51% and 550 °C, 31%, respectively. The yield dependence on calcination temperature for catalysts with a constant PEG ratio is similar to that of a bell curve, which becomes wider and flatters with an increase in PEG ratio. For most catalysts, the FAME yield increases as the size of the crystallites decreases. The dependence of FAME and the intermediate yield on oil conversion confirms that all catalysts have strong base sites.

Analysis of the Granulometric Composition of the Feedstock Influence on Mechanical Properties of Iron Ore Pellets

The paper investigates the effect of high-temperature roasting and cooling modes of roasted iron ore pellets on their strength and porosity. These characteristics depend on the initial iron ore raw materials properties, the parameters of the raw pellets, the firing temperature, the holding time at this temperature, the heating and cooling rate, and take into account the change in these indicators in connection with the chemical and mineralogical compositions of the pellets. It has been established that the strength of iron ore pellets obtained at the optimum firing temperature depends on the characteristics of the initial finely dispersed iron ore raw material. The relationship between the content of draw rock and the strength of calcined pellets has been revealed. A significant influence of the raw pellets porosity on the strength of the calcined pellets was found. It is shown that the crushing strength of pellets cooled in air is higher than the strength of pellets cooled with water, and a decrease in the final cooling temperature leads to an increase in the strength of the pellets. It is substantiated that the heating rate should not exceed the rate of gas diffusion, and with a decrease in the size of finely dispersed iron ore raw materials, the shrinkage of the pellet layer increases during heating. It is shown that shrinkage appears at temperatures lower than the optimal calcining temperature and insignificantly affects the strength of the pellets. The results obtained can be used to substantiate resource-and-energy efficient operating modes of horizontal-grate machines in ferrous metallurgy.

Influence of sintering temperature on the electrochemical properties of P2-type Na0.67Mn0.7Ni0.2Mg0.1O2 cathodes for sodium-ion batteries

Sodium-ion batteries are thought to be ideal alternatives to Lithium-ion batteries due to their similar electrochemical properties. However, several technique obstacles in cathode materials still impede the commercialized adoption of Sodium-ion batteries. Herein, the Mg-doping P2-type Na0.67Mn0.7Ni0.2Mg0.1O2 cathode materials were synthesized via a two-step process, including sol-gels and solid-state reaction method. This paper pays much attention to the optimal calcination temperature in the synthesis procedure and its effects are subsequently investigated. According to the results, under a series of calcination temperatures from 800 to 950 ​°C, Na0.67Mn0.7Ni0.2Mg0.1O2 cathode materials shows different particle sizes and crystalline structures, exhibiting varied electrochemical properties. Among them, samples calcinated at 900 ​°C display a high specific discharge capacity of 120.9 ​mAh g−1, and a stable cycling performance of 67.2% retention at 1 C rate for 100 cycles. The results suggest that calcination temperature at approximately 900 ​°C could effectively promote the electrochemical performance, which provides a good reference for the synthesis of cathode materials in sodium-ion batteries.

Catalyst Development for HCl Oxidation to Cl2 in the Fluorochemical Industry

The catalytic oxidation of gaseous HCl (containing a small amount of HF) to Cl2 is important and highly desired for chlorine recycling in the fluorochemical industry. In the present work, a series of Al-doped MgF2 (Al–MgF2) materials were synthesized via a sol–gel method, followed by calcination at different temperatures and then these synthesized Al–MgF2 materials were used as supports to prepare RuO2/Al–MgF2 catalysts by an incipient impregnation method. These developed catalysts were evaluated in the oxidation of HCl with an upper-bound HF concentration of 400 ppm, as is common in the fluorochemical industry. Specific attention was paid to investigating the effects of calcination temperature for preparing Al–MgF2 supports on the activity and stability of the resultant catalysts. It is found that at an optimal calcination temperature, Al can be incorporated into the framework of rutile structure MgF2, which can further modify the cell parameters of MgF2 close to those of RuO2, modulate the interactions between RuO2 and the support, and yet affect the chemical environment of RuO2 to enhance the catalytic activity and stability. The study on the catalytic kinetics reveals that the estimated apparent activation energy is in line with the incorporated amount of Al into the framework of MgF2 and shows an inverted volcano relationship with the calcination temperature for preparing Al–MgF2 supports. The lowest apparent activation energy of RuO2/Al–MgF2 can be achieved when the Al–MgF2 composite is calcined at 400 °C, and the resultant catalyst shows long-term stability with high activity for the oxidation of HCl containing a small amount of HF.

Pozzolanic reactivity of aluminum-rich sewage sludge ash: Influence of calcination process and effect of calcination products on cement hydration

The application of aluminum-based flocculant in wastewater treatment results in a large amount of aluminum-rich sewage sludge. This work investigated the influence of calcination process on physicochemical characteristics and pozzolanic activity of aluminum (Al)-rich sludge ash and studied the effect of sludge ash on cement hydration. The results showed that higher calcination temperature from 600 ℃ to 900 ℃ increased the amorphous content in sludge ash. The pozzolanic activity of sludge ash calcined at 800 ℃ and 900 ℃ was confirmed by Frattini test. In view of strength activity index of blended mortar and energy conservation, the optimal calcination condition of sewage sludge ash was calcined at 800 ℃ with air-cooling. The addition of sludge ash promoted the transformation of ettringite to monosulfate phase in cement paste. However, the high Al concentration dissolved from S6 and S7 ash inhibited significantly the cement hydration and resulted in low compressive strength values of the blended mortars. The pozzolanic reaction of S8 and S9 ash produced more hydration heat and additional Al-bearing products such as katoite and monosulfate which contributed to the strength development of mortars. Furthermore, the heavy metals in sewage sludge can be immobilized in ash structure during calcination process and the structure of hydration products, which ensures the environmental security of sludge ash utilization in construction materials.

Effect of calcination temperature and Ti substitution on optical properties of (Fe,Cr)2O3 cool black pigment prepared by spray pyrolysis.

Near-infrared (NIR) reflective Fe1.5Cr0.5O3 black pigments were synthesized by spray pyrolysis, and the effect of calcination temperature and Ti substitution on the optical properties were investigated. As the calcination temperature increased from 500 °C to 800 °C, the prepared Fe1.5Cr0.5O3 powder had α-Fe2O3 phase without any impurities and the NIR reflectance steadily increased. On the otherhand, the smallest chroma value was observed at 700 °C. Therefore, in terms of achieving high NIR reflectance with keeping good blackness, the optimal calcination temperature was determined to be 700 °C. Substitution of Ti corresponding to 5–15% of the total metal ions in Fe1.5Cr0.5O3 largely affected the NIR reflectance and chroma value, but there was no significant change in the optical band gap. Ti substitution of 5 mol% could further improve the NIR reflectance of the Fe1.5Cr0.5 black pigment without significant loss of blackness, but above 10% or higher the NIR reflectance largely decreased due to the loss of crystallinity. Resultantly, Fe1.4Cr0.5Ti0.1O3+δ (5% Ti substituted black pigment) was confirmed to have improved heat-shielding performance compared to Fe1.5Cr0.5O3 in a temperature rise test under near-infrared illumination.

Synthesis and luminescent properties of novel Li1.0Nb0.6Ti0.5O3: Dy3+ phosphors for white light-emitting diodes

Novel Li1.0Nb0.6Ti0.5O3: xDy3+ white-emitting phosphors were synthesized by two methods, the solid-state reaction method and the sol-gel method. The effects of the preparation method, processing temperature and rare earth ion concentration on the luminescence properties of the samples were studied systematically in this paper. The phosphors prepared by two methods have the same orthorhombic “M-phase” solid solution structures and the particle sizes are in the scope of 1.5–2.5 μm. Under an excitation of 390 nm, the photoluminescence peaks of all samples were concentrated at 484 nm and 582 nm, related to the 4F9/2 → 6H15/2 and 4F9/2 → 6H13/2 electron transitions of Dy3+ ions. With the doping concentration of Dy3+ increasing, the luminescence intensities of Li1.0Nb0.6Ti0.5O3: xDy3+ phosphors reach its relative maximum at x = 2 wt%. Moreover, the optimal calcination temperature of the samples prepared by the sol-gel method is about 850 °C, which is 200 °C lower than that of solid-state reaction method. The color coordinates of the phosphors prepared by two methods were confined to white light region, closed to the standard white coordinates. These results lay solid foundation for the promising application of Li1.0Nb0.6Ti0.5O3: Dy3+ as phosphors in white light-emitting diodes.