CN101948132A - Simple process for preparing magnesium fluorogermanate: manganese red fluorescent powder - Google Patents
Simple process for preparing magnesium fluorogermanate: manganese red fluorescent powder Download PDFInfo
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- CN101948132A CN101948132A CN2010102871174A CN201010287117A CN101948132A CN 101948132 A CN101948132 A CN 101948132A CN 2010102871174 A CN2010102871174 A CN 2010102871174A CN 201010287117 A CN201010287117 A CN 201010287117A CN 101948132 A CN101948132 A CN 101948132A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses a simple process for preparing magnesium fluorogermanate: manganese red fluorescent powder, which is characterized by comprising the following steps of: accurately weighing raw materials in a certain molar ratio, and grinding the raw materials in an agate mortar; and then filling materials in two different modes respectively, putting the materials in a muffle furnace, heating the materials to between 1,100 and 1,200 DEG C at the heating speed of 6 DEG C per minute, preserving the heat for 1 to 3 hours, taking out the sample after the materials are cooled to room temperature, putting the sample into the agate mortar for secondary grinding, putting the powder in the muffle furnace, heating the powder to between 1,100 and 1,200 DEG C at the same heating speed, preserving the heat for 5 to 40 hours, and cooling the powder along with the furnace to obtain the magnesium fluorogermanate: manganese red fluorescent powder, wherein the excitation band of the red fluorescent powder is 280 to 440 nanometers and the red fluorescent powder emits red light with main emitting peak at 657 nanometers. The process has the advantages of short reaction time and energy conservation; and the obtained fluorescent powder has high luminous intensity.
Description
Technical field
The present invention relates to a kind of preparation fluogermanic acid magnesium: the simple and easy technology of manganese red look fluorescent material.
Background technology
The fluorescent material that the emmission spectrum peak value is positioned at 630～680nm long wave red spectral band has extremely important using value, yet the emmission spectrum peak value is positioned at the less of this wave band in the present commercially available fluorescent material.Because fluogermanic acid magnesium: manganese has the emission spectrum that is positioned at 657nm place uniqueness, and high in short-wave ultraviolet ray excited stability down, and hot properties is good, is very suitable high voltage mercury lamp lamp phosphor therefore.But traditional fluogermanic acid magnesium for preparing: its temperature control program of the method for manganese is 1100 ℃ of insulation 2h, rises to 1100 ℃ of insulation 40h again after reducing to room temperature, and the subject matter of existence is that the production cycle is long, and the drawbacks limit of time consumption and energy consumption its further application.
The objective of the invention is to propose a kind of new preparation fluogermanic acid magnesium: the technology of manganese, advantage are the shortening heat treatment time greatly, and effectively improve the luminescent properties of material, raise the efficiency.
Summary of the invention
A kind of preparation fluogermanic acid magnesium: the simple and easy technology of manganese red look fluorescent material, it is characterized in that accurately taking by weighing raw material by certain mol proportion, place agate mortar to grind; Then respectively with two kinds of different modes filling materials, place retort furnace to rise to 1100-1200 ℃ with the heat-up rate of 6 ℃/min, insulation 1-3h, take out sample after waiting to reduce to room temperature, place agate mortar to carry out regrind, place retort furnace to rise to 1100-1200 ℃ again with same heat-up rate, insulation 5-40h, furnace cooling promptly gets fluogermanic acid magnesium: manganese red look fluorescent material, and its excitation band extends to 440nm from 280nm always, and the emission main peak is positioned at the red light of 657nm.
The invention has the advantages that and shortened the reaction times, save energy has been optimized preparation means, improves luminous efficiency.
Embodiment
During operation, MgO (〉=98.5%): GeO at first in molar ratio
2(99.999%): MgF
2(99.5%): MnCO
3(99.9%)=and 3.5-3.51: accurately take by weighing raw material at 1.0: 0.5: 0.01; Be that improvement project (a) is put into the corundum monkey with precursor with two kinds of different modes filling materials then, place a big ceramic crucible of adding a cover after adding a cover again, and traditional way (b) is directly put into and is added a cover corundum crucible, place retort furnace to rise to 1100-1200 ℃ with the heat-up rate of 6 ℃/min, insulation 1-3h, take out sample after waiting to reduce to room temperature, carry out regrind with agate mortar, place retort furnace to rise to 1100-1200 ℃ again with same heat-up rate, insulation 5-40h, furnace cooling promptly gets fluogermanic acid magnesium: manganese red look fluorescent material.
Embodiment 1
At first according to the mol ratio MgO of traditional technology: GeO
2: MgF
2: MnCO
3=3.5: accurately take by weighing raw material at 1.0: 0.5: 0.01, putting into agate mortar carefully grinds, make its thorough mixing even, precursor is put into the corundum monkey according to a mode, after adding a cover, place a big ceramic crucible again, add a cover, use traditional technology temperature control program to place air atmosphere to carry out two-segment calcining, at first the temperature rise rate with 6 ℃/min rises to 1100 ℃ of insulation 2h, take out behind the furnace cooling and carry out regrind, rise to 1100 ℃ of insulation 40h, furnace cooling with same temperature rise rate once more.The sample of the b modes of emplacement preparation of generally using with traditional technology is compared, and adopts its luminous position of the prepared sample of this modes of emplacement identical, but intensity obviously increases, and is 1.25 times of traditional technology.
Embodiment 2
According to the condition of embodiment 1, change the temperature control program and at first rise to 1100 ℃, insulation 2h with the temperature rise rate of 6 ℃/min, take out sample after waiting to reduce to room temperature, carry out regrind, place retort furnace to rise to 1200 ℃ again with same heat-up rate with agate mortar, insulation 5h, furnace cooling.Do not change according to the luminous position of the prepared sample of this temperature control program, luminous intensity is 1.61 times of preparation sample luminous intensity under the traditional technology condition.
Embodiment 3
According to 1100 ℃ of embodiment 2 improved temperature program(me)s, 2h; 1200 ℃, 5h adopts modes of emplacement a, and the mol ratio that changes MgO in the raw material is 3.51, and prepared sample luminous position is identical, and intensity is 1.1 times of 3.5 o'clock prepared sample luminous intensities for the MgO mol ratio.
Claims (4)
1. preparation fluogermanic acid magnesium: the processing condition of manganese are: MgO (〉=98.5%): GeO in molar ratio
2(99.999%): MgF
2(99.5%): MnCO
3(99.9%)=and 3.5-3.51: accurately take by weighing raw material at 1.0: 0.5: 0.01; Be that improvement project (a) is put into the corundum monkey with precursor with two kinds of different modes filling materials respectively then, place a big ceramic crucible of adding a cover after adding a cover again, and traditional way (b) is directly put into and is added a cover corundum crucible, place retort furnace to rise to 1100-1200 ℃ with the heat-up rate of 6 ℃/min, insulation 1-3h, take out sample after waiting to reduce to room temperature, carry out regrind with agate mortar, place retort furnace to rise to 1100-1200 ℃ again with same heat-up rate, insulation 5-40h, furnace cooling promptly gets fluogermanic acid magnesium: manganese red look fluorescent material, and its excitation band extends to 440nm from 280nm always, and the emission main peak is positioned at the red light of 657nm.
2. according to 1 described preparation fluogermanic acid magnesium: the processing condition of manganese is characterized in that proportion of raw materials is mol ratio MgO: GeO
2: MgF
2: MnCO
3=3.5-3.51: 1.0: 0.5: 0.01.
3. according to 1 described preparation fluogermanic acid magnesium: the processing condition of manganese, it is characterized in that according to following two kinds of different modes filling material be that improvement project (a) is put into the corundum monkey with precursor, place a big ceramic crucible of adding a cover after adding a cover again, and traditional way (b) is put into directly and is added a cover corundum crucible.
4. according to 1 described preparation fluogermanic acid magnesium: the processing condition of manganese, it is characterized in that carrying out two-segment calcining in the service routine temperature control furnace air atmosphere, the parameter that adopts is 1100-1200 ℃, insulation 1-3h; 1100-1200 ℃, insulation 5-40h, temperature rise rate is 6 ℃/min, furnace cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102871174A CN101948132A (en) | 2010-09-16 | 2010-09-16 | Simple process for preparing magnesium fluorogermanate: manganese red fluorescent powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102871174A CN101948132A (en) | 2010-09-16 | 2010-09-16 | Simple process for preparing magnesium fluorogermanate: manganese red fluorescent powder |
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| CN101948132A true CN101948132A (en) | 2011-01-19 |
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| CN2010102871174A Pending CN101948132A (en) | 2010-09-16 | 2010-09-16 | Simple process for preparing magnesium fluorogermanate: manganese red fluorescent powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421496A (en) * | 2012-05-16 | 2013-12-04 | 海洋王照明科技股份有限公司 | Manganese and titanium co-doped fluorine magnesium germanate luminescent material and preparation method and application thereof |
| CN107488451A (en) * | 2017-06-26 | 2017-12-19 | 浙江转喆科技有限公司 | A kind of light conversion agent and preparation method thereof and agricultural red conversion film and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB712301A (en) * | 1951-07-11 | 1954-07-21 | Westinghouse Electric Int Co | Improvements in or relating to luminescent materials |
| GB857333A (en) * | 1956-11-30 | 1960-12-29 | British Thomson Houston Co Ltd | Improvements in luminescent materials |
| JPS54158387A (en) * | 1978-06-05 | 1979-12-14 | Toshiba Corp | Production of magnesium fluorogermanate phosphor |
-
2010
- 2010-09-16 CN CN2010102871174A patent/CN101948132A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB712301A (en) * | 1951-07-11 | 1954-07-21 | Westinghouse Electric Int Co | Improvements in or relating to luminescent materials |
| GB857333A (en) * | 1956-11-30 | 1960-12-29 | British Thomson Houston Co Ltd | Improvements in luminescent materials |
| JPS54158387A (en) * | 1978-06-05 | 1979-12-14 | Toshiba Corp | Production of magnesium fluorogermanate phosphor |
Non-Patent Citations (5)
| Title |
|---|
| 《J. Electrochem. Soc.: Solid State Science》 19710228 E. Kostiner et al. Magnesium Germanate and Fluorogermanate 351-353 1-4 第118卷, 第2期 2 * |
| 《Journal of The Optical Society of America》 19500930 Luke Thorington Temperature Dependence of the Emission of an Improved Manganese-Activated Magnesium Germanate Phosphor 579-583 1-4 第40卷, 第9期 2 * |
| 《全彩色蓄光材料的制备及发光性能研究》 20100410 王芳等 全彩色蓄光材料的制备及发光性能研究-氟锗酸镁：锰制备工艺改进 1-15 1 , * |
| 《发光学与发光材料》 20041031 徐叙瑢等 《发光学与发光材料》 化学工业出版社 311-312、601 1-4 , 第1版 1 * |
| 《固体发光材料》 20030831 孙家跃等 化学工业出版社 化学工业出版社 354-356 1-4 , 第1版 1 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421496A (en) * | 2012-05-16 | 2013-12-04 | 海洋王照明科技股份有限公司 | Manganese and titanium co-doped fluorine magnesium germanate luminescent material and preparation method and application thereof |
| CN103421496B (en) * | 2012-05-16 | 2016-12-14 | 海洋王照明科技股份有限公司 | Manganese Ti doped fluorine magnesium germanate luminescence material, preparation method and applications |
| CN107488451A (en) * | 2017-06-26 | 2017-12-19 | 浙江转喆科技有限公司 | A kind of light conversion agent and preparation method thereof and agricultural red conversion film and preparation method thereof |
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Application publication date: 20110119 |