CN103421504B - Praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, preparation method and application thereof - Google Patents
Praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, preparation method and application thereof Download PDFInfo
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Abstract
A kind of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, has the Y that following chemistry is logical2-x-ySiO5:xPr3+, yYb3+, wherein, x is 0.01～0.08, and y is 0～0.1.In the photoluminescence spectra of this praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, the excitation wavelength of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material is 980nm, in 485nm wavelength zone by Pr3+Ion3P0→3H4Transition radiation formed glow peak, it is possible to as blue light emitting material.The present invention also provides for the preparation method of this praseodymium ytterbium codope yttrium silicate up-conversion luminescent material and uses the Organic Light Emitting Diode of this praseodymium ytterbium codope yttrium silicate up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, preparation method and Organic Light Emitting Diode.
Background technology
Organic Light Emitting Diode (OLED) owing to modular construction is simple, the characteristic such as production cost is cheap, self-luminous, response time are short, flexible, and obtain a very wide range of application.But the OLED blue light material owing to obtaining stability and high efficiency at present is relatively difficult, significantly limit white light OLED device and the development of light source industry.
Upconverting fluorescent material can launch visible ray under long wave (as infrared) radiation excitation, even ultraviolet light, at optical fiber communication technology, fibre amplifier, 3 D stereo shows, the field such as biomolecule fluorescence labelling, infrared detective is with a wide range of applications.But, can by infrared, the long-wave radiation such as red-green glow inspires the praseodymium ytterbium codope yttrium silicate up-conversion luminescent material of blue emission, has not yet to see report.
Summary of the invention
Based on this, it is necessary to providing a kind of can be inspired the praseodymium ytterbium codope yttrium silicate up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this praseodymium ytterbium codope yttrium silicate up-conversion luminescent material.
A kind of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, has following chemical formula Y2-x-ySiO5:xPr3+, yYb3+, wherein, x is 0.01～0.08, and y is 0～0.1.
Wherein in an embodiment, x is 0.05, y is 0.06.
The preparation method of a kind of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, comprises the following steps: according to Y2-x-ySiO5:xPr3+, yYb3+The stoichiometric proportion of each element weighs Y2O3, Pr2O3, Yb2O3And Na2SiO3Powder body, wherein x is 0.01～0.08, and y is 0～0.1；
Y will be weighed2O3, Pr2O3And Yb2O3Powder body mix homogeneously is dissolved in acid flux material and carries out crystallization treatment obtains crystal；
Add dissolved with Na after crystal is dissolved in a solvent2SiO3The solution of powder body, adding ammonia adjustment pH value is 1～6, obtains mixed solution；
At 150 DEG C～500 DEG C, described mixed solution being incubated 2 hours～10 hours, is precipitated thing, dry after the precipitate obtained is adopted cleaning mixture washing, obtaining chemical general formula is Y2-x-ySiO5:xPr3+, yYb3+Praseodymium ytterbium codope yttrium silicate up-conversion luminescent material.
Wherein in an embodiment, x is 0.05, y is 0.06.
Wherein in an embodiment, described mixed solution is incubated 3 hours at 300 DEG C.
Wherein in an embodiment, described being dissolved in a solvent by crystal, wherein said solvent is distilled water or the mixed solution of distilled water and dehydrated alcohol, described Na2SiO3The molar concentration of the solution of powder body is 0.005mol/L～0.03mol/L.
Wherein in an embodiment, described acid flux material includes nitric acid that mass percentage concentration is 30% or mass percentage concentration is the sulphuric acid of 30%.
Wherein in an embodiment, described pH value is 5.
Wherein in an embodiment, described cleaning mixture is distilled water and dehydrated alcohol.
A kind of Organic Light Emitting Diode, including the substrate stacked gradually, negative electrode, organic luminous layer, transparent anode and transparent encapsulated layer, doped with praseodymium ytterbium codope yttrium silicate up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of this praseodymium ytterbium codope yttrium silicate up-conversion luminescent material is Y2-x-ySiO5:xPr3+, yYb3+, wherein x is 0.01～0.08, and y is 0～0.1.
The hydrothermal method mild condition of above-mentioned praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, synthesis temperature is low is relatively easy to control, the granularity of product and morphology controllable, the powder body complete crystallization of preparation, good dispersion, less costly, simultaneous reactions process produces without the three wastes, comparatively environmental protection；In the photoluminescence spectra of the praseodymium ytterbium codope yttrium silicate up-conversion luminescent material of preparation, the excitation wavelength of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material is 980nm, in 485nm wavelength zone by Pr3+Ion3P0→3H4Transition radiation formed glow peak, it is possible to as blue light emitting material.
Accompanying drawing explanation
Fig. 1 is the structural representation of the Organic Light Emitting Diode of an embodiment.
Fig. 2 is the luminescence generated by light spectrogram of the praseodymium ytterbium codope yttrium silicate up-conversion luminescent material of embodiment 1 preparation.
Fig. 3 is the XRD spectra of the praseodymium ytterbium codope yttrium silicate up-conversion luminescent material of embodiment 1 preparation.
Fig. 4 is dispersed with praseodymium ytterbium codope yttrium silicate up-conversion luminescent material to form the spectrogram of the Organic Light Emitting Diode emitted white light in transparent encapsulated layer prepared by embodiment 1.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, praseodymium ytterbium codope yttrium silicate up-conversion luminescent material and preparation method thereof is further elucidated with.
The praseodymium ytterbium codope yttrium silicate up-conversion luminescent material of one embodiment, its chemical formula is Y2-x-ySiO5:xPr3+, yYb3+, wherein, x is 0.01～0.08, and y is 0～0.1.
Preferably, x is 0.05, y is 0.06.
In the photoluminescence spectra of this praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, the excitation wavelength of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material is 980nm, when material is subject to the radiation of long wavelength (such as 980nm) time, and Yb3+Ionic absorption emittance, to Pr3+Ion-transfer, Pr3+Ion excitation arrives3P0Excited state, then to3H4Energy state transitions, sends the blue light of 485nm, it is possible to as blue light emitting material.
The preparation method of above-mentioned praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, comprises the following steps:
Step S11, according to Y2-x-ySiO5:xPr3+, yYb3+The stoichiometric proportion of each element weighs Y2O3, Pr2O3, Yb2O3And Na2SiO3Powder body, wherein x is 0.01～0.08, and y is 0～0.1.
In this step, it is preferred that x is 0.05, y is 0.06.
Step S12, Y will be weighed2O3, Pr2O3And Yb2O3Powder body mix homogeneously is dissolved in acid flux material and carries out crystallization treatment obtains crystal；
In this step, it is preferred that described acid flux material includes nitric acid that mass percentage concentration is 30% or mass percentage concentration is the sulphuric acid of 30%；
Step S13, the crystal in step S12 is dissolved in a solvent after add dissolved with Na2SiO3The solution of powder body, adding ammonia adjustment pH value is 1～6, obtains mixed solution.
In this step, it is preferred that described Na2SiO3The molar concentration of the solution of powder body is 0.005mol/L～0.03mol/L
In this step, it is preferred that described solvent is distilled water or the mixed solution of distilled water and dehydrated alcohol.
Step S15, at 150 DEG C～500 DEG C, described mixed solution being incubated 2 hours～10 hours, be precipitated thing, dry after the precipitate obtained is adopted cleaning mixture washing, obtaining praseodymium ytterbium codope yttrium silicate up-conversion luminescent material chemical general formula is Y2-x-ySiO5:xPr3+, yYb3+。
In this step, it is preferred that mixed solution is transferred in the stainless steel cauldron of tetrafluoroethene lining, at 300 DEG C, it is incubated 3 hours.
In this step, it is preferred that described cleaning mixture is distilled water and dehydrated alcohol.
In this step, it is preferred that x is 0.05, y is 0.06.
The hydrothermal method mild condition of above-mentioned praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, synthesis temperature is low is relatively easy to control, the granularity of product and morphology controllable, the powder body complete crystallization of preparation, good dispersion, less costly, simultaneous reactions process produces without the three wastes, comparatively environmental protection；In the photoluminescence spectra of the praseodymium ytterbium codope yttrium silicate up-conversion luminescent material of preparation, the excitation wavelength of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material is 980nm, in 485nm wavelength zone by Pr3+Ion3P0→3H4Transition radiation formed glow peak, it is possible to as blue light emitting material.
Referring to Fig. 1, the Organic Light Emitting Diode 100 of an embodiment, this Organic Light Emitting Diode 100 includes the substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 that stack gradually.Being dispersed with praseodymium ytterbium codope yttrium silicate up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material is Y2-x-ySiO5:xPr3+, yYb3+, wherein, x is 0.01～0.08, and y is 0～0.1.
Being dispersed with praseodymium ytterbium codope yttrium silicate up-conversion luminescent material 6 in the transparent encapsulated layer 5 of Organic Light Emitting Diode 100, the excitation wavelength of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material is 980nm, in 485nm wavelength zone by Pr3+Ion3P0→3H4Transition radiation formed glow peak, red-green glow excite and can launch blue light, blue light forms the Organic Light Emitting Diode emitted white light with red-green glow after mixing.
It is specific embodiment below.
Embodiment 1
Select Y2O3, Pr2O3And Yb2O3Powder body is 0.89mmol, 0.05mmol, 0.06mmol mixing by each component molal quantity.It is dissolved in the nitric acid solvent that concentration is 30% carrying out crystallization treatment after mixing and obtains crystal, then crystal to be dissolved in distilled water and adds molar concentration in the solution be 0.005mol/LNa2SiO3Solution 200ml, adds ammonia, and regulating pH value is 5.Then mixed solution is transferred in the stainless steel cauldron of teflon lined, be incubated 3h at 300 DEG C, be precipitated thing.Again the precipitate ethanol obtained and distilled water cyclic washing, being evaporated at 100 DEG C, obtaining chemical general formula is Y1.89SiO5:0.05Pr3+, 0.06Yb3+Up-conversion phosphor.
Referring to Fig. 2, Fig. 2, to show the praseodymium ytterbium codope yttrium silicate up-conversion luminescent material chemical general formula that this enforcement obtains be Y2O3:0.05Pr3+, 0.06Yb3+Photoluminescence spectra figure with the contrast being co-doped with ytterbium element that undopes.As seen from Figure 2, the excitation wavelength of the praseodymium ytterbium codope yttrium silicate up-conversion luminescent material that the present embodiment obtains is 980nm, in 485nm wavelength zone by Pr3+Ion3P0→3H4Transition radiation formed glow peak, this praseodymium ytterbium codope yttrium silicate up-conversion luminescent material can as blue light emitting material.The curve 2 of Fig. 2 is the comparative example of undoped p ytterbium element, and as seen from the figure, the luminous intensity of the luminescent material being doped with ytterbium element is remarkably reinforced.
Refer to the XRD curve that curve in Fig. 3, Fig. 3 is the praseodymium ytterbium codope yttrium silicate up-conversion luminescent material implementing 1 preparation, test comparison standard PDF card.Comparison PDF card diffraction maximum show the peak crystallization of yttrium silicate, it does not have the diffraction maximum of doped chemical and other impurity occurs, illustrates that the product that this preparation method obtains has good crystalline quality.
Referring to curve 1 in Fig. 4, Fig. 4 is be dispersed with praseodymium ytterbium codope yttrium silicate up-conversion luminescent material in transparent encapsulated layer to form the spectrogram of the Organic Light Emitting Diode emitted white light, and curve 2 is the contrast not adding praseodymium ytterbium codope yttrium silicate up-conversion luminescent material.Can be seen that in figure, praseodymium ytterbium codope yttrium silicate up-conversion luminescent material by the red light of long wave, can inspire the blue light of shortwave, blend together white light.
Embodiment 2
Select Y2O3, Pr2O3And Yb2O3Powder body is 0.82mmol, 0.08mmol, 0.1mmol mixing by each component molal quantity.It is dissolved in the sulfuric acid solvent that concentration is 30% carrying out crystallization treatment after mixing and obtains crystal, then crystal to be dissolved in distilled water and adds molar concentration in the solution be 0.01mol/LNa2SiO3Solution 100ml, adds ammonia, and regulating pH value is 1.Then mixed solution is transferred in the stainless steel cauldron of teflon lined, be incubated 2h at 150 DEG C, be precipitated thing.Again the precipitate ethanol obtained and distilled water cyclic washing, being evaporated at 100 DEG C, obtaining chemical general formula is Y1.82SiO5:0.08Pr3+, 0.1Yb3+Up-conversion phosphor.
Embodiment 3
Select Y2O3, Pr2O3Powder body is 0.99mmol, 0.01mmol mixing by each component molal quantity.It is dissolved in the nitric acid solvent that concentration is 30% carrying out crystallization treatment after mixing and obtains crystal, then crystal to be dissolved in distilled water and adds molar concentration in the solution be 0.02mol/LNa2SiO3Solution 50ml, adds ammonia, and regulating pH value is 5.Then mixed solution is transferred in the stainless steel cauldron of teflon lined, be incubated 3h at 300 DEG C, be precipitated thing.Again the precipitate ethanol obtained and distilled water cyclic washing, being evaporated at 100 DEG C, obtaining chemical general formula is Y1.99SiO5:0.01Pr3+Up-conversion phosphor.
Embodiment 4
Select Y2O3, Pr2O3And Yb2O3Powder body is 0.92mmol, 0.03mmol, 0.05mmol mixing by each component molal quantity.It is dissolved in the nitric acid solvent that concentration is 30% carrying out crystallization treatment after mixing and obtains crystal, then crystal to be dissolved in distilled water and adds molar concentration in the solution be 0.01mol/LNa2SiO3Solution 100ml, adds ammonia, and regulating pH value is 5.Then mixed solution is transferred in the stainless steel cauldron of teflon lined, be incubated 3h at 300 DEG C, be precipitated thing.Again the precipitate ethanol obtained and distilled water cyclic washing, being evaporated at 100 DEG C, obtaining chemical general formula is Y1.92SiO5:0.03Pr3+, 0.05Yb3+Up-conversion phosphor.
Embodiment 5
Select Y2O3, Pr2O3And Yb2O3Powder body is 0.90mmol, 0.06mmol, 0.04mmol mixing by each component molal quantity.It is dissolved in the nitric acid solvent that concentration is 30% carrying out crystallization treatment after mixing and obtains crystal, then crystal to be dissolved in distilled water and adds molar concentration in the solution be 0.01mol/LNa2SiO3Solution 100ml, adds ammonia, and regulating pH value is 5.Then mixed solution is transferred in the stainless steel cauldron of teflon lined, be incubated 3h at 300 DEG C, be precipitated thing.Again the precipitate ethanol obtained and distilled water cyclic washing, being evaporated at 100 DEG C, obtaining chemical general formula is Y1.90SiO5:0.06Pr3+, 0.04Yb3+Up-conversion phosphor.
Embodiment 6
Select Y2O3, Pr2O3And Yb2O3Powder body is 0.90mmol, 0.07mmol, 0.03mmol mixing by each component molal quantity.It is dissolved in the nitric acid solvent that concentration is 30% carrying out crystallization treatment after mixing and obtains crystal, then crystal to be dissolved in distilled water and adds molar concentration in the solution be 0.01mol/LNa2SiO3Solution 100ml, adds ammonia, and regulating pH value is 5.Then mixed solution is transferred in the stainless steel cauldron of teflon lined, be incubated 3h at 300 DEG C, be precipitated thing.Again the precipitate ethanol obtained and distilled water cyclic washing, being evaporated at 100 DEG C, obtaining chemical general formula is Y1.90SiO5:0.07Pr3+, 0.03Yb3+Up-conversion phosphor.
Embodiment 7
Select Y2O3, Pr2O3And Yb2O3Powder body is 0.96mmol, 0.02mmol, 0.02mmol mixing by each component molal quantity.It is dissolved in the nitric acid solvent that concentration is 30% carrying out crystallization treatment after mixing and obtains crystal, then crystal to be dissolved in distilled water and adds molar concentration in the solution be 0.01mol/LNa2SiO3Solution 100ml, adds ammonia, and regulating pH value is 5.Then mixed solution is transferred in the stainless steel cauldron of teflon lined, be incubated 3h at 300 DEG C, be precipitated thing.Again the precipitate ethanol obtained and distilled water cyclic washing, being evaporated at 100 DEG C, obtaining chemical general formula is Y1.96SiO5:0.02Pr3+, 0.02Yb3+Up-conversion phosphor.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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, it is also possible to making some deformation and improvement, these broadly fall into 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 praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, it is characterised in that: there is following chemical general formula Y2-x-ySiO5: xPr3+,yYb3+, wherein, x is 0.01～0.08,0 < y≤0.1.
2. praseodymium ytterbium codope yttrium silicate up-conversion luminescent material according to claim 1, it is characterised in that described x is 0.05, y is 0.06.
3. the preparation method of a praseodymium ytterbium codope yttrium silicate up-conversion luminescent material, it is characterised in that comprise the following steps:
According to Y2-x-ySiO5: xPr3+,yYb3+The stoichiometric proportion of each element weighs Y2O3, Pr2O3,Yb2O3And Na2SiO3Powder body, wherein x is 0.01～0.08,0 < y≤0.1；
The Y that will weigh2O3, Pr2O3And Yb2O3Powder body mix homogeneously is dissolved in acid flux material, carries out crystallization treatment and obtains crystal；
Add dissolved with Na after crystal is dissolved in a solvent2SiO3The solution of powder body, adding ammonia adjustment pH value is 1～6, obtains mixed solution；And
At 150 DEG C～500 DEG C, described mixed solution being incubated 2 hours～10 hours, is precipitated thing, dry after the precipitate obtained is adopted cleaning mixture washing, obtaining chemical general formula is Y2-x-ySiO5: xPr3+,yYb3+Praseodymium ytterbium codope yttrium silicate up-conversion luminescent material.
4. the preparation method of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material according to claim 3, it is characterised in that described x is 0.05, y is 0.06.
5. the preparation method of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material according to claim 3, it is characterised in that described mixed solution is incubated 3 hours at 300 DEG C.
6. the preparation method of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material according to claim 3, it is characterised in that described dissolved in a solvent by crystal, wherein said solvent is distilled water or the mixed solution of distilled water and dehydrated alcohol, described Na2SiO3The molar concentration of the solution of powder body is 0.005mol/L～0.03mol/L.
7. the preparation method of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material according to claim 3, it is characterised in that described acid flux material is mass percentage concentration be 30% nitric acid or mass percentage concentration be the sulphuric acid of 30%.
8. the preparation method of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material according to claim 3, it is characterised in that described pH value is 5.
9. the preparation method of praseodymium ytterbium codope yttrium silicate up-conversion luminescent material according to claim 3, it is characterised in that described cleaning mixture is distilled water and dehydrated alcohol.
10. an Organic Light Emitting Diode, including the substrate stacked gradually, negative electrode, organic luminous layer, transparent anode and transparent encapsulated layer, it is characterized in that, doped with praseodymium ytterbium codope yttrium silicate up-conversion luminescent material in described transparent encapsulated layer, the chemical general formula of described praseodymium ytterbium codope yttrium silicate up-conversion luminescent material is Y2-x-ySiO5: xPr3+,yYb3+, wherein, x is 0.01～0.08,0 < y≤0.1.
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| Pr3+:Y2SiO5晶体中橙—蓝频率上转换过程;李建福等;《吉林大学学报(理学版)》;20061130;976-979 * |
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