CN105018078B - Luminescent material Mg3SiO4F2 and preparation method thereof - Google Patents
Luminescent material Mg3SiO4F2 and preparation method thereof Download PDFInfo
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- CN105018078B CN105018078B CN201410167052.8A CN201410167052A CN105018078B CN 105018078 B CN105018078 B CN 105018078B CN 201410167052 A CN201410167052 A CN 201410167052A CN 105018078 B CN105018078 B CN 105018078B
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- 239000000463 material Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 230000005284 excitation Effects 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 54
- 239000007789 gas Substances 0.000 claims description 45
- 229910052909 inorganic silicate Inorganic materials 0.000 claims description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 34
- 239000012298 atmosphere Substances 0.000 claims description 31
- 229910052786 argon Inorganic materials 0.000 claims description 27
- 229910052681 coesite Inorganic materials 0.000 claims description 17
- 229910052906 cristobalite Inorganic materials 0.000 claims description 17
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 17
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- 229910052682 stishovite Inorganic materials 0.000 claims description 17
- 229910052905 tridymite Inorganic materials 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 10
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims 2
- 239000007790 solid phase Substances 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 description 34
- 239000000843 powder Substances 0.000 description 25
- 238000005245 sintering Methods 0.000 description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 10
- 238000001228 spectrum Methods 0.000 description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000005286 illumination Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 238000004020 luminiscence type Methods 0.000 description 6
- 239000012925 reference material Substances 0.000 description 6
- 238000001354 calcination Methods 0.000 description 5
- 229910052855 humite Inorganic materials 0.000 description 5
- 229910001428 transition metal ion Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 241001025261 Neoraja caerulea Species 0.000 description 3
- 244000154870 Viola adunca Species 0.000 description 3
- 235000005811 Viola adunca Nutrition 0.000 description 3
- 235000013487 Viola odorata Nutrition 0.000 description 3
- 235000002254 Viola papilionacea Nutrition 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- -1 rare-earth ions Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 244000172533 Viola sororia Species 0.000 description 1
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Abstract
The invention relates to a luminescent material Mg3SiO4F2 and a preparation method thereof. The luminescent material Mg3SiO4F2 is obtained by high-temperature solid-phase roasting; and visible light is emitted under the excitation of ultraviolet light at the wavelength of 250-275 nm, and emission peaks of the luminescent material Mg3SiO4F2 include at least one of 350-415 nm, 500-520 nm and 712-740 nm.
Description
Technical field
The present invention relates to a kind of luminescent material and preparation method thereof is and in particular to a kind of luminescent material Mg3SiO4F2And its system
Preparation Method.
Background technology
In illumination market, white light LEDs are to develop one of technology the swiftest and the most violent in recent years.(incandescent with traditional lighting mode
Osram lamp and fluorescent lamp) compare, LED has small volume (many, multiple combination), caloric value low (not having thermal radiation), power consumption
Measure little (low-voltage, low current start), life-span length (more than 10,000 hours), (shatter-proof, impact resistance is not fragile, discarded object can return for environmental protection
Receive, not do not pollute), can planar package easy exploiting the advantages of become compact product.
State-of-the art mainly by two ways realize white light LEDs (see Fig. 1) (S.Ye, etc.,
Mater.Sci.Eng.,R,2010,71,1-34)：The first is multi-chip type white light LEDs, via two kinds or more differences of combination
The LED combination of coloured light is to form white light；Equations of The Second Kind be using fluorescent material by blue-ray LED or blue light produced by UV-LED or
Ultraviolet light is respectively converted into dual wavelength or three wavelength white lights, and technique is referred to as fluorescent material conversion of white light LED (Phosphor
Converted-LED).White light LEDs commodity are the most universal with blue-light LED chip collocation yellow fluorescent powder in the market, but closely
The application increasing prevalence of Nian Lai, ruddiness and green light fluorescent powder.If it is for backlight, blue, green and red assorted light
Spectrum is separated from each other, and color representation improves；And in lighting use, then need to be formed wavelength be 500nm about to 650nm,
The continuous spectrum close with sunshine.In the generation of white light LEDs, red light fluorescent powder is except for glimmering with blue-ray LED and green glow
The cooperation of light powder produces outside white light, also can produce white light with green, blue light fluorescent powder and purple light or ultraviolet LED cooperation, also can be used for mending
Repay " YAG:The ruddiness lacking in Ce+ blue-ray LED ", to improve colour rendering index or to reduce colour temperature.
The existing method preparing fluorescent material mostly is the conducts such as expensive rare earth luminous ion or transition metal ions of adulterating
The centre of luminescence (S.Ye, etc., Mater.Sci.Eng., R, 2010,71,1-34), increased the manufacturing cost of fluorescent material, no
Popularization and application beneficial to LED.Thus, research and development novel high-performance, red, the green fluorescence powder of low cost meet LED technology growth requirement and
Trend, and be conducive to lifting the whole competitiveness in LED fluorescent powder and illuminating device for the China, wherein red light fluorescent powder is glimmering with green glow
Light powder becomes new research and development focus after yellow fluorescent powder.
Content of the invention
It is contemplated that overcoming the shortcoming of prior art, the invention provides a kind of advanced luminescent material Mg3SiO4F2And its
Preparation method.
The invention provides a kind of luminescent material Mg3SiO4F2, described luminescent material Mg3SiO4F2By high temperature solid-state roasting
Mode obtain；Visible ray, described luminescent material Mg is launched under the ultraviolet excitation of 250-275nm wavelength3SiO4F2Send out
Penetrate peak and include at least one of 350-415nm, 500-520nm and 712-740nm.
Described luminescent material can be applicable to field of LED illumination, mixes acquisition white light with other fluorescent material.When emission peak exists
During 350-415nm scope, described luminescent material can be used as royal purple emitting phosphor；Send out described in when emission peak is in 500-520nm scope
Luminescent material can be used as green light fluorescent powder；When emission peak is in 712-740nm scope, described luminescent material can be used as red light fluorescent powder.
The material emission center of the present invention may be from internal colour center or chemical imperfection, also referred to as intrinsic luminescent material.
The present invention also provides one kind to prepare described luminescent material Mg3SiO4F2Method, methods described includes raw material
MgF2, SiO2, MgO in molar ratio 1:1:2 dry mixed uniformly, carry out high temperature solid-state roasting, during roasting at 1000-1500 DEG C
Between be 2-6 hour, finally cool to room temperature with the furnace, described luminescent material after grinding, can be obtained.
It is preferred that described roasting can be carried out under argon gas atmosphere or argon gas/hydrogen mixed gas atmosphere.
It is preferred that described roasting under an argon atmosphere, roasting can be carried out in electric furnace, can first will take out in electric furnace very during roasting
Sky, is then charged with high-purity argon gas, and gas pressure can be maintained to be 0.2-0.4MPa.
It is preferred that described roasting under argon gas/hydrogen mixed gas atmosphere, the percent by volume of argon gas in described mixed gas
Can be 5%, roasting is carried out in electric furnace, first vacuumizes in electric furnace during roasting, is then charged with high-purity argon gas/hydrogen mixed gas,
Gas pressure can be maintained to be 0.2-0.4MPa.
One preferred embodiment of methods described is to be evacuated to 10Pa in described electric furnace.
Under different calcination atmospheres, can achieve the regulation and control to luminescent material luminous peak position or color.
Beneficial effects of the present invention：
Compared with prior art, the fluorescent material of present invention preparation, the rare earth luminous ion of costliness of need not adulterating or transition
Metal ion etc. as the centre of luminescence, by changing roasting system, achievable blue violet light (380-410nm), green glow (520nm),
Ruddiness (720/740nm) is launched, can be used as the one-color fluorescence powder (as green powder 520nm) in field of LED illumination and other fluorescent material
Mixing obtains white light.Mg due to the present invention3SiO4F2Fluorescent material need not adulterate costliness rare earth luminous ion or transition metal
Ion, as the centre of luminescence, is conducive to Simplified flowsheet, cost-effective, meets the demand for development of advanced luminescent material, is suitable for industry
Metaplasia is produced, and can be used for White-light LED illumination field.
Brief description
Fig. 1 mainly realizes the mode of white light LEDs for two kinds of state-of-the art；
Fig. 2 is roasting gained luminescent material Mg at 1150 DEG C of air atmosphere3SiO4F2Luminous collection of illustrative plates；
Fig. 3 is roasting gained luminescent material Mg at 1150 DEG C of air atmosphere3SiO4F2XRD spectrum；
Fig. 4 is the lower 1300 DEG C of roasting gained luminescent material Mg of Ar atmosphere3SiO4F2Luminous collection of illustrative plates；
Fig. 5 is Ar/H2The lower 1300 DEG C of roasting gained luminescent material Mg of atmosphere3SiO4F2Luminous collection of illustrative plates.
Specific embodiment
Be described in further detail by detailed description below and referring to the drawings to the present invention it is thus understood that, below
Embodiment is only the description of the invention, is not the restriction to present invention, any does not make substance to present invention
The technical scheme of change still falls within protection scope of the present invention.
The invention discloses a kind of new luminescent material Mg3SiO4F2And preparation method thereof, described luminescent material is a kind of
Without doping with rare-earth ions, as the fluorescent material of light emitting ionic, its centre of luminescence may be from interior transition metal ions etc.
Portion's colour center or chemical imperfection, also referred to as intrinsic luminescent material.The preparation process of this luminescent material is:Mg will be constituted3SiO4F2Former
Material MgF2, SiO2, MgO stoichiometrically, i.e. mol ratio 1:1:2 dry mixed are uniform, in air atmosphere or argon gas atmosphere or argon
It is sintered under gas/hydrogen mixed gas atmosphere, sintering temperature scope is 1000-1500 DEG C, roasting time 2-6h, last along with the furnace cooling
To room temperature.According to the difference of calcination atmosphere, the luminescent material obtained by the present invention is in the ultraviolet excitation of 250-275nm wavelength
Under, launch visible ray, luminous peak position includes 386nm (bluish violet), 500-520nm (green), and 710-760nm (red) three
Main emission peak.The luminous expensive rare earth ion that need not adulterate of this material is it is not required that the other such as containing transition metal is sent out
Photoion, is conducive to simplifying preparation technology and cost-effective, meets the demand for development of advanced luminescent material, prepared
Mg3SiO4F2Fluorescent material can be applicable to illuminating material or other field of photoelectric material.
This material is a kind of LED fluorescent material of burst of ultraviolel, can be applicable to White-light LED illumination field etc., can conduct
One-color fluorescence powder (as green powder 520nm) in field of LED illumination mixes acquisition white light with other fluorescent material.
For achieving the above object, the technical solution used in the present invention is as follows：
A kind of new luminescent material Mg3SiO4F2And preparation method thereof, it is a kind of golden without doping with rare-earth ions or transition
The ultraviolet excited fluorescence material of the centres of luminescence such as genus；
As a kind of preferred version, described fluorescent material Mg3SiO4F2Preparing raw material be MgF2, SiO2, MgO.And it is each
The mol ratio of composition compares 1 for standard stoichiometry:1:2；
A kind of new luminescent material Mg3SiO4F2And preparation method thereof, by raw material MgF2, SiO2, MgO in molar ratio 1:1:
2 dry mixed uniformly, are sintered, sintering temperature is under air atmosphere or argon gas atmosphere or argon gas/hydrogen mixed gas atmosphere
1000-1500 DEG C, roasting time 2-6h, finally cool to room temperature with the furnace, final sample after grinding, can be obtained.
As a kind of preferred version, using high temperature solid-state method of roasting, at a temperature of 1000-1500 DEG C, it is incubated 2-6h,
After cool to room temperature with the furnace, grind.
As a kind of preferred version, in described high temperature solid-state roasting process, any atmosphere can not be passed through, that is, in air
Sinter under atmosphere, sintering temperature is 1000-1500 DEG C, roasting time 2-6h finally cools to room temperature with the furnace, can obtain after grinding
Whole sample.
As a kind of preferred version, during the high temperature solid-phase sintering described in structure, high-purity argon gas can be passed through as sintering
Atmosphere.Now, first will be evacuated to 10Pa in electric furnace, be then charged with high-purity argon gas, pressure is 0.2-0.4MPa, roasting
Temperature is 1000-1500 DEG C, and roasting time 2-6h finally cools to room temperature with the furnace, can obtain final sample after grinding.
As a kind of preferred version, in described high temperature solid-state roasting process, high-purity argon gas/hydrogen mixing can be passed through
Gas (hydrogen 5% volume ratio) is as calcination atmosphere.Now, first will be evacuated to 10Pa in electric furnace, be then charged with high-purity mixed
Close gas, pressure is 0.2-0.4MPa, sintering temperature is 1000-1500 DEG C, roasting time 2-6h finally cools to room temperature with the furnace,
Final sample can be obtained after grinding.
The method that the present invention passes through high temperature solid-state roasting, obtains a kind of novel fluorescent material Mg3SiO4F2, and by changing
Become roasting system, it is possible to obtain can launch blue violet light (380-410nm), green glow (520nm), ruddiness (720/740nm) new
Fluorescent material.Under different calcination atmospheres, can achieve the regulation and control to luminescent material luminous peak position (or color).
Fig. 2 is roasting gained luminescent material Mg at 1150 DEG C of air atmosphere3SiO4F2Luminous collection of illustrative plates (embodiment 1)；Can
See, the transmitting peak position of the phosphor material powder obtained by the present embodiment is in 500nm (green glow) and 712nm (ruddiness).
Fig. 3 is roasting gained luminescent material Mg at 1150 DEG C of air atmosphere3SiO4F2XRD spectrum (embodiment 1)；With mark
The PDF card 71-2401 of quasi- thing phase coincide preferably, illustrates that the fluorescent material synthesizing has Mg3SiO4F2Crystal structure, i.e. humite
Structure.
The lower 1300 DEG C of roasting gained luminescent material Mg of Fig. 4 Ar atmosphere3SiO4F2Luminous collection of illustrative plates (embodiment 2)；It can be seen that, this
The transmitting peak position of the phosphor material powder obtained by embodiment, in 500nm (green glow) and 714nm (ruddiness), is wherein launched with 714nm
Based on peak.
Fig. 5 Ar/H2The lower 1300 DEG C of roasting gained luminescent material Mg of atmosphere3SiO4F2Luminous collection of illustrative plates (embodiment 3)；Can
See, the emission peak of the phosphor material powder obtained by the present embodiment is the wide range transmitting positioned at 350-415nm (blue light), exists simultaneously
520nm and 720nm about also occur in that emission peak.
Include some exemplary embodiments further below so that the present invention is better described.It should be understood that the present invention is detailed
The above-mentioned embodiment stated, and following examples are only illustrative of the invention and is not intended to limit the scope of the invention, this area
Technical staff made according to the above of the present invention some nonessential improve and adjustment belongs to the protection of the present invention
Scope.In addition, concrete proportioning in following technological parameters, time, temperature etc. are also only exemplary, those skilled in the art are permissible
Suitable value is selected in the range of above-mentioned restriction.
Embodiment 1
By MgF2,SiO2, MgO in molar ratio 1:1:2, being converted into mass ratio is MgF2:SiO2:MgO=3.1:3:4 weigh
And dry mixed is uniform.Above-mentioned mixed material is put in electric furnace, roasting 4h at 1150 DEG C of air atmosphere, along with the furnace cooling is to room
Temperature, takes out and grinds.
Fig. 2 is fluorescent material Mg obtained by embodiment 13SiO4F2Luminous collection of illustrative plates it is seen then that glimmering obtained by the present embodiment
The transmitting peak position of light powder material is in 500nm (green glow) and 712nm (ruddiness).Fig. 3 is fluorescent material Mg3SiO4F2XRD spectrum,
It coincide preferably with the PDF card 71-2401 of reference material phase, illustrate that the fluorescent material synthesizing has Mg3SiO4F2Crystal structure, i.e. silicon
Magnesite structure.
Embodiment 2
By MgF2,SiO2, MgO in molar ratio 1:1:2, being converted into mass ratio is MgF2:SiO2:MgO=3.1:3:4 weigh
And dry mixed is uniform.Above-mentioned raw materials are put in electric furnace, is passed through high-purity argon gas as calcination atmosphere.Now, first by electric furnace
It is evacuated to 10Pa, is then charged with high-purity argon gas, pressure is 0.2-0.4MPa, sintering temperature is 1300 DEG C, roasting time
2h, finally cools to room temperature with the furnace, can obtain final sample after grinding.
Fig. 4 is fluorescent material Mg obtained by embodiment 23SiO4F2Luminous collection of illustrative plates it is seen then that glimmering obtained by the present embodiment
The transmitting peak position of light powder material in 500nm (green glow) and 714nm (ruddiness), wherein based on 714nm emission peak.This fluorescent material
Mg3SiO4F2The PDF card 71-2401 of XRD spectrum and reference material phase coincide preferably, i.e. humite structure.
Embodiment 3
By MgF2,SiO2, MgO in molar ratio 1:1:2, being converted into mass ratio is MgF2:SiO2:MgO=3.1:3:4 weigh
And dry mixed is uniform.Above-mentioned raw materials are put in electric furnace, is passed through high-purity argon gas/hydrogen (5% volume ratio) gaseous mixture as roasting
Burn atmosphere.Now, first will be evacuated to 10Pa in electric furnace, be then charged with high-purity argon gas/hydrogen mixed gas, pressure is 0.2-
0.4MPa, sintering temperature is 1300 DEG C, and roasting time 2h finally cools to room temperature with the furnace, can obtain final sample after grinding.
Fig. 5 is fluorescent material Mg obtained by embodiment 33SiO4F2Luminous collection of illustrative plates it is seen then that glimmering obtained by the present embodiment
The emission peak of light powder material be positioned at 350-415nm (blue light) wide range transmitting, simultaneously in 520nm and 720nm about also occur
Emission peak.This fluorescent material Mg3SiO4F2The PDF card 71-2401 of XRD spectrum and reference material phase coincide preferably, i.e. silicon magnesium
Stone structure.
Embodiment 4
By MgF2,SiO2, MgO in molar ratio 1:1:2, being converted into mass ratio is MgF2:SiO2:MgO=3.1:3:4 weigh
And dry mixed is uniform.Above-mentioned raw materials are put in electric furnace, in air atmosphere, roasting 2h at 1500 DEG C, along with the furnace cooling is to room
Temperature；Take out and grind.
The emission peak of obtained phosphor material powder is located at 500nm and 712nm, and fluorescent material Mg3SiO4F2's
XRD spectrum is identical with the PDF card 71-2401 of reference material phase preferably, i.e. humite structure.
Embodiment 5
By MgF2,SiO2, MgO in molar ratio 1:1:2, being converted into mass ratio is MgF2:SiO2:MgO=3.1:3:4 weigh
And dry mixed is uniform.Above-mentioned raw materials are put in electric furnace, is passed through high-purity argon gas as sintering atmosphere.Now, first by electric furnace
Take out black vacuum to 10Pa, be then charged with high-purity argon gas, pressure is 0.2-0.4MPa, and sintering temperature is 1200 DEG C, during sintering
Between 3h, finally cool to room temperature with the furnace, final sample after grinding, can be obtained.
The emission peak of obtained phosphor material powder be located at 500nm (green glow) and about 714nm (ruddiness), wherein with
Based on 714nm emission peak.This fluorescent material Mg3SiO4F2The PDF card 71-2401 of XRD spectrum and reference material phase coincide relatively
Good, i.e. humite structure.
Embodiment 6
By MgF2,SiO2, MgO in molar ratio 1:1:2, being converted into mass ratio is MgF2:SiO2:MgO=3.1:3:4 weigh
And dry mixed is uniform.Above-mentioned raw materials are put in electric furnace, is passed through high-purity argon gas/hydrogen (5% volume ratio) gaseous mixture as roasting
Burn atmosphere.Now, first will be evacuated to 10Pa in electric furnace, be then charged with high-purity argon gas/hydrogen mixed gas, pressure is 0.2-
0.4MPa, sintering temperature is 1000 DEG C, and roasting time 6h finally cools to room temperature with the furnace, can obtain final sample after grinding.
The emission peak of obtained phosphor material powder is the wide range transmitting positioned at 350-415nm (blue violet light), exists simultaneously
520nm and 720nm about also occur in that emission peak.This fluorescent material Mg3SiO4F2XRD spectrum and reference material phase PDF card
71-2401 coincide preferably, i.e. humite structure.
The Mg of the present invention3SiO4F2Fluorescent material need not adulterate costliness rare earth luminous ion or transition metal ions conduct
The centre of luminescence, is conducive to Simplified flowsheet, cost-effective, meets the demand for development of advanced luminescent material, and suitable industrialized production can
For White-light LED illumination field.
Claims (6)
1. a kind of luminescent material Mg3SiO4F2It is characterised in that described luminescent material Mg3SiO4F2By high temperature solid-state roasting
Mode obtains；Visible ray, described luminescent material Mg is launched under the ultraviolet excitation of 250-275 nm wavelength3SiO4F2Transmitting
Peak includes at least one of 350-415 nm, 500-520 nm and 712-740 nm.
2. one kind prepares luminescent material Mg described in claim 13SiO4F2Method it is characterised in that methods described include will be former
Material MgF2、SiO2, MgO in molar ratio 1: 1:2 dry mixed uniformly, carry out high temperature solid-state roasting at 1000-1500 DEG C, roasting
The burning time is 2-6 hour, finally cools to room temperature with the furnace, can obtain described luminescent material after grinding.
3. method according to claim 2 is it is characterised in that described roasting is in argon gas atmosphere or argon gas/hydrogen mixed gas
Carry out under atmosphere.
4. method according to claim 3 it is characterised in that described roasting under an argon atmosphere, enter in electric furnace by roasting
OK, first vacuumize in electric furnace during roasting, be then charged with high-purity argon gas, maintenance gas pressure is 0.2-0.4MPa.
5. method according to claim 3 is it is characterised in that described roasting under argon gas/hydrogen mixed gas atmosphere, described
In mixed gas, the percent by volume of argon gas is 5%, and roasting is carried out in electric furnace, first vacuumizes in electric furnace, Ran Houchong during roasting
Enter high-purity argon gas/hydrogen mixed gas, maintenance gas pressure is 0.2-0.4 MPa.
6. the method according to claim 4 or 5 is it is characterised in that be evacuated to 10Pa in described electric furnace.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6592696B1 (en) * | 1998-10-09 | 2003-07-15 | Motorola, Inc. | Method for fabricating a multilayered structure and the structures formed by the method |
| CN102391859A (en) * | 2011-12-02 | 2012-03-28 | 福州大学 | Green fluorescent powder for white LED (light-emitting diode) use, its preparation method and application |
| CN103525415A (en) * | 2013-10-08 | 2014-01-22 | 长春理工大学 | 1064nm lead fluoride based up-conversion luminescence material and preparation method thereof |
-
2014
- 2014-04-24 CN CN201410167052.8A patent/CN105018078B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6592696B1 (en) * | 1998-10-09 | 2003-07-15 | Motorola, Inc. | Method for fabricating a multilayered structure and the structures formed by the method |
| CN102391859A (en) * | 2011-12-02 | 2012-03-28 | 福州大学 | Green fluorescent powder for white LED (light-emitting diode) use, its preparation method and application |
| CN103525415A (en) * | 2013-10-08 | 2014-01-22 | 长春理工大学 | 1064nm lead fluoride based up-conversion luminescence material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| "Importance of Crystallization Hierarchies in Microstructural Evolution of Silicate Glass–Ceramics";W. E. Lee et al.，;《J. Am. Ceram. Soc.》;20070331;第90卷(第3期);第727–737页 * |
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