CN106634976B - A kind of orange light long lad phosphor and preparation method thereof - Google Patents
A kind of orange light long lad phosphor and preparation method thereof Download PDFInfo
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Abstract
A kind of orange light long lad phosphor and preparation method thereof, is related to fluorescent powder.Orange light long lad phosphor structural formula are as follows: M1‑x‑ yAlSi5O2N7:Ybx,Lny；Wherein, 0.001≤x≤0.1,0≤y≤0.1；M includes at least at least one of Ba and Mg, Ca, Sr, Ba etc.；Ln is at least one of Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm etc..Preparation: M presoma, Yb presoma, Ln precursor, Al presoma and Si presoma are calcined at 1200~1800 DEG C in a reducing atmosphere；Or first sintering obtains Yb under reducing atmosphere2+And Ln3+The silicate compound of the M metal of doping, then be sintered again in 1200~1800 DEG C under reducing atmosphere with Si presoma and Al presoma.
Description
Technical field
The present invention relates to fluorescent powders, more particularly, to a kind of orange light long lad phosphor and preparation method thereof.
Background technique
Long-afterglow material as a kind of energy storage material, have can after excitation light source stopping the characteristic of continuous illumination and
By people's extensive concern, since being paid close attention to and being studied by researcher at the end of the 20th century, blue and green long afterglow material obtained compared with
Good development, and mostly using aluminate as matrix based on.Such as commercial blue long afterflow (CaAl2O4:Eu2+,Nd3+) and
Green long afterglow (SrAl2O4:Eu2+,Dy3+) persistence of material can be more than 10h (reference literature 1 and 2).And more long wave
Long long-afterglow material, opposite type is less if the long-afterglow material of feux rouges and infrared light, and long-persistence luminous performance
It is relatively poor, furthermore due to feux rouges and infrared light long-afterglow material in recent years in terms of show it is strong
Competitiveness.So the long-afterglow material of exploitation and development long wavelength are of great significance.
From principle of luminosity, it is desirable to obtain red long afterglow luminous material, active ions generally can be Eu2+, Eu3 +, Pr3+And Cr3+Deng.Such as the Eu that document 3 is reported2+The CaS material of activation can be shown after ultraviolet light energy storage
Peak value is the lasting feux rouges persistent quality of 650nm.For another example reported in document 4 in Y2O2S:Eu3+,Ti4+,Mg2+In equally can
Obtaining long afterglow is Eu3+Characteristic emission long afterglow phenomenon.In document 5, peak value is that 611nm feux rouges long afterglow phenomenon can be
La2Ti2O7:Pr3+Middle realization, and persistence can be more than 1h.It is above rare earth ion doped red long-afterglow material
Material.In recent years, the feux rouges long after glow luminous material of transition metal activation has been similarly obtained some development, and Photobiology at
The fields such as picture have obtained certain application, the feux rouges long-afterglow material Zn as obtained in document 63Ga2Ge2O10:Cr3+, ultraviolet
After light (254nm) irradiation, Cr can be shown3+The long afterglow qualities of characteristic emission.In spite of part red long afterglow material
Some development are obtained, but type lacks relatively, furthermore the Y due to reporting respectively in such as document 3 and 42O2S:Eu3+,Ti4 +,Mg2+And CaS:Eu2+Feux rouges long-afterglow material belongs to sulfide, and poor water resistance and unstable property restrict its development.
Therefore the stable long after glow luminous material of exploitation property is of great significance.And nitrogen oxides is typically exhibited as luminescent material
Excellent stability.In addition, developing development of the feux rouges long-afterglow material of the new centre of luminescence for long after glow luminous material
It is critically important, and with Yb2+The patent document of long after glow luminous material as the centre of luminescence then seldom has been reported that.
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.
Summary of the invention
The object of the present invention is to provide it is simple, high-efficient and be conducive to industrialized production be suitable for white light LEDs and the sun
A kind of orange light long lad phosphor and preparation method thereof of energy battery.
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 one in Ba and Mg, Ca, Sr, Ba etc.
Kind；Ln is at least one of Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm etc..
The orange light long lad phosphor the preparation method is as follows:
By M presoma, Yb presoma, Ln precursor, Al presoma and Si presoma in a reducing atmosphere in 1200~
It is calcined at 1800 DEG C；Or
First sintering obtains Yb under reducing atmosphere2+And Ln3+The silicate compound of the M metal of doping, then with Si presoma
It is sintered again in 1200~1800 DEG C under reducing atmosphere with Al presoma.
The M presoma can be selected from least one in nitrate of the carbonate of M, the oxide of M, the oxalates of M and M etc.
Kind；
The Yb presoma can 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 presoma can 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 presoma can be selected from least one of oxide of Al and the nitrate of Al etc.；
The Si presoma can be selected from least one of nitride of the oxide of Si, Si etc.；
The reducing atmosphere can be selected from ammonia or nitrogen hydrogen mixeding gas.
The temperature that the elder generation is sintered under reducing atmosphere can be 1200~1800 DEG C, and the time of sintering can be 3~15h.
The present invention provides a kind of orange light long-afterglow materials and preparation method thereof.The long lad phosphor has completely new
Chemical composition, with Yb2+As activator.M can be improved by the doping of trivalent rare earth ions1-x-yAlSi5O2N7:Yb2+It is remaining
Brightness intensity and time.The fluorescent powder can be excited by the light in 200~480nm wave-length coverage and launch peak wavelength positioned at 615
The orange light of~625nm range, stop the wave band exciting light shine after, can generate it is long-persistence luminous, to make the phosphor
Material can store ultraviolet light and purplish blue light is converted into orange light.Long-afterglow fluorescent powder, preparation method thereof provided by the invention is simple, chemical
Performance is stablized, the application scenarios suitable for white light LEDs, solar battery or biomarker.
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of 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 under 300nm excitation；
Fig. 3 is the length of the different time after 254nm excitation stops of long after glow luminous material 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, irradiates 2min by 254nm ultraviolet light
Afterwards, the long afterglow attenuation curve measured.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, following embodiment is only section Example of the invention.
Embodiment 1
According to BaCO3(analysis is pure), SiO2(analysis is pure) and Yb2O3(analysis is pure) molar ratio is 1.94 ︰, 1 ︰ 0.03, respectively
Above-mentioned raw materials are ground by feeding, dry after be reloaded into corundum crucible, in high temperature furnace, in H2/N2Gaseous mixture (gas content
Ratio is H2︰ N2=5 ︰ 95, gas flow rate 100mL/min) in 1300 DEG C of sintering 3h, furnace cooling to room temperature obtains Yb2+It mixes
Miscellaneous Ba2SiO4Persursor material.Then by this precursor and Si3N4It is mixed with AlN according to the amount that molar ratio is 1 ︰, 3 ︰ 2, grinding
It mixes, be reloaded into boron nitride crucible after drying, is put into high temperature furnace, in H2/N2(gas content ratio is H to gaseous mixture2︰ N2=
5 ︰ 95, gas flow rate 100mL/min) in 1600 DEG C of sintering 6h, furnace cooling to room temperature take out after grind after obtain it is required
Long after glow luminous material.
Material obtained in embodiment 1 is analyzed using X-ray diffraction, obtains its X ray diffracting spectrum, such as Fig. 1
It is shown.It is inquired in international crystallographic data library, confirming this map and belonging to rhombic system space group is Imm2's and chemical group
As BaAlSi5O2N7Standard diagram (ICSD 240276) unanimously, apparent miscellaneous peak is not observed.
Fluorescent material obtained in embodiment 1 is analyzed using Fluorescence Spectrometer, under 300nm ultraviolet excitation
Emission peak is located at 615nm, under 254nm ultraviolet excitation, can show Characteristics of Long Luminosity.It can be seen that the fluorescent powder energy quilt
Ultraviolet excitation and emit orange light, to make the fluorescent material that 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) molar ratio is
1.54 ︰, 0.4 ︰, 1 ︰ 0.03, respectively feeding above-mentioned raw materials are ground, dry after be reloaded into corundum crucible, in high temperature furnace,
H2/N2(gas content ratio is H to gaseous mixture2︰ N2=5 ︰ 95, gas flow rate 100mL/min) in 1300 DEG C of sintering 3h, with furnace
It is cooled to room temperature, obtains Yb2+The Ba of doping1.6Sr0.4SiO4Persursor material.Then by this precursor and Si3N4With AlN according to
Molar ratio be 1 ︰, 3 ︰ 2 amount mix, be ground, dry after be reloaded into boron nitride crucible, be put into high temperature furnace, in H2/N2It is mixed
Closing gas, (gas content ratio is H2︰ N2=5 ︰ 95, gas flow rate 100mL/min) in 1600 DEG C of sintering 6h, furnace cooling to room
Temperature obtains required long after glow luminous material after grinding after taking out.
Material obtained in embodiment 2 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) unanimously, apparent miscellaneous peak is not observed.
Fluorescent material obtained in embodiment 2 is analyzed using Fluorescence Spectrometer, under 300nm ultraviolet excitation
To its launching light spectrogram, as shown in Figure 2.It can be seen that the fluorescent powder can emit orange light by ultraviolet excitation, to make the fluorescence
Material can convert uv light into orange light.In addition, the sample is removed exciting light after 254nm ultraviolet light excites 2min
Source, the twilight sunset emission spectrum of test sample different time.As shown in figure 3, the twilight sunset emission spectrum 1, after 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) molar ratio is 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, dry after be reloaded into corundum crucible, be put into high temperature furnace, in H2/N2Mixing
(gas content ratio is H to gas2︰ N2=5 ︰ 95, gas flow rate 100mL/min) in 1300 DEG C of sintering 3h, furnace cooling 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 be 1 ︰, 3 ︰ 2 amount mix, be ground, dry after be reloaded into boron nitride crucible, in high temperature furnace, in H2/N2Gaseous mixture
(gas content ratio is H2︰ N2=5 ︰ 95, gas flow rate 100mL/min) in 1600 DEG C of sintering 6h, furnace cooling takes to room temperature
Required long after glow luminous material is obtained after grinding after out.
Material obtained in embodiment 3~6 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) unanimously, apparent miscellaneous peak is not observed.
Fluorescent material obtained in embodiment 3~6 is analyzed using Fluorescence Spectrometer, in 300nm ultraviolet excitation
Under obtain its emission spectrum.Except there are Nd in the emission spectrum for the embodiment 3 for being co-doped with trivalent rare earth ions3+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) molar ratio is
1.52 ︰, 0.4 ︰, 0.03 ︰ 0.005, respectively feeding above-mentioned raw materials are ground, dry after be reloaded into 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 100mL/min) in 1300 DEG C of sintering 3h,
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 molar ratio be 1 ︰, 3 ︰ 2 amount mix, be ground, dry after be reloaded into 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 100mL/min) in 1600 DEG C of sintering 6h,
Furnace cooling obtains required long after glow luminous material after grinding after taking out to room temperature.
Material obtained in embodiment 7 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) unanimously, apparent miscellaneous peak is not observed.
Fluorescent material obtained in embodiment 7 is analyzed using Fluorescence Spectrometer, under 300nm ultraviolet excitation
To its emission spectrum without significant change compared with Fig. 2.After stopping 254nm ultraviolet excitation, have than 1 sample of embodiment stronger
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) molar ratio is
1.52 ︰, 0.4 ︰, 0.03 ︰ 0.01, respectively feeding above-mentioned raw materials are ground, dry after be reloaded into 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 100mL/min) in 1300 DEG C of sintering 3h,
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 molar ratio be 1 ︰, 3 ︰ 2 amount mix, be ground, dry after be reloaded into 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 100mL/min) in 1600 DEG C of sintering 6h,
Furnace cooling obtains required long after glow luminous material after grinding after taking out to room temperature.
Material obtained in embodiment 8 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) unanimously, apparent miscellaneous peak is not observed.
Fluorescent material obtained in embodiment 8 is analyzed using Fluorescence Spectrometer, under 300nm ultraviolet excitation
To its emission spectrum compared with Fig. 2, in addition to there is Er at 523nm3+F-f characteristic absorption other than, without other significant changes.?
254nm ultraviolet excitation 2min and stop after, embodiment 8 have stronger afterglow intensity and longer persistence.Such as Fig. 4 institute
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) molar ratio is 1.52 ︰, 0.4 ︰, 3 ︰, 2 ︰, 0.03 ︰ 0.005, and above-mentioned raw materials are ground, dry by feeding respectively
After be reloaded into boron nitride crucible, be put into high temperature furnace, in H2/N2(gas content ratio is H to gaseous mixture2︰ N2=5 ︰ 95, gas stream
Speed is 1600 DEG C of sintering 6h in 100mL/min), and furnace cooling to room temperature obtains required long-persistence luminous material after grinding after taking out
Material.
Material obtained in embodiment 9 is analyzed using X-ray diffraction, confirm the diffracting spectrum of this sample with
BaAlSi5O2N7Standard diagram (ICSD 240276) unanimously, apparent miscellaneous peak is not observed.
Fluorescent material obtained in embodiment 9 is analyzed using Fluorescence Spectrometer, under 300nm ultraviolet excitation
To its emission spectrum compared with Fig. 2, no significant change.After stopping 254nm ultraviolet excitation, embodiment 9 equally shows orange
Red long-afterglow property.
Claims (7)
1. a kind of orange red 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 includes at least at least one of Ba and Mg, Ca, Sr, Ba；Ln is
At least one of Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm.
2. the preparation method of orange light long lad phosphor as described in claim 1, it is characterised in that specific step is as follows:
By M presoma, Yb presoma, Ln precursor, Al presoma and Si presoma in a reducing atmosphere with 1200~1800 DEG C
Lower calcining；The Al presoma is selected from least one of oxide or nitrate of Al of aluminium nitride or Al, wherein aluminium nitride
It is necessary；Or
First sintering obtains Yb under reducing atmosphere2+And Ln3+The silicate compound of the M metal of doping, then with Si presoma and Al
Presoma is sintered for 1200~1800 DEG C again under reducing atmosphere.
3. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the M presoma is selected from M
At least one of carbonate, the oxide of M, the oxalates of M and the nitrate of M.
4. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the Yb presoma is selected from
At least one of the carbonate of Yb, the oxide of Yb, the oxalates of Yb and nitrate of Yb.
5. the preparation method of orange light long lad phosphor as claimed in claim 2, it is characterised in that the Ln presoma is selected from
At least one of the carbonate of Ln, the oxide of Ln, the oxalates of Ln and nitrate of Ln.
6. the preparation method of orange light long lad phosphor according to claim 2, it is characterised in that the reducing atmosphere choosing
From ammonia or nitrogen hydrogen mixeding gas.
7. the preparation method of orange light long lad phosphor according to claim 2, it is characterised in that the elder generation is in also Primordial Qi
The temperature being sintered under atmosphere is 1200 DEG C~1800 DEG C, and the time of sintering is 3~15h.
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