CN106318382A - Nitride red steady persistence material and preparing method thereof - Google Patents
Nitride red steady persistence material and preparing method thereof Download PDFInfo
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Abstract
Chemical composition formula of a nitride red steady persistence material is: MnSi7- 3(x+y)A14XGa4yN12:C. D, wherein, M is one of or multiple Ca, Sr, Mg, Li and Y, C is Ce3+ or Eu2+, and D is one of or multiple Dy3+, Tm3+, Ho3+ and Nd3+, 0.7<=x<=1.3 and 0<=y<=0.2. n varies with the value of x and y as well as valence state of M, which is fixed and satisfies the valence state conservation. The nitride red steady persistence material is prepared from the steps of calculating and measuring each raw material based on formula according to stoichiometric ratio of each element, then mixing them in glove box, under the nitrogen atmosphere and the pressure of 0. 8- 1. 0Mpa with the temperature rate within 5oC/min heating the mixture to 800oC and preserving heat for 30min, then heating the it to 1,600oC and preserving heat for 30min, finally heating it to 1,750 -2,000oC and preserving heat for 1h, and cooling it to the room temperature with the furnace. After the illumination by ultraviolet light or visible light, the invention will emit continuous and visible red persistence with the persistence time reaching 60min -150min, higher heat stability and chemical stability.
Description
Technical field
The invention belongs to luminescent material technical field, relate to a kind of nitride red long after glow luminous material and preparation side thereof
Method.
Background technology
Long after glow luminous material is a class embedded photoluminescent material, through the short irradiation of the light source such as daylight and long wave ultraviolet
After, a part of luminous energy is stored, after closing light source, remains to continue to release with the form of visible ray lentamente within a very long time
Put this portion of energy.The purposes of long after glow luminous material is quite varied, in addition to as luminous mark material, as emergency access
Illumination, fire direction board etc. other need on weak illumination instruction equipment, the most energy-conservation environmental protection again, it is also possible to be applied to optoelectronic information
Field (high energy particle and defect damage detector, three-dimensional information storage etc.).It addition, some long-afterglow materials are alternatively arranged as fluorescence
Powder is in the LED, and especially AC LED, it has the characteristic of transmitting can effectively solve in exchange in a period of time after excitation
Stroboscopic (degree of depth of stroboscopic i.e. electric light source luminous flux fluctuation, the fluctuation degree of depth is the biggest, and the stroboscopic degree of depth is the biggest) problem present in LED.
Traditional long-afterglow material mainly has zinc sulfide and calcium sulfide fluorophor.Since the nineties in 20th century, Eu2+Aluminates system and
Silicate systems becomes the main body of long after glow luminous material, and this two classes long after glow luminous material is in luminosity, persistence, change
Learn stability aspect and be better than the long-afterglow material of conventional vulcanized objects system.The glow color one of this two classes long after glow luminous material
As be green, blue, aeruginous.The long-afterglow material of the longwave transmissions in long after glow luminous material, has special optical
Matter, has BELAND, green short-wavelength afterglowing material broader practice prospect in low light illuminant and emergent instruction.But Eu2+Aluminum
More than Yellow light-emitting low temperature the most a small amount of in hydrochlorate oxide system and silicate oxide system long after glow luminous material and the length of HONGGUANG
Brightness material, and with other commerciality long-afterglow materials compare, great majority have poor chemical stability, luminous intensity low and lasting time
Between short feature, it is difficult to meet and be actually needed.Therefore, study a kind of novel effective red long afterglow material to be highly desirable to.
The advantages such as additionally, nitride is due to its Stability Analysis of Structures, chemical stability is good, and covalency is strong, have good application prospect.
Patent " orange-yellow long-afterglow luminescent material and production method " (application number ZL200410020722.X, notification number
CN1266250, day for announcing 2006.07.26) and patent " red rare-earth phosphorescent body with long afterglow " (patent No. ZL02125512.1, public
Announcement CN1216125, day for announcing 2005.08.24) disclose the long after glow luminous material with sulfide as substrate, but these are long
The preparation technology of afterglow material is more complicated, and easily produces the harmful gas of sulfur-bearing in preparation process, can be to human body
Work the mischief with environment.Patent " orange-yellow long persistence phosphor and preparation method thereof " (patent No. 200710056035.7, bulletin
Number CN100575452, day for announcing 2009.12.30) disclose with Eu2+Orange-yellow long-afterglow luminescent material for active ions
SrSiO5:Eu2+, Dy3+, this materials synthesis difficulty stability is bad, is unfavorable for that industrialization produces.
Summary of the invention
The present invention provides a kind of nitride red long after glow luminous material, can produce red long under 250-600nm excites
Twilight sunset, reaches 60min-150min persistence, and its granule is in the bulk of rule.
It is a further object to provide the preparation method of above-mentioned long-afterglow material, pressure is 0.8-1.0Mpa, temperature
Obtain, at spending 1750 DEG C-2000 DEG C, the red long afterglow material that a kind of performance is more stable.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of nitride red long-afterglow material, its chemical constitution formula is MnSi7-3(x+y)Al4xGa4yN12: C. D, wherein M is
Ca2+, Sr2+, Mg2+, Li+, Y3+One or more, C is Ce3+Or Eu2+, D is Dy3+, Tm3+, Ho3+, Nd3+In
One, 0.7≤x≤1.3,0≤y≤0.2, n changes along with the value of x, the value of y and the variation of valence of M, its value fix and
Meet valence state conservation.
The excitation spectrum scope of this nitride red long-afterglow material is at 250nm-600nm, and emission spectrum is that wide bag is launched,
Its peak value is adjustable at 590-670nm, and halfwidth is 70-90nm.
Its structure is monocline Cmc21 (no. 36), RN4, R=Al, Si, Ga, tetrahedron concurrent connects and composes substantially
Skeleton, cation Ca2+, Sr2+, Mg2+, Li+, Y3+One or more be present among gap as charge compensation.
Another technical scheme of the present invention is: the preparation side of a kind of nitride red long after glow luminous material
Method, specifically sequentially includes the following steps:
Step 1: according to chemical constitution formula MnSi7-3(x+y)Al4xGa4yN12: C. D, wherein M is Ca2+, Sr2+, Mg2+, Li+,
Y3+One or more, C is Ce3+Or Eu2+, D is Dy3+, Tm3+, Ho3+, Nd3+In one, 0.7≤x≤1.3,0≤y
≤ 0.2, n change along with the value of x, the value of y and the variation of valence of M, and its value is fixed and meets valence state conservation；By each element
Stoichiometric proportion calculates and weighs and includes AlN, Si3N4, GaN, and Ca3N2、 Sr3N2、 Mg3N2、 Li3One in N, YN or
Multiple, DCl3, CCl3Consumption.
Step 2: than calculating and weigh each raw material dosage, by this raw material by the metering of each element chemistry according to above-mentioned composition formula
Glove box mixes, under nitrogen atmosphere, 0.8-1.0Mpa pressure, within 5 DEG C/min of heating rate, mixture is heated
To 800 DEG C, it is incubated 30min, is then heated to 1600 DEG C, be incubated 30min, finally heated to 1750-2000 DEG C, be incubated 1h,
Cool to room temperature with the furnace.
Step 3: the powder body obtained by step 2 is ground, obtains nitride red long-afterglow material powder body.
The present invention, after ultraviolet light or radiation of visible light, can send the most visible red twilight sunset, reach persistence
60min-150min, the twilight sunset spectrum of this afterglowing material has longer wavelength (590-670nm), and within the specific limits can be real
Now wavelength is adjustable, has higher heat stability and chemical stability simultaneously.Can be effectively used for luminous mark material, optical telecommunications
Breath, WLEDs field etc..
Accompanying drawing explanation
Fig. 1 is XRD figure spectrum (a) of the long after glow luminous material that the embodiment of the present invention 1 prepares, SEM figure (b), excites and send out
Penetrate figure (c), decay of afterglow curve chart (d)；
Fig. 2 is XRD figure spectrum (a) of the long after glow luminous material that the embodiment of the present invention 2 prepares, SEM figure (b), excites and transmitting figure
(c), decay of afterglow curve chart (d)；
Fig. 3 is XRD figure spectrum (a) of the long after glow luminous material that the embodiment of the present invention 3 prepares, SEM figure (b), excites and transmitting figure
(c), decay of afterglow curve chart (d)；
Fig. 4 is XRD figure spectrum (a) of the long after glow luminous material that embodiment 4 prepares, SEM figure (b), excite and transmitting figure (c), remaining
Brightness attenuation curve figure (d)；
Fig. 5 is gained electromagnetic radiation wavelength of the present invention and graph of a relation persistence.
Detailed description of the invention
A kind of nitride red long-afterglow material, its chemical constitution formula is: MnSi7-3(x+y)Al4xGa4yN12: C. D, wherein
M is Ca2+, Sr2+, Mg2+, Li+, Y3+One or more, C is Ce3+Or Eu2+, D is Dy3+, Tm3+, Ho3+, Nd3+In
One, 0.7≤x≤1.3, preferably 0.8≤x≤1.2,0≤y≤0.2, n is along with the value of x, the value of y and the variation of valence of M
And change, its value is fixed and meets valence state conservation.
Embodiment 1: by Ca0.15Sr0.831Al0.9Ga0.1SiN3:0.01Eu2+,0.006Tm3+Shown metering ratio, weighs
0.2000g Ca3N2, 2.17303g Sr3N2, 0.9949g AlN, 0.2258g GaN, 1.2611g Si3N4, 0.0697g
EuCl3, 0.04045g TmCl3.Raw material is mixed in glove box and grinds uniformly, at nitrogen atmosphere, 1.0Mpa pressure
Under, within 5 DEG C/min of heating rate, heat the mixture to 800 DEG C, be incubated 30min, be then heated to 1600 DEG C, insulation
30min, is incubated 1h, cools to room temperature with the furnace by finally heated to 1750 DEG C.The powder body obtained is ground, obtains red nitridation
Thing long-afterglow material.Fig. 1 (a) is the X ray diffracting spectrum of gained sample.Fig. 1 (b) is the SEM figure of gained sample, can obtain gained
Sample particle is block, and disperses the most uniform.Excitation and emission spectra figure such as Fig. 1 (c) institute of this long after glow luminous material
Showing, showing in figure that this long after glow luminous material emission spectrum is broadband emission, peak value is positioned near 620nm, belongs to Eu2+'s
4f65d1→4f7Transition, the chromaticity coordinates using CIE chromaticity diagram to be calculated this long after glow luminous material transmitting light is x=0.6337,
Y=0.3658, is positioned at red emission area.With uviol lamp or blue light illumination, in the dark observe in a period of time after stopping irradiating,
Material presents red afterglow.Fig. 1 (d) is the decay of afterglow curve chart of this luminescent material, it is seen that this luminescence material
Material can continuously send out the distinguishable luminosity of human eye of nearly 2 hours at 0.32mcd/m2Above visible ray.From Fig. 1 (c)
The emission spectrum of shown luminescent material, the chromaticity coordinates calculated (0.6337,0.3658), and decay of afterglow curve chart,
Can illustrate that the long after glow luminous material prepared is red long afterglow luminous material.
Embodiment 2: by Ca0.976Al0.8Ga0.2SiN3:0.015Eu2+,0.006Dy3+Shown metering ratio, weighs
1.3013g Ca3N2, , 0.8844g AlN, 0.4516g GaN, 1.2611g Si3N4, 0.1046g EuCl3,
0.03950g DyCl3. raw material mixed in glove box and grinds uniformly, under nitrogen atmosphere, 0.8Mpa pressure, heating up
Within 5 DEG C/min of speed, heat the mixture to 800 DEG C, be incubated 30min, be then heated to 1600 DEG C, be incubated 30min,
Post-heating, to 1850 DEG C, is incubated 1h, cools to room temperature with the furnace.The powder body obtained is ground, obtains nitride red long afterglow material
Material.Fig. 2 (a) is the X ray diffracting spectrum of gained sample.Fig. 2 (b) is the SEM figure of gained sample, and can obtain gained sample particle is
Bulk, and disperse the most uniform.Shown in excitation and emission spectra figure such as Fig. 2 (c) of this long after glow luminous material, figure shows
This long after glow luminous material emission spectrum is broadband emission, and peak value is positioned near 670nm, belongs to Eu2+4f65d1→4f7Jump
Moving, the chromaticity coordinates using CIE chromaticity diagram to be calculated this long after glow luminous material transmitting light is x=0.6275, y=0.3707, position
In red emission area.With uviol lamp or blue light illumination, in the dark observing after stopping irradiating in a period of time, material presents redness
Afterglow.Fig. 2 (d) is the decay of afterglow curve chart of this luminescent material, it is seen that this luminescent material can persistently be sent out
Go out the distinguishable luminosity of human eye of nearly 70 minutes at 0.32mcd/m2Above visible ray.From the luminous material shown in Fig. 2 (c)
The emission spectrum of material, the chromaticity coordinates calculated (0.6275,0.3707), and decay of afterglow curve chart, it may be said that bright prepared
Long after glow luminous material be red long afterglow luminous material.
Embodiment 3: by Ca0.931Li0.1Al1.2Si0.85N3:0.01Eu2+,0.006Tm3+Shown metering ratio, weighs
1.2413g Ca3N2, 0.0313g Li3N, 1.3265g AlN, 1.0719g Si3N4, 0.0697g EuCl3,
0.04045g TmCl3. raw material mixed in glove box and grinds uniformly, under nitrogen atmosphere, 0.9Mpa pressure, heating up
Within 5 DEG C/min of speed, heat the mixture to 800 DEG C, be incubated 30min, be then heated to 1600 DEG C, be incubated 30min,
Post-heating, to 1950 DEG C, is incubated 1h, cools to room temperature with the furnace.The powder body obtained is ground, obtains nitride red long afterglow material
Material.Fig. 3 (a) is the X ray diffracting spectrum of gained sample.Fig. 3 (b) is the SEM figure of gained sample, and can obtain gained sample particle is
Bulk, and disperse the most uniform.Shown in excitation and emission spectra figure such as Fig. 3 (c) of this long after glow luminous material, figure shows
This long after glow luminous material emission spectrum is broadband emission, and peak value is positioned near 650nm, belongs to Eu2+4f65d1→4f7Jump
Moving, the chromaticity coordinates using CIE chromaticity diagram to be calculated this long after glow luminous material transmitting light is x=0.6522, y=0.347, position
In red emission area.With uviol lamp or blue light illumination, in the dark observing after stopping irradiating in a period of time, material presents redness
Afterglow.Fig. 3 (d) is the decay of afterglow curve chart of this luminescent material, it is seen that this luminescent material can persistently be sent out
Go out the distinguishable luminosity of human eye of the nearly 80 minutes visible ray at more than 0.32mcd/m2.From the luminous material shown in Fig. 3 (c)
The emission spectrum of material, the chromaticity coordinates calculated (0.6522,0.347), and decay of afterglow curve chart, it may be said that bright prepared
Long after glow luminous material be red long afterglow luminous material.
Embodiment 4: by Ca0.2Mg0.05Sr0.731Al0.8Ga0.2SiN3:0.01Eu2+,0.006Ho3+Shown metering ratio, claims
Take 0.2667g Ca3N2, 1.9115g Sr3N2,0.0454Mg3N2, 0.8844g AlN, 0.4516g GaN, 1.2611g
Si3N4, 0.0697g EuCl3, 0.03986g HoCl3. raw material is mixed in glove box and grinds uniformly, at nitrogen gas
Under atmosphere, 1.0Mpa pressure, within 5 DEG C/min of heating rate, heat the mixture to 800 DEG C, be incubated 30min, then heat
To 1600 DEG C, it is incubated 30min, finally heated to 2000 DEG C, is incubated 1h, cools to room temperature with the furnace.The powder body obtained is ground,
Obtain nitride red long-afterglow material.Fig. 4 (a) is the X ray diffracting spectrum of gained sample.Fig. 4 (b) is gained sample
SEM schemes, it is seen that gained sample particle is block, and disperses the most uniform.The exciting and launch light of this long after glow luminous material
Shown in spectrogram such as Fig. 4 (c), showing that this long after glow luminous material emission spectrum is broadband emission in figure, it is attached that peak value is positioned at 635nm
Closely, Eu is belonged to2+4f65d1→4f7Transition, uses CIE chromaticity diagram to be calculated this long after glow luminous material and launches the color of light
Coordinate is x=0.5452, y=0.4473, is positioned at red emission area.With uviol lamp or blue light illumination, when stopping irradiating latter one section
In in the dark observe, material presents orange red afterglow.Fig. 4 (d) is the decay of afterglow curve chart of this luminescent material, from figure
In can be seen that, this luminescent material can continuously send out the distinguishable luminosity of human eye of nearly 90 minutes at 0.32mcd/m2Above
Visible ray.From the emission spectrum of the luminescent material shown in Fig. 4 (c), the chromaticity coordinates calculated (0.5452,0.4473), with
And decay of afterglow curve chart, it may be said that bright prepared long after glow luminous material is orange-red long afterglow Luminescent Material.
MnSi7-3(x+y)Al4xGa4yN12: in C. D, under institute's doping with rare-earth ions species content permanence condition, regulate it and change
Learning proportion of composing, general performance is: when 450nm wavelength excite lower and meet other variable constant in the case of, it launches light
Spectrum peak is gradually reduced along with the increase of x；Under exciting at 450nm wavelength, its Emission Spectrum Peals gradually subtracts along with the increase of y
Under；Under exciting at 450nm wavelength, its Emission Spectrum Peals is gradually increased along with the increase of the content of C；Along with sample emissions light
The wavelength of spectrum peak is elongated, tends to persistence shortening.In regulation chemical formula, M's is elementary composition, the content of x, y, and rare earth
The content of element, can make its emission spectrum change at 610nm to 680nm, for obtained different samples, its emission peak wavelength with
Persistence graph of a relation as figure 5 illustrates.
Embodiments of the present invention are set forth by specific case used herein, and the explanation of above example is only used
In helping to understand method and the core concept thereof of the present invention.It should be pointed out that, for the ordinary person of the art,
Without departing from the principles of the invention, it is also possible to the present invention is carried out some improvement and modification, these improve and modify also to fall
Enter in the protection domain of the claims in the present invention.
Claims (4)
1. a nitride red long-afterglow material, it is characterised in that: its chemical constitution formula is: MnSi7-3(x+y)Al4xGa4yN12:
C. D, wherein M is Ca2+, Sr2+, Mg2+, Li+, Y3+One or more, C is Ce3+Or Eu2+, D is Dy3+, Tm3+, Ho3 +, Nd3+In one, 0.7≤x≤1.3,0≤y≤0.2, n changes along with the value of x, the value of y and the variation of valence of M,
Its value is fixed and meets valence state conservation.
The nitride red long-afterglow material of one the most according to claim 1, it is characterised in that: more than this nitride red length
The excitation spectrum scope of brightness material is at 250nm-600nm, and emission spectrum is that wide bag is launched, and its peak value is adjustable at 590-670nm, and half
High a width of 70-90nm.
The nitride red long-afterglow material of one the most according to claim 1 and 2, it is characterised in that: its structure is monocline
Structure C mc21 (no. 36), RN4, R=Al, Si, Ga, tetrahedron concurrent connects and composes basic framework, cation Ca2+, Sr2+,
Mg2+, Li+, Y3+One or more be present among gap as charge compensation.
4. the preparation method of a nitride red long-afterglow material, it is characterised in that: specifically comprise the following steps that
1) according to chemical constitution formula MnSi7-3(x+y)Al4xGa4yN12: C. D, wherein M is Ca2+, Sr2+, Mg2+, Li+, Y3+'s
One or more, C is Ce3+Or Eu2+, D is Dy3+, Tm3+, Ho3+, Nd3+In one, 0.7≤x≤1.3,0≤y≤0.2,
N changes along with the value of x, the value of y and the variation of valence of M, and its value is fixed and meets valence state conservation；Based on each element chemistry
Amount ratio calculates and weighs and includes AlN, Si3N4, GaN, and Ca3N2、 Sr3N2、 Mg3N2、 Li3One or many in N, YN
Kind, DCl3, CCl3Consumption；
2) each raw material weighed is mixed in glove box, under nitrogen atmosphere, 0.8-1.0Mpa pressure, heating rate 5 DEG C/
Within min, heat the mixture to 800 DEG C, be incubated 30min, be then heated to 1600 DEG C, be incubated 30min, finally heated extremely
1750-2000 DEG C, it is incubated 1h, cools to room temperature with the furnace；
3) powder body obtained by step 2 is ground, obtain nitride red long-afterglow material powder body.
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| CN103113884A (en) * | 2013-02-05 | 2013-05-22 | 江门市远大发光材料有限公司 | LED (light-emitting diode) plant growth lamp based on nitride red fluorescent powder |
| CN104238249A (en) * | 2013-06-21 | 2014-12-24 | 深圳市绎立锐光科技开发有限公司 | Light-emitting device and related projection system |
| CN105385014A (en) * | 2015-12-11 | 2016-03-09 | 华南农业大学 | Light conversion agricultural film, and making method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101688115A (en) * | 2007-07-09 | 2010-03-31 | 夏普株式会社 | Group of phosphor particles, and light-emitting device using the same |
| US20130001470A1 (en) * | 2009-05-15 | 2013-01-03 | Cree, Inc. | Luminescent particles, methods and light emitting devices including the same |
| CN103113884A (en) * | 2013-02-05 | 2013-05-22 | 江门市远大发光材料有限公司 | LED (light-emitting diode) plant growth lamp based on nitride red fluorescent powder |
| CN104238249A (en) * | 2013-06-21 | 2014-12-24 | 深圳市绎立锐光科技开发有限公司 | Light-emitting device and related projection system |
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Application publication date: 20170111 |