CN101205465A - White light emission luminescent material and method for making same - Google Patents

White light emission luminescent material and method for making same Download PDF

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Publication number
CN101205465A
CN101205465A CNA2007101153521A CN200710115352A CN101205465A CN 101205465 A CN101205465 A CN 101205465A CN A2007101153521 A CNA2007101153521 A CN A2007101153521A CN 200710115352 A CN200710115352 A CN 200710115352A CN 101205465 A CN101205465 A CN 101205465A
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CN
China
Prior art keywords
white light
nitrate
luminescent material
light emission
fluorescent material
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Pending
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CNA2007101153521A
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Chinese (zh)
Inventor
吕孟凯
邱子凤
周媛媛
杨忠森
周广军
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Shandong University
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Shandong University
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Priority to CNA2007101153521A priority Critical patent/CN101205465A/en
Publication of CN101205465A publication Critical patent/CN101205465A/en
Pending legal-status Critical Current

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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02BCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

Abstract

The invention provides a white light-emitting fluorescent material and a preparation method thereof, wherein the chemical formula of the fluorescent material is Ba2LaZrO5.5:Ce<3+>. The preparation method of the white light-emitting fluorescent material includes the following steps: firstly, barium nitrate, lanthanum nitrate, zirconium nitrate and cerous nitrate are dissolved in deionized water; secondly, urea and citric acid, which are added in the solution, are heated up and stirred after dissolution; thirdly, combustion sintering at 500 to 900 DEG C is completed; finally, the sintering product is ground and made into the white light-emitting luminescent material through heat treatment after thermal insulation at 1,050 to 1,150 DEG C. The fluorescent material prepared through adopting combustion method can emit white light and has higher emission intensity, uniform phase, small product granularity (at nanometer grade) and excellent chemical stability; moreover, the fluorescent material prepared by the invention does not have toxicity or generates radiation, and belongs to environment-friendly luminescent material; meanwhile, the fluorescent material has simple and safe preparation process and relatively low production temperature, thereby saving energy sources.

Description

A kind of white light emission luminescent material and preparation method thereof
Technical field
The present invention relates to a kind of white light emission luminescent material and this preparation methods, belong to the luminescent material technical field.
Technical background
Japan in 1993 at first goes up at blue GaN photodiode (LED) and obtains technological breakthrough, and realizes white light LEDs, the developmental stage of the 4th lighting source of forward in recent years in 1996---and the direction based on the semiconductor illuminating light source of white light LEDs develops.Compare with the traditional lighting light source, white light LEDs has many advantages, as: volume is little, less energy consumption, response is fast, the life-span is long, pollution-free etc., therefore be called the 4th generation lighting source.The plurality of advantages of white light LEDs makes it that huge following illumination market and remarkable energy-conservation prospect be arranged.
At present, the technological approaches of realization white light emission mainly contains following several:
(1) Red Green Blue led chip or primitive colours LED pipe mix the realization white light.The former is three chip-shaped, and the latter is that three luminotrons are packaging.Three chip-shaped luminescent materials mainly contain GaAsP, ALGaAs, GaP:Zn 2O etc. glow; ALGalnP/GaAs, ALGalnP/GaP etc. glow and orange light; The GaP:N green light; The lnGaN blue light-emitting.Red, green, blue LED is encapsulated in the bag, and light efficiency can reach 20lm/W, and luminous efficiency is higher, and color developing is good.Primitive colours LED mixes, and adjusts the may command color by Red Green Blue light.But three chip-shaped three primary colors mixed costs are higher, and have red, green, blue led chip light decay different and easily produce defective such as metachromatism.
(2) the blue-light excited yellow-green fluorescence powder that sends of blue led chip is luminous, blue light is mixed with yellow, green glow send white light.Blue light lnGaN single-chip excites YAG fluorescent material, sends white light, and light efficiency can reach 15lm/W.This method is luminous, the luminous efficiency height, and preparation is simple, the temperature stability height, color developing might as well.But color becomes with angle, and light consistency is poor.Obviously, according to the colorimetry principle, also can send white light with blue-light excited ruddiness, green light fluorescent powder.
(3) UV-light or purple LED excite three primary colors fluorescent material, send white light.Obviously also can select two primary colours, four primary colours, five primary colours fluorescent material for use, realize white light LEDs equally.The white light of this method is decided by fluorescent material, easily realizes higher color developing, and the white light preparation method is also simple and easy to do.But have luminous efficiency low, temperature stability is poor, defectives such as the easy omission of purple light.
By above-mentioned situation as can be seen, no matter be the principle that adopts complementary color, or three primary colours blended principle, all exist certain drawback.In addition, mostly the preparation of existing luminescent material is to realize that by solid sintering technology this method sintering temperature height (being higher than 1300 ℃) wastes energy, and has luminescence center shortcoming pockety in matrix.
Summary of the invention
Reduce at luminous efficiency in the white light LEDs manufacturing processed, drawbacks such as colour rendering index instability, the invention provides a kind of luminous efficiency height, the white light emission luminescent material that colour rendering index is stable, this fluorescent material is under the exciting of near-ultraviolet light, its emission wavelength ranges comprises three kinds of colors of red, green, blue, can realize the white light emission under single thing mutually.A kind of preparation method of this white light emission luminescent material is provided simultaneously.
The chemical formula of white light emission luminescent material of the present invention is:
Ba 2LaZrO 5.5:Ce 3+
The preparation method of above-mentioned white light emission luminescent material may further comprise the steps:
(1) 200: 100: 100 in molar ratio: 1-10 got nitrate of baryta, lanthanum nitrate, zirconium nitrate (Zr (NO 3) 45H 2O) and cerous nitrate, be dissolved in the deionized water together;
(2) in above-mentioned solution, add relative four kinds of nitrate mole total amount 2-5 doubly urea and 1-3 doubly-water citric acid, the dissolving back 100 ℃-180 ℃ following heated and stirred 10-50 minute;
(3) with above-mentioned solution at 500 ℃ of-900 ℃ of following sintering 5-40 minutes, products therefrom is ground the back 1050 ℃-1150 ℃ insulations 1 hour, can obtain being the white light emission luminescent material Ba of micro-yellow powder shape 2LaZrO 5.5: Ce 3+
The present invention adopts the white light emission luminescent material Ba of combustion method preparation 2LaZrO 5.5: Ce 3+, emissive porwer is higher, and thing is mutually even, and the product granularity is little, belong to nano level, and chemical stability is good.In addition, the fluorescent material that the present invention obtains is nontoxic, radiationless, belongs to the environmental type luminescent material, and preparation technology is simple, safety.Because this method is to prepare presoma in liquid phase, each components contents can accurately be controlled, and reactive component can mix on molecular level, and synthesis temperature is relatively low, can save the energy.
Embodiment
Embodiment 1
200: 100: 100 in molar ratio: 1 took by weighing nitrate of baryta 100g, lanthanum nitrate 62.16g, zirconium nitrate (Zr (NO respectively 3) 45H 2O) 82.12g and cerous nitrate 0.62g, the urea 91.92g that four kinds of nitrate mole total amounts are 2 times, the citric acid 80.48g that four kinds of nitrate mole total amounts are 1 times, be dissolved in the deionized water, 100 ℃ of following heated and stirred 50 minutes, 500 ℃ of following sintering 40 minutes, products therefrom is ground the back 1050 ℃ of insulations 1 hour then, can obtain being the white light emission luminescent material Ba of micro-yellow powder shape 2LaZrO 5.5: Ce 3+
Embodiment 2
200: 100: 100 in molar ratio: 3 took by weighing nitrate of baryta 100g, lanthanum nitrate 62.16g, zirconium nitrate (Zr (NO respectively 3) 45H 2O) 82.12g and cerous nitrate 1.86g, the urea 115.47g that four kinds of nitrate mole total amounts are 2.5 times, the citric acid 121.32g that four kinds of nitrate mole total amounts are 1.5 times, be dissolved in the deionized water, 120 ℃ of following heated and stirred 40 minutes, 600 ℃ of following sintering 35 minutes, products therefrom is ground the back 1050 ℃ of insulations 1 hour then, can obtain being the white light emission luminescent material Ba of micro-yellow powder shape 2LaZrO 5.5: Ce 3+
Embodiment 3
200: 100: 100 in molar ratio: 5 took by weighing nitrate of baryta 100g, lanthanum nitrate 62.16g, zirconium nitrate (Zr (NO respectively 3) 45H 2O) 82.12g and cerous nitrate 3.1g, the urea 116g that four kinds of nitrate mole total amounts are 2.5 times, the citric acid 162.57g that four kinds of nitrate mole total amounts are 2 times, be dissolved in the deionized water, 140 ℃ of following heated and stirred 30 minutes, 700 ℃ of following sintering 20 minutes, products therefrom is ground the back 1100 ℃ of insulations 1 hour then, can obtain being the white light emission luminescent material Ba of micro-yellow powder shape 2LaZrO 5.5: Ce 3+
Embodiment 4
200: 100: 100 in molar ratio: 8 took by weighing nitrate of baryta 100g, lanthanum nitrate 62.16g, zirconium nitrate (Zr (NO respectively 3) 45H 2O) 82.12g and cerous nitrate 4.96g, the urea 140.29g that four kinds of nitrate mole total amounts are 3 times, the citric acid 204.71g that four kinds of nitrate mole total amounts are 2.5 times, be dissolved in the deionized water, 160 ℃ of following heated and stirred 20 minutes, 800 ℃ of following sintering 10 minutes, products therefrom is ground the back 1150 ℃ of insulations 1 hour then, can obtain being the white light emission luminescent material Ba of micro-yellow powder shape 2LaZrO 5.5: Ce 3+
Embodiment 5
200: 100: 100 in molar ratio: 10 took by weighing nitrate of baryta 100g, lanthanum nitrate 62.16g, zirconium nitrate (Zr (NO respectively 3) 45H 2O) 82.12g and cerous nitrate 6.2g, the urea 235g that four kinds of nitrate mole total amounts are 5 times, the citric acid 246.86g that four kinds of nitrate mole total amounts are 3 times, be dissolved in the deionized water, 180 ℃ of following heated and stirred 10 minutes, 900 ℃ of following sintering 5 minutes, products therefrom is ground the back 1150 ℃ of insulations 1 hour then, can obtain being the white light emission luminescent material Ba of micro-yellow powder shape 2LaZrO 5.5: Ce 3+

Claims (2)

1. white light emission luminescent material, it is characterized in that: the chemical formula of this white light emission luminescent material is: Ba 2LaZrO 5.5: Ce 3+
2. the preparation method of a white light emission luminescent material, the chemical formula of this white light emission luminescent material is Ba 2LaZrO 5.5: Ce 3+, it is characterized in that: may further comprise the steps:
(1) 200: 100: 100 in molar ratio: 1-10 got nitrate of baryta, lanthanum nitrate, zirconium nitrate and cerous nitrate, was dissolved in together in the deionized water;
(2) in above-mentioned solution, add relative four kinds of nitrate mole total amount 2-5 urea and 1-3 Citric acid monohydrate Food grade doubly doubly, the dissolving back 100 ℃-180 ℃ following heated and stirred 10-50 minute;
(3) with above-mentioned solution at 500 ℃ of-900 ℃ of following sintering 5-40 minutes, products therefrom is ground the back 1050 ℃-1150 ℃ insulations 1 hour, can obtain being the white light emission luminescent material Ba of micro-yellow powder shape 2LaZrO 5.5: Ce 3+
CNA2007101153521A 2007-12-14 2007-12-14 White light emission luminescent material and method for making same Pending CN101205465A (en)

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Application Number Priority Date Filing Date Title
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CN101205465A true CN101205465A (en) 2008-06-25

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102942928A (en) * 2012-11-30 2013-02-27 苏州大学 Zirconate-base red phosphor, method for preparing same and application
CN113502160A (en) * 2021-08-17 2021-10-15 淄博职业学院 Blue light excited ultraviolet fluorescent powder and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102942928A (en) * 2012-11-30 2013-02-27 苏州大学 Zirconate-base red phosphor, method for preparing same and application
CN113502160A (en) * 2021-08-17 2021-10-15 淄博职业学院 Blue light excited ultraviolet fluorescent powder and preparation method thereof

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Open date: 20080625