An innovative two-step route was successfully applied to the ionic liquid-assisted synthesis of C@ZrSiO4 ceramic pigments, which is able to reduce the reflux time from many hours to a few minutes. The structure and morphology of the inclusion pigments were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). And the chromatic value of the pigments was measured by the CIE color system. The results show that the pigment in the absence of ionic liquid (IL) exhibited homogeneous single t-ZrO2 phase, while the samples in the presence of IL showed coexistence of two crystal phases (m-ZrO2 and ZrSiO4). The CIE coordination L* value decreased with the increase of TEOS amounts due to the pure zircon formation. The as-prepared pigment showed high tinting ability, as L*=37.16, a*=0.71, b*=0.3, making it promising candidate for ceramic decoration.
Encapsulated carbon black pigment was prepared by layer-by-layer self-assembly method. The RX8002 carbon black particles were well coated by a SiO2 layer, which makes it has good connection with ZrSiO4 layer. Meanwhile, dense ZrSiO4 layer was coated on the C@SiO2 particles surface to prevent the corrosive effects of glaze. The structure and morphology of samples were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The chromatic value of the pigments was measured by the CIE color system. The results show that the carbon black particles can be well coated by SiO2 and ZrSiO4 layer. When the TEOS/H2O ratio is 0.002 and the ZrSiO4/C ratio is 0.71, the chromatic value of the encapsulated carbon black pigment is 42.55, and the pigment has a good stability in glaze.
C@ZrSiO4 inclusion pigment was prepared by using commercial carbon black RX8002C and phenolic resin (PF) as compound carbon source via non-hydrolytic sol-gel (NHSG) process. The RX8002C carbon could well disperse in phenolic resin solution, which developed a compound carbon source after calcination. Dense ZrSiO4 layer was coated on the carbon surface as a protector. The structure and morphology of samples were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The chromatic value of the pigments was measured by the CIE color system. The results show that the compound colorants can be well coated by ZrSiO4 dense layer to develop a black inclusion pigment. When the compound proportion is 1:4 and the compound colorants amount is 4wt.%, the chromatic value of the C@ZrSiO4 inclusion pigment is 27.54.
Corundum structurealumina (α-Al2O3) powders were prepared via a non-hydrolytic sol-gel (NHSG) method using aluminum as raw material, ethanol as solvent, and iodine as catalyst. X-ray diffraction (XRD), differential thermal analysis (DTA), thermo gravimetric analysis (TG) were used to characterize the crystal phase of the products, while scanning electron microscopy (SEM) and transmission electron microscope (TEM) were employed to analyze the morphology. The results indicated that γ-Al2O3 was completely changed to α-Al2O3 at 1100 o C with a bit of aggregation. When 3 wt.% polyethylene glycol 600 (PEG 600) was introduced on the NHSG process, the dispersion was improved and the particle size decreased to100 nm.
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