CN103045260B - Holmium-doped yttrium oxysulfide up-conversion luminescent material as well as preparation method and application thereof - Google Patents
Holmium-doped yttrium oxysulfide up-conversion luminescent material as well as preparation method and application thereof Download PDFInfo
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- CN103045260B CN103045260B CN201110316226.9A CN201110316226A CN103045260B CN 103045260 B CN103045260 B CN 103045260B CN 201110316226 A CN201110316226 A CN 201110316226A CN 103045260 B CN103045260 B CN 103045260B
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- yttrium oxysulfide
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- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 53
- GFKJCVBFQRKZCJ-UHFFFAOYSA-N oxygen(2-);yttrium(3+);trisulfide Chemical compound [O-2].[O-2].[O-2].[S-2].[S-2].[S-2].[Y+3].[Y+3].[Y+3].[Y+3] GFKJCVBFQRKZCJ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910052689 Holmium Inorganic materials 0.000 claims description 43
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims description 39
- 239000000843 powder Substances 0.000 claims description 30
- 238000001354 calcination Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 239000010431 corundum Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 5
- 239000011707 mineral Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 230000005284 excitation Effects 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 abstract description 5
- 238000000103 photoluminescence spectrum Methods 0.000 abstract description 5
- 230000005472 transition radiation Effects 0.000 abstract 1
- 230000005855 radiation Effects 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 150000000922 Holmium Chemical class 0.000 description 4
- WHBHBVVOGNECLV-OBQKJFGGSA-N 11-deoxycortisol Chemical compound O=C1CC[C@]2(C)[C@H]3CC[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 WHBHBVVOGNECLV-OBQKJFGGSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001215 fluorescent labelling Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The invention relates to a holmium-doped yttrium oxysulfide up-conversion luminescent material which has a chemical formula of Y2O2S:xHo<3+>, wherein x is more than or equal to 0.01 and less than or equal to 0.05. In a photoluminescence spectrum of the holmium-doped yttrium oxysulfide up-conversion luminescent material, the excitation wavelength of the holmium-doped yttrium oxysulfide up-conversion luminescent material is 640nm, a luminescent peak is formed by transition radiation of Ho<3+> ions 5F3->5I8 in a 490nm wavelength area, and the holmium-doped yttrium oxysulfide up-conversion luminescent material can be used as a blue light emitting material. The invention further provides a preparation method of the holmium-doped yttrium oxysulfide up-conversion luminescent material and an organic light-emitting diode using the holmium-doped yttrium oxysulfide up-conversion luminescent material.
Description
[technical field]
The present invention relates to a kind of holmium doping yttrium oxysulfide 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 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 holmium doping yttrium oxysulfide 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 holmium doping yttrium oxysulfide up-conversion luminescent material, the preparation method of blue light and be used the Organic Light Emitting Diode of this holmium doping yttrium oxysulfide up-conversion luminescent material by long-wave radiation.
A holmium doping yttrium oxysulfide up-conversion luminescent material, its chemical formula for its chemical formula be Y
2o
2s:xHo
3+, 0.01≤x≤0.05 wherein.
In a preferred embodiment, x is 0.03.
A preparation method for holmium doping yttrium oxysulfide up-conversion luminescent material, comprises the following steps: step 1, take Y
2o
3, Ho
2o
3, S and Na
2cO
3powder, wherein Y
2o
3, Ho
2o
3, S, Na
2cO
3mol ratio be (0.95～0.99): (0.01～0.05): 1: 1.5; Step 2, the powder taking in step 1 is mixed and obtains presoma; Step 3, under reducing atmosphere, by the calcination 0.5 hour～5 hours at 800 ℃～1000 ℃ of described presoma, be cooled to afterwards 100 ℃～500 ℃, then be incubated 0.5 hour～within 3 hours, obtain powder product; Step 4, remove the Na in described powder product
2cO
3, obtain holmium doping yttrium oxysulfide up-conversion luminescent material.
In a preferred embodiment, Y
2o
3, Ho
2o
3, S, Na
2cO
3mol ratio be 0.97: 0.03: 1: 1.5.
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 800 ℃ of described presoma.
In a preferred embodiment, in step 3 by described presoma calcination at 800 ℃ 3 hours, be cooled to afterwards 250 ℃, then be incubated 2 hours and obtain described powder product.
In a preferred embodiment, described reducing atmosphere is argon hydrogen mixture, and wherein the molar content of hydrogen is 5%.
In a preferred embodiment, in step 4, the powder product that step 3 is obtained obtains described holmium doping yttrium oxysulfide up-conversion luminescent material by deionized water rinsing to neutral post-drying after putting into mineral acid immersion.
A kind of Organic Light Emitting Diode, this Organic Light Emitting Diode comprises substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer stacking gradually, in described transparent encapsulated layer, doped with holmium doping yttrium oxysulfide up-conversion luminescent material, the chemical formula of this holmium doping yttrium oxysulfide up-conversion luminescent material is Y
2o
2s:xHo
3+, 0.01≤x≤0.05 wherein
The preparation method of above-mentioned holmium doping yttrium oxysulfide 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 holmium doping yttrium oxysulfide up-conversion luminescent material of preparation, the excitation wavelength of holmium doping yttrium oxysulfide up-conversion luminescent material is 640nm, in 490nm wavelength zone by Ho
3+ion
5f
3→
5i
8transition 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 holmium doping yttrium oxysulfide up-conversion luminescent material of embodiment 1 preparation.
Fig. 3 is the XRD spectra of the holmium doping yttrium oxysulfide up-conversion luminescent material prepared of an embodiment.
[embodiment]
Below in conjunction with the drawings and specific embodiments, holmium doping yttrium oxysulfide up-conversion luminescent material and preparation method thereof is further illustrated.
The holmium doping yttrium oxysulfide up-conversion luminescent material of one embodiment, its chemical formula is Y
2o
2s:xHo
3+, 0.01≤x≤0.05 wherein.
Preferably, x is 0.03.
In the photoluminescence spectra of this holmium doping yttrium oxysulfide up-conversion luminescent material, the excitation wavelength of holmium doping yttrium oxysulfide up-conversion luminescent material is 640nm, when material is subject to long wavelength's (as 640nm) radiation, and Ho
3+ionic absorption energy, is energized into
5f
3excited state, then to
5i
8energy state transition, just sends the blue light of 490nm, can be used as blue light emitting material.
The preparation method of above-mentioned holmium doping yttrium oxysulfide up-conversion luminescent material, comprises the following steps:
Step S11, take Y
2o
3, Ho
2o
3, singly refer to sulphur (S) and Na
2cO
3powder, wherein Y
2o
3, Ho
2o
3, S, Na
2cO
3mol ratio be (0.95～0.99): (0.01～0.05): 1: 1.5.
In this step, Y
2o
3, Ho
2o
3, S, Na
2cO
3mol ratio be 0.97: 0.03: 1: 1.5.
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, under reducing atmosphere, by presoma calcination 0.5 hour～5 hours at 800 ℃～1000 ℃, be cooled to afterwards 100 ℃～500 ℃, then be incubated 0.5 hour～within 3 hours, obtain powder product.
Preferably, presoma calcination 3 hours at 800 ℃.
Preferably, at 800 ℃～1000 ℃, calcination is cooled to 250 ℃ 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 800 ℃～1000 ℃, be cooled to afterwards 100 ℃～500 ℃, then be incubated 0.5 hour～after 3 hours, furnace cooling obtains powder product to room temperature.
Preferably, reducing atmosphere is argon hydrogen mixture, and wherein the molar content of hydrogen is 5%.
Step S17, remove the Na in described powder product
2cO
3, obtain holmium doping yttrium oxysulfide up-conversion luminescent material.
Preferably, the powder product obtaining obtains holmium doping yttrium oxysulfide up-conversion luminescent material with deionized water rinsing to neutral rear filtering drying after putting into mineral acid immersion.Mineral acid can be sulfuric acid, hydrochloric acid or nitric acid, and in present embodiment, mineral acid is dilute hydrochloric acid.
The preparation method of above-mentioned holmium doping yttrium oxysulfide 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 holmium doping yttrium oxysulfide up-conversion luminescent material of preparation, the excitation wavelength of holmium doping yttrium oxysulfide up-conversion luminescent material is 640nm, in 490nm wavelength zone by Ho
3+ion
5f
3→
5i
8transition 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 holmium doping yttrium oxysulfide up-conversion luminescent material 6, the chemical formula of holmium doping yttrium oxysulfide up-conversion luminescent material is Y
2o
2s:xHo
3+, 0.01≤x≤0.05 wherein.
In the transparent encapsulated layer 5 of Organic Light Emitting Diode 100, be dispersed with holmium doping yttrium oxysulfide up-conversion luminescent material 6, holmium doping yttrium oxysulfide up-conversion luminescent material in 490nm wavelength zone by Ho
3+ion
5f
3→
5i
8transition radiation form glow peak, by red-green glow, excite and can launch blue light, blue light mixes the Organic Light Emitting Diode that formation emits white light afterwards with red-green glow.
Be specific embodiment below.
Embodiment 1
Selecting purity is 99.99% powder, Y
2o
3, Ho
2o
3, simple substance S and Na
2cO
3fusing assistant powder, its quality is respectively 2.318g, 0.189g, 1.074g, 0.836g.In corundum mortar, grind and it evenly mixed in 40 minutes, then at the argon hydrogen gas mixture of hydrogen 5% as calcination at 800 ℃, protection gas 3 hours.Then be cooled to 250 ℃ of insulations 2 hours, then naturally cool to room temperature taking-up powder, put into hot dilute hydrochloric acid and soak 1 hour, then extremely neutral with deionized water rinsing, overanxious oven dry, obtains final fluorescent material.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the holmium doping yttrium oxysulfide up-conversion luminescent material obtaining.As seen from Figure 2, the excitation wavelength of holmium that the present embodiment obtains doping yttrium oxysulfide up-conversion luminescent material is 640nm, in 490nm wavelength zone by Ho
3+ion
5f
3→
5i
8transition radiation form glow peak, this holmium doping yttrium oxysulfide up-conversion luminescent material can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3 curve 1 for implementing the XRD spectra of the holmium doping yttrium oxysulfide up-conversion luminescent material of 1 preparation, curve 2 for sintering temperature under equal conditions be the correlation curve of 500 ℃.During low temperature, reaction not exclusively, also has Y
2o
3peak, pyroreaction is complete, shows Y
2o
2the peak of S.
Embodiment 2
Selecting purity is 99.99% powder, Y
2o
3, Ho
2o
3, simple substance S and Na
2cO
3fusing assistant powder, its quality is respectively 2.196g, 0.378g, 1.103g, 0.858g.In corundum mortar, grind and it evenly mixed in 20 minutes, then at the argon hydrogen gas mixture of hydrogen 5% as calcination at 500 ℃, protection gas 5 hours.Then be cooled to 100 ℃ of insulations 0.5 hour, then naturally cool to room temperature taking-up powder, put into hot dilute hydrochloric acid and soak 1 hour, then extremely neutral with deionized water rinsing, overanxious oven dry, obtains final fluorescent material.
Embodiment 3
Selecting purity is 99.99% powder, Y
2o
3, Ho
2o
3, simple substance S and Na
2cO
3fusing assistant powder, its quality is respectively 2.416g, 0.038g, 1.636g, 1.052g.In corundum mortar, grind and it evenly mixed in 60 minutes, then at the argon hydrogen gas mixture of hydrogen 5% as calcination at 1000 ℃, protection gas 0.5 hour.Then be cooled to 500 ℃ of insulations 3 hours, then naturally cool to room temperature taking-up powder, put into hot dilute hydrochloric acid and soak 1 hour, then extremely neutral with deionized water rinsing, overanxious oven dry, obtains final fluorescent material.
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 (7)
1. a preparation method for holmium doping yttrium oxysulfide up-conversion luminescent material, is characterized in that, comprises the following steps:
Step 1, take Y
2o
3, Ho
2o
3, S and Na
2cO
3powder, wherein Y
2o
3, Ho
2o
3, S, Na
2cO
3mol ratio be (0.95～0.99): (0.01～0.05): 1:1.5;
Step 2, the powder taking in step 1 is mixed and obtains presoma;
Step 3, under reducing atmosphere, by the calcination 0.5 hour～5 hours at 800 ℃～1000 ℃ of described presoma, be cooled to afterwards 100 ℃～500 ℃, then be incubated 0.5 hour～within 3 hours, obtain powder product;
Step 4, remove the Na in described powder product
2cO
3, obtain holmium doping yttrium oxysulfide up-conversion luminescent material.
2. the preparation method of holmium doping yttrium oxysulfide up-conversion luminescent material according to claim 1, is characterized in that Y
2o
3, Ho
2o
3, S, Na
2cO
3mol ratio 0.97:0.03:1:1.5.
3. the preparation method of holmium doping yttrium oxysulfide up-conversion luminescent material according to claim 1, is characterized in that, in step 2, powder is ground 20 minutes～60 minutes in corundum alms bowl body.
4. the preparation method of holmium according to claim 1 doping yttrium oxysulfide up-conversion luminescent material, is characterized in that, step 3 kind is by the calcination 3 hours at 800 ℃ of described presoma.
5. the preparation method of holmium according to claim 1 doping yttrium oxysulfide up-conversion luminescent material, is characterized in that, in step 3, by the calcination 3 hours at 800 ℃ of described presoma, is cooled to afterwards 250 ℃, then is incubated 2 hours and obtains described powder product.
6. the preparation method of holmium doping yttrium oxysulfide up-conversion luminescent material according to claim 1, is characterized in that, described reducing atmosphere is argon hydrogen mixture, and wherein the molar content of hydrogen is 5%.
7. the preparation method of holmium according to claim 1 doping yttrium oxysulfide up-conversion luminescent material, it is characterized in that, in step 4, the powder product that step 3 is obtained obtains described holmium doping yttrium oxysulfide up-conversion luminescent material by deionized water rinsing to neutral post-drying after putting into mineral acid immersion.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3647707A (en) * | 1969-09-08 | 1972-03-07 | Gen Electric | Alkali monosulfide recrystallization of lanthanide oxysulfide luminescent material |
| US6132642A (en) * | 1994-07-01 | 2000-10-17 | Sarnoff Corporation | Method of preparing small particle size phosphors |
-
2011
- 2011-10-17 CN CN201110316226.9A patent/CN103045260B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3647707A (en) * | 1969-09-08 | 1972-03-07 | Gen Electric | Alkali monosulfide recrystallization of lanthanide oxysulfide luminescent material |
| US6132642A (en) * | 1994-07-01 | 2000-10-17 | Sarnoff Corporation | Method of preparing small particle size phosphors |
Non-Patent Citations (4)
| Title |
|---|
| Eiichiro Nakazawa et al..Trapping mechanism in the afterglow process of the rare-earth activated Y2O2S phosphors.《Journal of Luminescence》.2007, * |
| Trapping mechanism in the afterglow process of the rare-earth activated Y2O2S phosphors;Eiichiro Nakazawa et al.;《Journal of Luminescence》;20071009;494-498 * |
| Upconversion luminescence of holmium and ytterbium co-doped yttrium oxysulfide phosphor;Xi-xian Luo et al.;《Materials Letters》;20061223;3696-3700 * |
| Xi-xian Luo et al..Upconversion luminescence of holmium and ytterbium co-doped yttrium oxysulfide phosphor.《Materials Letters》.2006, * |
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