CN1133710C - Photoluminescent spherical porous ceramic material with ultra-long afterglow and its synthesizing process - Google Patents
Photoluminescent spherical porous ceramic material with ultra-long afterglow and its synthesizing process Download PDFInfo
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- CN1133710C CN1133710C CNB011306564A CN01130656A CN1133710C CN 1133710 C CN1133710 C CN 1133710C CN B011306564 A CNB011306564 A CN B011306564A CN 01130656 A CN01130656 A CN 01130656A CN 1133710 C CN1133710 C CN 1133710C
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Abstract
The present invention relates to a spherical ultralong persistence photoluminescent porous ceramic material and a preparation method thereof. Firstly, raw materials are proportionally weighed according to chemical constituents and are uniformly mixed by a stirrer for drying and prefiring, and a solution with dissolved organic and inorganic dispersing agents is added. Secondly, a spraying prilling tower is used for spray granulating and drying, the mixture is sintered in a high temperature furnace at a reducing atmosphere, and then the spherical ultralong persistence photoluminescent porous ceramic material with good loose degree is synthesized. The method of the present invention solves the problem of hard groups of materials sintered by traditional ceramic sintering methods and firstly synthesizes a spherical porous light-accumulating ceramic material. The method not only greatly increases the extinction property of photoluminescent phosphor materials in traditional aluminate systems, but also greatly improves anti-hydrolysis property thereof. After irradiated by natural light or other light sources for a short time, the photoluminescent porous ceramic material prepared by the method can continuously send out light for more than 20 hours in dark places within a visual brightness range of human eyes.
Description
Technical field the present invention relates to a kind of spherical overlength afterglow photoluminescence porous ceramic film material and synthetic method thereof, belong to material science, particularly inorganic non-metallic function ceramics luminescent material is mainly concerned with the synthetic of a kind of novel globular overlength afterglow photoluminescence porous ceramic film material.
In the background technology long afterglow luminescence material research early be sulfide luminescent material, comprise CaS:Bi (blue blue light); (CaSr) S:Bi (coloured light turns blue); ZnS:Cu (glow green); (ZnCd) S:Cu (jaundice look or orange coloured light).Comparatively famous in the sulfide is ZnS:Cu, and it is first steady persistence light-storing material with practical application meaning.But this material is unstable on chemical property, demonstrates relatively poor light resistance, having under certain humidity and the radiation and can decompose in UV-light, so blackening, reduce luminance brightness.Make it and to use out of doors and to be directly exposed under the sunlight.And the lasting fluorescent lifetime of ZnS:Cu has only dozens of minutes, and it is longer to want its fluorescent lifetime, and brightness is higher, must add a spot of radioactive substance such as Co, Pm etc. in this luminescent material.
About utilizing rare-earth ion activated luminous alkali earth metal aluminate luminescent material, as far back as nineteen forty-six, Froelich etc. just find SrO.Al
2O
3: Eu, behind the process light source activation, can send wavelength is the coloured light that has of 400～520nm, and has applied for United States Patent (USP) U.S.Patent 2392814.Nineteen sixty-eight, Palilla finds SrO.Al
2O
3: the luminescence process of Eu at first is quick attenuation process of experience, in low luminous intensity scope, also exists the lasting luminous of long period then.But in a very long time, this phenomenon does not cause people's attention, up to the nineties, the researchist finds, when other mixes up rare earth ion altogether when introducing in this system, original intensity and afterglow property are improved greatly, and be better than sulfide base long persistence luminescent material in the past far away, have many patents to come out successively in recent years.Disclosing a kind of chemical constitution as Chinese patent CN1188788A and United States Patent (USP) U.S.Patent 5686022 is MO.Al
2O
3: Eu, the long persistence phosphor material of N is more than 12 hours time of persistence.Patent CN1241612A has reported a kind of MO.Al that utilizes after surface modification and parcel are handled
2O
3: Eu, Dy long persistence phosphor material, mobile and dispersed to improve it.Japanese Patent 8-170076 has reported a kind of MO.a of consisting of (Al
1-bB
b)
2O
3: the long after glow luminous material of cR.Chinese patent CN1115779A has also reported a kind of aM in addition
1-x-y-zO.bAl
2O
3: Eu
x, A
y, B
zLong after glow luminous material.
But the prepared luminescent material hard aggregation of above-mentioned this system or similar system is relatively more severe, and in water hydrolysis can take place, and makes its application be subjected to certain restriction.
Summary of the invention the objective of the invention is to propose a kind of synthetic spherical overlength afterglow photoluminescence porous ceramic film material and synthetic method thereof, so that solve the hard aggregation of luminescent powder behind high temperature sintering in the past, reduces aftertreatment technology.In addition, by adjusting the composition of phosphorescent substance matrix, to improve the resistance to hydrolysis energy of original long persistence phosphor powder.
The spherical overlength afterglow photoluminescence porous ceramic film material that the present invention proposes, its theoretical chemistry composition formula is: M (1-m-n) O.xAl
2O
3.ySiO
2.zB
2O
3: Eu
m, RE
nWherein M is one or more among Mg, Ca, Sr, the Ba; The x value is 0.5～3.5; The y value is 0.001～1.0; The z value is 0.001～0.15; The m value is 0.0001～0.10; The n value is 0.0001～0.3.RE can in the lanthanon one or more as La, Dy, Nd, Pr, Ho etc., also can be in the part transition metal ion one or more, as Sb, Co, Sn etc.
The synthetic method of the spherical overlength afterglow photoluminescence porous ceramic film material that the present invention proposes may further comprise the steps:
(1) with the M alkaline-earth metal, the carbonate of Al, Si, B, oxyhydroxide, oxide compound or organic compound salt are pressed chemical constitution formula M (1-m-n) O.xAl with above-mentioned materials
2O
3.ySiO
2.zB
2O
3: Eu
m, RE
nThe ratio of component batching weighing, wherein M is one or more among Mg, Ca, Sr, the Ba; The x value is 0.5～3.5; The y value is 0.001～1.0; The z value is 0.001～0.15; The m value is 0.0001～0.10; The n value is 0.0001～0.3; RE is one or more in the lanthanon, or is in the transition metal ion one or more.
(2) by the stirrer uniform mixing,, carry out pre-burning 1～3h at 700 ℃～900 ℃ then at 50～90 ℃ of drying 2～4h.
(3) powder after the pre-burning is added the solution that is dissolved with the organic-inorganic dispersion agent.This dispersion agent is ethanol, tetraethoxy, NH
4Cl, NH
4F, NH
4H
2PO
4, CaCl
2, CaF
2, BaCl
2, BaF
2In one or more the aqueous solution, disperse, mix, adjusting liquid-solid ratio is 1.5～1.
(4) utilize the mist projection granulating tower carry out mist projection granulating, 50～90 ℃ of dryings.
(5) (1%～6%H under reducing atmosphere
2-N
2In the gas mixture), in 1200～1450 ℃ High Temperature Furnaces Heating Apparatus, burn till, can synthesize the extraordinary M of shatter value (1-m-n) O.xAl
2O
3.ySiO
2.zB
2O
3: Eu
m, RE
nSpherical overlength afterglow photoluminescence porous ceramic film material.
In the method for the present invention, in the time of also can mixing, directly add the organic-inorganic dispersion agent, after spraying drying, directly under reducing atmosphere, burn till, also can synthesize the extraordinary M of shatter value (1-m-n) O.xAl without pre-burning at the raw material of the above-mentioned the first step
2O
3.ySiO
2.zB
2O
3: Eu
m, RE
nSpherical overlength afterglow photoluminescence porous ceramic film material.
The inventive method has solved in the past the traditional ceramics sintering process fully and effectively and has burnt till the hard aggregation problem of material, and has synthesized spherical porous first and hold the light ceramic material.M (1-m-n) O.xAl
2O
3.ySiO
2.zB
2O
3: Eu
m, RE
nThis matrix makes not only in the past that the photo absorption performance of aluminates system photoluminescence phosphor material increases greatly, and its anti-hydrolysis properties is also had significantly improve.The photoluminescence porous ceramic film material that makes by this method in the visual brightness range of human eye, can continue luminous more than 20 hours behind natural light or other light source short irradiation in the dark.
Compared with prior art, the present invention is a kind of novel spherical overlength afterglow photoluminescence porous ceramic film material, its luminosity height, and time of persistence is long, and physicochemical property stability is fine.Particularly: (1) uses spray granulating and drying equipment, helps synthesizing porous globe-type luminescence pottery.(2) add the organic-inorganic dispersion agent, help improving the dispersion effect of powder, more help the uniform mixing of material, and play the effect of charge compensation agent, strengthen illumination effect.(3) SiO
2And B
2O
3Adding, not only play the effect of solubility promoter, and be added in the parent lattice, form the part defective, not only be beneficial to the diffusion of luminescence center ionic, and can also with mix up the same effect of playing the trap center effectively of rare earth ion altogether, thereby prolong time of persistence, improve luminescent properties.(4) in addition, SiO
2Adding, can effectively improve the photo absorption performance of overlength afterglow photoluminescence porous ceramics, and can improve the resistance to hydrolysis energy of phosphorescent substance matrix, thereby its physical and chemical stability can be improved.(5) phosphorescent substance porous spherical particle has increased the surface-area of particle, and photo absorption performance is increased, and holds between the light time and shortens.
Description of drawings:
Fig. 1 is the microscopic appearance figure of mist projection granulating gained raw material.
Fig. 2 burns till gained porous spherical luminescent powder figure for high temperature.
Embodiment:
Embodiment 1:
(1) presses Sr
0.92O.0.99Al
2O
3.0.17SiO
2.0.04B
2O
3: Eu
0.01, Dy
0.07Form, take by weighing SrCO
3665g, Al (OH)
3750g, SiO
250g, H
3BO
325g, Eu
2O
310g, Dy
2O
360g.In above-mentioned compound, add deionized water 3L, utilize stirrer fully to stir, mix, 60 ℃ of dryings 2 hours.Dried compound is packed in the crucible, 800 ℃ of pre-burnings 1 hour.The NH that powder after the pre-burning is added an amount of organic-inorganic dispersion agent ethanol (50ml), tetraethoxy (20ml) and 0.1mol/l
4The aqueous solution of F (10ml), and add pure water, adjust liquid-solid ratio to 1.3: 1, stirred 4 hours, carry out mist projection granulating, drying.The crucible of then dry powder material being packed into once more is at weakly reducing atmosphere 3%H
2-N
2Under the gas mixture,, can make overlength afterglow photoluminescence porous ceramic film material in 1380 ℃ of roastings 2.5 hours.
Present embodiment institute synthetic overlength afterglow photoluminescence porous ceramic film material, these material true qualities are light yellow, can well be excited by the visible light of 260～450nm wavelength region, and glow color is yellow-green colour, the emission peak wavelength is positioned at about 520nm, and original intensity reaches about 32000mcd/m
2, be time of persistence more than 20 hours.The exterior appearance of phosphor particles is tangible porous spherical particle, and good anti-hydrolysis properties is arranged.The microcosmic type looks of the powder behind its mist projection granulating and burn till after phosphor powder build looks see shown in figure [1], [2].
Embodiment 2:
Form Sr by name
0.89O.1.07Al
2O
3.0.02SiO
2.0.03B
2O
3: Eu
0.04, Dy
0.07, take by weighing SrCO
3625g, Al (OH)
3790g, SiO
25g, H
3BO
315g, Eu
2O
330g, Dy
2O
365g.In above-mentioned compound, add deionized water 3.5L, utilize stirrer fully to stir, mix, 70 ℃ of dryings 2 hours.Dried compound is packed in the crucible, carried out pre-burning 1.5 hours at 800 ℃.The BaCl that powder after the pre-burning is added an amount of organic-inorganic dispersion agent ethanol (40ml), 0.1mol/l
2(10ml) and the NH of 0.1mol/l
4The aqueous solution of F (5ml), and add pure water, adjust liquid-solid ratio to 1.2: 1, stirred 5 hours, carry out mist projection granulating, drying.The crucible of then exsiccant powder material being packed into once more is at weakly reducing atmosphere 2.5%H
2-N
2Under the gas mixture,, can make overlength afterglow photoluminescence porous ceramic film material in 1320 ℃ of roastings 4 hours.
Present embodiment institute synthetic overlength afterglow photoluminescence porous ceramic film material, it is yellow that these material true qualities are, and can well be excited by the visible light of 280～420nm wavelength region, and it is green that glow color is, the emission peak wavelength is positioned at about 514nm, and original intensity reaches about 25000mcd/m
2, be time of persistence more than 15 hours.The exterior appearance of phosphor particles is porous spherical, and resistance to hydrolysis can be relatively poor.
Embodiment 3:
Form Sr by name
0.83O.1.8Al
2O
3.0.24SiO
2.0.07B
2O
3: Eu
0.04, Dy
0.12, La
0.01, take by weighing SrCO
3600g, Al
2O
3900g, SiO
270g, H
3BO
340g, Eu
2O
330g, Dy
2O
3100g, La
2O
310g.In above-mentioned compound, add deionized water 4.5L, utilize stirrer fully to stir, mix, 80 ℃ of dryings 2 hours.Dried compound is packed in the crucible, carried out pre-burning 2 hours at 800 ℃.The NH that powder after the pre-burning is added an amount of organic-inorganic dispersion agent ethanol (80ml), 0.1mol/l
4H
2PO
4(20ml) and the NH of 0.1mol/l
4The aqueous solution of F (5ml), and add pure water, adjust liquid-solid ratio to 1.4: 1, stirred 6 hours, carry out mist projection granulating, drying.The crucible of then exsiccant powder material being packed into once more is at weakly reducing atmosphere 3.5%H
2-N
2Under the gas mixture,, can make overlength afterglow photoluminescence porous ceramic film material in 1390 ℃ of roastings 3 hours.
Present embodiment institute synthetic overlength afterglow photoluminescence porous ceramic film material, these material true qualities are shallow white, can well be excited by the visible light of 230～450nm wavelength region, and glow color is blue-greenish colour, the emission peak wavelength is positioned at about 490nm, and original intensity reaches about 7300mcd/m
2, be time of persistence more than 25 hours.The exterior appearance of phosphor particles is porous spherical, has extraordinary resistance to hydrolysis energy.
Embodiment 4:
By name form 2 (Sr, Ba)
0.95O.3.07Al
2O
3.0.8SiO
2.0.10B
2O
3: Eu
0.05, Dy
0.15, take by weighing SrCO
3500g, BaCO
380g, Al
2O
3640g, SiO
2100g, H
3BO
325g, Eu
2O
320g, Dy
2O
355g.
Take by weighing SrCO
3600g, Al
2O
3900g, SiO
270g, H
3BO
340g, Eu
2O
330g, Dy
2O
3100g, La
2O
310g.In above-mentioned compound, add deionized water 5L, utilize stirrer fully to stir, mix, 70 ℃ of dryings 2 hours.Dried compound is packed in the crucible, carried out pre-burning 2 hours at 900 ℃.The NH that powder after the pre-burning is added an amount of organic-inorganic dispersion agent ethanol (100ml), 0.1mol/l
4H
2PO
4(20ml) and the BaCl of 0.1mol/l
2The aqueous solution (5ml), and add pure water, adjust liquid-solid ratio to 1.2: 1, stirred 4 hours, carry out mist projection granulating, drying.The crucible of then exsiccant powder material being packed into once more is at weakly reducing atmosphere 4.0%H
2-N
2Under the gas mixture,, can make overlength afterglow photoluminescence porous ceramic film material in 1400 ℃ of roastings 3 hours.
Present embodiment institute synthetic overlength afterglow photoluminescence porous ceramic film material, it is yellow that these material true qualities are, and can well be excited by the visible light of 260～430nm wavelength region, and glow color is blue-greenish colour, the emission peak wavelength is positioned at about 490nm, and original intensity reaches about 5400mcd/m
2, be time of persistence more than 18 hours.The exterior appearance of phosphor particles is porous spherical, and resistance to hydrolysis can be good.
Embodiment 5:
Form Ca by name
0.71O.1.02Al
2O
3.0.33SiO
2.0.08B
2O
3: Eu
0.05, Nd
0.24, take by weighing CaCO
3140g, Al (OH)
3315g, SiO
240g, H
3BO
320g, Eu
2O
320g, Nd
2O
380g.In above-mentioned compound, add an amount of organic-inorganic dispersion agent ethanol (70ml), the CaCl of 0.1mol/l
2The aqueous solution (10ml), and add pure water, adjust liquid-solid ratio to 1.15: 1, stirred 4 hours, carry out mist projection granulating, drying.Utilize stirrer fully to stir, mix, 80 ℃ of dryings 2.5 hours.Dried compound is packed in the crucible, carried out pre-burning 2 hours at 900 ℃.The crucible of then exsiccant powder material being packed into once more is at weakly reducing atmosphere 2.0%H
2-N
2Under the gas mixture,, can make overlength afterglow photoluminescence porous ceramic film material in 1250 ℃ of roastings 2.5 hours.
Present embodiment institute synthetic overlength afterglow photoluminescence porous ceramic film material, these material true qualities are canescence, can well be excited by the visible light of 250～400nm wavelength region, and glow color is yellow-green colour, the emission peak wavelength is positioned at about 440nm, and original intensity reaches about 2300mcd/m
2, be time of persistence more than 10 hours.
Embodiment 6:
Form Sr by name
0.89O.1.73Al
2O
3.0.17SiO
2.0.04B
2O
3: Eu
0.02, Dy
0.09, take by weighing SrCO
3640g, Al
2O
3860g, SiO
250g, H
3BO
325g, Eu
2O
315g, Dy
2O
380g, Sb
2O
315g.
Add deionized water 5L, and add an amount of organic-inorganic dispersion agent ethanol, NH
4H
2PO
4And CaHPO
4, adjust liquid-solid ratio to 1.2: 1, utilize stirrer to stir 6 hours, thorough mixing is even, carries out mist projection granulating, drying, the crucible of then dry powder material being packed into once more, under weakly reducing atmosphere,, can make overlength afterglow photoluminescence porous ceramic film material in 1370 ℃ of roastings 4 hours.
Present embodiment institute synthetic overlength afterglow photoluminescence porous ceramic film material, these material true qualities are shallow white, can well be excited by the visible light of 250～460nm wavelength region, and it is blue green that glow color is, the emission peak wavelength is positioned at about 490nm, and original intensity reaches about 6300mcd/m
2, be time of persistence more than 20 hours.The exterior appearance of phosphor particles is porous spherical, and hydrolysis property is good.
Embodiment 7:
Form Sr by name
0.81O.3.50Al
2O
3.0.20SiO
2.0.04B
2O
3: Eu
0.04, Dy
0.15, take by weighing SrCO
3580g, Al
2O
31740g, SiO
260g, H
3BO
325g, Eu
2O
330g, Dy
2O
3135g, Sb
2O
315g.
Add deionized water 8L, utilize stirrer fully to stir, mix, 80 ℃ of dryings 3 hours.Dried compound is packed in the crucible, carried out pre-burning 2 hours at 850 ℃.The NH that powder after the pre-burning is added an amount of organic-inorganic dispersion agent ethanol (120ml), tetraethoxy (15ml) and 0.1mol/l
4The aqueous solution of Cl (10ml), and add pure water, adjust liquid-solid ratio to 1.3: 1, stirred 6 hours, carry out mist projection granulating, drying.The crucible of then exsiccant powder material being packed into once more is at weakly reducing atmosphere 3.5%H
2-N
2Under the gas mixture,, can make overlength afterglow photoluminescence porous ceramic film material in 1450 ℃ of roastings 3 hours.
Present embodiment institute synthetic overlength afterglow photoluminescence porous ceramic film material, these material true qualities are shallow white, can well be excited by the visible light of 250～430nm wavelength region, and it is light yellow that glow color is, the emission peak wavelength is positioned at about 535nm, and original intensity reaches about 1800mcd/m
2, be time of persistence more than 8 hours.The exterior appearance of phosphor particles is porous spherical, and hydrolysis property is good.
Claims (2)
1, a kind of spherical overlength afterglow photoluminescence porous ceramic film material is characterized in that the theoretical chemistry composition formula of this material is: M (1-m-n) O.xAl
2O
3.ySiO
2.zB
2O
3: Eu
m, RE
nWherein M is one or more among Mg, Ca, Sr, the Ba; The x value is 0.5～3.5; The y value is 0.001～1.0; The z value is 0.001～0.15; The m value is 0.0001～0.10; The n value is 0.0001～0.3; RE is one or more in the lanthanon, or is in the transition metal ion one or more.
2, a kind of synthetic method of spherical overlength afterglow photoluminescence porous ceramic film material is characterized in that this method may further comprise the steps:
(1) with the M alkaline-earth metal, the carbonate of Al, Si, B, oxyhydroxide, oxide compound or organic compound salt are pressed chemical constitution formula M (1-m-n) O.xAl with above-mentioned materials
2O
3.ySiO
2.zB
2O
3: Eu
m, RE
nThe ratio of component batching weighing, wherein M is one or more among Mg, Ca, Sr, the Ba; The x value is 0.5～3.5; The y value is 0.001～1.0; The z value is 0.001～0.15; The m value is 0.0001～0.10; The n value is 0.0001～0.3; RE is one or more in the lanthanon, or is in the transition metal ion one or more;
(2) make the above-mentioned raw materials uniform mixing with stirrer,, carry out pre-burning 1～3h at 700 ℃～900 ℃ then at 50～90 ℃ of drying 2～4h;
(3) adding of the powder after the pre-burning is dissolved with in the solution of organic or inorganic dispersion agent, this dispersion agent is ethanol, tetraethoxy, NH
4Cl, NH
4F, NH
4H
2PO
4, CaCl
2, CaF
2, BaCl
2, BaF
2In one or more the aqueous solution, disperse, mix, liquid-solid ratio wherein is 1.5～1: 1;
(4) utilize the mist projection granulating tower carry out mist projection granulating, 50～90 ℃ of dryings;
(5) be 1%～6%H at composition
2-N
2In the reducing atmosphere of gas mixture, burn till in 1200～1450 ℃ High Temperature Furnaces Heating Apparatus, promptly obtaining chemical formula is M (1-m-n) O.xAl
2O
3.ySiO
2.zB
2O
3: Eu
m, RE
nSpherical overlength afterglow photoluminescence porous ceramic film material.
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|---|---|---|---|---|
| CN101403475B (en) * | 2008-11-13 | 2011-08-17 | 北京航空航天大学 | Energy accumulation luminous stone and its production method |
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| CN1673190B (en) * | 2004-03-24 | 2010-04-28 | 北京航空航天大学 | Multifunctional ceramic layer preparation process |
| JP4880892B2 (en) * | 2004-10-18 | 2012-02-22 | 株式会社東芝 | Phosphor, phosphor manufacturing method, and light emitting device using the same |
| CN100473710C (en) * | 2006-11-20 | 2009-04-01 | 四川新力光源有限公司 | Rare earth multielement coactivate long persistence luminescent material and preparation method thereof |
| CN106381141A (en) * | 2016-08-31 | 2017-02-08 | 广州珠江光电新材料有限公司 | Boron-containing aluminosilicate long afterglow phosphor and preparation method thereof |
| CN107936962B (en) * | 2017-11-02 | 2018-12-07 | 杭州鼎好新材料有限公司 | A kind of green long-time afterglow luminescent powder and preparation method thereof |
| CN109133978A (en) * | 2018-08-31 | 2019-01-04 | 王召惠 | A kind of preparation method of high intensity high thermal conductivity porous ceramics |
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| CN101403475B (en) * | 2008-11-13 | 2011-08-17 | 北京航空航天大学 | Energy accumulation luminous stone and its production method |
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