CN106554777B - A kind of coloration is with adjustable luminescent material of temperature and the preparation method and application thereof - Google Patents
A kind of coloration is with adjustable luminescent material of temperature and the preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a kind of colorations with adjustable luminescent material of temperature and the preparation method and application thereof.Chemical composition expression are as follows: Lu(1‑x)PrxNbO4, x is active ions Pr in formula3+Opposite matrix rare earth ion Lu3+The molar content accounted for, value range: 0.001≤x≤0.10.Present invention utilizes LuNbO4NbO in matrix4 3‑The effective of group shines, and crystallinity is high, and luminous mass is good.Due to containing rare earth ion Lu in host material3+, be conducive to Pr3+The doping of ion.LuNbO4Host emission blue light, Pr3+In LuNbO4Mainly emit feux rouges in matrix.As the temperature rises, matrix is to Pr3+The energy transfer efficiency of ion is gradually increased, Pr3+Red emission temperature quenching does not occur yet in higher temperature, cause blue emission gradually to weaken, red emission gradually increases.The luminescent material increases the controllability with luminescent chromaticity with temperature, does not need to avoid the light absorption between different luminescent materials with the luminescent material mixing of a variety of different colorations when preparing light-sensitive device.Synthesis step is simple, easily operated.
Description
Technical field
The invention belongs to embedded photoluminescent materials and lighting display technology field.More particularly, to a kind of coloration with temperature
Adjustable luminescent material and the preparation method and application thereof.
Background technique
Luminescent material it is widely used, realize there are many luminous excitation energy forms of luminescent material, such as ultraviolet-visible
Light, gas discharge, electric field, X-ray, cathode-ray etc..With the extensive use of high-quality illumination and display device, preparation method
Simply, luminous efficiency is high, rare earth luminescent material with long service life is more and more important.
Shine is that interior of articles absorbs the process that light radiation is converted into after energy in some way.When object is by such as light
Irradiation, after extra electric field or beam bombardment, the energy that material absorbs is released by way of light.It is most important to shine
There are two types of forms, absorbs excitation energy one is host material and is converted into light emitting species release.Another kind is that matrix will absorb
Energy transmission to active ions, realized and shone by the radiation transistion between active ions difference energy level.Such as luminescent material
YNbO4:Eu3+/Tb3+, LaNbO4:Eu3+/Tb3+, matrix YNbO4And LaNbO4Black light can be absorbed and emit blue light, base
Matter transfers energy to the rare earth ion Eu of doping3+And Tb3+Afterwards, it is made to issue bright feux rouges and green light respectively.Refering to document
1:X.M Liu, Y. Lu, C. Chen, et al., J. Phys. Chem. C, 2014,118,27516-27524. ginseng
Read document 2:K. Li, Y. Zhang, X.J. Li, et al., Phys. Chem. Chem. Phys., 2015,17,
4283-4292.
Rare earth niobates (LnNbO4) due to good chemical stability, high thermal stability and radiation conversion effect
Rate, self-activating centre of luminescence NbO4 3-, and be easy to the advantages that rare earth ion doped and be widely used in field of light emitting materials.
Under near ultraviolet excitation, Pr3+Ion have feature blue green light (3P0→3H4) and feux rouges (1D2→3H4) transmitting, in closed shell transition
Metal niobates LuNbO4In matrix, charge migration Pr between valence3+ + Nb5+↔ Pr4+ + Nb4+State makes3P0Excitation state is effectively sudden
It goes out,1D2Transmitting enhancing, to make Pr3+In LuNbO4Mainly emit feux rouges in matrix.Temperature is increased, matrix is to Pr3+The energy of ion
Transmission efficiency enhancing is measured, causes the transmitting ratio of blue light and feux rouges to change, luminescent chromaticity may be implemented and continuously may be used with temperature
It adjusts.
Summary of the invention
It is high that the object of the present invention is to provide a kind of crystallinity, and luminous mass is good, and preparation method is simple, pollution-free and illuminant colour
The Pr that degree can be continuously adjusted with temperature3+The luminescent material that the coloration of activation is continuously adjusted with temperature.
It is a further object to provide the preparation methods of above-mentioned luminescent material.
Coloration of the invention has following chemical composition expression: Lu with the luminescent material that temperature is continuously adjusted(1-x)
PrxNbO4, x is active ions Pr in formula3+Opposite matrix rare earth ion Lu3+The molar content accounted for, value range: 0.001
≤x≤0.10。
Host material selected by the present invention is LuNbO4, active ions are trivalent rare earth praseodymium ion Pr3+.Swash in black light
It gives, host emission blue light, Pr3+Mainly emit feux rouges in the matrix.500 K are increased to from 300 K with temperature, blue light and red
Light emitting ratio changes, and luminescent chromaticity is continuously adjusted out of purple-purple pink colour-pink range.
Under the near ultraviolet excitation that wavelength is 240 ~ 290 nm at room temperature (300 K), work as Pr3+The Mole percent of doping
Content is 0.001≤x≤0.10, and luminous chromaticity coordinate value is x=0.191 ~ 0.242, y=0.073 ~ 0.143
Purple.
The luminescent chromaticity is adjustable with temperature, with Lu(1-x)PrxNbO4For (x=0.005) sample, it is in wavelength
Under the near ultraviolet excitation of 240 ~ 290 nm, when temperature T be the K of 300 K≤T≤375, luminous chromaticity coordinate value be x=
The purple of 0.225 ~ 0.324, y=0.091 ~ 0.151；When temperature T is the K of 375 K < T≤450, luminous coloration is sat
Scale value is the opera pink of x=0.324 ~ 0.446, y=0.151 ~ 0.230；When temperature T be the K of 450 K < T≤500,
Its luminous chromaticity coordinate value is the pink of x=0.446 ~ 0.474, y=0.230 ~ 0.255.
Above-mentioned coloration includes the following steps: with the preparation method of the adjustable luminescent material of temperature
S1. according to chemical composition embodied in chemical composition expression formula described in claim 1, raw material is accurately weighed, is filled
Divide ground and mixed uniform, obtains mixture；
S2. it by mixture tabletting, is then placed in reaction vessel, in a reducing atmosphere, is placed in temperature programming in resistance furnace
And it roasts, cooled to room temperature；
S3. step S2 products therefrom is taken out into grinding to get product is arrived.
Wherein, raw material described in step S1 are as follows: luteium oxide, praseodymium oxide and niobium oxide.
Preferably, being fully ground described in step S1 uniformly mixed is that dehydrated alcohol is added in agate mortar as medium
It is uniform to carry out ground and mixed.
Preferably, tabletting described in step S2 is that tabletting is carried out in cold isostatic press, and mixture obtained by step S1 is existed
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure.
Furthermore it is preferred that reaction vessel described in step S2 is corundum crucible.
Preferably, reducing atmosphere described in step S2 refers to the carbon monoxide atmosphere generated by heating carbon block.
Preferably, the heating-up time described in step S2 is 2-5 h.
It is highly preferred that the heating-up time described in step S2 is 4 h.
Preferably, the condition of roasting described in step S2 is 1200 ~ 1300 DEG C, roasts 4-10 h.
It is highly preferred that the condition of roasting described in step S2 is 1220 ~ 1260 DEG C, 5 h are roasted.
Most preferably, the condition of roasting described in step S2 is 1250 DEG C, roasts 5 h.
Compared with prior art, the invention has the following beneficial effects:
1. present invention utilizes LuNbO4NbO in matrix4 3-The effective of group shines, and crystallinity is high, and luminous mass is good.
2. due to containing rare earth ion Lu in host material3+, be conducive to Pr3+The doping of ion.
3. LuNbO4Host emission blue light, Pr3+In LuNbO4Mainly emit feux rouges in matrix.
4. with Pr3+The raising of doping concentration, matrix is to Pr3+The energy transfer efficiency of ion is gradually increased, Pr3+It is red
Light emitting (1D2→3H4Transition) in doping x=0.005, generation concentration is quenched, and cause blue emission gradually to weaken, feux rouges hair
It penetrates first to enhance and weaken afterwards.Work as Pr3+Doping be 0.001≤x≤0.10 when, LuNbO4:xPr3+In 261nm near ultraviolet excitation
Under luminescent chromaticity coordinate be respectively positioned on purple light area.
5. as the temperature rises, matrix is to Pr3+The energy transfer efficiency of ion is gradually increased, Pr3+Red emission
(1D2→3H4Transition) at higher temperature (450-500 K) temperature quenching does not occur yet, cause blue emission gradually to weaken, it is red
Light emitting gradually increases.Therefore, which increases the controllability with luminescent chromaticity with temperature, is preparing light-sensitive device
When do not need luminescent material mixing with a variety of different colorations, avoid the light absorption between different luminescent materials.
6. luminescent material synthesis step of the invention is simple, easily operated.
Detailed description of the invention
A is excitation spectrum of the luminescent material of (embodiment 5) of the invention when monitoring 613 nm in Fig. 1, and b is the present invention
Emission spectrum of (embodiment 5) luminescent material under 261 nm near ultraviolet excitations.
Fig. 2 is the luminescent material of (embodiment 1,3,5,10,11,14 and 19) of the invention in 261 nm black lights
The lower emission spectrum of excitation is host emission (blue light, 390 nm) and Pr in interior illustration3+Ion1D2→3H4Transition transmitting is (red
Light, 613 nm) relative intensity with Pr3+The raised trend chart of doping concentration.
Fig. 3 is the luminescent material of (embodiment 1,3,5,10,11,14 and 19) of the invention in 261 nm black lights
Position view of the chromaticity coordinates in 1931 chromatic diagram of CIE under excitation.
Fig. 4 is 5 luminescent material of the embodiment transmitting light of temperature from 300 K to 500 K under 261 nm near ultraviolet excitations
It composes, is matrix blue emission and Pr in interior illustration3+Ion1D2→3H4The integrated intensity of transition red emission is with the raised change of temperature
Change tendency chart.
Fig. 5 be 5 luminescent material of embodiment under 261 nm near ultraviolet excitations temperature from 300 K to the chromaticity coordinates of 500 K
Position view in 1931 chromatic diagram of CIE.
Specific embodiment:
The present invention is further illustrated below in conjunction with Figure of description and specific embodiment, but embodiment is not to the present invention
It limits in any form.Unless stated otherwise, the present invention uses reagent, method and apparatus routinely try for the art
Agent, method and apparatus.
Unless stated otherwise, following embodiment agents useful for same and material are commercially available.
Embodiment 1:
Weigh luteium oxide (Lu2O3) 0.5963 g, praseodymium oxide (Pr6O11) 0.0005 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.999Pr0.001NbO4。
Embodiment 2:
Weigh luteium oxide (Lu2O3) 0.5957 g, praseodymium oxide (Pr6O11) 0.0010 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.998Pr0.002NbO4。
Embodiment 3:
Weigh luteium oxide (Lu2O3) 0.5951 g, praseodymium oxide (Pr6O11) 0.0015 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.997Pr0.003NbO4。
Embodiment 4:
Weigh luteium oxide (Lu2O3) 0.5945 g, praseodymium oxide (Pr6O11) 0.0020 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.996Pr0.004NbO4。
Embodiment 5:
Weigh luteium oxide (Lu2O3) 0.5939g, praseodymium oxide (Pr6O11) 0.0026 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.995Pr0.005NbO4。
Embodiment 6:
Weigh luteium oxide (Lu2O3) 0.5933 g, praseodymium oxide (Pr6O11) 0.0031 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.994Pr0.006NbO4。
Embodiment 7:
Weigh luteium oxide (Lu2O3) 0.5927 g, praseodymium oxide (Pr6O11) 0.0036 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.993Pr0.007NbO4。
Embodiment 8:
Weigh luteium oxide (Lu2O3) 0.5921 g, praseodymium oxide (Pr6O11) 0.0041 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.992Pr0.008NbO4。
Embodiment 9:
Weigh luteium oxide (Lu2O3) 0.5915 g, praseodymium oxide (Pr6O11) 0.0046 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.991Pr0.009NbO4。
Embodiment 10:
Weigh luteium oxide (Lu2O3) 0.5909 g, praseodymium oxide (Pr6O11) 0.0051 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.99Pr0.01NbO4。
Embodiment 11:
Weigh luteium oxide (Lu2O3) 0.5850 g, praseodymium oxide (Pr6O11) 0.0102 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.98Pr0.02NbO4。
Embodiment 12:
Weigh luteium oxide (Lu2O3) 0.5790 g, praseodymium oxide (Pr6O11) 0.0153 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.97Pr0.03NbO4。
Embodiment 13:
Weigh luteium oxide (Lu2O3) 0.5730 g, praseodymium oxide (Pr6O11) 0.0204 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.96Pr0.04NbO4。
Embodiment 14:
Weigh luteium oxide (Lu2O3) 0.5671 g, praseodymium oxide (Pr6O11) 0.0255 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.95Pr0.05NbO4。
Embodiment 15:
Weigh luteium oxide (Lu2O3) 0.5611 g, praseodymium oxide (Pr6O11) 0.0306 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.94Pr0.06NbO4。
Embodiment 16:
Weigh luteium oxide (Lu2O3) 0.5551 g, praseodymium oxide (Pr6O11) 0.0358 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, temperature programming 4h to 1250 DEG C in resistance furnace, it is sintered 5 h, cooled to room temperature；By sample
Product take out grinding, finally obtain product, chemical composition expression formula are as follows: Lu0.93Pr0.07NbO4。
Embodiment 17:
Weigh luteium oxide (Lu2O3) 0.5491 g, praseodymium oxide (Pr6O11) 0.0409 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.92Pr0.08NbO4。
Embodiment 18:
Weigh luteium oxide (Lu2O3) 0.5432 g, praseodymium oxide (Pr6O11) 0.0460 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.91Pr0.09NbO4。
Embodiment 19:
Weigh luteium oxide (Lu2O3) 0.5372 g, praseodymium oxide (Pr6O11) 0.0511 g, niobium oxide (Nb2O5) 0.3987 g,
In agate mortar, dehydrated alcohol is added as medium, is fully ground and is uniformly mixed；Mixture is placed in cold isostatic press
The slice of cylinder that diameter is 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In Carbon monoxide reduction atmosphere, 4 h to 1250 DEG C of temperature programming in resistance furnace is sintered 5 h, cooled to room temperature；It will
Sample takes out grinding, finally obtains product, chemical composition expression formula are as follows: Lu0.90Pr0.10NbO4。
According to preparation method of the present invention obtain it is a series of have different active ions (active ions refer to that trivalent is dilute
Native ion Pr3+) concentration (as molar content x, and value range 0.001≤x≤0.10) LuNbO4: xPr3+It shines
Material is in monitoring Pr3+The excitation spectrum that is measured when main 613 nm of emission peak and at 261 nm (peak position of Host lattice absorption band)
Emission spectrum under near ultraviolet excitation is shown in Figure 1 to represent with embodiment 5.It can be observed that Lu(1-x)PrxNbO4
(0.001≤x≤0.10) serial emission material has a very strong wide band absorption in ultra-violet (UV) band, the excitation spectrum of sample (a institute in Fig. 1
Showing) display Host lattice absorption band is 240 ~ 290 nm, the acromion positioned at Host lattice absorption band low energy direction belongs to Pr3+ + Nb5+
↔ Pr4+ + Nb4+Electric charge transfer (IVCT) band, the absorption peak within the scope of 440-500 nm then come from Pr between valence3+Ion
From3H4Ground state arrives3P0,1,2, 1I6The f-f transition absorption of excitation state.Under Host lattice absorption band (261 nm) excitation, the transmitting of sample
Spectrum (in Fig. 1 shown in b) shows blue light (~ 390 nm) transmitting and the Pr of matrix3+Feux rouges (~ 613 nm)1D2→3H4Transition
Transmitting.
Lu(1-x)PrxNbO4Transmitting of (0.001≤x≤0.10) the serial emission material under 261 nm near ultraviolet excitations
Spectrum is shown in Figure 2 to represent with embodiment 1,3,5,10,11,14 and 19.It can be observed that with Pr3+Doping concentration
Raising, matrix is to Pr3+The energy transfer efficiency of ion is gradually increased, and causes matrix blue emission to weaken, Pr3+Feux rouges hair
It penetrates after enhancing reaches maximum value in x=0.005 and gradually weakens because of generation concentration quenching, so that the transmitting ratio of blue light and feux rouges
Example is not with Pr3+Big variation occurs for the increase of doping concentration.
By the chromaticity coordinate figure in Fig. 3 it is observed that Lu(1-x)PrxNbO4(0.001≤x≤0.10) serial emission material
Expect that the chromaticity coordinates under 261 nm near ultraviolet excitations is x=0.191 ~ 0.242, y=0.073 ~ 0.143, is located at purple
Light area.
Representative sample Lu0.995Pr0.005NbO4(embodiment 5) under 261 nm near ultraviolet excitations temperature from 300 K to 500
The emission spectrum of K is shown in Figure 4.It can be observed that increase with temperature, matrix is to Pr3+Energy transfer efficiency gradually increase and
Temperature quenching may occur for matrix, and Pr3+Red emission in LuNbO4There is good thermal stability in matrix, lead to blue light
It is gradually reduced with the ratio of feux rouges with temperature raising.
By representative sample Lu in Fig. 50.995Pr0.005NbO4(embodiment 5) different temperatures under 261 nm near ultraviolet excitations
When position of the chromaticity coordinate in 1931 CIE chromaticity diagrams it is observed that when temperature is increased to 500 K from 300 K, shine
Coloration is continuously adjusted in purple light-purple powder light-pink light range.
Claims (3)
1. a kind of coloration is with the adjustable luminescent material of temperature, it is characterised in that:
Chemical composition expression are as follows: Lu(1-x)PrxNbO4, x is active ions Pr in formula3+Opposite matrix rare earth ion Lu3+It accounts for
Molar content, value range: 0.001≤x≤0.005.
2. the preparation method of luminescent material described in claim 1, it is characterised in that include the following steps:
S1. according to chemical composition embodied in above-mentioned chemical composition expression formula, raw material is accurately weighed, it is equal to be fully ground mixing
It is even, obtain mixture；
S2. it by mixture tabletting, is then placed in reaction vessel, in a reducing atmosphere, is placed in temperature programming in resistance furnace and roasts
It burns, cooled to room temperature；
S3. step S2 products therefrom is taken out into grinding to get product is arrived；
Raw material described in step S1 are as follows: luteium oxide, praseodymium oxide and niobium oxide；
Be fully ground described in step S1 be uniformly mixed be in agate mortar be added dehydrated alcohol as medium carry out grinding mix
It closes uniform；
Tabletting described in step S2 is that tabletting is carried out in cold isostatic press, by mixture obtained by step S1 in 150 MPa pressure
Under be pressed into the slice of cylinder that diameter is 12.5 mm and high 5 mm；
Reaction vessel described in step S2 is corundum crucible；
Reducing atmosphere described in step S2 refers to the carbon monoxide atmosphere generated by heating carbon block；
Heating-up time described in step S2 is 3-6 h；
The condition of roasting described in step S2 is 1200 ~ 1300 DEG C, roasts 5-10 h.
3. coloration described in claim 1 is with the adjustable luminescent material of temperature aobvious by the various illuminations of excitaton source of black light
Show or luminescence generated by light in terms of application.
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| CN102492423A (en) * | 2011-12-19 | 2012-06-13 | 重庆市科学技术研究院 | Red fluorescent material used for white LED (light-emitting diode) and preparation method thereof |
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