CN104762084A - Preparation method of jellyfish-like rare-earth-doped MoO3 green upconversion luminescent material - Google Patents
Preparation method of jellyfish-like rare-earth-doped MoO3 green upconversion luminescent material Download PDFInfo
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- CN104762084A CN104762084A CN201510167161.4A CN201510167161A CN104762084A CN 104762084 A CN104762084 A CN 104762084A CN 201510167161 A CN201510167161 A CN 201510167161A CN 104762084 A CN104762084 A CN 104762084A
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Abstract
The invention relates to a preparation method of a jellyfish-like rare-earth-doped MoO3 green upconversion luminescent material, which comprises the following steps: weighing a raw material MoO3 and rare-earth salt, wherein all the raw material is solid crystal powder; uniformly mixing the weighed materials by grinding, adding into an aluminum oxide crucible, covering a monocrystalline silicon chip on the crucible as a substrate, putting into a muffle furnace, heating to 1000-1250 DEG C in an air atmosphere at the rate of 5-20 DEG C/minute, and keeping the temperature for 1-2 hours; and after finishing keeping the temperature, carrying out furnace cooling to room temperature, and taking out the monocrystalline silicon chip, wherein the jellyfish-like rare-earth-doped molybdenum oxide green upconversion luminescent material is deposited on the silicon chip. The product is a rare-earth-doped MoO3 luminescent material with special shape and efficient upconversion luminescence characteristic, and can obtain efficient green upconversion luminescence under the excitation of a 980nm-wavelength laser. The method has the advantages of simple preparation technique and low cost, and is suitable for mass production.
Description
Technical field the present invention relates to a kind of preparation method of rear-earth-doped oxide compound up-conversion luminescent material.
Background technology up-conversion luminescence is, by multi-photon mechanism, long-wave radiation is converted to short-wave radiation, and the photon energy namely absorbed is lower than the photon energy of launching.Up-conversion luminescent material can launch visible ray under ir radiation excites, at the various camera techniques of display video picture, optoelectronics device, new light sources, X-ray intensifying screen, nuclear physics, the detection of radiation field and record, medical radiology image, the fields such as printing mark is false proof, optical sensing, all solidstate short wavelength laser and biological label are with a wide range of applications.Rare earth element, because of the electron structure of its uniqueness, has the spectral quality that general element is incomparable, makes rare earth become a huge luminous treasure-house, for new and high technology provides luminescence and the laserable material of many superior performances.At present, also rare-earth-doped fluoride material is mainly concentrated on to the research of rear-earth-doped up-conversion luminescent material, and matrix of oxide have good mechanical performance, Stability Analysis of Structures, damage threshold and preparation technology is simple, high being more suitable for of productive rate is produced and the advantage such as application.Its weak point: the phonon energy that oxide compound is higher makes to be that the rear-earth-doped luminous material luminous efficiency of matrix is low with oxide compound, and the more difficult control of its microscopic appearance.
It is more easy to control that summary of the invention the object of this invention is to provide a kind of microscopic appearance, and preparation technology is simple, with low cost, is applicable to the rear-earth-doped MoO of jellyfish shape of batch production
3the preparation method of green up conversion luminescent material.
The present invention is a kind of rear-earth-doped MoO mixing the jellyfish shape at high temperature obtained by Using Gas Evaporation Method with compound and the rare-earth salts containing molybdenum with certain mass ratio
3efficient green up-conversion luminescent material.
The rear-earth-doped MoO of above-mentioned jellyfish shape
3the preparation method of green up conversion luminescent material is as follows:
(1) MoO is taken
3starting material and rare-earth salts, wherein, MoO
3starting material are Ammonium Heptamolybdate (NH
4)
6mo
7o
244H
2o, positive ammonium molybdate (NH
4)
2moO
4, ammonium dimolybdate (NH
4)
2mo
2o
7or ammonium tetramolybdate (NH
4)
2mo
4o
132H
2o, rare-earth salts is Erbium trinitrate Er (NO
3)
35H
2o and ytterbium nitrate Yb (NO
3)
35H
2o, Erbium trichloride ErCl
36H
2o and Ytterbium trichloride YbCl
36H
2o or Erbium trioxide Er
2o
3with ytterbium oxide Yb
2o
3deng, all raw materials are solid crystal powder;
(2) by the above-mentioned material taken through grinding be mixed after, load alumina crucible, crucible is coated with monocrystalline silicon piece as substrate, then retort furnace is put into together, rise to 1000 DEG C ~ 1250 DEG C with the speed of 5 DEG C/min ~ 20 DEG C/min in air atmosphere, and keep 1 ~ 2 hour in this temperature;
(3) insulation terminates rear furnace cooling, to be cooledly to room temperature, takes out monocrystalline silicon piece, and namely what silicon chip deposited is the rear-earth-doped oxidation molybdenum green up conversion luminescent material of jellyfish shape.
Rare earth Er ion doping MoO of the present invention
3efficient green up-conversion luminescent material is a kind of disc self-organizing structures with jellyfish form of autonomous growth under non-equilibrium condition, and disc centre has the octahedra MoO of well-crystallized
3particle clusters, cluster outer by the center of circle to circumference along radial direction MoO
3particle size reduces gradually.Under hot conditions, ammonium molybdate decomposes, and is taken out of by part rare earth ion and be deposited on monocrystalline silicon sheet surface to form rear-earth-doped MoO in evaporative process
3material.Because rare earth ion Yb is the effective sensitizing agent of Er ion, thus efficient up-conversion luminescence can be obtained under 980nm wavelength laser excites.
The present invention compared with prior art tool has the following advantages:
(1) product of the present invention is a kind of rear-earth-doped MoO with efficient Upconversion luminescence with special appearance
3luminescent material, it can obtain efficient green up-conversion luminescence under 980nm wavelength laser excites;
(2) preparation technology of the present invention is simple, with low cost, is applicable to batch production.
Accompanying drawing explanation
The electron scanning micrograph figure of the luminescent material of Fig. 1 prepared by the embodiment of the present invention 1;
The electron scanning micrograph figure of the luminescent material localized micro tissue of Fig. 2 prepared by the embodiment of the present invention 1;
The X-ray diffraction spectrogram of the luminescent material of Fig. 3 prepared by the embodiment of the present invention 1;
The electronic probe figure of the luminescent material of Fig. 4 prepared by the embodiment of the present invention 1;
The light micrograph figure of the luminescent material of Fig. 5 prepared by the embodiment of the present invention 1 under natural light and 976nm laser radiation;
The luminescent spectrum figure of the luminescent material of Fig. 6 prepared by the embodiment of the present invention 1 under 976nm laser excitation.
Embodiment
In the mode of specific embodiment, the invention will be further described below:
Embodiment 1
(1) 10g Ammonium Heptamolybdate (NH is taken
4)
6mo
7o
244H
2o, 0.2g Erbium trinitrate Er (NO
3)
35H
2o and 1.8g ytterbium nitrate Yb (NO
3)
35H
2o, all raw materials are solid crystal powder;
(2) by the above-mentioned material taken after fully grinding is mixed, load alumina crucible, then cover monocrystalline silicon piece at mouth of pot and put into retort furnace together, rising to 1250 DEG C with the speed of 5 DEG C/min in air atmosphere, and keep 1 hour in this temperature;
(3) terminate to take out monocrystalline silicon piece after furnace cooling until insulation, namely obtain rare earth Er and the ion co-doped MoO of Yb of jellyfish shape at monocrystalline silicon sheet surface
3green up conversion luminescent material.
As can be seen from the luminescent material electron scanning micrograph figure prepared by the present embodiment shown in Fig. 1, obtained luminescent material be diameter at about 150nm, the disk presenting plane jellyfish shape, disc centre has macrobead to exist.Some disk independent distribution, some disk overlaps, and has obvious line of delimitation in the place of overlap.As can be seen from the electron scanning micrograph figure of the localized micro tissue of the luminescent material prepared by the present embodiment shown in Fig. 2, from disc centre along radial direction outward, grain-size reduces gradually.As can be seen from the X-ray diffraction spectrogram of the luminescent material prepared by the present embodiment shown in Fig. 3, except the diffraction peak of silicon single crystal, all the other diffraction peaks all correspond to square phase MoO
3, because Er and the Yb ion of doping is less, there is not the diffraction peak containing Er and Yb compound.As can be seen from the electronic probe figure of the luminescent material prepared by the present embodiment shown in Fig. 4, disk is elementary composition by Mo and O, and the content due to Er and Yb fails to detect the distribution of Er and Yb very little.As can be seen from the light micrograph figure of the luminescent material prepared by the present embodiment shown in Fig. 5 under natural light and 976nm laser radiation, launch obvious visible ray at 976nm laser excitation lower disc, and light-emitting zone and disk one_to_one corresponding.As can be seen from the luminescent spectrum figure of the luminescent material prepared by the present embodiment shown in Fig. 6 under 976nm laser excitation, under 976nm laser excitation, it is luminous that disk launches ultraviolet, blueness, green, redness and infrared up conversion respectively in 300nm ~ 900nm wavelength band, corresponds respectively to Er
3+ion
2h
9/2→
4i
15/2,
4f
5/2→
4i
15/2,
2h
11/2→
4i
15/2,
4s
3/2→
4i
15/2,
4f
9/2→
4i
15/2with
4s
3/2→
4i
13/2transition, wherein the strongest in the Green upconversion luminescent of 500nm ~ 580nm.
Embodiment 2
(1) the positive ammonium molybdate (NH of 10g is taken
4)
2moO
4, 0.2g Erbium trichloride ErCl
36H
2o and 1.8g Ytterbium trichloride YbCl
36H
2o, all raw materials are solid crystal powder;
(2) by the above-mentioned material taken after fully grinding is mixed, load alumina crucible, then cover monocrystalline silicon piece at mouth of pot and put into retort furnace together, rising to 1100 DEG C with the speed of 15 DEG C/min in air atmosphere, and keep 1.5 hours in this temperature;
(3) terminate to take out monocrystalline silicon piece after furnace cooling until insulation, namely obtain rare earth Er and the ion co-doped MoO of Yb of jellyfish shape at monocrystalline silicon sheet surface
3green up conversion luminescent material.
Embodiment 3
(1) 10g ammonium tetramolybdate (NH is taken
4)
2mo
4o
132H
2o, 0.2g Erbium trioxide Er
2o
3with 1.8g ytterbium oxide Yb
2o
3, all raw materials are solid crystal powder;
(2) by the above-mentioned material taken after fully grinding is mixed, load alumina crucible, then cover monocrystalline silicon piece at mouth of pot and put into retort furnace together, rising to 1000 DEG C with the speed of 20 DEG C/min in air atmosphere, and keep 2 hours in this temperature;
(3) terminate to take out monocrystalline silicon piece after furnace cooling until insulation, namely obtain rare earth Er and the ion co-doped MoO of Yb of jellyfish shape at monocrystalline silicon sheet surface
3green up conversion luminescent material.
Claims (1)
1. the rear-earth-doped MoO of jellyfish shape
3the preparation method of green up conversion luminescent material, is characterized in that:
(1) MoO is taken
3starting material and rare-earth salts, wherein, MoO
3starting material are Ammonium Heptamolybdate (NH
4)
6mo
7o
244H
2o, positive ammonium molybdate (NH
4)
2moO
4, ammonium dimolybdate (NH
4)
2mo
2o
7or ammonium tetramolybdate (NH
4)
2mo
4o
132H
2o, rare-earth salts is Erbium trinitrate Er (NO
3)
35H
2o and ytterbium nitrate Yb (NO
3)
35H
2o, Erbium trichloride ErCl
36H
2o and Ytterbium trichloride YbCl
36H
2o or Erbium trioxide Er
2o
3with ytterbium oxide Yb
2o
3deng, all raw materials are solid crystal powder;
(2) by the above-mentioned material taken through grinding be mixed after, load alumina crucible, crucible is coated with monocrystalline silicon piece as substrate, then retort furnace is put into together, rise to 1000 DEG C ~ 1250 DEG C with the speed of 5 DEG C/min ~ 20 DEG C/min in air atmosphere, and keep 1 ~ 2 hour in this temperature;
(3) insulation terminates rear furnace cooling, to be cooledly to room temperature, takes out monocrystalline silicon piece, and namely what silicon chip deposited is the rear-earth-doped oxidation molybdenum green up conversion luminescent material of jellyfish shape.
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|---|---|---|---|
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|---|---|---|---|
| CN201510167161.4A CN104762084A (en) | 2015-04-10 | 2015-04-10 | Preparation method of jellyfish-like rare-earth-doped MoO3 green upconversion luminescent material |
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ID=53644189
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778911A (en) * | 2016-04-01 | 2016-07-20 | 大连民族大学 | Rare-earth doped photoluminescence material by using YbMoO4 as substrate and preparation method thereof |
| CN110079315A (en) * | 2019-04-08 | 2019-08-02 | 昆明理工大学 | A kind of thermochromism MoO3: Yb, Er up-conversion phosphor, preparation method and its reversible regulation method of up-conversion luminescence |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103555329A (en) * | 2013-11-07 | 2014-02-05 | 韦胜国 | Preparation method of LED (Light Emitting Diode) red fluorescent powder |
| CN104371715A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Water-soluble molybdenum trioxide up-conversion nanometer material and preparation method thereof |
-
2015
- 2015-04-10 CN CN201510167161.4A patent/CN104762084A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103555329A (en) * | 2013-11-07 | 2014-02-05 | 韦胜国 | Preparation method of LED (Light Emitting Diode) red fluorescent powder |
| CN104371715A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Water-soluble molybdenum trioxide up-conversion nanometer material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 徐叙瑢著: "发光材料的制备", 《发光学与发光材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778911A (en) * | 2016-04-01 | 2016-07-20 | 大连民族大学 | Rare-earth doped photoluminescence material by using YbMoO4 as substrate and preparation method thereof |
| CN110079315A (en) * | 2019-04-08 | 2019-08-02 | 昆明理工大学 | A kind of thermochromism MoO3: Yb, Er up-conversion phosphor, preparation method and its reversible regulation method of up-conversion luminescence |
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Application publication date: 20150708 |