CN106118647A - A kind of neodymium doping chlorine germanate up-conversion luminescent material, preparation method and applications - Google Patents
A kind of neodymium doping chlorine germanate up-conversion luminescent material, preparation method and applications Download PDFInfo
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- CN106118647A CN106118647A CN201610421226.8A CN201610421226A CN106118647A CN 106118647 A CN106118647 A CN 106118647A CN 201610421226 A CN201610421226 A CN 201610421226A CN 106118647 A CN106118647 A CN 106118647A
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Abstract
A kind of neodymium doping chlorine germanate up-conversion luminescent material, its chemical formula is R2GeCl6: xNd3+, wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01～0.08.In the photoluminescence spectra of this neodymium doping chlorine germanate up-conversion luminescent material, the excitation wavelength of neodymium doping chlorine germanate up-conversion luminescent material is 796nm, in 469nm wavelength zone by Nd3+Ion2P3/2→4I15/2Transition radiation formed glow peak, can be as blue light emitting material.The present invention also provides for the preparation method of this neodymium doping chlorine germanate up-conversion luminescent material and uses the Organic Light Emitting Diode of this neodymium doping chlorine germanate up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of neodymium doping chlorine germanate up-conversion luminescent material, preparation method and Organic Light Emitting 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 on the neodymium doping chlorine germanate of blue emission
Changing luminous material, has not yet to see report.
Summary of the invention
Based on this, it is necessary to provide a kind of neodymium doping chlorine germanate up-conversion luminescence that can be inspired blue light by long-wave radiation
Material, preparation method and use this neodymium doping chlorine germanate up-conversion luminescent material Organic Light Emitting Diode.
A kind of neodymium doping chlorine germanate up-conversion luminescent material, its chemical formula is R2GeCl6: xNd3+, wherein, R is lithium unit
Element, sodium element, potassium element, rubidium element, at least one in cesium element, x is 0.01～0.08.
Described x is 0.05.
The preparation method of a kind of neodymium doping chlorine germanate up-conversion luminescent material, comprises the following steps
Step one, according to R2GeCl6: xNd3+The stoichiometric proportion of each element weighs RCl, GeCl4And NdCl3Powder body, its
In, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01～0.08；
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 R2GeCl6: xNd3+Neodymium doping chlorine germanate up-conversion luminescent material.
Described RCl, GeCl4And NdCl3The each component molar of powder body is than for 2:1:(0.01～0.08).
Described x is 0.05.
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 neodymium doping chlorine germanate up-conversion luminescent material, described neodymium doping chlorine in described transparent encapsulated layer
The chemical formula of germanate up-conversion luminescent material is R2GeCl6: xNd3+, wherein, R is elemental lithium, sodium element, potassium element, rubidium unit
Element, at least one in cesium element, x is 0.01～0.08.
X is 0.05.
The preparation method of above-mentioned neodymium doping chlorine germanate up-conversion luminescent material is relatively simple, and cost is relatively low, simultaneous reactions
During without the three wastes produce, more environmental protection；In the photoluminescence spectra of the neodymium doping chlorine germanate up-conversion luminescent material of preparation,
The excitation wavelength of neodymium doping chlorine germanate up-conversion luminescent material is 796nm, in 469nm wavelength zone by Nd3+Ion 2P3/2→
4I15/2Transition 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 luminescence generated by light spectrogram of the neodymium doping chlorine germanate up-conversion luminescent material of embodiment 1 preparation.
Fig. 3 is the Raman spectrum of the neodymium doping chlorine germanate up-conversion luminescent material of embodiment 1 preparation.
Fig. 4 is doped with neodymium doping chlorine germanate up-conversion luminescent material material shape in transparent encapsulated layer prepared by embodiment 1
Become the spectrogram of the Organic Light Emitting Diode emitted white light.
Detailed description of the invention
With specific embodiment, neodymium doping chlorine germanate up-conversion luminescent material and preparation method thereof is entered below in conjunction with the accompanying drawings
One step illustrates.
The neodymium doping chlorine germanate up-conversion luminescent material of one embodiment, its chemical formula is R2GeCl6: xNd3+, wherein,
R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01～0.08.
Preferably, x is 0.05.
In the photoluminescence spectra of this neodymium doping chlorine germanate up-conversion luminescent material, on neodymium doping chlorine germanate, conversion is sent out
The excitation wavelength of luminescent material is 796nm, when material by the radiation of long wavelength (such as 796nm) when, Nd3+Ion is at
?2P3/2Excited state, then to4I15/2Transition, is issued by the blue light of 469nm, can be as blue light emitting material.
The preparation method of above-mentioned neodymium doping chlorine germanate up-conversion luminescent material, comprises the following steps:
Step S11, according to R2GeCl6: xNd3+The stoichiometric proportion of each element weighs RCl, GeCl4And NdCl3Powder body, its
In, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01～0.08.
In this step, described RCl, GeCl4And NdCl3The each component molar of powder body is than for 2:1:(0.01～0.08).
In this step, it is preferred that x is 0.05.
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 R2GeCl6: xNd3+Neodymium doping chlorine germanate up-conversion luminescent material,
Wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01～0.08.
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 neodymium doping chlorine germanate up-conversion luminescent material is relatively simple, and cost is relatively low, simultaneous reactions
During without the three wastes produce, more environmental protection；In the photoluminescence spectra of the neodymium doping chlorine germanate up-conversion luminescent material of preparation,
The excitation wavelength of neodymium doping chlorine germanate up-conversion luminescent material is 796nm, in 469nm wavelength zone by Nd3+Ion2P3/2→4I15/2Transition 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 neodymium mix
Miscellaneous chlorine germanate up-conversion luminescent material 6, the chemical formula of neodymium doping chlorine germanate up-conversion luminescent material is R2GeCl6: xNd3+,
Wherein, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01～0.08, in this device
Organic luminous layer 3 send red-green glow, part red-green glow excite transparent encapsulated layer 5 is dispersed with neodymium doping chlorine germanate on change
Luminescent material 6 sends blue light, and last redgreenblue just blendes together white light.
It is specific embodiment below.
Embodiment 1
Selecting purity is the powder body of 99.99%, by LiCl, GeCl4And NdCl3The each component of powder body is 2:1 in molar ratio:
0.05 grinds in corundum mortar and makes it uniformly mix in 40 minutes, and then calcination 3 hours at 950 DEG C in Muffle furnace, the coldest
But being incubated 2 hours to 200 DEG C, then furnace cooling takes out to room temperature, obtains block materials, after pulverizing, available chemical general formula is
Li2GeCl6: 0.05Nd3+Up-conversion phosphor.
Process prepared by Organic Light Emitting Diode
The substrate 1 stacked gradually uses sodium calcium, 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 neodymium doping chlorine germanate up-conversion luminescent material 6, neodymium
The chemical formula of doping chlorine germanate up-conversion luminescent material is Li2GeCl6: 0.05Nd3+。
Refer to Fig. 2, Fig. 2 and show the photoluminescence spectra of the neodymium doping chlorine germanate up-conversion luminescent material obtained
Figure.As seen from Figure 2, the excitation wavelength of the neodymium doping chlorine germanate up-conversion luminescent material that the present embodiment obtains is 796nm,
In 469nm wavelength zone by Nd3+Ion2P3/2→4I15/2Transition radiation formed glow peak, this neodymium doping chlorine germanate on conversion send out
Luminescent material can be as blue light emitting material.
Referring to Fig. 3, in Fig. 3, curve is the Raman light of the neodymium doping chlorine germanate up-conversion luminescent material implementing 1 preparation
Spectrum, Raman spectrum as seen from the figure, Raman peaks show zirconium aluminum oxide characteristic peak as seen from the figure, does not occur mixing
Miscellaneous element and the peak of other impurity, illustrate that doped chemical defines good being bonded with host material.
Referring to Fig. 4, Fig. 4 curve 1 is doped with neodymium doping chlorine germanate up-conversion luminescent material material in transparent encapsulated layer
Forming the spectrogram of the Organic Light Emitting Diode emitted white light, curve 2 has neodymium doping chlorine germanate for undoped p in transparent encapsulated layer
The contrast of up-conversion luminescent material material.Figure can be seen that, figure 4, it can be seen that neodymium doping chlorine germanate up-conversion luminescent material
Can be inspired the blue light of shortwave by the red light of long wave, blue light forms white light after mixing with HONGGUANG.
Embodiment 2
Selecting purity is the powder body of 99.99%, by LiCl, GeCl4And NdCl3The each component of powder body is 2:1 in molar ratio:
0.01, grind in corundum mortar and make it uniformly mix in 20 minutes, then calcination 3 hours at 800 DEG C in Muffle furnace, the coldest
But being incubated 0.5 hour to 250 DEG C, then furnace cooling takes out to room temperature, obtains block materials, after pulverizing, available chemical general formula is
Li2GeCl6: 0.01Nd3+Up-conversion phosphor.
Embodiment 3
Selecting purity is the powder body of 99.99%, by LiCl, GeCl4And NdCl3The each component of powder body is 2:1 in molar ratio:
0.08, grind in corundum mortar and make it uniformly mix in 60 minutes, then calcination 3 hours at 1000 DEG C in Muffle furnace, then
Being cooled to 250 DEG C and be incubated 2 hours, then furnace cooling takes out to room temperature, obtains block materials, after pulverizing, available chemical general formula is
Li2GeCl6: 0.08Nd3+Up-conversion phosphor.
Embodiment 4
Selecting purity is the powder body of 99.99%, by NaCl, GeCl4And NdCl3The each component of powder body is 2:1 in molar ratio:
0.05, grind in corundum mortar and make it uniformly mix in 30 minutes, then calcination 3 hours at 900 DEG C in Muffle furnace, the coldest
But being incubated 0.5 hour to 300 DEG C, then furnace cooling takes out to room temperature, obtains block materials, after pulverizing, available chemical general formula is
Na2GeCl6: 0.05Nd3+Up-conversion phosphor.
Embodiment 5
Selecting purity is the powder body of 99.99%, by NaCl, GeCl4And NdCl3The each component of powder body is 2:1 in molar ratio:
0.01, grind in corundum mortar and make it uniformly mix in 60 minutes, then calcination 2 hours at 850 DEG C in Muffle furnace, the coldest
But being incubated 0.5 hour to 300 DEG C, then furnace cooling takes out to room temperature, obtains block materials, after pulverizing, available chemical general formula is
Na2GeCl6: 0.01Nd3+Up-conversion phosphor.
Embodiment 6
Selecting purity is the powder body of 99.99%, by NaCl, GeCl4And NdCl3The each component of powder body is 2:1 in molar ratio:
0.08, grind in corundum mortar and make it uniformly mix in 60 minutes, then calcination 2 hours at 850 DEG C in Muffle furnace, the coldest
But being incubated 0.5 hour to 300 DEG C, then furnace cooling takes out to room temperature, obtains block materials, after pulverizing, available chemical general formula is
Na2GeCl6: 0.08Nd3+Up-conversion phosphor.
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 neodymium doping chlorine germanate up-conversion luminescent material, it is characterised in that: its chemical general formula is R2GeCl6: xNd3+, its
In, R is elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, and x is 0.01～0.08.
Neodymium the most according to claim 1 doping chlorine germanate up-conversion luminescent material, it is characterised in that described x is 0.05.
3. the preparation method of a neodymium doping chlorine germanate up-conversion luminescent material, it is characterised in that comprise the following steps:
Step one, according to R2GeCl6: xNd3+The stoichiometric proportion of each element weighs RCl, GeCl4And NdCl3Powder body, wherein, R is
Elemental lithium, sodium element, potassium element, rubidium element, at least one in cesium element, x is 0.01～0.08；
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 R2GeCl6: xNd3+Neodymium doping chlorine germanate up-conversion luminescent material.
The preparation method of neodymium the most according to claim 3 doping chlorine germanate up-conversion luminescent material, it is characterised in that institute
State RCl, GeCl4And NdCl3The each component molar of powder body is than for 2:1:(0.01～0.08).
The preparation method of neodymium the most according to claim 3 doping chlorine germanate up-conversion luminescent material, it is characterised in that institute
Stating x is 0.05.
The preparation method of neodymium the most according to claim 3 doping chlorine germanate up-conversion luminescent material, it is characterised in that step
Described in rapid two, mixing is to be ground in corundum alms bowl 20 minutes～60 minutes by described powder body.
The preparation method of neodymium the most according to claim 3 doping chlorine germanate up-conversion luminescent material, it is characterised in that step
By described presoma calcination 3 hours at 950 DEG C in rapid three.
The preparation method of neodymium the most according to claim 3 doping chlorine germanate up-conversion luminescent material, it is characterised in that step
Chilling temperature in rapid four 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 in described transparent encapsulated layer, be dispersed with neodymium doping chlorine germanate up-conversion luminescence material
Material, the chemical formula of described neodymium doping chlorine germanate up-conversion luminescent material is R2GeCl6: xNd3+, wherein, R is elemental lithium, sodium unit
Element, potassium element, rubidium element, at least one in cesium element, x is 0.01～0.08.
Organic Light Emitting Diode the most according to claim 9, it is characterised in that described x is 0.05.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107523300A (en) * | 2017-10-10 | 2017-12-29 | 南通纺织丝绸产业技术研究院 | A kind of Er3+Vanadium germanate light-converting material of doping and preparation method thereof |
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| CN104745182A (en) * | 2013-12-26 | 2015-07-01 | 海洋王照明科技股份有限公司 | Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof |
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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 |
| CN104745182A (en) * | 2013-12-26 | 2015-07-01 | 海洋王照明科技股份有限公司 | Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof |
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| CN107523300A (en) * | 2017-10-10 | 2017-12-29 | 南通纺织丝绸产业技术研究院 | A kind of Er3+Vanadium germanate light-converting material of doping and preparation method thereof |
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