CN104212444A - Neodymium doped double alkaline-earth metal fluoride up-conversion luminescent material, preparation method and applications thereof - Google Patents
Neodymium doped double alkaline-earth metal fluoride up-conversion luminescent material, preparation method and applications thereof Download PDFInfo
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Abstract
The invention discloses a neodymium doped double alkaline-earth metal fluoride up-conversion luminescent material, which is represented by a chemical formula: AmB<1-m>F2:xNd3+, wherein m is in a range of 0.1 to 0.9, the A represents a magnesium element, a calcium element, a strontium element, or a barium element, and the B represents a magnesium element, a calcium element, a strontium element, or a barium element. In the photoluminescence spectrum of the up-conversion luminescent material, the excitation wavelength of the up-conversion luminescent material is at 586 nm, a luminescence peak is formed in the 469nm wavelength zone by the transition radiation of Nd3+ ion from the 2P3/2 to 4I15/2, and the up-conversion luminescent material can be used as a blue light luminescent material. The invention also provides a preparation method of the up-conversion luminescent material, and an organic light emitting diode using the up-conversion luminescent material.
Description
Technical field
The present invention relates to the doping of a kind of neodymium and fluoridize two alkaline earth salt up-conversion luminescent material, preparation method and Organic Light Emitting Diode.
Background technology
Organic Light Emitting Diode (OLED) because unit construction is simple, the characteristic such as cheap, the luminous of production cost, reaction times is short, flexible, and obtain a very wide range of application.But because the OLED blue light material obtaining stability and high efficiency is at present more difficult, significantly limit the development of white light OLED device and light source industry.
Upconverting fluorescent material can launch visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in the field such as optical fiber communication technology, fibre amplifier, 3 D stereo display, biomolecules fluorescence labelling, infrared detective.But, can by infrared, two alkaline earth salt up-conversion luminescent material is fluoridized in the neodymium doping that the long-wave radiations such as red-green glow inspire blue emission, has not yet to see report.
Summary of the invention
Based on this, be necessary to provide a kind of neodymium that can inspire blue light by long-wave radiation to adulterate the Organic Light Emitting Diode fluoridized two alkaline earth salt up-conversion luminescent material, preparation method and use this neodymium to adulterate and fluoridize two alkaline earth salt up-conversion luminescent material.
Two alkaline earth salt up-conversion luminescent material is fluoridized in a kind of neodymium doping, and its chemical formula is A
mb
1-mf
2: xNd
3+, wherein, x is 0.002 ~ 0.03, m be 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, and B is magnesium elements, calcium constituent, the one in strontium element and barium element.
Described x is 0.01, m is 0.5.
A preparation method for two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping, comprises the following steps:
Step one, according to A
mb
1-mf
2: xNd
3+the stoichiometric ratio of each element takes AF
2, BF
2, and NdF
3powder, wherein, x is 0.002 ~ 0.03, m be 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, and B is magnesium elements, calcium constituent, the one in strontium element and barium element;
Step 2, the powder taken mixed obtain presoma in described step one;
Step 3, by the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of the presoma in described step 2,
Step 4, the precursor after process in described step 3 is cooled to 100 DEG C ~ 300 DEG C, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is A
mb
1-mf
2: xNd
3+neodymium doping fluoridize two alkaline earth salt up-conversion luminescent material.
Described AF
2, BF
2, and NdF
3the each component molar of powder is than being (0.1 ~ 0.9): (0.1 ~ 0.9): (0.002 ~ 0.03).
Described AF
2, BF
2, and NdF
3the each component molar of powder is than being 0.5:0.49:0.01.
Described in step 2, mixing is that described powder is ground 20 minutes ~ 60 minutes in corundum alms bowl.
By the calcination 3 hours at 950 DEG C of described presoma in step 3.
Cooling temperature in step 4 is 200 DEG C, and soaking time is 2 hours.
A kind of 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, be dispersed with neodymium doping in described transparent encapsulated layer and fluoridize two alkaline earth salt up-conversion luminescent material, the chemical formula that two alkaline earth salt up-conversion luminescent material is fluoridized in described neodymium doping is A
mb
1-mf
2: xNd
3+, wherein, x is 0.002 ~ 0.03, m be 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, and B is magnesium elements, calcium constituent, the one in strontium element and barium element.
X is 0.01, m is 0.5.
The preparation method that two alkaline earth salt up-conversion luminescent material is fluoridized in above-mentioned neodymium doping is comparatively simple, and cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; The neodymium doping of preparation is fluoridized in the photoluminescence spectra of two alkaline earth salt up-conversion luminescent material, and the excitation wavelength that two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation formed glow peak, can as blue light emitting material.
Accompanying drawing explanation
Fig. 1 is the structural representation of the Organic Light Emitting Diode of an embodiment.
Fig. 2 is the photoluminescence spectrogram that two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping prepared by embodiment 1.
Fig. 3 is the XRD spectra that two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping prepared by embodiment 1.
Fig. 4 fluoridizes doped with neodymium doping the spectrogram that two alkaline earth salt up-conversion luminescent material forms the Organic Light Emitting Diode emitted white light in the transparent encapsulated layer of embodiment 1 preparation.
Embodiment
Fluoridize two alkaline earth salt up-conversion luminescent material and preparation method thereof below in conjunction with the drawings and specific embodiments to neodymium doping to illustrate further.
Two alkaline earth salt up-conversion luminescent material is fluoridized in the neodymium doping of one embodiment, and its chemical formula is A
mb
1-mf
2: xNd
3+, wherein, x is 0.002 ~ 0.03, m be 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, and B is magnesium elements, calcium constituent, the one in strontium element and barium element.
Preferably, x is 0.01, m is 0.5.
Preferably, elements A and B are two kinds of not identical elements.
The doping of this neodymium is fluoridized in the photoluminescence spectra of two alkaline earth salt up-conversion luminescent material, and the excitation wavelength that two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping is 586nm, when material is subject to the radiation of long wavelength (as 586nm) time, and Nd
3+ion has just been in
2p
3/2excited state, then to
4i
15/2transition, just sends the blue light of 469nm, can as blue light emitting material.
The preparation method of two alkaline earth salt up-conversion luminescent material is fluoridized in above-mentioned neodymium doping, comprises the following steps:
Step S11, according to A
mb
1-mf
2: xNd
3+the stoichiometric ratio of each element takes AF
2, BF
2, and NdF
3powder, wherein, x is 0.002 ~ 0.03, m be 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, and B is magnesium elements, calcium constituent, the one in strontium element and barium element.
In this step, described AF
2, BF
2, and NdF
3the each component molar of powder is than being (0.1 ~ 0.9): (0.1 ~ 0.9): (0.002 ~ 0.03).
In this step, described AF
2, BF
2, and NdF
3the each component molar of powder is than being 0.5:0.49:0.01.
Step S13, the powder taken mixed obtain presoma in step S11.
In this step, powder is ground in corundum alms bowl the presoma obtaining mixing for 20 minutes ~ 60 minutes, preferred grinding 40 minutes.
Step S15, by presoma calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C,
Preferably, presoma calcination 3 hours at 950 DEG C.
Step S17, be cooled to 100 DEG C ~ 500 DEG C by after the precursor after process in step S15, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is A
mb
1-mf
2: xNd
3+, wherein, x is 0.002 ~ 0.03, m be 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, and B is magnesium elements, calcium constituent, the one in strontium element and barium element.
Preferably, the precursor after process in step S15 is cooled to 200 DEG C, then is incubated 2 hours.
The preparation method that two alkaline earth salt up-conversion luminescent material is fluoridized in above-mentioned neodymium doping is comparatively simple, and cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; The neodymium doping of preparation is fluoridized in the photoluminescence spectra of two alkaline earth salt up-conversion luminescent material, and the excitation wavelength that two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation formed glow peak, can as blue light emitting material.
Refer to Fig. 1, the Organic Light Emitting Diode 100 of an embodiment, this Organic Light Emitting Diode 100 comprises the substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 that stack gradually.Be dispersed with neodymium doping in transparent encapsulated layer 5 and fluoridize two alkaline earth salt up-conversion luminescent material 6, the chemical formula that two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping is A
mb
1-mf
2: xNd
3+, wherein, x is 0.002 ~ 0.03, m is 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, B is magnesium elements, calcium constituent, the one in strontium element and barium element, the organic luminous layer 3 in this device sends red-green glow, part red-green glow excites in transparent encapsulated layer 5 and is dispersed with neodymium doping and fluoridizes two alkaline earth salt up-conversion luminescent material 6 and send blue light, and last redgreenblue just blendes together white light.
Be specific embodiment below.
Embodiment 1
Select purity be 99.99% powder, by MgF
2, CaF
2and NdF
3the each component of powder is 0.1mmol by mole number, 0.89mmol and 0.01mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, then 200 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is Mg
0.1ca
0.89f
2: 0.01Nd
3+up-conversion phosphor.
Process prepared by Organic Light Emitting Diode:
The substrate 1 stacked gradually uses soda-lime glass, negative electrode 2 uses metal A g layer, organic luminous layer 3 uses Ir (piq) 2 (acac) Chinese name (methyl ethyl diketone) closes iridium (III), transparent anode 4 uses tin indium oxide ITO two (1-phenyl-isoquinoline 99.9), and transparent encapsulated layer 5 tetrafluoroethylene.Be dispersed with neodymium doping in transparent encapsulated layer 5 and fluoridize two alkaline earth salt up-conversion luminescent material 6, the chemical formula that two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping is Mg
0.1ca
0.89f
2: 0.01Nd
3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of two alkaline earth salt up-conversion luminescent material is fluoridized in the neodymium doping obtained.As seen from Figure 2, the excitation wavelength that two alkaline earth salt up-conversion luminescent material is fluoridized in the neodymium doping that the present embodiment obtains is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation form glow peak, the doping of this neodymium is fluoridized two alkaline earth salt up-conversion luminescent material and be can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is the XRD curve that two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping prepared by enforcement 1, contrast PDF card, diffraction peak is depicted as the peak crystallization of fluoridizing two alkaline earth salts, there is not the diffraction peak of doped element and other impurity, illustrate that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, Fig. 4 curve 1 is fluoridize doped with neodymium doping the spectrogram that two alkaline earth salt up-conversion luminescent material material forms the Organic Light Emitting Diode emitted white light in transparent encapsulated layer, and curve 2 is the contrast of not fluoridizing two alkaline earth salt up-conversion luminescent material material in transparent encapsulated layer doped with neodymium doping.Can find out in figure, up-conversion luminescent material by the red light of long wave, can inspire the blue light of shortwave, forms white light after blue light mixes with ruddiness.
Embodiment 2
Select purity be 99.99% powder, by MgF
2, CaF
2and NdF
3the each component of powder is 0.5mmol by mole number, 0.47mmol and 0.03mmol grinds and makes its Homogeneous phase mixing in 20 minutes in corundum mortar, then calcination 3 hours at 800 DEG C in retort furnace, then 250 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is Mg
0.5ca
0.47f
2: 0.03Nd
3+up-conversion phosphor.
Embodiment 3
Select purity be 99.99% powder, by MgF
2, SrF
2and NdF
3the each component of powder is 0.8mmol by mole number, 0.198mmol and 0.002mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, then 250 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is Mg
0.2sr
0.798f
2: 0.002Nd
3+up-conversion phosphor.
Embodiment 4
Select purity be 99.99% powder, by MgF
2, SrF
2and NdF
3the each component of powder is 0.3mmol by mole number, 0.68mmol and 0.02mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, then 250 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is M
g0.3sr
0.68f
2: 0.02Nd
3+up-conversion phosphor.
Embodiment 5
Select purity be 99.99% powder, by MgF
2, BaF
2and NdF
3the each component of powder is 0.4mmol by mole number, 0.57mmol and 0.03mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 5 hours at 800 DEG C in retort furnace, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is M
g0.4ba
0.57f
2: 0.03Nd
3+up-conversion phosphor.
Embodiment 6
Select purity be 99.99% powder, by MgF
2, BaF
2and NdF
3the each component of powder is 0.9mmol by mole number, 0.098mmol and 0.002mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, then 500 DEG C are cooled to be incubated 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is Mg
0.9ba
0.098f
2: 0.002Nd
3+up-conversion phosphor.
Embodiment 7
Select purity be 99.99% powder, by CaF
2, BaF
2and NdF
3the each component of powder is 0.49mmol by mole number, 0.5mmol and 0.01mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, then 250 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is Ca
0.49ba
0.5f
2: 0.01Nd
3+up-conversion phosphor.
Embodiment 8
Select purity be 99.99% powder, by CaF
2, BaF
2and NdF
3the each component of powder is 0.37mmol by mole number, 0.6mmol and 0.03mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 5 hours at 800 DEG C in retort furnace, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Ca
0.37ba
0.6f
2: 0.03Nd
3+up-conversion phosphor.
Embodiment 9
Select purity be 99.99% powder, by SrF
2, CaF
2, and NdF
3the each component of powder is 0.198mmol by mole number, 0.8mmol and 0.002mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, then 500 DEG C are cooled to be incubated 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is Sr
0.198ca
0.8f
2: 0.002Nd
3+up-conversion phosphor.
Embodiment 10
Select purity be 99.99% powder, by SrF
2, CaF
2, and NdF
3the each component of powder is 0.29mmol by mole number, 0.7mmol and 0.01mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, then 250 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is Sr
0.29ca
0.7f
2: 0.01Nd
3+up-conversion phosphor.
Embodiment 11
Select purity be 99.99% powder, by BaF
2, SrF
2and NdF
3the each component of powder is 0.4mmol by mole number, 0.57mmol and 0.03mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 5 hours at 800 DEG C in retort furnace, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Ba
0.4sr
0.57f
2: 0.03Nd
3+up-conversion phosphor.
Embodiment 12
Select purity be 99.99% powder, by BaF
2, SrF
2and NdF
3the each component of powder is 0.3mmol by mole number, 0.698mmol and 0.002mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, then 500 DEG C are cooled to be incubated 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is Ba
0.3sr
0.698f
2: 0.002Nd
3+up-conversion phosphor.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping, it is characterized in that: its chemical general formula is A
mb
1-mf
2: xNd
3+, wherein, x is 0.002 ~ 0.03, m be 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, and B is magnesium elements, calcium constituent, the one in strontium element and barium element.
2. two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping according to claim 1, and it is characterized in that, described x is 0.01, m is 0.5.
3. a preparation method for two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping, it is characterized in that, comprises the following steps:
Step one, according to A
mb
1-mf
2: xNd
3+the stoichiometric ratio of each element takes AF
2, BF
2, and NdF
3powder, wherein, x is 0.002 ~ 0.03, m be 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, and B is magnesium elements, calcium constituent, the one in strontium element and barium element;
Step 2, the powder taken mixed obtain presoma in described step one;
Step 3, by the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of described presoma,
Step 4, the precursor after process in described step 3 is cooled to 100 DEG C ~ 300 DEG C, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is A
mb
1-mf
2: xNd
3+neodymium doping fluoridize two alkaline earth salt up-conversion luminescent material.
4. the preparation method of two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping according to claim 3, it is characterized in that, described AF
2, BF
2, and NdF
3the each component molar of powder is than being (0.1 ~ 0.9): (0.1 ~ 0.9): (0.002 ~ 0.03).
5. the preparation method of two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping according to claim 3, it is characterized in that, described AF
2, BF
2, and NdF
3the each component molar of powder is than being 0.5:0.49:0.01.
6. the preparation method of two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping according to claim 3, and it is characterized in that, described in step 2, mixing is that described powder is ground 20 minutes ~ 60 minutes in corundum alms bowl.
7. the preparation method of two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium according to claim 3 doping, it is characterized in that, by the calcination 3 hours at 950 DEG C of described presoma in step 3.
8. the preparation method of two alkaline earth salt up-conversion luminescent material is fluoridized in neodymium doping according to claim 3, and it is characterized in that, the cooling temperature in step 4 is 200 DEG C, and soaking time is 2 hours.
9. an Organic Light Emitting Diode, this Organic Light Emitting Diode comprises the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, it is characterized in that, be dispersed with neodymium doping in described transparent encapsulated layer and fluoridize two alkaline earth salt up-conversion luminescent material, the chemical formula that two alkaline earth salt up-conversion luminescent material is fluoridized in described neodymium doping is A
mb
1-mf
2: xNd
3+, wherein, x is 0.002 ~ 0.03, m be 0.1 ~ 0.9, A is magnesium elements, calcium constituent, the one in strontium element and barium element, and B is magnesium elements, calcium constituent, the one in strontium element and barium element.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is 0.01, m is 0.5.
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| CN113403065B (en) * | 2021-04-30 | 2022-11-18 | 河北大学 | Fluoride-based stress luminescent material, preparation method and application thereof |
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Application publication date: 20141217 |