CN105255496A - Up-conversion luminescent material and preparing method thereof - Google Patents
Up-conversion luminescent material and preparing method thereof Download PDFInfo
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- CN105255496A CN105255496A CN201510704277.7A CN201510704277A CN105255496A CN 105255496 A CN105255496 A CN 105255496A CN 201510704277 A CN201510704277 A CN 201510704277A CN 105255496 A CN105255496 A CN 105255496A
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- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000001556 precipitation Methods 0.000 claims description 13
- 238000009413 insulation Methods 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000005352 clarification Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- -1 rare earth ions Chemical class 0.000 abstract description 7
- 230000005284 excitation Effects 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 239000003086 colorant Substances 0.000 abstract description 3
- 239000013049 sediment Substances 0.000 abstract 3
- 239000006184 cosolvent Substances 0.000 abstract 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 abstract 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000004020 luminiscence type Methods 0.000 description 5
- 229910052688 Gadolinium Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012716 precipitator Substances 0.000 description 3
- 238000003836 solid-state method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 229910052775 Thulium Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006862 quantum yield reaction Methods 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The invention relates to an up-conversion luminescent material and a preparing method thereof and belongs to the technical field of luminescent materials. The general formula of the material is Gd2-y-zO3-xSx:Ery3+, Mzn+, wherein 0<=x<=1, 0.01<=y<=0.2, 0.01<=z<=0.12, and Mn+ is Tm3+ and/or Tb3+ rare earth ions or Li+. At first, Gd2O3 and Er2O3 are mixed uniformly according to the stoichiometric ratio of the material to obtain a mixture, and then the mixture is added into a salpeter solution to be mixed to prepare sediment; the prepared sediment is dried and ground, then elemental sulfur, or other raw materials and cosolvent NaCO3 are added into the sediment according to the stoichiometric ratio, the vacuum degree is 0.1-10 Pa, temperature is 700 DEG C-1100 DEG C, and the temperature is kept for 2-5 h, so that the Gd2-y-zO3-xSx:Ery3+, Mzn+ luminescent material is prepared, wherein 0<=x<=1, 0.01<=y<=0.2, 0.01<=z<=0.12. The particle size of the prepared up-conversion luminescent material ranges from about 100 nanometers to about 10 micrometers, and light of different colors can be emitted under near UV excitation.
Description
Technical field
The present invention relates to a kind of up-conversion luminescent material and preparation method thereof, belong to luminescent material technical field.
Background technology
In optical frequency, conversion is method very important in physics, and the materials and devices based on upper transfer principle has very important application prospect in laser, communication, the energy, medical treatment, military affairs, aerospace and people's daily life.Upper switch technology should obtain application widely in a lot of fields, but at present, due to the restriction of production technology aspect, a lot of product does not reach the requirement needed for up-conversion luminescence.
Recent years, the up-conversion of research was various, and its shape phase is also varied.Such as glass, pottery, monocrystalline and polycrystal powder etc., its chemical combination consists of oxide compound, fluorochemical, sulfide, oxysulfide and oxyhalogenide etc.And rare-earth oxide sulfate has lower phonon energy (200-300cm relative to fluorochemical
-1), physicochemical property are stablized, and excitation intensity requires relatively low.
The production method that comparative maturity prepared by current fluorescent material has high temperature solid-state method and the precipitator method, but high temperature solid-state method and the precipitator method all also exist respective shortcoming.High temperature solid-state method long reaction time, the temperature of needs is high, and crystal grain is thick, and process is wayward; Precipitator method crystallization is poor, causes luminous efficiency poor.Therefore the luminous efficiency that production method can improve rare earth luminescent material is improved further.This invention proposes under vacuum, by the formation of Crystal Growth Mechanism and impurity phase under its conditions of research such as control vacuum tightness, temperature, soaking time, and the volatilization situation etc. of sulphur.What under vacuum condition, synthesis can be very fast reaches temperature required, and preparation particle size is less, is conducive to the practical application of this kind of luminescent material.
The present invention is preparing rare-earth oxide sulfate (Gd
2o
2s) on single-matrix basis, designing a kind ofly has the material of wider absorption band to turn light to assist rare earth ion for sunlight, light in the broadband range utilizing this absorbed not to be utilized, then by transmission ofenergy to rare earth ion, light is converted to the light that can be utilized by rare earth ion again, thus makes erbium ion in this substrate material, realize broadband to turn light with collaborative luminous.
Summary of the invention
For above-mentioned prior art Problems existing and deficiency, the invention provides a kind of up-conversion luminescent material and preparation method thereof.The up-conversion luminescent material that the present invention prepares has the particle diameter of about 100 nanometers to about 10 microns, and under near ultraviolet excitation, realize the luminescence of different colours, compared with other materials, its crystalline structure and luminescent properties more excellent, quantum yield is high, and be more suitable for actual application, the present invention is achieved through the following technical solutions.
A kind of up-conversion luminescent material, this material general formula is Gd
2-y-zo
3-xs
x: Er
y 3+, M
z n+, wherein 0≤x≤1,0.01≤y≤0.2,0.01≤z≤0.12, M
n+for Tm
3+and/or Tb
3+rare earth ion, or Li
+.
A preparation method for up-conversion luminescent material, its concrete steps are as follows:
(1) first by Gd
2o
3and Er
2o
3mix according to the stoichiometric ratio of material and obtain compound, then add in salpeter solution and mix, at temperature is 90 ~ 120 DEG C, be stirred to solution clarification, then add LiOH precipitation agent until pH be 12, sealing thermal insulation 2h, finally prepare throw out after cleaning;
(2) according to measuring than adding elemental sulfur and solubility promoter NaCO after throw out oven dry step (1) prepared, grinding
3, vacuum tightness be 0.1 ~ 10Pa, temperature be 700 ~ 1100 DEG C of conditions under insulation 2 ~ 5h prepare Gd
2-y-zo
3-xs
x: Er
y 3+, M
z n+luminescent material, wherein 0≤x≤1,0.01≤y≤0.2,0.01≤z≤0.12, M
n+for Li
+.
In described step (1), the concentration of salpeter solution is 0.8 ~ 1.8mol/l.
Solubility promoter NaCO in described step (2)
3add-on be 20 ~ 50% of throw out quality.
A preparation method for up-conversion luminescent material, its concrete steps are as follows:
(1) first by Gd
2o
3and Er
2o
3mix according to the stoichiometric ratio of material and obtain compound, add in salpeter solution and mix, at temperature is 90 ~ 120 DEG C, is stirred to solution clarification, then add precipitation agent until pH be 12, sealing thermal insulation 2h, finally prepare throw out after cleaning;
(2) according to measuring than adding elemental sulfur, Tm after throw out oven dry step (1) prepared, grinding
2o
3and/or Tb
2o
3, solubility promoter NaCO
3, vacuum tightness be 0.1 ~ 30Pa, temperature be 700 ~ 1100 DEG C of conditions under insulation 2 ~ 5h prepare Gd
2-y-zo
3-xs
x: Er
y 3+, M
z n+luminescent material, wherein 0≤x≤1,0.01≤y≤0.2,0.01≤z≤0.12, M
n+for Tm
3+and/or Tb
3+rare earth ion.
In described step (1), the concentration of salpeter solution is 0.8 ~ 1.8mol/l.
In described step (1), precipitation agent is NaOH.
Solubility promoter NaCO in described step (2)
3add-on be 20 ~ 50% of throw out quality.
The invention has the beneficial effects as follows:
(1) up-conversion luminescent material that the present invention prepares has the particle diameter of about 100 nanometers to about 10 microns, and under near ultraviolet excitation, realizes the luminescence of different colours, compared with other materials, its crystalline structure and luminescent properties more excellent, quantum yield is high, is more suitable for actual application;
(2) method of the present invention is compared with additive method, and it is more even that co-precipitation makes dopant ion distribute, and vacuum solid state reaction makes temperature of reaction obviously reduce, and the crystalline structure and the luminescent properties that are conducive to raising material also can be cost-saving.
Accompanying drawing explanation
Fig. 1 is the Gd that the embodiment of the present invention 1 prepares
1.75o
2s:Er
0.2 3+ ,li
0.05 +up-conversion luminescence spectrogram under 980nm wavelength excites.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
This up-conversion luminescent material, this materials chemistry formula is Gd
1.75o
2s:Er
0.2 3+ ,li
0.05 +.
The preparation method of this up-conversion luminescent material, its concrete steps are as follows:
(1) first by Gd
2o
3and Er
2o
3be that 0.875:0.1 mixes and obtains 5g compound according to mol ratio, then mixing in 250mL salpeter solution (concentration is 0.8mol/l) is joined, solution clarification is stirred at temperature is 120 DEG C, then add LiOH precipitation agent until pH be 12, sealing thermal insulation 2h, finally prepare throw out after cleaning;
(2) throw out that step (1) prepared is dried, be that 1.75:1 adds elemental sulfur and solubility promoter NaCO according to the mol ratio of Gd and S in throw out after grinding
3(solubility promoter NaCO
3add-on be 50% of throw out quality, vacuum tightness be 10Pa, temperature is incubated 2h under being 1100 DEG C of conditions and prepares Gd
1.75o
2s:Er
0.2 3+ ,li
0.05 +luminescent material.
The Gd that the present embodiment prepares
1.75o
2s:Er
0.2 3+ ,li
0.05 +as shown in Figure 1, this material has obvious utilizing emitted light to the up-conversion luminescence spectrogram of luminescent material under 980nm wavelength excites within the scope of ruddiness, green glow and blue light three as can be seen from Figure 1.
Embodiment 2
This up-conversion luminescent material, this materials chemistry formula is Gd
1.84o
2.5s
0.5: Er
0.08 3+, Tm
0.08 3+.
The preparation method of this up-conversion luminescent material, its concrete steps are as follows:
(1) first by Gd
2o
3and Er
2o
3mix according to mol ratio 0.92:0.04 and obtain 10g compound, then mixing in 150mL salpeter solution (concentration is 1.8mol/l) is joined, solution clarification is stirred at temperature is 90 DEG C, then add precipitation agent until pH be 12, sealing thermal insulation 2h, finally prepare throw out after cleaning; Wherein precipitation agent is NaOH;
(2) elemental sulfur, Tm is added according to according to the mol ratio 1.84:0.5:0.04 of Gd, S and Tm in throw out after throw out oven dry step (1) prepared, grinding
2o
3, solubility promoter NaCO
3(solubility promoter NaCO
3add-on be 20% of throw out quality, vacuum tightness be 0.1Pa, temperature is incubated 5h to prepare chemical formula is Gd under being 700 DEG C of conditions
1.84o
2.5s
0.5: Er
0.08 3+, Tm
0.08 3+luminescent material.
Embodiment 3
This up-conversion luminescent material, this materials chemistry formula is Gd
1.76o
2s:Er
0.08 3+, Tm
0.08 3+, Tb
0.08 3+.
The preparation method of this up-conversion luminescent material, its concrete steps are as follows:
(1) first by Gd
2o
3and Er
2o
3mix according to mol ratio 0.88:0.04 and obtain 50g compound, then mixing in 200mL salpeter solution (concentration is 1.5mol/l) is joined, solution clarification is stirred at temperature is 100 DEG C, then add precipitation agent until pH be 12, sealing thermal insulation 2h, finally prepare throw out after cleaning; Wherein precipitation agent is NaOH;
(2) elemental sulfur, Tm is added according to according to the mol ratio 1.76:1:0.04:0.04 of Gd, S, Tm and Tb in throw out after throw out oven dry step (1) prepared, grinding
2o
3, Tb
2o
3, solubility promoter NaCO
3(solubility promoter NaCO
3add-on be 35% of throw out quality), vacuum tightness be 5Pa, temperature is incubated 2.5h to prepare chemical formula is Gd under being 1000 DEG C of conditions
1.76o
2s:Er
0.08 3+, Tm
0.08 3+, Tb
0.08 3+luminescent material.
Embodiment 4
This up-conversion luminescent material, this materials chemistry formula is Gd
1.96o
2s:Er
0.02 3+, Tb
0.02 3+.
The preparation method of this up-conversion luminescent material, its concrete steps are as follows:
(1) first by Gd
2o
3and Er
2o
3mix according to mol ratio 0.98:0.01 and obtain 100g compound, then mixing in 150mL salpeter solution (concentration is 1.2mol/l) is joined, solution clarification is stirred at temperature is 110 DEG C, then add precipitation agent until pH be 12, sealing thermal insulation 2h, finally prepare throw out after cleaning; Wherein precipitation agent is NaOH;
(2) elemental sulfur, Tb is added according to according to the mol ratio 1.96:1:0.01 of Gd, S and Tb in throw out after throw out oven dry step (1) prepared, grinding
2o
3, solubility promoter NaCO
3(solubility promoter NaCO
3add-on be 40% of throw out quality), vacuum tightness be 1Pa, temperature is incubated 3.5h to prepare chemical formula is Gd under being 1100 DEG C of conditions
1.96o
2s:Er
0.02 3+, Tb
0.02 3+luminescent material.
Below by reference to the accompanying drawings the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (8)
1. a up-conversion luminescent material, is characterized in that: this material general formula is Gd
2-y-zo
3-xs
x: Er
y 3+, M
z n+, wherein 0≤x≤1,0.01≤y≤0.2,0.01≤z≤0.12, M
n+for Tm
3+and/or Tb
3+rare earth ion, or Li
+.
2. a preparation method for up-conversion luminescent material according to claim 1, is characterized in that concrete steps are as follows:
(1) first by Gd
2o
3and Er
2o
3mix according to the stoichiometric ratio of material and obtain compound, then add in salpeter solution and mix, at temperature is 90 ~ 120 DEG C, be stirred to solution clarification, then add LiOH precipitation agent until pH be 12, sealing thermal insulation 2h, finally prepare throw out after cleaning;
(2) according to measuring than adding elemental sulfur and solubility promoter NaCO after throw out oven dry step (1) prepared, grinding
3, vacuum tightness be 0.1 ~ 10Pa, temperature be 700 ~ 1100 DEG C of conditions under insulation 2 ~ 5h prepare Gd
2-y-zo
3-xs
x: Er
y 3+, M
z n+luminescent material, wherein 0≤x≤1,0.01≤y≤0.2,0.01≤z≤0.12, M
n+for Li
+.
3. the preparation method of up-conversion luminescent material according to claim 2, is characterized in that: in described step (1), the concentration of salpeter solution is 0.8 ~ 1.8mol/l.
4. the preparation method of up-conversion luminescent material according to claim 2, is characterized in that: solubility promoter NaCO in described step (2)
3add-on be 20 ~ 50% of throw out quality.
5. a preparation method for up-conversion luminescent material according to claim 1, is characterized in that concrete steps are as follows:
(1) first by Gd
2o
3and Er
2o
3mix according to the stoichiometric ratio of material and obtain compound, add in salpeter solution and mix, at temperature is 90 ~ 120 DEG C, is stirred to solution clarification, then add precipitation agent until pH be 12, sealing thermal insulation 2h, finally prepare throw out after cleaning;
(2) according to measuring than adding elemental sulfur, Tm after throw out oven dry step (1) prepared, grinding
2o
3and/or Tb
2o
3, solubility promoter NaCO
3, vacuum tightness be 0.1 ~ 30Pa, temperature be 700 ~ 1100 DEG C of conditions under insulation 2 ~ 5h prepare Gd
2-y-zo
3-xs
x: Er
y 3+, M
z n+luminescent material, wherein 0≤x≤1,0.01≤y≤0.2,0.01≤z≤0.12, M
n+for Tm
3+and/or Tb
3+rare earth ion.
6. the preparation method of up-conversion luminescent material according to claim 5, is characterized in that: in described step (1), the concentration of salpeter solution is 0.8 ~ 1.8mol/l.
7. the preparation method of up-conversion luminescent material according to claim 5, is characterized in that: in described step (1), precipitation agent is NaOH.
8. the preparation method of up-conversion luminescent material according to claim 5, is characterized in that: solubility promoter NaCO in described step (2)
3add-on be 20 ~ 50% of throw out quality.
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|---|---|---|---|
| CN201510704277.7A CN105255496B (en) | 2015-10-27 | 2015-10-27 | A kind of up-conversion luminescent material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510704277.7A CN105255496B (en) | 2015-10-27 | 2015-10-27 | A kind of up-conversion luminescent material and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN105255496A true CN105255496A (en) | 2016-01-20 |
| CN105255496B CN105255496B (en) | 2017-10-27 |
Family
ID=55095434
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112322293A (en) * | 2020-11-09 | 2021-02-05 | 厦门大学 | Multiband oxysulfide elastic stress luminescent material and preparation method thereof |
| CN116515487A (en) * | 2023-04-27 | 2023-08-01 | 长春理工大学 | Gd synthesized by double-carbon reduction 2 O 2 S:Tb 3+ Preparation technology of micron-sized fluorescent material |
-
2015
- 2015-10-27 CN CN201510704277.7A patent/CN105255496B/en active Active
Non-Patent Citations (3)
| Title |
|---|
| TIMUR SH ATABAEV等: "Bifunctional Gd2O3:Er3+ particles with enhanced visible upconversion luminescence", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| W. KUZNIK等: "Changes of fluorescent spectral features after successive rare earth doping of gadolinium oxide powders", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 郭艳艳等: "Li +，Er3 + 共掺杂Gd2O3半透明陶瓷的显微结构与上转换发光研究", 《中国稀土学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112322293A (en) * | 2020-11-09 | 2021-02-05 | 厦门大学 | Multiband oxysulfide elastic stress luminescent material and preparation method thereof |
| CN116515487A (en) * | 2023-04-27 | 2023-08-01 | 长春理工大学 | Gd synthesized by double-carbon reduction 2 O 2 S:Tb 3+ Preparation technology of micron-sized fluorescent material |
| CN116515487B (en) * | 2023-04-27 | 2024-04-09 | 长春理工大学 | Gd synthesized by double-carbon reduction 2 O 2 S:Tb 3+ Preparation technology of micron-sized fluorescent material |
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