CN103045237B - Neodymium-ytterbium double-doped barium chloride up-conversion luminescent material as well as preparation method and application thereof - Google Patents
Neodymium-ytterbium double-doped barium chloride up-conversion luminescent material as well as preparation method and application thereof Download PDFInfo
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- CN103045237B CN103045237B CN201110316210.8A CN201110316210A CN103045237B CN 103045237 B CN103045237 B CN 103045237B CN 201110316210 A CN201110316210 A CN 201110316210A CN 103045237 B CN103045237 B CN 103045237B
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Abstract
The invention relates to a neodymium-ytterbium double-doped barium chloride up-conversion luminescent material which has a chemical formula of BaCl2:xNd<3+>,yYb<3+>, wherein x is more than or equal to 0.01 and less than or equal to 0.05, and y is more than or equal to 0.01 and less than or equal to 0.06. In a photoluminescence spectrum of the neodymium-ytterbium double-doped barium chloride up-conversion luminescent material, the excitation wavelength of the neodymium-ytterbium double-doped barium chloride up-conversion luminescent material is 586nm, a luminescent peak is formed by transition radiation of Nd<3+> ions 2P3/2->4I15/2 in a 469nm wavelength area, and the neodymium-ytterbium double-doped barium chloride up-conversion luminescent material can emit short-wave blue light. The invention further provides a preparation method of the neodymium-ytterbium double-doped barium chloride up-conversion luminescent material and an organic luminescent device using the neodymium-ytterbium double-doped barium chloride up-conversion luminescent material.
Description
[technical field]
The present invention relates to a kind of neodymium ytterbium codope bariumchloride up-conversion luminescent material, preparation method and organic luminescent device.
[background technology]
Organic luminescent device (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 neodymium ytterbium codope bariumchloride 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 be inspired neodymium ytterbium codope bariumchloride up-conversion luminescent material, the preparation method of blue light and be used the organic luminescent device of this neodymium ytterbium codope bariumchloride up-conversion luminescent material by long-wave radiation.
A neodymium ytterbium codope bariumchloride up-conversion luminescent material, its chemical formula is BaCl
2: xNd
3+, yYb
3+, wherein, x is that 0.01～0.05, y is 0.01～0.06.
In a preferred embodiment, x is that 0.02, y is 0.03.
A preparation method for neodymium ytterbium codope bariumchloride up-conversion luminescent material, comprises the following steps: step 1, according to BaCl
22H
2o, Nd
2o
3and Yb
2o
3each powder is (89～98) in molar ratio: (1～5): (1～6);
Step 2, the powder taking in step 1 is mixed and obtains presoma;
Step 3, by the calcination 0.5 hour～5 hours at 500 ℃～900 ℃ of described presoma, be cooled to afterwards 100 ℃～300 ℃, then be incubated 0.5 hour～within 3 hours, obtain neodymium ytterbium codope bariumchloride up-conversion luminescent material, wherein chemical formula is BaCl
2: xNd
3+, yYb
3+, wherein, x is that 0.01～0.05, y is 0.01～0.06.
In a preferred embodiment, x is that 0.02, y is 0.03.
In a preferred embodiment, in step 2, powder is ground 20 minutes～60 minutes in corundum alms bowl body.
In a preferred embodiment, step 3 kind is by the calcination 3 hours at 750 ℃ of described presoma.
In a preferred embodiment, in step 3, by the calcination 3 hours at 750 ℃ of described presoma, be cooled to afterwards 200 ℃, then be incubated 2 hours and obtain neodymium ytterbium codope bariumchloride up-conversion luminescent material.
In a preferred embodiment, the calcination 0.5 hour～5 hours at 500 ℃～900 ℃ of presoma described in step 3, be cooled to afterwards 100 ℃～300 ℃, then be incubated 0.5 hour～after 3 hours, furnace cooling obtains bulk material to room temperature, and described bulk material is pulverized and obtained target product.
In a preferred embodiment, in step 2, the presoma that the powder ball milling taking in step 1 is obtained mixing.
A kind of organic luminescent device, this organic luminescent device comprises negative electrode, luminescent layer, conductive layer and the anode stacking gradually, the material of described luminescent layer is neodymium ytterbium codope bariumchloride up-conversion luminescent material, and the chemical formula of this neodymium ytterbium codope bariumchloride up-conversion luminescent material is BaCl
2: xNd
3+, yYb
3+, wherein, x is that 0.01～0.05, y is 0.01～0.06.
The preparation method of above-mentioned neodymium ytterbium codope bariumchloride 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 neodymium ytterbium codope bariumchloride up-conversion luminescent material of preparation, the excitation wavelength of neodymium ytterbium codope bariumchloride up-conversion luminescent material is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation form glow peak, send blue light shortwave luminous.
[accompanying drawing explanation]
Fig. 1 is the organic light-emitting device structural representation of an embodiment.
Fig. 2 is the photoluminescence spectrogram of the neodymium ytterbium codope bariumchloride up-conversion luminescent material of embodiment 1 preparation.
Fig. 3 is the XRD spectra of the neodymium ytterbium codope bariumchloride up-conversion luminescent material of embodiment 1 preparation.
[embodiment]
Below in conjunction with the drawings and specific embodiments, neodymium ytterbium codope bariumchloride up-conversion luminescent material and preparation method thereof is further illustrated.
The neodymium ytterbium codope bariumchloride up-conversion luminescent material of one embodiment, its chemical formula is BaCl
2: xNd
3+, yYb
3+, wherein, x is that 0.01～0.05, y is 0.01～0.06.
Preferably, x is that 0.02, y is 0.03.
In the photoluminescence spectra of this neodymium ytterbium codope bariumchloride up-conversion luminescent material, the preparation method of neodymium ytterbium codope bariumchloride 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 neodymium ytterbium codope bariumchloride up-conversion luminescent material of preparation, the excitation wavelength of neodymium ytterbium codope bariumchloride up-conversion luminescent material is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation form glow peak, send blue light shortwave luminous.
The preparation method of above-mentioned neodymium ytterbium codope bariumchloride up-conversion luminescent material, comprises the following steps:
Step S11, according to BaCl
22H
2o, Nd
2o
3and Yb
2o
3each powder is (86～96) in molar ratio: (1～5): (1～6).
In this step, preferred, BaCl
22H
2o, Nd
2o
3and Yb
2o
3each powder is 90: 2: 3 in molar ratio.
Step S13, the powder taking in step S11 is mixed and obtains presoma.
In this step, powder is ground in corundum alms bowl body 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 500 ℃～900 ℃, be cooled to afterwards 100 ℃～300 ℃, then be incubated 0.5 hour～within 3 hours, obtain neodymium ytterbium codope bariumchloride up-conversion luminescent material, wherein chemical formula is BaCl
2: xNd
3+, yYb
3+, wherein, x is that 0.01～0.05, y is 0.01～0.06.
In a preferred embodiment, x is that 0.02, y is 0.03.
Preferably, presoma calcination 3 hours at 750 ℃.
Preferably, at 500 ℃～900 ℃, calcination is cooled to 200 ℃ after 0.5 hour～5 hours, then is incubated 2 hours.
Preferably, presoma is put into retort furnace calcination 0.5 hour～5 hours at 500 ℃～900 ℃, be cooled to afterwards 100 ℃～300 ℃, be incubated again 0.5 hour～after 3 hours, furnace cooling obtains bulk material to room temperature, then bulk material is pulverized and obtained neodymium ytterbium codope bariumchloride up-conversion luminescent material.
The preparation method of above-mentioned neodymium ytterbium codope bariumchloride 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 neodymium ytterbium codope bariumchloride up-conversion luminescent material of preparation, the excitation wavelength of neodymium ytterbium codope bariumchloride up-conversion luminescent material is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation form glow peak, send blue light shortwave luminous.
Refer to Fig. 1, the organic luminescent device 100 of one embodiment, this organic luminescent device 100 comprises substrate 1, negative electrode 2, organic luminous layer 3, the transparent anode 4 stacking gradually and the transparent encapsulated layer 5 that is mixed with up-conversion phosphor 6, fluorescent material 6 materials in transparent encapsulated layer 5 are neodymium ytterbium codope bariumchloride up-conversion luminescent material, and its chemical formula is BaCl
2: xNd
3+, yYb
3+, wherein, x is 0.01～0.05, y is 0.01～0.06, 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 neodymium ytterbium codoped zirconium white up-conversion luminescent material 6 and sends blue light, and last redgreenblue just blendes together white light.
The material of the luminescent layer 2 of organic luminescent device 100 is neodymium ytterbium codope bariumchloride up-conversion luminescent material, and the excitation wavelength of neodymium ytterbium codope bariumchloride up-conversion luminescent material is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation form glow peak, send blue light shortwave luminous.The curve 1 of Fig. 2 is the illuminated diagram of having applied neodymium ytterbium codope bariumchloride up-conversion luminescent material, and curve 2 is not contain the comparative example of this neodymium ytterbium codope bariumchloride up-conversion luminescent material.Visible up-conversion luminescent material can inspire blue light by red-green glow, and colour mixture becomes the device of white light.
Be specific embodiment below.
Embodiment 1
Selecting purity is 99.99% powder, by 10mmol NH
4cl, 95mmol BaCl
22H
2o, 2mmolNd
2o
3with 3mmol Yb
2o
3powder grinds and it was evenly mixed in 40 minutes in corundum mortar, and then then calcination 3 hours at 750 ℃ is cooled to 200 ℃ of insulations 2 hours, then furnace cooling takes out to room temperature, obtains block materials, and after pulverizing, can obtain chemical general formula is BaCl
2: 0.02Nd
3+, 0.03Yb
3+up-conversion phosphor.
Refer to Fig. 2, curve 1 is the photoluminescence spectra of the present embodiment sample, and curve 2 is the sample comparative example of the ytterbium that undopes.The excitation wavelength of the neodymium ytterbium codope bariumchloride up-conversion luminescent material that the present embodiment obtains is 586nm, when material is subject to long wavelength's (as 586nm) radiation, and Nd
3+the energy of this illumination of ionic absorption, now Nd
3ion just in
2p
3/2excited state, then to
4i
15/2transition, just sends the blue light of 469nm, can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve, for implementing the XRD curve of the neodymium ytterbium codope bariumchloride up-conversion luminescent material of 1 preparation, contrasts PDF card, and diffraction peak is depicted as the crystal orientation of bariumchloride, there is not the relevant peak of neodymium ytterbium element, illustrate that two kinds of elements are the lattices that entered bariumchloride.
Embodiment 2
Selecting purity is 99.99% powder, by 22mmol NH
4cl, 89mmol BaCl
22H
2o, 5mmolNd
2o
3with 6mmol Yb
2o
3powder grinds and it was evenly mixed in 40 minutes in corundum mortar, and then then calcination 0.5 hour at 900 ℃ is cooled to 100 ℃ of insulations 0.5 hour, then furnace cooling takes out to room temperature, obtains block materials, and after pulverizing, can obtain chemical general formula is BaCl
2: 0.01Nd
3+, 0.06Yb
3+up-conversion phosphor.
Embodiment 3
Selecting purity is 99.99% powder, by 4mmol NH
4cl, 98mmol BaCl
22H
2o, 1mmol Nd
2o
3with 1mmol Yb
2o
3powder grinds and it was evenly mixed in 60 minutes in corundum mortar, and then then calcination 5 hours at 500 ℃ is cooled to 300 ℃ of insulations 3 hours, then furnace cooling takes out to room temperature, obtains block materials, and after pulverizing, can obtain chemical general formula is BaCl
2: 0.05Nd
3+, 0.01Yb
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 (3)
1. a neodymium ytterbium codope bariumchloride up-conversion luminescent material, is characterized in that: its chemical formula is BaCl
2: xNd
3+, yYb
3+, wherein, x is that 0.05, y is 0.01.
2. a preparation method for neodymium ytterbium codope bariumchloride up-conversion luminescent material, is characterized in that, comprises the following steps:
Selecting purity is 99.99% powder, by 4mmol NH
4cl, 98mmol BaCl
22H
2o, 1mmol Nd
2o
3with 1mmol Yb
2o
3powder grinds and it was evenly mixed in 60 minutes in corundum mortar, and then then calcination 5 hours at 500 ℃ is cooled to 300 ℃ of insulations 3 hours, then furnace cooling takes out to room temperature, obtains block materials, and after pulverizing, can obtain chemical general formula is BaCl
2: 0.05Nd
3+, 0.01Yb
3+up-conversion phosphor.
3. an organic luminescent device, this organic luminescent device comprises substrate, negative electrode, organic luminous layer, the transparent anode stacking gradually and the transparent encapsulated layer that is mixed with up-conversion phosphor, it is characterized in that, the chemical formula of the up-conversion phosphor in transparent encapsulated layer is BaCl
2: xNd
3+, yYb
3+, wherein, x is that 0.05, y is 0.01.
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| JPH06158041A (en) * | 1992-11-17 | 1994-06-07 | Fujitsu Ltd | Production of stimulable phosphor, and x-ray image conversion panel obtained using the stimulable phosphor |
| JPH10147778A (en) * | 1996-09-17 | 1998-06-02 | Konica Corp | Production of rare-earth-activated alkaline earth metal fluoride halide accelerated phosphor or precursor thereof, production apparatus therefor, accelerated phosphor or precursor thereof, and radiation image conversion panel |
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