CN104449728A - Dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material as well as preparation method and application thereof - Google Patents

Dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material as well as preparation method and application thereof Download PDF

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CN104449728A
CN104449728A CN201310442641.8A CN201310442641A CN104449728A CN 104449728 A CN104449728 A CN 104449728A CN 201310442641 A CN201310442641 A CN 201310442641A CN 104449728 A CN104449728 A CN 104449728A
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luminescent material
barium fluoride
conversion luminescent
doped barium
dysprosium
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周明杰
陈吉星
王平
钟铁涛
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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

The invention discloses a dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material. The dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material has the following chemical general formula of aBaF2-bRF-cYF3:xDy<3+>, wherein a is 0.1-0.3, b is 0.05-0.15, c is 0.55-0.8, x is 0.01-0.08, and R is at least one of lithium element, sodium element, potassium element, rubidium element and cesium element. In the photoluminescence spectra of the dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material, the excitation wavelength of the dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material is 796nm, a luminescence peak is formed by a transition radiation from <4>F9/2 to <6>F15/2 of Dy<3+> ions in a 482nm wavelength area, and the dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material can be used as a blue-light luminescent material. The invention further provides a preparation method for the dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material, and an organic light emitting diode using the dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material.

Description

Dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material, preparation method and application thereof
Technical field
The present invention relates to a kind of dysprosium doped barium fluoride alkali yttrium 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 is short, flexible, and obtain a very wide range of application.But because the OLED blue light material obtaining stability and high efficiency is at present more difficult, significantly limit the development of white light OLED device and light source industry.
Upconverting fluorescent material can launch visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in the field such as optical fiber communication technology, fibre amplifier, 3 D stereo display, biomolecules fluorescence labelling, infrared detective.But, can by infrared, the long-wave radiations such as red-green glow inspire the dysprosium doped barium fluoride alkali yttrium 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 inspire the dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material.
A kind of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material, has following chemical formula aBaF 2-bRF-cYF 3: xDy 3+, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element.
Described a is 0.2, b be 0.11, c be 0.65, x is 0.04.
A preparation method for dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material, comprises the following steps: according to aBaF 2-bRF-cYF 3: xDy 3+the stoichiometric ratio of each element takes BaO, R 2cO 3, Y 2o 3and Dy 2o 3powder, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element;
The powder taken is mixed be dissolved in acid solvent and carry out crystallization treatment and obtain crystallisate;
Crystallisate is dissolved in a solvent, then to add ammoniacal liquor adjust ph be 1 ~ 6, obtain mixing solutions;
Described mixing solutions is transferred in the stainless steel cauldron of tetrafluoroethylene lining, at 150 DEG C ~ 500 DEG C, be incubated 2 hours ~ 10 hours, be precipitated thing, dry after the throw out obtained is adopted washings washing, obtaining chemical general formula is aBaF 2-bRF-cYF 3: xDy 3+dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material.
Described a is 0.2, b be 0.11, c be 0.65, x is 0.04.
Described mixing solutions is transferred in the stainless steel cauldron of tetrafluoroethylene lining, at 300 DEG C, be incubated 3 hours.
Describedly dissolved in a solvent by crystallisate, wherein said solvent is the mixing solutions of distilled water or distilled water and dehydrated alcohol.
Described acid solvent comprises hydrofluoric acid or Neutral ammonium fluoride or ammonium bifluoride.
Described pH value is 5.
Described washings is distilled water and dehydrated alcohol.
A kind of Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, doped with dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of this dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material is aBaF 2-bRF-cYF 3: xDy 3+, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element.
Hydrothermal method mild condition, the synthesis temperature of above-mentioned dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material are low more easy to control, the granularity of product and morphology controllable, the powder complete crystallization of preparation, good dispersity, cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of the dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material of preparation, the excitation wavelength of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material is 796nm, in 482nm wavelength zone by Dy 3+ion 4f 9/2→ 6f 15/2transition radiation formed glow peak, can 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 photoluminescence spectrogram of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material prepared by embodiment 1.
Fig. 3 is the Raman spectrogram of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material prepared by embodiment 1.
Fig. 4 is the spectrogram doped with the Organic Light Emitting Diode of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material formation in the transparent encapsulated layer of embodiment 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments, dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material and preparation method thereof is illustrated further.
The dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material of one embodiment, its chemical formula is aBaF 2-bRF-cYF 3: xDy 3+, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element.
Preferably, a is 0.2, b be 0.11, c be 0.65, x is 0.04.
In the photoluminescence spectra of this dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material, the excitation wavelength of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material is 796nm, when material is subject to the radiation of long wavelength (as 796nm) time, Dy 3+ion excitation arrives 4f 9/2excited state, then to 6f 15/2energy state transitions, sends the blue light of 482nm, can as blue light emitting material.
The preparation method of above-mentioned dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material, comprises the following steps:
Step S11, according to aBaF 2-bRF-cYF 3: xDy 3+the stoichiometric ratio of each element takes BaO, R 2cO 3, Y 2o 3, and Dy 2o 3powder, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element.
In this step, preferably, a is 0.2, b be 0.11, c be 0.65, x is 0.04.
Step S13, the powder taken mixed be dissolved in acid solvent and carry out crystallization treatment and obtain crystallisate in step S11, crystallisate is dissolved in a solvent, then to add ammoniacal liquor adjust ph be 1 ~ 6, obtain mixing solutions.
In this step, preferably, described acid solvent comprises hydrofluoric acid or Neutral ammonium fluoride or ammonium bifluoride;
In this step, preferably, described solvent is the mixing solutions of distilled water or distilled water and dehydrated alcohol.
Step S15, described mixing solutions is transferred in the stainless steel cauldron of tetrafluoroethylene lining, 2 hours ~ 10 hours are incubated at 150 DEG C ~ 500 DEG C, be precipitated thing, dry after the throw out obtained is adopted washings washing, obtaining dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material chemical general formula is aBaF 2-bRF-cYF 3: xDy 3+, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element.
In this step, preferably, mixing solutions is transferred in the stainless steel cauldron of tetrafluoroethylene lining, at 300 DEG C, be incubated 3 hours.
In this step, preferably, described washings is distilled water and dehydrated alcohol.
In this step, preferably, a is 0.2, b be 0.11, c be 0.65, x is 0.04.
Hydrothermal method mild condition, the synthesis temperature of above-mentioned dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material are low more easy to control, the granularity of product and morphology controllable, the powder complete crystallization of preparation, good dispersity, cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of the dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material of preparation, the excitation wavelength of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material is 796nm, in 482nm wavelength zone by Dy 3+ion 4f 9/2→ 6f 15/2transition radiation formed glow peak, can 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 the substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 that stack gradually.Be dispersed with dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material is aBaF 2-bRF-cYF 3: xDy 3+, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element.
Be dispersed with dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material 6 in the transparent encapsulated layer 5 of Organic Light Emitting Diode 100, the excitation wavelength of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material is 796nm, in 482nm wavelength zone by Dy 3+ion 4f 9/2→ 6f 15/2transition radiation form glow peak, excited can be launched blue light by red-green glow, blue light mixes with red-green glow and afterwards forms the Organic Light Emitting Diode emitted white light.
Be specific embodiment below.
Embodiment 1
Select BaO, Li 2cO 3, Y 2o 3and Dy 2o 3powder is 0.2mmol, 0.11mmol, 0.65mmol and 0.04mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 3 hours, obtains chemical general formula for 0.2BaF with 950 DEG C of calcinations 2-0.11LiF-0.65YF 3: 0.04Dy 3+up-conversion phosphor.
Refer to Fig. 2, Figure 2 shows that the dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material chemical general formula that this enforcement obtains is 0.2BaF 2-0.11LiF-0.65YF 3: 0.04Dy 3+photoluminescence spectra figure.As seen from Figure 2, the excitation wavelength of the dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material that the present embodiment obtains is 796nm, in 482nm wavelength zone by Dy 3+ion 4f 9/2→ 6f 15/2transition radiation formed glow peak, this dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is the Raman spectrum of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material prepared by enforcement 1, Raman peaks in figure is depicted as barium fluoride alkali yttrium characteristic peak, there is not the peak of doped element and other impurity, illustrate that doped element and substrate material define good bonding.
Fig. 4 is the spectrogram doped with the Organic Light Emitting Diode of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material formation in the transparent encapsulated layer of embodiment 1 preparation, and curve 2 is the contrast not adding fluorescent material.Can find out in figure that dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material by the red light of long wave, can inspire the blue light of shortwave, after blue light mixes with ruddiness, form white light.
Embodiment 2
Select BaO, Li 2cO 3, Y 2o 3and Dy 2o 3powder is 0.1mmol, 0.15mmol, 0.74mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 150 DEG C of insulation 2h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 2 hours, obtains chemical general formula for 0.1BaF with 800 DEG C of calcinations 2-0.15LiF-0.74YF 3: 0.01Dy 3+up-conversion phosphor.
Embodiment 3
Select BaO, Li 2cO 3, Y 2o 3and Dy 2o 3powder is 0.3mmol, 0.05mmol, 0.55mmol and 0.08mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 5 hours, obtains chemical general formula for 0.3BaF with 1000 DEG C of calcinations 2-0.05LiF-0.55YF 3: 0.08Dy 3+up-conversion phosphor.
Embodiment 4
Select BaO, Na 2cO 3, Y 2o 3and Dy 2o 3powder is 0.2mmol, 0.11mmol, 0.65mmol and 0.04mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 3 hours, obtains chemical general formula for 0.2BaF with 950 DEG C of calcinations 2-0.11NaF-0.65YF 3: 0.04Dy 3+up-conversion phosphor.
Embodiment 5
Select BaO, Na 2cO 3, Y 2o 3and Dy 2o 3powder is 0.1mmol, 0.15mmol, 0.74mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 150 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 2 hours, obtains chemical general formula for 0.1BaF with 800 DEG C of calcinations 2-0.15NaF-0.74YF 3: 0.01Dy 3+up-conversion phosphor.
Embodiment 6
Select BaO, Na 2cO 3, Y 2o 3and Dy 2o 3powder is 0.3mmol, 0.05mmol, 0.55mmol and 0.08mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 100 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 5 hours, obtains chemical general formula for 0.3BaF with 1000 DEG C of calcinations 2-0.05NaF-0.55YF 3: 0.08Dy 3+up-conversion phosphor.
Embodiment 7
Select BaO, K 2cO 3, Y 2o 3and Dy 2o 3powder is 0.2mmol, 0.11mmol, 0.65mmol and 0.04mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 3 hours, obtains chemical general formula for 0.2BaF with 950 DEG C of calcinations 2-0.11KF-0.65YF 3: 0.04Dy 3+up-conversion phosphor.
Embodiment 8
Select BaO, K 2cO 3, Y 2o 3and Dy 2o 3powder is 0.1mmol, 0.15mmol, 0.74mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 150 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 2 hours, obtains chemical general formula for 0.1BaF with 800 DEG C of calcinations 2-0.15KF-0.74YF 3: 0.01Dy 3+up-conversion phosphor.
Embodiment 9
Select BaO, K 2cO 3, Y 2o 3and Dy 2o 3powder is 0.3mmol, 0.05mmol, 0.55mmol and 0.08mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 100 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 5 hours, obtains chemical general formula for 0.3BaF with 1000 DEG C of calcinations 2-0.05KF-0.55YF 3: 0.08Dy 3+up-conversion phosphor.
Embodiment 10
Select BaO, Rb 2cO 3, Y 2o 3and Dy 2o 3powder is 0.2mmol, 0.11mmol, 0.65mmol and 0.04mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 3 hours, obtains chemical general formula for 0.2BaF with 950 DEG C of calcinations 2-0.11RbF-0.65YF 3: 0.04Dy 3+up-conversion phosphor.
Embodiment 11
Select BaO, Rb 2cO 3, Y 2o 3and Dy 2o 3powder is 0.1mmol, 0.15mmol, 0.74mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 150 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 2 hours, obtains chemical general formula for 0.1BaF with 800 DEG C of calcinations 2-0.15RbF-0.74YF 3: 0.01Dy 3+up-conversion phosphor.
Embodiment 12
Select BaO, Rb 2cO 3, Y 2o 3and Dy 2o 3powder is 0.3mmol, 0.05mmol, 0.55mmol and 0.08mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 100 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 5 hours, obtains chemical general formula for 0.3BaF with 1000 DEG C of calcinations 2-0.05RbF-0.55YF 3: 0.08Dy 3+up-conversion phosphor.
Embodiment 13
Select BaO, Cs 2cO 3, Y 2o 3and Dy 2o 3powder is 0.2mmol, 0.11mmol, 0.65mmol and 0.04mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 300 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 3 hours, obtains chemical general formula for 0.2BaF with 950 DEG C of calcinations 2-0.11CsF-0.65YF 3: 0.04Dy 3+up-conversion phosphor.
Embodiment 14
Select BaO, Cs 2cO 3, Y 2o 3and Dy 2o 3powder is 0.1mmol, 0.15mmol, 0.74mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 1.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 150 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 2 hours, obtains chemical general formula for 0.1BaF with 800 DEG C of calcinations 2-0.15CsF-0.74YF 3: 0.01Dy 3+up-conversion phosphor.
Embodiment 15
Select BaO, Cs 2cO 3, Y 2o 3and Dy 2o 3powder is 0.3mmol, 0.05mmol, 0.55mmol and 0.08mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid solvent and carry out crystallization treatment and obtain crystallisate, then crystallisate is dissolved in distilled water and adds ammoniacal liquor in the solution, adjust ph is 5.Then mixing solutions is transferred in the stainless steel cauldron of teflon lined, at 100 DEG C of insulation 3h, be precipitated thing.Again the throw out ethanol obtained and distilled water repetitive scrubbing, evaporate to dryness at 100 DEG C, puts into retort furnace and within 5 hours, obtains chemical general formula for 0.3BaF with 1000 DEG C of calcinations 2-0.05CsF-0.55YF 3: 0.08Dy 3+up-conversion phosphor.
The above embodiment only have expressed several embodiment 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, 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 doped barium fluoride alkali yttrium up-conversion luminescent material, is characterized in that, has following chemical general formula aBaF 2-bRF-cYF 3: xDy 3+, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element.
2. dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material according to claim 1, is characterized in that, described a is 0.2, b be 0.11, c be 0.65, x is 0.04.
3. a preparation method for dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material, is characterized in that, comprise the following steps:
According to aBaF 2-bRF-cYF 3: xDy 3+the stoichiometric ratio of each element takes BaO, R 2cO 3, Y 2o 3and Dy 2o 3powder, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element;
Being mixed by the powder taken is dissolved in acid solvent, carries out crystallization treatment and obtains crystallisate;
Crystallisate is dissolved in a solvent, then to add ammoniacal liquor adjust ph be 1 ~ 6, obtain mixing solutions; And
Transferred to by described mixing solutions in the stainless steel cauldron of tetrafluoroethylene lining, be incubated 2 hours ~ 10 hours, be precipitated thing at 150 DEG C ~ 500 DEG C, dry after the throw out obtained is adopted washings washing, obtaining chemical general formula is aBaF 2-bRF-cYF 3: xDy 3+dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material.
4. the preparation method of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material according to claim 3, is characterized in that, described a is 0.2, b be 0.11, c be 0.65, x is 0.04.
5. the preparation method of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material according to claim 3, it is characterized in that, described mixing solutions is transferred in the stainless steel cauldron of tetrafluoroethylene lining, at 300 DEG C, be incubated 3 hours.
6. the preparation method of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material according to claim 3, is characterized in that, is describedly dissolved in a solvent by crystallisate, and wherein said solvent is the mixing solutions of distilled water or distilled water and dehydrated alcohol.
7. the preparation method of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material according to claim 3, it is characterized in that, described acid solvent is hydrofluoric acid, Neutral ammonium fluoride or ammonium bifluoride.
8. the preparation method of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material according to claim 3, it is characterized in that, described pH value is 5.
9. the preparation method of dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material according to claim 3, it 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, anode and the transparent encapsulated layer that stack gradually, it is characterized in that, doped with dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material in described transparent encapsulated layer, the chemical general formula of described dysprosium doped barium fluoride alkali yttrium up-conversion luminescent material is aBaF 2-bRF-cYF 3: xDy 3+, wherein, a is 0.1 ~ 0.3, b be 0.05 ~ 0.15, c be 0.55 ~ 0.8, x be 0.01 ~ 0.08, R is elemental lithium, sodium element, potassium element, at least one in rubidium element and cesium element.
CN201310442641.8A 2013-09-25 2013-09-25 Dysprosium-doped barium fluoride basic yttrium up-conversion luminescent material as well as preparation method and application thereof Pending CN104449728A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108865120A (en) * 2018-08-13 2018-11-23 福州大学 A kind of europium ion-doped CaF2The preparation method and applications of light function powder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108865120A (en) * 2018-08-13 2018-11-23 福州大学 A kind of europium ion-doped CaF2The preparation method and applications of light function powder
CN108865120B (en) * 2018-08-13 2021-03-02 福州大学 Europium ion doped CaF2Preparation method and application of optical functional powder

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