CN106634992A - Cubic strontium sodium niobate red fluorescent powder and preparation method thereof - Google Patents
Cubic strontium sodium niobate red fluorescent powder and preparation method thereof Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
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Abstract
The invention discloses a cubic strontium sodium niobate red fluorescent powder and a preparation method thereof. The method includes the steps of: 1) weighing SrCO3 and Nb2O5 as raw materials according to the molar ratio of (0.625-0.875):1, placing the weighed raw materials in a mortar, and grinding the raw materials at room temperature until the raw materials are mixed uniformly for later use; 2) placing an Al2O3 crucible in a furnace, maintaining the temperature at 1100-1200 DEG C for 3-9 h, cooling the crucible to 300 DEG C at the rate of 2 DEG C/min, cooling the crucible along with the furnace to room temperature and taking the crucible out. The cubic strontium sodium niobate powder having dispersed appearance and uniform distribution is produced in a molten salt manner. Compared with other methods, the molten salt method is easy to carry out and is controllable in granularity, has good crystal morphology and high physical-phase purity, and is short in synthesis period. The method is suitable for preparing cubic particle powder which is dispersed uniformly. Through the molten salt method, the cubic strontium sodium niobate (Na0.5Sr0.25NbO3) powder is completely crystallized, has dispersed appearance and uniform particles, and is high in color purity.
Description
Technical field
The invention belongs to white light LED fluorescent powder matrix preparing technical field, is related to a kind of cubic SrNb2 O6 sodium redness glimmering
Light powder and preparation method thereof, and in particular to one kind prepares Na using molten-salt growth method0.5Sr0.25NbO3The method of powder.
Background technology
Niobates is the widely used phosphor host of a class, with good heat endurance, chemical stability simultaneously
And easily modified and doping, it is obtained in fields such as ferroelectricity, dielectric and piezoelectricity and is widely applied.Niobates such as SrNb2 O6
Barium, potassium-sodium niobate, SrNb2 O6 sodium etc. also show valuable application potential in ceramics, film, photocatalysis.Wherein SrNb2 O6
Sodium has quadratic tungsten bronze structure, and this structure is a kind of derivative of perovskite structure.In this special structure cationic
It is easy to be replaced by rare earth ion, so as to become a kind of matrix for being especially suitable for and adulterating, is applied to illumination field.
The synthetic method of current fluorescent material mainly includes high temperature solid-state method, homogeneous co-precipitation process, sol-gel processing, burning
Method, hydro-thermal method etc., problem present in it includes that sintering temperature is high, and synthesis cycle is long, and particle is uneven, and excitation is not high.
The content of the invention
The technical problem to be solved is to provide a kind of cubic SrNb2 O6 sodium red fluorescence powder and its preparation side
Method, the cubic SrNb2 O6 sodium powder body that the method is obtained appearance dispersion, is evenly distributed using molten-salt growth method, compared with additive method,
Molten-salt growth method has easily operated, and granularity is controllable, and crystal morphology is good, and thing phase purity is high, the advantages of synthesis cycle is short, is adapted to prepare point
Dissipate uniform cubic granular powder, the present invention has synthesized that perfect crystalline, appearance dispersion, particle be uniform, color using molten-salt growth method
The high cubic SrNb2 O6 sodium Na of purity0.5Sr0.25NbO3Powder.
To achieve these goals, the technical solution used in the present invention is, a kind of cubic SrNb2 O6 sodium red fluorescence powder
Preparation method, comprise the following steps：
1) with SrCO3And Nb2O5As raw material, and it is (0.625～0.875) according to mol ratio：1 ratio is carried out respectively
Weigh, the raw material for weighing is placed in mortar, grinding at room temperature makes it stand-by after being well mixed；
2) step 1) in the SrCO that weighs3And Nb2O5Gross mass be M, wherein M=MSrCO3+MNb2O5, the quality of NaCl is
M, according to M：M=1：The ratio of (3～9) weighs NaCl as fused salt, and by itself and step 1) raw material that weighs mixes, will mix
Thing is fully ground at room temperature prepared mixed powder；
3) by step 2) gained mixed powder is placed in crucible and uses Al2O3Lid is covered；
4) by Al2O3Crucible is placed in stove, and 3～9h is incubated at 1100～1200 DEG C, and with 2 DEG C/min speed 300 are cooled to
DEG C, then cool to room temperature taking-up with the furnace；
5) removal step 4) products therefrom fused salt, after fused salt is removed completely, by product drying, grinding, that is, obtain
Na0.5Sr0.25NbO3Powder.
Step 5) in soaked repeatedly by deionized water, wash removal fused salt, and by silver nitrate inspection washing clear liquid sentence
It is disconnected whether still to have remaining fused salt.
Step 4) in the heating mode of chamber type electric resistance furnace be：From room temperature, with the ramp of 3 DEG C/min to 600 DEG C, then
With the ramp of 5 DEG C/min to 1100～1200 DEG C.
Step 1) in milling time be 2h.
Step 1) described in mortar be agate mortar.
Step 2) in milling time be 2h.
Step 3) described in crucible be alumina crucible.
A kind of cubic SrNb2 O6 sodium red fluorescence powder, its chemical composition is Na0.5Sr0.25NbO3。
Compared with prior art, the invention has the advantages that：The present invention is prepared by molten-salt growth method can make powder pure
Degree is high, pattern is good, uniform particle sizes；By the test of XRD, SEM and analysis, it is of the invention prepared by
Na0.5Sr0.25NbO3Powder purity be up to good 100%, crystal property, uniform particle sizes, average grain diameter be 10～16 μm, pattern is attractive in appearance
For cubic and decentralization is high.
Description of the drawings
Fig. 1 is cubic Na obtained in the embodiment of the present invention 10.5Sr0.25NbO3The XRD of powder；
Fig. 2 is cubic Na obtained in the embodiment of the present invention 10.5Sr0.25NbO3The SEM figures of powder.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
1) with SrCO3And Nb2O5It is 0.825 according to mol ratio as raw material：1 ratio is weighed respectively, will be weighed
Good raw material is placed in agate mortar, and 2h is ground at room temperature makes it stand-by after being well mixed；
2) SrCO is made3And Nb2O5Gross mass be M (M=MSrCO3+MNb2O5), the quality of NaCl is m, according to M：M=1：5
Ratio weigh NaCl as fused salt, and by itself and step 1) gained raw material mixes, and mixture is fully ground at room temperature 2h
Prepared mixed powder；
3) step 2 gained mixed powder is placed in into Al2O3Al is used in crucible2O3Lid is covered.
4) by Al2O3Crucible is placed in stove, from room temperature, with the ramp of 3 DEG C/min to 600 DEG C, then with 5 DEG C/min
Ramp to 1150 DEG C, insulation 9h after be cooled to 300 DEG C with 2 DEG C/min speed, then cool to the furnace room temperature taking-up；
5) by step 4) products therefrom deionized water soaks, washs repeatedly, be then with silver nitrate inspection washing clear liquid
It is no still to have remaining fused salt, after fused salt is removed completely, by product drying, grinding, that is, obtain Na0.5Sr0.25NbO3Powder.
Fig. 1 show the cubic Na obtained by the present embodiment0.5Sr0.25NbO3The XRD of powder, as can be seen from the figure
Sample diffraction peak fits like a glove with standard card JCPDS Card NO.27-0788, and without miscellaneous peak, illustrates obtained sample
Thing phase purity is higher.
Fig. 2 show cubic Na obtained in the present embodiment0.5Sr0.25NbO3The SEM of powder schemes, as can be seen from the figure sample
Product particle is uniformly dispersed, and average grain diameter is 10～16 μm, and degree of crystallinity is high, and pattern is attractive in appearance for cubic and favorable dispersibility.
Embodiment 2
1) with SrCO3And Nb2O5It is 0.75 according to mol ratio as raw material：1 ratio is weighed respectively, will be weighed
Raw material be placed in agate mortar, at room temperature grind 2h make its be well mixed after it is stand-by；
2) SrCO is made3And Nb2O5Gross mass be M (M=MSrCO3+MNb2O5), the quality of NaCl is m, according to M：M=1：3
Ratio weigh NaCl as fused salt, and by itself and step 1) gained raw material mixes, and mixture is fully ground at room temperature 2h
Prepared mixed powder；
3) step 2 gained mixed powder is placed in into Al2O3Al is used in crucible2O3Lid is covered.
4) by Al2O3Crucible is placed in stove, from room temperature, with the ramp of 3 DEG C/min to 600 DEG C, then with 5 DEG C/min
Ramp to 1100 DEG C, insulation 6h after be cooled to 300 DEG C with 2 DEG C/min speed, then cool to the furnace room temperature taking-up；
5) by step 4) products therefrom deionized water soaks, washs repeatedly, be then with silver nitrate inspection washing clear liquid
It is no still to have remaining fused salt, after fused salt is removed completely, by product drying, grinding, that is, obtain Na0.5Sr0.25NbO3Powder.
Embodiment 3
1) with SrCO3And Nb2O5It is 0.675 according to mol ratio as raw material：1 ratio is weighed respectively, will be weighed
Good raw material is placed in agate mortar, and 2h is ground at room temperature makes it stand-by after being well mixed；
2) SrCO is made3And Nb2O5Gross mass be M (M=MSrCO3+MNb2O5), the quality of NaCl is m, according to M：M=1：5
Ratio weigh NaCl as fused salt, and by itself and step 1) gained raw material mixes, and mixture is fully ground at room temperature 2h
Prepared mixed powder；
3) step 2 gained mixed powder is placed in into Al2O3Al is used in crucible2O3Lid is covered.
4) by Al2O3Crucible is placed in stove, from room temperature, with the ramp of 3 DEG C/min to 600 DEG C, then with 5 DEG C/min
Ramp to 1150 DEG C, insulation 3h after be cooled to 300 DEG C with 2 DEG C/min speed, then cool to the furnace room temperature taking-up；
5) by step 4) products therefrom deionized water soaks, washs repeatedly, be then with silver nitrate inspection washing clear liquid
It is no still to have remaining fused salt, after fused salt is removed completely, by product drying, grinding, that is, obtain Na0.5Sr0.25NbO3Powder.
Embodiment 4
1) with SrCO3And Nb2O5It is 0.625 according to mol ratio as raw material：1 ratio is weighed respectively, will be weighed
Good raw material is placed in agate mortar, and 2h is ground at room temperature makes it stand-by after being well mixed；
2) SrCO is made3And Nb2O5Gross mass be M (M=MSrCO3+MNb2O5), the quality of NaCl is m, according to M：M=1：7
Ratio weigh NaCl as fused salt, and by itself and step 1) gained raw material mixes, and mixture is fully ground at room temperature 2h
Prepared mixed powder；
3) step 2 gained mixed powder is placed in into Al2O3Al is used in crucible2O3Lid is covered.
4) by Al2O3Crucible is placed in stove, from room temperature, with the ramp of 3 DEG C/min to 600 DEG C, then with 5 DEG C/min
Ramp to 1200 DEG C, insulation 3h after be cooled to 300 DEG C with 2 DEG C/min speed, then cool to the furnace room temperature taking-up；
5) by step 4) products therefrom deionized water soaks, washs repeatedly, be then with silver nitrate inspection washing clear liquid
It is no still to have remaining fused salt, after fused salt is removed completely, by product drying, grinding, that is, obtain Na0.5Sr0.25NbO3Powder.
Embodiment 5
1) with SrCO3And Nb2O5It is 0.875 according to mol ratio as raw material：1 ratio is weighed respectively, will be weighed
Good raw material is placed in agate mortar, and 2h is ground at room temperature makes it stand-by after being well mixed；
2) SrCO is made3And Nb2O5Gross mass be M (M=MSrCO3+MNb2O5), the quality of NaCl is m, according to M：M=1：9
Ratio weigh NaCl as fused salt, and by itself and step 1) gained raw material mixes, and mixture is fully ground at room temperature 2h
Prepared mixed powder；
3) step 2 gained mixed powder is placed in into Al2O3Al is used in crucible2O3Lid is covered.
4) by Al2O3Crucible is placed in stove, from room temperature, with the ramp of 3 DEG C/min to 600 DEG C, then with 5 DEG C/min
Ramp to 1150 DEG C, insulation 6h after be cooled to 300 DEG C with 2 DEG C/min speed, then cool to the furnace room temperature taking-up；
5) by step 4) products therefrom deionized water soaks, washs repeatedly, be then with silver nitrate inspection washing clear liquid
It is no still to have remaining fused salt, after fused salt is removed completely, by product drying, grinding, that is, obtain Na0.5Sr0.25NbO3Powder.
Claims (8)
1. a kind of preparation method of cubic SrNb2 O6 sodium red fluorescence powder, it is characterised in that comprise the following steps：
1) with SrCO3And Nb2O5As raw material, and it is (0.625～0.875) according to mol ratio：1 ratio is weighed respectively,
The raw material for weighing is placed in mortar, grinding at room temperature makes it stand-by after being well mixed；
2) step 1) in the SrCO that weighs3And Nb2O5Gross mass be M, the quality of NaCl is m, according to M：M=1：(3～9)
Ratio weighs NaCl as fused salt, and by itself and step 1) raw material that weighs mixes, and mixture is fully ground at room temperature system
Obtain mixed powder；
3) by step 2) gained mixed powder is placed in crucible and uses Al2O3Lid is covered；
4) by Al2O3Crucible is placed in stove, and 3～9h is incubated at 1100～1200 DEG C, and with 2 DEG C/min speed 300 DEG C are cooled to,
Then room temperature taking-up is cooled to the furnace；
5) removal step 4) products therefrom fused salt, after fused salt is removed completely, by product drying, grinding, that is, obtain
Na0.5Sr0.25NbO3Powder.
2. a kind of preparation method of cubic SrNb2 O6 sodium red fluorescence powder according to claim 1, it is characterised in that step
It is rapid 5) in soaked repeatedly by deionized water, wash removal fused salt, and by silver nitrate inspection washing clear liquid judge whether still have
Remaining fused salt.
3. a kind of preparation method of cubic SrNb2 O6 sodium red fluorescence powder according to claim 1, it is characterised in that step
It is rapid 4) in the heating mode of chamber type electric resistance furnace be：From room temperature, with the ramp of 3 DEG C/min to 600 DEG C, then with 5 DEG C/min
Ramp to 1100～1200 DEG C.
4. a kind of preparation method of cubic SrNb2 O6 sodium red fluorescence powder according to claim 1, it is characterised in that step
It is rapid 1) in milling time be 2h.
5. a kind of preparation method of cubic SrNb2 O6 sodium red fluorescence powder according to claim 1, it is characterised in that step
It is rapid 1) described in mortar be agate mortar.
6. a kind of preparation method of cubic SrNb2 O6 sodium red fluorescence powder according to claim 1, it is characterised in that step
It is rapid 2) in milling time be 2h.
7. a kind of preparation method of cubic SrNb2 O6 sodium red fluorescence powder according to claim 1, it is characterised in that step
It is rapid 3) described in crucible be alumina crucible.
8. a kind of cubic SrNb2 O6 sodium red fluorescence powder, it is characterised in that its chemical composition is Na0.5Sr0.25NbO3。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108144607A (en) * | 2017-12-26 | 2018-06-12 | 吉林大学 | Iridium acid strontium class catalyst, preparation method and its application in terms of electro-catalysis cracks acid aquatic products oxygen |
| CN108275748A (en) * | 2018-01-31 | 2018-07-13 | 河南大学 | A kind of SrNb2 O6 sodium material and the preparation method and application thereof |
| CN109319840A (en) * | 2018-11-15 | 2019-02-12 | 北京工业大学 | A method of preparing SrNb2 O6/strontium carbonate composite nano materials |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108144607A (en) * | 2017-12-26 | 2018-06-12 | 吉林大学 | Iridium acid strontium class catalyst, preparation method and its application in terms of electro-catalysis cracks acid aquatic products oxygen |
| CN108144607B (en) * | 2017-12-26 | 2020-06-09 | 吉林大学 | Strontium iridate catalyst, preparation method and application thereof in aspect of producing oxygen by electrocatalytic cracking of acidic water |
| CN108275748A (en) * | 2018-01-31 | 2018-07-13 | 河南大学 | A kind of SrNb2 O6 sodium material and the preparation method and application thereof |
| CN109319840A (en) * | 2018-11-15 | 2019-02-12 | 北京工业大学 | A method of preparing SrNb2 O6/strontium carbonate composite nano materials |
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Application publication date: 20170510 |