Preparation method of MxSr(1-x)TiO3:Eu3+ high-purity red fluorescent powder used for high-color-gamut LEDs

A red light phosphor, high color gamut technology, applied in chemical instruments and methods, luminescent materials, semiconductor devices, etc., can solve the problem of uneven mixing of activators, low color purity of red light, and uneven particle size of phosphor particles. and other problems, to achieve the effect of uniform particle size distribution, high red color purity, and low equipment requirements

Active Publication Date: 2016-05-04
SHENZHEN JUFEI OPTOELECTRONICS
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Problems solved by technology

[0005] For this reason, the technical problem to be solved by the present invention is to overcome the Eu obtained by traditional solid-phase method 3+ Activate SrTiO 3 Due to the direct high-temperature calcination of the red light phosphor material, the activator in the obtained phosphor is unevenly mixed, resulting in a broadband emission peak of the red light phosphor, low color purity of red light, and the technical bottleneck of uneven particle size of the phosphor powder. Thus a high color gamut LED with M x Sr 1-x TiO 3 : Eu 3+ Preparation method of high-purity red phosphor

Method used

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  • Preparation method of MxSr(1-x)TiO3:Eu3+ high-purity red fluorescent powder used for high-color-gamut LEDs
  • Preparation method of MxSr(1-x)TiO3:Eu3+ high-purity red fluorescent powder used for high-color-gamut LEDs
  • Preparation method of MxSr(1-x)TiO3:Eu3+ high-purity red fluorescent powder used for high-color-gamut LEDs

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Embodiment 1

[0030] Embodiment 1 This embodiment discloses a kind of M x Sr 1-x TiO 3 : Eu 3+ The preparation method of high-purity red fluorescent powder, the specific steps are as follows:

[0031] (1) According to the molar ratio of Ca:Sr:Ti=0.2:0.8:1, weigh 0.395g of CaCO 3 Powder, 2.126g of Sr(OH) 2 ·8H 2 O and 4.021g of Ti(SO 4 ) 2 9H 2 O. According to Eu 3+ The molar concentration is 4mo% (referring to Eu 3+ Accounted for matrix material Ca 0.2 Sr 0.8 TiO 3 molar concentration), weigh 0.070g of Eu 2 o 3 Powder.

[0032] (2) the CaCO in step 1) 3 , Sr(OH) 2 ·8H 2 O, Ti(SO 4 ) 2 9H 2 O and Eu 2 o 3 Put the powder together in 100mL of 30% HNO 3 In solution, incubate at 50°C for 90 minutes to obtain clear Ca 2+ 、Sr 2+ 、Ti 4+ and Eu 3+ mixture.

[0033] (3) According to C 6 h 8 o 7 (citric acid): the molar ratio of Ti=2.25:1, weigh 4.728g of C 6 h 8 o 7 ·H 2 O is placed in the solution of step 2), and then the solution is placed on a magnetic stirrer,...

Embodiment 2

[0037] Embodiment 2 This embodiment discloses a M x Sr 1-x TiO 3 : Eu 3+ The preparation method of high-purity red fluorescent powder, the specific steps are as follows:

[0038] (1) According to the molar ratio of Mg:Ba:Sr:Ti=0.1:0.4:0.5:1, weigh 0.040g of MgO, 0.789g of BaCO 3 Powder, 1.329g of Sr(OH) 2 ·8H 2 O and 4.021g of Ti(SO 4 ) 2 9H 2 O. According to Eu 3+ The molar concentration is 1mol% (referring to Eu 3+ Accounting for matrix material Mg 0.1 Ba 0.4 Sr 0. 5 TiO 3 molar concentration), weigh 0.018g of Eu 2 o 3 Powder.

[0039] (2) MgO, BaCO in step 1) 3 , Sr(OH) 2 ·8H 2 O, Ti(SO 4 ) 2 9H 2 O and Eu 2 o 3 Put the powder together in 100mL of 30% HNO 3 In solution, keep warm at 70°C for 45min to obtain clear Mg 2+ 、Ba 2+ 、Sr 2+ 、Ti 4+ and Eu 3+ mixture.

[0040] (3) According to C 6 h 8 o 7 (citric acid): the ratio of Ti=3.2:1, weigh 6.724g of C 6 h 8 o 7 ·H 2 O is placed in the solution of step 2), and then the solution is place...

Embodiment 3

[0044] Embodiment 3 This embodiment discloses a M x Sr 1-x TiO 3 : Eu 3+ The preparation method of high-purity red fluorescent powder, the specific steps are as follows:

[0045] (1) According to the molar ratio of Zn:Sr:Ti=0.05:0.95:1, weigh 0.041g of ZnO powder, 2.525g of Sr(OH) 2 ·8H 2 O and 4.021g of Ti(SO 4 ) 2 9H 2 O. According to Eu 3+ The molar concentration is 0.2mol% (referring to Eu 3+ Accounted for matrix material Zn 0.05 Sr 0.95 TiO 3 molar concentration), weigh 0.004g of Eu 2 o 3 Powder.

[0046] (2) ZnO, Sr(OH) in step 1) 2 ·8H 2 O, Ti(SO 4 ) 2 9H 2 O and Eu 2 o 3 Put the powder together in 100mL of 30% HNO 3 solution, at 70°C for 40 minutes to obtain clear Zn 2+ 、Sr 2+ 、Ti 4+ and Eu 3+ mixture.

[0047] (3) According to C 6 h 8 o 7 (citric acid): Ti=3.8:1 ratio, weigh 7.985g of C 6 h 8 o 7 ·H 2 O is placed in the solution of step 2), and then the solution is placed on a magnetic stirrer, and the magnetic rotor speed is control...

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Abstract

The invention belongs to the technical field of fluorescent powder preparation achieved through a wet chemical method and particularly relates to a preparation method of MxSr(1-x)TiO3:Eu3+ high-purity red fluorescent powder used for high-color-gamut LEDs. MxSr(1-x)TiO3:Eu3+ (0<x<=0.5) high-purity red fluorescent powder prepared through a sol-gel method and used for LEDs is calcinated at low temperature at the later stage so that the MxSr(1-x)TiO3:Eu3+ high-purity red fluorescent powder can be obtained. Compared with a traditional high-temperature solid-phase method, the later-stage calcination temperature needed by the sol-gel method is low, the requirement for equipment is low, energy consumption is low, and the preparation method is suitable for industrial production. Eu3+ in the obtained fluorescent powder is uniform in dispersion and can easily enter MxSr(1-x)TiO3 to achieve energy transmission; emission peak half-wave width of the obtained red fluorescent powder is small, and the red light color purity is high; particle size distribution is uniform, the red fluorescent powder can be easily mixed with glue in later-stage application of the fluorescent powder, and the MxSr(1-x)TiO3:Eu3+ high-purity red fluorescent powder is suitable for being used for the high-color-gamut white-light LEDs.

Description

technical field [0001] The invention belongs to the technical field of preparing fluorescent powder by wet chemical method, and in particular relates to a M x Sr 1-x TiO 3 : Eu 3+ A preparation method of high-purity red phosphor powder. Background technique [0002] At present, rare earth luminescent materials have become the core materials in the fields of information display, lighting source, and optoelectronic devices. Among them, the most widely used is the phosphor material that can be excited by ultraviolet light-blue light (200-500nm) to produce different luminescent colors. The high color purity, high luminous intensity and evenly distributed particle size of phosphor powder can significantly improve the performance of LED devices. Red phosphor is a necessary material for white LEDs with high color gamut. At present, red phosphor matrix materials mainly include aluminate, silicate, tungstate and titanate, etc. There are differences in color purity and luminous ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/67H01L33/50
CPCC09K11/7728H01L33/502
Inventor 高丹鹏王旭改邢其彬
Owner SHENZHEN JUFEI OPTOELECTRONICS
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