CN106118648A - A kind of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, preparation method and applications - Google Patents
A kind of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, preparation method and applications Download PDFInfo
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Abstract
A kind of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, its chemical formula is ZrS Ga2S3‑R2S:xPr3+, yYb3+, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01～0.06, and y is 0.01～0.04.In the photoluminescence spectra of this praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, the excitation wavelength of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr3+Ion3P0→3H4Transition radiation formed glow peak, can be as blue light emitting material.The present invention also provides for the preparation method of this praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material and uses the Organic Light Emitting Diode of this praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, preparation method and organic
Optical diode.
Background technology
Organic Light Emitting Diode (OLED) owing to modular construction is simple, production cost is cheap, self-luminous, response time are short,
The characteristic such as flexible, and obtained a very wide range of application.But it is more tired owing to obtaining the OLED blue light material of stability and high efficiency at present
Difficulty, significantly limit white light OLED device and the development of light source industry.
Upconverting fluorescent material can launch visible ray under long wave (as infrared) radiation excitation, even ultraviolet light,
The fields such as optical fiber communication technology, fibre amplifier, 3 D stereo show, biomolecule fluorescence labelling, infrared detective have
It is widely applied prospect.But, can be by infrared, the long-wave radiation such as red-green glow inspires the praseodymium ytterbium codope zirconium gallium sulfur of blue emission
Chalcogenide glasses up-conversion luminescent material, has not yet to see report.
Summary of the invention
Based on this, it is necessary to provide a kind of praseodymium ytterbium codope zirconium gallium chalcogenide glass that can be inspired blue light by long-wave radiation
Up-conversion luminescent material, preparation method and use organic of this praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material
Optical diode.
A kind of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, its chemical formula is ZrS-Ga2S3-R2S:
xPr3+, yYb3+, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, x be 0.01～
0.06, y is 0.01～0.04.
Described x is 0.03, and y is 0.02.
The preparation method of a kind of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, comprises the following steps
Step one, according to ZrS-Ga2S3-R2S:xPr3+, yYb3+The stoichiometric proportion of each element weighs ZrO, Al2O3,
Na2O, Pr2O3And Ho2O3Powder body, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, x
Being 0.01～0.06, y is 0.01～0.04；
Step 2, the powder body mix homogeneously weighed in described step one is obtained presoma；
Step 3, by calcination 0.5 hour～5 hours at 800 DEG C～1100 DEG C of the presoma in described step 2,
Step 4, will in described step 3 process after precursor be cooled to 100 DEG C～300 DEG C, then be incubated 0.5 hour～
3 hours, being cooled to room temperature, obtaining chemical general formula is ZrS-Ga2S3-R2S:xPr3+, yYb3+Praseodymium ytterbium codope zirconium gallium sulfide
Glass up-conversion luminescent material.
Described ZrS, Ga2S3, R2S, Pr2S3And Yb2S3Powder body each component molar ratio (0.57～0.8): (0.12～0.3):
(0.03～0.06): (0.005～0.03): (0.005～0.02).
Described x is 0.03, and y is 0.02.
Described in step 2, mixing is to be ground in corundum alms bowl 20 minutes～60 minutes by described powder body.
By described presoma calcination 3 hours at 950 DEG C in step 3.
Chilling temperature in step 4 is 200 DEG C, and temperature retention time is 2 hours.
A kind of Organic Light Emitting Diode, including the substrate stacked gradually, negative electrode, organic luminous layer, anode and transparent enclosure
Layer, it is characterised in that be dispersed with praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, institute in described transparent encapsulated layer
The chemical formula stating praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material is ZrS-Ga2S3-R2S:xPr3+, yYb3+, its
In, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01～0.06, y be 0.01～
0.04。
X is 0.03, and y is 0.02.
The preparation method of above-mentioned praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material is relatively simple, and cost is relatively
Low, produce without the three wastes during simultaneous reactions, more environmental protection；The praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescence of preparation
In the photoluminescence spectra of material, the excitation wavelength of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material is 578nm,
In 483nm wavelength zone by Pr3+Ion3P0→3H4Transition radiation formed glow peak, can be 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 spectrum of the praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material of embodiment 1 preparation
Figure.
Fig. 3 is the Raman spectrum of the praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material of embodiment 1 preparation.
Fig. 4 is to send out doped with conversion on praseodymium ytterbium codope zirconium gallium chalcogenide glass in transparent encapsulated layer prepared by embodiment 1
Luminescent material material forms the spectrogram of the Organic Light Emitting Diode emitted white light.
Detailed description of the invention
Below in conjunction with the accompanying drawings with specific embodiment to praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material and
Preparation method is further elucidated with.
The praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material of one embodiment, its chemical formula is ZrS-
Ga2S3-R2S:xPr3+, yYb3+, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, x
Being 0.01～0.06, y is 0.01～0.04.
Preferably, x is 0.03, and y is 0.02.
In the photoluminescence spectra of this praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, praseodymium ytterbium codope zirconium
The excitation wavelength of gallium chalcogenide glass up-conversion luminescent material is 578nm, when material is by the radiation of long wavelength (such as 578nm)
Time, Pr3+Ion is at3P0Excited state, then to3H4Transition, is issued by the blue light of 483nm, can be as blue light emitting
Material.
The preparation method of above-mentioned praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, comprises the following steps:
Step S11, according to ZrS-Ga2S3-R2S:xPr3+, yYb3+The stoichiometric proportion of each element weighs ZrO, Al2O3,
Na2O, Pr2O3And Ho2O3Powder body, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, x
Being 0.01～0.06, y is 0.01～0.04.
In this step, described ZrS, Ga2S3, R2S, Pr2S3And Yb2S3Powder body each component molar ratio (0.57～0.8):
(0.12～0.3): (0.03～0.06): (0.005～0.03): (0.005～0.02).
In this step, it is preferred that x is 0.03, y is 0.02.
Step S13, the powder body mix homogeneously weighed in step S11 is obtained presoma.
In this step, presoma powder body being ground 20 minutes in corundum alms bowl～being uniformly mixed for 60 minutes, preferably
Grinding 40 minutes.
Step S15, by presoma calcination 0.5 hour～5 hours at 800 DEG C～1100 DEG C,
Preferably, presoma calcination 3 hours at 950 DEG C.
Step S17, will step S15 process after precursor after be cooled to 100 DEG C～300 DEG C, then be incubated 0.5 hour
～3 hours, it is cooled to room temperature, obtaining chemical general formula is ZrS-Ga2S3-R2S:xPr3+, yYb3+Praseodymium ytterbium codope zirconium gallium sulfuration
Thing glass up-conversion luminescent material, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, x
Being 0.01～0.06, y is 0.01～0.04.
Preferably, the precursor after processing in step S15 is cooled to 200 DEG C, then is incubated 2 hours.
The preparation method of above-mentioned praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material is relatively simple, and cost is relatively
Low, produce without the three wastes during simultaneous reactions, more environmental protection；The praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescence of preparation
In the photoluminescence spectra of material, the excitation wavelength of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material is 578nm,
In 483nm wavelength zone by Pr3+Ion3P0→3H4Transition radiation formed glow peak, can be as blue light emitting material.
Referring to Fig. 1, the Organic Light Emitting Diode 100 of an embodiment, this Organic Light Emitting Diode 100 includes layer successively
Folded substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and transparent encapsulated layer 5.Transparent encapsulated layer 5 is dispersed with praseodymium ytterbium
Codope zirconium gallium chalcogenide glass up-conversion luminescent material 6, praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material
Chemical formula is ZrS-Ga2S3-R2S:xPr3+, yYb3+, wherein, R is elemental lithium, sodium element, potassium element, and rubidium element, in cesium element
At least one, x is 0.01～0.06, and y is 0.01～0.04, and the organic luminous layer 3 in this device sends red-green glow, and part is red
Green glow excites and is dispersed with praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material 6 in transparent encapsulated layer 5 and sends blue light,
Last redgreenblue just blendes together white light.
It is specific embodiment below.
Embodiment 1
Selecting purity is the powder body of 99.99%, by ZrS, Ga2S3, Li2S, Pr2S3And Yb2S3The each component of powder body is in molar ratio
Grinding 40 minutes in corundum mortar for 0.2:0.05:0.015:0.01 makes it uniformly mix, then in Muffle furnace at 950 DEG C
Calcination 3 hours, is then cooled to 200 DEG C and is incubated 2 hours, then furnace cooling takes out to room temperature, obtains block materials, can after pulverizing
Obtaining chemical general formula is 0.7ZrS-0.2Ga2S3-0.05Li2S:0.03Pr3+, 0.02Yb3+Up-conversion phosphor.
Process prepared by Organic Light Emitting Diode
The substrate 1 stacked gradually uses soda-lime glass, negative electrode 2 to use metal Ag layer, organic luminous layer 3 to use Ir (piq) 2
(acac) Chinese name closes iridium (III) two (1-phenyl-isoquinolin) (acetylacetone,2,4-pentanedione), transparent anode 4 uses tin indium oxide ITO,
And transparent encapsulated layer 5 politef.Transparent encapsulated layer 5 is dispersed with on praseodymium ytterbium codope zirconium gallium chalcogenide glass conversion send out
Luminescent material 6, the chemical formula of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material is 0.7ZrS-0.2Ga2S3-
0.05Li2S:0.03Pr3+, 0.02Yb3+。
Refer to Fig. 2, Fig. 2 and show the photic of the praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material that obtains
Luminescent spectrum figure.As seen from Figure 2, the praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material that the present embodiment obtains
Excitation wavelength be 578nm, in 483nm wavelength zone by Pr3+Ion3P0→3H4Transition radiation form glow peak, this praseodymium ytterbium is altogether
Doping zirconium gallium chalcogenide glass up-conversion luminescent material can be as blue light emitting material.
Referring to Fig. 3, in Fig. 3, curve is the praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescence material implementing 1 preparation
The Raman spectrum of material, Raman spectrum as seen from the figure, Raman peaks show zirconium aluminum oxide characteristic peak as seen from the figure,
The peak of doped chemical and other impurity does not occur, illustrates that doped chemical defines good being bonded with host material.
Referring to Fig. 4, Fig. 4 curve 1 is to change doped with on praseodymium ytterbium codope zirconium gallium chalcogenide glass in transparent encapsulated layer
Luminescent material material forms the spectrogram of the Organic Light Emitting Diode emitted white light, and curve 2 has praseodymium ytterbium for undoped p in transparent encapsulated layer
The contrast of codope zirconium gallium chalcogenide glass up-conversion luminescent material material.Figure can be seen that, figure 4, it can be seen that praseodymium ytterbium is co-doped with
Miscellaneous zirconium gallium chalcogenide glass up-conversion luminescent material can be inspired the blue light of shortwave by the red light of long wave, and blue light is with red
White light is formed after light mixing.
Embodiment 2
Selecting purity is the powder body of 99.99%, by ZrS, Ga2S3, Li2S, Pr2S3And Yb2S3The each component of powder body is in molar ratio
For 0.8:0.12:0.06:0.005:0.005, grind in corundum mortar and make it uniformly mix, then in Muffle furnace in 20 minutes
Calcination 3 hours at 800 DEG C, are then cooled to 250 DEG C and are incubated 0.5 hour, then furnace cooling takes out to room temperature, obtains block material
Material, after pulverizing, available chemical general formula is 0.8ZrS-0.12Ga2S3-0.06Li2S:0.01Pr3Up-conversion phosphor.
Embodiment 3
Selecting purity is the powder body of 99.99%, by ZrS, Ga2S3, Li2S, Pr2S3And Yb2S3The each component of powder body is in molar ratio
For 0.57:0.3:0.03:0.03:0.02, grind in corundum mortar and make it uniformly mix, then in Muffle furnace in 60 minutes
Calcination 3 hours at 1000 DEG C, are then cooled to 250 DEG C and are incubated 2 hours, then furnace cooling takes out to room temperature, obtains block materials,
After pulverizing, available chemical general formula is 0.57ZrS-0.3Ga2S3-0.03Li2S:0.06Pr3+, 0.04Yb3+Up-conversion phosphor.
Embodiment 4
Selecting purity is the powder body of 99.99%, by ZrS, Ga2S3, Na2S, Pr2S3And Yb2S3The each component of powder body is in molar ratio
For 0.2:0.05:0.015:0.01, grind in corundum mortar and make it uniformly mix in 30 minutes, then in Muffle furnace 900 DEG C
Lower calcination 3 hours, is then cooled to 300 DEG C and is incubated 0.5 hour, then furnace cooling takes out to room temperature, obtains block materials, pulverizes
Rear available chemical general formula is 0.7ZrS-0.2Ga2S3-0.05Na2S:0.03Pr3+, 0.02Yb3+Up-conversion phosphor.
Embodiment 5
Selecting purity is the powder body of 99.99%, by ZrS, Ga2S3, Na2S, Pr2S3And Yb2S3The each component of powder body is in molar ratio
For 0.8:0.12:0.06:0.005:0.005, grind in corundum mortar and make it uniformly mix, then in Muffle furnace in 60 minutes
Calcination 2 hours at 850 DEG C, are then cooled to 300 DEG C and are incubated 0.5 hour, then furnace cooling takes out to room temperature, obtains block material
Material, after pulverizing, available chemical general formula is 0.8ZrS-0.12Ga2S3-0.06Na2S:0.01Pr3+, 0.01Yb3+Upper conversion glimmering
Light powder.
Embodiment 6
Selecting purity is the powder body of 99.99%, by ZrS, Ga2S3, Na2S, Pr2S3And Yb2S3The each component of powder body is in molar ratio
For 0.57:0.3:0.03:0.03:0.02, grind in corundum mortar and make it uniformly mix, then in Muffle furnace in 60 minutes
Calcination 2 hours at 850 DEG C, are then cooled to 300 DEG C and are incubated 0.5 hour, then furnace cooling takes out to room temperature, obtains block material
Material, after pulverizing, available chemical general formula is 0.57ZrS-0.3Ga2S3-0.03Na2S:0.06Pr3+, 0.04Yb3+Upper conversion glimmering
Light powder.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, it is characterised in that: its chemical general formula is ZrS-
Ga2S3-R2S:xPr3+, yYb3+, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, x
Being 0.01～0.06, y is 0.01～0.04.
Praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material the most according to claim 1, it is characterised in that institute
Stating x is 0.03, and y is 0.02.
3. the preparation method of a praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material, it is characterised in that include with
Lower step:
Step one, according to ZrS-Ga2S3-R2S:xPr3+, yYb3+The stoichiometric proportion of each element weighs ZrS, Ga2S3, R2S, Pr2S3
And Yb2S3Powder body, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, x be 0.01～
0.06, y is 0.01～0.04；
Step 2, the powder body mix homogeneously weighed in described step one is obtained presoma；
Step 3, by described presoma calcination 0.5 hour～5 hours at 800 DEG C～1100 DEG C,
Step 4, will described step 3 process after precursor be cooled to 100 DEG C～300 DEG C, then be incubated 0.5 hour～3 little
Time, it is cooled to room temperature, obtaining chemical general formula is ZrS-Ga2S3-R2S:xPr3+, yYb3+Praseodymium ytterbium codope zirconium gallium chalcogenide glass
Up-conversion luminescent material.
The preparation method of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material the most according to claim 3, its
It is characterised by, described ZrS, Ga2S3, R2S, Pr2S3And Yb2S3The each component molar of powder body is than for (0.57～0.8): (0.12～
0.3): (0.03～0.06): (0.005～0.03): (0.005～0.02).
The preparation method of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material the most according to claim 3, its
Being characterised by, described x is 0.03, and y is 0.02.
The preparation method of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material the most according to claim 3, its
Being characterised by, described in step 2, mixing is to be ground in corundum alms bowl 20 minutes～60 minutes by described powder body.
The preparation method of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material the most according to claim 3, its
It is characterised by, by described presoma calcination 3 hours at 950 DEG C in step 3.
The preparation method of praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material the most according to claim 3, its
Being characterised by, the chilling temperature in step 4 is 200 DEG C, and temperature retention time is 2 hours.
9. an Organic Light Emitting Diode, substrate that this Organic Light Emitting Diode includes stacking gradually, negative electrode, organic luminous layer,
Anode and transparent encapsulated layer, it is characterised in that be dispersed with in described transparent encapsulated layer on praseodymium ytterbium codope zirconium gallium chalcogenide glass
Changing luminous material, the chemical formula of described praseodymium ytterbium codope zirconium gallium chalcogenide glass up-conversion luminescent material is ZrS-Ga2S3-
R2S:xPr3+, yYb3+, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01
～0.06, y is 0.01～0.04.
Organic Light Emitting Diode the most according to claim 9, it is characterised in that described x is 0.03, y is 0.02.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104342153A (en) * | 2013-08-05 | 2015-02-11 | 海洋王照明科技股份有限公司 | Dysprosium and ytterbium co-doped alkali yttrium fluoride glass up-conversion luminescent material, and preparation method and application thereof |
| CN104927852A (en) * | 2014-03-21 | 2015-09-23 | 海洋王照明科技股份有限公司 | Upconversion fluorescent powder on zirconium-gallium sulphide basal body and preparation method of upconversion fluorescent powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104342153A (en) * | 2013-08-05 | 2015-02-11 | 海洋王照明科技股份有限公司 | Dysprosium and ytterbium co-doped alkali yttrium fluoride glass up-conversion luminescent material, and preparation method and application thereof |
| CN104927852A (en) * | 2014-03-21 | 2015-09-23 | 海洋王照明科技股份有限公司 | Upconversion fluorescent powder on zirconium-gallium sulphide basal body and preparation method of upconversion fluorescent powder |
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