CN103965896A - Praseodymium holmium co-doped zirconium aluminium oxide glass upconversion luminescence material, and preparation method and application thereof - Google Patents

Praseodymium holmium co-doped zirconium aluminium oxide glass upconversion luminescence material, and preparation method and application thereof Download PDF

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Publication number
CN103965896A
CN103965896A CN201310035308.5A CN201310035308A CN103965896A CN 103965896 A CN103965896 A CN 103965896A CN 201310035308 A CN201310035308 A CN 201310035308A CN 103965896 A CN103965896 A CN 103965896A
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Prior art keywords
aluminum oxide
glass
zirconium aluminum
luminous material
praseodymium holmium
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周明杰
王平
陈吉星
张振华
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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

A praseodymium holmium co-doped zirconium aluminum oxide glass upconversion luminescence material has a chemical formula of ZrO-Al2O3-Na2O:xPr<3+>, yHo<3+>, wherein x is 0.01- 0.06, and y is 0.01-0.04. In the photoluminescence spectrum of the praseodymium holmium co-doped zirconium aluminum oxide glass upconversion luminescence material, the praseodymium holmium co-doped zirconium aluminum oxide glass upconversion luminescence material has excitation wavelength of 578 nm, forms a luminescence peak at 483 nm wavelength zone by transition radiation of by Pr<3+> from 3P0 to 3H4, and can be used as a blue light luminescent material. The invention also provides a preparation method of the praseodymium holmium co-doped zirconium aluminum oxide glass upconversion luminescent material and an organic light-emitting diode using the praseodymium holmium co-doped zirconium aluminum oxide glass upconversion luminescent material.

Description

Praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, preparation method and application thereof
Technical field
The present invention relates to a kind of praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, 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 be short, flexible, and obtained the utmost point, apply widely.But owing to obtaining at present, the OLED blue light material of stability and high efficiency is more difficult, has limited greatly the development of white light OLED device and light source industry.
Upconverting fluorescent material can be launched visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in fields such as optical fiber communication technology, fibre amplifier, 3 D stereo demonstration, biomolecules fluorescence labelling, infrared detectives.But, can be by infrared, the long-wave radiations such as red-green glow inspire the praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass of blue emission, have not yet to see report.
Summary of the invention
Based on this, being necessary to provide a kind of can be inspired praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, the preparation method of blue light and be used the Organic Light Emitting Diode of this praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass by long-wave radiation.
A praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, its chemical formula is ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+, wherein, x is that 0.01～0.06, y is 0.01～0.04.
Described x is that 0.03, y is 0.02.
A preparation method for praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, comprises the following steps:
Step 1, according to ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+the stoichiometric ratio of each element takes ZrO, Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3powder, wherein, x is that 0.01～0.06, y is 0.01～0.04;
Step 2, the powder taking in described step 1 is mixed and obtains presoma;
Step 3, by the calcination 0.5 hour ~ 5 hours at 800 ℃ ~ 1100 ℃ of the presoma in described step 2;
Step 4, the precursor after processing in described step 3 is cooled to 100 ℃ ~ 300 ℃, then is incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass.
Described ZrO, Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3each component mol ratio of powder is (0.57 ~ 0.8): (0.12 ~ 0.3): (0.03 ~ 0.06): (0.01 ~ 0.06): (0.01 ~ 0.04).
Described x is that 0.03, y is 0.02.
Described in step 2, mixing is described powder to be ground in corundum alms bowl 20 minutes ~ 60 minutes.
In step 3 by the calcination 3 hours at 950 ℃ of described presoma.
Cooling temperature in step 4 is 200 ℃, 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, in described transparent encapsulated layer, be dispersed with praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, the chemical formula of described praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass is ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+, wherein, x is that 0.01～0.06, y is 0.01～0.04.
X is that 0.03, y is 0.02.
The preparation method of above-mentioned praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass is comparatively simple, and cost is lower, produces comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass of preparation, the excitation wavelength of praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass is 578nm, in 483nm wavelength zone by Pr 3+ion 3p 0→ 3h 4transition radiation form glow peak, can be used 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 the praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass of embodiment 1 preparation.
Fig. 3 is the Raman spectrum of the praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass of embodiment 1 preparation.
Fig. 4 forms the spectrogram of the Organic Light Emitting Diode emitting white light doped with praseodymium holmium codoped zirconium aluminum oxide changing luminous material material on glass in the transparent encapsulated layer of embodiment 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments, praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass and preparation method thereof is further illustrated.
The praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass of one embodiment, its chemical formula is ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+, wherein, x is that 0.01～0.06, y is 0.01～0.04.
Preferably, x is that 0.03, y is 0.02.
In the photoluminescence spectra of this praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, the excitation wavelength of praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass is 578nm, when material is subject to long wavelength's (as 578nm) radiation, and Pr 3+ion just in 3p 0excited state, then to 3h 4transition, just sends the blue light of 483nm, can be used as blue light emitting material.
The preparation method of above-mentioned praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, comprises the following steps:
Step S11, according to ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+the stoichiometric ratio of each element takes ZrO, Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3powder, wherein, x is that 0.01～0.06, y is 0.01～0.04.
In this step, described ZrO, Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3each component mol ratio of powder is (0.57 ~ 0.8): (0.12 ~ 0.3): (0.03 ~ 0.06): (0.01 ~ 0.06): (0.01 ~ 0.04).
In this step, preferred, x is that 0.03, y is 0.02.
Step S13, the powder taking in step S11 is mixed and obtains presoma.
In this step, powder is ground in corundum alms bowl to the 20 minutes ~ presoma that obtains mixing for 60 minutes, preferably grind 40 minutes.
Step S15, by presoma calcination 0.5 hour ~ 5 hours at 800 ℃ ~ 1100 ℃,
Preferably, presoma calcination 3 hours at 950 ℃.
After step S17, the precursor after will be in step S15 processing, be cooled to 100 ℃ ~ 300 ℃, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, wherein, x is that 0.01～0.06, y is 0.01～004.
Preferably, the precursor after processing in step S15 is cooled to 200 ℃, then is incubated 2 hours.
The preparation method of above-mentioned praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass is comparatively simple, and cost is lower, produces comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass of preparation, the excitation wavelength of praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass is 578nm, in 483nm wavelength zone by Pr 3+ion 3p 0→ 3h 4transition radiation form glow peak, can be used 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 substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 stacking gradually.In transparent encapsulated layer 5, be dispersed with praseodymium holmium codoped zirconium aluminum oxide changing luminous material 6 on glass, the chemical formula of praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass is ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+, wherein, x is 0.01～0.06, y is 0.01～0.04, organic luminous layer 3 in this device sends red-green glow, and part red-green glow excites and in transparent encapsulated layer 5, is dispersed with praseodymium holmium codoped zirconium aluminum oxide changing luminous material 6 on glass and sends blue light, and last redgreenblue just blendes together white light.
Be specific embodiment below.
Embodiment 1
Selecting purity is 99.99% powder, by ZrO, and Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3each component of powder makes it evenly mix for 40 minutes for 0.7:0.2:0.05:0.03:0.02 grinds in corundum mortar in molar ratio, then calcination 3 hours at 950 ℃ in retort furnace, then be cooled to 200 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtain block materials, after pulverizing, can obtain chemical general formula is 0.7ZrO-0.2Al 2o 3-0.05Na 2o:0.03Pr 3+, 0.02Ho 3+up-conversion phosphor.
Process prepared by Organic Light Emitting Diode:
The substrate 1 stacking gradually uses soda-lime glass, negative electrode 2 to use metal A g layer, organic luminous layer 3 to use Ir (piq) 2 (acac) Chinese name to close iridium (III), transparent anode 4 use tin indium oxide ITO two (1-phenyl-isoquinoline 99.9) (methyl ethyl diketones), and transparent encapsulated layer 5 tetrafluoroethylene.In transparent encapsulated layer 5, be dispersed with thulium doped tellurate changing luminous material 6 on glass, the chemical formula of thulium doped with fluorine silex glass up-conversion luminescent material is 0.7ZrO-0.2Al 2o 3-0.05Na 2o:0.03Pr 3+, 0.02Ho 3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass obtaining.As seen from Figure 2, the excitation wavelength of the praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass that the present embodiment obtains is 578nm, in 483nm wavelength zone by Pr 3+ion 3p 0→ 3h 4transition radiation form glow peak, this praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is for implementing the Raman spectrum of the praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass of 1 preparation, Raman spectrum as seen from the figure, Raman peaks is depicted as zirconium aluminum oxide characteristic peak as seen from the figure, the peak that does not occur doped element and other impurity, illustrates that doped element and substrate material have formed good bonding.
Refer to Fig. 4, Fig. 4 curve 1 is for form the spectrogram of the Organic Light Emitting Diode emitting white light in transparent encapsulated layer doped with praseodymium holmium codoped zirconium aluminum oxide changing luminous material material on glass, and curve 2 is not doped with the contrast of praseodymium holmium codoped zirconium aluminum oxide changing luminous material material on glass in transparent encapsulated layer.In figure, can find out, as can be seen from Figure 4, praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass can inspire the blue light of shortwave by the red light of long wave, after blue light mixes with ruddiness, forms white light.
Embodiment 2
Selecting purity is 99.99% powder, by ZrO, and Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3each component of powder is 0.8:0.12:0.06:0.01:0.01 in molar ratio, in corundum mortar, grind and it was evenly mixed in 20 minutes, then calcination 3 hours at 800 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, after pulverizing, can obtain chemical general formula is 0.8ZrO-0.12Al 2o 3-0.06Na 2o:0.01Pr 3+, 0.01Ho 3+up-conversion phosphor.
Embodiment 3
Selecting purity is 99.99% powder, by ZrO, and Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3each component of powder is 0.57:0.3:0.03:0.06:0.04 in molar ratio, in corundum mortar, grind and it was evenly mixed in 60 minutes, then calcination 3 hours at 1000 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtain block materials, after pulverizing, can obtain chemical general formula is 0.57ZrO-0.3Al 2o 3-0.03Na 2o:0.06Pr 3+, 0.04Ho 3+up-conversion phosphor.
Embodiment 4
Selecting purity is 99.99% powder, by ZrO, and Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3each component of powder is 0.6:0.25:0.08:0.04:0.03 in molar ratio, in corundum mortar, grind and it was evenly mixed in 30 minutes, then calcination 3 hours at 900 ℃ in retort furnace, then be cooled to 300 ℃ of insulations 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, after pulverizing, can obtain chemical general formula is 0.6ZrO-0.25Al 2o 3-0.08Na 2o:0.04Pr 3+, 0.03Ho 3+up-conversion phosphor.
Embodiment 5
Selecting purity is 99.99% powder, by ZrO, and Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3each component of powder is 0.65:0.22:0.04:0.05:0.04 in molar ratio, in corundum mortar, grind and it was evenly mixed in 60 minutes, then calcination 2 hours at 850 ℃ in retort furnace, then be cooled to 300 ℃ of insulations 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, after pulverizing, can obtain chemical general formula is 0.65ZrO-0.22Al 2o 3-0.04Na 2o:0.05Pr 3+, 0.04Ho 3+up-conversion phosphor.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore 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 praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, is characterized in that: its chemical general formula is ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+, wherein, x is that 0.01～0.06, y is 0.01～0.04.
2. praseodymium holmium codoped zirconium aluminum oxide according to claim 1 changing luminous material on glass, is characterized in that, described x is that 0.03, y is 0.02.
3. a preparation method for praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, is characterized in that, comprises the following steps:
Step 1, according to ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+the stoichiometric ratio of each element takes ZrO, Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3powder, wherein, x is that 0.01～0.06, y is 0.01～0.04;
Step 2, the powder taking in described step 1 is mixed and obtains presoma;
Step 3, by the calcination 0.5 hour ~ 5 hours at 800 ℃ ~ 1100 ℃ of described presoma;
Step 4, the precursor after processing in described step 3 is cooled to 100 ℃ ~ 300 ℃, then is incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass.
4. the preparation method of praseodymium holmium codoped zirconium aluminum oxide according to claim 3 changing luminous material on glass, is characterized in that described ZrO, Al 2o 3, Na 2o, Pr 2o 3and Ho 2o 3each component mol ratio of powder is (0.57 ~ 0.8): (0.12 ~ 0.3): (0.03 ~ 0.06): (0.01 ~ 0.06): (0.01 ~ 0.04).
5. the preparation method of praseodymium holmium codoped zirconium aluminum oxide according to claim 3 changing luminous material on glass, is characterized in that, described x is that 0.03, y is 0.02.
6. the preparation method of praseodymium holmium codoped zirconium aluminum oxide according to claim 3 changing luminous material on glass, is characterized in that, described in step 2, mixing is described powder to be ground in corundum alms bowl 20 minutes ~ 60 minutes.
7. the preparation method of praseodymium holmium codoped zirconium aluminum oxide according to claim 3 changing luminous material on glass, is characterized in that, in step 3 by the calcination 3 hours at 950 ℃ of described presoma.
8. the preparation method of praseodymium holmium codoped zirconium aluminum oxide according to claim 3 changing luminous material on glass, is characterized in that, the cooling temperature in step 4 is 200 ℃, and soaking time is 2 hours.
9. an Organic Light Emitting Diode, this Organic Light Emitting Diode comprises substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer stacking gradually, it is characterized in that, in described transparent encapsulated layer, be dispersed with praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass, the chemical formula of described praseodymium holmium codoped zirconium aluminum oxide changing luminous material on glass is ZrO-Al 2o 3-Na 2o:xPr 3+, yHo 3+, wherein, x is that 0.01～0.06, y is 0.01～0.04.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is that 0.03, y is 0.02.
CN201310035308.5A 2013-01-30 2013-01-30 Praseodymium holmium co-doped zirconium aluminium oxide glass upconversion luminescence material, and preparation method and application thereof Pending CN103965896A (en)

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Application publication date: 20140806