CN103421503A - Holmium and ytterbium doped gadolinium oxide salt up-conversion luminescent material and preparation method and application thereof - Google Patents

Holmium and ytterbium doped gadolinium oxide salt up-conversion luminescent material and preparation method and application thereof Download PDF

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CN103421503A
CN103421503A CN2012101511791A CN201210151179A CN103421503A CN 103421503 A CN103421503 A CN 103421503A CN 2012101511791 A CN2012101511791 A CN 2012101511791A CN 201210151179 A CN201210151179 A CN 201210151179A CN 103421503 A CN103421503 A CN 103421503A
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luminescent material
conversion luminescent
salt
holmium
gadolinium sesquioxide
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周明杰
王平
陈吉星
黄辉
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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 holmium and ytterbium doped gadolinium oxide salt up-conversion luminescent material has the following chemical general formula of Gd2O3:xHo<3+>,yYb<3+>, wherein X is 0.01-0.08, and y is 0-0.1. In a photoluminescence spectrum of the holmium and ytterbium doped gadolinium oxide salt up-conversion luminescent material, the excitation wavelength of the holmium and ytterbium doped gadolinium oxide salt up-conversion luminescent material is 640 nm, in a wavelength region of 490 nm, luminescence peaks can be produced by transition radiation from <5>F3 to <5>I8 of Ho<3+> ions, and the holmium and ytterbium doped gadolinium oxide salt up-conversion luminescent material can be used as a blue light luminescent material. The invention also provides a preparation method of the holmium and ytterbium doped gadolinium oxide salt up-conversion luminescent material, and organic light-emitting diodes using the holmium and ytterbium doped gadolinium oxide salt up-conversion luminescent material.

Description

Holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material, preparation method and application thereof
Technical field
The present invention relates to a kind of holmium ytterbium doping gadolinium sesquioxide salt 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 holmium ytterbium doping gadolinium sesquioxide salt 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 holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material, the preparation method of blue light and be used the Organic Light Emitting Diode of this holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material by long-wave radiation.
A kind of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material, have following chemical formula Gd 2O 3: xHo 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 0.06 therein.
A kind of preparation method of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material, comprise the following steps: according to Gd 2O 3: xHo 3+, yYb 3+The stoichiometric ratio of each element takes Gd 2O 3, Ho 2O 3And Yb 2O 3Powder, wherein x is that 0.01～0.08, y is 0～0.1;
The powder taken is mixed to be dissolved in acid solvent and carry out crystallization treatment and obtain crystallisate;
Crystallisate is dissolved in solvent, then add ammoniacal liquor to regulate pH value to be 1～6, to obtain mixing solutions;
Described mixing solutions is incubated to 2 hours～10 hours under 150 ℃～500 ℃, is precipitated thing, adopt the washings washing rear dry the throw out obtained,, obtain holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material.
In embodiment, x is that 0.05, y is 0.06 therein.
In embodiment, described mixing solutions is incubated 3 hours under 300 ℃ therein.
Therein in embodiment, described crystallisate is dissolved in solvent to the mixing solutions that wherein said solvent is distilled water or distilled water and dehydrated alcohol.
Therein in embodiment, described acid solvent comprises the sulfuric acid that nitric acid that mass percentage concentration is 30% or mass percentage concentration are 30%.
In embodiment, described pH value is 5 therein.
In embodiment, described washings is distilled water and dehydrated alcohol therein.
A kind of Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the encapsulated layer that stack gradually, in described encapsulated layer, doped with holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material, the chemical formula of this holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material is Gd 2O 3: xHo 3+, yYb 3+, wherein x is that 0.01～0.08, y is 0～0.1.
Hydrothermal method mild condition, the synthesis temperature of above-mentioned holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material are low 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 the holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material of preparation, the excitation wavelength of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material is 640nm, at the 490nm wavelength zone by Ho 3+Ion 5F 3→ 5I 8Transition 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 holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material that Fig. 2 is embodiment 1 preparation;
The XRD spectra of the holmium ytterbium doping gadolinium sesquioxide salt 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 neodymium ytterbium codope aluminum oxide up-conversion luminescent material.
Embodiment
Below in conjunction with the drawings and specific embodiments, holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material and preparation method thereof is further illustrated.
The holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material of one embodiment, its chemical formula is Gd 2O 3: xHo 3+, yYb 3+, wherein, x is that 0.01～0.08, y is 0～0.1.
Preferably, x is that 0.05, y is 0.06.
In the photoluminescence spectra of this holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material, the excitation wavelength of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material is 640nm, when material is subject to long wavelength's (as 640nm) radiation, and Yb 3+The ionic absorption quantity of radiant energy, to Ho 3+Ion-transfer, Ho 3+Ion excitation arrives 5F 3Excited state, then to 5I 8The energy state transition, send the blue light of 490nm, can be used as blue light emitting material.
The preparation method of above-mentioned holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material comprises the following steps:
Step S11, according to Gd 2O 3: xHo 3+, yYb 3+The stoichiometric ratio of each element takes Gd 2O 3, Ho 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 0.06.
Step S13, the powder taken in step S11 is mixed to be dissolved in acid solvent and carry out crystallization treatment and obtain crystallisate, crystallisate is dissolved in solvent, then add ammoniacal liquor to regulate pH value to be 1～6, to obtain mixing solutions.
In this step, preferred, described acid solvent comprises the sulfuric acid that nitric acid that mass percentage concentration is 30% or mass percentage concentration are 30%;
In this step, preferred, the mixing solutions that described solvent is distilled water or distilled water and dehydrated alcohol.
Step S15, described mixing solutions is incubated to 2 hours～10 hours under 150 ℃～500 ℃, is precipitated thing, the throw out obtained is adopted after the washings washing dry, obtaining holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material chemical general formula is Gd 2O 3: xHo 3+, yYb 3+.
In this step, preferred, mixing solutions is transferred in the stainless steel cauldron of tetrafluoroethylene lining, and under 300 ℃, insulation is 3 hours.
In this step, preferred, described washings is distilled water and dehydrated alcohol.
In this step, preferred, x is that 0.05, y is 0.06.
Hydrothermal method mild condition, the synthesis temperature of above-mentioned holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material are low 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 the holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material of preparation, the excitation wavelength of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material is 640nm, at the 490nm wavelength zone by Ho 3+Ion 5F 3→ 5I 8Transition 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 holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material is Gd 2O 3: xHo 3+, yYb 3+, wherein, x is that 0.01～0.08, y is 0～0.1.
Be dispersed with holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material 6 in the transparent encapsulated layer 5 of Organic Light Emitting Diode 100, the excitation wavelength of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material is 640nm, at the 490nm wavelength zone by Ho 3+Ion 5F 3→ 5I 8Transition 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 Gd 2O 3, Ho 2O 3And Yb 2O 3Powder is 0.89mmol by the each component mole number, 0.05mmol, and 0.06mmol mixes.Carry out crystallization treatment in the nitric acid solvent that to be dissolved in concentration after mixing be 30% and obtain crystallisate, then be dissolved in crystallisate in distilled water and add ammoniacal liquor in solution, regulating pH value is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 ℃ of insulation 3h, be precipitated thing.Again ethanol and distilled water repetitive scrubbing for the throw out that obtains, 100 ℃ of lower evaporates to dryness, obtaining chemical general formula is Gd 2O 3: 0.05Ho 3+, 0.06Yb 3+Up-conversion phosphor.
Refer to Fig. 2, Figure 2 shows that the holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material chemical general formula that this enforcement obtains is Gd 2O 3: 0.05Ho 3+, 0.06Yb 3+Photoluminescence spectra figure with the contrast of mixing altogether the ytterbium element of undoping.As seen from Figure 2, the excitation wavelength of the holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material that the present embodiment obtains is 640nm, Yb 3+Absorb luminous energy, to Ho 3+Ion transport, make Ho 3+Ion produces 5F 3→ 5I 8Transition radiation form 490nm wavelength zone glow peak, this holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material can be used as blue light emitting material.Curve 1 is the photoluminescence spectrum of embodiment 1, and curve 2 is the Comparative Examples (Gd of ytterbium element of not adulterating 2O 3: 0.05Ho 3+), contrast the codope of known holmium ytterbium and can access better illumination effect.Holmium ion is luminescence center, and ytterbium ion has served as the sensitized ions of phototransformation, strengthens luminous.
Refer to Fig. 3, in Fig. 3, curve is for implementing the XRD curve of the 1 holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material prepared, test comparison standard P DF card.Diffraction peak in contrast PDF card figure is the peak crystallization of gadolinium sesquioxide, the diffraction peak of doped element and other impurity do not occur; Illustrate that the product that this preparation method obtains has good crystalline quality.
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 neodymium ytterbium codope aluminum oxide up-conversion luminescent material, curve 2 is not doped with the contrast of praseodymium ytterbium neodymium ytterbium codope aluminum oxide up-conversion luminescent material.In figure, can find out, fluorescent material can inspire the blue light of shortwave by the red light of long wave, blendes together white light.
Embodiment 2
Select Gd 2O 3, Ho 2O 3And Yb 2O 3Powder is 0.82mmol by the each component mole number, 0.08mmol, and 0.1mmol mixes.Carry out crystallization treatment in the sulfuric acid solvent that to be dissolved in concentration after mixing be 30% and obtain crystallisate, then be dissolved in crystallisate in distilled water and add ammoniacal liquor in solution, regulating pH value is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 150 ℃ of insulation 2h, be precipitated thing.Again ethanol and distilled water repetitive scrubbing for the throw out that obtains, 100 ℃ of lower evaporates to dryness, obtaining chemical general formula is Gd 2O 3: 0.08Ho 3+, 0.1Yb 3+Up-conversion phosphor.
Embodiment 3
Select Gd 2O 3, Ho 2O 3Powder is 0.99mmol by the each component mole number, and 0.01mmol mixes.Carry out crystallization treatment in the nitric acid solvent that to be dissolved in concentration after mixing be 30% and obtain crystallisate, then be dissolved in crystallisate in distilled water and add ammoniacal liquor in solution, regulating pH value is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 ℃ of insulation 3h, be precipitated thing.Again ethanol and distilled water repetitive scrubbing for the throw out that obtains, 100 ℃ of lower evaporates to dryness, obtaining chemical general formula is Gd 2O 3: 0.01Ho 3+Up-conversion phosphor.
Embodiment 4
Select Gd 2O 3, Ho 2O 3And Yb 2O 3The powder powder is 0.92mmol by the each component mole number, 0.03mmol, and 0.05mmol mixes.Carry out crystallization treatment in the nitric acid solvent that to be dissolved in concentration after mixing be 30% and obtain crystallisate, then be dissolved in crystallisate in distilled water and add ammoniacal liquor in solution, regulating pH value is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 ℃ of insulation 3h, be precipitated thing.Again ethanol and distilled water repetitive scrubbing for the throw out that obtains, 100 ℃ of lower evaporates to dryness, obtaining chemical general formula is Gd 2O 3: 0.03Ho 3+, 0.05Yb 3+Up-conversion phosphor.
Embodiment 5
Select Gd 2O 3, Ho 2O 3And Yb 2O 3Powder is 0.90mmol by the each component mole number, 0.06mmol, and 0.04mmol mixes.Carry out crystallization treatment in the nitric acid solvent that to be dissolved in concentration after mixing be 30% and obtain crystallisate, then be dissolved in crystallisate in distilled water and add ammoniacal liquor in solution, regulating pH value is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 ℃ of insulation 3h, be precipitated thing.Again ethanol and distilled water repetitive scrubbing for the throw out that obtains, 100 ℃ of lower evaporates to dryness, obtaining chemical general formula is Gd 2O 3: 0.06Ho 3+, 0.04Yb 3+Up-conversion phosphor.
Embodiment 6
Select Gd 2O 3, Ho 2O 3And Yb 2O 3Powder is 0.90mmol by the each component mole number, 0.07mmol, and 0.03mmol mixes.Carry out crystallization treatment in the nitric acid solvent that to be dissolved in concentration after mixing be 30% and obtain crystallisate, then be dissolved in crystallisate in distilled water and add ammoniacal liquor in solution, regulating pH value is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 ℃ of insulation 3h, be precipitated thing.Again ethanol and distilled water repetitive scrubbing for the throw out that obtains, 100 ℃ of lower evaporates to dryness, obtaining chemical general formula is Gd 2O 3: 0.07Ho 3+, 0.03Yb 3+Up-conversion phosphor.
Embodiment 7
Select Gd 2O 3, Ho 2O 3And Yb 2O 3Powder is 0.96mmol by the each component mole number, 0.02mmol, and 0.02mmol mixes.Carry out crystallization treatment in the nitric acid solvent that to be dissolved in concentration after mixing be 30% and obtain crystallisate, then be dissolved in crystallisate in distilled water and add ammoniacal liquor in solution, regulating pH value is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 ℃ of insulation 3h, be precipitated thing.Again ethanol and distilled water repetitive scrubbing for the throw out that obtains, 100 ℃ of lower evaporates to dryness, obtaining chemical general formula is Gd 2O 3: 0.02Ho 3+, 0.02Yb 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 holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material, is characterized in that: have following chemical general formula Gd 2O 3: xHo 3+, yYb 3+, wherein, x is that 0.01～0.08, y is 0～0.1.
2. holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material according to claim 1, is characterized in that, described x is that 0.05, y is 0.06.
3. the preparation method of a holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material, is characterized in that, comprises the following steps:
According to Gd 2O 3: xHo 3+, yYb 3+The stoichiometric ratio of each element takes Gd 2O 3, Ho 2O 3And Yb 2O 3Powder, wherein x is that 0.01～0.08, y is 0～0.1;
The powder taken is mixed and is dissolved in acid solvent, carry out crystallization treatment and obtain crystallisate;
Crystallisate is dissolved in solvent, then add ammoniacal liquor to regulate pH value to be 1～6, to obtain mixing solutions; And
Described mixing solutions is incubated to 2 hours～10 hours under 150 ℃～500 ℃, is precipitated thing, adopt the washings washing rear dry the throw out obtained, obtaining chemical general formula is Gd 2O 3: xHo 3+, yYb 3+Holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material.
4. the preparation method of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material according to claim 3, is characterized in that, described x is that 0.05, y is 0.06.
5. the preparation method of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material according to claim 3, is characterized in that, described mixing solutions is incubated 3 hours under 300 ℃.
6. the preparation method of holmium ytterbium according to claim 3 doping gadolinium sesquioxide salt up-conversion luminescent material, is characterized in that, described crystallisate dissolved in solvent to the mixing solutions that wherein said solvent is distilled water or distilled water and dehydrated alcohol.
7. the preparation method of holmium ytterbium according to claim 3 doping gadolinium sesquioxide salt up-conversion luminescent material, is characterized in that, described acid solvent is the sulfuric acid that the mass percentage concentration nitric acid that is 30% or mass percentage concentration are 30%.
8. the preparation method of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material according to claim 3, is characterized in that, described pH value is 5.
9. the preparation method of holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material according to claim 3, is characterized in that, described washings is distilled water and dehydrated alcohol.
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 encapsulated layer, doped with holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material, the chemical general formula of described holmium ytterbium doping gadolinium sesquioxide salt up-conversion luminescent material is Gd 2O 3: xHo 3+, yYb 3+, wherein, x is that 0.01～0.08, y is 0～0.1.
CN2012101511791A 2012-05-16 2012-05-16 Holmium and ytterbium doped gadolinium oxide salt up-conversion luminescent material and preparation method and application thereof Pending CN103421503A (en)

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Application publication date: 20131204