CN106010516A - Manganese-excited aluminosilicate fluorescent powder and preparation method thereof - Google Patents
Manganese-excited aluminosilicate fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses manganese-excited aluminosilicate fluorescent powder and a preparation method thereof. The chemical formula of the manganese-excited aluminosilicate fluorescent powder is Sr1-xAl2Si2O8: xMn<2+>, wherein in the formula, x is 0.02-0.2. The preparation method comprises the following steps: S1, weighing a mixture of raw materials strontium carbonate, aluminum trichloride, silicic acid and manganese dioxide in a chemical ratio of the chemical composition Sr1-xAl2Si2O8: xMn<2+>; S2, adding a fluxing agent for grinding, and uniformly grinding so as to obtain a mixture; S3, feeding the mixture obtained in step S2 into a crucible, sintering for 4-6 hours inside a high-temperature furnace in the presence of a reducing atmosphere at 1400-1600 DEG C, and cooling, thereby obtaining the manganese-excited aluminosilicate fluorescent powder, wherein the addition amount of the fluxing agent accounts for 0.7-0.9% of the weight of the raw materials; the fluxing agent is a mixture of ammonium acetate and ammonium sulfide; the weight ratio of ammonium acetate to ammonium sulfide is (6-8):1. The manganese-excited aluminosilicate fluorescent powder disclosed by the invention is good in dispersity, high in luminous intensity and good in stability, the advantages are related to the weight ratio of ammonium acetate to ammonium sulfide in the fluxing agent, and when the weight ratio of ammonium acetate to ammonium sulfide is (6-8):1, the highest luminous intensity can be achieved.
Description
Technical field
The invention belongs to field of light emitting materials, be specifically related to aluminosilicate fluorescent powder that a kind of manganese excites and preparation method thereof.
Background technology
Global energy price is surging and in the case of global warming, energy-saving and cost-reducing and environmental conservation is than the most more
Important, energy conservation object and the standard ratio of environmental conservation that the whole world is guided by national policy or enforces are the clearest and the most definite and anxious
Compel.Gradually eliminating electric filament lamp before within 2007, first Australia announce 2012, European Union announces no longer to sell electric filament lamp in 2009 in succession,
When the most Canadian, Japanese, California, USA has corresponding popularization electricity-saving lamp to substitute electric filament lamp plans or restriction use
Between table.The Chinese government is the most also proposed the illumination policy of " National Semiconductor illuminating engineering " (referring mainly to LED), energetically
Promote and universal energy-conserving and environment-protective lighting engineering.
White-light LED illumination has energy-saving and environmental protection, life-span length, low consumption, low grade fever, high brightness, waterproof, shockproof, light beam are concentrated,
The advantages such as easy maintenance it is considered to be 21 century most likely enter a kind of New Solid cold light source and most in general lighting field
One of high-technology field of development prospect.
Summary of the invention
It is an object of the invention to provide aluminosilicate fluorescent powder that a kind of manganese excites and preparation method thereof.
The above-mentioned purpose of the present invention is achieved by techniques below scheme:
The aluminosilicate fluorescent powder that a kind of manganese excites, chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x span is
0.02～0.2, it is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x span is 0.02～0.2；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in reducing atmosphere and 1400～1600 DEG C of conditions in high temperature furnace
Lower sintering 4～6 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.7～0.9% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide,
The weight ratio of ammonium acetate and ammonium sulfide is 6～8:1.
Further, described aluminosilicate fluorescent powder, chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.1,
It is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.1；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 7:1.
Further, described aluminosilicate fluorescent powder, chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.02,
It is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.02；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Tie 6 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 6:1.
Further, described aluminosilicate fluorescent powder, chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.2,
It is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.2；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Tie 4 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 8:1.
Further, described reducing atmosphere is Carbon monoxide reduction atmosphere.
Advantages of the present invention:
The aluminosilicate fluorescent powder good dispersion that the present invention provides, luminous intensity is high, and stability is high, in these advantages and flux
Ammonium acetate is relevant with the weight ratio of ammonium sulfide, and when the weight ratio of ammonium acetate and ammonium sulfide is 6～8:1, luminous intensity is the highest.
Detailed description of the invention
Further illustrate the essentiality content of the present invention below in conjunction with embodiment, but do not limit scope with this.To the greatest extent
The present invention is explained in detail by pipe with reference to preferred embodiment, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent, without deviating from the spirit and scope of technical solution of the present invention.
Embodiment 1: the preparation of aluminosilicate fluorescent powder
Chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.1, is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.1；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 7:1.
Embodiment 2: the preparation of aluminosilicate fluorescent powder
Chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.02, is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.02；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Tie 6 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 6:1.
Embodiment 3: the preparation of aluminosilicate fluorescent powder
Chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.2, it is characterised in that is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.2；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Tie 4 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 8:1.
Embodiment 4: the preparation of aluminosilicate fluorescent powder
Chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.1, is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.1；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 6:1.
Embodiment 5: the preparation of aluminosilicate fluorescent powder
Chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.1, is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.1；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 8:1.
The weight ratio of embodiment 6: comparative example, ammonium acetate and ammonium sulfide is 5:1
Chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.1, is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.1；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 5:1.
The weight ratio of embodiment 7: comparative example, ammonium acetate and ammonium sulfide is 9:1
Chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is 0.1, is made by the steps and forms:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.1；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 9:1.
Embodiment 8: effect example
The luminescent properties of the fluorescent material of testing example 1～7 preparation respectively, the excitation and emission spectra of different embodiment fluorescent material
Position is basically identical, but luminous intensity, stability of photoluminescence and dispersibility have relatively big difference, result such as table 1.Wherein, luminous strong
Degree, on the basis of embodiment 1, is set to 100, and remaining embodiment is the relative luminous intensity relative to embodiment 1.
The luminescent properties of the different embodiment fluorescent material of table 1 and dispersibility
| Luminous intensity | Stability of photoluminescence | Dispersibility | |
| Embodiment 1 | 100 | Highly stable | Dispersibility is the best |
| Embodiment 4 | 98 | More stable | Dispersibility is preferable |
| Embodiment 5 | 99 | More stable | Dispersibility is preferable |
| Embodiment 6 | 66 | Unstable | Poor dispersion |
| Embodiment 7 | 68 | Unstable | Poor dispersion |
The test result of embodiment 2,3 is basically identical with embodiment 4,5.
Above-mentioned test result indicate that, the aluminosilicate fluorescent powder good dispersion that the present invention provides, luminous intensity is high, and stability is high,
These advantages are relevant with the weight ratio of ammonium acetate in flux and ammonium sulfide, when the weight ratio of ammonium acetate and ammonium sulfide is 6～8:1,
Luminous intensity is the highest.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but does not limit protection scope of the present invention with this.
It will be understood by those within the art that, technical scheme can be modified or equivalent, and not take off
Essence and protection domain from technical solution of the present invention.
Claims (5)
1. the aluminosilicate fluorescent powder that manganese excites, chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x span is
0.02～0.2, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x span is 0.02～0.2；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in reducing atmosphere and 1400～1600 DEG C of conditions in high temperature furnace
Lower sintering 4～6 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.7～0.9% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide,
The weight ratio of ammonium acetate and ammonium sulfide is 6～8:1.
Aluminosilicate fluorescent powder the most according to claim 1, chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is
0.1, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.1；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1500 DEG C
Tie 5 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 7:1.
Aluminosilicate fluorescent powder the most according to claim 1, chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is
0.02, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.02；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1400 DEG C
Tie 6 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 6:1.
Aluminosilicate fluorescent powder the most according to claim 1, chemical formula is Sr1-xAl2Si2O8:xMn2+, wherein x value is
0.2, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Sr1-xAl2Si2O8:xMn2+Stoichiometric proportion weigh raw material, described raw material be strontium carbonate,
The mixture of aluminum chloride, silicic acid and manganese dioxide, wherein, x value is 0.2；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, burns in high temperature furnace under the conditions of reducing atmosphere and 1600 DEG C
Tie 4 hours, cool down and i.e. obtain described aluminosilicate fluorescent powder；
Wherein, the addition of flux is the 0.9% of raw material weight, and described flux is the mixture of ammonium acetate and ammonium sulfide, second
The weight ratio of acid ammonium and ammonium sulfide is 8:1.
5. according to the arbitrary described aluminosilicate fluorescent powder of Claims 1 to 4, it is characterised in that: described reducing atmosphere is an oxidation
Carbon reducing atmosphere.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106866132A (en) * | 2017-01-13 | 2017-06-20 | 南京工业大学 | It is a kind of for fluorescence ceramics for illuminating or showing and preparation method thereof |
-
2016
- 2016-06-28 CN CN201610489152.1A patent/CN106010516A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| WUBIN DAI: "A Single-Phased Sr1-y-3x/2Al2Si2O8: xCe3+, yMn2+ with Efficient Energy Transfer as a Potential Phosphor for White-Light-Emitting Diodes", 《J. AM. CERAM. SOC.》 * |
| 洪广言: "《稀土发光材料——基础与应用》", 30 April 2011, 科学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106866132A (en) * | 2017-01-13 | 2017-06-20 | 南京工业大学 | It is a kind of for fluorescence ceramics for illuminating or showing and preparation method thereof |
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