CN110452697A - It is a kind of to emit simultaneous feux rouges and the luminescent material of blue green light and preparation method thereof - Google Patents
It is a kind of to emit simultaneous feux rouges and the luminescent material of blue green light and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to luminescent material preparation technical fields, and in particular to a kind of to emit and feux rouges and the luminescent material of blue green light and preparation method thereof.The chemical composition of the luminescent material is xSm2O3·(1‑1.5x)ZrO2·(1‑2.5y)SiO2·yP2O5(x=0.002~0.12;y=0.001~0.1).Preparation method coats collosol and gel combination high-temperature calcination preparation process using nano material.After light-illuminating, the luminescent material can emitting bright red light, stop illumination after observe green light of turning blue within sustainable 12 hours or more in the dark.Fluorescence spectrum shows that the emission peak bands of a spectrum of the luminescent material are very wide.Materials chemistry property stabilized illumination of the present invention is had excellent performance, and can both develop can also be used as light storage ceramic material for fluorescent material or have both the material of standby fluorescence and light storage function.
Description
Technical field
The present invention relates to luminescent ceramic materials and preparation method thereof, in particular to a kind of to emit simultaneous feux rouges and blue green light
Luminescent material and preparation method thereof, belong to luminescent material preparation technical field.
Background technique
It is a kind of special embedded photoluminescent material that light-storing material, which is also known as long after glow luminous material, it, which can collect energy storage with releasing, to be
One, it is considered to be a kind of pollution-free, the novel illumination and display material of environmental protection and energy saving, the deep concern by people.Its traffic,
The fields such as military affairs, safety, electric appliance, building and information storage are using more and more extensive.People start from the research of light-storing material
Early 20th century.Madame Curie had found that element radium had long afterglow phenomenon at that time, was once used for illuminating material, but since radium element has
Radioactivity and stop using.Currently, common light-storing material mainly has sulfide, aluminate, silicate, phosphate etc..Silicic acid
Alkali long after glow luminous material stable system, the advantages such as material is cheap and easy to get, sintering temperature is low and be often used as long afterglow by people
The matrix of luminescent material.Chinese invention patent CN104073255A discloses a kind of Eu3+Adulterate A2ZrSi2O7(wherein A is alkali gold
Belong to) preparation method and application of blue-green silicic acid zirconates fluorescent powder；Chinese invention patent CN107129801A discloses a kind of Li+
Codope is come the method that improves silicate fluorescent powder long afterglow property, chemical expression Sr2MgSiO7:xEu2+yDy3+zLi+, Li+Doping increase Lacking oxygen, increase captured electronics, to improve persistence.For long after glow luminous material
For, select suitable matrix to be very important.Luminescent material x (Sm of the present invention2O3)·(1-1.5x)ZrO2·(1-2.5y)
SiO2·yP2O5(x=0.002~0.12;Y=0.001 ~ 0.1), with Sm3+And Zr4+As the common centre of luminescence, can emit and red
Light and blue green light, stable chemical performance, luminescent properties are excellent.Appropriate doping P5+And Sm3+, make mineralizer and reproducibility with NaF
High-temperature calcination under atmosphere, the stability and crystal property for being conducive to the luminescent properties for improving material and improving material.
Summary of the invention
Simultaneous feux rouges and the luminescent material of blue green light and preparation method thereof can be emitted the purpose of the present invention is to provide a kind of.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of luminescent material that can emit simultaneous feux rouges and blue green light, chemical composition xSm2O3·(1-1.5x)ZrO2·(1-
2.5y)SiO2·yP2O5(x=0.002~0.12; y= 0.001~0.1)。
Preparation method the following steps are included:
1) raw material ZrO is stoichiometrically weighed respectively2, ethyl orthosilicate, (NH4)2HPO4、Sm2O3, and press xSm2O3·
(1-1.5x)ZrO2·(1-2.5y)SiO2·yP2O5(x=0.002~0.12;Y=0.001 ~ 0.1) molar percentage be
0.3-1.0 mol% weighs mineralizer boric acid；
2) by volume it is that 1:1-5 is mixed with dehydrated alcohol ethyl orthosilicate, it is dilute that water progress appropriate is added after mixing
It releases, forms clear solution；
3) by (NH soluble easily in water described in step 1)4)2HPO4Dissolution of raw material is made into 2M concentration in water with spare；Take concentrated nitric acid slow
Slowly it is added drop-wise to Sm2O3In powder and until stirring while adding and making it completely dissolved, distilled water is added and dilutes 3-5 times, is then added
Fluxing agent boric acid is made into clear solution, spare；
4) by above step 1) the weighed nanometer ZrO of institute2, the clear solution of step 2, step 3) (NH4)2HPO4Solution and
Sm2O3The clear solution mixing prepared with boric acid, and pH value is adjusted between 1-6, it is stirred continuously in 60-95 DEG C of water-bath, to
It takes out, is placed in drying box 4-8 hours dry at 100-120 DEG C after forming gel；
5) xerogel of step 4) is placed in crucible and is put into high temperature furnace, in weak reducing atmosphere (H2/N2Gaseous mixture
Body or CO) in, it is calcined 2-4 hours at 1100-1300 DEG C, a kind of luminescent material that can emit simultaneous feux rouges and blue green light is made
x(Sm2O3)·(1-1.5x)ZrO2·(1-2.5y)SiO2·yP2O5(x=0.002~0.12; y= 0.001~0.1)。
Remarkable advantage of the invention is:
Material prepared by the present invention after light-illuminating, the luminescent material can emitting bright red light, stop illumination after
Observe within sustainable 12 hours or more in dark green light of turning blue, fluorescence spectrum shows the emission peak bands of a spectrum of the luminescent material very
Width both has Zr4+Characteristic emission, but also with Sm3+Characteristic emission, Sm3+And Zr4+As the common centre of luminescence.A small amount of P5 +And Sm3+Doping introducing great role is played to material emission performance improvement.Materials chemistry property prepared by the present invention is steady
It is excellent to determine luminescent properties, can both develop can also be used as light storage ceramic material for fluorescent material or have both standby fluorescence and light storage function
The material of energy.
Detailed description of the invention
Fig. 1: 0.02Sm2O3·0.97ZrO2·0.875SiO2·0.05P2O5And 0.02Sm2O3·0.97ZrO2·SiO2
X-ray diffraction pattern；
Fig. 2: 0.02Sm2O3·0.97ZrO2·0.875SiO2·0.05P2O5Fluorescence spectra；
Fig. 3: 0.02Sm2O3·0.97ZrO2·0.875SiO2·0.05P2O5And ZrO2·SiO2Decay of afterglow curve；
Fig. 4: 0.02Sm2O3·0.97ZrO2·0.875SiO2·0.05P2O5And ZrO2·SiO2Heat release curve.
Specific embodiment
Further to disclose rather than the present invention is limited, the present invention is described in further detail below in conjunction with example.
Embodiment 1
A kind of luminescent material that can emit simultaneous feux rouges and blue green light, chemical composition 0.01Sm2O3·0.985ZrO2·
0.75SiO2·0.1P2O5。
Preparation method the following steps are included:
1) raw material ZrO is stoichiometrically weighed respectively2, ethyl orthosilicate, (NH4)2HPO4、Sm2O3, and press
0.01Sm2O3·0.985ZrO2·0.75SiO2·0.1P2O5Molar percentage be 0.3 mol% weigh mineralizer boric acid；
2) by volume it is that 1:5 is mixed with dehydrated alcohol ethyl orthosilicate, it is dilute that water progress appropriate is added after mixing
It releases, forms clear solution；
3) by (NH soluble easily in water described in step 1)4)2HPO4Dissolution of raw material is made into 2M concentration in water with spare；Take concentrated nitric acid slow
Slowly it is added drop-wise to Sm2O3In powder and until stirring while adding and making it completely dissolved, distilled water is added and dilutes 3-5 times, is then added
Fluxing agent boric acid is made into clear solution, spare；
4) by above step 1) the weighed nanometer ZrO of institute2, the clear solution of step 2, step 3) (NH4)2HPO4Solution and
Sm2O3The clear solution mixing prepared with boric acid, and adjusting pH value is 6, is stirred continuously in 60 DEG C of water-bath, gel to be formed
After take out, be placed in drying box 4 hours dry at 100 DEG C；
5) xerogel of step 4) is placed in crucible and is put into high temperature furnace, in weak reducing atmosphere (H2/N2Gaseous mixture
Body or CO) in, it is calcined 4 hours at 1100 DEG C, a kind of luminescent material that can emit simultaneous feux rouges and blue green light is made
0.01Sm2O3·0.985ZrO2·0.75SiO2·0.1P2O5.After light-illuminating, the luminescent material can emitting bright it is red
Coloured light observes green light of turning blue in sustainable 6 hours or more in the dark after stopping illumination.
Embodiment 2
A kind of luminescent material that can emit simultaneous feux rouges and blue green light, chemical composition 0.1Sm2O3·0.85ZrO2·
0.975SiO2·0.01P2O5。
Preparation method the following steps are included:
1) raw material ZrO is stoichiometrically weighed respectively2, ethyl orthosilicate, (NH4)2HPO4、Sm2O3, and press 0.1Sm2O3·
0.85ZrO2·0.975SiO2·0.01P2O5Molar percentage be 1.0 mol% weigh mineralizer boric acid；
2) by volume it is that 1:4 is mixed with dehydrated alcohol ethyl orthosilicate, it is dilute that water progress appropriate is added after mixing
It releases, forms clear solution；
3) by (NH soluble easily in water described in step 1)4)2HPO4Dissolution of raw material is made into 2M concentration in water with spare；Take concentrated nitric acid slow
Slowly it is added drop-wise to Sm2O3In powder and until stirring while adding and making it completely dissolved, distilled water is added and dilutes 5 times, is then added and helps
Flux boric acid is made into clear solution, spare；
4) by above step 1) the weighed nanometer ZrO of institute2, the clear solution of step 2, step 3) (NH4)2HPO4Solution and
Sm2O3The clear solution mixing prepared with boric acid, and adjusting pH value is to be stirred continuously in 80 DEG C of water-bath between 3, it is to be formed
It takes out, is placed in drying box 6 hours dry at 110 DEG C after gel；
5) xerogel of step 4) is placed in crucible and is put into high temperature furnace, in weak reducing atmosphere (H2/N2Gaseous mixture
Body or CO) in, it is calcined 2 hours at 1300 DEG C, a kind of luminescent material that can emit simultaneous feux rouges and blue green light is made
0.1Sm2O3·0.85ZrO2·0.975SiO2·0.01P2O5.After light-illuminating, the luminescent material can emitting bright it is red
Coloured light observes green light of turning blue in sustainable 9 hours or more in the dark after stopping illumination.
Embodiment 3
A kind of luminescent material that can emit simultaneous feux rouges and blue green light, chemical composition 0.02Sm2O3·0.97ZrO2·
0.875SiO2·0.05P2O5。
Preparation method the following steps are included:
1) raw material ZrO is stoichiometrically weighed respectively2, ethyl orthosilicate, (NH4)2HPO4、Sm2O3, and press
0.02Sm2O3·0.97ZrO2·0.875SiO2·0.05P2O5Molar percentage be 1.0 mol% weigh mineralizer boric acid；
2) by volume it is that 1:5 is mixed with dehydrated alcohol ethyl orthosilicate, it is dilute that water progress appropriate is added after mixing
It releases, forms clear solution；
3) by (NH soluble easily in water described in step 1)4)2HPO4Dissolution of raw material is made into 2M concentration in water with spare；Take concentrated nitric acid slow
Slowly it is added drop-wise to Sm2O3In powder and until stirring while adding and making it completely dissolved, distilled water is added and dilutes 3-5 times, is then added
Fluxing agent boric acid is made into clear solution, spare；
4) by above step 1) the weighed nanometer ZrO of institute2, the clear solution of step 2, step 3) (NH4)2HPO4Solution and
Sm2O3The clear solution mixing prepared with boric acid, and adjusting pH value is 5, is stirred continuously in 95 DEG C of water-bath, gel to be formed
After take out, be placed in drying box 6 hours dry at 120 DEG C；
5) xerogel of step 4) is placed in crucible and is put into high temperature furnace, in weak reducing atmosphere (H2/N2Gaseous mixture
Body or CO) in, it is calcined 4 hours at 1200 DEG C, a kind of luminescent material that can emit simultaneous feux rouges and blue green light is made
0.02Sm2O3·0.97ZrO2·0.875SiO2·0.05P2O5.After light-illuminating, which can emitting bright
Red light observes green light of turning blue in sustainable 12 hours or more in the dark after stopping illumination.
Fig. 1 is 0.02Sm2O3·0.97ZrO2·0.875SiO2·0.05P2O5And 0.02Sm2O3·0.97ZrO2·SiO2
X-ray diffraction pattern.It is characterized by X-ray powder diffraction instrument, the results showed that the XRD of the long after glow luminous material
Map and standard diagram PDF#06-0266 are almost the same.After light-illuminating, the luminescent material can emitting bright red
Light, sustainable observe is turned blue green light 12 hours or more in the dark after stopping illumination.Fig. 2 is 0.02Sm2O3·
0.97ZrO2·0.875SiO2·0.05P2O5Fluorescence spectra.Fluorescence spectrum shows the emission peak spectrum of the luminescent material in figure
Band is very wide, wherein 453,466,481 nm belong to Zr4+Characteristic emission peak, belong to blue light scope；And 567 nm emission peaks belong to
Sm3+'s6H5/2-4G5/2Energy level transition is located at green range；603 nm and 615 nm emission peaks belong to Sm3+'s6H7/2-4G5/2
Energy level transition, and 650 nm and 660 nm emission peaks belong to Sm3+'s6H9/2-4G5/2Energy level transition, category feux rouges scope.
Fig. 3 is 0.02Sm2O3·0.97ZrO2·0.875SiO2·0.05P2O5And ZrO2·SiO2Decay of afterglow it is bent
Line.It can be seen from the figure that introducing Doped ions Sm3+And P5+The afterglow property of material can be improved significantly.Fig. 4 is
0.02Sm2O3·0.97ZrO2·0.875SiO2·0.05P2O5And ZrO2·SiO2Heat release curve.As can be seen from the figure draw
Enter Doped ions Sm3+And P5+The cold temperature deficiency concentration that material can be improved significantly, is conducive to changing for the luminescent properties of material
It is kind.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (5)
1. a kind of luminescent material that can emit simultaneous feux rouges and blue green light, it is characterised in that: the chemical composition of the luminescent material
For xSm2O3·(1-1.5x)ZrO2·(1-2.5y)SiO2·yP2O5, x=0.002 ~ 0.12, y=0.001 ~ 0.1.
2. a kind of luminescent material preparation method that can emit simultaneous feux rouges and blue green light as described in claim 1, feature exist
In: the following steps are included:
1) raw material ZrO is stoichiometrically weighed respectively2, ethyl orthosilicate, (NH4)2HPO4、Sm2O3, and press xSm2O3·(1-
1.5x)ZrO2·(1-2.5y)SiO2·yP2O5Molar percentage be 0.3-1.0 mol% weigh mineralizer boric acid；
2) by volume it is that 1:1-5 is mixed with dehydrated alcohol ethyl orthosilicate, it is dilute that water progress appropriate is added after mixing
It releases, forms clear solution；
3) by (NH soluble easily in water described in step 1)4)2HPO4Dissolution of raw material is made into 2M concentration in water with spare；Take concentrated nitric acid slow
Slowly it is added drop-wise to Sm2O3In powder and until stirring while adding and making it completely dissolved, distilled water is added and dilutes 3-5 times, is then added
Fluxing agent boric acid is made into clear solution, spare；
4) by above step 1) the weighed nanometer ZrO of institute2, the clear solution of step 2, step 3) (NH4)2HPO4Solution and
Sm2O3The clear solution mixing prepared with boric acid, and pH value is adjusted between 1-6, it is stirred continuously in 60-95 DEG C of water-bath,
It takes out, is placed in drying box dry after gel to be formed；
5) xerogel of step 4) is placed in crucible and is put into high temperature furnace, calcined in weak reducing atmosphere, institute is made
State the luminescent material that can emit simultaneous feux rouges and blue green light.
3. preparation method according to claim 2, it is characterised in that: drying described in step (4) is specially 100-120 DEG C
It is 4-8 hours dry.
4. preparation method according to claim 2, it is characterised in that: step (5) the weak reducing atmosphere is H2And N2
Mixed gas or CO gas.
5. preparation method according to claim 2, it is characterised in that: step (5) calcining is specially in 1100-1300
It is calcined 2-4 hours at DEG C.
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| CN111171816A (en) * | 2020-01-08 | 2020-05-19 | 闽南师范大学 | Yellow-green long-afterglow luminescent material and preparation method thereof |
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