CN104212454A - Dysprosium doped alkaline-earth metal oxygen yttrium silicate up-conversion luminescent material, preparation method and applications thereof - Google Patents
Dysprosium doped alkaline-earth metal oxygen yttrium silicate up-conversion luminescent material, preparation method and applications thereof Download PDFInfo
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- CN104212454A CN104212454A CN201310207177.4A CN201310207177A CN104212454A CN 104212454 A CN104212454 A CN 104212454A CN 201310207177 A CN201310207177 A CN 201310207177A CN 104212454 A CN104212454 A CN 104212454A
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Abstract
The invention discloses a dysprosium doped alkaline-earth metal oxygen yttrium silicate up-conversion luminescent material, which has a formula of Me2Y8(SiO4)6O2:xDy3+, wherein the x is in a range of 0.01 to 0.08, the Me represents a magnesium element, calcium element, strontium element, or barium element. In the photoluminescence spectrum of the up-conversion luminescent material, the excitation wavelength of the up-conversion luminescent material is 796 nm, the obtained luminescent peak is at 482 nm, the Dy3+ ions jump from the 4F9/2 to 6F15/2, lights are given off during the process, 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
Technical field
The present invention relates to a kind of dysprosium doped alkaline earth silicic acid oxygen yttrium 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 dysprosium doped alkaline earth silicic acid oxygen yttrium 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 inspire the dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material.
A kind of dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material, has following chemical formula Me
2y
8(SiO
4)
6o
2: xDy
3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
X is 0.04.
A preparation method for dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material, comprises the following steps: according to Me
2y
8(SiO
4)
6o
2: xDy
3+the stoichiometric ratio of each element takes MeO, Y
2o
3, SiO and Dy
2o
3powder, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element;
The powder taken is mixed be dissolved in acidic solution 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, 2 hours ~ 10 hours are incubated at 150 DEG C ~ 500 DEG C, be precipitated thing, it is dry after the throw out obtained is adopted washings washing, then by dried throw out 800 DEG C ~ 1000 DEG C calcinations 0.5 hour ~ 5 hours, obtaining chemical general formula is Me
2y
8(SiO
4)
6o
2: xDy
3+dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material.
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 acidic solution is nitric acid, sulfuric acid or hydrochloric acid.
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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of this dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material is Me
2y
8(SiO
4)
6o
2: xDy
3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
Hydrothermal method mild condition, the synthesis temperature of above-mentioned dysprosium doped alkaline earth silicic acid oxygen yttrium salt 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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material of preparation, the excitation wavelength of dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material is 796nm, and the glow peak of the 482nm obtained is Dy
3+ion
4f
9/2→
6f
15/2transition radiation luminous, 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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material prepared by embodiment 1.
Fig. 3 is the Raman spectrum of dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material prepared by embodiment 1.
Fig. 4 is the spectrogram doped with the Organic Light Emitting Diode of dysprosium doped alkaline earth silicic acid oxygen yttrium salt 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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material and preparation method thereof is illustrated further.
The dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material of one embodiment, its chemical formula is Me
2y
8(SiO
4)
6o
2: xDy
3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
Preferably, x is 0.04.
In the photoluminescence spectra of this dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material, the excitation wavelength of dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material is 796nm, and the glow peak of the 482nm obtained is Dy
3+ion
4f
9/2→
6f
15/2transition radiation luminous, can as blue light emitting material.
The preparation method of above-mentioned dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material, comprises the following steps:
Step S11, according to Me
2y
8(SiO
4)
6o
2: xDy
3+the stoichiometric ratio of each element takes MeO, Y
2o
3, SiO and Dy
2o
3powder, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
In this step, preferably, x is 0.04.
In this step, preferably, MeO, Y
2o
3, SiO and Dy
2o
3powder mol ratio is 2:4:6:(0.01 ~ 0.08);
Step S13, the powder taken mixed be dissolved in acidic solution 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 fluorine-containing acidic solution comprises nitric acid, sulfuric acid or hydrochloric acid;
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, it is dry after the throw out obtained is adopted washings washing, then by dried throw out 800 DEG C ~ 1000 DEG C calcinations 0.5 hour ~ 5 hours, obtaining dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material chemical general formula is Me
2y
8(SiO
4)
6o
2: xDy
3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium 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, x is 0.04.
Hydrothermal method mild condition, the synthesis temperature of above-mentioned dysprosium doped alkaline earth silicic acid oxygen yttrium salt 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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material of preparation, the excitation wavelength of dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material is 796nm, and the glow peak of the 482nm obtained is Dy
3+ion
4f
9/2→
6f
15/2transition radiation luminous, 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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material is Me
2y
8(SiO
4)
6o
2: xDy
3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
Be dispersed with dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material 6 in the transparent encapsulated layer 5 of Organic Light Emitting Diode 100, dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material excitation wavelength be 796nm, the glow peak of the 482nm obtained is Dy
3+ion
4f
9/2→
6f
15/2transition radiation luminous, excited can be launched blue light by red-green glow, blue light mixes with red-green glow and forms the Organic Light Emitting Diode emitted white light afterwards.
Be specific embodiment below.
Embodiment 1
Select MgO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.04mmol mixing by each component mole number.Be dissolved in after mixing in salpeter solution 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, dried throw out puts into retort furnace calcination 3 hours under 950 DEG C of conditions, and obtaining chemical general formula is Mg
2y
8(SiO
4)
6o
2: 0.04Dy
3+up-conversion phosphor.
The preparation of Organic Light Emitting Diode stacks gradually, and substrate 1 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 dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material is Mg
2y
8(SiO
4)
6o
2: 0.04Dy
3+.
Refer to Fig. 2, Figure 2 shows that the dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material chemical general formula that this enforcement obtains is Mg
2y
8(SiO
4)
6o
2: 0.04Dy
3+photoluminescence spectra figure.As seen from Figure 2, the excitation wavelength of the dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material obtained for the present embodiment is 796nm, and the glow peak of the 482nm obtained is Dy
3+ion
4f
9/2→
6f
15/2transition radiation luminous, this dysprosium doped alkaline earth silicic acid oxygen yttrium salt 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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material prepared by enforcement 1, Raman peaks in figure is depicted as alkaline earth silicic acid oxygen yttrium salt 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 alkaline earth silicic acid oxygen yttrium salt 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, up-conversion luminescent material by the red light of long wave, can inspire the blue light of shortwave, forms white light after blue light mixes with ruddiness.
Embodiment 2
Select MgO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in salpeter solution 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, dried throw out puts into retort furnace calcination 2 hours under 800 DEG C of conditions, and obtaining chemical general formula is Mg
2y
8(SiO
4)
6o
2: 0.01Dy
3+up-conversion phosphor.
Embodiment 3
Select MgO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.08mmol mixing by each component mole number.Carry out crystallization treatment in vitriolization solution after mixing 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, dried throw out puts into retort furnace calcination 3 hours under 1000 DEG C of conditions, and obtaining chemical general formula is Mg
2y
8(SiO
4)
6o
2: 0.08Dy
3+up-conversion phosphor.
Embodiment 4
Select CaO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.04mmol mixing by each component mole number.Be dissolved in after mixing in salpeter solution 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, dried throw out puts into retort furnace calcination 3 hours under 950 DEG C of conditions, and obtaining chemical general formula is Ca
2y
8(SiO
4)
6o
2: 0.04Dy
3+up-conversion phosphor.
Embodiment 5
Select CaO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in salpeter solution 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, dried throw out puts into retort furnace calcination 2 hours under 800 DEG C of conditions, and obtaining chemical general formula is Ca
2y
8(SiO
4)
6o
2: 0.01Dy
3+up-conversion phosphor.
Embodiment 6
Select CaO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.08mmol mixing by each component mole number.Carry out crystallization treatment in vitriolization solution after mixing 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, dried throw out puts into retort furnace calcination 3 hours under 1000 DEG C of conditions, and obtaining chemical general formula is Ca
2y
8(SiO
4)
6o
2: 0.08Dy
3+up-conversion phosphor.
Embodiment 7
Select SrO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.04mmol mixing by each component mole number.Be dissolved in after mixing in salpeter solution 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, dried throw out puts into retort furnace calcination 3 hours under 950 DEG C of conditions, and obtaining chemical general formula is Sr
2y
8(SiO
4)
6o
2: 0.04Dy
3+up-conversion phosphor.
Embodiment 8
Select SrO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in salpeter solution 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, dried throw out puts into retort furnace calcination 2 hours under 800 DEG C of conditions, and obtaining chemical general formula is Sr
2y
8(SiO
4)
6o
2: 0.01Dy
3+up-conversion phosphor.
Embodiment 9
Select SrO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.08mmol mixing by each component mole number.Carry out crystallization treatment in vitriolization solution after mixing 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, dried throw out puts into retort furnace calcination 3 hours under 1000 DEG C of conditions, and obtaining chemical general formula is Sr
2y
8(SiO
4)
6o
2: 0.08Dy
3+up-conversion phosphor.
Embodiment 10
Select BaO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.04mmol mixing by each component mole number.Be dissolved in after mixing in salpeter solution 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, dried throw out puts into retort furnace calcination 3 hours under 950 DEG C of conditions, and obtaining chemical general formula is Ba
2y
8(SiO
4)
6o
2: 0.04Dy
3+up-conversion phosphor.
Embodiment 11
Select BaO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.01mmol mixing by each component mole number.Be dissolved in after mixing in salpeter solution 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, dried throw out puts into retort furnace calcination 2 hours under 800 DEG C of conditions, and obtaining chemical general formula is Ba
2y
8(SiO
4)
6o
2: 0.01Dy
3+up-conversion phosphor.
Embodiment 12
Select BaO, Y
2o
3, SiO and Dy
2o
3powder is 2mmol, 4mmol, 6mmol and 0.08mmol mixing by each component mole number.Carry out crystallization treatment in vitriolization solution after mixing 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, dried throw out puts into retort furnace calcination 3 hours under 1000 DEG C of conditions, and obtaining chemical general formula is Ba
2y
8(SiO
4)
6o
2: 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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material, is characterized in that: have following chemical general formula Me
2y
8(SiO
4)
6o
2: xDy
3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
2. dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material according to claim 1, it is characterized in that, described x is 0.04.
3. a preparation method for dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material, is characterized in that, comprise the following steps:
According to Me
2y
8(SiO
4)
6o
2: xDy
3+the stoichiometric ratio of each element takes MeO, Y
2o
3, SiO and Dy
2o
3powder, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element;
Being mixed by the powder taken is dissolved in acidic solution, 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
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, it is dry after the throw out obtained is adopted washings washing, then by dried throw out 800 DEG C ~ 1000 DEG C calcinations 0.5 hour ~ 5 hours, obtaining chemical general formula is Me
2y
8(SiO
4)
6o
2: xDy
3+dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material.
4. the preparation method of dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material according to claim 3, it is characterized in that, described x is 0.04.
5. the preparation method of dysprosium doped alkaline earth silicic acid oxygen yttrium salt 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 alkaline earth silicic acid oxygen yttrium salt 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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material according to claim 3, it is characterized in that, described acidic solution is nitric acid, sulfuric acid or hydrochloric acid.
8. the preparation method of dysprosium doped alkaline earth silicic acid oxygen yttrium salt 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 alkaline earth silicic acid oxygen yttrium salt 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 alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material in described transparent encapsulated layer, the chemical general formula of described dysprosium doped alkaline earth silicic acid oxygen yttrium salt up-conversion luminescent material is Me
2y
8(SiO
4)
6o
2: xDy
3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
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| CN107353902A (en) * | 2017-07-31 | 2017-11-17 | 长安大学 | Silicate fluorescent material for LED white lights and preparation method thereof |
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