CN105950139A - Manganese ion activated fluorosilicate red fluorescent powder and preparation method thereof - Google Patents
Manganese ion activated fluorosilicate red fluorescent powder and preparation method thereof Download PDFInfo
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
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Abstract
The invention discloses a manganese ion activated fluorosilicate red fluorescent powder and a preparation method thereof. A chemical composition of the fluorosilicate red fluorescent powder is Mg1-xSiO2F2: xMn<2+>, wherein x is 0.06-0.20. The fluorosilicate red fluorescent powder is prepared by the following steps: 1, weighing a mixture of raw materials magnesium carbonate, sodium fluoride, silicic acid and manganese dioxide according to a stoichiometric ratio of Mg1-xSiO2F2: xMn<2+>, wherein x is 0.06-0.20; 2, adding a fluxing agent, and performing grinding and uniform mixing to obtain a mixture; 3, gluing the mixture obtained in step 2 into a crucible, performing sintering for 3 to 5 hours under the condition of 1,300 to 1,500 DEG C in a reducing atmosphere in a high-temperature furnace, and performing cooling, wherein the addition of the fluxing agent is 0.6 to 0.8 percent of the weight of the raw materials, the fluxing agent is a mixture of sodium sulfide and boric acid, and the weight ratio of the sodium sulfide and the boric acid is (5-7):1. The nanometer fluorosilicate red fluorescent powder is high in dispersibility, luminous intensity and stability, the advantages are related to the weight ratio of the sodium sulfide and boric acid in the fluxing agent, and when the weight ratio of the sodium sulfide and the boric acid is (5-7):1, the luminous intensity is the highest.
Description
Technical field
The invention belongs to LED luminescent material field, be specifically related to a kind of manganese ion activated fluosilicate red fluorescence powder and system thereof
Preparation Method.
Background technology
Light emitting diode (LED) is a kind of semiconductor electronic component converting electrical energy into luminous energy.This electronic component is as far back as 1962
Year occurs, can only send the HONGGUANG of low luminosity in early days, develop other monochromatic versions, the light that can send even to this day afterwards
Throughout visible ray, infrared ray and ultraviolet, range is also raised to higher level, is referred to as " forth generation light source ".Due to
It has the advantages such as energy-saving and environmental protection, safety, life-span length, has been widely used in the various aspects in industry and life, bag
Include instruction, show, decorate, the field such as backlight, general lighting.
For the white LED lamp that application is wide, the method realizing white light LEDs at present mainly has three kinds: (1) is in indigo plant
Optical chip yellow fluorescent powder applied over, mainly YAG:Ce, utilize blue light and gold-tinted to be mixed into white light；(2) by red, green,
The chip portfolio encapsulation of blue three-color, the luminescence of chip institute is directly mixed into white light；(3) with black light chip excite red, green,
The fluorescent material of blue three-color is mixed into white light.In these three method, the 1st kind of method is that presently most maturation is also main flow
Method, but the product color rendering index of the method is on the low side, typically about 70, colour temperature is higher, generally at more than 5500K, with
The optimum visual of human eye requires to there is certain deviation, it is therefore desirable to mix a certain amount of red fluorescence powder.And other two kinds of methods are also
Need to use red fluorescence powder, to send required HONGGUANG.In addition, in many other kinds of LED light sources or device
Also red fluorescence powder can be used.Therefore, there is the bigger market demand for red fluorescence powder in LED industry.
Summary of the invention
It is an object of the invention to provide a kind of manganese ion activated fluosilicate red fluorescence powder and preparation method thereof.
The above-mentioned purpose of the present invention is achieved by techniques below scheme:
A kind of fluosilicate red nano-fluorescent powder, its chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x span is
0.06～0.20, it is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Changing sodium, silicic acid and the mixture of manganese dioxide, wherein, x span is 0.06～0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in reducing atmosphere and 1300～1500 DEG C of conditions in high temperature furnace
Lower sintering 3～5 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.6～0.8% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid,
The weight ratio of sodium sulfide and boric acid is 5～7:1.
Further, described fluosilicate red nano-fluorescent powder, its chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x
Value 0.10, is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.10；
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 4 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 6:1.
Further, described fluosilicate red nano-fluorescent powder, its chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x
Value 0.06, is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.06；
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 1300 DEG C
Tie 5 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.6% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 5:1.
Further, described fluosilicate red nano-fluorescent powder, its chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x
Value 0.20, is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.20；
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 3 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 7:1.
Further, described reducing atmosphere is Carbon monoxide reduction atmosphere.
Advantages of the present invention:
The fluosilicate red nano-fluorescent powder good dispersion that the present invention provides, luminous intensity is high, and stability is high, these advantages with
In flux, sodium sulfide is relevant with boric acid weight ratio, and when the weight ratio of sodium sulfide and boric acid is 5～7:1, 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 fluosilicate red nano-fluorescent powder
Chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.10；
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 4 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 6:1.
Embodiment 2: the preparation of fluosilicate red nano-fluorescent powder
Chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x value 0.06, it is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.06；
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 1300 DEG C
Tie 5 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.6% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 5:1.
Embodiment 3: the preparation of fluosilicate red nano-fluorescent powder
Chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x value 0.20, it is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.20；
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 3 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 7:1.
Embodiment 4: the preparation of fluosilicate red nano-fluorescent powder
Chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.10；
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 4 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 5:1.
Embodiment 5: the preparation of fluosilicate red nano-fluorescent powder
Chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.10；
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 4 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 7:1.
The weight ratio of embodiment 6: comparative example, sodium sulfide and boric acid is 4:1
Chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.10；
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 4 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 4:1.
The weight ratio of embodiment 7: comparative example, sodium sulfide and boric acid is 8:1
Chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x value 0.10, it is made by the steps and forms:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.10；
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 4 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 8:1.
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 | 99 | More stable | Dispersibility is preferable |
| Embodiment 5 | 99 | More stable | Dispersibility is preferable |
| Embodiment 6 | 73 | Unstable | Poor dispersion |
| Embodiment 7 | 73 | Unstable | Poor dispersion |
The test result of embodiment 2,3 is basically identical with embodiment 4,5.
Above-mentioned test result indicate that, the fluosilicate red nano-fluorescent powder good dispersion that the present invention provides, luminous intensity is high, surely
Qualitative height, these advantages are relevant with sodium sulfide in flux and boric acid weight ratio, when the weight ratio of sodium sulfide and boric acid is 5～7:1,
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. a fluosilicate red nano-fluorescent powder, its chemical composition is Mg1-xSiO2F2:xMn2+；Wherein, x span
It is 0.06～0.20, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Changing sodium, silicic acid and the mixture of manganese dioxide, wherein, x span is 0.06～0.20；
Step S2, adds flux and is ground, be ground and obtain mixture；
Step S3, mixture step S2 obtained loads crucible, in reducing atmosphere and 1300～1500 DEG C of conditions in high temperature furnace
Lower sintering 3～5 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.6～0.8% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid,
The weight ratio of sodium sulfide and boric acid is 5～7:1.
Fluosilicate red nano-fluorescent powder the most according to claim 1, its chemical composition is Mg1-xSiO2F2:xMn2+；
Wherein, x value 0.10, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.10；
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 4 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.7% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 6:1.
Fluosilicate red nano-fluorescent powder the most according to claim 1, its chemical composition is Mg1-xSiO2F2:xMn2+；
Wherein, x value 0.06, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.06；
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 1300 DEG C
Tie 5 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.6% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 5:1.
Fluosilicate red nano-fluorescent powder the most according to claim 1, its chemical composition is Mg1-xSiO2F2:xMn2+；
Wherein, x value 0.20, it is characterised in that be made by the steps and form:
Step S1, by chemical composition Mg1-xSiO2F2:xMn2+Stoichiometric proportion weigh raw material, described raw material is magnesium carbonate, fluorine
Change sodium, silicic acid and the mixture of manganese dioxide, wherein, x value 0.20；
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 3 hours, cool down and i.e. obtain described fluosilicate red nano-fluorescent powder；
Wherein, the addition of flux is the 0.8% of raw material weight, and described flux is the mixture of sodium sulfide and boric acid, sulfuration
The weight ratio of sodium and boric acid is 7:1.
5. according to the arbitrary described fluosilicate red nano-fluorescent powder of Claims 1 to 4, it is characterised in that: described reducing atmosphere
For Carbon monoxide reduction atmosphere.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773832A (en) * | 2021-10-15 | 2021-12-10 | 烟台布莱特光电材料有限公司 | Fluosilicate red fluorescent powder and preparation method thereof |
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| CN101100605A (en) * | 2007-07-13 | 2008-01-09 | 中山大学 | Alkaline earth halogen silicate phosphor powder and preparation method thereof |
| CN104877675A (en) * | 2015-05-12 | 2015-09-02 | 岭南师范学院 | Mixed-valence-state europium (Eu) ion doped single-matrix color-adjustable fluorescent powder and preparation method thereof |
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2016
- 2016-06-29 CN CN201610494572.9A patent/CN105950139A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100605A (en) * | 2007-07-13 | 2008-01-09 | 中山大学 | Alkaline earth halogen silicate phosphor powder and preparation method thereof |
| CN104877675A (en) * | 2015-05-12 | 2015-09-02 | 岭南师范学院 | Mixed-valence-state europium (Eu) ion doped single-matrix color-adjustable fluorescent powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113773832A (en) * | 2021-10-15 | 2021-12-10 | 烟台布莱特光电材料有限公司 | Fluosilicate red fluorescent powder and preparation method thereof |
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