Utilizationof dta for two-step synthesisof Cu–Mn–Cr spinel

The novel two-step synthesis method decreasing the calcining temperature necessary for formation of spinel lattice and as well for reaching of bright and clear hue of the pigments prepared were investigated. This work aims to utilization of DTA for synthesis monitoring. Influence of raw materials and temperature of calcination on color properties were observed. The characterization of the samples was performed by X-ray diffraction and colorimetry in the CIE L*a*b* system. It was proved that the black spinel pigment Cu_2.3Mn_2.8Cr_4.9O_x can be prepared at finally temperature 700°C as one-phase system with high quality black hue.     

Synthesis and description of SrSn0.6Ln0.4O3 perovskite pigments

Inorganic pigments containing lanthanides based on pseudo cubic structure of SrSnO₃ have been prepared by solid state reaction between SrCO₃, SnO₂ and lanthanide oxides (Tb₄O₇, Pr₆O₁₁, CeO₂) in the temperature range 1300–1550°C. The resultant materials were characterised by XRD, TG-DTA and colourimetric techniques were used. The most interesting colour properties were provided by SrTb_0.4Sn_0.6O₃ prepared by firing at temperature 1500°C which has light yellow-green colour hue. The increase of temperature 1300–1500°C caused the creation of pigments with deeper and brighter colour hue. Colour properties of the samples prepared by calcination at 1550°C were of inferior quality due to structural changes from pseudo cubic to orthorhombic system.     

Transient thermal response of phase change material embedded with graphene nanoplatelets in an energy storage unit

This research was focused on the preparation of mixed metal oxide pigments doped with terbium ions with the general formula of Sn_0.752Co_0.08P_0.16Tb_0.008O₂. These pigments were synthesised by solid-state reactions at high calcination temperatures. The temperature range was chosen from 1350 to 1500 °C. The goal was to develop conditions for the synthesis of this type of pigments and to determine the influence of terbium ions on the colour properties of these compounds. All prepared pigments were applied into the organic matrix and into the ceramic glaze. Thermal behaviours of the reaction mixtures were investigated using differential thermal and thermogravimetric analysis. Synthesised Sn_0.752Co_0.08P_0.16Tb_0.008O₂ pigments were compared with concurrently prepared pigment Sn_0.760Co_0.08P_0.16O₂ depending on the calcination temperature with respect to the colour properties in CIE L*a*b* colour space, furthermore from the point of particle size distribution and phase composition. All compounds provided blue–violet hues that are stable in ceramic glazes.     

Study of perovskite compounds

Perovskites belong to the great group of the inorganic pigments and thanks to their excellent properties they have been widely used in an industry. CaTiO₃, BaTiO₃ and SrTiO₃ with the perovskite structure were prepared in this work. These compounds were synthesized with using the solid state reaction by calcination in temperature region 1000–1200°C. The thermal analysis was used for characterization of thermal behaviour and formation of tested perovskites. The main aim of this work was studied the influence of calcination temperature on colour properties of perovskites. Colour properties of powdered compounds and samples applied into ceramic transparent glaze P 07491 were also studied. The tested compounds can be described by different light colour hues and that depending on calcining temperature. The structures of the powdered compounds were studied by X-ray diffraction analysis.     

Synthesis of ZrO2-based ceramic pigments

The pigments used in ceramic applications are of nature predominantly inorganic and they should be thermally stable, insoluble in glazing, resistant to the chemical and physical agents' attacks. This work aimed at the synthesis by the polymeric precursor method of ZrO₂-based inorganic pigments, doped with Fe, Ni, Co, Cr and Cu cations. The fired pigments were characterized by thermogravimetry (TG), differential thermal analysis (DTA) and X-ray diffraction (XRD). Among the metals used to zirconium-doping, the best result was achieved with the cations Cu, which presented the monophase pigment, even as 20 mol% of dopant. Up to the temperature of 1000°C the pigments presented a good thermal stability. This revised version was published online in August 2006 with corrections to the Cover Date.     

Study of thermal behaviour and stability of Co-doped malayaite ceramic pigments

This contribution deals with the preparation and characterization of Co-doped malayaite pigments. Pigment samples were prepared by solid-state reaction at different firing temperatures (1200–1400 °C). For characterization of thermal behaviour, pigment formation and thermal stability were studied by the methods of thermal analyses. The compounds were evaluated from standpoint of their phase composition and particle size distribution. The XRD analysis of samples prepared at 1,300–1,400 °C indicates the occurrence of two-phase compounds, i.e. the malayaite and the cassiterite. Average value of mean particle size of tested malayaites is moved ~10 μm. The great attention was focused on determination of impact of firing temperature on the pigment-application properties. Because the malayaite compounds belong into ceramic pigments, the pigment-application properties were observed after application into organic matrix in mass tone and middle-temperature glaze in different pigment amounts. Generally, the colour appearance of tested malayaites is dependent on the firing temperature and it moves in different shades of blue colour. From pigmentary point of view, it is possible to recommend 15 % of mass pigment for sufficient colouring of middle-temperature glaze. The higher firing temperature provides the formation of pigment samples with the higher saturation and the higher values of hue angle. For preparation of Co-doped malayaite pigments with the excellent colour properties, the firing temperature 1,350 °C is necessary.     

Preparation and selected properties of pigments on base of Ln-doped CaSnO<Subscript>3</Subscript>

Inorganic pigments containing lanthanides based on orthorhombic perovskite structure of CaSnO₃ have been prepared by solid state reaction of CaCO₃, SnO₂ and lanthanide oxides (Tb₄O₇, Pr₆O₁₁, CeO₂). The TG-DTA analysis indicates the formation of Ca-stannates around of temperature 1200°C, but from the pigmentary — application point of view, it is better to synthesize the product at higher temperature (1400 or 1500°C). The resultant materials were characterised by XRD, particle size distribution and measurement of colour properties. The doping of Ca-stannates by ions of rare earth elements (Tb, Pr, Ce) brings the production of two-and three-phase systems. The most interesting colour properties provided the stannate doped by ions of terbium and cerium and synthesized by heating at temperature 1400°C. The pigment has reddish brown colour hue.     

Thermal analysis of the Bi2O3-Y2O3-ZrO2 pigments

The synthesis of new compounds based on Bi₂O₃ is investigated because they can be used as new colour inorganic pigments. Chemical compounds of the Bi_2-xY_x/2Zr_3x/₈O₃ type were synthetised. The host lattice of these pigments is Bi₂O₃ that is doped by Y³⁺ and Zr⁴⁺ ions. The incorporation of doped ions provides interesting colours and contributes to a growth of the thermal stability of these compounds. The simultaneous TG-DTA measurements were used for determination of the temperature region of the pigment formation and thermal stability of pigments. This paper also contains the results of the pigment characterization by X-ray powder diffraction and their colour properties.     

Yellow pigments based on Fe2TiO5 and TiO2

The aim of our research was to prepare yellow pigments based on structure of pseudobrookite Fe₂TiO₅. Part of Fe was substituted with Li and Ti from Fe₂TiO₅ to Li_0.05Fe_0.07Ti_2.44O₅. Synthesis and pigmentary-application properties in the Li₂O–Fe₂O₃–TiO₂ system were studied for 800 and 900°C using classical ceramic method of preparation. The main attention was aimed to usage of four different sources of titanium compounds as raw materials. We studied the influence of different sources of titanium compounds on the structural and the colour properties of the prepared pigments. The thermal analysis was used for characterization of titanium compounds and determination of their thermal stability.     

Thermal study of the Ce<Subscript>0.9</Subscript>Tb<Subscript>0.1</Subscript>O<Subscript>2</Subscript> pigment prepared by different synthesis

The inorganic ceramic compounds based on the CeO₂ belong into the group of high-temperature pigments. The pigments have been prepared by the classical dry process (i.e. solid-state reaction) in the temperature range from 1,300 to 1,600 °C and by the coprecipitation at the three different temperatures: 400, 600 and 1,100 °C. The principal of these pigments makes the host lattice of the CeO₂, which is doped by terbium ions. This incorporation of the doped ions leads to obtaining of the interesting dark orange colour after application into ceramic glaze. The aim of our research was to improve and optimize the synthesis conditions of these pigments. The samples were submitted to thermal analysis (TG–DTA) for determination of the temperature interval of the pigment formation and the thermal stability of pigments. The compounds were also measured from the point of view of their colouring, structure and particle size distribution.     

Thermal analysis of pigments based on Bi2O3

The synthesis of new pigments based on Bi₂O₃ is investigated because they give interesting orange hues and can substitute the pigments problematic from the environmental point of view. Chemical compounds of the Bi_2–xZr_3x/4O₃ type were synthesized. The host lattice of these pigments is Bi₂O₃ that is doped by Zr⁴⁺ ions. The area of ZrO₂ solubility in Bi₂O₃ at 800°C forming solid solution of both oxides was studied. The incorporation of doped ions provides interesting colours and contributes to a growth of the thermal stability of these compounds. The simultaneous TG-DTA measurements were used for determination of the temperature region of the pigment formation and thermal stability of pigments.     

Study of ceramic pigments based on cobalt doped Y2O3–Al2O3 system

Ceramic pigments based on Y₂O₃–Al₂O₃ system doped by cobalt as a colourant agent were synthesized by solid-state reaction at temperatures up to 1,400 °C. The reactivity of initial mixtures of components was improved by the mineralizer LiF and the mechanical activation in a planetary ball mill. The temperature region of the product formation was followed by the method of thermal analysis. The effect of the synthetic method on the phase composition of the products was studied by X-ray diffraction analysis. Studied pigment-application properties of the product include the measurement of optical properties in the visible region of light and particle size distribution. The simple solid-state reaction led to the formation of turquoise samples that contain mainly blue CoAl₂O₄ spinel and next to it also YAlO₃ perovskite and Y₃Al₅O₁₂ garnet phases. The mineralizer LiF promotes the formation of yttrium aluminium double oxides of sandy-yellow to grey–brown colour hue, although the samples also contain small amount of blue CoAl spinel phase. Intensive milling process did not results in CoAl spinel phase and the samples contain yttrium aluminium perovskite and cobalt oxide. Evaluation of Kubelka–Munk absorption as a function of the pigment concentration was found that hiding is complete by adding of 5 mass% of pigment to the ceramic glaze. Resulting colour hue of all pigment applications into ceramic glaze is blue. The size of particles lies in the range of 7–26 μm.     

Thermal analysis of the (Bi<Subscript>2</Subscript>O<Subscript>3</Subscript>)<Subscript>1−x</Subscript>(Y<Subscript>2</Subscript>O<Subscript>3</Subscript>)<Subscript>x</Subscript> pigments

The synthesis of new compounds based on Bi₂O₃ is investigated because they can be used as new ecological inorganic pigments. Chemical compounds of the (Bi₂O₃)_1−x(Y₂O₃)_x type were synthesized. The host lattice of these pigments is Bi₂O₃ that is doped by Y³⁺ ions. The incorporation of doped ions provides the interesting colours and contributes to a growth of the thermal stability of these compounds. The simultaneous TG-DTA measurements were used for determination of the temperature region of the pigment formation and thermal stability of pigments. This paper also contains the results of the pigment characterization by X-ray powder diffraction and their colour properties.     

Thermal analysis of the Bi2O3-Er2O3-Zro2 pigments

The synthesis of new compounds based on Bi₂O₃ is investigated because they can be used as new ecological inorganic pigments. Chemical compounds of the Bi_2−xEr_x/2Zr_3x/8O₃ type were synthetized. The host lattice of these pigments is Bi₂O₃ that is doped by Er³⁺ and Zr⁴⁺ ions. The incorporation of doped ions provides interesting colours and contributes to a growth of the thermal stability of these compounds. The simultaneous TG-DTA measurements were used for determination of the temperature region of the pigment formation and thermal stability of pigments. This paper also contains the results of the pigment characterization by X-ray powder diffraction and their colour properties.     

Characterization of metal oxide-doped lutetium orthoferrite powders from the pigmentary point of view

This thesis deals with the preparation and characterization of inorganic pigments based on perovskite structure of metal oxide-doped LuFeO₃. Powder samples were prepared by the conventional ceramic method, i.e., solid-state reaction. Heating temperature was chosen according to results of TG/DTA. Prepared pigments were incorporated into an organic binder system, and their color properties were evaluated by measuring the reflectance in the visible region of light. The most interesting color properties were obtained by preparation of sample Lu_0.98Ca_0.02FeO_3?δ with mineralizer LiF at the temperature 900 °C. Mean size of its particles is 4 μm. X-ray diffraction analysis confirmed a single-phase orthorhombic structure with lattice parameters a = 0.521310 nm, b = 0.55535 nm, and c = 0.75626 nm. Thermal stability of the sample is limited by the temperature of 1,150 °C. Further, the effectiveness of other metal oxide (CoO-, ZnO-, Bi₂O₃-, and Sb₂O₃)-doped Lu_0.98Ca_0.02FeO_3?δ system was evaluated with respect to their phase composition, thermal stability, particle size distribution, and color properties. The conclusions of the research showed that a sample containing antimony oxide is the mixture with the best pigmentary-application properties. The powder has a clear orange color, high thermal stability up to 1,340 °C, and mean particle size 4 μm.     

Synthesis of nickel-iron spinel by non-conventional methods

Nickel-iron black ceramic pigments of (Fe_0.8Mg_0.2)(Fe_0.2Ni_0.8Cr)O₄ and (Fe_0.8Mg_0.1Zn_0.1)(Fe_0.2Ni_0.8Cr)O₄ compositions have been prepared by non conventional methods such as coprecipitation, microemulsion and polymeric gel routes (alkoxides hydrolysis-condensation), and compared with ceramic samples prepared by the solid state reaction from oxide precursors. The mineralising effect of a 2NaCl:NaF flux agent has been also analysed. Both non conventional methods and mineraliser presence increase the reactivity of the samples. The highest reactivity and the best black colour are obtained in the polymeric gel sample prepared from alkoxides; coprecipitated and microemulsion fired pigments are partially solubilised by glazes due to the small particle size exhibited, leading to brown colours.     

Synthesis and colour properties of pigments based on terbium-dopped Mg<Subscript>2</Subscript>SnO<Subscript>4</Subscript>

The main aim of this work was to synthesize the magnesium orthostannate doped by terbium cations and tested whether these materials can be used for colouring of the different materials, e.g. organic binder and ceramic glazes. Initial composition of pigments was counted according the general formula 2MgO(1 − x)SnO₂–xTbO₂, where values of x varied from 0.1 to 0.5 in 0.1 steps. The simultaneous TG/DTA measurements of mixture containing tin oxide, magnesium carbonate hydroxide and terbium oxide showed that the formation of a new compound started at temperature 1,029 °C, but single-phase system was not prepared. Granulometric compositions of samples that were prepared by calcining at temperatures 1,300–1,400 °C are characterized by values of median (d ₅₀) in range 4–8 μm. The calcining temperature 1,500 °C caused the increase of the particle sizes at around 12 μm. The composition of sample 2MgO–1.5SnO₂–0.5TbO₂ and heating temperature 1,500 °C are the most suitable conditions for preparation of colourfully interesting pigment that can be recommended also for colouring of ceramic glazes. Especially, for colouring of decorative lead containing glaze G 07091 containing 5 wt% of PbO and 8 wt% of Al₂O₃.     

Synthesis and characterization of LnFeO<Subscript>3</Subscript> pigments

This work is focused on determination of the optimum firing temperature which leads to formation of the compounds LnFeO₃ with good pigment-application properties (Ln=Gd, La, Yb, Tm, Lu). Based on results of thermal analysis the compounds were prepared by the solid-state reaction at temperature 900 and 1000°C. Colours of pigments vary depending on type of used lanthanoid (from light sienna to dark brown) and also on the type of precursor. Generally, the compounds prepared from iron oxide have more interesting color properties. Colour of these compounds is brighter and deeper. Increasing of the calcination temperature from 900 to 1000°C causes the darkening of colour. The most problably, the darkening is connected with partial reduction of Fe³⁺ to Fe²⁺.     

Study of Sb‐doped SnO2 Gray Ceramic Pigment with Cassiterite Structure

In this study, Sb_xSn_1?xO₂ (0 ≤ x ≤ 0.5) compositions were synthesized by the ceramic method from Sb₂O₃‐SnO₂ and Sb₂O₅‐SnO₂ mixtures and characterized by Differential thermal analysis (DTA) and thermogravimetric analysis (TG), X‐ray diffraction, UV‐V‐NIR spectroscopy and CIE L*a*b* (Commission Internationale de l'Eclairage L*a*b*) parameters measurements. Solid solutions with cassiterite structure were obtained at 1300 °C. These solid solutions are stable into glazes. From Sb₂O₃, light gray coloured materials were obtained. From Sb₂O₅, bluish gray coloured materials were obtained at 1300 °C/6h when x ≥ 0.3. Sb_xSn_1?xO₂ with 0.3 ≤ x < 0.5, T = 1300 °C and Sb₂O₅ might be established as compositional range, fired temperature and antimony precursor to obtain gray ceramic pigments in this system.     

Study of ceramic pigments based on Er2Ce2?x Mo x O7

This contribution is focused on the synthesis, characterization and optical properties of new inorganic pigments which are environment friendly and can substitute some toxic metals in interesting colour compounds. Pyrochlores belong to the group of high-temperature pigments, and are a variety of actual and potential applications for several materials. Examples include catalysts, thermal barrier coatings, solid electrolytes, nuclear waste forms and host materials for luminescence centers. The pigments were prepared by the solid state reaction and also by method of suspension mixing of materials in the series with increasing content of molybdenum. The pigments were applied into organic matrix and ceramic glaze. The colour properties of these applications were investigated depending on content of Mo, method of preparation and temperature of calcination (1350?C1550?°C after step 50?°C). The optimum conditions for their synthesis were determined. The pigments were evaluated from standpoint of their structure, colour and particle sizes. Characterization of Er₂Ce_2?x Mo _x O₇ pigments (x?=?0.1, 0.3, 0.5 and 0.7) suggests that they have a potential to be alternative yellow or orange colourants for paints, plastics, ceramics and building materials.