CN101348714A - Red rare earth luminescent material for purple light LED conversion white light and preparation thereof - Google Patents

Red rare earth luminescent material for purple light LED conversion white light and preparation thereof Download PDF

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Publication number
CN101348714A
CN101348714A CNA2008100511552A CN200810051155A CN101348714A CN 101348714 A CN101348714 A CN 101348714A CN A2008100511552 A CNA2008100511552 A CN A2008100511552A CN 200810051155 A CN200810051155 A CN 200810051155A CN 101348714 A CN101348714 A CN 101348714A
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rare earth
luminescent material
white light
moo
sio
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刘益春
张昕彤
刘玉学
赵成久
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Northeast Normal University
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Northeast Normal University
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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
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    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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Abstract

The invention belongs to the luminescence and display technical field, in particular to a novel red rare earth luminescent material for transferring white light by a violet LED. The structural formula of the novel red rare earth luminescent material is M.N1-a-b(MoO4)2-x(SiO4)x:Ra.Rb, wherein M refers to alkali metal Li element or K element or alkali metal Li and Ba element or K and Ba element; N1-a-b refers to alkali metal Na element; and quantitive latent solvent is added. The materials of the compositions of the M.N1-a-b (MoO4) 2-x (SiO4) x: Ra.Rb are weighed by weight percent; the weighed materials are fully grinded and uniformly mixed and then added into an alumina crucible which is covered and placed into a high-temperature furnace and sintered in the air; after the mixture is cooled, the mixture is taken out and crushed and then added into the alumina crucible which is then covered and placed into the high-temperature furnace and sintered in the air; and the mixture is cooled, taken out and grinded, and then the red crystal powder which gives out red light within 365 nanometers under excitation of the violet LED is obtained.

Description

Red rare earth luminescent material for purple light LED conversion white light and preparation method
Technical field:
The invention belongs to luminous and the technique of display field, be specifically related to the novel red rare earth luminescent material of a kind of LED conversion of white light into purple light.
Background technology:
At present because the fast development of semiconductor technology, except the technology of blue-ray LED conversion of white light has been tending towards ripe, and the technology of LED conversion of white light into purple light is being risen.In order further to improve the luminous efficiency that improves LED conversion of white light into purple light, colour rendering index etc., make it reach commodity practicability, except the improvement of purple LED chip technology, it mainly is that conversion of white light is red with rare-earth trichromatic, blue, the performance of green luminescent material improves, and particularly the improvement of the luminous efficiency of red lanthanide luminescent material, stability improves.And present existing red lanthanide luminescent material such as CaS:Eu 2+, SrCaS:Eu 2+, Y 2O 2S:Eu 2+, SrSiO 4: Eu 2+Etc. unstable properties, influence its luminescent properties.At present, at the red lanthanide luminescent material of developing, as: the rare-earth activated molybdate of development such as Zhongshan University, the coloured institute in Beijing, tungsten hydrochlorate etc.And the present invention activates the molybdate red luminescent material of alkaline-earth metal silicon, luminous efficiency height, good stability by novel rare-earth, and synthesis technique is simple, nontoxic, pollution-free, is a kind of heavy duty detergent luminescent material.
Summary of the invention:
The novel rare-earth red illuminating material that the purpose of this invention is to provide a kind of LED conversion of white light into purple light.
The preparation method of red rare earth luminescent material for purple light LED conversion white light is as follows:
1. material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb, wherein M is Li or K, or Ba, N 1-a-bBe Na, Ra is the Eu element, when Rb is the Tb element, takes by weighing the following seven kinds of materials of high purity by its weight percent:
Li 2CO 3Or K 2CO 3Or Li 2CO 3And Ba 2CO 3Or K 2CO 3And Ba 2CO 3-3.188-2.926
MoO 3-85.824-81.824 Na 2CO 3-3.219-2.953
SiO 2-5.910-5.648 Eu 2O 3-5.754-5.493
NH 4F-0.05-0.04 Tb 4O 7-0.055-0.050
2. with the above-mentioned material that takes by weighing after grinding is mixed, the alumina crucible of packing into add a cover put into High Temperature Furnaces Heating Apparatus air 600-900 ℃ sintering 2-3 hour.
3. the cooling back is taken out and is pulverized, and reinstalls in the alumina crucible and adds a cover, and puts into 600-900 ℃ of sintering 2-4 of High Temperature Furnaces Heating Apparatus air hour, and cooling is taken out porphyrize and obtained exciting the crystal powder that sends bright ruddiness down at 365nm and purple LED.The rare earth luminescent material of itself and greening, blue light is coated on the purple LED tube core after the mixed routinely can sends white light.
The rare-earth red luminous material of LED conversion of white light into purple light of the present invention is characterized in that its structural formula: MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb, (1) Ra are rare-earth activated dose of Eu, and Rb is rare earth coactivator Tb, and M is basic metal Li or K or alkaline-earth metal Ba, N 1-a-bBe Alkali-Metal Na. span 1 〉=x 〉=0 of x in (2) structural formula, span 1 〉=a 〉=0.05 of a, span 0.05 〉=b 〉=0 of b also can add quantitative NH 4F reduces synthesis temperature and reduces the loss of oxygen generation phonon energy, improves luminous efficiency stability.
Advantage: the rare-earth red material of LED conversion of white light into purple light of the present invention is characterized in that:
1. adopt the Si element can replace part Mo element, its luminous efficiency and stability are improved and have reduced material cost.
2. rare earth Eu element is an activator, and the Tb element is a coactivator, and the luminous efficiency of its Eu is improved.
3. NH 4F reduces synthesis temperature as solubility promoter, reduces the loss that phonon energy causes simultaneously, has improved the luminous efficiency and the stability of material.
Embodiment:
Example 1
1. material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is K, N 1-a-bBe Na, Ra is the Eu element, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
K 2CO 3-4.125 MoO 3-81.877
Na 2CO 3-2.621 SiO 2-5.972
Eu 2O 3-5.325 NH 4F-0.03
Tb 4O 4-0.05
2. with the above-mentioned material that takes by weighing after grinding is mixed, the alumina crucible of packing into is added a cover and is put into High Temperature Furnaces Heating Apparatus 900 ℃ of sintering of air 3 hours.
3. porphyrize is taken out in cooling back, reinstalls to add a cover in the High Temperature Furnaces Heating Apparatus in the air 900 ℃ of sintering in the alumina crucible 3 hours, and cooling is taken out porphyrize and promptly obtained exciting the crystal powder that sends bright ruddiness down at ultraviolet 365nm and purple LED.
Example 2
Material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is Li, N 1-a-bBe Na, Ra is the Eu element, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
Li 2CO 3-2.935 MoO 3-81.952-82.552
Na 2CO 3-2.965 SiO 2-5.650-5.972
Eu 2O 3-5.496 NH 4F-0.03
Tb 4O 7-0.05
2. the sintering synthesis step goes on foot 800 ℃ of sintering temperatures, 2 hours time with example 1,, and 3. go on foot 800 ℃ of sintering temperatures, 2.5 hours time.
Example 3
Material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is Li and Ba, N 1-a-bBe Na, Ra is the Eu element, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
Li 2CO 3-2.055 MoO 3-82.552
Ba 2CO 3-0.965 SiO 2-5.896
Na 2CO 3-2.965 NH 4F-0.03
Eu2O3-5.496 Tb 4O 7-0.05
2. the sintering synthesis step goes on foot 600 ℃ of sintering temperatures, 2.5 hours time with example 1,, and 3. go on foot 600 ℃ of sintering temperatures, 4 hours time
Example 4
Material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is K and Ba, N 1-a-bBe Na, Ra is the Eu element, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
K 2CO 3-3.555 MoO 3-81.552
Ba 2CO 3-0.956 SiO 2-5.896
Na 2CO 3-2.465 NH 4F-0.03
Eu 2O 3-5.496 Tb 4O 7-0.05
2. the sintering synthesis step goes on foot 700 ℃ of sintering temperatures, 3 hours time with example 1,, and 3. go on foot 700 ℃ of sintering temperatures, 3 hours time.
Example 5
Material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is Li, N 1-a-bBe Na, Ra is the Eu element, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
Li 2CO 3-2.835 MoO 3-83.052
Na 2CO 3-3.065 SiO 2-5.472
Eu 2O 3-5.496 NH 4F-0.03
Tb 4O 7-0.05
Sintering synthesis step, sintering temperature, time are with example 1.
Example 6
Material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is Li and Ba, N 1-a-bBe Na, Ra is the Eu element, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
Li 2CO 3-1.055 MoO 3-81.552
Ba 2CO 3-1.956 SiO 2-6.896
Na 2CO 3-2.965 NH 4F-0.03
Eu 2O 3-5.496 Tb 4O 7-0.05
Sintering synthesis step, sintering temperature, time are with example 2.
Example 7
Material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is K and Ba, N 1-a-bDuring for the Na element, Ra is Eu, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
Li 2CO 3-2.555 MoO 3-82.603
Na 2CO 3-3.565 SiO 2-5.472
Eu 2O 3-5.945 NH 4F-0.03
Tb 4O 7-0.05
Sintering synthesis step, sintering temperature, time are with example 1.
Example 8
Material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is Ba and Li, N 1-a-bDuring for the Na element, Ra is Eu, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
Li 2CO 3-1.155 MoO 3-81.692
Ba 2CO 3-1.856 SiO 2-6.882
Na 2CO 3-2.839 NH 4F-0.03
Eu 2O 3-5.496 Tb 4O 7-0.05
Sintering synthesis step, sintering temperature, time are with example 1.
Example 9
Material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is K, N 1-a-bDuring for the Na element, Ra is Eu, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
K 2CO 3-3.125 MoO 3-81.877
Na 2CO 3-3.621 SiO 2-5.972
Eu 2O 3-5.325 NH 4F-0.03
Tb 4O 7-0.05
Sintering synthesis step, sintering temperature, time are with example 1.
Example 10
Material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb
When M is Li, N 1-a-bDuring for the Na element, Ra is Eu, when Rb is the Tb element, takes by weighing following seven kinds of high purity materials by its weight percent:
Li 2CO 3-2.235 MoO 3-82.673
Na 2CO 3-3.665 SiO 2-5.402
Eu 2O 3-5.945 NH 4F-0.03
Tb 4O 7-0.05
Sintering synthesis step, sintering temperature, time are with example 1.

Claims (3)

1, red rare earth luminescent material for purple light LED conversion white light is characterized in that its chemical structural formula is: MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb, wherein (1) Ra is rare-earth activated dose of Eu, and Rb is rare earth coactivator Tb, and M is basic metal Li or K or alkaline-earth metal Ba, N 1-a-bBe Alkali-Metal Na; (2) span 1 〉=x 〉=0 of x, span 1 〉=a 〉=0.05 of a, span 0.05 〉=b 〉=0 of b.
2, the preparation method of red rare earth luminescent material for purple light LED conversion white light is characterized in that:
1. material is chosen according to chemical structural formula MN 1-a-b(MoO 4) 2-x(SiO 4) x: RaRb, wherein M is Li or K, or Ba, N 1-a-bBe Na, Ra is the Eu element, when Rb is the Tb element, takes by weighing the following material of high purity by its weight percent:
Li 2CO 3Or K 2CO 3Or Li 2CO 3And Ba 2CO 3Or K 2CO 3And Ba 2CO 3-3.188-2.926
MoO 3-85.824-81.824 Na 2CO 3-3.219-2.953
SiO 2-5.910-5.648 Eu 2O 3-5.754-5.493
NH 4F-0.05-0.04 Tb 4O 7-0.055-0.050；
2. with the above-mentioned material that takes by weighing after grinding is mixed, the alumina crucible of packing into add a cover put into High Temperature Furnaces Heating Apparatus air 600-900 ℃ sintering 2-3 hour;
3. the cooling back is taken out and is pulverized, reinstall in the alumina crucible and add a cover, put into 600-900 ℃ of sintering 2-4 of High Temperature Furnaces Heating Apparatus air hour, cooling is taken out porphyrize and is obtained exciting the crystal powder that sends bright ruddiness down at 365nm and purple LED, the rare earth luminescent material of itself and greening, blue light is coated on the purple LED tube core after the mixed routinely can sends white light.
3, according to the preparation method of the described red rare earth luminescent material for purple light LED conversion white light of claim 2, it is characterized in that: 2. go on foot 900 ℃ of sintering temperatures, 3 hours time, and 3. go on foot 900 ℃ of sintering temperatures, 4 hours time.
CNA2008100511552A 2008-09-12 2008-09-12 Red rare earth luminescent material for purple light LED conversion white light and preparation thereof Pending CN101348714A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
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CN101906301A (en) * 2010-02-05 2010-12-08 四川新力光源有限公司 Red fluorescent powder and preparation method thereof and light-emitting diode light source device
CN101693834B (en) * 2009-09-24 2012-07-04 东北师范大学 Rare-earth red light-emitting material for converting purple light LED into white light and preparation process thereof
WO2014067113A1 (en) * 2012-10-31 2014-05-08 海洋王照明科技股份有限公司 Silicate luminescent material and preparation method therefor
CN103881719A (en) * 2012-12-22 2014-06-25 奇美实业股份有限公司 Phosphor and light emitting device
CN104371721A (en) * 2014-10-17 2015-02-25 乐山东承新材料有限公司 Rare earth red fluorescent powder and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101693834B (en) * 2009-09-24 2012-07-04 东北师范大学 Rare-earth red light-emitting material for converting purple light LED into white light and preparation process thereof
CN101906301A (en) * 2010-02-05 2010-12-08 四川新力光源有限公司 Red fluorescent powder and preparation method thereof and light-emitting diode light source device
CN101906301B (en) * 2010-02-05 2013-06-05 四川新力光源股份有限公司 Red fluorescent powder and preparation method thereof and light-emitting diode light source device
WO2014067113A1 (en) * 2012-10-31 2014-05-08 海洋王照明科技股份有限公司 Silicate luminescent material and preparation method therefor
CN103881719A (en) * 2012-12-22 2014-06-25 奇美实业股份有限公司 Phosphor and light emitting device
US9096798B2 (en) 2012-12-22 2015-08-04 Chi Mei Corporation Phosphor and luminescent device
CN103881719B (en) * 2012-12-22 2015-11-04 奇美实业股份有限公司 Phosphor and light emitting device
CN104371721A (en) * 2014-10-17 2015-02-25 乐山东承新材料有限公司 Rare earth red fluorescent powder and preparation method thereof

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