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A nano-scale low-valent ion complex doping type γ~ce 2 the s 3 Red pigment and preparation method thereof

A technology of compound doping and red pigment, applied in the field of inorganic pigments, can solve the problems of unstable crystal structure, no longer showing bright red, changes in absorption spectrum, etc., and achieve easy control of influencing factors, uniform particle size and simple process. Effect

Active Publication Date: 2019-10-15
JINGDEZHEN CERAMIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to γ~Ce 2 S 3 Belonging to Cubic Th 3 P 4 type structure, there are cation vacancies in the lattice, and the vacancies form a twisted S in the cubic crystal structure 4 Tetrahedral voids, resulting in γ~Ce 2 S 3 The crystal structure is very unstable, and it is easy to reverse and transform into β phase under high temperature, thus losing the red color
Therefore, the problem of crystal structure stability cannot be solved essentially only by simple encapsulation. At present, although ion doping is also used to achieve lattice stability, research has found that although single ion doping can achieve lattice stability, it is easy to so that γ~Ce 2 S 3 The electronic transition energy of the pigment f→d changes, and the absorption spectrum changes, so that the bright red color is no longer displayed

Method used

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  • A nano-scale low-valent ion complex doping type γ~ce <sub>2</sub> the s <sub>3</sub> Red pigment and preparation method thereof
  • A nano-scale low-valent ion complex doping type γ~ce <sub>2</sub> the s <sub>3</sub> Red pigment and preparation method thereof
  • A nano-scale low-valent ion complex doping type γ~ce <sub>2</sub> the s <sub>3</sub> Red pigment and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In this embodiment, nano-scale low-valent ion composite doping type γ~Ce 2 S 3 The preparation method of red pigment, its step is as follows:

[0031] (1) Preparation of cerium oxysulfide precursor suspension containing doped ionic elements by solvothermal method

[0032] 3.50gCeCl 3 ·7H 2 O, 0.13gEu 2 (SO 4 ) 3 ·H 2 O, 0.06gSnCl 2 2H 2 O and 0.40g 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;

[0033] (2) Preparation of cerium oxysulfide precursor powder containing doped ionic elements

[0034] After the above suspension is centrifuged, washed with water, washed with alcohol, and dried, a cerium oxysulfide precursor powder containing doping elements Eu and Sn is obtained;

[0035] (3) Ion composite doping type γ~Ce...

Embodiment 2

[0040] In this embodiment, nano-scale low-valent ion composite doping type γ~Ce 2 S 3 The preparation method of red pigment, its step is as follows:

[0041] (1) Preparation of cerium oxysulfide precursor suspension containing doped ionic elements by solvothermal method

[0042] 3.91gCe(NO 3 ) 3 ·6H 2 O, 0.175gEu 2 (SO 4 ) 3 ·H 2 O, 0.21g SmCl 3 ·6H 2 O and 0.35g thiourea were successively dissolved in 70ml ethylene glycol, stirred vigorously for 100min, then transferred to a stainless steel reaction kettle lined with polytetrafluoroethylene, and reacted at 250°C for 15h to obtain Eu, Sm containing doping elements The cerium oxysulfide precursor suspension;

[0043] (2) Preparation of cerium oxysulfide precursor powder containing doped ionic elements

[0044] After the above suspension is centrifuged, washed with water, washed with alcohol, and dried, a cerium oxysulfide precursor powder containing doping elements Eu and Sm is obtained;

[0045] (3) Ion composite ...

Embodiment 3

[0049] In this embodiment, nano-scale low-valent ion composite doping type γ~Ce 2 S 3 The preparation method of red pigment differs from embodiment one in that:

[0050] The sulfur source in the present embodiment step (1) is tetraethylthiuram disulfide (C 10 h 20 N 2 S 4 ), the consumption is 1.5g; in the step (2), the additive is calcium carbonate, and its consumption is 3.0wt% of the precursor powder, and the consumption of the sintering aid diboron trioxide is 3.0wt% of the precursor powder.

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Abstract

The invention discloses a nano-scale low-valent ion composite doped gamma-Ce2S3 red pigment, wherein the ion valence of the doped ion M is 2, at least two kinds of the doped ions exist, a molar ratioof Ce<3+> to M[total] is 2(1-x):3x, and x is more than 0 and is less than or equal to 0.1. The invention further discloses a preparation method of the nano-scale low-valent ion composite doped gamma-Ce2S3 red pigment. According to the present invention, the composite doped low-valent ions enter the gamma-Ce2S3 crystal lattice, and the doping is achieved by replacing the Ce<3+> ions and filling thecation vacancy in the crystal lattice, such that the gamma-Ce2S3 crystal lattice is effectively stabilized, and the high-temperature stability of the pigment is substantially improved so as to substantially expand the application of the material under the high temperature condition; and the preparation method has advantages of simple process, easy operation, easy control of influence factors, lowproduction cost, and easy promotion and application.

Description

technical field [0001] The invention relates to the technical field of inorganic pigments, in particular to an ion-doped γ-Ce 2 S 3 Red pigment and its preparation method. Background technique [0002] γ~Ce 2 S 3 The pigment is bright red, stable in color, strong in hiding power, resistant to ultraviolet radiation, safe and non-toxic, and has become the first choice to replace toxic cadmium selenium red pigments, and has a wide range of applications in plastics, rubber, high-grade coatings and other fields. However, γ~Ce 2 S 3 The pigment can only be used at a temperature lower than 350°C. If the temperature exceeds this temperature, it will quickly decompose and lose red, thus affecting its application at high temperature. [0003] In order to improve γ~Ce 2 S 3 The high temperature stability of the existing technology mainly adopts the wrapping technology, that is, coating one or more layers of transparent high temperature stable materials on the surface of the pig...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00B82Y40/00
CPCC01F17/288C01P2002/72C01P2004/03C01P2004/32C01P2004/62C01P2004/64C01P2006/63
Inventor 王竹梅李月明沈宗洋马振国宋福生
Owner JINGDEZHEN CERAMIC UNIV
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