CN103571472A - Dysprosium-doped alkali tantalate up-conversion luminescence material, and preparation method and application thereof - Google Patents
Dysprosium-doped alkali tantalate up-conversion luminescence material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a dysprosium-doped alkali tantalate up-conversion luminescence material. The chemical formula of the dysprosium-doped alkali tantalate up-conversion luminescence material is RTa1-xO3:xDy<3+>, wherein R is one or more of a lithium element, a sodium element and a potassium element, and x is 0.002-0.06. The dysprosium-doped alkali tantalate up-conversion luminescence material can be excited through long wave radiation to emit blue light. The invention also provides a preparation method of the dysprosium-doped alkali tantalate up-conversion luminescence material, and an application of the dysprosium-doped alkali tantalate up-conversion luminescence material.
Description
Technical field
The present invention relates to a kind of dysprosium alkali-doped tantalate up-conversion luminescent material, its preparation method and use the Organic Light Emitting Diode of this dysprosium alkali-doped tantalate up-conversion luminescent material.
Background technology
Organic Light Emitting Diode (OLED) because unit construction is simple, the characteristic such as cheap, the luminous of production cost, reaction times be short, flexible, and obtained the utmost point, apply widely.But owing to obtaining at present, the OLED blue light material of stability and high efficiency is more difficult, has limited greatly the development of white light OLED device and light source industry.
Upconverting fluorescent material can be launched visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in fields such as optical fiber communication technology, fibre amplifier, 3 D stereo demonstration, biomolecules fluorescence labelling, infrared detectives.But, can be by infrared, the long-wave radiations such as red-green glow inspire the dysprosium alkali-doped tantalate up-conversion luminescent material of blue emission, have not yet to see report.
Summary of the invention
Based on this, being necessary to provide a kind of can be inspired dysprosium alkali-doped tantalate up-conversion luminescent material, its preparation method of blue light and be used the Organic Light Emitting Diode of this dysprosium alkali-doped tantalate up-conversion luminescent material by long-wave radiation.
An alkali-doped tantalate up-conversion luminescent material, its chemical formula is RTa
1-xo
3: xDy
3+, wherein, R is elemental lithium, in sodium element or potassium element one or more, x is 0.002 ~ 0.06.
In an embodiment, x is 0.03 therein.
A preparation method, comprise the following steps:
According to RTa
1-xo
3: xDy
3+the stoichiometric ratio of each element takes R
2o, Ta
2o
5and Dy
2o
3powder, wherein, R is elemental lithium, in sodium element or potassium element one or more, x is 0.002 ~ 0.06;
The powder taking is dissolved in and in nitric acid, is mixed with the solution that the concentration of concentration metallic cation is 0.5mol/L ~ 3mol/L;
Described solution mist is changed into after mist to carrier gas, to pass into temperature be that the silica tube of 100 ℃ ~ 220 ℃ generates presoma, wherein the diameter of silica tube is that diameter is 30mm ~ 150mm, and length is 0.5m ~ 3m, and the flow of carrier gas is 1L/min ~ 15L/min;
Described presoma being calcined at 600 ℃ ~ 1300 ℃ and within 2 hours ~ 5 hours, obtained chemical formula is RTa
1-xo
3: xDy
3+dysprosium alkali-doped tantalate up-conversion luminescent material.
In an embodiment, x is 0.03 therein.
Therein in an embodiment, the powder taking is dissolved in to the step that is mixed with solution in nitric acid and also comprises: in described solution, add dispersion agent, the concentration of described dispersion agent is 0.005mol/L ~ 0.05mol/L.
In an embodiment, described dispersion agent is polyoxyethylene glycol therein.
Therein in an embodiment, the step that described solution mist is changed into mist is, carrier gas and described solution are passed into together in spraying gun and makes described solution mist change into mist, and described carrier gas is rare gas element or reducing gas.
In an embodiment, the flow of described carrier gas is 5L/min ~ 8L/min therein.
A kind of Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, in described transparent encapsulated layer, doped with dysprosium alkali-doped tantalate up-conversion luminescent material, the chemical general formula of described dysprosium alkali-doped tantalate up-conversion luminescent material is RTa
1-xo
3: xDy
3+, wherein, R is elemental lithium, in sodium element or potassium element one or more, x is 0.002 ~ 0.06.
In an embodiment, x is 0.03 therein.
The preparation method of above-mentioned dysprosium alkali-doped tantalate up-conversion luminescent material is comparatively simple, and cost is lower; In the photoluminescence spectra of dysprosium alkali-doped tantalate up-conversion luminescent material of preparation, the excitation wavelength of dysprosium alkali-doped tantalate up-conversion luminescent material is 796nm, in 482nm wavelength zone by Dy
3+ion
4f
9/2→
6f
15/2transition radiation form glow peak, realized that by the infrared long-wave radiation to green glow, to inspire blue light shortwave luminous; In the transparent encapsulated layer of Organic Light Emitting Diode, be dispersed with dysprosium alkali-doped tantalate up-conversion luminescent material, the excitation wavelength of dysprosium alkali-doped tantalate up-conversion luminescent material is 796nm, in 482nm wavelength zone by Dy
3+ion
4f
9/2→
6f
15/2transition radiation form glow peak, by red-green glow, excite and can launch blue light, blue light mixes the Organic Light Emitting Diode that formation emits white light afterwards with red-green glow.
Accompanying drawing explanation
Fig. 1 is the structural representation of the spray pyrolysis equipment of an embodiment;
Fig. 2 is the structural representation of the Organic Light Emitting Diode of an embodiment
Fig. 3 is the photoluminescence spectrogram of the dysprosium alkali-doped tantalate up-conversion luminescent material of embodiment 1 preparation;
Fig. 4 is the XRD spectra of the dysprosium alkali-doped tantalate up-conversion luminescent material of embodiment 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments to dysprosium alkali-doped tantalate up-conversion luminescent material, its preparation method and use the Organic Light Emitting Diode of this dysprosium alkali-doped tantalate up-conversion luminescent material further to illustrate.
The dysprosium alkali-doped tantalate up-conversion luminescent material of one embodiment, its chemical formula is RTa
1-xo
3: xDy
3+, wherein, R is elemental lithium, in sodium element or potassium element one or more, x is 0.002 ~ 0.06.
Preferably, x is 0.03.
In the photoluminescence spectra of this dysprosium alkali-doped tantalate up-conversion luminescent material, the excitation wavelength of dysprosium alkali-doped tantalate up-conversion luminescent material is 796nm, when material is subject to long wavelength's (as 796nm) radiation, and Dy
3+the energy of this illumination of ionic absorption, now Dy
3+ion by
4f
9/2→
6f
15/2transition, sends the blue light of 482nm, has realized that by the infrared long-wave radiation to green glow, to inspire blue light shortwave luminous.
The preparation method of above-mentioned dysprosium alkali-doped tantalate up-conversion luminescent material, comprises the following steps;
Step S101, according to RTa
1-xo
3: xDy
3+the stoichiometric ratio of each element takes R
2o, Ta
2o
5and Dy
2o
3powder, wherein, R is elemental lithium, in sodium element or potassium element one or more, x is 0.002 ~ 0.06.
Preferably, x is 0.03.
Being appreciated that in this step also can be according to mol ratio 1:(0.96 ~ 0.998): (0.002 ~ 0.06) takes R
2o, Ta
2o
5and Dy
2o
3powder.
Step S102, the powder taking is dissolved in and in nitric acid, is mixed with the solution that the concentration of metallic cation is 0.5mol/L ~ 3mol/L.
Metallic cation in solution is R
+, Ta
5+and Dy
3+, R
+for lithium ion, in sodium ion or potassium ion one or more.
In present embodiment, the concentration of metallic cation is 0.5mol/L ~ 3mol/L.
Preferably, the powder taking being dissolved in to the step that is mixed with solution in nitric acid also comprises: in solution, add dispersion agent, the concentration of dispersion agent is 0.005mol/L ~ 0.05mol/L.In present embodiment, dispersion agent is polyoxyethylene glycol.
Refer to Fig. 1, the spray pyrolysis equipment 100 shown in Fig. 1 comprises container for storing liquid 10, gas-holder 20, spraying gun 30, silica tube 40 and collector 50.
In present embodiment, solution prepared by step S102 is deposited in container for storing liquid 10.
S103, solution mist is changed into after mist to carrier gas, to pass into temperature be that the silica tube 40 of 100 ℃ ~ 220 ℃ generates presomas, wherein the diameter of silica tube 40 is 30mm ~ 150mm, and length is 0.5m ~ 3m, and the flow of carrier gas is 1L/min ~ 15L/min.
Preferably, the diameter of silica tube is 95mm, and length is 1.4m, and the flow of carrier gas is 5L/min.
In present embodiment, use spraying gun 30 by solution atomization, spraying gun 30 is compression atomizing device.Concrete, the solution of the carrier gas of gas-holder 20 interior storages and container for storing liquid 10 interior storages is together passed into spraying gun 30 and make solution mist change into mist.Carrier gas is rare gas element or reducing gas, as: at least one in nitrogen, argon gas and hydrogen, the flow of carrier gas is 5L/min ~ 8L/min.
Solution mist passes into from one end of silica tube 40 after changing into mist, and at the interior generation presoma of silica tube 40, presoma is trickle powder, and pulverous presoma is the other end ejection from silica tube with carrier gas.Further, presoma is used collector 50 to collect after silica tube 40 flows out.In present embodiment, collector 50 is the acidproof filtration funnel of micropore.
S104, presoma is calcined at 600 ℃ ~ 1300 ℃ within 2 hours ~ 5 hours, to obtain chemical formula be RTa
1-xo
3: xDy
3+dysprosium alkali-doped tantalate up-conversion luminescent material.
Preferably, presoma is placed in the calcination 3 hours at 1100 ℃ of temperature programmed control stove.
The preparation method of above-mentioned dysprosium alkali-doped tantalate up-conversion luminescent material is spray pyrolysis, and raw material mixes under solution state, can guarantee uniform component distribution, and technological process is simple, component loss is few, can accurately control stoichiometric ratio, is especially applicable to preparing polycomponent composite powder; Micro mist is by being suspended in airborne droplet drying, and particle is generally the spherical of rule, and few reunion, without follow-up washing, grinds, and guarantees the high purity of product, high reactivity; Whole process completed rapidly in short several seconds, so drop has little time to occur solute segregation in reaction process, further guaranteed the homogeneity that component distributes; Reaction process is simple, and a step obtains finished product, and without filtration, washing, dry, crushing process, simple to operation, production process is continuous, and production capacity is large, and production efficiency is high, is very beneficial for large suitability for industrialized production; In the photoluminescence spectra of the dysprosium alkali-doped tantalate up-conversion luminescent material of preparation, the excitation wavelength of dysprosium alkali-doped tantalate up-conversion luminescent material is 796nm, when material is subject to the radiation of wavelength (as 796nm), and Dy
3+the energy of this illumination of ionic absorption, now Dy
3+ion
4f
9/2→
6f
15/2transition, sends the blue light of 482nm, has realized that by the infrared long-wave radiation to green glow, to inspire blue light shortwave luminous.
Refer to Fig. 2, the Organic Light Emitting Diode 100 of an embodiment, this Organic Light Emitting Diode 100 comprises substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 stacking gradually.In transparent encapsulated layer 5, be dispersed with dysprosium alkali-doped tantalate up-conversion luminescent material 6, the chemical formula of dysprosium alkali-doped tantalate up-conversion luminescent material is RTa
1-xo
3: xDy
3+, wherein, R is elemental lithium, in sodium element or potassium element one or more, x is 0.002 ~ 0.06.
In the transparent encapsulated layer 5 of Organic Light Emitting Diode 100, be dispersed with dysprosium alkali-doped tantalate up-conversion luminescent material 6, the excitation wavelength of dysprosium alkali-doped tantalate up-conversion luminescent material is 796nm, in 482nm wavelength zone by Dy
3+ion
4f
9/2→
6f
15/2transition radiation form glow peak, by red-green glow, excite and can launch blue light, blue light mixes the Organic Light Emitting Diode that formation emits white light afterwards with red-green glow.
Be specific embodiment below.
Embodiment 1
Take Li
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 1mmol, and 0.97mmol and 0.03mmol are dissolved in the solution that is mixed with 1.5mol/L in nitric acid, and add the polyoxyethylene glycol additive of 0.01mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 5L/min.It is that the silica tube of 180 ℃ generates presoma that solution presoma enters temperature with argon carrier, and wherein the diameter of silica tube is 95mm, and length is 1.4m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 3 hours, and 1100 ℃ of calcining temperatures, obtain LiTa
0.97o
3: 0.03Dy
3+up-conversion phosphor.
Refer to Fig. 3, the photoluminescence spectra of the dysprosium alkali-doped tantalate up-conversion luminescent material that in Fig. 3, curve 1 obtains for the present embodiment.As seen from Figure 3, the excitation wavelength of the dysprosium alkali-doped tantalate up-conversion luminescent material that embodiment 1 obtains is 796nm, when material is subject to long wavelength's (as 796nm) radiation, and Dy now
3+ion
4f
9/2→
6f
15/2transition, just sends the blue light of 482nm, can be used as blue light emitting material.
Refer to Fig. 4, in Fig. 4, curve is for implementing the XRD curve of the dysprosium alkali-doped tantalate up-conversion luminescent material of 1 preparation, test comparison standard P DF card, each diffraction peak in figure is the peak crystallization of alkali tantalate, the diffraction peak that does not occur doped element and other impurity, illustrates that thulium ion and holmium ion are the lattices that doping has entered alkali tantalate.
Take Li
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 1mmol, 0.998mmol and 0.002mmol, is dissolved in the solution that is mixed with 3mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.05mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 15L/min.It is that the silica tube of 220 ℃ generates presoma that solution presoma enters temperature with argon carrier, and wherein the diameter of silica tube is 150mm, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 5 hours, and 1300 ℃ of calcining temperatures, obtain LiTa
0.998o
3: 0.002Dy
3+up-conversion phosphor.
Take Li
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 1mmol, 0.94mmol and 0.06mmol, is dissolved in the solution that is mixed with 0.5mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.005mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 150 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 2 hours, and 600 ℃ of calcining temperatures, obtain LiTa
0.94o
3: 0.06Dy
3+up-conversion phosphor.
Take Na
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 1mmol, 0.97mmol and 0.03mmol, is dissolved in the solution that is mixed with 1.5mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.01mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 5L/min.It is that the silica tube of 180 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 3 hours, and 1100 ℃ of calcining temperatures, obtain NaTa
0.97o
3: 0.03Dy
3+up-conversion phosphor.
Embodiment 5
Take Na
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 1mmol, 0.998mmol and 0.002mmol, is dissolved in the solution that is mixed with 3mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.05mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 15L/min.It is that the silica tube of 220 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 5 hours, and 1300 ℃ of calcining temperatures, obtain NaTa
0.998o
3: 0.002Dy
3+up-conversion phosphor.
Take Na
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 1mmol, 0.94mmol and 0.06mmol, is dissolved in the solution that is mixed with 0.5mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.005mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 150 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 2 hours, and 600 ℃ of calcining temperatures, obtain NaTa
0.94o
3: 0.06Dy
3+up-conversion phosphor.
Embodiment 7
Take K
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 1mmol, 0.97mmol and 0.03mmol, is dissolved in the solution that is mixed with 1.5mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.01mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 180 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 3 hours, and 1100 ℃ of calcining temperatures, obtain KTa
0.97o
3: 0.03Dy
3+up-conversion phosphor.
Embodiment 8
Take K
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 1mmol, 0.998mmol and 0.002mmol, is dissolved in the solution that is mixed with 3mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.05mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 15L/min.It is that the silica tube of 220 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 5 hours, and 1300 ℃ of calcining temperatures, obtain KTa
0.998o
3: 0.002Dy
3+up-conversion phosphor.
Embodiment 9
Take K
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 1mmol, 0.94mmol and 0.06mmol, is dissolved in the solution that is mixed with 0.5mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.005mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 150 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 2 hours, and 600 ℃ of calcining temperatures, obtain KTa
0.94o
3: 0.06Dy
3+up-conversion phosphor.
Embodiment 10
Take Na
2o, K
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 0.4mmol, 0.6mmol, 0.94mmol and 0.06mmol, is dissolved in the solution that is mixed with 0.5mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.005mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 150 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 2 hours, and 600 ℃ of calcining temperatures, obtain Na
0.4k
0.6ta
0.94o
3: 0.06Dy
3+up-conversion phosphor.
Embodiment 11
Take Na
2o, K
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 0.7mmol, 0.3mmol, 0.94mmol and 0.06mmol, is dissolved in the solution that is mixed with 0.5mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.005mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 150 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 2 hours, and 600 ℃ of calcining temperatures, obtain Na
0.7k
0.3ta
0.94o
3: 0.06Dy
3+up-conversion phosphor.
Embodiment 12
Take Li
2o, Na
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 0.2mmol, 0.8mmol, 0.94mmol and 0.06mmol, is dissolved in the solution that is mixed with 0.5mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.005mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 150 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 2 hours, and 600 ℃ of calcining temperatures, obtain Li
0.2na
0.8ta
0.94o
3: 0.06Dy
3+up-conversion phosphor.
Embodiment 13
Take Li
2o, Na
2o, Ta
2o
5and Dy
2o
3powder, its molar weight is respectively 0.5mmol, 0.5mmol, 0.94mmol and 0.06mmol, is dissolved in the solution that is mixed with 0.5mol/L in nitric acid, and adds the polyoxyethylene glycol additive of 0.005mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 150 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 2 hours, and 600 ℃ of calcining temperatures, obtain Li
0.5na
0.5ta
0.94o
3: 0.06Dy
3+up-conversion phosphor.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a dysprosium alkali-doped tantalate up-conversion luminescent material, is characterized in that: its chemical formula is RTa
1-xo
3: xDy
3+, wherein, R is elemental lithium, in sodium element or potassium element one or more, x is 0.002 ~ 0.06.
2. dysprosium alkali-doped tantalate up-conversion luminescent material according to claim 1, is characterized in that, x is 0.03.
3. a preparation method for dysprosium alkali-doped tantalate up-conversion luminescent material, is characterized in that, comprises the following steps:
According to RTa
1-xo
3: xDy
3+the stoichiometric ratio of each element takes R
2o, Ta
2o
5and Dy
2o
3powder, wherein, R is elemental lithium, in sodium element or potassium element one or more, x is 0.002 ~ 0.06;
The powder taking is dissolved in and in nitric acid, is mixed with the solution that the concentration of metallic cation is 0.5mol/L ~ 3mol/L;
Described solution mist is changed into after mist to carrier gas, to pass into temperature be that the silica tube of 100 ℃ ~ 220 ℃ generates presoma, wherein the diameter of silica tube is 30mm～150mm, and length is 0.5m ~ 3m, and the flow of carrier gas is 1L/min ~ 15L/min;
Described presoma is calcined at 600 ℃ ~ 1300 ℃ and within 2 hours ~ 5 hours, obtained chemical formula RTa
1-xo
3: xDy
3+dysprosium alkali-doped tantalate up-conversion luminescent material.
4. the preparation method of dysprosium alkali-doped tantalate up-conversion luminescent material according to claim 3, is characterized in that, x is 0.03.
5. the preparation method of dysprosium alkali-doped tantalate up-conversion luminescent material according to claim 3, it is characterized in that, the powder taking is dissolved in to the step that is mixed with solution in nitric acid also to be comprised: in described solution, add dispersion agent, the concentration of described dispersion agent is 0.005mol/L ~ 0.05mol/L.
6. the preparation method of dysprosium alkali-doped tantalate up-conversion luminescent material according to claim 5, is characterized in that, described dispersion agent is polyoxyethylene glycol.
7. the preparation method of dysprosium alkali-doped tantalate up-conversion luminescent material according to claim 3, it is characterized in that, the step that described solution mist is changed into mist is, carrier gas and described solution are passed into together in spraying gun and makes described solution mist change into mist, and described carrier gas is rare gas element or reducing gas.
8. the preparation method of dysprosium alkali-doped tantalate up-conversion luminescent material according to claim 3, is characterized in that, the flow of described carrier gas is 5L/min ~ 8L/min.
9. an Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, it is characterized in that, in described transparent encapsulated layer, doped with dysprosium alkali-doped tantalate up-conversion luminescent material, the chemical general formula of described dysprosium alkali-doped tantalate up-conversion luminescent material is RTa
1-xo
3: xDy
3+, wherein, R is elemental lithium, in sodium element or potassium element one or more, x is 0.002 ~ 0.06.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, x is 0.03.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104178152A (en) * | 2013-05-22 | 2014-12-03 | 海洋王照明科技股份有限公司 | Dysprosium-doped alkali tantalate up-conversion luminescent material and preparation method and application thereof |
| CN109135741A (en) * | 2018-07-20 | 2019-01-04 | 同济大学 | A kind of tantalic acid alkali elastic stress luminescent material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178152A (en) * | 2013-05-22 | 2014-12-03 | 海洋王照明科技股份有限公司 | Dysprosium-doped alkali tantalate up-conversion luminescent material and preparation method and application thereof |
| CN109135741A (en) * | 2018-07-20 | 2019-01-04 | 同济大学 | A kind of tantalic acid alkali elastic stress luminescent material and preparation method thereof |
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Application publication date: 20140212 |