CN106701081A - Praseodymium-doped sulphur yttrium germanate up-conversion luminescent material, preparation method and application thereof - Google Patents
Praseodymium-doped sulphur yttrium germanate up-conversion luminescent material, preparation method and application thereof Download PDFInfo
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- CN106701081A CN106701081A CN201610415254.9A CN201610415254A CN106701081A CN 106701081 A CN106701081 A CN 106701081A CN 201610415254 A CN201610415254 A CN 201610415254A CN 106701081 A CN106701081 A CN 106701081A
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Abstract
The invention relates to a praseodymium-doped sulphur yttrium germanate up-conversion luminescent material. A chemical formula of the praseodymium-doped sulphur yttrium germanate up-conversion luminescent material is M2Y8(GeO4)6S2:xPr<3+>, wherein M is at least one of magnesium, calcium, strontium and barium, and x is 0.01-0.06. In photoluminescence spectra of the praseodymium-doped sulphur yttrium germanate up-conversion luminescent material, the excitation wavelength of the praseodymium-doped sulphur yttrium germanate up-conversion luminescent material is 578nm, and in a 483nm wavelength region, transition radiation of Pr<3+> from 3P0 to 3H4 forms a luminescent peak, so that the praseodymium-doped sulphur yttrium germanate up-conversion luminescent material can be taken as a blue light luminescent material. The invention also provides a preparation method of the praseodymium-doped sulphur yttrium germanate up-conversion luminescent material and an organic light emitting diode adopting the praseodymium-doped sulphur yttrium germanate up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material, preparation method and Organic Light Emitting Diode.
Background technology
Organic Light Emitting Diode (OLED) is because modular construction is simple, production cost is cheap, self-luminous, reaction time are short,
The characteristic such as flexible, and obtained a very wide range of application.But because the OLED blue light materials for obtaining stability and high efficiency at present are relatively stranded
Difficulty, significantly limit the development of white light OLED device and light source industry.
Upconverting fluorescent material can launch visible ray, or even ultraviolet light under long wave (such as infrared) radiation excitation,
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 is inspired on the praseodymium doped germanic acid sulphur yttrium of blue emission
Changing luminous material, has not yet to see report.
The content of the invention
Based on this, it is necessary to provide a kind of praseodymium doped germanic acid sulphur yttrium up-conversion luminescence that blue light can be inspired by long-wave radiation
Material, preparation method and the Organic Light Emitting Diode using the praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material.
A kind of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material, its chemical formula is M2Y8(GeO4)6S2：xPr3+, wherein, M is
Magnesium elements, calcium constituent, strontium element, at least one in barium element, x is 0.01~0.06.
Wherein in one embodiment, the x is 0.03.
A kind of preparation method of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material, comprises the following steps
Step one, according to M2Y8(GeO4)6S2：xPr3+The stoichiometric proportion of each element weighs MS, Y2O3, GeO2And Pr2O3Powder
Body, its mol ratio is 2：4：6：(0.005~0.06), wherein, M is magnesium elements, calcium constituent, strontium element, in barium element at least
It is a kind of；
Step 2, presoma is obtained by the powder weighed in the step one is well mixed；
Step 3, by the presoma in the step 2 at 800 DEG C~1100 DEG C calcination 0.5 hour~5 hours,
Step 4, the precursor after being processed in the step 3 is cooled to 100 DEG C~300 DEG C, then it is incubated 0.5 hour~
3 hours, room temperature is cooled to, obtains chemical general formula for M2Y8(GeO4)6S2：xPr3+Praseodymium doped germanic acid sulphur yttrium up-conversion luminescence material
Material.
Wherein in one embodiment, the MS, Y2O3, GeO2And Pr2O3Powder, its mol ratio is 2：4：6：(0.005~
0.06)。
Wherein in one embodiment, the x is 0.03.
Wherein in one embodiment, mixing described in step 2 be the powder is ground in corundum alms bowl 20 minutes~
60 minutes.
Wherein in one embodiment, in step 3 by the presoma at 950 DEG C calcination 3 hours.
Wherein in one embodiment, the chilling temperature in step 4 is 200 DEG C, and soaking time is 2 hours.
A kind of Organic Light Emitting Diode, including substrate, negative electrode, organic luminous layer, anode and the transparent enclosure for stacking gradually
Layer, it is characterised in that praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material, the praseodymium doped germanium are dispersed with the transparent encapsulated layer
The chemical formula of sour sulphur yttrium up-conversion luminescent material is M2Y8(GeO4)6S2：xPr3+, wherein, M is magnesium elements, calcium constituent, strontium element,
At least one in barium element, x is 0.01~0.06.
X is 0.03 in one embodiment wherein.
The preparation method of above-mentioned praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material is relatively simple, and cost is relatively low, simultaneous reactions
During three wastes produce, more environmental protection；In the photoluminescence spectra of the praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material of preparation,
The excitation wavelength of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material is 578nm, in 483nm wavelength zones by Pr3+Ion3P0→3H4's
Transition radiation forms glow peak, can be as blue light emitting material.
Brief description of the drawings
Fig. 1 is the structural representation of the Organic Light Emitting Diode of an implementation method.
Fig. 2 is the luminescence generated by light spectrogram of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material prepared by embodiment 1.
Specific embodiment
Praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material and preparation method thereof is entered with specific embodiment below in conjunction with the accompanying drawings
One step is illustrated.
The praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material of one implementation method, its chemical formula is M2Y8(GeO4)6S2：xPr3+,
Wherein, M is magnesium elements, calcium constituent, strontium element, at least one in barium element, and x is 0.01~0.06.
Preferably, x is 0.03.
In the photoluminescence spectra of the praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material, hair is changed on praseodymium doped germanic acid sulphur yttrium
The excitation wavelength of luminescent material is 578nm, when material is subject to the radiation of long wavelength (such as 578nm), Pr3+Ion is at
3P0Excitation state, Ran Houxiang3H4Transition, is issued by the blue light of 483nm, can be as blue light emitting material.
The preparation method of above-mentioned praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material, comprises the following steps：
Step S11, according to M2Y8(GeO4)6S2：xPr3+The stoichiometric proportion of each element weighs MS, Y2O3, GeO2And Pr2O3
Powder, its mol ratio is 2：4：6：(0.005~0.06), wherein, M is magnesium elements, calcium constituent, strontium element, in barium element extremely
Few one kind,
In the step, the MS, Y2O3, GeO2And Pr2O3Powder, its mol ratio is 2：4：6：(0.005~0.06).
In the step, it is preferred that x is 0.03.
Step S13, presoma is obtained by the powder weighed in step S11 is well mixed.
In the step, powder is ground 20 minutes~60 minutes in corundum alms bowl and obtains well mixed presoma, preferably
Grinding 40 minutes.
Step S15, by presoma at 800 DEG C~1100 DEG C calcination 0.5 hour~5 hours,
Preferably, presoma calcination 3 hours at 950 DEG C.
Step S17, will be processed in step S15 after precursor after be cooled to 100 DEG C~300 DEG C, then be incubated 0.5 hour
~3 hours, room temperature is cooled to, obtains chemical general formula for M2Y8(GeO4)6S2：xPr3+Praseodymium doped germanic acid sulphur yttrium up-conversion luminescence
Material, wherein, M is magnesium elements, calcium constituent, strontium element, at least one in barium element, and x is 0.01~0.06.
Preferably, the precursor after being processed in step S15 is cooled to 200 DEG C, then is incubated 2 hours.
The preparation method of above-mentioned praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material is relatively simple, and cost is relatively low, simultaneous reactions
During three wastes produce, more environmental protection；In the photoluminescence spectra of the praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material of preparation,
The excitation wavelength of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material is 578nm, in 483nm wavelength zones by Pr3+Ion3P0→3H4's
Transition radiation forms glow peak, can be as blue light emitting material.
Fig. 1 is referred to, the Organic Light Emitting Diode 100 of an implementation method, the 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.Praseodymium is dispersed with transparent encapsulated layer 5 to mix
Miscellaneous germanic acid sulphur yttrium up-conversion luminescent material 6, the chemical formula of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material is M2Y8(GeO4)6S2：
xPr3+, wherein, M is magnesium elements, calcium constituent, strontium element, at least one in barium element, and x is 0.01~0.06, in the device
Organic luminous layer 3 sends red-green glow, and part red-green glow is dispersed with conversion hair on praseodymium doped germanic acid sulphur yttrium in exciting transparent encapsulated layer 5
Luminescent material 6 sends blue light, and last redgreenblue just blendes together white light.
It is below specific embodiment.
Embodiment 1
From the powder that purity is 99.99%, by MgS, Y2O3, GeO and Pr2O3Powder each component is in molar ratio 2：4：
6：0.04 in corundum mortar grinding make within 40 minutes its uniform mixing, then calcination 3 hours at 950 DEG C in the Muffle furnace, then
It is cooled to 200 DEG C and is incubated 2 hours, then furnace cooling is taken out to room temperature, obtains block materials, chemical general formula is can obtain after crushing is
Mg2Y8(GeO4)6S2：0.08Pr3+Up-conversion phosphor.
Process prepared by Organic Light Emitting Diode
The substrate 1 for stacking gradually uses Ir (piq) 2 using soda-lime glass, negative electrode 2 using Ag layers of metal, organic luminous layer 3
(acac) Chinese name closes iridium (III), transparent anode 4 and uses tin indium oxide ITO two (1- phenyl-isoquinolin) (acetylacetone,2,4-pentanediones),
And the polytetrafluoroethylene (PTFE) of transparent encapsulated layer 5.Thulium doped tellurate glass up-conversion luminescent material 6 is dispersed with transparent encapsulated layer 5,
The chemical formula of thulium doping fluorine silica glass up-conversion luminescent material is Mg2Y8(GeO4)6S2：0.08Pr3+。
Fig. 2 is referred to, Fig. 2 show the photoluminescence spectra of the praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material for obtaining
Figure.As seen from Figure 2, the excitation wavelength of the praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material that the present embodiment is obtained is 578nm,
In 483nm wavelength zones by Pr3+Ion3P0→3H4Transition radiation formed glow peak, the praseodymium doped germanic acid sulphur yttrium up-conversion luminescence
Material can be used as blue light emitting material.
Embodiment 2
From the powder that purity is 99.99%, by MgS, Y2O3, GeO and Pr2O3Powder each component is in molar ratio 2：4：
6：0.025, grinding makes its uniform mixing for 20 minutes in corundum mortar, then calcination 3 hours at 800 DEG C in the Muffle furnace, so
After be cooled to 250 DEG C and be incubated 0.5 hour, then furnace cooling is taken out to room temperature, obtains block materials, chemistry is can obtain after crushing logical
Formula is Mg2Y8(GeO4)6S2：0.05Pr3+Up-conversion phosphor.
Embodiment 3
From the powder that purity is 99.99%, by MgS, Y2O3, GeO and Pr2O3Powder each component is in molar ratio 2：4：
6：0.6, grinding makes its uniform mixing for 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in the Muffle furnace, then
It is cooled to 250 DEG C and is incubated 2 hours, then furnace cooling is taken out to room temperature, obtains block materials, chemical general formula is can obtain after crushing is
Mg2Y8(GeO4)6S2：0.12Pr3+Up-conversion phosphor.
Embodiment 4
From the powder that purity is 99.99%, by CaS, Y2O3, GeO and Pr2O33Powder each component is in molar ratio 2：4：
6：0.04, grinding makes its uniform mixing for 30 minutes in corundum mortar, then calcination 3 hours at 900 DEG C in the Muffle furnace, then
It is cooled to 300 DEG C and is incubated 0.5 hour, then furnace cooling is taken out to room temperature, obtains block materials, and chemical general formula is can obtain after crushing
It is Ca2Y8(GeO4)6S2：0.08Pr3+Up-conversion phosphor.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Shield scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material, it is characterised in that：Its chemical general formula is M2Y8(GeO4)6S2：
xPr3+, wherein, M is magnesium elements, calcium constituent, strontium element, at least one in barium element, and x is 0.01~0.06.
2. praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material according to claim 1, it is characterised in that the x is 0.03.
3. a kind of preparation method of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material, it is characterised in that comprise the following steps：
Step one, according to M2Y8(GeO4)6S2：xPr3+The stoichiometric proportion of each element weighs MS, Y2O3, GeO2And Pr2O3Powder,
Its mol ratio is 2：4：6：(0.005~0.06), wherein, M is magnesium elements, calcium constituent, strontium element, in barium element at least one
Kind, x is 0.01~0.06；
Step 2, presoma is obtained by the powder weighed in the step one is well mixed；
Step 3, by the presoma at 800 DEG C~1100 DEG C calcination 0.5 hour~5 hours,
Step 4, the precursor after being processed in the step 3 is cooled to 100 DEG C~300 DEG C, then to be incubated 0.5 hour~3 small
When, room temperature is cooled to, chemical general formula is obtained for M2Y8(GeO4)6S2：xPr3+Praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material.
4. the preparation method of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material according to claim 3, it is characterised in that institute
State MS, Y2O3, GeO2And Pr2O3Powder, its mol ratio is 2：4：6：(0.005~0.06).
5. the preparation method of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material according to claim 3, it is characterised in that institute
It is 0.03 to state x.
6. the preparation method of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material according to claim 3, it is characterised in that step
Mixing is to grind the powder in corundum alms bowl 20 minutes~60 minutes described in rapid two.
7. the preparation method of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material according to claim 3, it is characterised in that step
In rapid three by the presoma at 950 DEG C calcination 3 hours.
8. the preparation method of praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material according to claim 3, it is characterised in that step
Chilling temperature in rapid four is 200 DEG C, and soaking time is 2 hours.
9. a kind of Organic Light Emitting Diode, substrate that the Organic Light Emitting Diode includes stacking gradually, negative electrode, organic luminous layer,
Anode and transparent encapsulated layer, it is characterised in that praseodymium doped germanic acid sulphur yttrium up-conversion luminescence material is dispersed with the transparent encapsulated layer
Material, the chemical formula of the praseodymium doped germanic acid sulphur yttrium up-conversion luminescent material is M2Y8(GeO4)6S2：xPr3+, wherein, M is magnesium unit
Element, calcium constituent, strontium element, at least one in barium element, x is 0.01~0.06.
10. Organic Light Emitting Diode according to claim 9, it is characterised in that the x is 0.03.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116120934A (en) * | 2023-04-19 | 2023-05-16 | 德州学院 | Blue-red long afterglow luminescent material for promoting plant growth and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116120934A (en) * | 2023-04-19 | 2023-05-16 | 德州学院 | Blue-red long afterglow luminescent material for promoting plant growth and preparation method and application thereof |
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