CN104650867A - Neodymium/holmium-codoped zirconium fluoride glass up-conversion luminescent material, preparation method and application thereof - Google Patents

Neodymium/holmium-codoped zirconium fluoride glass up-conversion luminescent material, preparation method and application thereof Download PDF

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CN104650867A
CN104650867A CN201310578159.7A CN201310578159A CN104650867A CN 104650867 A CN104650867 A CN 104650867A CN 201310578159 A CN201310578159 A CN 201310578159A CN 104650867 A CN104650867 A CN 104650867A
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neodymium
luminescent material
fluoride glass
conversion luminescent
zrf
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周明杰
陈吉星
王平
黄辉
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention relates to a neodymium/holmium-codoped zirconium fluoride glass up-conversion luminescent material, a chemical formula is ZrF4: xHo<3+>, yNd<3+>, wherein x is 0.005-0.05, y is 0.002-0.03. In a photoluminescence spectrum of the neodymium/holmium-codoped zirconium fluoride glass up-conversion luminescent material, the excitation wavelength of the neodymium/holmium-codoped zirconium fluoride glass up-conversion luminescent material is 586nm, a luminescence peak is formed by transition radiation of Nd<3+>ion 2P3/2-4I15/2 in a 469nm wavelength zone, and the luminescent material can be taken as a blue light luminescent material. The invention also provides a preparation method of the neodymium/holmium-codoped zirconium fluoride glass up-conversion luminescent material and an organic light-emitting diode by using the neodymium/holmium-codoped zirconium fluoride glass up-conversion luminescent material.

Description

Neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material, preparation method and application thereof
Technical field
The present invention relates to a kind of neodymium holmium codoped Zirkonium fluoride glass 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, the long-wave radiations such as red-green glow inspire the neodymium holmium codoped Zirkonium fluoride glass 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 inspire the neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material.
A kind of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material, its chemical general formula is ZrF 4: xHo 3+, yNd 3+, wherein, x is 0.005 ~ 0.05, y is 0.002 ~ 0.03.
Described x is 0.03, y is 0.01.
A preparation method for neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material, comprises the following steps:
Step one, according to ZrF 4: xHo 3+, yNd 3+the stoichiometric ratio of each element takes ZrF 4, HoF 3and NdF 3powder, wherein, x is 0.005 ~ 0.05, y is 0.002 ~ 0.03;
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 ZrF 4: xHo 3+, yNd 3+neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material.
Described ZrF 4, HoF 3and NdF 3the each component molar of powder is than being (92 ~ 99.3): (0.5 ~ 5): (0.2 ~ 3).
Described ZrF 4, HoF 3and NdF 3the each component molar of powder is than being 96:3:1.
Described in described 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 described step 3.
Cooling temperature in described step 4 is 250 DEG C, and soaking time is 2 hours.
A kind of 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, be dispersed with neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material is ZrF 4: xHo 3+, yNd 3+, wherein, x is 0.005 ~ 0.05, y is 0.002 ~ 0.03.
Described x is 0.03, y is 0.01.
The preparation method of above-mentioned neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material is comparatively simple, and cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of the neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material of preparation, the excitation wavelength of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material 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 of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material prepared by embodiment 1.
Fig. 3 is the Raman spectrum of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material prepared by embodiment 1.
Fig. 4 is the spectrogram forming the Organic Light Emitting Diode emitted white light in the transparent encapsulated layer of embodiment 1 preparation doped with neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material.
Embodiment
Below in conjunction with the drawings and specific embodiments, neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material and preparation method thereof is illustrated further.
The neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material of one embodiment, its chemical formula is ZrF 4: xHo 3+, yNd 3+, wherein x is 0.005 ~ 0.05, y is 0.002 ~ 0.03.
Preferably, x is 0.03, y is 0.01.
In the photoluminescence spectra of this neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material, the excitation wavelength of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material 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 above-mentioned neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material, comprises the following steps:
Step S11, according to ZrF 4: xHo 3+, yNd 3+the stoichiometric ratio of each element takes ZrF 4, HoF 3and NdF 3powder, wherein, x is 0.005 ~ 0.05, y is 0.002 ~ 0.03.
In this step, described ZrF 4, HoF 3and NdF 3the each component molar of powder is than being (92 ~ 99.3): (0.5 ~ 5): (0.2 ~ 3).
In this step, preferred ZrF 4, HoF 3and NdF 33the each component molar of powder is than being 96:3:1.
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 ZrF 4: xHo 3+, yNd 3+, wherein, x is 0.005 ~ 0.05, y is 0.002 ~ 0.03.
Preferably, the precursor after process in step S15 is cooled to 250 DEG C, then is incubated 2 hours.
The preparation method of above-mentioned neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material is comparatively simple, and cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of the neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material of preparation, the excitation wavelength of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material 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 holmium codoped Zirkonium fluoride glass up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material is ZrF 4: xHo 3+, yNd 3+wherein x is 0.005 ~ 0.05, y is 0.002 ~ 0.03, and 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 holmium codoped Zirkonium fluoride glass up-conversion luminescent material 6 and sends blue light, and last redgreenblue just blendes together white light.
Be specific embodiment below.
Embodiment 1
Select purity be 99.99% powder, by ZrF 4, HoF 3and NdF 3the each component of powder is respectively 0.96mmol by mole number, 0.03mmol 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 ZrF 4: 0.03Ho 3+, 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 holmium codoped Zirkonium fluoride glass up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material is ZrF 4: 0.03Ho 3+, 0.01Nd 3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material obtained.As can be seen from Fig. 2 curve 1, the excitation wavelength of the neodymium holmium codoped Zirkonium fluoride glass 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 neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material can be used as blue light emitting material, and curve 2 is not containing the neodymium doping Zirconium tetrafluoride sample comparative example ZrF of holmium doping 4: 0.01Nd 3+, contrast known, add the sample of holmium codoped, luminous position does not change, and luminous efficiency significantly improves.
Refer to Fig. 3, in Fig. 3, curve is neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material XRD curve prepared by enforcement 1, contrast PDF card, and diffraction peak is depicted as the crystal orientation of Zirconium tetrafluoride, do not occur illustrating that two kinds of elements are the lattices entering Zirconium tetrafluoride in the peak that neodymium holmium element is relevant.
Refer to Fig. 4, Fig. 4 curve 1 is the spectrogram forming the Organic Light Emitting Diode emitted white light in transparent encapsulated layer doped with neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material, and curve 2 is not doped with the contrast of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material in transparent encapsulated layer.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 ZrF 4, HoF 3and NdF 3the each component of powder is 0.965mmol by mole number, 0.005mmol, 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, and obtain block materials, can obtain chemical general formula after pulverizing is ZrF 4: 0.005Ho 3+, 0.03Nd 3+up-conversion phosphor.
Embodiment 3
Select purity be 99.99% powder, by ZrF 4, HoF 3and NdF 3the each component of powder is 0.948mmol by mole number, 0.05mmol, 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, and obtain block materials, can obtain chemical general formula after pulverizing is ZrF 4: 0.05Ho 3+, 0.002Nd 3+up-conversion phosphor.
Embodiment 4
Select purity be 99.99% powder, by ZrF 4, HoF 3and NdF 3the each component of powder is 0.97mmol by mole number, 0.02mmol, 0.01mmol grinds and makes its Homogeneous phase mixing in 40 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, and obtain block materials, can obtain chemical general formula after pulverizing is ZrF 4: 0.02Ho 3+, 0.01Nd 3+up-conversion phosphor.
Embodiment 5
Select purity be 99.99% powder, by ZrF 4, HoF 3and NdF 3the each component of powder is 0.94mmol by mole number, 0.03mmol, 0.03mmol 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, and obtain block materials, can obtain chemical general formula after pulverizing is ZrF 4: 0.04Ho 3+, 0.03Nd 3+up-conversion phosphor.
Embodiment 6
Select purity be 99.99% powder, by ZrF 4, HoF 3and NdF 3the each component of powder is 0.92mmol by mole number, 0.05mmol, 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, and obtain block materials, can obtain chemical general formula after pulverizing is ZrF 4: 0.05Ho 3+, 0.02Nd 3+up-conversion phosphor.
Embodiment 7
Select purity be 99.99% powder, by ZrF 4, HoF 3and NdF 3the each component of powder is 0.93mmol by mole number, 0.04mmol, 0.03mmol 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, and obtain block materials, can obtain chemical general formula after pulverizing is ZrF 4: 0.03Ho 3+, 0.03Nd 3+up-conversion phosphor.
Embodiment 8
Select purity be 99.99% powder, by ZrF 4, HoF 3and NdF 3the each component of powder is 0.95mmol by mole number, 0.02mmol, 0.03mmol grinds and makes its Homogeneous phase mixing in 20 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, and obtain block materials, can obtain chemical general formula after pulverizing is ZrF 4: 0.02Ho 3+, 0.03Nd 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 neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material, is characterized in that: its chemical general formula is ZrF 4: xHo 3+, yNd 3+, wherein, x is 0.005 ~ 0.05, y is 0.002 ~ 0.03.
2. neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material according to claim 1, it is characterized in that, described x is 0.03, y is 0.01.
3. a preparation method for neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material, is characterized in that, comprise the following steps:
Step one, according to ZrF 4: xHo 3+, yNd 3+the stoichiometric ratio of each element takes ZrF 4, HoF 3and NdF 3powder, wherein, x is 0.005 ~ 0.05, y is 0.002 ~ 0.03;
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 ZrF 4: xHo 3+, yNd 3+neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material.
4. the preparation method of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material according to claim 3, is characterized in that, described ZrF 4, HoF 3and NdF 3the each component molar of powder is than being (92 ~ 99.3): (0.5 ~ 5): (0.2 ~ 3).
5. the preparation method of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material according to claim 3, is characterized in that, described ZrF 4, HoF 3and NdF 3the each component molar of powder is than being 96:3:1.
6. the preparation method of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material according to claim 3, 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 neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material according to claim 3, is characterized in that, by the calcination 3 hours at 950 DEG C of described presoma in step 3.
8. the preparation method of neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material according to claim 3, it is characterized in that, the cooling temperature in step 4 is 250 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 holmium codoped Zirkonium fluoride glass up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described neodymium holmium codoped Zirkonium fluoride glass up-conversion luminescent material is ZrF 4: xHo 3+, yNd 3+, wherein, x is 0.005 ~ 0.05, y is 0.002 ~ 0.03.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is 0.03, y is 0.01.
CN201310578159.7A 2013-11-18 2013-11-18 Neodymium/holmium-codoped zirconium fluoride glass up-conversion luminescent material, preparation method and application thereof Pending CN104650867A (en)

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