CN103421500A - Praseodymium and ytterbium double-doped molybdate up-conversion luminescent material and preparation method thereof, and organic light emitting diode - Google Patents

Praseodymium and ytterbium double-doped molybdate up-conversion luminescent material and preparation method thereof, and organic light emitting diode Download PDF

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CN103421500A
CN103421500A CN2012101485072A CN201210148507A CN103421500A CN 103421500 A CN103421500 A CN 103421500A CN 2012101485072 A CN2012101485072 A CN 2012101485072A CN 201210148507 A CN201210148507 A CN 201210148507A CN 103421500 A CN103421500 A CN 103421500A
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luminescent material
molybdate
conversion luminescent
praseodymium
ytterbium codope
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周明杰
王平
陈吉星
张振华
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

A praseodymium and ytterbium double-doped molybdate up-conversion luminescent material has the following chemical general formula of LiLa1-x-y(MoO4)2:xPr<3+>,yYb<3+>, wherein x is 0.01-0.08, and y is 0-0.1. In photoluminescence spectra of the praseodymium and ytterbium double-doped molybdate up-conversion luminescent material, an excitation wavelength of the praseodymium and ytterbium double-doped molybdate up-conversion luminescent material is 980 nm, a luminescent peak is formed by transition radiation of Pr<3+> ion <3>P0 -> <3>H4 in a 485 nm wavelength area, and thus the material can be used as a blue light luminescent material. The invention also provides a preparation method of the praseodymium and ytterbium double-doped molybdate up-conversion luminescent material and an organic light emitting diode using the praseodymium and ytterbium double-doped molybdate up-conversion luminescent material.

Description

Praseodymium ytterbium codope molybdate up-conversion luminescent material, preparation method and Organic Light Emitting Diode
Technical field
The present invention relates to a kind of praseodymium ytterbium codope molybdate up-conversion luminescent material, preparation method and Organic Light Emitting Diode.
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, because the OLED blue light material that obtains at present stability and high efficiency is more difficult, 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, be 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 praseodymium ytterbium codope molybdate 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 praseodymium ytterbium codope molybdate up-conversion luminescent material, the preparation method of blue light and be used the Organic Light Emitting Diode of this praseodymium ytterbium codope molybdate up-conversion luminescent material by long-wave radiation.
A kind of praseodymium ytterbium codope molybdate up-conversion luminescent material, have following chemical formula LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+, wherein x is that 0.01 ~ 0.08, y is 0 ~ 0.1.
In embodiment, x is that 0.05, y is 0.08 therein.
A kind of preparation method of praseodymium ytterbium codope molybdate up-conversion luminescent material comprises the following steps:
According to LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+The stoichiometric ratio of each element takes Li 2O, La 2O 3, MoO 3, Pr 2O 3And Yb 2O 3Powder, wherein x is that 0.01 ~ 0.08, y is 0 ~ 0.1;
The powder taken is dissolved in to acid solvent, adds afterwards dispersion agent and basic solvent to obtain containing sedimentary mixture simultaneously;
It is 7 ~ 9 that adjusting contains sedimentary mixture pH value, then filters, and, with dehydrated alcohol and distilled water wash, is precipitated thing; And
Throw out is dried under 900 ℃ ~ 1300 ℃ to burning, drying the burning time is 2 hours ~ 5 hours, and obtaining chemical general formula is LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+Praseodymium ytterbium codope molybdate up-conversion luminescent material.
In embodiment, described x is that 0.05, y is 0.08 therein.
Therein in embodiment, described acid solvent is the sulfuric acid that the mass percentage concentration hydrochloric acid that is 30% or mass percentage concentration are 30%.
In embodiment, described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol therein.
In embodiment, described basic solvent is ammoniacal liquor therein.
In embodiment, described pH value is 5 therein.
In embodiment, described throw out is transferred in retort furnace and is dried and burn under 1000 ℃ therein, and drying the burning time is 3 hours.
A kind of Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, transparent anode and the transparent encapsulated layer that stack gradually, in described transparent encapsulated layer, doped with praseodymium ytterbium codope molybdate up-conversion luminescent material, the chemical general formula of this praseodymium ytterbium codope molybdate up-conversion luminescent material is LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+, wherein x is that 0.01 ~ 0.08, y is 0 ~ 0.1.
The hydrothermal method mild condition of above-mentioned praseodymium ytterbium codope molybdate up-conversion luminescent material, synthesis temperature hang down more easy to control, and granularity and the pattern of product are controlled, the powder complete crystallization of preparation, good dispersity, cost is lower, produces comparatively environmental protection in the simultaneous reactions process without the three wastes; In the photoluminescence spectra of praseodymium ytterbium codope molybdate up-conversion luminescent material of preparation, the excitation wavelength of praseodymium ytterbium codope molybdate up-conversion luminescent material is 980nm, at the 485nm wavelength zone by Pr 3+Ion 3P 0→ 3H 4Transition radiation form glow peak, can be used as blue light emitting material.
The accompanying drawing explanation
The structural representation of the Organic Light Emitting Diode that Fig. 1 is an embodiment.
The photoluminescence spectrogram of the praseodymium ytterbium codope molybdate up-conversion luminescent material that Fig. 2 is embodiment 1 preparation.
The XRD spectra of the praseodymium ytterbium codope molybdate up-conversion luminescent material that Fig. 3 is embodiment 1 preparation.
In the transparent encapsulated layer that Fig. 4 is embodiment 1 preparation doped with the spectrogram of the Organic Light Emitting Diode of praseodymium ytterbium praseodymium ytterbium codope molybdate up-conversion luminescent material.
Embodiment
Below in conjunction with the drawings and specific embodiments, praseodymium ytterbium codope molybdate up-conversion luminescent material and preparation method thereof is further illustrated.
The praseodymium ytterbium codope molybdate up-conversion luminescent material of one embodiment, have following chemical general formula LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+, wherein x is that 0.01 ~ 0.08, y is 0 ~ 0.1.
Preferably, x is that 0.05, y is 0.08.
In the photoluminescence spectra of this praseodymium ytterbium codope molybdate up-conversion luminescent material, the excitation wavelength of praseodymium ytterbium codope molybdate up-conversion luminescent material is 980nm, when material is subject to long wavelength's (as 980nm) radiation, and Yb 3+The ionic absorption quantity of radiant energy, to Pr 3+Ion-transfer, Pr 3+Ion excitation arrives 3P 0Excited state, then to 3H 4The energy state transition, send the blue light of 485nm, can be used as blue light emitting material.
The preparation method of above-mentioned praseodymium ytterbium codope molybdate up-conversion luminescent material comprises the following steps:
Step S11, according to LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+The stoichiometric ratio of each element takes Li 2O, La 2O 3, MoO 3, Pr 2O 3And Yb 2O 3Powder, wherein x is that 0.01 ~ 0.08, y is 0 ~ 0.1.
In this step, preferred, x is that 0.05, y is 0.08.
Step S13, will in the powder taken in step S11, add acid solvent, add afterwards dispersion agent and basic solvent to obtain containing sedimentary mixture simultaneously.
In this step, preferred, described acid solvent comprises the sulfuric acid that hydrochloric acid that mass percentage concentration is 30% or mass percentage concentration are 30%;
In this step, preferred, described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
In this step, preferred, described basic solvent is ammoniacal liquor.
In this step, dispersion agent is that same ammoniacal liquor splashes into together, and the effect of ammoniacal liquor is neutralization acidity the throw out that produces oxyhydroxide and oxide compound, and the dispersion agent effect is that the throw out that prevents generation is reunited.
It is 7 ~ 9 that step S15, adjusting contain sedimentary mixture pH value, then filters, and, with dehydrated alcohol and distilled water wash, is precipitated thing.
In this step, preferred, described pH value is 5.
Step S17, throw out is dried under 900 ℃ ~ 1300 ℃ to burning, drying the burning time is 2 hours ~ 5 hours, and obtaining chemical general formula is LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+Praseodymium ytterbium codope molybdate up-conversion luminescent material.
In this step, preferred, described throw out is transferred in retort furnace and is dried and burn under 1000 ℃, and drying the burning time is 3 hours.
The hydrothermal method mild condition of above-mentioned praseodymium ytterbium codope molybdate up-conversion luminescent material, synthesis temperature hang down more easy to control, and granularity and the pattern of product are controlled, the powder complete crystallization of preparation, good dispersity, cost is lower, produces comparatively environmental protection in the simultaneous reactions process without the three wastes; In the photoluminescence spectra of praseodymium ytterbium codope molybdate up-conversion luminescent material of preparation, the excitation wavelength of praseodymium ytterbium codope molybdate up-conversion luminescent material is 980nm, at the 485nm wavelength zone by Pr 3+Ion 3P 0→ 3H 4Transition radiation form glow peak, can be used as blue light emitting material.
Refer to Fig. 1, 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 stacked gradually.Be dispersed with praseodymium ytterbium codope molybdate up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical general formula of praseodymium ytterbium codope molybdate up-conversion luminescent material is LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+, wherein x is that 0.01 ~ 0.08, y is 0 ~ 0.1.
Be dispersed with praseodymium ytterbium codope molybdate up-conversion luminescent material 6 in the transparent encapsulated layer 5 of Organic Light Emitting Diode 100, the excitation wavelength of praseodymium ytterbium codope molybdate up-conversion luminescent material is 980nm, at the 485nm wavelength zone by Pr 3+Ion 3P 0→ 3H 4Transition radiation form glow peak, excite and can launch blue light by red-green glow, blue light mixes the Organic Light Emitting Diode that formation emits white light afterwards with red-green glow.
It is below specific embodiment.
Embodiment 1
Select Li 2O, La 2O 3, MoO 3, Pr 2O 3And Yb 2O 3Powder is 0.5mmol by the each component mole number, 0.89mmol, and 2mmol, 0.05mmol, 0.06mmol mixes.In the hydrochloric acid solvent that to be dissolved in mass percentage concentration after mixing be 30%, drip oxalic acid adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, the pH value of regulating mixing solutions is 8 left and right, within standing 2 hours, make precipitation fully, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours under 1000 ℃, obtaining chemical general formula is LiLa 0.89(MoO 4) 2: 0.05Pr 3+, 0.06Yb 3+Praseodymium ytterbium codope molybdate up-conversion luminescent material.
Refer to Fig. 2, Figure 2 shows that the praseodymium ytterbium codope molybdate up-conversion luminescent material chemical general formula that this enforcement obtains is LiLa 0.89(MoO 4) 2: 0.05Pr 3+, 0.06Yb 3+Photoluminescence spectra figure.As seen from Figure 2, curve 1 is 980nm for the excitation wavelength of the praseodymium ytterbium codope molybdate up-conversion luminescent material that the present embodiment obtains, at the 485nm wavelength zone by Pr 3+Ion 3P 0→ 3H 4Transition radiation form glow peak, this praseodymium ytterbium codope molybdate up-conversion luminescent material can be used as blue light emitting material, curve 2 is to undope and mix altogether Yb under same preparation condition with the embodiment of the present invention 3+The contrast LiLa of element 0.89(MoO 4) 2: 0.05Pr 3+.The contrast accompanying drawing can find out that Yb is arranged 3+The luminous intensity of coactivated sample is significantly improved.
Refer to Fig. 3, in Fig. 3, curve is for implementing the XRD curve of the 1 praseodymium ytterbium codope molybdate up-conversion luminescent material prepared, test comparison standard P DF card.Contrast PDF card, diffraction peak is depicted as the crystalline phase of molybdate, the peak that doped element is relevant do not occur, illustrates that doped element is the lattice that has entered molybdate.
In the transparent encapsulated layer that Fig. 4 is embodiment 1 preparation, doped with the spectrogram of the Organic Light Emitting Diode of praseodymium ytterbium praseodymium ytterbium codope molybdate up-conversion luminescent material, curve 2 is not doped with the contrast of praseodymium ytterbium praseodymium ytterbium codope molybdate up-conversion luminescent material.Can find out in figure, doped with the Organic Light Emitting Diode of praseodymium ytterbium praseodymium ytterbium codope molybdate up-conversion luminescent material, can inspire the blue light of shortwave by the red light of long wave, blend together white light.
Embodiment 2
Select Li 2O, La 2O 3, MoO 3, Pr 2O 3And Yb 2O 3Powder is 0.5mmol by the each component mole number, 0.82mmol, and 2mmol, 0.08mmol, 0.1mmol mixes.In the sulfuric acid that to be dissolved in mass percentage concentration after mixing be 30%, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, the pH value of regulating mixing solutions is 8 left and right, within standing 2 hours, make precipitation fully, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours under 900 ℃, obtaining chemical general formula is LiLa 0.82(MoO 4) 2: 0.08Pr 3+, 0.1Yb 3+Praseodymium ytterbium codope molybdate up-conversion luminescent material.
Embodiment 3
Select Li 2O, La 2O 3, MoO 3, Pr 2O 3Powder is 0.5mmol by the each component mole number, 0.99mmol, and 2mmol, 0.01mmol mixes.In the hydrochloric acid solvent that to be dissolved in mass percentage concentration after mixing be 30%, drip trolamine adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, the pH value of regulating mixing solutions is 8 left and right, within standing 2 hours, make precipitation fully, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours under 1300 ℃, obtaining chemical general formula is LiLa 0.99(MoO 4) 2: 0.01Pr 3+Praseodymium ytterbium codope molybdate up-conversion luminescent material.
Embodiment 4
Select Li 2O, La 2O 3, MoO 3, Pr 2O 3Powder is 0.5mmol by the each component mole number, 0.92mmol, and 2mmol, 0.08mmol mixes.In the hydrochloric acid solvent that to be dissolved in mass percentage concentration after mixing be 30%, drip water soluble starch adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, the pH value of regulating mixing solutions is 8 left and right, within standing 2 hours, make precipitation fully, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 3 hours under 1100 ℃, obtaining chemical general formula is LiLa 0.92(MoO 4) 2: 0.08Pr 3+Praseodymium ytterbium codope molybdate up-conversion luminescent material.
Embodiment 5
Select Li 2O, La 2O 3, MoO 3, Pr 2O 3And Yb 2O 3Powder is 0.5mmol by the each component mole number, 0.89mmol, and 2mmol, 0.01mmol, 0.1mmol mixes.In the hydrochloric acid solvent that to be dissolved in mass percentage concentration after mixing be 30%, drip polyoxyethylene glycol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, the pH value of regulating mixing solutions is 8 left and right, within standing 2 hours, make precipitation fully, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2.5 hours under 1000 ℃, obtaining chemical general formula is LiLa 0.89(MoO 4) 2: 0.01Pr 3+, 0.1Yb 3+Praseodymium ytterbium codope molybdate up-conversion luminescent material.
Embodiment 6
Select Li 2O, La 2O 3, MoO 3, Pr 2O 3And Yb 2O 3Powder is 0.5mmol by the each component mole number, 0.9mmol, and 2mmol, 0.05mmol, 0.05mmol mixes.In the sulfuric acid that to be dissolved in mass percentage concentration after mixing be 30%, drip oxalic acid adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, the pH value of regulating mixing solutions is 8 left and right, within standing 2 hours, make precipitation fully, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours under 800 ℃, obtaining chemical general formula is LiLa 0.9(MoO 4) 2: 0.05Pr 3+, 0.05Yb 3+Praseodymium ytterbium codope molybdate up-conversion luminescent material.
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 praseodymium ytterbium codope molybdate up-conversion luminescent material, is characterized in that: have following chemical general formula LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+, wherein x is that 0.01 ~ 0.08, y is 0 ~ 0.1.
2. praseodymium ytterbium codope molybdate up-conversion luminescent material according to claim 1, is characterized in that, described x is that 0.05, y is 0.08.
3. the preparation method of a praseodymium ytterbium codope molybdate up-conversion luminescent material, is characterized in that, comprises the following steps:
According to LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+The stoichiometric ratio of each element takes Li 2O, La 2O 3, MoO 3, Pr 2O 3And Yb 2O 3Powder, wherein x is that 0.01 ~ 0.08, y is 0 ~ 0.1;
The powder taken is dissolved in to acid solvent, adds afterwards dispersion agent and basic solvent to obtain containing sedimentary mixture simultaneously;
It is 7 ~ 9 that adjusting contains sedimentary mixture pH value, then filters, and, with dehydrated alcohol and distilled water wash, is precipitated thing; And
Throw out is dried under 900 ℃ ~ 1300 ℃ to burning, drying the burning time is 2 hours ~ 5 hours, and obtaining chemical general formula is LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+Praseodymium ytterbium codope molybdate up-conversion luminescent material.
4. the preparation method of praseodymium ytterbium codope molybdate up-conversion luminescent material according to claim 3, is characterized in that, described x is that 0.05, y is 0.08.
5. the preparation method of praseodymium ytterbium codope molybdate up-conversion luminescent material according to claim 3, is characterized in that, described acid solvent is the sulfuric acid that the mass percentage concentration hydrochloric acid that is 30% or mass percentage concentration are 30%.
6. the preparation method of praseodymium ytterbium codope molybdate up-conversion luminescent material according to claim 3, is characterized in that, described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
7. the preparation method of praseodymium ytterbium codope molybdate up-conversion luminescent material according to claim 3, is characterized in that, described basic solvent is ammoniacal liquor.
8. the preparation method of praseodymium ytterbium codope molybdate up-conversion luminescent material according to claim 3, is characterized in that, described pH value is 5.
9. the preparation method of praseodymium ytterbium codope molybdate up-conversion luminescent material according to claim 3, is characterized in that, described throw out is transferred in retort furnace and dried and burn under 1000 ℃, and drying the burning time is 3 hours.
10. an Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, transparent anode and the transparent encapsulated layer that stack gradually, it is characterized in that, in described transparent encapsulated layer, doped with praseodymium ytterbium codope molybdate up-conversion luminescent material, the chemical general formula of described praseodymium ytterbium codope molybdate up-conversion luminescent material is LiLa 1-x-y(MoO 4) 2: xPr 3+, yYb 3+, wherein x is that 0.01 ~ 0.08, y is 0 ~ 0.1.
CN2012101485072A 2012-05-14 2012-05-14 Praseodymium and ytterbium double-doped molybdate up-conversion luminescent material and preparation method thereof, and organic light emitting diode Pending CN103421500A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109266347A (en) * 2018-11-23 2019-01-25 陕西科技大学 It is a kind of can be by red fluorescence powder and preparation method thereof that blue chip effectively excites

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109266347A (en) * 2018-11-23 2019-01-25 陕西科技大学 It is a kind of can be by red fluorescence powder and preparation method thereof that blue chip effectively excites

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Application publication date: 20131204