CN104212456A - Holmium doped double alkaline-earth metal yttrium fluoride up-conversion luminescent material, preparation method, and organic light emitting diode - Google Patents

Holmium doped double alkaline-earth metal yttrium fluoride up-conversion luminescent material, preparation method, and organic light emitting diode Download PDF

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CN104212456A
CN104212456A CN201310206305.3A CN201310206305A CN104212456A CN 104212456 A CN104212456 A CN 104212456A CN 201310206305 A CN201310206305 A CN 201310206305A CN 104212456 A CN104212456 A CN 104212456A
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luminescent material
conversion luminescent
yttrium fluoride
alkaline earth
fluoride salt
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周明杰
陈吉星
王平
冯小明
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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 holmium doped double alkaline-earth metal yttrium fluoride up-conversion luminescent material, which is represented by a chemical formula: AmB<1-m>Y2F8:xHo3+, wherein x is in a range of 0.01 to 0.08, m is in a range of 0.1 to 0.9, the A represents a magnesium element, a calcium element, a strontium element, or a barium element, and the B represents a magnesium element, a calcium element, a strontium element, or a barium element. In the photoluminescence spectrum of the holmium doped double alkaline-earth metal yttrium fluoride up-conversion luminescent material, the excitation wave length of the up-conversion luminescent material is at 640 nm, a luminescence peak is formed in the 490 nm wavelength zone by the transition excitation of the Ho3+ ion from the 5F3 to 5I8, and the up-conversion luminescent material can be used as a blue light luminescent material. The invention also provides a preparation method of the up-conversion luminescent material, and an organic light emitting diode using the up-conversion luminescent material.

Description

Holmium doping two alkaline earth yttrium fluoride salt up-conversion luminescent material, preparation method and Organic Light Emitting Diode
Technical field
The present invention relates to the doping of a kind of holmium two alkaline earth yttrium fluoride 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 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 two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping of blue emission, have not yet to see report.
Summary of the invention
Based on this, be necessary to provide a kind of holmium that can inspire blue light by long-wave radiation to adulterate two alkaline earth yttrium fluoride salt up-conversion luminescent material, preparation method and use this holmium to adulterate the Organic Light Emitting Diode of two alkaline earth yttrium fluoride salt up-conversion luminescent material.
The two alkaline earth yttrium fluoride salt up-conversion luminescent material of a kind of holmium doping, has following chemical formula A mb 1-my 2f 8: xHo 3+, wherein, to be 0.1 ~ 0.9, A be in magnesium, calcium, strontium and barium element one that x is 0.01 ~ 0.08, m, B is the one in magnesium, calcium, strontium and barium element.
Described x is 0.05, y is 0.3.
A preparation method for the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping, comprises the following steps:
According to A mb 1-my 2f 8: xHo 3+the stoichiometric ratio of each element takes AO, BO, Y 2o 3and Ho 2o 3powder, wherein, to be 0.1 ~ 0.9, A be in magnesium, calcium, strontium and barium element one that x is 0.01 ~ 0.08, m, B is the one in magnesium, calcium, strontium and barium element;
The powder taken is dissolved in the acid solvent containing fluorine, adds dispersion agent afterwards and basic solvent obtains containing sedimentary mixture simultaneously;
Regulating containing sedimentary mixture ph is 7 ~ 9, then filters, and with dehydrated alcohol and distilled water wash, is precipitated thing; And
Throw out is dried burning at 900 DEG C ~ 1400 DEG C, and drying the burning time is 2 hours ~ 5 hours, and obtaining chemical general formula is A mb 1-my 2f 8: xHo 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
Described x is 0.05, y is 0.3.
Described acid solvent is hydrofluoric acid, Neutral ammonium fluoride or ammonium bifluoride.
Described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
Described basic solvent is ammoniacal liquor.
Described pH value is 5.
Described throw out is transferred in retort furnace to dry at 1200 DEG C and is burnt, and drying the burning time is 2 hours.
A kind of Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the encapsulated layer that stack gradually, doped with the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping in described encapsulated layer, the chemical general formula of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of this holmium doping is A mb 1-my 2f 8: xHo 3+, wherein, to be 0.1 ~ 0.9, A be in magnesium, calcium, strontium and barium element one that x is 0.01 ~ 0.08, m, B is the one in magnesium, calcium, strontium and barium element.
Hydrothermal method mild condition, the synthesis temperature of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of above-mentioned holmium doping 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 two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping of preparation, the excitation wavelength of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping is 640nm, in 490nm wavelength zone by Ho 3+ion 5f 35i 8transition 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 the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping prepared by embodiment 1.
Fig. 3 is the XRD spectra of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping prepared by embodiment 1.
Fig. 4 is the spectrogram doped with the Organic Light Emitting Diode of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping in the transparent encapsulated layer of embodiment 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments, two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping and preparation method thereof is illustrated further.
The two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping of one embodiment, has following chemical general formula A mb 1-my 2f 8: xHo 3+, wherein, to be 0.1 ~ 0.9, A be in magnesium, calcium, strontium and barium element one that x is 0.01 ~ 0.08, m, B is the one in magnesium, calcium, strontium and barium element.
Preferably, x is 0.05, y is 0.3.
Preferably, be identical element when element A is different with B element.
The preparation method of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of above-mentioned holmium doping, comprises the following steps:
Step S11, according to A mb 1-my 2f 8: xHo 3+the stoichiometric ratio of each element takes AO, BO, Y 2o 3and Ho 2o 3powder, wherein, to be 0.1 ~ 0.9, A be in magnesium, calcium, strontium and barium element one that x is 0.01 ~ 0.08, m, B is the one in magnesium, calcium, strontium and barium element.
In this step, preferably, x is 0.05, y is 0.3.
Step S13, the acid solvent that will add in the powder taken in step S11 containing fluorine, add dispersion agent afterwards simultaneously and basic solvent obtains containing sedimentary mixture.
In this step, preferably, described acid solvent comprises hydrochloric acid, sulfuric acid or nitric acid;
In this step, preferably, described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
In this step, preferably, described basic solvent is ammoniacal liquor.
In this step, dispersion agent is that same ammoniacal liquor instills together, and the effect of ammoniacal liquor is neutralization acidity and produces the throw out of oxyhydroxide and oxide compound, and dispersion agent effect prevents the throw out generated from reuniting.
Step S15, adjustment are 7 ~ 9 containing sedimentary mixture ph, then filter, and with dehydrated alcohol and distilled water wash, are precipitated thing.
In this step, preferably, described pH value is 5.
Step S17, throw out is dried burning at 900 DEG C ~ 1300 DEG C, drying the burning time is 2 hours ~ 5 hours, and obtaining chemical general formula is A mb 1-my 2f 8: xHo 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
In this step, preferably, described throw out is transferred in retort furnace to dry at 1200 DEG C and is burnt, and drying the burning time is 3 hours.
Hydrothermal method mild condition, the synthesis temperature of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of above-mentioned holmium doping 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 two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping of preparation, the excitation wavelength of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping is 640nm, in 490nm wavelength zone by Ho 3+ion 5f 35i 8transition 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 encapsulated layer 5 that stack gradually.Be dispersed with the two alkaline earth yttrium fluoride salt up-conversion luminescent material 6 of holmium doping in encapsulated layer 5, the chemical general formula of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping is A mb 1-my 2f 8: xHo 3+, wherein, to be 0.1 ~ 0.9, A be in magnesium, calcium, strontium and barium element one that x is 0.01 ~ 0.08, m, B is the one in magnesium, calcium, strontium and barium element.
Be dispersed with the two alkaline earth yttrium fluoride salt up-conversion luminescent material 6 of holmium doping in the encapsulated layer 5 of Organic Light Emitting Diode 100, the excitation wavelength of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping is 640nm, in 490nm wavelength zone by Ho 3+ion 5f 35i 8transition 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 MgO, CaO, Y 2o 3and Ho 2o 3powder is 0.5mmol, 0.45mmol, 1mmol and 0.05mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid, dropping oxalic acid adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 1000 DEG C, dry burning 2 hours, obtaining chemical general formula is Mg 0.5ca 0.45y 2f 8: 0.05Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
The substrate 1 stacked gradually uses soda-lime glass, negative electrode 2 uses metal A g layer, organic luminous layer 3 uses Ir (piq) 2 (acac) Chinese name (methyl ethyl diketone) closes iridium (III), transparent anode 4 uses tin indium oxide ITO two (1-phenyl-isoquinoline 99.9), and transparent encapsulated layer 5 tetrafluoroethylene.Be dispersed with the two alkaline earth yttrium fluoride salt up-conversion luminescent material 6 of holmium doping in transparent encapsulated layer 5, the chemical formula of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping is Mg 0.5ca 0.45y 2f 8: 0.05Ho 3+.
Refer to Fig. 2, Figure 2 shows that the two alkaline earth yttrium fluoride salt up-conversion luminescent material chemical general formula of holmium doping that this enforcement obtains is Mg 0.5ca 0.45y 2f 8: 0.05Ho 3+photoluminescence spectra figure.As seen from Figure 2, the excitation wavelength of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping obtained for the present embodiment is 640nm, in 490nm wavelength zone by Ho 3+ion 5f 35i 8transition radiation form glow peak, the two alkaline earth yttrium fluoride salt up-conversion luminescent material of this holmium doping can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is the XRD curve of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping prepared by enforcement 1, test comparison standard P DF card.Contrast PDF card, can find out that diffraction peak is depicted as the peak crystallization of two alkaline earth yttrium fluoride salt, not occur the diffraction peak of doped element and other impurity, illustrate that the product that this preparation method obtains has good crystalline quality.
Fig. 4 is the spectrogram doped with the Organic Light Emitting Diode of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping in the transparent encapsulated layer of embodiment 1 preparation, curve 2 is not doped with the contrast of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping, can find out in figure, up-conversion luminescent material can by the red light of long wave, inspire the blue light of shortwave, after blue light mixes with ruddiness, form white light.
Embodiment 2
Select MgO, CaO, Y 2o 3and Ho 2o 3powder is 0.82mmol, 0.1mmol, 1mmol and 0.08mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid, dropping ethanol adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 1300 DEG C, dry burning 2 hours, obtaining chemical general formula is Mg 0.82ca 0.1y 2f 8: 0.08Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
Embodiment 3
Select MgO, SrO, Y 2o 3and Ho 2o 3powder is 0.89mmol, 0.1mmol, 1mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid, dropping trolamine adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 1000 DEG C, dry burning 2 hours, obtaining chemical general formula is Mg 0.89sr 0.1y 2f 8: 0.01Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
Embodiment 4
Select MgO, SrO, Y 2o 3and Ho 2o 3powder is 0.26mmol, 0.7mmol, 1mmol and 0.06mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid, dropping ethanol adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 1000 DEG C, dry burning 2 hours, obtaining chemical general formula is Mg 0.26sr 0.7y 2f 8: 0.06Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
Embodiment 5
Select MgO, BaO, Y 2o 3and Ho 2o 3powder is 0.34mmol, 0.6mmol, 1mmol and 0.06mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid, dropping ethanol adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 900 DEG C, dry burning 3 hours, obtaining chemical general formula is Mg 0.34ba 0.6y 2f 8: 0.06Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
Embodiment 6
Select MgO, BaO, Y 2o 3and Ho 2o 3powder is 0.43mmol, 0.5mmol, 1mmol and 0.07mmol mixing by each component mole number.Be dissolved in after mixing in Neutral ammonium fluoride, dropping ethanol adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 1300 DEG C, dry burning 4 hours, obtaining chemical general formula is Mg 0.43ba 0.5y 2f 8: 0.07Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
Embodiment 7
Select CaO, SrO, Y 2o 3and Ho 2o 3powder is 0.55mmol, 0.4mmol, 1mmol and 0.05mmol mixing by each component mole number.Be dissolved in after mixing in ammonium bifluoride, dropping oxalic acid adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 1000 DEG C, dry burning 2 hours, obtaining chemical general formula is Ca 0.55sr 0.4y 2f 8: 0.05Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
Embodiment 8
Select CaO, SrO, Y 2o 3and Ho 2o 3powder is 0.76mmol, 0.2mmol, 1mmol, 0.04mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid, dropping ethanol adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 900 DEG C, dry burning 2 hours, obtaining chemical general formula is Ca 0.76sr 0.2y 2f 8: 0.04Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
Embodiment 9
Select SrO, BaO, Y 2o 3and Ho 2o 3powder is 0.9mmol, 0.09mmol, 1mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid, dropping trolamine adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 1300 DEG C, dry burning 2 hours, obtaining chemical general formula is Sr 0.9ba 0.09y 2f 8: 0.01Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
Embodiment 10
Select SrO, BaO, Y 2o 3and Ho 2o 3powder is 0.1mmol, 0.82mmol, 1mmol and 0.08mmol mixing by each component mole number.Be dissolved in after mixing in hydrofluoric acid, dropping trolamine adds ammoniacal liquor as dispersion agent simultaneously makes mixing solutions not regeneration precipitation, continue to drip ammoniacal liquor, the pH value regulating mixing solutions is about 8, leave standstill and within 2 hours, make precipitation complete, adopt filter cone for filtration collecting precipitation thing, then throw out dehydrated alcohol and distilled water repetitive scrubbing, finally placed in retort furnace by the throw out of collection and at 1000 DEG C, dry burning 2 hours, obtaining chemical general formula is Sr 0.82ba 0.1y 2f 8: 0.08Ho 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
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. the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping, is characterized in that: have following chemical general formula A mb 1-my 2f 8: xHo 3+, wherein, to be 0.1 ~ 0.9, A be in magnesium, calcium, strontium and barium element one that x is 0.01 ~ 0.08, m, B is the one in magnesium, calcium, strontium and barium element.
2. the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping according to claim 1, it is characterized in that, described x is 0.05, y is 0.3.
3. a preparation method for the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping, is characterized in that, comprise the following steps:
According to A mb 1-my 2f 8: xHo 3+the stoichiometric ratio of each element takes AO, BO, Y 2o 3and Ho 2o 3powder, wherein, to be 0.1 ~ 0.9, A be in magnesium, calcium, strontium and barium element one that x is 0.01 ~ 0.08, m, B is the one in magnesium, calcium, strontium and barium element;
The powder taken is dissolved in the acid solvent containing fluorine, adds dispersion agent afterwards and basic solvent obtains containing sedimentary mixture simultaneously;
Regulating containing sedimentary mixture ph is 7 ~ 9, then filters, and with dehydrated alcohol and distilled water wash, is precipitated thing; And
Throw out is dried burning at 900 DEG C ~ 1400 DEG C, and drying the burning time is 2 hours ~ 5 hours, and obtaining chemical general formula is A mb 1-my 2f 8: xHo 3+the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping.
4. the preparation method of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping according to claim 3, it is characterized in that, described x is 0.05, y is 0.3.
5. the preparation method of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping according to claim 3, it is characterized in that, described acid solvent is hydrofluoric acid, Neutral ammonium fluoride or ammonium bifluoride.
6. the preparation method of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping according to claim 3, it is characterized in that, described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
7. the preparation method of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping according to claim 3, it is characterized in that, described basic solvent is ammoniacal liquor.
8. the preparation method of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping according to claim 3, it is characterized in that, described pH value is 5.
9. the preparation method of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping according to claim 3, is characterized in that, described throw out is transferred in retort furnace to dry at 1200 DEG C and burnt, and drying the burning time is 2 hours.
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 the two alkaline earth yttrium fluoride salt up-conversion luminescent material of holmium doping in described transparent encapsulated layer, the chemical general formula of the two alkaline earth yttrium fluoride salt up-conversion luminescent material of described holmium doping is A mb 1-my 2f 8: xHo 3+, wherein, to be 0.1 ~ 0.9, A be in magnesium, calcium, strontium and barium element one that x is 0.01 ~ 0.08, m, B is the one in magnesium, calcium, strontium and barium element.
CN201310206305.3A 2013-05-29 2013-05-29 Holmium doped double alkaline-earth metal yttrium fluoride up-conversion luminescent material, preparation method, and organic light emitting diode Pending CN104212456A (en)

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Application publication date: 20141217