CN102321481B - Triple-doped sulfur oxide up-conversion white light material and preparation method thereof - Google Patents
Triple-doped sulfur oxide up-conversion white light material and preparation method thereof Download PDFInfo
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- CN102321481B CN102321481B CN2011101922563A CN201110192256A CN102321481B CN 102321481 B CN102321481 B CN 102321481B CN 2011101922563 A CN2011101922563 A CN 2011101922563A CN 201110192256 A CN201110192256 A CN 201110192256A CN 102321481 B CN102321481 B CN 102321481B
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- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 27
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 17
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 title abstract 2
- 239000002994 raw material Substances 0.000 claims description 19
- 238000009413 insulation Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- 239000012190 activator Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 230000001235 sensitizing effect Effects 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 241000282693 Cercopithecidae Species 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention relates to a triple-doped sulfur oxide up-conversion white light material and a preparation method thereof. The material is characterized in that the structural formula of the material is (Ln1-x-y-zYbxTmyREz)2O2S, wherein x = 0.04-0.1, y = 0.005-0.01, and z = 0.005-0.01. The material used as an up-conversion white light material can generate high-efficiency white light, thus the material can be applied in the fields of solid-state color three-dimensional display, background light, liquid crystal display and the like; and the material is synthesized by a solid-phase method, and the preparation method is simple and is easy to operate.
Description
Technical field
The present invention relates to conversion of white light material and preparation method thereof, relate in particular to conversion of white light material and preparation method thereof on a kind of three doping oxysulfides.
Background technology
Up-conversion luminescence can be transformed into versicolor visible light by non-linear multiphoton process with near infrared light, is one of effective ways that produce at present white light.White light source based on up-conversion luminescence is a kind of very potential LCD backlight source, because it need not by optical filtering technique, and can design colour temperature.In addition, and compare based on the white light source of down conversion, last conversion of white light source can be exported up to several ten thousand cd/m
2Brightness and the performance of luminescent powder without any decay.Simultaneously, because following conversion of white light LED exists following three shortcomings: different LED devices raises along with temperature, and luminosity decline degree difference is very big, consequently causes the drift of the chromaticity coordinates of mixed white light; Excite yellow fluorescent powder with the blue led chip, lack the red spectrum composition in the white light that blue light and gold-tinted combination obtain, so the colour rendering index of light source is lower; The near ultraviolet LED chip may produce ultraviolet and pollute.Therefore, explore the focus that high-quality last conversion of white light material becomes current research.
Summary of the invention
The objective of the invention is to provide in order to improve the deficiencies in the prior art conversion of white light material and preparation method thereof on a kind of three doping oxysulfides.It is higher that this kind gone up the conversion of white light material luminous efficiency, by the three different ions concentration designs of mixing, makes material send efficient nearly white light, thereby can be used for fields such as solid state color 3-D display, bias light and liquid-crystal display.The synthetic employing solid phase method preparation of this material, and the preparation method is simple, and easy to operate.
Technical scheme of the present invention is: conversion of white light material on a kind of three doping oxysulfides, the structural formula that it is characterized in that material is (Ln
1-x-y-zYb
xTm
yRE
z)
2O
2S, x=0.04～0.1, y=0.005～0.01, z=0.005～0.01; Its raw material is Ln
2O
3, sensitizing agent, activator and fusing assistant, wherein Ln
2O
3Be at least La
2O
3, Y
2O
3Or Gd
2O
3In a kind of; Sensitizing agent is Yb
2O
3Activator is Tm
2O
3And RE
2O
3, RE wherein
2O
3Be Er
2O
3, Ho
2O
3Or Eu
2O
3In a kind of; Fusing assistant is AL
2CO
3And sublimed sulphur, wherein AL
2CO
3Be at least Li
2CO
3, Na
2CO
3Or K
2CO
3In a kind of; The wherein mole number of sublimed sulphur and Ln
2O
3, sensitizing agent and activator the ratio of total mole number be 3.5～4.5: 1, AL
2CO
3Mole number with and Ln
2O
3, sensitizing agent and activator the ratio of total mole number be 1.5～2: 1.
The present invention also provides the preparation method of above-mentioned materials, adopts the molten method preparation of sulphur; Its step is as follows:
1. take by weighing desired raw material by above-mentioned molar percentage, the raw material that weighs up is mixed;
2. the raw material that mixes is packed in the set crucible with cover, fill high temperature resistant powder and compacting in the gap of two crucibles;
3. crucible gradient increased temperature to 1050～1250 ℃ of compound will be housed, and insulation 3h～5h is cooled to room temperature with stove then;
4. the product behind the sintering also stirs with hot wash, suction filtration;
5. the product after will washing is put into the constant temperature air dry oven dries, and obtains the conversion of white light material.
The gradient increased temperature of preferred steps described in 3. is for to be warmed up to 300～350 ℃ with 2～3 ℃/min of temperature rise rate, and insulation 1h～2h, is warmed up to 1050～1250 ℃ with 3～3.5 ℃/min of temperature rise rate then, and insulation 3h～5h.
Wherein step specific implementation method 3. is to pack in the monkey with cover the raw material that mixes and compacting, then monkey is put into big crucible, fill full high temperature resistant powder and compacting in the gap of two crucibles, at last big crucible is added a cover, wherein high temperature resistant powder is selected aluminum oxide powder, magnesia powder, zirconia powder or activated carbon powder commonly used.In monkey, by residual air in the excessive S reaction monkey, form reducing atmosphere, prevent that synthetic product is oxidized in high temperature air.
5. step is for the abundant excessive Li of flush away
2CO
3(or Na
2CO
3Or K
2CO
3) and reaction intermediate Li
2S
x(or Na
2S
xOr K
2S
x).
Beneficial effect:
1. the conversion of white light material is under the laser excitation of 980nm wavelength on the three doping oxysulfides that synthesize of the present invention, and luminous intensity can reach 10
6The order of magnitude, on change RGB light intensity ratio near 1: 1: 1.This material can produce efficient white light as last conversion of white light material.
2. synthetic method of the present invention is simple, has avoided creating with expensive device such as atmosphere furnace the reducing atmosphere of this material of preparation, has saved production cost; Last handling process is simple and convenient, and is time saving and energy saving.
Embodiment
The present invention is further illustrated below in conjunction with embodiment, but should not limit protection scope of the present invention with this.
The present invention synthesizes (Ln with the molten method of sulphur
1-x-y-zYb
xTm
yRE
z)
2O
25 specific embodiments of S (wherein x=0.04～0.1, y=0.005～0.01, z=0.005～0.01) are as shown in table 1:
Table 1
Embodiment 1
#:
Form as in the table 11
#Shown in, concrete preparation method comprises the following steps:
1. take by weighing 0.95molLa by mole per-cent
2O
3, 0.04molYb
2O
3, 0.005molTm
2O
3, 0.005molEr
2O
3, 1.5molLi
2CO
3, the 3.5mol sublimed sulphur;
2. the raw material that weighs up is mixed; The raw material that mixes is packed in the set crucible with cover, fill alumina powder and compacting in the gap of two crucibles;
The set crucible that 3. compound will be housed is warmed up to 350 ℃ with 3 ℃/min, and insulation 1h, then is warmed up to 1050 ℃ with 3 ℃/min, and insulation 5h, is cooled to room temperature with stove then;
4. will synthesize block product and directly put into beaker, use the deionized water filtering and washing;
5. at last product being put into the constant temperature air dry oven dries.
Test result to conversion of white light material on this three doping oxysulfide is as follows:
With process 5. in after the oven dry powder with X-ray diffractometer (XRD D/Max2500) carries out the phase composite analysis, the position that the result shows main diffraction peak all with six side La
2O
2S is corresponding, and does not have the peak of other material phases to exist.Powder is carried out compressing tablet, and (Horiba Jobin Yvon FL3-221), is excitation wavelength with 980nm laser, carries out the emmission spectrum test in 400～800nm wavelength region, and the luminous intensity of the spectrum that records can reach 10 to adopt fluorescence spectrophotometer
6The order of magnitude, on change RGB light intensity ratio near 1: 1: 1.The emmission spectrum that records is carried out the chromaticity coordinates match, and the result is x=0.2416, y=0.3305, nearly white light.
Embodiment 2
#:
Form as in the table 12
#Shown in, concrete preparation method comprises the following steps:
1. take by weighing 0.2molLa by mole per-cent
2O
3+ 0.7275mol Y
2O
3, 0.06molYb
2O
3, 0.0075molTm
2O
3, 0.005molEr
2O
3, 0.5molLi
2CO
3+ 1molNa
2CO
3With the 3.5mol sublimed sulphur;
2. the raw material that weighs up is mixed; The raw material that mixes is packed in the set crucible with cover, fill magnesium oxide powder and compacting in the gap of two crucibles;
The set crucible that 3. compound will be housed is warmed up to 300 ℃ with 2 ℃/min, and insulation 1h, then is warmed up to 1100 ℃ with 3.5 ℃/min, and insulation 3h, is cooled to room temperature with stove then;
4. will synthesize block product and directly put into beaker, use the deionized water filtering and washing;
5. at last product being put into the constant temperature air dry oven dries.
Test result to conversion of white light material on this three doping oxysulfide is as follows:
Process 5. middle product is Y
2O
2The S pure phase, the luminous intensity of the spectrum that records can reach 10
6The order of magnitude, on change RGB light intensity ratio near 1: 1: 1.The chromaticity coordinates fitting result is x=0.2556, y=0.3298, nearly white light.。
Embodiment 3
#:
Form as in the table 13
#Shown in, concrete preparation method comprises the following steps:
1. take by weighing 0.9155molY by mole per-cent
2O
3, 0.07molYb
2O
3, 0.0075molTm
2O
3, 0.007mol Ho
2O
3, 1molNa
2CO
3+ 0.75molK
2CO
3With the 4mol sublimed sulphur;
2. the raw material that weighs up is mixed; The raw material that mixes is packed in the set crucible with cover, fill Zirconium oxide powder and compacting in the gap of two crucibles;
The set crucible that 3. compound will be housed is warmed up to 320 ℃ with 2.5 ℃/min, and insulation 1.5h, then is warmed up to 1150 ℃ with 3 ℃/min, and insulation 5h, is cooled to room temperature with stove then;
4. will synthesize block product and directly put into beaker, use the deionized water filtering and washing;
5. at last product being put into the constant temperature air dry oven dries.
Test result to conversion of white light material on this three doping oxysulfide is as follows:
Process 5. middle product is Y
2O
2The S pure phase, the luminous intensity of the spectrum that records can reach 10
6The order of magnitude, on change RGB light intensity ratio near 1: 1: 1.The chromaticity coordinates fitting result is x=0.3078, y=0.3225, nearly white light.。
Embodiment 4
#:
Form as in the table 14
#Shown in, concrete preparation method comprises the following steps:
1. take by weighing 0.901molGd by mole per-cent
2O
3, 0.08molYb
2O
3, 0.01molTm
2O
3, 0.009mol Eu
2O
3, 1.75molK
2CO
3With the 4mol sublimed sulphur;
2. the raw material that weighs up is mixed; The raw material that mixes is packed in the set crucible with cover, fill activated carbon powder and compacting in the gap of two crucibles;
The set crucible that 3. compound will be housed is warmed up to 330 ℃ with 3 ℃/min, and insulation 1.5h, then is warmed up to 1200 ℃ with 3.5 ℃/min, and insulation 4h, is cooled to room temperature with stove then;
4. will synthesize block product and directly put into beaker, use the deionized water filtering and washing;
5. at last product being put into the constant temperature air dry oven dries.
Test result to conversion of white light material on this three doping oxysulfide is as follows:
Process 5. middle product is Gd
2O
2The S pure phase, the luminous intensity of the spectrum that records can reach 10
6The order of magnitude, on change RGB light intensity ratio near 1: 1: 1.The chromaticity coordinates fitting result is x=0.2957, y=0.3129, nearly white light.
Embodiment 5
#:
Form as in the table 15
#Shown in, concrete preparation method comprises the following steps:
1. take by weighing 0.176molLa by mole per-cent
2O
3+ 0.528molY
2O
3+ 0.176molGd
2O
3, 0.1molYb
2O
3, 0.01molTm
2O
3, 0.01mol Ho
2O
3, 0.5mol Li
2CO
3+ 1molNa
2CO
3+ 0.5molK
2CO
3With the 4.5mol sublimed sulphur;
2. the raw material that weighs up is mixed; The raw material that mixes is packed in the set crucible with cover, fill alumina powder and compacting in the gap of two crucibles;
The set crucible that 3. compound will be housed is warmed up to 300 ℃ with 2 ℃/min, and insulation 2h, then is warmed up to 1250 ℃ with 3 ℃/min, and insulation 5h, is cooled to room temperature with stove then;
4. will synthesize block product and directly put into beaker, use the deionized water filtering and washing;
5. at last product being put into the constant temperature air dry oven dries.
Test result to conversion of white light material on this three doping oxysulfide is as follows:
Process 5. middle product is Y
2O
2The S pure phase, the luminous intensity of the spectrum that records can reach 10
6The order of magnitude, on change RGB light intensity ratio near 1: 1: 1.The chromaticity coordinates fitting result is x=0.3278, y=0.3321, nearly white light.
Claims (2)
1. conversion of white light material on the doping oxysulfide, the structural formula that it is characterized in that material is (Ln
1-x-y-zYb
xTm
yRE
z)
2O
2S, wherein x=0.04～0.1, y=0.005～0.01, z=0.005～0.01; Its raw material is Ln
2O
3, sensitizing agent, activator and fusing assistant, wherein Ln
2O
3Be at least La
2O
3, Y
2O
3Or Gd
2O
3In a kind of; Sensitizing agent is Yb
2O
3Activator is Tm
2O
3And RE
2O
3, RE wherein
2O
3Be Er
2O
3, Ho
2O
3Or Eu
2O
3In a kind of; Fusing assistant is AL
2CO
3And sublimed sulphur, wherein AL
2CO
3Be at least Li
2CO
3, Na
2CO
3Or K
2CO
3In a kind of; The wherein mole number of sublimed sulphur and Ln
2O
3, sensitizing agent and activator the ratio of total mole number be 3.5～4.5:1, AL
2CO
3Mole number with and Ln
2O
3, sensitizing agent and activator the ratio of total mole number be 1.5～2:1.
2. one kind prepares the method that goes up the conversion of white light material as claimed in claim 1, and its step is as follows:
1. take by weighing desired raw material, the raw material that weighs up is mixed;
2. the raw material that mixes is packed in the set crucible with cover, fill high temperature resistant powder and compacting in the gap of two crucibles;
The crucible that 3. compound will be housed is warmed up to 300～350 ℃ with 2～3 ℃/min of temperature rise rate, and insulation 1h～2h, is warmed up to 1050～1250 ℃ with 3～3.5 ℃/min of temperature rise rate then, and insulation 3h～5h, is cooled to room temperature with stove then;
4. the product behind the sintering also stirs with hot wash, suction filtration;
5. the product after will washing is put into the constant temperature air dry oven dries, and obtains the conversion of white light material.
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|---|---|---|---|
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|---|---|---|---|
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|---|---|---|---|---|
| CN102618284B (en) * | 2012-03-15 | 2014-10-01 | 吉林大学 | Bioluminescent nanoparticle with 800-nanometer strong near infrared up-conversion emission characteristic and application thereof |
| CN102703080B (en) * | 2012-06-12 | 2014-04-16 | 华东理工大学 | Sulfur oxide high-efficiency infrared up-conversion fluorescent powder and preparation method thereof |
| CN103849399B (en) * | 2012-11-29 | 2016-04-20 | 海洋王照明科技股份有限公司 | oxysulfide luminescent material and preparation method thereof |
| CN105602564B (en) * | 2016-03-03 | 2017-11-07 | 盐城工学院 | A kind of enhanced rare-earth oxide sulfate up-conversion luminescent material of Zn and preparation method |
| CN106929019B (en) * | 2017-03-13 | 2019-08-23 | 盐城工学院 | A kind of preparation method of multiple spectra response luminescent material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730608A (en) * | 2004-09-27 | 2006-02-08 | 中国科学院长春光学精密机械与物理研究所 | The purple light of violet light diode is converted to the rare-earth trichromatic luminescent material of white light |
| CN101724397A (en) * | 2009-11-26 | 2010-06-09 | 哈尔滨工业大学 | Rare-earth doped bismuth titanate up-conversion luminescence nanometer crystal material |
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2011
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730608A (en) * | 2004-09-27 | 2006-02-08 | 中国科学院长春光学精密机械与物理研究所 | The purple light of violet light diode is converted to the rare-earth trichromatic luminescent material of white light |
| CN101724397A (en) * | 2009-11-26 | 2010-06-09 | 哈尔滨工业大学 | Rare-earth doped bismuth titanate up-conversion luminescence nanometer crystal material |
Non-Patent Citations (2)
| Title |
|---|
| 掺铥硫氧化钇的特殊余辉性质;雷炳富等;《高等学校化学学报》;20030615;第24卷(第05期);782-784 * |
| 雷炳富等.掺铥硫氧化钇的特殊余辉性质.《高等学校化学学报》.2003,第24卷(第05期),782-784. |
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