CN102786928A - Blue-green phosphor and preparation method thereof - Google Patents
Blue-green phosphor and preparation method thereof Download PDFInfo
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- CN102786928A CN102786928A CN2012102288387A CN201210228838A CN102786928A CN 102786928 A CN102786928 A CN 102786928A CN 2012102288387 A CN2012102288387 A CN 2012102288387A CN 201210228838 A CN201210228838 A CN 201210228838A CN 102786928 A CN102786928 A CN 102786928A
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- bluish
- fluorescent material
- green fluorescent
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- powder
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Abstract
The invention discloses a blue-green phosphor and a preparation method thereof. A general chemical formula of the blue-green phosphor is BaMgAl10O17:xEu<2+>,yMn<2+>, wherein x = 0.01 to 0.12 and y = 0.01 to 0.12. The preparation method comprises using BaMgAl10O17 as base materials, introducing Eu<2+> and Mn<2+> as a luminescence center, adding a fluoride cosolvent, employing a carbon-buried reduction process, solid-phase sintering for one time and reducing, and then grinding, drying and sieving to obtain the blue-green phosphor. The blue-green phosphor has advantages of complete crystal form, good uniformity, good safety performance, simple process operation of preparation and cheap raw materials, and is suitable for industrial production.
Description
Technical field
What the present invention relates to is a kind of bluish-green fluorescent material that is applicable to plasma panel display (PDP) and preparation method thereof, and bluish-green fluorescence property is accomplished in same matrix, practices thrift cost, easy and simple to handle, belongs to rare earth luminescent material field.
Background introduction
Color PDP (plasma panel display) because of have large screen display and high brightness, 160 ° of wide visual angles, take up room little, clear image, digitizing work, immunity from interference is strong, operating temperature range is wide, be applicable to that harsh environment etc. is different from the advantage of conventional display spare, is widely used in airport, station, harbour, market, hotel, hospital, bank, stock exchange, Playgrounds, exhibition hall, company, public place of entertainment etc.
In the development of color PDP, the development of fluorescent material is crucial.And present most widely used color PDP fluorescent powder, color PDP fluorescent powder has redness, green, blue colour fluorescent powder at present, is called for short three primary colors fluorescent powder.Color PDP fluorescent powder commonly used has systems such as silicate, aluminate, borate, phosphoric acid salt.Using more at present, red fluorescence powder is blue colour fluorescent powder BaMgAl
10O
17: Eu (BAM), red fluorescence powder (Y, Gd) BO:Eu and green emitting phosphor (BaA1
12O
19: Mn) form the PDP fluorescent material with three basic colour together.
At present; The red, green, blue fluorescent material that PDP uses passes through respectively under the H2 reducing atmosphere, and high-temperature solid phase calcination obtains, and means that three groups of parallel fluorescent material calcining furnaces of needs realize; The loss that increased the operation cost that industry is produced widely, has caused human and material resources, and H
2Application brought bigger potential safety hazard to operation site.
Summary of the invention
The object of the invention provides a kind of bluish-green fluorescent material in order to solve above-mentioned technical problem.
Two of the object of the invention provides the preparation method of above-mentioned a kind of bluish-green fluorescent material.
Know-why of the present invention
Owing to have advantages such as high-luminous-efficiency and high color purity, can pass through adjustment luminescence center Eu at BAM aspect blueness, the blue-green fluorescent powder
2+And Mn
2+Content regulate and control the fluorescence property of bluish-green fluorescent material.
Technical scheme of the present invention
A kind of bluish-green fluorescent material, its chemical general formula are BaMgAl
10O
17: xEu
2+, yMn
2+, wherein, x=0.01-0.12, y=0.01-0.12.
The preparation method of above-mentioned a kind of bluish-green fluorescent material is promptly with BaMgAl
10O
17Be matrix, introduce Eu
2+, Mn
2+As luminescence center, add the fusing assistant fluorochemical after, adopt and bury carbon reduction technology, carry out a solid phase and burn till and reduce, again through grind, dry, sieving promptly gets bluish-green fluorescent material.
The preparation method of above-mentioned a kind of bluish-green fluorescent material, its preparation process specifically comprises the steps:
(1), according to chemical general formula BaMgAl
10O
17: xEu
2+, yMn
2+, calculate BaCO respectively
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3Quality, weighing takes by weighing fluorochemical as fusing assistant, thorough mixing evenly obtains powder mixture in mortar;
Described Al
2O
3Be the powder that ultrasonic-field coupled activation hydrolysis metallic aluminium preparation gets, promptly adopt ultrasonic activation technology that metal aluminum foil is handled after, utilize the galvanic cell characteristic of metallic aluminium-air to carry out electrode reaction, obtain high-purity Al (OH)
3Gel then carries out 1000 ~ 1100 ℃ of thermal treatments and obtains;
Described fluoride flux is BaF
2, MgF
2, AlF
3Or CaF
2, its quality is BaCO
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3The 3-10% of the powder total mass that mixes;
(2), the powder mixture of step (1) gained adopted buries carbon reduction technology and in retort furnace, calcine, the calcination process controlled temperature is 1200-1500 ℃, the time obtains the bluish-green fluorescent material bullion of white powder after being 2-6h;
The described carbon reduction technology of burying specifically comprises the steps:
At first, with the used raw material BaCO of the bluish-green fluorescent material of preparation
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3Evenly obtaining powder mixture with fusing assistant fluorochemical thorough mixing in mortar packs in the monkey of a band aluminum oxide screen plate top cover;
The gac that is no more than 2/3 big crucible volume is packed in the big crucible;
Then, monkey is imbedded in the gac in the big crucible, simultaneously, after the layer of active carbon that tiles again on the aluminum oxide screen plate top cover of monkey, together placed retort furnace to calcine together with big crucible the monkey that places big crucible;
(3), the bluish-green fluorescent material bullion of the white powder of gained in the step (2) ground 1h in the sand mill of 1600r/min after, controlled temperature is 100 ~ 120 ℃ to carry out drying, sieves, and is preferably 200 mesh sieves, promptly obtains bluish-green fluorescent material.
Beneficial effect of the present invention
The preparation method of a kind of bluish-green fluorescent material of the present invention; Have simple, the easy handling of production technique, preparation cost is cheap, and bluish-green fluorescence property is gathered in a kind of luminous host; In terms of existing technologies; Avoided the loaded down with trivial details technology of twice preparation fluorescent material, the consumption of having lowered human and material resources has greatly solved H
2The unsafe factor of reducing environment, security is improved, and is suitable for suitability for industrialized production.
The preparation method of a kind of bluish-green fluorescent material among the present invention, the Al that adopts ultrasonic-field coupled activation hydrolysis metallic aluminium to prepare
2O
3Powder is starting material, with respect to available technology adopting analytical pure or spectroscopically pure Al
2O
3Be raw material, relative reduction production cost.
Blue, the green fluorescence excellent performance of the bluish-green fluorescent material of the present invention's preparation has the higher indigo plant of relative intensity, green fluorescence emission peak at 451nm and 514nm place respectively, therefore is adapted in the PDP color monitor.
Description of drawings
The XRD figure of the bluish-green fluorescent material of gained among Fig. 1, the embodiment 1;
The emmission spectrum of the bluish-green fluorescent material EX=340nm of gained among Fig. 2 a, the embodiment 1;
The emmission spectrum of the bluish-green fluorescent material EM=451nm of gained among Fig. 2 b, the embodiment 1;
The emmission spectrum of the bluish-green fluorescent material EM=520nm of gained among Fig. 2 c, the embodiment 1.
Embodiment
Below through concrete embodiment and combine accompanying drawing that the present invention is further set forth, but do not limit the present invention.
Used Al in the embodiment of the invention
2O
3Be the powder that ultrasonic-field coupled activation hydrolysis metallic aluminium preparation gets, promptly adopt ultrasonic activation technology that metal aluminum foil is handled after, utilize the galvanic cell characteristic of metallic aluminium-air to carry out electrode reaction, obtain high-purity Al (OH)
3Gel is to heat-treat under 1000 ~ 1100 ℃ to obtain in temperature then.
Other starting material comprise BaF
2, MgF
2, AlF
3CaF
2, BaCO
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3Be the laboratory and use analytical pure.
Embodiment 1
(1), according to chemical general formula BaMgAl
10O
17: xEu
2+, yMn
2+Wherein (x=0.04 y=0.01), calculates BaCO respectively
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3Amount, weighing takes by weighing AlF
3As fusing assistant, thorough mixing evenly obtains powder mixture in mortar;
Fusing assistant AlF
3Quality be above-mentioned BaCO
3, MgO, Al
2O
3, Eu
2O
3And MnCO
310% of the powder total mass that mixes;
(2), with the powder mixture of step (1) gained as in the retort furnace, bury under the carbon reduction technology, calcining temperature is 1500 ℃, calcination time is 2h, obtains white powder;
(3), the white powder of gained in the step (2) ground 1h in the sand mill of 1600r/min after, controlled temperature is to carry out drying, mistake 200 mesh sieves under 100-120 ℃, promptly obtains the bluish-green fluorescent material BaMgAl of uniform granularity
10O
17: 0.04Eu
2+, 0.01Mn
2+
To utilize D/max 2200PC type X-ray diffractometer to its BaMgAl to the bluish-green fluorescent material of above-mentioned gained
10O
17: 0.04Eu
2+, 0.01Mn
2+Carry out structural analysis, its XRD figure is seen shown in Figure 1, can find that from Fig. 1 its XRD figure is consistent with the relative intensity and the diffraction peak position of the diffraction peak of standard spectrogram (the PDF card number is 26-0163), and Eu is described
2+And Mn
2+Mix and do not change BaMgAl
10O
17Structure.
Bluish-green fluorescent material BaMgAl with above-mentioned gained
10O
17: 0.04Eu
2+, 0.01Mn
2+, measuring its emmission spectrum with F-4500, its result sees Fig. 2 a, Fig. 2 b and Fig. 2 c respectively.
Can find out that from Fig. 2 a when being excitation wavelength with 340nm, its emission peak explains that 451 and 514 fluorescent material turns blue, green glow;
Can find out that from Fig. 2 b under 451nm, seeking excitation wavelength is 340nm;
Can find out that from Fig. 2 c under 514nm, seeking excitation wavelength is 340nm.
Therefore, excitation wavelength is chosen to be 340nm, the bluish-green fluorescent material BaMgAl of above-mentioned gained
10O
17: 0.04Eu
2+, 0.01Mn
2+Excite down at this wavelength, indigo plant, green bimodal can occur.
Embodiment 2
(1), according to chemical general formula BaMgAl
10O
17: xEu
2+, yMn
2+, calculate BaCO respectively
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3Amount, weighing takes by weighing BaF
2As fusing assistant, thorough mixing evenly obtains powder mixture in mortar;
Fusing assistant BaF
2Quality be above-mentioned BaCO
3, MgO, Al
2O
3, Eu
2O
3And MnCO
35% of the powder total mass that mixes;
(2), with the powder mixture of step (1) gained as in the retort furnace, bury under the carbon reduction technology, calcining temperature is 1400 ℃, calcination time is 4h, obtains white powder;
(3), the white powder of gained in the step (2) ground 1h in the sand mill of 1600r/min after, controlled temperature is to carry out drying, mistake 200 mesh sieves under 100-120 ℃, promptly obtains the bluish-green fluorescent material BaMgAl of uniform granularity
10O
17: 0.12Eu
2+, 0.04Mn
2+
(1), according to chemical general formula BaMgAl
10O
17: xEu
2+, yMn
2+Wherein (x=0.04 y=0.12), calculates BaCO respectively
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3Amount, weighing takes by weighing AlF
3As fusing assistant, thorough mixing evenly obtains powder mixture in mortar;
Fusing assistant AlF
3Quality be above-mentioned BaCO
3, MgO, Al
2O
3, Eu
2O
3And MnCO
35% of the powder total mass that mixes;
(2), with the powder mixture of step (1) gained as in the retort furnace, bury under the carbon reduction technology, calcining temperature is 1400 ℃, calcination time is 3h, obtains white powder;
(3), the white powder of gained in the step (2) ground 1h in the sand mill of 1600r/min after, controlled temperature is to carry out drying, mistake 200 mesh sieves under 100-120 ℃, promptly obtains the bluish-green fluorescent material BaMgAl of uniform granularity
10O
17: 0.04Eu
2+, 0.12Mn
2+
Embodiment 4
(1), according to chemical general formula BaMgAl
10O
17: xEu
2+, yMn
2+Wherein (x=0.01 y=0.01), calculates BaCO respectively
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3Amount, weighing takes by weighing MgF
2As fusing assistant, thorough mixing evenly obtains powder mixture in mortar;
Fusing assistant MgF
2Quality be above-mentioned BaCO
3, MgO, Al
2O
3, Eu
2O
3And MnCO
33% of the powder total mass that mixes;
(2), with the powder mixture of step (1) gained as in the retort furnace, bury under the carbon reduction technology, calcining temperature is 1350 ℃, calcination time is 5h, obtains white powder;
(3), the white powder of gained in the step (2) ground 1h in the sand mill of 1600r/min after, controlled temperature is to carry out drying, mistake 200 mesh sieves under 100-120 ℃, promptly obtains the bluish-green fluorescent material BaMgAl of uniform granularity
10O
17: 0.01Eu
2+, 0.11Mn
2+
Embodiment 5
(1), according to chemical general formula BaMgAl
10O
17: xEu
2+, yMn
2+Wherein (x=0.08 y=0.02), calculates BaCO respectively
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3Amount, weighing takes by weighing CaF
2As fusing assistant, thorough mixing evenly obtains powder mixture in mortar;
Fusing assistant CaF
2Quality be above-mentioned BaCO
3, MgO, Al
2O
3, Eu
2O
3And MnCO
37% of the powder total mass that mixes;
(2), with the powder mixture of step (1) gained as in the retort furnace, bury under the carbon reduction technology, calcining temperature is 1200 ℃, calcination time is 6h, obtains white powder;
(3), the white powder of gained in the step (2) ground 1h in the sand mill of 1600r/min after, controlled temperature is to carry out drying, mistake 200 mesh sieves under 100-120 ℃, promptly obtains the bluish-green fluorescent material BaMgAl of uniform granularity
10O
17: 0.07Eu
2+, 0.03Mn
2+
The above content is merely the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (5)
1. a bluish-green fluorescent material is characterized in that its chemical general formula is BaMgAl
10O
17: xEu
2+, yMn
2+, wherein, x=0.01-0.12, y=0.01-0.12.
2. the preparation method of a kind of bluish-green fluorescent material as claimed in claim 1 is characterized in that the MgAl with Ba
10O
17Be matrix, introduce Eu
2+, Mn
2+As luminescence center, add the fusing assistant fluorochemical, adopt and bury carbon reduction technology, carry out a solid phase and burn till and reduce, again through grind, dry, sieving promptly gets bluish-green fluorescent material.
3. like the preparation method of claims 2 described bluish-green fluorescent material, it is characterized in that specifically comprising being prepared as follows step:
(1), according to chemical general formula BaMgAl
10O
17: xEu
2+, yMn
2+, take by weighing BaCO respectively
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3And fluoride flux, thorough mixing evenly obtains powder mixture in mortar;
Wherein said Al
2O
3Prepare the powder that gets for ultrasonic-field coupled activation hydrolysis metallic aluminium;
(2), the powder mixture of step (1) gained adopted buries carbon reduction technology and in retort furnace, calcine, the calcination process controlled temperature is 1200-1500 ℃, the time obtains the bluish-green fluorescent material bullion of white powder after being 2-6h;
(3), the bluish-green fluorescent material bullion of the white powder of gained in the step (2) ground 1h in the sand mill of 1600r/min after, 100-120 ℃ of baking oven inner drying, sieve, promptly obtain bluish-green fluorescent material.
4. like the preparation method of claim 2 or 3 described a kind of bluish-green fluorescent material, the consumption that it is characterized in that described fluoride flux is BaCO
3, MgO, Al
2O
3, Eu
2O
3And MnCO
3The 3-10% of the powder total mass that mixes.
5. the preparation method of a kind of bluish-green fluorescent material as claimed in claim 4 is characterized in that described fluoride flux is BaF
2, MgF
2, AlF
3Or CaF
2
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|---|---|---|---|
| CN2012102288387A CN102786928A (en) | 2012-07-04 | 2012-07-04 | Blue-green phosphor and preparation method thereof |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409137A (en) * | 2013-08-22 | 2013-11-27 | 中国计量学院 | An ultraviolet ray excited SrMgAl10O17: eu2+, mn2+blue-green phosphor |
| CN103614136A (en) * | 2013-12-09 | 2014-03-05 | 兰州大学 | High-brightness and high-thermostability double-peak blue fluorescent powder and preparation method thereof |
| CN109135733A (en) * | 2018-06-21 | 2019-01-04 | 东台市天源光电科技有限公司 | A kind of Blue-green phosphor and preparation method thereof |
| CN111847878A (en) * | 2020-08-08 | 2020-10-30 | 苏奕堂 | Energy-storage luminous ceramic glaze and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838533A (en) * | 2009-03-20 | 2010-09-22 | 兰州大学 | Fluorescent material for LED and preparation method thereof |
-
2012
- 2012-07-04 CN CN2012102288387A patent/CN102786928A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838533A (en) * | 2009-03-20 | 2010-09-22 | 兰州大学 | Fluorescent material for LED and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| PING YANG ET AL: "Energy transfer and photoluminescence of BaMgAl10O17 co-doped with Eu2+ and Mn2+", 《OPTICAL MATERIALS》, vol. 26, 11 March 2004 (2004-03-11), pages 327 - 331 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409137A (en) * | 2013-08-22 | 2013-11-27 | 中国计量学院 | An ultraviolet ray excited SrMgAl10O17: eu2+, mn2+blue-green phosphor |
| CN103614136A (en) * | 2013-12-09 | 2014-03-05 | 兰州大学 | High-brightness and high-thermostability double-peak blue fluorescent powder and preparation method thereof |
| CN109135733A (en) * | 2018-06-21 | 2019-01-04 | 东台市天源光电科技有限公司 | A kind of Blue-green phosphor and preparation method thereof |
| CN111847878A (en) * | 2020-08-08 | 2020-10-30 | 苏奕堂 | Energy-storage luminous ceramic glaze and preparation method thereof |
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Application publication date: 20121121 |