CN104119893A - Praseodymium holmium co-doped niobate up-conversion luminescent material, preparation method and organic light-emitting diodes - Google Patents
Praseodymium holmium co-doped niobate up-conversion luminescent material, preparation method and organic light-emitting diodes Download PDFInfo
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- CN104119893A CN104119893A CN201310150019.XA CN201310150019A CN104119893A CN 104119893 A CN104119893 A CN 104119893A CN 201310150019 A CN201310150019 A CN 201310150019A CN 104119893 A CN104119893 A CN 104119893A
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Abstract
A praseodymium holmium co-doped niobate up-conversion luminescent material has the following chemical general formula of MeNbO3:xPr<3+>, yHo<3+>, wherein x is 0.01-0.08, y is 0.01-0.06, and Me is one of lithium, sodium, potassium, rubidium and cesium elements. In a photoluminescence spectrum of the praseodymium holmium co-doped niobate up-conversion luminescent material, the excitation wavelength of the praseodymium holmium co-doped niobate up-conversion luminescent material is 578 nm, in a wavelength region of 483 nm, luminescence peaks can be produced by transition radiation from <3>P0 to <3>H4 of Pr<3+> ions, and the praseodymium holmium co-doped niobate up-conversion luminescent material can be used as a blue light luminescent material. The invention also provides a preparation method of the praseodymium holmium co-doped niobate up-conversion luminescent material, and organic light-emitting diodes using the praseodymium holmium co-doped niobate up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of praseodymium holmium codoped niobate 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, apply widely and obtained the utmost point.But owing to obtaining at present, the OLED blue light material of stability and high efficiency is more difficult, has 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, is with a wide range of applications in fields such as optical fiber communication technology, fibre amplifier, 3 D stereo demonstration, biomolecules fluorescence labelling, infrared detectives.But, can be by infrared, the long-wave radiations such as red-green glow inspire the praseodymium holmium codoped niobate up-conversion luminescent material of blue emission, have not yet to see report.
Summary of the invention
Based on this, being necessary to provide a kind of can be inspired praseodymium holmium codoped niobate up-conversion luminescent material, the preparation method of blue light and be used the Organic Light Emitting Diode of this praseodymium holmium codoped niobate up-conversion luminescent material by long-wave radiation.
A kind of praseodymium holmium codoped niobate up-conversion luminescent material, has following chemical formula MeNbO
3: xPr
3+, yHo
3+, wherein, x is that 0.01～0.08, y is that 0.01～0.06, Me is the one in elemental lithium, sodium element, potassium element, rubidium element and cesium element.
X is that 0.04, y is 0.03.
A preparation method for praseodymium holmium codoped niobate up-conversion luminescent material, comprises the following steps:
According to MeNbO
3: xPr
3+, yHo
3+the stoichiometric ratio of each element takes Me
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder, wherein, x is that 0.01～0.08, y is that 0.01～0.06, Me is the one in elemental lithium, sodium element, potassium element, rubidium element and cesium element;
The powder taking is dissolved in to acid solvent, adds afterwards dispersion agent and basic solvent to obtain containing sedimentary mixture simultaneously;
It is 7～9 that adjusting contains sedimentary mixture pH value, then filters, and with dehydrated alcohol and distilled water wash, is precipitated thing; And
Throw out is dried at 900 DEG C～1400 DEG C to burning, drying the burning time is 2 hours～5 hours, and obtaining chemical general formula is MeNbO
3: xPr
3+, yHo
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Described x is that 0.04, y is 0.03.
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 8.
Described throw out is transferred in retort furnace and is dried and burn at 1200 DEG C, and drying the burning time is 3 hours.
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 praseodymium holmium codoped niobate up-conversion luminescent material, the chemical general formula of this praseodymium holmium codoped niobate up-conversion luminescent material is MeNbO
3: xPr
3+, yHo
3+, wherein, x is that 0.01～0.08, y is that 0.01～0.06, Me is the one in elemental lithium, sodium element, potassium element, rubidium element and cesium element.
Hydrothermal method mild condition, the synthesis temperature of above-mentioned praseodymium holmium codoped niobate 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 simultaneous reactions process without the three wastes; In the photoluminescence spectra of praseodymium holmium codoped niobate up-conversion luminescent material of preparation, the excitation wavelength of praseodymium holmium codoped niobate up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation form glow peak, can be used as blue light emitting material.
Brief description of the drawings
Fig. 1 is the structural representation of the Organic Light Emitting Diode of an embodiment.
Fig. 2 is the photoluminescence spectrogram of the praseodymium holmium codoped niobate up-conversion luminescent material prepared of embodiment 1.
Fig. 3 is the XRD spectra of the praseodymium holmium codoped niobate up-conversion luminescent material prepared of embodiment 1.
Fig. 4 is the spectrogram doped with the Organic Light Emitting Diode of praseodymium holmium codoped niobate up-conversion luminescent material in the transparent encapsulated layer prepared of embodiment 1.
Embodiment
Below in conjunction with the drawings and specific embodiments, praseodymium holmium codoped niobate up-conversion luminescent material and preparation method thereof is further illustrated.
The praseodymium holmium codoped niobate up-conversion luminescent material of one embodiment, has following chemical general formula MeNbO
3: xPr
3+, yHo
3+, wherein, x is that 0.01～0.08, y is that 0.01～0.06, Me is the one in elemental lithium, sodium element, potassium element, rubidium element and cesium element.
Preferably, x is that 0.04, y is 0.03.
In the photoluminescence spectra of this praseodymium holmium codoped niobate up-conversion luminescent material, the excitation wavelength of praseodymium holmium codoped niobate up-conversion luminescent material is 578nm, in the time that material is subject to long wavelength's (as 578nm) radiation, and Pr
3+ion excitation arrives
3p
0excited state, then to
3h
4energy state transition, sends the blue light of 483nm, can be used as blue light emitting material.
The preparation method of above-mentioned praseodymium holmium codoped niobate up-conversion luminescent material, comprises the following steps:
Step S11, according to MeNbO
3: xPr
3+, yHo
3+the stoichiometric ratio of each element takes Me
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder, wherein, x is that 0.01～0.08, y is that 0.01～0.06, Me is the one in elemental lithium, sodium element, potassium element, rubidium element and cesium element.
In this step, preferred, x is that 0.04, y is 0.03.
Step S13, will in the powder taking in step S11, add acid solvent, add afterwards dispersion agent and basic solvent to obtain containing sedimentary mixture simultaneously.
In this step, preferred, described acid solvent is hydrofluoric acid, Neutral ammonium fluoride or ammonium bifluoride.
In this step, preferred, described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
In this step, preferred, described basic solvent is ammoniacal liquor.
In this step, dispersion agent is that same ammoniacal liquor splashes into together, and the effect of ammoniacal liquor is neutralization acidity the throw out that produces oxyhydroxide and oxide compound, and dispersion agent effect is that the throw out that prevents generation is reunited.
It is 7～9 that step S15, adjusting contain sedimentary mixture pH value, then filters, and with dehydrated alcohol and distilled water wash, is precipitated thing.
In this step, preferred, described pH value is 8.
Step S17, throw out is dried at 900 DEG C～1300 DEG C to burning, drying the burning time is 2 hours～5 hours, and obtaining chemical general formula is MeNbO
3: xPr
3+, yHo
3+praseodymium holmium codoped niobate up-conversion luminescent material.
In this step, preferred, described throw out is transferred in retort furnace and is dried and burn at 1200 DEG C, and drying the burning time is 3 hours.
Hydrothermal method mild condition, the synthesis temperature of above-mentioned praseodymium holmium codoped niobate 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 simultaneous reactions process without the three wastes; In the photoluminescence spectra of praseodymium holmium codoped niobate up-conversion luminescent material of preparation, the excitation wavelength of praseodymium holmium codoped niobate up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation form glow peak, can be used as blue light emitting material.
Refer to Fig. 1, the Organic Light Emitting Diode 100 of an embodiment, this Organic Light Emitting Diode 100 comprises the substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the encapsulated layer 5 that stack gradually.In encapsulated layer 5, be dispersed with praseodymium holmium codoped niobate up-conversion luminescent material 6, the chemical general formula of praseodymium holmium codoped niobate up-conversion luminescent material is MeNbO
3: xPr
3+, yHo
3+, wherein, x is that 0.01～0.08, y is that 0.01～0.06, Me is the one in elemental lithium, sodium element, potassium element, rubidium element and cesium element.
In the encapsulated layer 5 of Organic Light Emitting Diode 100, be dispersed with praseodymium holmium codoped niobate up-conversion luminescent material 6, the excitation wavelength of praseodymium holmium codoped niobate up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation form glow peak, excite and can launch blue light by red-green glow, blue light mixes the Organic Light Emitting Diode that afterwards formation emits white light with red-green glow.
Be specific embodiment below.
Embodiment 1
Select Li
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.04mmol and 0.03mmol mix.In acid-soluble dose of the rear dissolved salt of mixing, drip oxalic acid adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 1000 DEG C, obtaining chemical general formula is LiNbO
3: 0.04Pr
3+, 0.03Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
The substrate 1 stacking gradually use soda-lime glass, negative electrode 2 use metal A g layer, organic luminous layer 3 use Ir (piq) 2 (acac) Chinese name two (1-phenyl-isoquinoline 99.9) (methyl ethyl diketones) close iridium (III), transparent anode 4 uses tin indium oxide ITO, and transparent encapsulated layer 5 tetrafluoroethylene.In transparent encapsulated layer 5, be dispersed with praseodymium holmium codoped niobate up-conversion luminescent material 6, the chemical formula of praseodymium holmium codoped niobate up-conversion luminescent material is LiNbO
3: 0.04Pr
3+, 0.03Ho
3+.
Refer to Fig. 2, Figure 2 shows that the praseodymium holmium codoped niobate up-conversion luminescent material chemical general formula that this enforcement obtains is LiNbO
3: 0.04Pr
3+, 0.03Ho
3+photoluminescence spectra figure.As seen from Figure 2, the excitation wavelength of the praseodymium holmium codoped niobate up-conversion luminescent material that the present embodiment obtains is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation form glow peak, this praseodymium holmium codoped niobate up-conversion luminescent material can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is the XRD curve of implementing the praseodymium holmium codoped niobate up-conversion luminescent material of 1 preparation, test comparison standard P DF card.Contrast PDF card, can see that the diffraction peak in publishing picture is the peak crystallization of niobate, does 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 praseodymium holmium codoped niobate up-conversion luminescent material in the transparent encapsulated layer prepared of embodiment 1, curve 1 is the spectrogram of the praseodymium holmium codoped niobate up-conversion luminescent material prepared of the embodiment of the present invention, curve 2 is the not contrast doped with praseodymium holmium codoped niobate up-conversion luminescent material, in figure, can find out, fluorescent material can be by the red light of long wave, the blue light that inspires shortwave, blendes together white light.
Embodiment 2
Select Li
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.01mmol and 0.01mmol mix.In acid-soluble dose of the rear dissolved salt of mixing, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 900 DEG C, obtaining chemical general formula is LiNbO
3: 0.01Pr
3+, 0.01Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 3
Select Li
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.08mmol and 0.06mmol mix.Mix in rear vitriolization solvent, drip trolamine adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 1300 DEG C, obtaining chemical general formula is LiNbO
3: 0.08Pr
3+, 0.06Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 4
Select Na
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.04mmol and 0.03mmol mix.Mix in rear vitriolization, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2.5 hours at 1100 DEG C, obtaining chemical general formula is NaNbO
3: 0.04Pr
3+, 0.03Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 5
Select Na
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.01mmol and 0.01mmol mix.Mix in rear vitriolization, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 3 hours at 1000 DEG C, obtaining chemical general formula is NaNbO
3: 0.01Pr
3+, 0.01Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 6
Select Na
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.08mmol and 0.06mmol mix.Mix in rear vitriolization, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 4 hours at 950 DEG C, obtaining chemical general formula is NaNbO
3: 0.08Pr
3+, 0.06Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 7
Select K
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.04mmol and 0.03mmol mix.After mixing, be dissolved in hydrochloric acid solvent, drip oxalic acid adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 1000 DEG C, obtaining chemical general formula is KNbO
3: 0.04Pr
3+, 0.03Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 8
Select K
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.01mmol and 0.01mmol mix.Mix in rear vitriolization, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 3 hours at 1000 DEG C, obtaining chemical general formula is KNbO
3: 0.01Pr
3+, 0.01Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 9
Select K
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.08mmol and 0.06mmol mix.Mix in rear vitriolization, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 4 hours at 950 DEG C, obtaining chemical general formula is KNbO
3: 0.08Pr
3+, 0.06Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 10
Select Rb
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.04mmol and 0.03mmol mix.After mixing, be dissolved in hydrochloric acid solvent, drip oxalic acid adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 1000 DEG C, obtaining chemical general formula is RbNbO
3: 0.04Pr
3+, 0.03Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 11
Select Rb
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.01mmol and 0.01mmol mix.After mixing, be dissolved in hydrochloric acid, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 3 hours at 1000 DEG C, obtaining chemical general formula is RbNbO
3: 0.01Pr
3+, 0.01Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 12
Select Rb
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.08mmol and 0.06mmol mix.Mix in rear vitriolization, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 4 hours at 950 DEG C, obtaining chemical general formula is RbNbO
3: 0.08Pr
3+, 0.06Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 13
Select Cs
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.04mmol and 0.03mmol mix.After mixing, be dissolved in hydrochloric acid solvent, drip oxalic acid adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 1000 DEG C, obtaining chemical general formula is CsNbO
3: 0.04Pr
3+, 0.03Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 14
Select Cs
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.01mmol and 0.01mmol mix.After mixing, be dissolved in hydrofluoric acid, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 3 hours at 1000 DEG C, obtaining chemical general formula is CsNbO
3: 0.01Pr
3+, 0.01Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
Embodiment 15
Select Cs
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder is 1mmol by each component mole number, 1mmol, and 0.08mmol and 0.06mmol mix.Mix in rear vitriolization, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 4 hours at 950 DEG C, obtaining chemical general formula is CsNbO
3: 0.08Pr
3+, 0.06Ho
3+praseodymium holmium codoped niobate up-conversion luminescent material.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a praseodymium holmium codoped niobate up-conversion luminescent material, is characterized in that: have following chemical general formula MeNbO
3: xPr
3+, yHo
3+, wherein, x is that 0.01～0.08, y is that 0.01～0.06, Me is the one in elemental lithium, sodium element, potassium element, rubidium element and cesium element.
2. praseodymium holmium codoped niobate up-conversion luminescent material according to claim 1, is characterized in that, described x is that 0.04, y is 0.03.
3. a preparation method for praseodymium holmium codoped niobate up-conversion luminescent material, is characterized in that, comprises the following steps:
According to MeNbO
3: xPr
3+, yHo
3+the stoichiometric ratio of each element takes Me
2o, Nb
2o
5, Pr
2o
3and Ho
2o
3powder, wherein, x is that 0.01～0.08, y is that 0.01～0.06, Me is the one in elemental lithium, sodium element, potassium element, rubidium element and cesium element;
The powder taking is dissolved in to acid solvent, adds afterwards dispersion agent and basic solvent to obtain containing sedimentary mixture simultaneously;
It is 7～9 that adjusting contains sedimentary mixture pH value, then filters, and with dehydrated alcohol and distilled water wash, is precipitated thing; And
Throw out is dried at 900 DEG C～1400 DEG C to burning, drying the burning time is 2 hours～5 hours, and obtaining chemical general formula is MeNbO
3: xPr
3+, yHo
3+praseodymium holmium codoped niobate up-conversion luminescent material.
4. the preparation method of praseodymium holmium codoped niobate up-conversion luminescent material according to claim 3, is characterized in that, described x is that 0.04, y is 0.03.
5. the preparation method of praseodymium holmium codoped niobate up-conversion luminescent material according to claim 3, is characterized in that, described acid solvent is hydrofluoric acid, Neutral ammonium fluoride or ammonium bifluoride.
6. the preparation method of praseodymium holmium codoped niobate up-conversion luminescent material according to claim 3, is characterized in that, described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
7. the preparation method of praseodymium holmium codoped niobate up-conversion luminescent material according to claim 3, is characterized in that, described basic solvent is ammoniacal liquor.
8. the preparation method of praseodymium holmium codoped niobate up-conversion luminescent material according to claim 3, is characterized in that, described pH value is 8.
9. the preparation method of praseodymium holmium codoped niobate up-conversion luminescent material according to claim 3, is characterized in that, described throw out is transferred in retort furnace and dried and burn at 1200 DEG C, and drying the burning time is 3 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, in described transparent encapsulated layer, doped with praseodymium holmium codoped niobate up-conversion luminescent material, the chemical general formula of described praseodymium holmium codoped niobate up-conversion luminescent material is MeNbO
3: xPr
3+, yHo
3+, wherein, x is that 0.01～0.08, y is that 0.01～0.06, Me is the one in elemental lithium, sodium element, potassium element, rubidium element and cesium element.
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| CN109233829A (en) * | 2018-09-14 | 2019-01-18 | 广东工业大学 | A kind of magnesium erbium ytterbium three mixes sodium niobate and its preparation method and application |
| CN111484844A (en) * | 2020-05-18 | 2020-08-04 | 广东拾传拾美新材料有限公司 | Calcium carbonate-calcium silicate up-conversion fluorescent powder and preparation method thereof |
| CN113355094A (en) * | 2021-05-17 | 2021-09-07 | 武汉大学 | Heterostructure material capable of realizing repetitive stress luminescence and preparation method thereof |
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| CN111484844A (en) * | 2020-05-18 | 2020-08-04 | 广东拾传拾美新材料有限公司 | Calcium carbonate-calcium silicate up-conversion fluorescent powder and preparation method thereof |
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