CN102191052A - Borate red luminescent material and preparation method thereof - Google Patents

Borate red luminescent material and preparation method thereof Download PDF

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Publication number
CN102191052A
CN102191052A CN2010101257185A CN201010125718A CN102191052A CN 102191052 A CN102191052 A CN 102191052A CN 2010101257185 A CN2010101257185 A CN 2010101257185A CN 201010125718 A CN201010125718 A CN 201010125718A CN 102191052 A CN102191052 A CN 102191052A
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luminescent material
red luminescent
preparation
compound
borate red
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周明杰
梁小芳
刘军
田梓峰
廖秋荣
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention discloses a borate red luminous material and a preparation method thereof. The formula for the borate luminescent material is M3Ln1-xRex(BO3)3, M thereof is Ca, Sr or Ba, Ln thereof is at least one of Y, La and Gd, Re thereof is Eu or Sm, and x thereof is equal to or more than 0.005 and equal to or less than 0.50. The preparation method comprises the following steps: weighing raw materials according to a proportion and allowing a material containing B to be excess; adding a certain amount of a flux; presintering at a low temperature; calcining at a temperature of 900 to 1300 DEG C; and cooling. The borate red luminous material is obtained. The preparation method has the advantages of simple process and low cost. The prepared borate red luminous material, which can emit red light with wavelengths of near 600 nm, has an excellent luminescent performance and can be used in PDPs (Plasma Display Panels) or mercury-free fluorescent lamps.

Description

Borate red luminescent material and preparation method thereof
Technical field
The present invention relates to the luminescent material technical field, relate in particular to a kind of borate red luminescent material and preparation method thereof.
Background technology
Compare with LCD display with traditional CRT monitor, plasma flat-panel display (PDP) has advantages such as the visual angle is wide, big area, response is fast, colour reproduction is good, can be made into the indicating meter of large-size.Compare with low pressure mercury lamp with traditional high voltage mercury lamp, non-mercury florescent lamp meets environmental protection ideas more because it does not contain the deleterious mercury of human body.In PDP and non-mercury florescent lamp, fluorescent material is one of key factor of its performance of restriction.
Summary of the invention
The technical problem to be solved in the present invention is, at the above-mentioned defective of prior art, provides a kind of borate red luminescent material of good luminous performance.
The technical problem that the present invention further will solve is, the preparation method of a kind of technology borate red luminescent material simple, with low cost also is provided.
In order to reach above-mentioned purpose, according to a first aspect of the present invention, provide a kind of borate red luminescent material, its chemical formula is M 3Ln 1-xRe x(B0 3) 3, wherein, M is Ca, Sr or Ba, and Ln is at least a among Y, La, the Gd, and Re is Eu or Sm, and the span of x is 0.005≤x≤0.50.
In borate red luminescent material of the present invention, preferably, the span of described x is 0.025≤x≤0.25.
In order to reach above-mentioned purpose, according to a second aspect of the present invention, provide a kind of preparation method of borate red luminescent material, may further comprise the steps:
1. be raw material to contain the M compound, to contain the Ln compound, contain the Re compound, contain the B compound, according to the molar ratio of each element in the above-mentioned chemical formula and make and contain the B compound and take by weighing each raw material by above-mentioned molar ratio excessive 5～30%, and taking by weighing fusing assistant according to molar ratio 1～10% with above-mentioned chemical formula, ground and mixed evenly forms compound;
2. compound is first 200～700 ℃ of following presintering, then 900～1300 ℃ of calcinings down;
3. step calcinate 2. is cooled to room temperature, promptly obtains borate red luminescent material.
In the preparation method of borate red luminescent material of the present invention, preferably, at least a in the oxide compound that the described M of containing compound is M, oxyhydroxide, nitrate, the carbonate, oxide compound or nitrate that the described Ln of containing compound is Ln, oxide compound or nitrate that the described Re of containing compound is Re, the described B of containing compound is a boric acid.
In the preparation method of borate red luminescent material of the present invention, preferably, described fusing assistant is at least a in boric acid, barium fluoride, magnesium fluoride, the Calcium Fluoride (Fluorspan).
In the preparation method of borate red luminescent material of the present invention, preferably, the presintering time of described step in 2. is 2～7h.
In the preparation method of borate red luminescent material of the present invention, preferably, the calcination time of described step in 2. is 1～24h.
In the preparation method of borate red luminescent material of the present invention, further preferably, the calcining temperature of described step in 2. is 1000～1200 ℃, and calcination time is 5～10h.
In the preparation method of borate red luminescent material of the present invention, preferably, 2. described step is: prior to 200～700 ℃ of presintering, cooling presintering product grinds to room temperature with compound, and then in 900～1300 ℃ of calcinings.
Borate red luminescent material of the present invention is with M 3Ln 1-x(BO 3) 3Be matrix, with Eu 3+Or Sm 3+Be light emitting ionic, its luminescence mechanism is: pass through M 3Ln 1-x(BO 3) 3For matrix is the strong absorption of the vacuum-ultraviolet light of 150～175nm to wavelength, give Eu with transmission ofenergy 3+Or Sm 3+Ion, thus ruddiness launched.
In the borate red luminescent material of the present invention, when Ln is Gd, at M 3Ln 1-x(BO 3) 3After matrix to wavelength is the strong absorption of vacuum-ultraviolet light of 150～175nm, realize matrix sensitization Gd 3+Highly excited level energy level, and Gd 3+ 6P JEnergy level and Eu 3+Or Sm 3+There is transmission ofenergy between the ion, gives Eu transmission ofenergy 3+Ion has further improved the intensity of launching ruddiness.
In the borate red luminescent material of the present invention, Eu 3+Or Sm 3+Ion is at M 3Ln 1-x(BO 3) 3Launching wavelength in the matrix and be positioned near the ruddiness of 600nm, have good luminous property, is the novel red luminescent material of a kind of PDP of can be used for or non-mercury florescent lamp.
Among the preparation method of borate red luminescent material of the present invention, one or more in adding boric acid, barium fluoride, magnesium fluoride, the Calcium Fluoride (Fluorspan) can make reaction more abundant, and can reduce the temperature of reaction as fusing assistant.
The preparation method of borate red luminescent material of the present invention, technology is simple, with low cost, and the borate red luminescent material of preparation has good luminous property, can be used for PDP or non-mercury florescent lamp.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is the Sr of the embodiment of the invention 1 3Y 0.95Eu 0.05(BO 3) 3The exciting light spectrogram of borate red luminescent material, the monitoring wavelength is 600nm;
Fig. 2 is the Ba of the embodiment of the invention 7 3Gd 0.95Sm 0.09(BO 3) 3The exciting light spectrogram of borate red luminescent material, the monitoring wavelength is 599nm;
Fig. 3 is the Ba of the embodiment of the invention 8 3Gd 0.95Eu 0.05(BO 3) 3The exciting light spectrogram of borate red luminescent material, the monitoring wavelength is respectively 600nm and 311nm;
Fig. 4 is the Sr of the embodiment of the invention 1 3Y 0.95Eu 0.05(BO 3) 3The emmission spectrum figure of borate red luminescent material, excitation wavelength is 172nm;
Fig. 5 is the Ba of the embodiment of the invention 7 3Gd 0.95Sm 0.5(BO 3) 3The emmission spectrum figure of borate red luminescent material, excitation wavelength is 172nm;
Fig. 6 is the Ba of the embodiment of the invention 8 3Gd 0.95Eu 0.05(BO 3) 3The emmission spectrum figure of borate red luminescent material, excitation wavelength is 172nm.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, the present invention is further described in detail below in conjunction with drawings and Examples.
Used rare earths material purity is more than the 4N in the embodiments of the invention, and other raw materials are common commercial goods, and purity is analytical pure.Use for convenience, can be with RE(rare earth) borate luminescent material grind into powder of the present invention.
Embodiment 1
Take by weighing Strontium carbonate powder SrCO 32.2145g, yttrium oxide Y 2O 30.5361g, boric acid H 3BO 31.0202g (according to products therefrom Sr 3Y 0.95Eu 0.05(BO 3) 3In the molar ratio equivalent of B element excessive 10%, down with), europium sesquioxide Eu 2O 30.0440g and magnesium fluoride MgF 20.0078g (be gained silicate red illuminating material Sr 3Y 0.95Eu 0.05(BO 3) 3Molar ratio 2.5%, down with).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 1000 ℃, cooling promptly gets Sr after the grinding 3Y 0.95Eu 0.05(BO 3) 3Borate red luminescent material.
Fig. 1 is the Sr of the embodiment of the invention 1 3Y 0.95Eu 0.05(BO 3) 3The exciting light spectrogram of borate red luminescent material, the monitoring wavelength X EmBe 600nm.Fig. 4 is the Sr of the embodiment of the invention 1 3Y 0.95Eu 0.05(BO 3) 3The emmission spectrum figure of borate red luminescent material, excitation wavelength lambda ExBe 172nm.As seen from Figure 4, the Sr of present embodiment 3Y 0.95Eu 0.05(BO 3) 3Borate red luminescent material is that the 600nm place launches ruddiness at wavelength, has good luminescent properties.
Embodiment 2
Take by weighing Strontium carbonate powder SrCO 32.2145g, lanthanum trioxide La 2O 30.7738g, boric acid H 3BO 31.0202g europium sesquioxide Eu (10%), 2O 30.0440g and Calcium Fluoride (Fluorspan) CaF 20.0098g (2.5%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 1000 ℃, cooling promptly gets Sr after the grinding 3La 0.95Eu 0.05(BO 3) 3Borate red luminescent material.
Embodiment 3
Take by weighing barium carbonate BaCO 32.9600g, yttrium oxide Y 2O 30.5361g, boric acid H 3BO 31.0202g europium sesquioxide Eu (10%), 2O 30.0440g and Calcium Fluoride (Fluorspan) CaF 20.0098g, magnesium fluoride MgF 20.0078g (5%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 1200 ℃, cooling promptly gets Ba after the grinding 3Y 0.95Eu 0.05(BO 3) 3Borate red luminescent material.
Embodiment 4
Take by weighing lime carbonate CaCO 31.5013g, yttrium oxide Y 2O 30.5361g, boric acid H 3BO 31.0202g europium sesquioxide Eu (10%), 2O 30.0440g and Calcium Fluoride (Fluorspan) CaF 20.0098g (2.5%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, fully grind once more at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 950 ℃, cooling promptly gets Ca after the grinding 3Y 0.95Eu 0.05(BO 3) 3Borate red luminescent material.
Embodiment 5
Take by weighing lime carbonate CaCO 31.5013g, lanthanum trioxide La 2O 30.7738g, boric acid H 3BO 31.0202g europium sesquioxide Eu (10%), 2O 30.0440g and magnesium fluoride MgF 20.0078g (2.5%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 950 ℃, cooling promptly gets Ca after the grinding 3La 0.95Eu 0.05(BO 3) 3Borate red luminescent material.
Embodiment 6
Take by weighing Strontium carbonate powder SrCO 32.2145g, gadolinium sesquioxide Gd 2O 30.8609g, boric acid H 3BO 31.0202g europium sesquioxide Eu (10%), 2O 30.0440g and magnesium fluoride MgF 20.0078g (25%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 1000 ℃, the room temperature cooling promptly gets Sr after the grinding 3Gd 0.95Eu 0.05(BO 3) 3Borate red luminescent material.
Embodiment 7
Take by weighing nitrate of baryta Ba (NO 3) 23.9201g, gadolinium sesquioxide Gd 2O 30.8609g, boric acid H 3BO 31.0202g Samarium trioxide Sm (10%), 2O 30.0436g and magnesium fluoride MgF 20.0078g (2.5%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 1000 ℃, the room temperature cooling promptly gets Ba after the grinding 3Gd 0.95Sm 0.05(BO 3) 3Borate red luminescent material.
Fig. 2 is the Ba of the embodiment of the invention 7 3Gd 0.95Sm 0.05(BO 3) 3The exciting light spectrogram of borate red luminescent material, the monitoring wavelength X EmBe 599nm.Fig. 5 is the Ba of the embodiment of the invention 7 3Gd 0.95Sm 0.05(BO 3) 3The emmission spectrum figure of borate red luminescent material, excitation wavelength lambda EmBe 172nm.As seen from Figure 5, the Ba of present embodiment 3Gd 0.95Sm 0.05(BO 3) 3Borate red luminescent material is that the 599nm place launches ruddiness at wavelength, has good luminescent properties.
Embodiment 8
Take by weighing barium carbonate BaCO 32.9600g, gadolinium sesquioxide Gd 2O 30.8609g, boric acid H 3BO 31.0202g europium sesquioxide Eu (10%), 2O 30.0440g and Calcium Fluoride (Fluorspan) CaF 20.0098g (2.5%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 1200 ℃, the room temperature cooling promptly gets Ba after the grinding 3Gd 0.95Eu 0.05(BO 3) 3Borate red luminescent material.
Fig. 3 is the Ba of the embodiment of the invention 8 3Gd 0.95Eu 0.05(BO 3) 3The exciting light spectrogram of borate red luminescent material, the monitoring wavelength is respectively λ Em=600nm and λ Em=311nm.Fig. 6 is the Ba of the embodiment of the invention 8 3Gd 0.95Eu 0.05(BO 3) 3The emmission spectrum figure of borate red luminescent material, excitation wavelength lambda ExBe 172nm.Among Fig. 3, λ EmThe excitation spectrum of=600nm indication is the Ba of present embodiment 3Gd 0.95Eu 0.05(BO 3) 3The excitation spectrum of borate red luminescent material, λ EmThe excitation spectrum of=311nm indication is the Ba of present embodiment 3Gd 0.95Eu 0.05(BO 3) 3Gd after borate red luminescent material is stimulated 3+Ionic excitation spectrum, i.e. Ba 3Gd 0.95(BO 3) 3Matrix is after the carrying out of the vacuum-ultraviolet light of 150～175nm absorbs by force to wavelength, realizes matrix sensitization Gd 3+The highly excited level energy level, Gd 3+Give Eu with transmission ofenergy again 3+Ionoluminescence.As seen from Figure 6, the Ba of present embodiment 3Gd 0.95Eu 0.05(BO 3) 3Borate red luminescent material is that the 600nm place launches ruddiness at wavelength, has good luminescent properties.
Embodiment 9
Take by weighing lime carbonate CaCO 31.5013g, Gadolinium trinitrate Gd (NO 3) 36H 2O 2.1435g, boric acid H 3BO 31.0202g europium nitrate Eu (NO (10%), 3) 36H 2O 0.1115g and magnesium fluoride MgF 20.0078g (2.5%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 950 ℃, the room temperature cooling promptly gets Ca after the grinding 3Gd 0.95Eu 0.05(BO 3) 3Borate red luminescent material.
Embodiment 10
Take by weighing barium carbonate BaCO 32.9600g, gadolinium sesquioxide Gd 2O 30.8156g, yttrium oxide Y 2O 30.0282g, boric acid H 3BO 31.0202g europium sesquioxide Eu (10%), 2O 30.0440g and Calcium Fluoride (Fluorspan) CaF 20.0098g, magnesium fluoride MgF 20.0078g (5%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 1200 ℃, cooling promptly gets Ba after the grinding 3Gd 0.90Y 0.05Eu 0.05(BO 3) 3Borate red luminescent material.
Embodiment 11
Take by weighing calcium oxide CaO 0.8412g, lanthanum trioxide La 2O 30.8105g, boric acid H 3BO 31.2057g europium sesquioxide Eu (30%), 2O 30.0044g and barium fluoride BaF 20.0701g (8%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 200 ℃ of following presintering 5h.At last, the regrinding product is calcined 24h down at 900 ℃, cooling promptly gets Ca after the grinding 3La 0.995Eu 0.005(BO 3) 3Borate red luminescent material.
Embodiment 12
Take by weighing hydrated barta Ba (OH) 22.5701g, Yttrium trinitrate Y (NO 3) 36H 2O 0.9573g, boric acid H 3BO 31.0202g europium nitrate Eu (NO (10%), 3) 36H 2O 1.1149g and boric acid H 3BO 30.0031g (1%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 700 ℃ of following presintering 2h.At last, the regrinding product is calcined 1h down at 1300 ℃, cooling promptly gets Ba after the grinding 3Y 0.50Eu 0.50(BO 3) 3Borate red luminescent material.
Embodiment 13
Take by weighing nitrate of baryta Ba (NO 3) 23.9201g, lanthanum nitrate La (NO 3) 36H 2O 2.1105g, boric acid H 3BO 31.1129g europium nitrate Eu (NO (20%), 3) 36H 2O 0.0557g and magnesium fluoride MgF 20.0312g (10%).After placing agate mortar fully to grind above-mentioned raw materials and the fusing assistant, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 600 ℃ of following presintering 3h.At last, the regrinding product is calcined 10h down at 1000 ℃, cooling promptly gets Ba after the grinding 3La 0.975Eu 0.025(BO 3) 3Borate red luminescent material.
Embodiment 14
Take by weighing nitrate of baryta Ba (NO 3) 23.9201g, gadolinium sesquioxide Gd 2O 30.6797g, boric acid H 3BO 31.0202g Samarium trioxide Sm (10%), 2O 30.2179g and magnesium fluoride MgF 20.0078g (2.5%).After placing agate mortar fully to grind the above-mentioned all substances, put into corundum crucible, be cooled to room temperature then, take out once more and fully grind at 500 ℃ of following presintering 2h.At last, the regrinding product is calcined 5h down at 1000 ℃, the room temperature cooling promptly gets Ba after the grinding 3Gd 0.75Sm 0.25(BO 3) 3Borate red luminescent material.
The above only is representative embodiment of the present invention, does not limit the present invention in any way, and all any modifications of being done within the spirit and principles in the present invention, is equal to and replaces or improvement etc., all should be included within protection scope of the present invention.
For example, after all raw materials and fusing assistant presintering at a lower temperature,, also be fine 900～1300 ℃ of following calcinings then without regrinding.

Claims (10)

1. a borate red luminescent material is characterized in that, its chemical formula is M 3Ln 1-xRe x(BO 3) 3, wherein, M is Ca, Sr or Ba, and Ln is at least a among Y, La, the Gd, and Re is Eu or Sm, and the span of x is 0.005≤x≤0.50.
2. borate red luminescent material according to claim 1 is characterized in that, the span of described x is 0.025≤x≤0.25.
3. the preparation method of a borate red luminescent material is characterized in that, may further comprise the steps:
1. be raw material to contain the M compound, to contain the Ln compound, contain the Re compound, contain the B compound, according to M 3Ln 1-xRe x(BO 3) 3In each element molar ratio and make and contain the B compound and take by weighing each raw material by above-mentioned molar ratio excessive 5～30%, and according to M 3Ln 1-xRe x(BO 3) 3Molar ratio 1～10% take by weighing fusing assistant, ground and mixed evenly forms compound, wherein, M is Ca, Sr or Ba, Ln is at least a among Y, La, the Gd, Re is Eu or Sm, the span of x is 0.005≤x≤0.50;
2. compound is first 200～700 ℃ of following presintering, then 900～1300 ℃ of calcinings down;
3. step calcinate 2. is cooled to room temperature, promptly obtains borate red luminescent material.
4. the preparation method of borate red luminescent material according to claim 3 is characterized in that, the span of described x is 0.025≤x≤0.25.
5. the preparation method of borate red luminescent material according to claim 3, it is characterized in that, at least a in the oxide compound that the described M of containing compound is M, oxyhydroxide, nitrate, the carbonate, oxide compound or nitrate that the described Ln of containing compound is Ln, oxide compound or nitrate that the described Re of containing compound is Re, the described B of containing compound is a boric acid.
6. the preparation method of borate red luminescent material according to claim 3 is characterized in that, described fusing assistant is at least a in boric acid, barium fluoride, magnesium fluoride, the Calcium Fluoride (Fluorspan).
7. the preparation method of borate red luminescent material according to claim 3 is characterized in that, the presintering time of described step in 2. is 2～7h.
8. the preparation method of borate red luminescent material according to claim 3 is characterized in that, the calcination time of described step in 2. is 1～24h.
9. the preparation method of borate red luminescent material according to claim 8 is characterized in that, the calcining temperature of described step in 2. is 1000～1200 ℃, and calcination time is 5～10h.
10. according to the preparation method of the arbitrary described borate red luminescent material of claim 3～9, it is characterized in that 2. described step is: prior to 200～700 ℃ of presintering, cooling presintering product is to room temperature with compound, grind, and then in 900～1300 ℃ of calcinings.
CN2010101257185A 2010-03-15 2010-03-15 Borate red luminescent material and preparation method thereof Pending CN102191052A (en)

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