CN104326739A - Mesosilicate neodymium high temperature ceramic pigment and preparation method thereof - Google Patents
Mesosilicate neodymium high temperature ceramic pigment and preparation method thereof Download PDFInfo
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- CN104326739A CN104326739A CN201410543206.9A CN201410543206A CN104326739A CN 104326739 A CN104326739 A CN 104326739A CN 201410543206 A CN201410543206 A CN 201410543206A CN 104326739 A CN104326739 A CN 104326739A
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Abstract
The invention discloses a mesosilicate neodymium high temperature ceramic pigment and a preparation method thereof. The preparation method of the mesosilicate neodymium high temperature ceramic pigment comprises the following steps: (1) adding neodymium nitrate and ethyl orthosilicate into a water / ethanol mixed solution, stirring evenly, adding polyethylene glycol, stirring for dispersing treatment to obtain neodymium and silicon-containing sol; (2) dropwise adding a precipitant into the neodymium and silicon-containing sol until the neodymium and silicon-containing sol pH is 8.5-9 to obtain a precipitation solution; (3) standing the precipitation solution, aging, centrifugally processing, then washing centrifuged precipitation solids with absolute ethanol to obtain a precipitate; (4) placing the precipitate into a blast drying box for drying, and then calcining the dried material at high temperature to obtain the mesosilicate neodymium high temperature ceramic pigment. The preparation method has the advantages of simple technological process, low equipment requirements and easy industrialized production; the obtained mesosilicate neodymium high temperature ceramic pigment has the advantages of uniform particle size, narrow particle size distribution, less aggregation, and color stability.
Description
Technical field
The present invention relates to a kind of ceramic pigment, particularly relate to a kind of disilicic acid neodymium high temperature pigment of ceramic and preparation method thereof.
Background technology
Rear earth element nd contains 3 4f electronics, and electronics can produce multiple spectrum item or wire spectral line in the transition between energy level of f-f subgrade.Under the exciting of outside energy, some narrow absorption peaks can be there is in neodymium element within the scope of visible region, especially strong absorption is had in 530 nanometers and 600 nanometers, due to the existence of these two narrow absorption peaks, when converting wavelength and the intensity of incident light, wavelength and the intensity of its reflected light also change thereupon, make the pigment containing neodymium produce the effect of variable color.Disilicic acid neodymium (Nd
2si
2o
7) can be used as a kind of high temperature pigment of ceramic with color changeable effect, the method for synthesis at present mainly comprises solid phase method and sol-gel method.Prepared by Nd for solid phase method
2si
2o
7ceramic pigment, because the mixing uniformity of raw material is relatively poor, easily forms impurity phase in sintering process.And sol-gel method, complicated process of preparation, colorant easily forms larger hard aggregation, is unfavorable for later stage attrition process.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, primary and foremost purpose of the present invention is the preparation method providing a kind of disilicic acid neodymium high temperature pigment of ceramic;
Another object of the present invention is to the disilicic acid neodymium high temperature pigment of ceramic providing above-mentioned preparation method to obtain.
Object of the present invention is achieved through the following technical solutions:
A preparation method for disilicic acid neodymium high temperature pigment of ceramic, comprises the steps:
(1) neodymium nitrate and tetraethoxy are joined in water/mixed alkoxide solution, stir, then add polyoxyethylene glycol, dispersed with stirring process, obtain the colloidal sol containing neodymium and silicon;
(2) contain to gained in the colloidal sol of neodymium and silicon and drip precipitation agent, until the pH of colloidal sol is 8.5 ~ 9.0, be precipitated liquid;
(3) by still aging for gained precipitated liquid, then centrifugal treating, then by absolute ethanol washing centrifugal solids precipitation, be precipitated thing;
(4) gained throw out is placed in air dry oven and carries out drying, then dry thing is carried out high-temperature calcination, obtain described disilicic acid neodymium high temperature pigment of ceramic.
In the preparation method of above-mentioned disilicic acid neodymium high temperature pigment of ceramic:
Preferably, the mol ratio of step (1) described neodymium nitrate and tetraethoxy is: neodymium nitrate: tetraethoxy=1:(1 ~ 1.4);
Preferably, the concentration of step (1) described neodymium nitrate in the described colloidal sol containing neodymium and silicon is 0.25 ~ 0.5 mol/L;
Preferably, the described water/mixed alkoxide solution of step (1) is the mixing solutions of water and ethanol, and the volume ratio of water and ethanol is 1:1;
Preferably, the concentration of step (1) described polyoxyethylene glycol in the described colloidal sol containing neodymium and silicon is 0.05 ~ 0.15 grams per milliliter;
Preferably, step (2) described precipitation agent is one in ammoniacal liquor or trimethylammonium hydroxide or both mixing; Preferred, the concentration of step (2) described precipitation agent is 2 mol/L;
Preferably, step (3) the described still aging time is 6 ~ 12 hours;
Preferably, the temperature of step (4) described drying is 60 DEG C, and time of drying is 18 ~ 24 hours;
Preferably, the temperature of step (4) described high-temperature calcination is 1000 ~ 1200 DEG C, and calcination time is 5 hours.
Disilicic acid neodymium high temperature pigment of ceramic is obtained according to above-mentioned preparation method.
The present invention has following advantage and effect relative to prior art:
(1) preparation method's technique of the present invention is simple, and product property is stablized, and production cost is low, is easy to industrialization promotion.
(2) disilicic acid neodymium high temperature pigment of ceramic epigranular of the present invention, reunites few.
Accompanying drawing explanation
Fig. 1 is the XRD figure of disilicic acid neodymium high temperature pigment of ceramic of the present invention.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
A kind of disilicic acid neodymium high temperature pigment of ceramic, its preparation method is:
(1) 23.6 grams of tetraethoxys and 44.1 grams of neodymium nitrates are taken, join (water/mixed alkoxide solution comprises 200 ml waters and 200 milliliters of ethanol) in 400 ml waters/mixed alkoxide solution, stir after 10 minutes, add 2.5 grams of polyoxyethylene glycol PEG-10000 again, stir after 30 minutes, obtain the colloidal sol containing neodymium and silicon of transparent and stable;
(2) contain to gained in the colloidal sol of neodymium and silicon and dropwise drip the ammonia soln that concentration is 2 mol/L, until the pH of colloidal sol reaches 8.7, form precipitation, be precipitated liquid;
(3) by after still aging for precipitated liquid 12 hours, centrifugal treating, and adopt absolute ethanol washing three times, be precipitated thing;
(4) throw out is placed in 60 DEG C of air dry ovens, after dry 24 hours, the temperature being placed in 1200 DEG C is calcined, and calcination time is 5 hours, obtains disilicic acid neodymium high temperature pigment of ceramic.
Get gained disilicic acid neodymium high temperature pigment of ceramic and carry out X-ray diffraction analysis, gained XRD figure as shown in Figure 1.
Gained disilicic acid neodymium high temperature pigment of ceramic epigranular, narrow diameter distribution, reunites few, in colour-stable.
Embodiment 2
A kind of disilicic acid neodymium high temperature pigment of ceramic, its preparation method is:
(1) 29.2 grams of tetraethoxys and 43.8 grams of neodymium nitrates are taken, join (water/mixed alkoxide solution comprises 150 ml waters and 150 milliliters of ethanol) in 300 ml waters/mixed alkoxide solution, stir after 10 minutes, add 3.5 grams of polyoxyethylene glycol PEG-10000 again, stir after 30 minutes, obtain the colloidal sol containing neodymium and silicon of transparent and stable;
(2) contain to gained in the colloidal sol of neodymium and silicon and dropwise drip the ammonia soln that concentration is 2 mol/L, until the pH of colloidal sol reaches 8.5, form precipitation, be precipitated liquid;
(3) by after still aging for precipitated liquid 6 hours, centrifugal treating, and adopt absolute ethanol washing three times, be precipitated thing;
(4) throw out is placed in 60 DEG C of air dry ovens, after dry 12 hours, the temperature being placed in 1000 DEG C is calcined, and calcination time is 5 hours, obtains disilicic acid neodymium high temperature pigment of ceramic.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. a preparation method for disilicic acid neodymium high temperature pigment of ceramic, is characterized in that comprising the steps:
(1) neodymium nitrate and tetraethoxy are joined in water/mixed alkoxide solution, stir, then add polyoxyethylene glycol, dispersed with stirring process, obtain the colloidal sol containing neodymium and silicon;
(2) contain to gained in the colloidal sol of neodymium and silicon and drip precipitation agent, until the pH of colloidal sol is 8.5 ~ 9.0, be precipitated liquid;
(3) by still aging for gained precipitated liquid, then centrifugal treating, then by absolute ethanol washing centrifugal solids precipitation, be precipitated thing;
(4) gained throw out is placed in air dry oven and carries out drying, then dry thing is carried out high-temperature calcination, obtain described disilicic acid neodymium high temperature pigment of ceramic.
2. the preparation method of a kind of disilicic acid neodymium high temperature pigment of ceramic according to claim 1, is characterized in that: the mol ratio of step (1) described neodymium nitrate and tetraethoxy is: neodymium nitrate: tetraethoxy=1:(1 ~ 1.4); The concentration of described neodymium nitrate in the described colloidal sol containing neodymium and silicon is 0.25 ~ 0.5 mol/L.
3. the preparation method of a kind of disilicic acid neodymium high temperature pigment of ceramic according to claim 1, is characterized in that: the described water/mixed alkoxide solution of step (1) is the mixing solutions of water and ethanol, and the volume ratio of water and ethanol is 1:1.
4. the preparation method of a kind of disilicic acid neodymium high temperature pigment of ceramic according to claim 1, is characterized in that: the concentration of step (1) described polyoxyethylene glycol in the described colloidal sol containing neodymium and silicon is 0.05 ~ 0.15 grams per milliliter.
5. the preparation method of a kind of disilicic acid neodymium high temperature pigment of ceramic according to claim 1, is characterized in that: step (2) described precipitation agent is one in ammoniacal liquor or trimethylammonium hydroxide or both mixing.
6. the preparation method of a kind of disilicic acid neodymium high temperature pigment of ceramic according to claim 5, is characterized in that: the concentration of step (2) described precipitation agent is 2 mol/L.
7. the preparation method of a kind of disilicic acid neodymium high temperature pigment of ceramic according to claim 1, is characterized in that: step (3) the described still aging time is 6 ~ 12 hours.
8. the preparation method of a kind of disilicic acid neodymium high temperature pigment of ceramic according to claim 1, is characterized in that: the temperature of step (4) described drying is 60 DEG C, and time of drying is 18 ~ 24 hours.
9. the preparation method of a kind of disilicic acid neodymium high temperature pigment of ceramic according to claim 1, is characterized in that: the temperature of step (4) described high-temperature calcination is 1000 ~ 1200 DEG C, and calcination time is 5 hours.
10. the disilicic acid neodymium high temperature pigment of ceramic that preparation method obtains according to any one of claim 1 ~ 9.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675098A (en) * | 2016-12-26 | 2017-05-17 | 深圳市丁鼎陶瓷科技有限公司 | Preparation technology of black pigment for zirconia ceramics |
| CN108794005A (en) * | 2018-06-06 | 2018-11-13 | 华南理工大学 | A kind of near-infrared high reflectance function ceramics colorant and preparation method thereof |
| CN108912738A (en) * | 2018-06-06 | 2018-11-30 | 华南理工大学 | A kind of near-infrared high reflectance ceramic pigment and preparation method thereof |
| CN114350350A (en) * | 2022-01-10 | 2022-04-15 | 华南理工大学 | Pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect as well as preparation method and application thereof |
-
2014
- 2014-10-14 CN CN201410543206.9A patent/CN104326739B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| SHANJUN KE ET AL.: "Crystallization kinetics of neodymium disilicate obtained by polymeric xerogels", 《J.MATER.SCI》, no. 49, 13 February 2014 (2014-02-13), pages 3736 - 3741 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675098A (en) * | 2016-12-26 | 2017-05-17 | 深圳市丁鼎陶瓷科技有限公司 | Preparation technology of black pigment for zirconia ceramics |
| CN108794005A (en) * | 2018-06-06 | 2018-11-13 | 华南理工大学 | A kind of near-infrared high reflectance function ceramics colorant and preparation method thereof |
| CN108912738A (en) * | 2018-06-06 | 2018-11-30 | 华南理工大学 | A kind of near-infrared high reflectance ceramic pigment and preparation method thereof |
| CN108794005B (en) * | 2018-06-06 | 2021-03-30 | 华南理工大学 | Near-infrared high-reflectivity functional ceramic pigment and preparation method thereof |
| CN108912738B (en) * | 2018-06-06 | 2021-08-10 | 华南理工大学 | Near-infrared high-reflectivity ceramic pigment and preparation method thereof |
| CN114350350A (en) * | 2022-01-10 | 2022-04-15 | 华南理工大学 | Pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect as well as preparation method and application thereof |
| CN114350350B (en) * | 2022-01-10 | 2023-02-14 | 华南理工大学 | Pigment with photoluminescence, mechanoluminescence and light-dependent heterochromatic effect as well as preparation method and application thereof |
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| CN104326739B (en) | 2016-04-13 |
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