CN101550338A - Nanometer rare-earth compound luminescent material and preparation method thereof - Google Patents
Nanometer rare-earth compound luminescent material and preparation method thereof Download PDFInfo
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- CN101550338A CN101550338A CNA2008100272570A CN200810027257A CN101550338A CN 101550338 A CN101550338 A CN 101550338A CN A2008100272570 A CNA2008100272570 A CN A2008100272570A CN 200810027257 A CN200810027257 A CN 200810027257A CN 101550338 A CN101550338 A CN 101550338A
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Abstract
The invention relates to a luminescent material and a preparation method thereof, in particular to a nanometer rare-earth compound luminescent material and a preparation method thereof. The preparation method of the luminescent material adopts a combustion method to synthesize a precursor of Sr4Al14O25: Eu <2+>, Dy <3+>, then nanometer phosphor powder Sr4Al14O25: Eu <2+>, Dy <3+> are synthesized by a high-temperature calcination method on the precursor under the protection of N2 at the temperature of 1300 DEG C, the analyzed nanometer phosphor powder is showed as a single phase of Sr4Al14O25 by analyzing an XRD map, and the average grain diameter of the analyzed nanometer phosphor powder is ranged from 20 nm to 40 nm.
Description
Technical field:
The present invention relates to luminescent material and preparation method thereof technical field, particularly a kind of nanometer rare-earth compound luminescent material and preparation method thereof.
Background technology:
Along with social development, scientific-technical progress, the situation from single variety to many kinds, many specification seriesization has appearred in rare earth luminescent material of China and non-rare earth luminescent material.The footprint that nowadays, rare earth luminescent material is all arranged on low-pressure gas luminescent lamp, high-intensity gas discharge lamp and other related productss.Rare earth material is a huge mine of luminescent materials, and in the various luminescent materials of human development, rare earth element is being brought into play important effect.Because have the 4f track in the electronic configuration of rare earth element atom, therefore, the rare earth element atom has abundant electronic level, for condition has been created in the transition of multiple energy level, thereby can obtain multiple luminescent properties.The advantage of rare earth luminescent material is that receptivity is strong, turnover ratio is high, can launch from ultraviolet to infrared spectrum, in the visible region, very strong emissive power is arranged, and physicochemical property are stable.Rare earth luminescent material can be divided into rare earth cathode-ray luminescence material, rare earth embedded photoluminescent material, X ray rare earth luminescent material, rare earth scintillator, rare earth up-conversion luminescent material and other rare earth function luminescent material again because of its mode of excitation difference.At present, rare earth luminescent material is mainly used in aspects such as colour kinescope, graphoscope, illumination, medical facilities, rare earth luminescent material consumption maximum be colour kinescope, graphoscope, rare-earth trichromatic energy saving lamp, plasma panel.
Rare earth luminescent material has become the main raw of light industry, demand increases day by day, but rare earth is a limited resources, should be on using towards concept development efficiently on a small quantity, at present, the nano luminescent material on the market is micron-sized material mostly, if, after the rare earth luminescent material nanometer, its application efficiency can reach several times or hundreds of times.Again, the compound and hydridization at material can allow rare earth luminescent material have more usefulness and variation.
Nano material is through the effort of industry about 20 years, technology and production capacity are day by day ripe at present, rare earth luminescent material can be further development of the nano rare earth luminescent material with this understanding, the present domestic rare earth industrial structure is unreasonable, scientific and technological content is not high, main products is wanted export dependence more than 60%, overall product is of low quality, description is few; High-tech content, the high value-added product proportion is on the low side, perspective, therefore the frontier nature technology is few, causes that corresponding industry development is slow, cost is higher.
High temperature solid-state method has been widely used in the synthetic of phosphorescent substance, but this method causes the powder luminescent properties that synthesizes impaired through regular meeting, and needs very high calcining temperature.In addition, the particle diameter of the phosphor powder that synthesizes with high temperature solid-state method is about tens microns, and the acquisition of less phosphor powder will obtain by ball milling macrobead powder, and experiment shows, can cause bringing more defective through ball milling twinkler powder, and luminous efficiency obviously reduces.
Summary of the invention:
One of purpose of the present invention provides a kind of nanometer rare-earth compound luminescent material, and this material is nano level phosphor powder Sr
4Al
14O
25: Eu
2+, Dy
3+
Two of purpose of the present invention provides a kind of preparation method of nanometer rare-earth compound luminescent material, it can realize rare earth luminescent material nanometer, sophistication, high efficiency and compoundization, makes this class material be issued to the highest function and benefit in the resource of consumes least.
The preparation method of nanometer rare-earth compound luminescent material of the present invention adopts following technical scheme:
Take by weighing Al (NO by stoichiometric ratio
3)
39H
2O and Sr (NO
3)
2In the 250ml beaker, use dissolved in distilled water, obtain settled solution, take by weighing Eu by stoichiometric ratio in addition
2O
3, Dy
2O
3Put into the 50ml beaker and, merge aforementioned two solution that make, in mixing solutions, add H with the concentrated nitric acid dissolving
3BO
3And CO (NH
2)
2, magnetic agitation is 2 hours in 70 ℃ water bath with thermostatic control, and particle dia can not become big under this low temperature environment;
After treating fully to stir, solution is transferred in the 300ml porcelain crucible and inserts rapidly in the retort furnace that is heated to 500 ℃ in advance, along with the carrying out of reaction, can be observed solution and seethe with excitement rapidly, evaporate, expand, burn and follow a large amount of ammonias to emit, whole process was finished in 5 minutes, after cooling, can be observed product and be faint yellow mushroom cloud-like, loose porous, grind a little, can become thin pale yellow powder, this pale yellow powder is nano level phosphor powder Sr
4Al
14O
25: Eu
2+, Dy
3+Presoma, with this pale yellow powder, put into corundum crucible; do protection gas with nitrogen in high temperature process furnances, calcined 3 hours for 1300 ℃, take out the cooling back; grind a little in agate mortar and promptly obtain the light green pressed powder, this pressed powder promptly is nano level phosphor powder Sr
4Al
14O
25: Eu
2+, Dy
3+
The present invention synthesizes Sr with combustion method
4Al
14O
25: Eu
2+, Dy
3+Presoma, use 1300 ℃, N then
2Presoma is carried out calcining method has synthesized nano level phosphor powder Sr down in protection
4Al
14O
25: Eu
2+, Dy
3+, the powder that analysis revealed synthesizes is Sr
4Al
14O
25Single phase, the median size of powder is in 20～40nm scope.
Description of drawings:
Fig. 1 is the XRD figure spectrum of presoma
Fig. 2 is the XRD figure spectrum of target product
Embodiment:
Fig. 1 is the XRD figure spectrum of presoma, analyze in the collection of illustrative plates diffraction peak and with standard card JSPDS74-1810 contrast, can find, press Sr
4Al
14O
25: Eu
2+, Dy
3+Material ratio carry out proportioning, do not observe Sr in the products of combustion of gained after 500 ℃ of burnings
4Al
14O
25Characteristic diffraction peak, but with SrAl
2O
4Be main characteristic peak (JCPDS34-379), also find SrAl simultaneously
4O
7And Sr
3Al
2O
6Characteristic peak owing to be according to Sr
4Al
14O
25: Eu
2+, Dy
3+Stoichiometric ratio prepare burden, combustion reactions is again to carry out under a very of short duration high temperature, the formation of crystalline phase is very insufficient, hence one can see that, low-temperature combustion method can not go out long-afterglow material Sr by one-step synthesis
4Al
14O
25: Eu
2+, Dy
3+
Fig. 2 is through the XRD figure of 1300 ℃ of high-temperature calcination after products spectrum, with standard card JSPDS74-1810 coincide fine, this explanation is through after the pyroprocessing, conversion has taken place in the crystalline form of matrix, among the figure, except Sr
4Al
14O
25Characteristic diffraction peak outside, do not observe the characteristic diffraction peak of other crystal formation, this explanation crystal is monophasic, it is very abundant that crystal formation transforms, the activator ion Eu that mixes on a small quantity
2+With assisted activation ion Dy
3+Do not change Sr
4Al
14O
25Crystalline structure.
Embodiment one
Get 52.52 gram Al (NO by stoichiometric ratio
3)
39H
2O, 8.46 gram Sr (NO
3)
2In the 250ml beaker, use dissolved in distilled water, obtain settled solution; Take by weighing 0.0352 gram Eu by stoichiometric ratio in addition
2O
3, 0.0373 the gram Dy
2O
3Put into the 50ml beaker and, merge two solution, add 3.7 gram H then with the concentrated nitric acid dissolving
3BO
3With 100 gram CO (NH
2)
2Magnetic agitation is 2 hours in 70 ℃ water bath with thermostatic control; after treating fully to stir; solution is transferred in the 300ml porcelain crucible and inserts rapidly be heated in advance in 500 ℃ of retort furnaces; carrying out along with reaction; can be observed solution seethes with excitement rapidly; evaporation; expand; burning also follows a large amount of ammonias to emit; whole process was finished in 5 minutes; after cooling, can be observed product and be faint yellow mushroom cloud-like, loose porous; grind a little; can become thin pale yellow powder,, put into corundum crucible the product of burning back gained; in high temperature process furnances, do protection gas with nitrogen; calcined 3 hours for 1300 ℃, take out the cooling back, grinds a little in agate mortar and promptly obtain the compound light green solid luminescence of nano rare earth powder.
Embodiment two
Get 52.52 gram Al (NO by stoichiometric ratio
3)
39H
2O and 8.46 gram Sr (NO
3)
2In the 250ml beaker, use dissolved in distilled water, obtain settled solution; Other takes by weighing 0.044 gram Eu
2O
3, 0.047 the gram Dy
2O
3Put into the 50ml beaker and, merge two solution, add 3.7 gram H then with the concentrated nitric acid dissolving
3BO
3With 100 gram CO (NH
2)
2Magnetic agitation is 2 hours in 70 ℃ water bath with thermostatic control; after treating fully to stir; solution is transferred in the 300ml porcelain crucible and inserts rapidly be heated in advance in 500 ℃ of retort furnaces; carrying out along with reaction; can be observed solution seethes with excitement rapidly; evaporation; expand; burning also follows a large amount of ammonias to emit; whole process was finished in 5 minutes; after cooling, can be observed product and be faint yellow mushroom cloud-like, loose porous; grind a little; can become thin pale yellow powder,, put into corundum crucible the product of burning back gained; in high temperature process furnances, do protection gas with nitrogen; calcined 3 hours for 1300 ℃, take out the cooling back, grinds a little in agate mortar and promptly obtain the compound light green solid luminescence of nano rare earth powder.
Embodiment three
Get 52.52 gram Al (NO by stoichiometric ratio
3)
39H
2O and 8.46 gram Sr (NO
3)
2In the 250ml beaker, use dissolved in distilled water, obtain settled solution; Other takes by weighing 0.053 gram Eu
2O
3, 0.056 the gram Dy
2O
3Put into the 50ml beaker and, merge two solution, add 3.7 gram H then with the concentrated nitric acid dissolving
3BO
3With 100 gram CO (NH
2)
2Magnetic agitation is 2 hours in 70 ℃ water bath with thermostatic control; after treating fully to stir; solution is transferred in the 300ml porcelain crucible and inserts rapidly be heated in advance in 500 ℃ of retort furnaces; carrying out along with reaction; can be observed solution seethes with excitement rapidly; evaporation; expand; burning also follows a large amount of ammonias to emit; whole process was finished in 5 minutes; after cooling, can be observed product and be faint yellow mushroom cloud-like, loose porous; grind a little; can become thin pale yellow powder,, put into corundum crucible the product of burning back gained; in high temperature process furnances, do protection gas with nitrogen; calcined 3 hours for 1300 ℃, take out the cooling back, grinds a little in agate mortar and promptly obtain the compound light green solid luminescence of nano rare earth powder.
Embodiment four
Get 52.52 gram Al (NO by stoichiometric ratio
3)
39H
2O and 8.46 gram Sr (NO
3)
2In the 250ml beaker, use dissolved in distilled water, obtain settled solution; Other takes by weighing 0.07 gram Eu
2O
3, 0.075 the gram Dy
2O
3Put into the 50ml beaker and, merge two solution, add 3.7 gram H then with the concentrated nitric acid dissolving
3BO
3With 100 gram CO (NH
2)
2Magnetic agitation is 2 hours in 70 ℃ water bath with thermostatic control; after treating fully to stir; solution is transferred in the 300ml porcelain crucible and inserts rapidly be heated in advance in 500 ℃ of retort furnaces; carrying out along with reaction; can be observed solution seethes with excitement rapidly; evaporation; expand; burning also follows a large amount of ammonias to emit; whole process was finished in 5 minutes; after cooling, can be observed product and be faint yellow mushroom cloud-like, loose porous; grind a little; can become thin pale yellow powder,, put into corundum crucible the product of burning back gained; in high temperature process furnances, do protection gas with nitrogen; calcined 3 hours for 1300 ℃, take out the cooling back, grinds a little in agate mortar and promptly obtain the compound light green solid luminescence of nano rare earth powder.
Claims (2)
1, a kind of nanometer rare-earth compound luminescent material is characterized in that: this material is nano level phosphor powder Sr
4Al
14O
25: Eu
2+, Dy
3+
2, a kind of preparation method of nanometer rare-earth compound luminescent material is characterized in that: take by weighing Al (NO by stoichiometric ratio
3)
39H
2O and Sr (NO
3)
2In the 250ml beaker, use dissolved in distilled water, obtain settled solution, take by weighing Eu by stoichiometric ratio
2O
3, Dy
2O
3Put into the 50ml beaker and, merge aforementioned two solution that make, in mixing solutions, add H with the concentrated nitric acid dissolving
3BO
3And CO (NH
2)
2, magnetic agitation in 70 ℃ of waters bath with thermostatic control;
After treating fully to stir; solution is transferred in the porcelain crucible and inserts rapidly in the retort furnace that is heated to 500 ℃ in advance; question response is finished; cooling can get pale yellow powder, and pale yellow powder is put into corundum crucible, does protection gas with nitrogen in high temperature process furnances; calcined 3 hours for 1300 ℃; take out the cooling back, grinds a little and promptly obtain the light green pressed powder, and this pressed powder promptly is nano level phosphor powder Sr
4Al
14O
25: Eu
2+, Dy
3+
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|---|---|---|---|
| CNA2008100272570A CN101550338A (en) | 2008-04-03 | 2008-04-03 | Nanometer rare-earth compound luminescent material and preparation method thereof |
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|---|---|---|---|
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|---|---|
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409137A (en) * | 2013-08-22 | 2013-11-27 | 中国计量学院 | An ultraviolet ray excited SrMgAl10O17: eu2+, mn2+blue-green phosphor |
| CN104099093A (en) * | 2013-04-07 | 2014-10-15 | 青海雅丰彩色印刷有限责任公司 | Method for preparing rare-earth-activated Sr4Al7O25 long-afterglow luminescent material |
-
2008
- 2008-04-03 CN CNA2008100272570A patent/CN101550338A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099093A (en) * | 2013-04-07 | 2014-10-15 | 青海雅丰彩色印刷有限责任公司 | Method for preparing rare-earth-activated Sr4Al7O25 long-afterglow luminescent material |
| CN103409137A (en) * | 2013-08-22 | 2013-11-27 | 中国计量学院 | An ultraviolet ray excited SrMgAl10O17: eu2+, mn2+blue-green phosphor |
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Address after: 523000 Guangdong Dongcheng Dongcheng Long Road East China Sea industrial zone Dongguan Dongguan topological Industry Co., Ltd. Applicant after: Dongguan Jieming Lighting Technology Co., Ltd. Address before: 523808 Guangdong province Dongguan City Songshan students Pioneering Park Dongguan lieming Lighting Technology Co. Ltd. Applicant before: Dongguan Jieming Lighting Technology Co., Ltd. |
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Application publication date: 20091007 |