CN102115669B - Boron aluminate luminescent material capable of generating green light and preparation method thereof - Google Patents

Boron aluminate luminescent material capable of generating green light and preparation method thereof Download PDF

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Publication number
CN102115669B
CN102115669B CN 200910239627 CN200910239627A CN102115669B CN 102115669 B CN102115669 B CN 102115669B CN 200910239627 CN200910239627 CN 200910239627 CN 200910239627 A CN200910239627 A CN 200910239627A CN 102115669 B CN102115669 B CN 102115669B
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aluminate luminescent
boron
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CN102115669A (en
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周明杰
梁小芳
刘军
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
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Abstract

The invention relates to a boron aluminate luminescent material capable of generating green light and a preparation method thereof. The chemical formula of the luminescent material capable of generating green light is M1-x-y-zGdxTbyNzAl3BO7, wherein M is at least one of Ba, Sr, N is Na, Li or K, and x, y, and z satisfy the relations: 0.001 <= x <= 0.20, 0.005 <= y <= 0.50, 0.02 <= z <= 0.30, 1-x-y-z > 0. The preparation method comprises the steps: weighing raw materials and a flux in proportion; grinding and mixing well, then pre-sintering under a lower temperature; then calcining under a temperature of 900 to 1100 DEG C for 1 to 24 hours; grinding after cooling; and obtaining the boron aluminate luminescent material capable of generating green light of the invention. The method of the invention is simple, has no pollution, and is benefit for industrial production. The obtained luminescent material capable of generating green light has short afterglow, high luminous intensity and excellent luminous performance, and can be widely used for PDP or mercury-free fluorescent lamp.

Description

Boron aluminate luminescent and preparation method thereof
Technical field
The invention belongs to the luminescent material technical field, more particularly, relate to a kind of boron aluminate luminescent and preparation method thereof.
Background technology
In recent years, luminescent material under the vacuum ultraviolet (VUV) optical excitation becomes more and more important, it one of is mainly used is large color screen high-resolution plasma flat-panel display (PDP), PDP utilizes Xe, the vacuum ultraviolet rays that the noble gas discharges such as Ar produce excites different fluorescent material to produce respectively red, green, blue three primary colours light, thereby obtains coloured image.Vacuum ultraviolet rays excites the quality of lower fluorescent material directly to determine the quality of coloured image and the life-span of device, plays an important role in the PDP technology.
Now widely used three primary colors fluorescent powder luminescent material mainly contains: rouge and powder Y 2O 3: Eu 3+, (Y, Gd) BO 3: Eu 3+, green powder Zn 2SiO 4: Mn 2+, BaAl 12O 19: Mn 2+With blue powder BaMgAl 10O 17: Eu 2+Yet green emitting phosphor is with Mn 2+Be luminescence center, due to Mn 2+Spin-forbidden transition 4T 1→ 6A 1Cause time of persistence long, be unfavorable for the demonstration of dynamic menu.Although can be by improving Mn 2+The doping content of ion reduces its time of persistence, but luminous intensity also sharply descends thereupon.Therefore, the new green light-emitting fluorescent powder material of exploitation is extremely urgent.
Summary of the invention
The technical problem to be solved in the present invention is, for the defects of prior art, provides the boron aluminate luminescent that a kind of luminous intensity is high, time of persistence is short.
The technical problem that the present invention further will solve is, a kind of preparation method of boron aluminate luminescent also is provided.
The technical solution adopted for the present invention to solve the technical problems is: a kind of boron aluminate luminescent, its chemical formula are M 1-x-y-zGd xTb yN zAl 3BO 7
Wherein, M is at least a in Ba, Sr, and N is Na, Li or K, and the span of x is 0.001≤x≤0.20, and the span of y is 0.005≤y≤0.50, and the span of z is 0.02≤z≤0.30, and 1-x-y-z＞0.
In boron aluminate luminescent of the present invention, preferably, the span of described x is 0.01≤x≤0.10, and the span of described y is 0.01≤y≤0.20, and the span of described z is 0.02≤z≤0.20.
A kind of preparation method of boron aluminate luminescent comprises the following steps:
1. take contain the M compound, contain the N compound, contain the Gd compound, contain the Tb compound, contain the Al compound, boride alloy is as raw material, molar ratio by each element in above-mentioned chemical formula takes each raw material, and adding fusing assistant by 5%～30% of raw material gross weight, ground and mixed evenly forms compound;
2. the compound of 1. step being made is at 200～700 ℃ of lower presintering 2～5h;
3. step presintering product 2. is cooled to room temperature, grinds;
4. with step grinding product calcining 3., calcining temperature is 900～1100 ℃, and calcination time is 1～24h;
5. step calcinate 4. is cooled to room temperature, namely obtains boron aluminate luminescent.
Wherein, preferably, at least a in the oxide compound that the described M of containing compound is M, oxyhydroxide, nitrate, carbonate, the described N of containing compound is the carbonate of N, oxide compound or nitrate that the described Gd of containing compound is Gd, oxide compound or nitrate that the described Tb of containing compound is Tb, at least a in the oxide compound that the described Al of containing compound is Al, oxyhydroxide, nitrate, carbonate, described boride alloy is boric acid or boron oxide, and described fusing assistant is at least a in boric acid, boron oxide, barium fluoride; Step 4. in, described calcining temperature is preferably 950～1050 ℃, described calcination time is preferably 4～14h; Step 5. in, preferably, step calcinate 4. is cooled to after room temperature its grinding, namely obtain boron aluminate luminescent of the present invention.
The luminescence mechanism of boron aluminate luminescent of the present invention is: be the strong absorption of the vacuum-ultraviolet light (VUV) of 150～175nm by aluminium borate matrix to wavelength, with transmission ofenergy to Gd 3+, then pass through Gd 3+ 6P JEnergy level and Tb 3+Between the transmission ofenergy that exists with transmission ofenergy to Tb 3+Tb 3+After absorbing energy, by the f-f transition radiation, launch green photon.Gd 3+ 6P JEnergy level and Tb 3+Between energy transfer process, strengthened Tb 3+Green emission intensity.
The present invention adopts Tb 3+As the luminescence center of green luminescent material, Tb 3+Feature transition meeting to launch wavelength be green glow in 540～545nm scope, due to the shielding of spin coupling to spin forbidden, make boron aluminate luminescent of the present invention have shorter time of persistence, and cancellation concentration is also higher, thereby has overcome Mn 2+The shortcoming that time of persistence is long.
The present invention adopts aluminium borate as the matrix of green luminescent material, and the aluminium borate stable chemical nature is to exist more by force between 140-180nm to absorb in the vacuum ultraviolet (VUV) optical wavelength, is the good luminescent material matrix that can be used for the vacuum ultraviolet (VUV) optical excitation.
The present invention adopts Gd 3+As the sensitizing agent of green luminescent material, due to Gd 3+Ion is sensitization Tb well 3+Ion improves Tb 3+Luminous intensity, can also improve green luminescent material of the present invention to the receptivity of vacuum-ultraviolet light, therefore, Gd 3+Doping greatly improved the luminous intensity of green luminescent material of the present invention.
Also doped with alkaline-earth metal ions, pass through Ca in green luminescent material of the present invention 2+, Sr 2+, Ba 2+Doping change band gap, thereby improved the luminescent properties of luminescent material.
The present invention also adopts alkalimetal ion as the charge compensation agent of green luminescent material, due to alkaline-earth metal ions and Gd 3+, Tb 3+Between have charge differences, affect illumination effect, according to the radius size of alkaline earth ion, optionally Li doped +, Na +Or K +Ion plays the effect of charge compensation, and keeps the balance of crystalline structure, thereby improves the luminescent properties of green luminescent material of the present invention.
The present invention has also added fusing assistant in preparation process, not only reduced sintering temperature, can also impel each raw material reaction more evenly fully.
Boron aluminate luminescent of the present invention is compared with existing commercial green luminescent material, not only has shorter 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 non-mercury florescent lamp, have broad application prospects.
Preparation method of the present invention has the 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 accompanying drawing:
Fig. 1 is the Sr of the embodiment of the present invention 3 preparations 0.76Gd 0.02Tb 0.1K 0.12Al 3BO 7The exciting light spectrogram of boron aluminate luminescent, supervisory wavelength 543nm;
Fig. 2 is the Sr of the embodiment of the present invention 3 preparations 0.76Gd 0.02Tb 0.1K 0.12Al 3BO 7The Sr of boron aluminate luminescent and comparative example preparation 0.78Tb 0.1Na 0.12Al 3BO 7The utilizing emitted light spectrogram of boron aluminate luminescent, excitation wavelength are 172nm.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is described in further detail.But, should be appreciated that protection scope of the present invention is not subjected to the restriction of these embodiment.
Raw materials usedly in following examples be common commercial goods, required rare earths material purity is more than 4N, and other raw material is analytical pure.In the preparation, take each raw material according to the molar ratio in chemical formula, and add fusing assistant by 5%～30% of raw material gross weight, after all substances ground and mixed is even, compound at 200～700 ℃ of lower presintering 2～5h, is cooled to room temperature and grinds, then in high-temperature calcination, after cooling, namely get boron aluminate luminescent of the present invention.Use for convenient, can be with boron aluminate luminescent grind into powder of the present invention.
Embodiment 1 preparation Sr 0.76Gd 0.02Tb 0.1Na 0.12Al 3BO 7Boron aluminate luminescent
Take Strontium carbonate powder SrCO 30.5610g, aluminium hydroxide Al (OH) 31.1701g, sodium carbonate Na 2CO 30.0319g, boric acid H 3BO 30.3092g, terbium sesquioxide Tb 4O 70.0935g, gadolinium sesquioxide Gd 2O 30.0181g and fusing assistant (5%) boric acid H 3BO 30.1092g.After all substances are placed in the abundant grinding of agate mortar, put into corundum crucible at 600 ℃ of lower presintering 2h, then be cooled to room temperature, again fully grind.At last, grinding product is calcined 5h under 1000 ℃ again, is cooled to room temperature, namely gets Sr after grinding 0.76Gd 0.02Tb 0.1Na 0.12Al 3BO 7Boron aluminate luminescent.
Embodiment 2 preparation Sr 0.76Gd 0.02Tb 0.1Li 0.12Al 3BO 7Boron aluminate luminescent
Take Strontium carbonate powder SrCO 30.5610g, aluminium hydroxide Al (OH) 31.1701g, Quilonum Retard Li 2CO 30.0222g, boric acid H 3BO 30.3092g, terbium sesquioxide Tb 4O 70.0935g, gadolinium sesquioxide Gd 2O 30.0181g and fusing assistant (5%) boric acid H 3BO 30.1087g.After all substances are placed in the abundant grinding of agate mortar, put into corundum crucible at 600 ℃ of lower presintering 2h, then be cooled to room temperature, again fully grind.At last, grinding product is calcined 5h under 1000 ℃ again, is cooled to room temperature, namely gets Sr after grinding 0.76Gd 0.02Tb 0.1Li 0.12Al 3BO 7Boron aluminate luminescent.
Embodiment 3 preparation Sr 0.76Gd 0.02Tb 0.1K 0.12Al 3BO 7Boron aluminate luminescent
Take Strontium carbonate powder SrCO 30.5610g, aluminium hydroxide Al (OH) 31.1701g, salt of wormwood K 2CO 30.0415g, boric acid H 3BO 30.3092g, terbium sesquioxide Tb 4O 70.0935g, gadolinium sesquioxide Gd 2O 30.0181g and fusing assistant (5%) boric acid H 3BO 30.1097g.After all substances are placed in the abundant grinding of agate mortar, put into corundum crucible at 600 ℃ of lower presintering 2h, then be cooled to room temperature, again fully grind.At last, grinding product is calcined 5h under 1000 ℃ again, is cooled to room temperature, namely gets Sr after grinding 0.76Gd 0.02Tb 0.1K 0.12Al 3BO 7Boron aluminate luminescent.
Fig. 1 is the Sr of the present embodiment preparation 0.76Gd 0.02Tb 0.1K 0.12Al 3BO 7The exciting light spectrogram of boron aluminate luminescent, supervisory wavelength are 543nm.Fig. 2 is the boron aluminate luminescent of the present embodiment preparation and the Sr of comparative example preparation 0.78Tb 0.1Na 0.12Al 3BO 7Boron aluminate luminescent utilizing emitted light spectrogram, excitation wavelength are 172nm.As shown in Figure 2, the 21st, the utilizing emitted light spectrogram of the boron aluminate luminescent of the present embodiment, the 22nd, the utilizing emitted light spectrogram of the aluminium borate luminescent material of comparative example, can find out, the green luminescent material of the present embodiment is compared with comparative example, luminous intensity significantly improves, and has more excellent luminescent properties.
Embodiment 4 preparation Ba 0.76Gd 0.02Tb 0.1K 0.12Al 3BO 7Boron aluminate luminescent
Take barium carbonate BaCO 30.7499g, aluminium hydroxide Al (OH) 31.1701g, salt of wormwood K 2CO 30.0415g, boric acid H 3BO 30.3092g, terbium sesquioxide Tb 4O 70.0935g, gadolinium sesquioxide Gd 2O 30.0181g and fusing assistant (10%) boric acid H 3BO 30.2382g.After all substances are placed in the abundant grinding of agate mortar, put into corundum crucible at 600 ℃ of lower presintering 2h, then be cooled to room temperature, again fully grind.At last, grinding product is calcined 5h under 1000 ℃ again, is cooled to room temperature, namely gets Ba after grinding 0.76Gd 0.02Tb 0.1K 0.12Al 3BO 7Boron aluminate luminescent.
Embodiment 5 preparation Sr 0.974Gd 0.001Tb 0.005Na 0.02Al 3BO 7Boron aluminate luminescent
Take strontium oxide SrO 0.5046g, aluminium oxide Al 2O 30.7647g, sodium carbonate Na 2CO 30.0053g, boric acid H 3BO 30.3092g, terbium sesquioxide Tb 4O 70.0048g, gadolinium sesquioxide Gd 2O 30.0009g and fusing assistant (5%) boric acid H 3BO 30.0795g.After all substances are placed in the abundant grinding of agate mortar, put into corundum crucible at 200 ℃ of lower presintering 5h, then be cooled to room temperature, again fully grind.At last, grinding product is calcined 24h under 900 ℃ again, is cooled to room temperature, namely gets Sr after grinding 0.974Gd 0.001Tb 0.005Na 0.02Al 3BO 7Boron aluminate luminescent.
Embodiment 6 preparation Sr 0.96Gd 0.01Tb 0.01Li 0.02Al 3BO 7Boron aluminate luminescent
Take strontium hydroxide Sr (OH) 20.5838g, aluminum nitrate Al (NO 3) 33.1949g, Quilonum Retard Li 2CO 30.0369g, boron oxide B 2O 30.1741g, six nitric hydrate terbium Tb (NO 3) 36H2O 0.0227g, gadolinium nitrate hexahydrate Gd (NO 3) 36H 2O 0.0225g and fusing assistant (10%) boric acid H 3BO 30.4035g.After all substances are placed in the abundant grinding of agate mortar, put into corundum crucible at 400 ℃ of lower presintering 4h, then be cooled to room temperature, again fully grind.At last, grinding product is calcined 14h under 950 ℃ again, is cooled to room temperature, namely gets Sr after grinding 0.96Gd 0.01Tb 0.01Li 0.02Al 3BO 7Boron aluminate luminescent.
Embodiment 7 preparation Ba 0.10Sr 0.10Gd 0.10Tb 0.50K 0.20Al 3BO 7Boron aluminate luminescent
Take nitrate of baryta Ba (NO 3) 20.1307g, strontium nitrate Sr (NO 3) 20.1058g, aluminium carbonate Al 2(CO 3) 31.7549g, salt of wormwood K 2CO 30.0691g, boric acid H 3BO 30.3092g, terbium sesquioxide Tb 4O 70.4673g, gadolinium sesquioxide Gd 2O 30.0906g and fusing assistant (20%) barium fluoride BaF 20.5855g.After all substances are placed in the abundant grinding of agate mortar, put into corundum crucible at 500 ℃ of lower presintering 3h, then be cooled to room temperature, again fully grind.At last, grinding product is calcined 4h under 1050 ℃ again, is cooled to room temperature, namely gets Ba after grinding 0.10Sr 0.10Gd 0.10Tb 0.50K 0.20Al 3BO 7Boron aluminate luminescent.
Embodiment 8 preparation Ba 0.30Gd 0.20Tb 0.20K 0.30Al 3BO 7Boron aluminate luminescent
Take barium carbonate BaCO 30.2960g, aluminium hydroxide Al (OH) 31.1700g, salt of wormwood K 2CO 30.1037g, boric acid H 3BO 30.3092g, terbium sesquioxide Tb 4O 70.1869g, gadolinium sesquioxide Gd 2O 30.1812g and fusing assistant (sum of the two 30%) boric acid H 3BO 30.2309g, barium fluoride BaF 20.4432g.After all substances are placed in the abundant grinding of agate mortar, put into corundum crucible at 700 ℃ of lower presintering 2h, then be cooled to room temperature, again fully grind.At last, grinding product is calcined 1h under 1100 ℃ again, is cooled to room temperature, namely gets Ba after grinding 0.30Gd 0.20Tb 0.20K 0.30Al 3BO 7Boron aluminate luminescent.
Comparative example prepares Sr 0.78Tb 0.1Na 0.12Al 3BO 7Boron aluminate luminescent
Take Strontium carbonate powder SrCO 30.5758g, aluminium hydroxide Al (OH) 31.1701g, sodium carbonate Na 2CO 30.0318g, boric acid H 3BO 30.3092g, terbium sesquioxide Tb 4O 70.0935g and fusing assistant (5%) boric acid H 3BO 30.1090g.After all substances are placed in the abundant grinding of agate mortar, put into corundum crucible at 600 ℃ of lower presintering 2h, then be cooled to room temperature, again fully grind.At last, grinding product is calcined 5h under 1000 ℃ again, and is cooling, namely gets Sr after grinding 0.78Tb 0.1Na 0.12Al 3BO 7Boron aluminate luminescent.

Claims (10)

1. a boron aluminate luminescent, is characterized in that, its chemical formula is M 1-x-y-zGd xTb yN zAl 3BO 7
Wherein, M is at least a in Ba, Sr, and N is Na, Li or K, and the span of x is 0.001≤x≤0.20, and the span of y is 0.005≤y≤0.50, and the span of z is 0.02≤z≤0.30, and 1-x-y-z＞0.
2. boron aluminate luminescent according to claim 1, is characterized in that, the span of described x is 0.01≤x≤0.10.
3. boron aluminate luminescent according to claim 1, is characterized in that, the span of described y is 0.01≤y≤0.20.
4. boron aluminate luminescent according to claim 1, is characterized in that, the span of described z is 0.02≤z≤0.20.
5. the preparation method of a boron aluminate luminescent, is characterized in that, comprises the following steps:
1. take contain the M compound, contain the N compound, contain the Gd compound, contain the Tb compound, contain the Al compound, boride alloy is as raw material, presses M 1-x-y-zGd xTb yN zAl 3BO 7In the molar ratio of each element take each raw material, and add fusing assistant by 5%～30% of raw material gross weight, ground and mixed evenly forms compound, wherein, M is at least a in Ba, Sr, and N is Na, Li or K, the span of x is 0.001≤x≤0.20, the span of y is 0.005≤y≤0.50, and the span of z is 0.02≤z≤0.30, and 1-x-y-z＞0;
2. the compound of 1. step being made is at 200～700 ℃ of lower presintering 2～5h;
3. step presintering product 2. is cooled to room temperature, grinds;
4. with step grinding product calcining 3., calcining temperature is 900～1100 ℃, and calcination time is 1～24h;
5. step calcinate 4. is cooled to room temperature, namely obtains boron aluminate luminescent.
6. the preparation method of boron aluminate luminescent according to claim 5, is characterized in that, the span of described x is 0.01≤x≤0.10, and the span of described y is 0.01≤y≤0.20, and the span of described z is 0.02≤z≤0.20.
7. the preparation method of boron aluminate luminescent according to claim 5, it is characterized in that, the described M of containing compound is the oxide compound of M, oxyhydroxide, nitrate, at least a in carbonate, the described N of containing compound is the carbonate of N, oxide compound or nitrate that the described Gd of containing compound is Gd, oxide compound or nitrate that the described Tb of containing compound is Tb, the described Al of containing compound is the oxide compound of Al, oxyhydroxide, nitrate, at least a in carbonate, described boride alloy is boric acid or boron oxide, described fusing assistant is boric acid, boron oxide, at least a in barium fluoride.
8. the preparation method of boron aluminate luminescent according to claim 5, is characterized in that, the calcining temperature of described step in 4. is 950～1050 ℃.
9. the preparation method of boron aluminate luminescent according to claim 5, is characterized in that, the calcination time of described step in 4. is 4～14h.
10. the preparation method of boron aluminate luminescent according to claim 5, is characterized in that, 5. described step is: step calcinate 4. is cooled to after room temperature its grinding, namely obtains boron aluminate luminescent.
CN 200910239627 2009-12-31 2009-12-31 Boron aluminate luminescent material capable of generating green light and preparation method thereof Expired - Fee Related CN102115669B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1922741A (en) * 2004-02-18 2007-02-28 独立行政法人物质·材料研究机构 Light emitting device and lighting fixture
CN101134895A (en) * 2006-08-15 2008-03-05 大连路明科技集团有限公司 Wide-spectrum excitation fluorescent material and synthesizing method and light-emitting apparatus using the same
CN101278030A (en) * 2005-09-30 2008-10-01 首尔半导体株式会社 Light emitting device and LCD backlight unit using the same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1922741A (en) * 2004-02-18 2007-02-28 独立行政法人物质·材料研究机构 Light emitting device and lighting fixture
CN101278030A (en) * 2005-09-30 2008-10-01 首尔半导体株式会社 Light emitting device and LCD backlight unit using the same
CN101134895A (en) * 2006-08-15 2008-03-05 大连路明科技集团有限公司 Wide-spectrum excitation fluorescent material and synthesizing method and light-emitting apparatus using the same

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