A zirconium silicate-encapsulated low-valent ion composite doped gamma-ce2s3 red pigment and its preparation method
A technology of compound doping, red pigment, applied in the field of inorganic pigments, can solve the problems of no longer showing bright red, insufficient thickness of the coating layer, unstable crystal structure, etc., achieve uniform particle size, and help popularization and application , the effect of easily controllable factors
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Embodiment 1
[0032] In this example, zirconium silicate-encapsulated low-valent ions are compositely doped with γ-Ce 2 S 3 The preparation method of red pigment, its step is as follows:
[0033] (1) Preparation of cerium oxysulfide precursor suspension containing doped ionic elements by solvothermal method
[0034] 3.5g CeCl 3 ·7H 2 O, 0.13g Eu 2 (SO 4 ) 3 ·H 2 O, 0.06g SnCl 2 2H 2 O and 0.4g of thiourea were dissolved in 70ml of ethylenediamine in turn, stirred vigorously for 120min, then transferred to a stainless steel reactor lined with polytetrafluoroethylene, and reacted at 200°C for 12h to obtain Eu, Sn containing doping elements The cerium oxysulfide precursor suspension;
[0035] (2) Preparation of precursor mixture powder
[0036] Add 4.0g tetraethyl orthosilicate to the above suspension, adjust the pH value of the system to 11.0 with ammonia water, then slowly add 30ml of zirconium butoxide ethylenediamine solution (dissolved concentration is 0.8mol / L) to make tetraet...
Embodiment 2
[0042] In this example, zirconium silicate-encapsulated low-valent ions are compositely doped with γ-Ce 2 S 3 The preparation method of red pigment, its step is as follows:
[0043] (1) Preparation of cerium oxysulfide precursor suspension containing doped ionic elements by solvothermal method
[0044] 3.91g Ce(NO 3 ) 3 ·6H 2 O, 0.175g Eu 2 (SO 4 ) 3 ·H 2 O, 0.21g SmCl 3 ·6H 2 O and 0.35g of thiourea were dissolved in 70ml of ethylenediamine in turn, stirred vigorously for 100min, then transferred to a stainless steel reactor lined with polytetrafluoroethylene, and reacted at 250°C for 15h to obtain Eu, Sm containing doping elements The cerium oxysulfide precursor suspension;
[0045] (2) Preparation of precursor mixture powder
[0046] Add 3.5g tetraethyl orthosilicate to the above suspension, adjust the pH value of the system to 10.5 with ammonia water, then slowly add 25ml of zirconium butoxide ethylenediamine solution (dissolved concentration is 0.8mol / L) to ma...
Embodiment 3
[0051] In this example, zirconium silicate-encapsulated low-valent ions are compositely doped with γ-Ce 2 S 3 The preparation method of red pigment differs from embodiment one in that:
[0052] The sulfur source in the present embodiment step (1) is tetraethylthiuram disulfide (C 10 h 20 N 2 S 4 ), consumption is 1.5g; In the step (2), silicon source is the sodium silicate ethylenediamine solution (dissolution concentration is 2.0mol / L) that 1.5g sodium silicate is dissolved in the ethylenediamine that makes; Step (3) The middle additive is calcium carbonate, and the consumption amount of the sintering aid diboron trioxide is 2.5wt% of the precursor powder.
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