CN105219389A - Strontium silicate magnesium raw powder's production technology is prepared in a kind of rare earth Eu, Dy doping - Google Patents
Strontium silicate magnesium raw powder's production technology is prepared in a kind of rare earth Eu, Dy doping Download PDFInfo
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- CN105219389A CN105219389A CN201510643254.XA CN201510643254A CN105219389A CN 105219389 A CN105219389 A CN 105219389A CN 201510643254 A CN201510643254 A CN 201510643254A CN 105219389 A CN105219389 A CN 105219389A
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Abstract
A kind of rare earth Eu, Dy doping of the present invention strontium silicate magnesium raw powder's production technology, first take strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate, water glass, reductive agent, the mol ratio of strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate, water glass, reductive agent is 1.8 ~ 1.98:0.95 ~ 2:0.01 ~ 0.1:0.01 ~ 0.1:1 ~ 2:3 ~ 30; First water glass is dissolved in the water and makes sodium silicate aqueous solution, subsequently strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate and reductive agent are dissolved completely in deionized water, pour sodium silicate aqueous solution into again, 90 ~ 100 DEG C are heated to subsequently with magnetic stirring apparatus, solution, after 0.3 ~ 1 hour, directly moves in the high temperature sintering furnace being heated to 650 ~ 900 DEG C in advance, along with the evaporation of moisture by Keep agitation, there is vigorous combustion, obtain fluffy spumescence product.The present invention adopts the water glass of cost cheaper to be raw material, and cost is low, and technique is simple.
Description
Technical field
The invention belongs to materialogy field, relate to a kind of inorganic non-metallic ultrafine powder, particularly relate to a kind of strontium silicate magnesium, specifically a kind of rare earth Eu, Dy doping strontium silicate magnesium raw powder's production technology.
Background technology
Long after glow luminous material is exactly the energy that can absorb and store ambient light radiation by day, the energy stored with the form slow releasing of visible ray to evening thus reach the material of illuminating effect.Compared with sulfide, aluminate long afterglow materials, silicate series long-afterglow material chemical stability is good, and water tolerance is strong, raw material SiO
2inexpensive, be easy to get, therefore the research and development of silicate fluorescent material is subject to extensive concern all over the world.
Obtain long-afterglow material, the preparation of its material is crucial.The preparation of current strontium silicate magnesium base long persistence luminescent material, is mainly undertaken by high temperature solid state reaction and sol-gel method.The powder granule that high temperature solid-state method obtains is comparatively thick, and sintering temperature is higher, long reaction time, has a certain impact after grinding to its luminescent properties, and the high theme not meeting current environmental protection of energy consumption.Sol-gel method is a kind of emerging wet chemical synthesis, although obtained powder can reach nano level, operation is loaded down with trivial details, wayward, and alkoxide used is harmful is unfavorable for scale operation.
Combustion synthesis method is a kind of advanced synthetic technology of material, and it utilizes chemical reaction self-heat generation to prepare material, has the advantages such as technique is simple, energy consumption is low, generated time is short, efficiency is high, product purity is high, less investment.Have at present and adopted combustion synthesis technology to prepare the research report of strontium silicate magnesium, originated as silicon with silicon sol.But because silicon sol solid content is low, price is high, thus have impact on its large-scale promotion application.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of rare earth Eu, Dy doping strontium silicate magnesium raw powder's production technology, described to this solves silicon sol solid content in preparation method of the prior art low, and price is high, is difficult to the technical problem of large-scale promotion.
The method of a kind of rare earth Eu, Dy doping of the present invention strontium silicate magnesium raw powder's production technology, comprises the following steps:
1) take strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate, water glass, reductive agent, the mol ratio of described strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate, water glass, reductive agent is 1.8 ~ 1.98:0.9 ~ 2:0.01 ~ 0.1:0.01 ~ 0.1:1 ~ 2:3 ~ 30;
2) be dissolved in the water by water glass and make sodium silicate aqueous solution, the concentration of described sodium silicate solution is between 0.5 ~ 2mol/L;
3) strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate and reductive agent are dissolved completely in deionized water, pour into again in sodium silicate aqueous solution, be heated to 90 ~ 100 DEG C subsequently, Keep agitation is after 0.3 ~ 1 hour, solution is directly moved in the high temperature sintering furnace being heated to 650 ~ 900 DEG C in advance, after moisture evaporation, obtain fluffy spumescence product rare earth Eu, Dy doping strontium silicate magnesium powder.
Further, described reductive agent is any one in urea, citric acid.
The present invention replaces silicon sol for raw material with water glass and adopts combustion synthesis technology to prepare rare earth Eu, Dy doping strontium silicate magnesium powder, thus there is not the problems such as sol-gel method expensive starting materials, technique is loaded down with trivial details, solid content is low, there is with low cost, the simple technique effect of technique.Method of the present invention does not need external heat source long duration of action, therefore there is not the problems such as sintering temperature is higher, long reaction time, the technique effect that to have that thermal treatment temp is low, quick, product is reunited few.
The present invention compares with prior art, and its technical progress is significant.The present invention adopts the water glass of cost cheaper to be raw material, and cost is low, is conducive to practical application, and equipment and process is simple.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of embodiment 1.
Embodiment
Below by specific embodiment, also the present invention is further elaborated by reference to the accompanying drawings, but do not limit the present invention.
Embodiment 1
In strontium nitrate: magnesium nitrate: europium nitrate: Dysprosium trinitrate: water glass: the mol ratio=1.97:1:0.01:0.02:1:6 ratio batching of urea, by strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate and urea are dissolved completely in deionized water, pour in the water glass be dissolved in the water again, 90 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 1 hour, solution is directly moved in the high temperature sintering furnace being heated to 850 DEG C in advance, along with the evaporation of moisture, vigorous combustion, obtain fluffy spumescence product, its XRD as shown in Figure 1, from XRD figure, product is strontium silicate magnesium Sr
2mgSiO
7: Eu, Dy powder.
Embodiment 2
In strontium nitrate: magnesium nitrate: europium nitrate: Dysprosium trinitrate: water glass: the mol ratio=1.8:0.95:0.1:0.1:1:30 ratio batching of urea, strontium nitrate, magnesium nitrate and urea are dissolved completely in deionized water, again the water glass be dissolved in the water is poured into, 100 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 0.3 hour, solution is directly moved in the high temperature sintering furnace being heated to 650 DEG C in advance, along with the evaporation of moisture, vigorous combustion, obtain fluffy spumescence product, all the other implementation conditions, all with embodiment 1, obtain strontium silicate magnesium Sr
2mgSiO
7: Eu, Dy powder.
Embodiment 3
In strontium nitrate: magnesium nitrate: europium nitrate, Dysprosium trinitrate, water glass: the mol ratio=1.98:2:0.01:0.01:2:3 ratio batching of citric acid, strontium nitrate, magnesium nitrate and citric acid are dissolved completely in deionized water, again the water glass be dissolved in the water is poured into, 95 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 0.5 hour, solution is directly moved in the high temperature sintering furnace being heated to 700 DEG C in advance, along with the evaporation of moisture, vigorous combustion, obtain fluffy spumescence product, all the other implementation conditions all with embodiment 1, obtain SrMgSiO
4: Eu, Dy powder.
Embodiment 4
In strontium nitrate: magnesium nitrate: europium nitrate, Dysprosium trinitrate, water glass: the mol ratio=1.96:0.99:0.02:0.02:1.98:5 ratio batching of citric acid, strontium nitrate, magnesium nitrate and citric acid are dissolved completely in deionized water, again the water glass be dissolved in the water is poured into, 98 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 0.6 hour, solution is directly moved in the high temperature sintering furnace being heated to 750 DEG C in advance, along with the evaporation of moisture, vigorous combustion, obtain fluffy spumescence product, all the other implementation conditions all with embodiment 1, obtain Ca
2mgSiO
7: Eu, Dy powder.
The content of above-described embodiment be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (2)
1. rare earth Eu, Dy doping strontium silicate magnesium raw powder's production technology, is characterized in that comprising the following steps:
1) take strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate, water glass, reductive agent, the mol ratio of described strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate, water glass, reductive agent is 1.8 ~ 1.98:0.95 ~ 2:0.01 ~ 0.1:0.01 ~ 0.1:1 ~ 2:3 ~ 30;
2) be dissolved in the water by water glass and make sodium silicate aqueous solution, the concentration of described sodium silicate solution is between 0.5 ~ 2mol/L;
3) strontium nitrate, magnesium nitrate, europium nitrate, Dysprosium trinitrate and reductive agent are dissolved completely in deionized water, pour into again in sodium silicate aqueous solution, be heated to 90 ~ 100 DEG C subsequently, Keep agitation is after 0.3 ~ 1 hour, solution is directly moved in the high temperature sintering furnace being heated to 650 ~ 900 DEG C in advance, after moisture evaporation, obtain fluffy spumescence product rare earth Eu, Dy doping strontium silicate magnesium powder.
2. a kind of method preparing strontium silicate magnesium powder according to claim 1, is characterized in that: described reductive agent is any one in urea, citric acid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942004A (en) * | 2019-04-10 | 2019-06-28 | 宁波大学 | A kind of strontium silicate magnesium nano material and preparation method thereof and purposes |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793284A (en) * | 2005-12-09 | 2006-06-28 | 天津理工大学 | Process for preparing silicon blue photoluminescent material |
| WO2009062579A1 (en) * | 2007-11-12 | 2009-05-22 | Merck Patent Gmbh | Coated phosphor particles with refractive index adaption |
| CN104140108A (en) * | 2014-07-07 | 2014-11-12 | 上海应用技术学院 | Method for preparing calcium magnesium silicate powder |
-
2015
- 2015-10-08 CN CN201510643254.XA patent/CN105219389A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793284A (en) * | 2005-12-09 | 2006-06-28 | 天津理工大学 | Process for preparing silicon blue photoluminescent material |
| WO2009062579A1 (en) * | 2007-11-12 | 2009-05-22 | Merck Patent Gmbh | Coated phosphor particles with refractive index adaption |
| CN104140108A (en) * | 2014-07-07 | 2014-11-12 | 上海应用技术学院 | Method for preparing calcium magnesium silicate powder |
Non-Patent Citations (2)
| Title |
|---|
| 徐咏钗等: "燃烧法合成Eu~(2+)、Dy~(3+)、Nd~(3+)共掺杂的硅酸盐长余辉发光材料Sr_2MgSi_2O_7和Sr_2ZnSi_2O_7", 《中南民族大学学报(自然科学版)》 * |
| 李东平等: "燃烧法合成新型蓝色硅酸盐长余辉材料及其发光性能的研究", 《稀有金属》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942004A (en) * | 2019-04-10 | 2019-06-28 | 宁波大学 | A kind of strontium silicate magnesium nano material and preparation method thereof and purposes |
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