CN106634976A - Orange red long-afterglow fluorescent powder and preparation method thereof - Google Patents
Orange red long-afterglow fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention provides orange red long-afterglow fluorescent powder and a preparation method thereof and relates to fluorescent powder. The structural formula of the orange red long-afterglow fluorescent powder is M1-x-yAlSi5O2N7:Ybx, Lny, wherein x is greater than or equal to 0.001 or smaller than or equal to 0.1, y is greater than or equal to 0 or smaller than or equal to 0.1, M contains, at least Ba and at least one of Mg, Ca, Sr, Ba and the like, and Ln is at least one of Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm and the like. The preparation method comprises the steps that an M precursor, a Yb precursor, a Ln precursor, an Al precursor and a Si precursor are calcinated in a reducing atmosphere at the temperature of 1200-1800 DEG C or are sintered under the reducing atmosphere firstly to obtain a silicate compound of Yb<2+> and Ln<3+> doped M metal, and then the silicate compound is sintered with the Si precursor and the Al precursor under the reducing atmosphere at the temperature of 1200-1800 DEG C again.
Description
Technical field
The present invention relates to fluorescent material, more particularly, to a kind of orange light long lad phosphor and preparation method thereof.
Background technology
Long-afterglow material as a kind of energy storage material, with can after excitation source stops the characteristic of continuous illumination and
By people's extensive concern, since being paid close attention to and studied by researcher from 20 end of the centurys, blue and green long afterglow material obtained compared with
Good development, and mostly using aluminate as based on matrix.Such as commercial blue long afterflow (CaAl2O4:Eu2+,Nd3+) and
Green long afterglow (SrAl2O4:Eu2+,Dy3+) persistence of material can exceed 10h (reference literature 1 and 2).And more long wave
Long long-afterglow material, relative species is less if the long-afterglow material of ruddiness and infrared light, and long-persistence luminous performance
It is relatively poor, furthermore due to ruddiness and infrared light long-afterglow material show at aspects such as bio-imagings in recent years it is strong
Competitiveness.So the long-afterglow material of exploitation and development long wavelength is significant.
For from principle of luminosity, it is desirable to obtain red long afterglow luminous material, active ions typically can be Eu2+, Eu3 +, Pr3+And Cr3+Deng.The such as Eu of the report of document 32+The CaS materials of activation, after ultraviolet light energy storage, can show
Peak value is the lasting ruddiness persistent quality of 650nm.For another example in document 4 report in Y2O2S:Eu3+,Ti4+,Mg2+In equally can
Long afterglow is obtained for Eu3+Characteristic emission long afterglow phenomenon.In document 5, peak value is that 611nm ruddiness long afterglows phenomenon can be
La2Ti2O7:Pr3+Middle realization, and persistence can exceed 1h.More than it is rare earth ion doped red long-afterglow material
Material.In recent years, the ruddiness long after glow luminous material of transition metal activation has been similarly obtained the development of some, and Photobiology into
The fields such as picture have obtained certain application, the ruddiness long-afterglow material Zn for such as obtaining in document 63Ga2Ge2O10:Cr3+, ultraviolet
After light (254nm) irradiation, Cr can be shown3+The long afterglow qualities of characteristic emission.Despite part red long afterglow material
Some development are obtained, but species is relative lacks, furthermore due to the Y reported respectively in such as document 3 and 42O2S:Eu3+,Ti4 +,Mg2+And CaS:Eu2+Ruddiness long-afterglow material belongs to sulfide, and poor water resistance and unstable property restrict its development.
Therefore long after glow luminous material stable in properties is developed significant.And nitrogen oxides is typically exhibited as luminescent material
Excellent stability.Additionally, the ruddiness long-afterglow material of the new centre of luminescence of exploitation is for the development of long after glow luminous material
It is critically important, and with Yb2+Then seldom have been reported that as the patent document of the long after glow luminous material of the centre of luminescence.
Bibliography：
1：Koen Van den Eeckhout, Philippe F.Smet, Dirk Poelman, Materials, Vol.3,
No.4,2536-2566,2010.
2：T.Matsuzawa, Y.Aoki, N.Takeuchi, Y.Murayama, Journal of the
Electrochemical Society, Vol.143, No.8,2670-2673,1996.
3：Philippe F.Smet, Iwan Moreels, Zeger Hens, Dirk Poelman, Materials,
Vol.3, No.4,2834-2883,2010.
4：Chia-Cheng Kang, Ru-Shi Liu, Jiin-Chyuan Chang, Biing-Jye Lee,
Chemistry of Materials, Vol.15, No.21,3966-3968,2003.
5：Ming-Hui Chu, Da-Peng Jiang, Cheng-Jiu Zhao, Bin Li, Chinese Physics
Letters, Vol.27, No.4,047203-1-047203-4,2010.
6：Zhengwei Pan, Yi-Ying Lu, Feng Liu, Nature Materials, Vol.11, No.1,58-
63,2012.
The content of the invention
It is an object of the invention to provide simple, efficiency high and be conducive to industrialized production suitable for white light LEDs and the sun
A kind of orange light long lad phosphor of energy battery and preparation method thereof.
The structural formula of the orange light long lad phosphor is as follows：
M1-x-yAlSi5O2N7:Ybx,Lny；
Wherein, 0.001≤x≤0.1,0≤y≤0.1；M includes at least at least in Ba, and Mg, Ca, Sr, Ba etc.
Kind；Ln is at least one in Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm etc..
The preparation method of the orange light long lad phosphor is as follows：
By M presomas, Yb presomas, Ln precursors, Al presomas and Si presomas in reducing atmosphere in 1200～
Calcine at 1800 DEG C；Or
First under reducing atmosphere sintering obtains Yb2+And Ln3+The silicate compound of the M metals of doping, then with Si presomas
Sinter again in 1200～1800 DEG C under reducing atmosphere with Al presomas.
The M presomas may be selected from least in nitrate of the carbonate of M, the oxide of M, the oxalates of M and M etc.
Kind；
The Yb presomas may be selected from nitrate of the carbonate of Yb, the oxide of Yb, the oxalates of Yb and Yb etc.
It is at least one；
The Ln presomas may be selected from nitrate of the carbonate of Ln, the oxide of Ln, the oxalates of Ln and Ln etc.
It is at least one；
The Al presomas may be selected from least one in the oxide of Al and the nitrate of Al etc.；
The Si presomas may be selected from least one in nitride of the oxide of Si, Si etc.；
The reducing atmosphere may be selected from ammonia or nitrogen hydrogen mixeding gas.
The temperature that the elder generation sinters under reducing atmosphere can be 1200～1800 DEG C, and the time of sintering can be 3～15h.
The invention provides a kind of orange light long-afterglow material and preparation method thereof.The long lad phosphor has brand-new
Chemical composition, with Yb2+As activator.M can be improved by the doping of trivalent rare earth ionses1-x-yAlSi5O2N7:Yb2+It is remaining
Brightness intensity and time.The fluorescent material can be excited by the light in 200～480nm wave-length coverages and launch peak wavelength positioned at 615
The orange light of～625nm scopes, stop the wave band exciting light shine after, can produce it is long-persistence luminous so that the phosphor
Material can store ultraviolet light and purplish blue light is converted into orange light.The long-afterglow fluorescent powder, preparation method thereof that the present invention is provided is simple, chemical
Stable performance, it is adaptable to the application scenarios of white light LEDs, solar cell or biomarker.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of the long after glow luminous material obtained in the embodiment of the present invention 1；
Fig. 2 is luminescence generated by light spectrogram of the long after glow luminous material obtained in the embodiment of the present invention 2 in the case where 300nm is excited；
Fig. 3 is the length of the long after glow luminous material different time after 254nm excites stopping obtained in the embodiment of the present invention 2
Twilight sunset launching light spectrogram；
Fig. 4 is the long after glow luminous material obtained by embodiment 1 and embodiment 8, and through 254nm ultraviolets 2min is irradiated
Afterwards, the long afterglow attenuation curve for measuring.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, following examples are only the section Examples of the present invention.
Embodiment 1
According to BaCO3(analysis is pure), SiO2(analysis is pure) and Yb2O3(analysis is pure) mol ratio is the ︰ 0.03 of 1.94 ︰ 1, respectively
Feeding is ground above-mentioned raw materials, be dried after reinstall corundum crucible, in high temperature furnace, in H2/N2Gaseous mixture (gas content
Ratio is H2︰ N2=5 ︰ 95, gas flow rate is 100mL/min) in 1300 DEG C of sintering 3h, along with the furnace cooling obtains Yb to room temperature2+Mix
Miscellaneous Ba2SiO4Persursor material.Then by this precursor and Si3N4With AlN according to the amount mixing that mol ratio is the ︰ 2 of 1 ︰ 3, grinding
Reinstall in boron nitride crucible after mixing, drying, be put in high temperature furnace, in H2/N2(gas content ratio is H to gaseous mixture2︰ N2=
5 ︰ 95, gas flow rate is 100mL/min) in 1600 DEG C of sintering 6h, obtain required after grinding after along with the furnace cooling to room temperature taking-up
Long after glow luminous material.
The material obtained in embodiment 1 is analyzed using X-ray diffraction, obtains its X ray diffracting spectrum, such as Fig. 1
It is shown.Inquire about in international crystallographic data storehouse, confirm this collection of illustrative plates and belong to rhombic system space group for Imm2's and chemical group
Become BaAlSi5O2N7Standard diagram (ICSD 240276) it is consistent, obvious miscellaneous peak is not observed.
The fluorescent material obtained in embodiment 1 is analyzed using XRF, under 300nm ultraviolet excitations
Emission peak is located at 615nm, under 254nm ultraviolet excitations, can show Characteristics of Long Luminosity.It can be seen that the fluorescent material energy quilt
Ultraviolet excitation and launch orange light so that the fluorescent material can convert uv light into orange light.
Embodiment 2
According to BaCO3(analysis is pure), SrCO3(analysis is pure), SiO2(analysis is pure) and Yb2O3(analysis pure) mol ratio is
The ︰ 0.03 of 1.54 ︰, 0.4 ︰ 1, respectively feeding above-mentioned raw materials are ground, be dried after reinstall corundum crucible, in high temperature furnace,
H2/N2(gas content ratio is H to gaseous mixture2︰ N2=5 ︰ 95, gas flow rate is 100mL/min) in 1300 DEG C of sintering 3h, with stove
Room temperature is cooled to, Yb is obtained2+The Ba of doping1.6Sr0.4SiO4Persursor material.Then by this precursor and Si3N4With AlN according to
Mol ratio be the ︰ 2 of 1 ︰ 3 amount mixing, be ground, be dried after reinstall in boron nitride crucible, be put in high temperature furnace, in H2/N2It is mixed
(gas content ratio is H to close gas2︰ N2=5 ︰ 95, gas flow rate is 100mL/min) in 1600 DEG C of sintering 6h, along with the furnace cooling is to room
Temperature obtains required long after glow luminous material after grinding after taking out.
The material obtained in embodiment 2 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) it is consistent, obvious miscellaneous peak is not observed.
The fluorescent material obtained in embodiment 2 is analyzed using XRF, under 300nm ultraviolet excitations
To its launching light spectrogram, as shown in Figure 2.It can be seen that the fluorescent material can be launched orange light by ultraviolet excitation, so that the fluorescence
Material can convert uv light into orange light.Additionally, the sample is removed into exciting light after 254nm ultraviolets excite 2min
Source, the twilight sunset emission spectrum of test sample different time.As shown in figure 3, the twilight sunset emission spectrum behind 1,3 and 5min.Twilight sunset
Emission spectrum and photoluminescence spectra (Fig. 2) shape have no significant difference.
Embodiment 3～6
According to BaCO3(analysis is pure), SrCO3(analysis is pure), SiO2(analysis is pure), Yb2O3(analysis is pure) and Ln2O3(analysis
It is pure) mol ratio be 1.92 ︰, 1 ︰ 0.03 ︰ 0.01, the Ln in embodiment 3～62O3Correspond respectively to Nd2O3, Dy2O3, Ho2O3,
Tm2O3.Respectively feeding above-mentioned raw materials are ground, be dried after reinstall corundum crucible, be put in high temperature furnace, in H2/N2Mixing
(gas content ratio is H to gas2︰ N2=5 ︰ 95, gas flow rate is 100mL/min) in 1300 DEG C of sintering 3h, along with the furnace cooling is to room
Temperature, obtains Yb2+And Ln3+The Ba of doping1.6Sr0.4SiO4Persursor material.Then by this precursor and Si3N4With AlN according to rubbing
You than for the ︰ 2 of 1 ︰ 3 amount mix, be ground, be dried after reinstall in boron nitride crucible, in high temperature furnace, in H2/N2Gaseous mixture
(gas content ratio is H2︰ N2=5 ︰ 95, gas flow rate is 100mL/min) in 1600 DEG C of sintering 6h, along with the furnace cooling to room temperature takes
Required long after glow luminous material is obtained after grinding after going out.
The material obtained in embodiment 3～6 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) it is consistent, obvious miscellaneous peak is not observed.
The fluorescent material obtained in embodiment 3～6 is analyzed using XRF, in 300nm ultraviolet excitations
Under obtain its emission spectrum.Except being co-doped with there is Nd in the emission spectrum of the embodiment 3 of trivalent rare earth ionses3+Characteristic absorption outside,
The luminescent spectrum diagram shape of embodiment 4, embodiment 5 and embodiment 6 is compared with Fig. 2 without significant change.And embodiment 3～6 is all
With long afterglow qualities.
Embodiment 7
According to BaCO3(analysis is pure), SrCO3(analysis is pure), Yb2O3(analysis is pure) and Tb4O7(analysis pure) mol ratio is
The ︰ 0.005 of 1.52 ︰, 0.4 ︰ 0.03, respectively feeding above-mentioned raw materials are ground, be dried after reinstall corundum crucible, in high temperature furnace
It is interior, in H2/N2(gas content ratio is H to gaseous mixture2︰ N2=5 ︰ 95, gas flow rate is 100mL/min) in 1300 DEG C of sintering 3h,
Along with the furnace cooling obtains Yb to room temperature2+And Tb3+The Ba of doping1.6Sr0.4SiO4Persursor material.Then by this precursor and Si3N4
With AlN according to the mixing of amount that mol ratio is the ︰ 2 of 1 ︰ 3, be ground, be dried after reinstall in boron nitride crucible, be put into high temperature furnace
It is interior, in H2/N2(gas content ratio is H to gaseous mixture2︰ N2=5 ︰ 95, gas flow rate is 100mL/min) in 1600 DEG C of sintering 6h,
Along with the furnace cooling obtains required long after glow luminous material after grinding to after room temperature taking-up.
The material obtained in embodiment 7 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) it is consistent, obvious miscellaneous peak is not observed.
The fluorescent material obtained in embodiment 7 is analyzed using XRF, under 300nm ultraviolet excitations
To its emission spectrum compared with Fig. 2 without significant change.After 254nm ultraviolet excitations are stopped, having higher than the sample of embodiment 1
Afterglow intensity and longer persistence.
Embodiment 8
According to BaCO3(analysis is pure), SrCO3(analysis is pure), Yb2O3(analysis is pure) and Er2O3(analysis pure) mol ratio is
The ︰ 0.01 of 1.52 ︰, 0.4 ︰ 0.03, respectively feeding above-mentioned raw materials are ground, be dried after reinstall corundum crucible, be put into high temperature furnace
It is interior, in H2/N2(gas content ratio is H to gaseous mixture2︰ N2=5 ︰ 95, gas flow rate is 100mL/min) in 1300 DEG C of sintering 3h,
Along with the furnace cooling obtains Yb to room temperature2+And Er3+The Ba of doping1.6Sr0.4SiO4Persursor material.Then by this precursor and Si3N4
With AlN according to the mixing of amount that mol ratio is the ︰ 2 of 1 ︰ 3, be ground, be dried after reinstall in boron nitride crucible, be put into high temperature furnace
It is interior, in H2/N2(gas content ratio is H to gaseous mixture2︰ N2=5 ︰ 95, gas flow rate is 100mL/min) in 1600 DEG C of sintering 6h,
Along with the furnace cooling obtains required long after glow luminous material after grinding to after room temperature taking-up.
The material obtained in embodiment 8 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) it is consistent, obvious miscellaneous peak is not observed.
The fluorescent material obtained in embodiment 8 is analyzed using XRF, under 300nm ultraviolet excitations
To its emission spectrum compared with Fig. 2, except there is Er at 523nm3+F-f characteristic absorptions beyond, without other significant changes.
After 254nm ultraviolet excitations 2min and stopping, embodiment 8 has higher afterglow intensity and longer persistence.Such as Fig. 4 institutes
Show, the attenuation curve of embodiment 8 and embodiment 1.
Embodiment 9
According to BaCO3(analysis is pure), SrCO3(analysis is pure), Si3N4(analysis is pure), AlN (analysis is pure), Yb2O3(analysis is pure)
And Tb4O7(analysis is pure) mol ratio is the ︰ 0.005 of 1.52 ︰, 0.4 ︰, 3 ︰, 2 ︰ 0.03, and respectively above-mentioned raw materials are ground, are dried by feeding
After reinstall boron nitride crucible, be put in high temperature furnace, in H2/N2(gas content ratio is H to gaseous mixture2︰ N2=5 ︰ 95, gas stream
Speed be 100mL/min) in 1600 DEG C sintering 6h, along with the furnace cooling to room temperature taking-up after grind after obtain needed for long-persistence luminous material
Material.
The material obtained in embodiment 9 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) it is consistent, obvious miscellaneous peak is not observed.
The fluorescent material obtained in embodiment 9 is analyzed using XRF, under 300nm ultraviolet excitations
To its emission spectrum compared with Fig. 2, without significant change.After 254nm ultraviolet excitations are stopped, embodiment 9 equally shows orange
Red long-afterglow property.
Claims (9)
1. a kind of orange light long lad phosphor, it is characterised in that its structural formula is as follows：
M1-x-yAlSi5O2N7:Ybx,Lny；
Wherein, 0.001≤x≤0.1,0≤y≤0.1；M is including at least at least one in Ba, and Mg, Ca, Sr, Ba；Ln is
At least one in Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm.
2. the preparation method of orange light long lad phosphor as claimed in claim 1, it is characterised in that it is comprised the following steps that：
By M presomas, Yb presomas, Ln precursors, Al presomas and Si presomas in reducing atmosphere in 1200～1800 DEG C
Lower calcining；Or
First under reducing atmosphere sintering obtains Yb2+And Ln3+The silicate compound of the M metals of doping, then with Si presomas and Al
Presoma is sintered again under reducing atmosphere in 1200～1800 DEG C.
3. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the M presomas are selected from M
Carbonate, the oxide of M, the nitrate of the oxalates of M and M at least one.
4. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the Yb presomas are selected from
At least one in the nitrate of the carbonate of Yb, the oxide of Yb, the oxalates of Yb and Yb.
5. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the Ln presomas are selected from
At least one in the nitrate of the carbonate of Ln, the oxide of Ln, the oxalates of Ln and Ln.
6. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the Al presomas are selected from
At least one in the oxide of Al and the nitrate of Al.
7. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the Si presomas are selected from
At least one in the oxide of Si, the nitride of Si.
8. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the reducing atmosphere is selected from
Ammonia or nitrogen hydrogen mixeding gas.
9. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the elder generation is in reducing atmosphere
The temperature of lower sintering is 1200～1800 DEG C, and the time of sintering is 3～15h.
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| CN114058371A (en) * | 2021-12-10 | 2022-02-18 | 南昌工程学院 | Yellow light long afterglow luminescent material and preparation method and application thereof |
| CN114907841A (en) * | 2022-05-23 | 2022-08-16 | 南昌工程学院 | Sm 2+ Activated near-infrared luminescent material and preparation method and application thereof |
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| CN105567235A (en) * | 2016-02-19 | 2016-05-11 | 厦门大学 | Nitric oxide red long-lasting phosphor material and preparation method thereof |
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| CN105567235A (en) * | 2016-02-19 | 2016-05-11 | 厦门大学 | Nitric oxide red long-lasting phosphor material and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| ZHUANG YIXI: "Study on Trap Levels in SrSi2AlO2N3:Eu2+,Ln3+ Persistent Phosphors Based on Host-Referred Binding Energy Scheme and Thermoluminescence Analysis", 《INORGANIC CHEMISTRY》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114058371A (en) * | 2021-12-10 | 2022-02-18 | 南昌工程学院 | Yellow light long afterglow luminescent material and preparation method and application thereof |
| CN114907841A (en) * | 2022-05-23 | 2022-08-16 | 南昌工程学院 | Sm 2+ Activated near-infrared luminescent material and preparation method and application thereof |
| CN114907841B (en) * | 2022-05-23 | 2023-05-26 | 南昌工程学院 | Sm (Sm) 2+ Activated near infrared luminescent material, preparation method and application thereof |
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