CN101747894B - Red luminescent material for converting white light with high color rendering property by purple LED and preparation method thereof - Google Patents
Red luminescent material for converting white light with high color rendering property by purple LED and preparation method thereof Download PDFInfo
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- CN101747894B CN101747894B CN2009102181320A CN200910218132A CN101747894B CN 101747894 B CN101747894 B CN 101747894B CN 2009102181320 A CN2009102181320 A CN 2009102181320A CN 200910218132 A CN200910218132 A CN 200910218132A CN 101747894 B CN101747894 B CN 101747894B
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- purple led
- white light
- color rendering
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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
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Abstract
The invention belongs to the technical field of luminescence and display and relates to a red luminescent material for converting white light with high color rendering property by a purple LED. The structural formula of the material is Mg4GeO5.5F:LxMyNz, wherein L is a transition metal element Mn, M is a metal sensitizing agent element Sn and Nz is a sensitizing agent element Pb. The preparation method comprises: weighing the materials in the structural formula by weight percentage, grinding and uniformly mixing the weighed materials, putting the materials in an aluminum trioxide crucible, sintering for 1-2 hours in a high temperature furnace at 600-800 DEG C in air atmosphere, cooling, taking out, crushing, putting in a crucible, sintering in the high temperature furnace at 1000-1300 DEG C for 2-3 hours, cooling, taking out and crushing to obtain the crystal powder emitting bright red light under the excitation of ultraviolet light (lambda is equal to 365nm) and the purple LED (lambda is equal to 400nm). The red luminescent material is mixed with rear-earth tricolor luminescent materials in a certain ratio and then coated on the tube core of the purple LED for emitting the white light with high color rendering property.
Description
Technical field
The invention belongs to luminous and the technique of display field, relate to red illuminating material of a kind of converting white light with high color rendering property by purple LED and preparation method thereof.
Background technology
Because plurality of advantages such as the fast development of semi-conductor (LED) technology, white light LEDs owing to its high light efficiency, develop the color, environmental protection, life-span length have become earlier the focus of countries in the world research.Blue-ray LED conversion of white light technology is comparative maturity, but lacks ruddiness in the spectrum, and color developing is not high, is difficult to satisfy the requirement of low colour temperature high-color rendering illumination.And the technology of LED conversion of white light into purple light has been risen, in order further to improve the luminous efficiency that improves LED conversion of white light into purple light, colour rendering index etc., makes it reach commodity practicability.To the improvement of purple LED chip technology, mainly be that performance red, blue to the used rare-earth trichromatic of conversion of white light, green luminescent material improves on the other hand on the one hand.Simultaneously; In order to satisfy the requirement of some special industries (for example: military affairs, medical science, museum etc.) to color rendering properties of light source; The novel red fluorescent material that the needs development is effectively excited by purple LED (λ=620-700nm); It is mixed with rare-earth trichromatic fluorescent powder by a certain percentage, thereby and spread upon and obtain the high-color rendering illuminating device on the purple LED chip.The present invention then relates to one type of novel transition metal and activates; And mix an amount of coactivated germanate red illuminating material of metal sensitizing agent Sn, Pb (λ=600-680nm); This type luminescent material has advantages such as luminous efficiency height, stability is high, color developing is good, synthesis technique is simple, is the high efficient luminous material that can be used for the converting white light with high color rendering property by purple LED way.
Summary of the invention
Technical scheme of the present invention is following:
1. material is chosen according to chemical structural formula Mg
4GeO
5.5F:L
xM
yN
z, work as L
xDuring for Mn, M
yBe Sn, N
zDuring for the metal Pb element, take by weighing the following material of high purity by its weight percent:
MgO:47.84%-50.5% MgF
2:10.7%-11.2%
GeO
2:35.3%-37% MnCO
3:0.4%-1.95%
SnO
2:0.54%-3.06% PbO:0.17%-1.34%
Weight of material per-cent sum is 100%.
2. with the above-mentioned material that takes by weighing through grinding be mixed even after, the alumina crucible of packing into add a cover put into High Temperature Furnaces Heating Apparatus under air atmosphere 600-800 ℃ sintering 1-2 hour.
3. porphyrize is taken out in the cooling back; Reinstall in the alumina crucible and add a cover; Put under the High Temperature Furnaces Heating Apparatus air atmosphere 1000-1300 ℃ sintering 2-3 hour, cooling is taken out porphyrize and is obtained that ((λ=400nm) excites the crystal powder that time sends bright red coloured light for λ=365nm) and purple LED at UV-light.With blue, green, the red luminescent material of itself and rare-earth trichromatic 1: 2: 8 in proportion: 18 were coated in the white light that can send high-color rendering on the purple LED tube core after mixing.
The red illuminating material of converting white light with high color rendering property by purple LED of the present invention is characterized in that its structural formula: Mg
4GeO
5.5F:L
xM
yN
z, (1) L
xBe transient metal Mn element, M
yBe metal sensitizing agent Sn element, N
zBe metal sensitizing agent Pb element, span 0.01≤x≤0.05 of x in (2) structural formula, span 0.01≤y≤0.06 of y, span 0.001≤z≤0.02 of z.
Its advantage of the red illuminating material of converting white light with high color rendering property by purple LED of the present invention is:
1. the transient metal Mn element is an activator, and sensitizing agent is metal Sn and Pb element, through realizing that transmission ofenergy is significantly improved the luminous efficiency of activator Mn.
2. high light efficiency, color developing is good, synthesis technique is simple.
Description of drawings
Accompanying drawing 1 for embodiment 1 through (λ=400nm) excites the red emission spectrogram of gained down at purple light after the high-temperature calcination;
Accompanying drawing .2 instance one (1: 2: 8: 18) spread upon purple LED (resulting white light LED part on the tube core of λ=400nm) after the mixing with blue, green, red (corresponding aluminate, silicate, the molybdate respectively) fluorescent material of rare-earth trichromatic and in proportion; Its white color coordinate is (x=0.282; Y=0.329), color rendition index is brought up to R
a=92 (do not mix instance color developing R for the moment
a=86);
Accompanying drawing 3 is the white light emission spectrogram of this white light LED part.
Embodiment (containing spectroscopic data)
Embodiment 1
1. material is chosen according to chemical structural formula Mg
4GeO
5.5F:L
xM
yN
z, work as L
xBe transient metal Mn element, M
yBe metal Sn element, N
zDuring for the metal Pb element, take by weighing the following material of high purity by its weight percent:
MgO:50.5% MgF
2:11.18%
GeO
2:37.3% MnCO
3:0.4%
SnO
2:0.54% PbO:0.08%
2. with the above-mentioned material that takes by weighing through grinding be mixed even after, the alumina crucible of packing into add a cover put into High Temperature Furnaces Heating Apparatus under air atmosphere the first time 600 ℃ of sintering of temperature 1 hour.
3. porphyrize is taken out in the cooling back; Reinstall and added a cover under the High Temperature Furnaces Heating Apparatus air atmosphere for the second time 1000 ℃ of sintering in the alumina crucible 2 hours, cooling is taken out porphyrize and is obtained promptly that ((λ=400nm) excites the crystal powder that descends to send bright red for λ=365nm) and purple LED at UV-light.
Material is chosen according to chemical structural formula Mg
4GeO
5.5F:L
xM
yN
z, work as L
xBe transient metal Mn element, M
yBe metal Sn element, N
zDuring for the metal Pb element, take by weighing the following material of high purity by its weight percent:
MgO:49.89% MgF
2:11%
GeO
2:36.8% MnCO
3:1%
SnO
2:1.14% PbO:0.17%
700 ℃ of first sintering temperature 1 hour, 1000 ℃ of sintering temperatures 2 hours for the second time, the sintering synthesis step is with embodiment 1.
Embodiment 3
Material is chosen according to chemical structural formula Mg
4GeO
5.5F:L
xM
yN
z, work as L
xBe transient metal Mn element, M
yBe metal Sn element, N
zDuring for the metal Pb element, take by weighing the following material of high purity by its weight percent:
MgO:49.18% MgF
2:10.88%
GeO
2:36.3% MnCO
3:1.2%
SnO
2:2.1% PbO:0.34%
750 ℃ of first sintering temperature 2 hours, 1150 ℃ of sintering temperatures 2 hours for the second time, the sintering synthesis step is with embodiment 1.
Embodiment 4
Material is chosen according to chemical structural formula Mg
4GeO
5.5F:L
xM
yN
z, work as L
xBe transient metal Mn element, M
yBe metal Sn element, N
zDuring for the metal Pb element, take by weighing the following material of high purity by its weight percent:
MgO:49.2% MgF
2:10.9%
GeO
2:36.2% MnCO
3:1.6%
SnO
2:1.58% PbO:0.43%
750 ℃ of first sintering temperature 2 hours, 1200 ℃ of sintering temperatures 2 hours for the second time, the sintering synthesis step is with embodiment 1.
Embodiment 5
Material is chosen according to chemical structural formula Mg
4GeO
5.5F:L
xM
yN
z, work as L
xBe transient metal Mn element, M
yBe metal Sn element, N
zDuring for the metal Pb element, take by weighing the following material of high purity by its weight percent:
MgO:49.4% MgF
2:10.7%
GeO
2:35.7% MnCO
3:1.92%
SnO
2:2.6% PbO:0.68%
800 ℃ of first sintering temperature 2 hours, 1250 ℃ of sintering temperatures 3 hours for the second time, the sintering synthesis step is with embodiment 1.
Embodiment 6
Material is chosen according to chemical structural formula Mg
4GeO
5.5F:L
xM
yN
z, work as L
xBe transient metal Mn element, M
yBe metal Sn element, N
zDuring for the metal Pb element, take by weighing the following material of high purity by its weight percent:
MgO:47.84% MgF
2:10.59%
GeO
2:35.3% MnCO
3:1.95%
SnO2:3.06% PbO:1.26%
800 ℃ of first sintering temperature 2 hours, 1300 ℃ of sintering temperatures 2 hours for the second time, the sintering synthesis step is with embodiment 1.
Embodiment 7
Material is chosen according to chemical structural formula Mg
4GeO
5.5F:L
xM
yN
z, work as L
xBe transient metal Mn element, M
yBe metal Sn element, N
zDuring for the metal Pb element, take by weighing the following material of high purity by its weight percent:
MgO:49.45% MgF
2:10.9%
GeO
2:36.47% MnCO
3:1.05%
SnO
2:0.79% PbO:1.34%
800 ℃ of first sintering temperature 1 hour, 1300 ℃ of sintering temperatures 2 hours for the second time, the sintering synthesis step is with embodiment 1.
Claims (2)
1. the preparation method of converting white light with high color rendering property by purple LED red illuminating material is characterized in that concrete steps are following:
1. material is chosen according to chemical structural formula Mg
4GeO
5.5F:L
xM
yN
z, work as L
xDuring for Mn, M
yBe Sn, N
zDuring for the metal Pb element, take by weighing the following material of high purity by its weight percent:
MgO:47.84%-50.5% MgF
2:10.7%-11.2%
GeO
2:35.3%-37% MnCO
3:0.4%-1.95%
SnO
2:0.54%-3.06% PbO:0.17%-1.34%
Weight of material per-cent sum is 100%;
2. with the above-mentioned material that takes by weighing through grinding be mixed even after, the alumina crucible of packing into add a cover put into High Temperature Furnaces Heating Apparatus under air atmosphere 600-800 ℃ sintering 1-2 hour;
3. porphyrize is taken out in the cooling back; Reinstall in the alumina crucible and add a cover; Put under the High Temperature Furnaces Heating Apparatus air atmosphere 1000-1300 ℃ sintering 2-3 hour; Cooling is taken out porphyrize and is obtained exciting the crystal powder that time sends bright red coloured light at λ=365nm UV-light and λ=400nm purple LED, and with blue, green, red 1: 2: 8 in proportion of itself and rare-earth trichromatic luminescent material: 18 were coated in the white light that can send high-color rendering on the purple LED tube core after mixing.
2. the converting white light with high color rendering property by purple LED red illuminating material is characterized in that its structural formula is: Mg
4GeO
5.5F:L
xM
yN
z, (1) L
xBe transient metal Mn element, M
yBe metal sensitizing agent Sn element, N
zBe metal sensitizing agent Pb element, span 0.01≤x≤0.05 of x in (2) structural formula, span 0.01≤y≤0.06 of y, span 0.001≤z≤0.02 of z.
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CN101747894B true CN101747894B (en) | 2012-12-05 |
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CN102585812B (en) * | 2011-12-27 | 2014-09-10 | 江苏博睿光电有限公司 | Dark red fluorescent powder and preparation method thereof |
CN106854467B (en) * | 2015-12-08 | 2019-08-09 | 有研稀土新材料股份有限公司 | Fluorine oxide fluorescent powder and light emitting device containing the fluorescent powder |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1823398A (en) * | 2003-07-15 | 2006-08-23 | 皇家飞利浦电子股份有限公司 | Colour tunable lighting element |
US20090134769A1 (en) * | 2007-09-14 | 2009-05-28 | Osram Sylvania Inc. | Phosphor blend for a compact fluorescent lamp and lamp containing same |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN1823398A (en) * | 2003-07-15 | 2006-08-23 | 皇家飞利浦电子股份有限公司 | Colour tunable lighting element |
US20090134769A1 (en) * | 2007-09-14 | 2009-05-28 | Osram Sylvania Inc. | Phosphor blend for a compact fluorescent lamp and lamp containing same |
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