CN101747895A - Green luminescent material and preparation method thereof - Google Patents

Green luminescent material and preparation method thereof Download PDF

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CN101747895A
CN101747895A CN200910188927A CN200910188927A CN101747895A CN 101747895 A CN101747895 A CN 101747895A CN 200910188927 A CN200910188927 A CN 200910188927A CN 200910188927 A CN200910188927 A CN 200910188927A CN 101747895 A CN101747895 A CN 101747895A
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luminescent material
green luminescent
compound
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周明杰
刘军
梁小芳
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 relates to a green luminescent material and a preparation method thereof. The green luminescent material adopts a chemical formula of M1-x-y-zGdxTbyNzAl2B2O7, wherein M is at least one component among Ca, Sr and Ba, N is Li, Na and K, the value range of x meets the relationship, i.e., 0.02 Less than or equal x Less than or equal 0.3, the value range of y meets the relationship, i.e., 0.01 Less than or equal y Less than or equal 0.4, z=x+y, and 1-x-y-z>0. The preparation method comprises the following steps: weighing all the raw materials according to the proportion, then fully grinding the raw materials, presintering the ground raw materials at the lower temperature, calcining for 2 to 12 h at the temperature of 800-1200 DEG C under the reducing atmosphere, and then grinding after cooling to obtain the green luminescent material. The preparation method is simple, pollution-free and is beneficial to industrialized production; and the obtained green luminescent material is short in afterglow time and high in luminous intensity, has the excellent luminous performance and can be widely used for a PDP or mercury-free fluorescent lamp.

Description

Green luminescent material and preparation method thereof
Technical field
The invention belongs to the luminescent material technical field, more particularly, relate to a kind of green luminescent material and preparation method thereof.
Background technology
In recent years, along with chromatic plasma flat pannel display (Plasma Display Panel, hereinafter to be referred as PDP) development of technology and to the pay attention to day by day of environmental protection, develop no mercury light source and become one of people's priority fields of study, wherein, efficient, the stable red, green, blue three-colour light-emitting material of research and development is one of gordian technique that solves subject matter in this field.
At present, commercial luminescent material mainly contains red illuminating material Y 2O 3: Eu 3+, (Y, Gd) BO 3: Eu 3+, green luminescent material Zn 2SiO 4: Mn 2+, BaAl 12O 19: Mn 2+With blue emitting material Y 2SiO 5: Ce 3+, LaPO 4: Tm 3+, BaMgAl 10O 17: Eu 2+Yet, green luminescent material Zn 2SiO 4: Mn 2+And BaAl 12O 19: Mn 2+With Mn 2+Be luminescence center, because Mn 2+Spin-forbidden transition 4T 1→ 6A 1Cause time of persistence long, be unfavorable for the demonstration of dynamic menu.Though can be by improving Mn 2+The ionic doping content reduces its time of persistence, but luminous intensity also sharply descends thereupon.Therefore, the new green luminescent material of exploitation is extremely urgent.
Summary of the invention
The technical problem to be solved in the present invention is, at the above-mentioned defective of prior art, provide a kind of luminous intensity height, sunset glow time short can be by the green luminescent material of vacuum ultraviolet (VUV) optical excitation.
The technical problem that the present invention further will solve is, a kind of preparation method of green luminescent material also is provided.
The technical solution adopted for the present invention to solve the technical problems is: a kind of green luminescent material, its chemical formula are M 1-x-y-zGd xTb yN zAl 2B 2O 7, wherein, M is at least a among Ca, Sr, the Ba, and N is Li, Na or K, and the span of x is 0.02≤x≤0.3, and the span of y is 0.01≤y≤0.4, z=x+y, and 1-x-y-z＞0.
Excite in the green luminescent material of the present invention, the span of described x is preferably 0.05≤x≤0.15, and the span of y is preferably 0.05≤y≤0.2.
A kind of preparation method of green luminescent material may further comprise the steps:
1. be raw material to contain the M compound, to contain the Gd compound, contain the Tb compound, contain the N compound, contain the Al compound, contain the B compound, molar ratio by each element in the above-mentioned chemical formula takes by weighing each raw material, and make and contain B compound routine in molar ratio excessive 5%～30%, the above-mentioned raw materials ground and mixed is evenly formed compound
2. the compound that 1. step is made is at 200～500 ℃ of following presintering 1～5h;
3. step presintering product 2. is cooled to room temperature, grinds evenly;
4. step grinding product is 3. calcined in reducing atmosphere, calcining temperature is 800～1200 ℃, and calcination time is 2～12h;
5. step calcinate 4. is cooled to room temperature, promptly obtains green luminescent material.
Wherein, the described M of containing compound is preferably carbonate, oxyhydroxide or the oxalate of M; The described Gd of containing compound is preferably oxide compound, nitrate or the oxalate of Gd; The described Tb of containing compound is preferably oxide compound, nitrate or the oxalate of Tb; The described N of containing compound is preferably the carbonate of N; The described Al of containing compound is preferably aluminum oxide or aluminium hydroxide; The described B of containing compound is preferably boron oxide or boric acid; Step 4. in, reducing atmosphere is preferably the atmosphere that forms with the mixed gas of nitrogen and hydrogen, hydrogen or CO (carbon monoxide converter) gas, calcining temperature is preferably 900～1100 ℃, calcination time is preferably 4～10h; Step 5. in, preferably, step calcinate 4. is cooled to room temperature after, grind, obtain green luminescent material of the present invention.
The present invention adopts Tb 3+As the luminescence center of green luminescent material, Tb 3+The feature transition 5D 4→ 7F 5Can launch the green glow that wavelength is 543nm, because the spin coupling to the shielding of spin forbidden, make green luminescent material of the present invention have short time of persistence, and cancellation concentration is also higher, thereby has been overcome Mn 2+The shortcoming that time of persistence is long.
The present invention adopts the matrix of borate as green luminescent material, because borate has good vacuum ultraviolet (VUV) receptivity, good luminescent properties, stable physics-chem characteristic and the good ability of vacuum-resistant ultraviolet radiation and anti-ion bombardment, so green luminescent material of the present invention also has excellent performance.
The present invention adopts Gd 3+As the sensitizing agent of green luminescent material, because Gd 3+Ion is sensitization Tb well 3+Ion and raising Tb 3+Luminous intensity, can also improve the receptivity of green luminescent material of the present invention to vacuum-ultraviolet light, therefore, Gd 3+Doping improved the luminous intensity of green luminescent material of the present invention greatly.
Also be doped with alkaline-earth metal ions in the green luminescent material of the present invention, pass through Ca 2+, Sr 2+, Ba 2+Doping change band gap, thereby improved the luminescent properties of luminescent material.
The present invention also adopts the charge compensation agent of alkalimetal ion as green luminescent material, because alkaline-earth metal ions and Gd 3+, Tb 3+Between have charge differences, influence illumination effect, the present invention is according to the radius size of alkaline earth ion, optionally Li doped +, Na +Or K +Ion is as the charge compensation agent, thereby improved the luminescent properties of green luminescent material.
Green luminescent material of the present invention is compared with existing commercial green luminescent material, not only has short time of persistence, be beneficial to the demonstration of dynamic menu, and has a good luminous intensity, possesses better luminescent properties, can be widely used in PDP or the non-mercury florescent lamp, have broad application prospects.
The preparation method of green luminescent material of the present invention has advantages such as simple to operate, pollution-free, that processing condition are easy to control, preparation temperature is low, and save energy is beneficial to suitability for industrialized production.
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 6 preparations 0.86Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7The exciting light spectrogram of green luminescent material, supervisory wavelength are 543nm;
Fig. 2 is the Sr of the embodiment of the invention 2 preparations 0.76Gd 0.02Tb 0.10Na 0.12Al 2B 2O 7The Sr of green luminescent material, embodiment 3 preparations 0.76Gd 0.02Tb 0.10Li 0.12Al 2B 2O 7The Sr of green luminescent material and embodiment 4 preparations 0.76Gd 0.02Tb 0.10K 0.12Al 2B 2O 7The emmission spectrum figure of green luminescent material, excitation wavelength is 172nm;
Fig. 3 is the Sr of the embodiment of the invention 6 preparations 0.86Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7The Sr of green luminescent material and comparative example preparation 0.90Tb 0.05Na 0.05Al 2B 2O 7The emmission spectrum comparison diagram of green luminescent material, excitation wavelength are 172nm;
Fig. 4 is the Sr of the embodiment of the invention 7 preparations 0.81Ba 0.05Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7The twilight sunset life test figure of green luminescent material, τ=2.35ms.
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.But, should be appreciated that protection scope of the present invention is not subjected to the restriction of these embodiment.
In an embodiment of the present invention, usedly contain Gd or the Tb compound is its corresponding oxide compound, nitrate or oxalate, its purity is more than the 4N, and promptly purity reaches more than 99.99%; The used B of containing compound is analytically pure boron oxide or boric acid; Used analytically pure carbonate, oxyhydroxide or the oxalate that contains the compound of Ca, Sr or Ba for its correspondence; The used analytically pure carbonate that contains the compound of Li, Na or K for its correspondence; The used Al of containing compound is analytically pure aluminum oxide or aluminium hydroxide.
In the preparation, molar ratio according to each element in the chemical formula takes by weighing each raw material, and make and contain B compound routine in molar ratio excessive 5%～30%, with all raw material ground and mixed evenly after, compound at 200～500 ℃ of following presintering 1～5h, is cooled to room temperature and grinds, again under reducing atmosphere in high-temperature calcination, after cooling, promptly get green luminescent material of the present invention.Use for convenience, can be with green luminescent material grind into powder of the present invention.
Embodiment 1Ca 0.76Gd 0.02Tb 0.10Na 0.12Al 2B 2O 7Green luminescent material
Take by weighing lime carbonate CaCO 30.3803g, aluminium hydroxide Al (OH) 30.7800g, boric acid H 3BO 3(0.7419g excessive 20%), yellow soda ash Na 2CO 30.0318g, terbium sesquioxide Tb 4O 70.0934g and gadolinium sesquioxide Gd 2O 30.0181g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 500 ℃ of following presintering 2h.At last, in volume ratio be 95: 5 N 2And H 2In the reducing atmosphere that mixed gas forms, the presintering product that fully grinds is calcined 10h down at 900 ℃, naturally cool to room temperature, promptly get white powder shaped Ca after the grinding 0.76Gd 0.02Tb 0.10Na 0.12Al 2B 2O 7Green luminescent material.
Embodiment 2Sr 0.76Gd 0.02Tb 0.10Na 0.12Al 2B 2O 7Green luminescent material
Take by weighing Strontium carbonate powder SrCO 30.5610g, aluminium hydroxide Al (OH) 30.7800g, boric acid H 3BO 3(0.7419g excessive 20%), yellow soda ash Na 2CO 30.0318g, terbium sesquioxide Tb 4O 70.0934g and gadolinium sesquioxide Gd 2O 30.0181g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 500 ℃ of following presintering 2h.At last, in volume ratio be 95: 5 N 2And H 2In the reducing atmosphere that mixed gas forms, the presintering product that fully grinds is calcined 10h down at 960 ℃, naturally cool to room temperature, promptly get white powder shaped Sr after the grinding 0.76Gd 0.02Tb 0.10Na 0.12Al 2B 2O 7Green luminescent material.
The Sr of present embodiment preparation 0.76Gd 0.02Tb 0.10Na 0.12Al 2B 2O 7The emmission spectrum of green luminescent material under the vacuum ultraviolet (VUV) optical excitation is shown among Fig. 2 21, and as can be seen, green luminescent material of the present invention has very strong luminous intensity.
Embodiment 3Sr 0.76Gd 0.02Tb 0.10Li 0.12Al 2B 2O 7Green luminescent material
Take by weighing Strontium carbonate powder SrCO 30.5610g, aluminium hydroxide Al (OH) 30.7800g, boric acid H 3BO 3(0.7419g excessive 20%), Quilonum Retard Li 2CO 30.0221g, terbium sesquioxide Tb 4O 70.0934g and gadolinium sesquioxide Gd 2O 30.0181g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 500 ℃ of following presintering 2h.At last, at H 2In the reducing atmosphere that forms, the presintering product that fully grinds is calcined 10h down at 960 ℃, naturally cool to room temperature, promptly get white powder shaped Sr after the grinding 0.76Gd 0.02Tb 0.10Li 0.12Al 2B 2O 7Green luminescent material.
The Sr of present embodiment preparation 0.76Gd 0.02Tb 0.10Li 0.12Al 2B 2O 7The emmission spectrum of green luminescent material under the vacuum ultraviolet (VUV) optical excitation is shown among Fig. 2 23, and as can be seen, green luminescent material of the present invention has very strong luminous intensity.
Embodiment 4Sr 0.76Gd 0.02Tb 0.10K 0.12Al 2B 2O 7Green luminescent material
Take by weighing Strontium carbonate powder SrCO 30.5610g, aluminium hydroxide Al (OH) 30.7800g, boric acid H 3BO 3(0.7419g excessive 20%), salt of wormwood K 2CO 30.0414g, terbium sesquioxide Tb 4O 70.0934g and gadolinium sesquioxide Gd 2O 30.0181g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 500 ℃ of following presintering 2h.At last, at H 2In the reducing atmosphere that forms, the presintering product that fully grinds is calcined 10h down at 960 ℃, naturally cool to room temperature, promptly get white powder shaped Sr after the grinding 0.76Gd 0.02Tb 0.10K 0.12Al 2B 2O 7Green luminescent material.
The Sr of present embodiment preparation 0.76Gd 0.02Tb 0.10K 0.12Al 2B 2O 7The emmission spectrum of green luminescent material under the vacuum ultraviolet (VUV) optical excitation is shown among Fig. 2 22, and as can be seen, green luminescent material of the present invention has very strong luminous intensity.
Embodiment 5Ba 0.76Gd 0.02Tb 0.10K 0.12Al 2B 2O 7Green luminescent material
Take by weighing barium carbonate BaCO 30.7498g, aluminium hydroxide Al (OH) 30.7800g, boric acid H 3BO 3(0.7419g excessive 20%), salt of wormwood K 2CO 30.0414g, terbium sesquioxide Tb 4O 70.0934g and gadolinium sesquioxide Gd 2O 30.0181g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 500 ℃ of following presintering 2h.At last, in the reducing atmosphere that CO forms, the presintering product that fully grinds is calcined 10h down at 950 ℃, naturally cool to room temperature, promptly get white powder shaped Ba after the grinding 0.76Gd 0.02Tb 0.10K 0.12Al 2B 2O 7Green luminescent material.
Embodiment 6Sr 0.86Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7Green luminescent material
Take by weighing Strontium carbonate powder SrCO 30.6348g, aluminium hydroxide Al (OH) 30.7800g, boric acid H 3BO 3(0.7419g excessive 20%), yellow soda ash Na 2CO 30.0186g, terbium sesquioxide Tb 4O 70.0467g and gadolinium sesquioxide Gd 2O 30.0181g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 500 ℃ of following presintering 2h.At last, in the reducing atmosphere that CO forms, the presintering product that fully grinds is calcined 10h down at 960 ℃, naturally cool to room temperature, promptly get white powder shaped Sr after the grinding 0.86Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7Green luminescent material.
Fig. 1 is the Sr of present embodiment 0.86Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7The exciting light spectrogram of green luminescent material, supervisory wavelength are 543nm.Fig. 3 is the Sr of present embodiment preparation 0.86Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7Green luminescent material and Sr comparative example preparation 0.90Tb 0.05Na 0.05Al 2B 2O 7The emmission spectrum comparison diagram of green luminescent material under the vacuum ultraviolet (VUV) optical excitation.As shown in Figure 3, the 31st, the Sr of comparative example preparation 0.90Tb 0.05Na 0.05Al 2B 2O 7The emmission spectrum of luminescent material, the 32nd, the Sr of present embodiment preparation 0.86Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7The emmission spectrum of green luminescent material as can be seen, is compared with comparative example, and the green luminescent material luminous intensity of present embodiment significantly improves, and has better luminescent properties.
Embodiment 7Sr 0.81Ba 0.05Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7Green luminescent material
Take by weighing Strontium carbonate powder SrCO 31.1958g, barium carbonate BaCO 30.0987g, aluminium hydroxide Al (OH) 31.5601g, boric acid H 3BO 3(1.4839g excessive 20%), yellow soda ash Na 2CO 30.0371g, terbium sesquioxide Tb 4O 70.0934g and gadolinium sesquioxide Gd 2O 30.0362g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 500 ℃ of following presintering 2h.At last, at H 2In the reducing atmosphere that forms, the presintering product that fully grinds is calcined 8h down at 960 ℃, naturally cool to room temperature, promptly get white powder shaped Sr after the grinding 0.81Ba 0.05Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7Green luminescent material.
Fig. 4 is the Sr of present embodiment preparation 0.81Ba 0.05Gd 0.02Tb 0.05Na 0.07Al 2B 2O 7The twilight sunset life test figure of green luminescent material.As shown in Figure 4, the twilight sunset life-span τ=2.35ms of green luminescent material of the present invention, time of persistence is short, is beneficial to the demonstration of dynamic menu.
Embodiment 8Ca 0.30Sr 0.08Gd 0.30Tb 0.01Na 0.31Al 2B 2O 7Green luminescent material
Take by weighing caoxalate CaC 2O 40.3842g, Strontium oxalate (1:1) monohydrate SrC 2O 4H 2O 0.1549g, aluminium oxide Al 2O 31.0196g, boric acid H 3BO 3(1.6076g excessive 30%), yellow soda ash Na 2CO 30.1642g, six nitric hydrate terbium Tb (NO 3) 36H 2O 0.0452g and six nitric hydrate gadolinium Gd (NO 3) 36H 2O 1.3537g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 200 ℃ of following presintering 5h.At last, in volume ratio be 95: 5 N 2And H 2In the reducing atmosphere that mixed gas forms, the presintering product that fully grinds is calcined 12h down at 800 ℃, naturally cool to room temperature, promptly get white powder shaped Ca after the grinding 0.30Sr 0.08Gd 0.30Tb 0.01Na 0.31Al 2B 2O 7Green luminescent material.
Embodiment 9Ca 0.10Ba 0.06Gd 0.02Tb 0.40Li 0.42Al 2B 2O 7Green luminescent material
Take by weighing calcium hydroxide Ca (OH) 20.0074g, hydrated barta Ba (OH) 20.1028g, aluminium hydroxide Al (OH) 31.5600g, boric acid H 3BO 3(1.4840g excessive 20%), Quilonum Retard Li 2CO 30.1551g, oxalic acid terbium Tb 2(C 2O 4) 31.1638g and ten oxalic acid hydrate gadolinium Gd 2(C 2O 4) 310H 2O 0.0758g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 300 ℃ of following presintering 3h.At last, at H 2In the reducing atmosphere that forms, the presintering product that fully grinds is calcined 10h down at 900 ℃, naturally cool to room temperature, promptly get white powder shaped Ca after the grinding 0.10Ba 0.06Gd 0.02Tb 0.40Li 0.42Al 2B 2O 7Green luminescent material.
Embodiment 10Ca 0.40Sr 0.05Ba 0.05Gd 0.05Tb 0.20K 0.25Al 2B 2O 7Green luminescent material
Take by weighing caoxalate CaC 2O 40.5122g, Strontium carbonate powder SrCO 30.0738g, hydrated barta Ba (OH) 20.0856g, aluminium oxide Al 2O 31.0196g, boron oxide B 2O 3(0.8006g excessive 15%), salt of wormwood K 2CO 30.1727g, terbium sesquioxide Tb 4O 70.3738g and gadolinium sesquioxide Gd 2O 3: 0.0906g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 400 ℃ of following presintering 2h.At last, at H 2In the reducing atmosphere that forms, the presintering product that fully grinds is calcined 4h down at 1100 ℃, naturally cool to room temperature, promptly get white powder shaped Ca after the grinding 0.40Sr 0.05Ba 0.05Gd 0.05Tb 0.20K 0.25Al 2B 2O 7Green luminescent material.
Embodiment 11Ba 0.60Gd 0.15Tb 0.05K 0.20Al 2B 2O 7Green luminescent material
Take by weighing barium carbonate BaCO 31.1840g, aluminium hydroxide Al (OH) 31.5600g, boron oxide B 2O 3(0.7310g excessive 5%), salt of wormwood K 2CO 30.1382g, oxalic acid terbium Tb 2(C 2O 4) 30.1454g and ten oxalic acid hydrate gadolinium Gd 2(C 2O 4) 310H 2O 0.5689g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 500 ℃ of following presintering 1h.At last, in the reducing atmosphere that CO forms, the presintering product that fully grinds is calcined 2h down at 1200 ℃, naturally cool to room temperature, promptly get white powder shaped Ba after the grinding 0.60Gd 0.15Tb 0.05K 0.20Al 2B 2O 7Green luminescent material.
Comparative example: Sr 0.90Tb 0.05Na 0.05Al 2B 2O 7Green luminescent material
Take by weighing Strontium carbonate powder SrCO 31.3286g, aluminium hydroxide Al (OH) 31.5600g, boric acid H 3BO 3(excessive 20%) 1.4839g, yellow soda ash Na 2CO 30.0264g and terbium sesquioxide Tb 4O 70.0934g.After placing agate mortar fully to grind above-mentioned all raw materials, put into corundum crucible, naturally cool to room temperature then, and fully grind once more at 500 ℃ of following presintering 2h.At last, in the reducing atmosphere that CO forms, the presintering product that fully grinds is calcined 10h down at 960 ℃, naturally cool to room temperature, promptly get white powder shaped Sr after the grinding 0.90Tb 0.05Na 0.05Al 2B 2O 7Green luminescent material.

Claims (10)

1. a green luminescent material is characterized in that, its chemical formula is M 1-x-y-zGd xTb yN zAl 2B 2O 7,
Wherein, M is at least a among Ca, Sr, the Ba, and N is Li, Na or K, and the span of x is 0.02≤x≤0.3, and the span of y is 0.01≤y≤0.4, z=x+y, and 1-x-y-z＞0.
2. green luminescent material according to claim 1 is characterized in that, the span of described x is 0.05≤x≤0.15.
3. green luminescent material according to claim 1 is characterized in that, the span of described y is 0.05≤y≤0.2.
4. the preparation method of a green luminescent material is characterized in that, may further comprise the steps:
1. be raw material to contain the M compound, to contain the Gd compound, contain the Tb compound, contain the N compound, contain the Al compound, contain the B compound, press M 1-x-y-zGd xTb yN zAl 2B 2O 7In the molar ratio of each element take by weighing each raw material, and make and contain B compound routine in molar ratio excessive 5%～30%, the above-mentioned raw materials ground and mixed is evenly formed compound, wherein, M is at least a among Ca, Sr, the Ba, and N is Li, Na or K, the span of x is 0.02≤x≤0.3, the span of y is 0.01≤y≤0.4, z=x+y, and 1-x-y-z＞0:
2. the compound that 1. step is made is at 200～500 ℃ of following presintering 1～5h;
3. step presintering product 2. is cooled to room temperature, grinds evenly;
4. step grinding product is 3. calcined in reducing atmosphere, calcining temperature is 800～1200 ℃, and calcination time is 2～12h;
5. step calcinate 4. is cooled to room temperature, promptly obtains green luminescent material.
5. the preparation method of green luminescent material according to claim 4 is characterized in that, the span of described x is 0.05≤x≤0.15, and the span of described y is 0.05≤y≤0.2.
6. the preparation method of green luminescent material according to claim 4 is characterized in that, carbonate, oxyhydroxide or oxalate that the described M of containing compound is M; Oxide compound, nitrate or oxalate that the described Gd of containing compound is Gd; Oxide compound, nitrate or oxalate that the described Tb of containing compound is Tb; The described N of containing compound is the carbonate of N; The described Al of containing compound is aluminum oxide or aluminium hydroxide; The described B of containing compound is boron oxide or boric acid.
7. the preparation method of green luminescent material according to claim 4 is characterized in that, the reducing atmosphere of described step in 4. is the atmosphere that mixed gas, hydrogen or the CO (carbon monoxide converter) gas with nitrogen and hydrogen forms.
8. the preparation method of green luminescent material according to claim 4 is characterized in that, the calcining temperature of described step in 4. is 900～1100 ℃.
9. the preparation method of green luminescent material according to claim 4 is characterized in that, the calcination time of described step in 4. is 4～10h.
10. the preparation method of green luminescent material according to claim 4 is characterized in that, 5. described step is: step calcinate 4. is cooled to room temperature, grinds, promptly obtain described green luminescent material.
CN200910188927A 2009-12-14 2009-12-14 Green luminescent material and preparation method thereof Pending CN101747895A (en)

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Cited By (1)

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CN105802617A (en) * 2016-04-07 2016-07-27 上海应用技术学院 Method for improving luminescent property of SrAl2B2O7:Tb<3+> green fluorescent powder

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Application publication date: 20100623