CN105950136A - White-light light-emitting material excited by laser light and preparation method thereof - Google Patents
White-light light-emitting material excited by laser light and preparation method thereof Download PDFInfo
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- CN105950136A CN105950136A CN201610363410.1A CN201610363410A CN105950136A CN 105950136 A CN105950136 A CN 105950136A CN 201610363410 A CN201610363410 A CN 201610363410A CN 105950136 A CN105950136 A CN 105950136A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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Abstract
The invention discloses a preparation method of a white-light light-emitting material excited by laser light. The preparation method of the white-light light-emitting material excited by the laser light comprises the following steps of (1), confecting an aqueous solution of Eu<3+>; (2), uniformly mixing a Y-type molecular sieve, silver nitrate powder and the aqueous solution of the Eu<3+> in deionized water, so as to obtain mixed liquor; (3), agitating the mixed liquor, which is obtained in step (2), under a light shielding condition, naturally cooling the agitated mixed liquor to be a room temperature, then washing the mixed liquor, centrifuging the washed mixed liquor, taking a lower product, drying the lower product, then carrying out heat preservation on the lower product for 0.5h to 3h at 500 DEG C to 900 DEG C in air, and naturally cooling the lower product subjected to the heat preservation to be the room temperature, so as to obtain an Ag-Eu codoped material which emits white light under the excitation of the laser light. The invention also discloses the preparation method of the white-light light-emitting material. The white-light light-emitting material excited by the laser light, which is provided by the invention, emits the white light under the excitation of 266nm of laser light, further, is higher in light-emitting intensity, but does not emit the white light under the excitation of a xenon lamp.
Description
Technical field
The present invention relates to luminescent material, particularly to white light emitting material and the preparation side thereof of a kind of laser excitation
Method.
Background technology
White light LEDs (WLED) as forth generation light source is energy-efficient because of it, environmental protection and life-span
The advantages such as length, are considered have a new generation with broad prospects for development lighting engineering.Meanwhile, WLED is again because of tool
The advantages such as colored is Well-recovered, energy consumption is relatively low, have increasingly in LCD backlight source field in recent years
Many application.The main way realizing WLED at present is that blue-light LED chip adds yellow fluorescent powder, which
Technology maturity is higher, advantage of lower cost, but this WLED is disadvantageous in that it is in red light
Spectrum district's luminescence is more weak, and this directly results in, and commercial WLED colour temperature is higher, the problem that color rendering index is relatively low.Profit
Being combined into white light with ultraviolet LED laser as excitaton source excited inorganic luminescent material is another kind of realization the most in vain
The possible approaches of light.But the white light emitting material that Ultra-Violet Laser excites is studied seldom at present.
Summary of the invention
In order to overcome the disadvantages mentioned above of prior art with not enough, it is an object of the invention to provide a kind of laser and swash
The white light emitting material sent out, emits white light under 266nm laser excitation, and luminous intensity is higher, and at xenon lamp
Luminescence under exciting is not white light.
Another object of the present invention is to provide the preparation method of the white light emitting material of a kind of laser excitation, system
Standby condition easily realizes, and preparation process is simple and easy to do.
The purpose of the present invention is achieved through the following technical solutions:
The preparation method of the white light emitting material of a kind of laser excitation, comprises the following steps:
(1) preparation Eu3+Aqueous solution;
(2) by Y type molecular sieve, silver nitrate powder and Eu3+Aqueous solution in deionized water, mix homogeneously,
Obtain mixed liquor;Eu in described mixed liquor3+With Ag+The mol ratio of ion is 0.5~3): 1;
(3) step (2) obtains mixed liquor and stirs under the conditions of lucifuge, washs after naturally cooling to room temperature,
Centrifuging and taking lower floor product, calcines 0.5~3h in 500~900 DEG C in atmosphere after drying, naturally cools to room temperature and obtain
The white light emitting material under laser excitation being co-doped with to Ag-Eu.
Step (1) described Eu3+The aqueous solution that aqueous solution is europium nitrate.
Eu in solution described in step (1)3+'sConcentration is 0.025~0.15mol/L.
Described in step (1), in solution, Y type molecular sieve mass concentration is 0.02~0.04g/mL.
Stirring described in step (3), particularly as follows: stir 12~36h in 60~90 DEG C of constant temperature.
Washing described in step (3), particularly as follows: use deionized water wash 1~3 times.
Step (3) described drying, particularly as follows: dry 6~24h at 60~150 DEG C.
It is incubated 0.5~3h in 500~900 DEG C, particularly as follows: with the speed of 3~10 DEG C/min described in step (3)
It is warming up to 500~900 DEG C, is incubated 0.5~3h.
The white light of the laser excitation that the preparation method of the white light emitting material of described a kind of laser excitation obtains is sent out
Luminescent material, with molecular sieve as substrate, is co-doped with Ag in molecular sieve+And Eu3+Ion.
The luminescence mechanism of the present invention is: under laser excitation, and Ag, Eu ion in the material of the present invention is respectively
Produce green, HONGGUANG, and there is therebetween certain energy transmission, the sample excited compared to xenon lamp,
Under the effect of 266nm laser, laser is easier to arrive in Y type molecular sieve internal structure, thus excites and be in
The Eu of symmetric position (SI, SU)3+, Eu3+The luminescence luminescence relative to Ag can significantly be strengthened,
By changing the ratio that Ag, Eu adulterate in molecular sieve, it is possible to achieve the regulation and control to spectrum, obtain laser and swash
Give the material emitted white light.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) luminescent material that the present invention obtains emits white light under 266nm laser excitation, and luminous intensity is higher,
And the luminescence under xenon lamp excites is not white light, one of key property of white light emitting material of the present invention.
(2) present invention uses Y type molecular sieve, Ag+And Eu3+Ion is raw material, uses simple ion
Two kinds of ions are incorporated in molecular sieve pore passage by exchange method, and preparation condition easily realizes, and preparation process is easy
Easy.
(3) heat treatment temperature of the present invention is only 500~900 DEG C, compared with traditional high temperature solid-state method, and temperature
Relatively low, save the energy.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the white light emitting material being embodiments of the invention gained.
Fig. 2 is the white light emitting material emission spectrum figure of the 266nm laser excitation of embodiments of the invention gained.
Fig. 3 is the white light emitting material emission spectrum figure that the 280nm xenon lamp of embodiments of the invention gained excites.
Fig. 4 is that the white light emitting material luminescent chromaticity of the 266nm laser excitation of embodiments of the invention gained is sat
Mark on a map.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not
It is limited to this.
Embodiment 1
Accurately weigh Y type molecular sieve 1.5g in 100mL conical flask, accurately weigh 0.4247g silver nitrate in
In conical flask, and add the Eu of the 0.2mol/L of 6.25mL3+Aqueous solution, be eventually adding 43.75mL go from
Sub-water, puts into stirring magneton.Conical flask explosion-proof plug is stoppered.Conical flask is put in the beaker of 400mL,
Add a certain amount of water in beaker, with tinfoil beaker wrapped and prevent Ag+Meet light to aoxidize.Beaker is put
On the stainless steel disc of thermostatic mixer, temperature detection probe is immersed in the water through tinfoil with thermometric, constant temperature 80 DEG C
Stirring 12h, naturally cools to room temperature, gained mixed solution and precipitate is transferred in centrifuge tube after stirring,
6000 turns/min is centrifuged 4min.Gained is centrifuged product and is placed in 80 DEG C of drying 12h in baking oven.Product after drying
Thing 5 DEG C/min in air atmosphere is warming up to 800 DEG C, is incubated 1h, naturally cools to room temperature and obtain end product.
The XRD figure of the white light emitting material of the laser excitation that the present embodiment prepares is as shown in Figure 1, it is known that,
Doping Ag+And Eu3+Product after two kinds of ions still remains the crystal structure of molecular sieve.
The white light emitting material that the present embodiment prepares is at emission spectrum figure such as Fig. 2 of 266nm laser excitation
Shown in, it has wide emission peak at about 500nm, and 576nm, 587nm, 617nm, 648nm, 695nm have
Sharp-pointed emission peak, and at 617nm, peak is the most maximum.
The white light emitting material that the present embodiment prepares emission spectrum figure under 280nm xenon lamp excites such as figure
Shown in 3, it has a wider emission peak at 530nm, has a narrower emission peak at 617nm, and the two is strong
Spend the most weak.
The white light emitting material that the present embodiment prepares luminescent chromaticity coordinate diagram under 266nm laser excitation
As shown in Figure 4, it is known that material chromaticity coordinate falls in white light field.
Embodiment 2
Accurately weigh Y type molecular sieve 1.5g in 100mL conical flask, accurately weigh 0.4247g silver nitrate in
In conical flask, and add the Eu of the 0.2mol/L of 18.75mL3+Aqueous solution, be eventually adding 31.25mL go from
Sub-water, puts into stirring magneton.Conical flask explosion-proof plug is stoppered.Conical flask is put in the beaker of 400mL,
Add a certain amount of water in beaker, with tinfoil beaker wrapped and prevent Ag+Meet light to aoxidize.Beaker is put
On the stainless steel disc of thermostatic mixer, temperature detection probe is immersed in the water through tinfoil with thermometric, constant temperature 80 DEG C
Stirring 24h, naturally cools to room temperature, gained mixed solution and precipitate is transferred in centrifuge tube after stirring,
6000 turns/min is centrifuged 4min.Gained is centrifuged product and is placed in 80 DEG C of drying 12h in baking oven.Product after drying
Thing 5 DEG C/min in air atmosphere is warming up to 600 DEG C, is incubated 2h, naturally cools to room temperature and obtain end product.
The XRD figure of the white light emitting material of the laser excitation that the present embodiment prepares is similar with Fig. 1, it is known that,
Doping Ag+And Eu3+Product after two kinds of ions still remains the crystal structure of molecular sieve.
The white light emitting material that the present embodiment prepares is at the emission spectrum figure of 266nm laser excitation and Fig. 2
Similar, it has wide emission peak at about 500nm, and 576nm, 587nm, 617nm, 648nm, 695nm have
Sharp-pointed emission peak, and at 617nm, peak is the most maximum.
The white light emitting material that the present embodiment prepares emission spectrum figure under 280nm xenon lamp excites and figure
3 are similar to, and it has a wider emission peak at 530nm, has a narrower emission peak at 617nm, and the two is strong
Spend the most weak.
The white light emitting material that the present embodiment prepares luminescent chromaticity coordinate diagram under 266nm laser excitation
Similar with Fig. 4, it is known that material chromaticity coordinate falls in white light field.
Embodiment 3
Accurately weigh Y type molecular sieve 1.5g in 100mL conical flask, accurately weigh 0.4247g silver nitrate in
In conical flask, and add the Eu of the 0.2mol/L of 25.00mL3+Aqueous solution, be eventually adding 25.00mL go from
Sub-water, puts into stirring magneton.Conical flask explosion-proof plug is stoppered.Conical flask is put in the beaker of 400mL,
Add a certain amount of water in beaker, with tinfoil beaker wrapped and prevent Ag+Meet light to aoxidize.Beaker is put
On the stainless steel disc of thermostatic mixer, temperature detection probe is immersed in the water through tinfoil with thermometric, constant temperature 70 DEG C
Stirring 36h, naturally cools to room temperature, gained mixed solution and precipitate is transferred in centrifuge tube after stirring,
6000 turns/min is centrifuged 4min.Gained is centrifuged product and is placed in 80 DEG C of drying 12h in baking oven.Product after drying
Thing 5 DEG C/min in air atmosphere is warming up to 600 DEG C, is incubated 3h, naturally cools to room temperature and obtain end product.
The XRD figure of the white light emitting material of the laser excitation that the present embodiment prepares is similar with Fig. 1, it is known that,
Doping Ag+And Eu3+Product after two kinds of ions still remains the crystal structure of molecular sieve.
The white light emitting material that the present embodiment prepares is at the emission spectrum figure of 266nm laser excitation and Fig. 2
Similar, it has wide emission peak at about 500nm, and 576nm, 587nm, 617nm, 648nm, 695nm have
Sharp-pointed emission peak, and at 617nm, peak is the most maximum.
The white light emitting material that the present embodiment prepares emission spectrum figure under 280nm xenon lamp excites and figure
3 are similar to, and it has a wider emission peak at 530nm, has a narrower emission peak at 617nm, and the two is strong
Spend the most weak.
The white light emitting material that the present embodiment prepares luminescent chromaticity coordinate diagram under 266nm laser excitation
Similar with Fig. 4, it is known that material chromaticity coordinate falls in white light field.
Embodiment 4
Accurately weigh Y type molecular sieve 1.5g in 100mL conical flask, accurately weigh 0.4247g silver nitrate in
In conical flask, and add the Eu of the 0.2mol/L of 31.25mL3+Aqueous solution, be eventually adding 18.75mL go from
Sub-water, puts into stirring magneton.Conical flask explosion-proof plug is stoppered.Conical flask is put in the beaker of 400mL,
Add a certain amount of water in beaker, with tinfoil beaker wrapped and prevent Ag+Meet light to aoxidize.Beaker is put
On the stainless steel disc of thermostatic mixer, temperature detection probe is immersed in the water through tinfoil with thermometric, constant temperature 80 DEG C
Stirring 12h, naturally cools to room temperature, gained mixed solution and precipitate is transferred in centrifuge tube after stirring,
6000 turns/min is centrifuged 4min.Gained is centrifuged product and is placed in 80 DEG C of drying 12h in baking oven.Product after drying
Thing 5 DEG C/min in air atmosphere is warming up to 500 DEG C, is incubated 1h, naturally cools to room temperature and obtain end product.
The XRD figure of the white light emitting material of the laser excitation that the present embodiment prepares is similar with Fig. 1, it is known that,
Doping Ag+And Eu3+Product after two kinds of ions still remains the crystal structure of molecular sieve.
The white light emitting material that the present embodiment prepares is at the emission spectrum figure of 266nm laser excitation and Fig. 2
Similar, it has wide emission peak at about 500nm, and 576nm, 587nm, 617nm, 648nm, 695nm have
Sharp-pointed emission peak, and at 617nm, peak is the most maximum.
The white light emitting material that the present embodiment prepares emission spectrum figure under 280nm xenon lamp excites and figure
3 are similar to, and it has a wider emission peak at 530nm, has a narrower emission peak at 617nm, and the two is strong
Spend the most weak.
The white light emitting material that the present embodiment prepares luminescent chromaticity coordinate diagram under 266nm laser excitation
Similar with Fig. 4, it is known that material chromaticity coordinate falls in white light field.
Embodiment 5
Accurately weigh Y type molecular sieve 1.5g in 100mL conical flask, accurately weigh 0.4247g silver nitrate in
In conical flask, and add the Eu of the 0.2mol/L of 37.50mL3+Aqueous solution, be eventually adding 12.50mL go from
Sub-water, puts into stirring magneton.Conical flask explosion-proof plug is stoppered.Conical flask is put in the beaker of 400mL,
Add a certain amount of water in beaker, with tinfoil beaker wrapped and prevent Ag+Meet light to aoxidize.Beaker is put
On the stainless steel disc of thermostatic mixer, temperature detection probe is immersed in the water through tinfoil with thermometric, constant temperature 80 DEG C
Stirring 24h, naturally cools to room temperature, gained mixed solution and precipitate is transferred in centrifuge tube after stirring,
6000 turns/min is centrifuged 4min.Gained is centrifuged product and is placed in 80 DEG C of drying 12h in baking oven.Product after drying
Thing 5 DEG C/min in air atmosphere is warming up to 800 DEG C, is incubated 2h, naturally cools to room temperature and obtain end product.
The XRD figure of the white light emitting material of the laser excitation that the present embodiment prepares is similar with Fig. 1, it is known that,
Doping Ag+And Eu3+Product after two kinds of ions still remains the crystal structure of molecular sieve.
The white light emitting material that the present embodiment prepares is at the emission spectrum figure of 266nm laser excitation and Fig. 2
Similar, it has wide emission peak at about 500nm, and 576nm, 587nm, 617nm, 648nm, 695nm have
Sharp-pointed emission peak, and at 617nm, peak is the most maximum.
The white light emitting material that the present embodiment prepares emission spectrum figure under 280nm xenon lamp excites and figure
3 are similar to, and it has a wider emission peak at 530nm, has a narrower emission peak at 617nm, and the two is strong
Spend the most weak.
The white light emitting material that the present embodiment prepares luminescent chromaticity coordinate diagram under 266nm laser excitation
Similar with Fig. 4, it is known that material chromaticity coordinate falls in white light field.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by described reality
Execute the restriction of example, the change made under other any spirit without departing from the present invention and principle, modification,
Substitute, combine, simplify, all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (9)
1. the preparation method of the white light emitting material of a laser excitation, it is characterised in that comprise the following steps:
(1) preparation Eu3+Aqueous solution;
(2) by Y type molecular sieve, silver nitrate powder and Eu3+Aqueous solution in deionized water, mix homogeneously,
Obtain mixed liquor;Eu in described mixed liquor3+With Ag+The mol ratio of ion is 0.5~3): 1;
(3) step (2) obtains mixed liquor and stirs under the conditions of lucifuge, washs after naturally cooling to room temperature,
Centrifuging and taking lower floor product, calcines 0.5~3h in 500~900 DEG C in atmosphere after drying, naturally cools to room temperature and obtain
The white light emitting material under laser excitation being co-doped with to Ag-Eu.
The preparation method of the white light emitting material of laser excitation the most according to claim 1, its feature exists
In, step (1) described Eu3+The aqueous solution that aqueous solution is europium nitrate.
The preparation method of the white light emitting material of laser excitation the most according to claim 2, its feature exists
In, Eu in solution described in step (1)3+'sConcentration is 0.025~0.15mol/L.
The preparation method of the white light emitting material of laser excitation the most according to claim 1, its feature exists
In, described in step (1), in solution, Y type molecular sieve mass concentration is 0.02~0.04g/mL.
The preparation method of the white light emitting material of laser excitation the most according to claim 1, its feature exists
In, the stirring described in step (3), particularly as follows: stir 12~36h in 60~90 DEG C of constant temperature.
The preparation method of the white light emitting material of laser excitation the most according to claim 1, its feature exists
In, the washing described in step (3), particularly as follows: use deionized water wash 1~3 times.
The preparation method of the white light emitting material of laser excitation the most according to claim 1, its feature exists
In, step (3) described drying, particularly as follows: dry 6~24h at 60~150 DEG C.
The preparation method of the white light emitting material of laser excitation the most according to claim 1, its feature exists
In, it is incubated 0.5~3h in 500~900 DEG C, particularly as follows: with the speed of 3~10 DEG C/min described in step (3)
It is warming up to 500~900 DEG C, is incubated 0.5~3h.
9. the preparation method of the white light emitting material of a kind of laser excitation described in any one of claim 1~8 obtains
The white light emitting material of the laser excitation arrived, it is characterised in that with molecular sieve as substrate, in molecular sieve altogether
Mix Ag+And Eu3+Ion.
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Cited By (1)
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CN108865121A (en) * | 2018-08-30 | 2018-11-23 | 华南理工大学 | A kind of red fluorescence powder and molecular sieve composite luminescent material and its preparation method and application |
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CN101743290A (en) * | 2007-07-09 | 2010-06-16 | 鲁汶天主教大学 | emissive lamps comprising metal clusters confined in molecular sieves |
WO2013092707A1 (en) * | 2011-12-21 | 2013-06-27 | Clariant Produkte (Deutschland) Gmbh | Method for modifying the pore size of zeolites |
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Application publication date: 20160921 |