CN102229802A - Rare earth double primary colour luminescent material for converting white light by utilizing violet light LED (light-emitting diode) and preparation method thereof - Google Patents
Rare earth double primary colour luminescent material for converting white light by utilizing violet light LED (light-emitting diode) and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of luminescence and display, relating to blue and yellow luminescent materials in a novel rare earth double primary colour luminescent material for converting white light by utilizing a violet light LED (light-emitting diode). The structural formulas of blue phosphor powder and yellow phosphor powder are MxN(4-x-y)Si3O8Cl4: Ry and WxS(4-x-y)Si3O8Cl4: Yy. Tz, wherein N is Sr element when M is Mg, and the phosphor powder is blue when R is Eu element. When W is Ca, S is Sr element and Y is Eu element, and the phosphor powder is yellow when T is Mn element. Materials are respectively weighed according to mass percent, after fully grinding and evenly mixing, calcining at a high temperature is carried out, a mixture is taken out after cooling is carried out, grinding is carried out, then high temperature calcining is carried out, and a sample is cooled and taken out to be ground, thus a power crystal emitting bright blue light or yellow light under the excitation of violet light is obtained. The blue phosphor powder and the yellow phosphor powder are mixed in a certain proportion to realize white light phosphor powder with different colour temperatures.
Description
Technical field
The invention belongs to luminous and the technique of display field, relate to a kind of LED conversion of white light into purple light rare earth two primary colours luminescent materials and preparation method thereof.
Background technology
Advantages such as white light LEDs is little owing to its volume, current consumption is low, the life-span is long, pollute less, thermal value is low with speed of response is fast become the first-selection of lighting engineering of future generation.Present commercial white light LEDs is to excite yellow fluorescent powder to produce white light with blue-light LED chip, causes having major defect aspect the color space homogeneity because the blue light of chip emission is participated in the formation white light directly, can't satisfy the needs of interior lighting.This technical barrier can utilize the influence of white color coordinate less purple light or near ultraviolet excitation broad band blueness are solved with the mode that yellow two primary colours fluorescent material produce white light.And the technology of utilizing purple light or near ultraviolet excitation two primary colours fluorescent material to generate white light requires the raising to the luminous efficiency of purple LED chip on the one hand, then needs on the other hand to develop at being fit to the blue and yellow two primary colours fluorescent material of the used high-performance of purple light or near-ultraviolet light conversion of white light.The present invention relates to that to modify its matrix scaffold structure regulating divalent europium luminous by the chlorine strontium silicate being mixed different alkali earth metals, realized the blue light of broad band and two kinds of luminescent materials of yellow emission, and prepared the white fluorescent powder that suitable purple LED excites from these two kinds of luminescent materials.These class two primary colours luminescent materials have advantages such as luminous efficiency height, synthesis technique is simple, colour temperature is adjustable, are the high efficient luminous materials that can be used for the LED conversion of white light into purple light purposes.
Summary of the invention
One of purpose of the present invention provides a kind of LED conversion of white light into purple light rare earth two primary colours luminescent materials.Two of purpose provides the preparation method of a kind of LED conversion of white light into purple light with rare earth two primary colours luminescent materials.
The LED conversion of white light into purple light preparation method of rare earth two primary colours luminescent materials:
1, the preparation method of blue colour fluorescent powder:
1. material chooses according to its chemical structural formula M
xN
4-x-ySi
3O
8Cl
4: R
y, when M was the Mg element, when N was the Sr element, when R was the Eu element, its weight percent took by weighing the following material of high purity:
SrCO
3：17.56％-26.44％ SrCl
2.6H
2O：53.67％-56.64％
SiO
2：18.36％-19.37％ Eu
2O
3：0.69％-3.5％
MgO：0.79％-3.07％
2. after the above-mentioned improved grinding that takes by weighing being mixed, the aluminum oxide of packing into monkey (30ml) is added a cover, monkey is packed in the big crucible (60ml), monkey is buried and added a cover (accompanying drawing one), put it in the High Temperature Furnaces Heating Apparatus 900 ℃～1100 ℃ calcinings 2 hours～4 hours down then with gac.
3. " porphyrize is taken out in sample cooling back, reinstalls the aluminum oxide monkey and adds a cover, and monkey is packed in the big crucible, with gac monkey is buried and is added a cover, and puts it in the High Temperature Furnaces Heating Apparatus 900 ℃～1100 ℃ calcinings 1 hour～3 hours down then.Cooling back is taken out porphyrize and is obtained that (λ=400nm) gives the crystal powder that sends brilliant blue light at purple light.
2, the preparation method of yellow fluorescent powder:
1. material chooses according to its chemical structural formula W
xS
4-x-ySi
3O
8Cl
4: Y
yWhen T was the Ca element as W, when S was the Sr element, when Y was the Eu element, when T was the Mn element, its weight percent took by weighing the following material of high purity:
SrCO
3：16.83％-28.02％ SrCl
2.6H
2O：47.25％-58.57％
SiO
2：15.96％-19.78％ Eu
2O
3：0.63％-2.59％
CaCO
3：1.87％-8.24％ MnCO
3：0-2.5％
2. after the above-mentioned improved grinding that takes by weighing being mixed, the aluminum oxide of packing into monkey is added a cover, and monkey is packed in the big crucible, with gac monkey is buried and is added a cover, and puts it in the High Temperature Furnaces Heating Apparatus 900 ℃～1100 ℃ calcinings 2 hours～4 hours down then.
3. porphyrize is taken out in sample cooling back, reinstalls the aluminum oxide monkey and adds a cover, and monkey is packed in the big crucible, with gac monkey is buried and is added a cover, and puts it in the High Temperature Furnaces Heating Apparatus 900 ℃～1100 ℃ calcinings 1 hour～3 hours down then.Cooling back is taken out porphyrize and is obtained that (λ=400nm) excites the crystal powder that sends bright sodium yellow down at purple light.
3, blueness that will make and yellow fluorescent powder be by 3: 4, obtains the white emitting fluorescent powder (accompanying drawing four) from warm white to cold white light different-colour after the mixed of 3: 3 or 2: 1.
Blue colour fluorescent powder and the yellow fluorescent powder of LED conversion of white light into purple light of the present invention in the broad band rare earth two primary colours luminescent materials, its structural formula: blue (M
xN
4-x-ySi
3O
8Cl
4: R
y), yellow (W
xS
4-x-ySi
3O
8Cl
4: Y
yT
z), when (1) was Mg as M, N was the Sr element, R is the Eu element, the powder crystal of the coloured light that obtains turning blue.When W is the Ca element, S is the Sr element, and Y is the Eu element, when T is the Mn element, and the powder crystal of the coloured light that obtains turning to be yellow, span 0.1≤x≤1 of x in (2) structural formula, span 0.02≤y≤0.08 of y, span 0≤z≤0.2 of z.
Broad band two its advantages of primary colours luminescent material that LED conversion of white light into purple light of the present invention is used are:
1. by single-matrix chlorine strontium silicate being carried out backbone modification when mixing magnesium elements and calcium constituent respectively, obtain the blue and xanchromatic fluorescent material of two kinds of broad bands.Regulate the white light that two primary colours luminescent material ratios obtain different-colour.
2. technology is simple, and is pollution-free.
Description of drawings
Accompanying drawing 1 is sample sample agglomerating synoptic diagram under the activated carbon reducing atmosphere.
Accompanying drawing 2 is for mixing magnesium and calcium constituent X ray material phase analysis figure afterwards.
Accompanying drawing 3 is for mixing the emmission spectrum figure under purple light (wavelength is 400nm) excites behind magnesium and the calcium constituent.
Accompanying drawing 4 for the blueness that makes and yellow fluorescent powder by the different white light of the resulting colour temperature of different mixed.Its chromaticity coordinates of warm white is (0.31,0.385), and positive its chromaticity coordinates of white light is (0.293,0.360), and its chromaticity coordinates of cold white light is (0.263,0.318).
Specific embodiments
Example one
The preparation of 1 blue colour fluorescent powder
Choosing of material according to its chemical structural formula
M 0.1 N 3.88 Si 3 O 8 Cl 4 : R 0.02 , when M is the Mg element, when N is the Sr element, when R is the Eu element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：23.58％ SrCl
2.6H
2O：55.22％
SiO
2：18.61％ Eu
2O
3：0.93％
MgO：1.66％
1. after the above-mentioned improved grinding that takes by weighing being mixed, the aluminum oxide of packing into monkey is added a cover, and monkey is packed in the big crucible, with gac monkey is buried and is added a cover, and puts it in the High Temperature Furnaces Heating Apparatus 900 ℃ of calcinings 2 hours down then.
2. porphyrize is taken out in sample cooling back, reinstalls the aluminum oxide monkey and adds a cover, and monkey is packed in the big crucible, with gac monkey is buried and is added a cover, and puts it in the High Temperature Furnaces Heating Apparatus 900 ℃ of calcinings 1 hour down then.Cooling back is taken out porphyrize and is obtained that (λ=400nm) gives the crystal powder that sends brilliant blue light at purple light.
The preparation of 2 yellow fluorescent powders
1. material chooses according to its chemical structural formula
W 0.1 S 3.88 Si 3 O 8 Cl 4 : Y 0.02 T 0 , when W is the Ca element, when S is the Sr element, when Y is the Eu element, when T is the Mn element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：23.01％ SrCl
2.6H
2O：53.88％
SiO
2：18.17％ Eu
2O
3：0.91％
CaCO
3：4.03％ MnCO
3：0％
2. after the above-mentioned improved grinding that takes by weighing being mixed, the aluminum oxide of packing into monkey is added a cover, and monkey is packed in the big crucible, with gac monkey is buried and is added a cover, and puts it in the High Temperature Furnaces Heating Apparatus 900 ℃ of calcinings 2 hours down then.
3. porphyrize is taken out in sample cooling back, reinstalls the aluminum oxide monkey and adds a cover, and monkey is packed in the big crucible, with gac monkey is buried and is added a cover, and puts it in the High Temperature Furnaces Heating Apparatus 900 ℃ of calcinings 1 hour down then.Cooling back is taken out porphyrize and is obtained that (λ=400nm) gives the crystal powder that sends bright sodium yellow at purple light.
Example two
The preparation of 1 blue colour fluorescent powder
1. material chooses according to its chemical structural formula
M 0.15 N 3.82 Si 3 O 8 Cl 4 : R 0.03 , when M is the Mg element, when N is the Sr element, when R is the Eu element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：22.01％ SrCl
2.6H
2O：55.21％
SiO
2：19.11％ Eu
2O
3：1.92％
MgO：1.75％
2. it puts into 950 ℃ of following calcinings of High Temperature Furnaces Heating Apparatus 2.5 hours.Put it into then in the High Temperature Furnaces Heating Apparatus and calcined 1.5 hours under 950 ℃.The sintering synthesis step is with example one.
The preparation of 2 yellow fluorescent powders
1. material chooses according to its chemical structural formula
W 0.15 S 3.81 Si 3 O 8 Cl 4 : Y 0.04 T 0 , when W is the Ca element, when S is the Sr element, when Y is the Eu element, when T is the Mn element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：23.09％ SrCl
2.6H
2O：51.01％
SiO
2：19.06％ Eu
2O
3：2.51％
CaCO
3：4.33％ MnCO
3：0％
2. it puts into 950 ℃ of following calcinings of High Temperature Furnaces Heating Apparatus 2.5 hours.Put it into then in the High Temperature Furnaces Heating Apparatus and calcined 1.5 hours under 950 ℃.The sintering synthesis step is with example one.
Example three
The preparation of 1 blue colour fluorescent powder
1. material chooses according to its chemical structural formula
M 0.35 N 3.71 Si 3 O 8 Cl 4 : R 0.04 , when M is the Mg element, when N is the Sr element, when R is the Eu element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：22.88％ SrCl
2.6H
2O：53.75％
SiO
2：18.71％ Eu
2O
3：2.91％
MgO：1.75％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 3 hours under 1000 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 2 hours under 1000 ℃.The sintering synthesis step is with example one.
The preparation of 2 yellow fluorescent powders
1. material chooses according to its chemical structural formula
W 0.35 S 3.71 Si 3 O 8 Cl 4 : Y 0.04 T 0 , when W is the Ca element, when S is the Sr element, when Y is the Eu element, when T is the Mn element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：22.21％ SrCl
2.6H
2O：53.58％
SiO
2：18.26％ Eu
2O
3：1.92％
CaCO
3：4.03％ MnCO
3：0％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 3 hours under 1000 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 2 hours under 1000 ℃.The sintering synthesis step is with example one.
Example four
1. the preparation of blue colour fluorescent powder
1. material chooses according to its chemical structural formula
M 0.3 N 3.64 Si 3 O 8 Cl 4 : R 0.06 , when M is the Mg element, when N is the Sr element, when R is the Eu element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：22.91％ SrCl
2.6H
2O：55.02％
SiO
2：19.11％ Eu
2O
3：1.42％
MgO：1.54％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 4 hours under 1050 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 3 hours under 1050 ℃.The sintering synthesis step is with example one.
2. the preparation of yellow fluorescent powder
1. material chooses according to its chemical structural formula
W 0.3 S 3.59 Si 3 O 8 Cl 4 : Y 0.06 T 0.05 , when W is the Ca element, when S is the Sr element, when Y is the Eu element, when T is the Mn element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：23.21％ SrCl
2.6H
2O：53.48％
SiO
2：17.37％ Eu
2O
3：1.41％
CaCO
3：4.03％ MnCO
3：0.5％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 4 hours under 1050 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 3 hours under 1050 ℃.The sintering synthesis step is with example one.
Example five
1. the preparation of blue colour fluorescent powder
1. material chooses according to its chemical structural formula
M 0.4 N 3.55 Si 3 O 8 Cl 4 : R 0.05 , when M is the Mg element, when N is the Sr element, when R is the Eu element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：19.58％ SrCl
2.6H
2O：56.22％
SiO
2：19.03％ Eu
2O
3：2.42％
MgO：2.75％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 4 hours under 1100 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 1 hour under 1100 ℃.The sintering synthesis step is with example one.
2. the preparation of yellow fluorescent powder
1. material chooses according to its chemical structural formula
W 0.4 S 3.45 Si 3 O 8 Cl 4 : Y 0.05 T 0.1 , when W is the Ca element, when S is the Sr element, when Y is the Eu element, when T is the Mn element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：23.23％ SrCl
2.6H
2O：50.66％
SiO
2：17.56％ Eu
2O
3：1.51％
CaCO
3：6.04％ MnCO
3：1.0％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 4 hours under 1100 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 1 hour under 900～1100 ℃.The sintering synthesis step is with example one.
Example six
1. the preparation of blue colour fluorescent powder
1. material chooses according to its chemical structural formula
M 0.5 N 3.44 Si 3 O 8 Cl 4 : R 0.06 , when M is the Mg element, when N is the Sr element, when R is the Eu element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：20.51％ SrCl
2.6H
2O：55.72％
SiO
2：18.60％ Eu
2O
3：2.42％
MgO：2.75％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 3 hours under 1000 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 3 hours under 1000 ℃.The sintering synthesis step is with example one.
2. the preparation of yellow fluorescent powder
1. material chooses according to its chemical structural formula
W 0.5 S 3.29 Si 3 O 8 Cl 4 : Y 0.06 T 0.15 , when W is the Ca element, when S is the Sr element, when Y is the Eu element, when T is the Mn element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：18.17％ SrCl
2.6H
2O：52.02％
SiO
2：18.05％ Eu
2O
3：2.22％
CaCO
3：8.04％ MnCO
3：1.5％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 3 hours under 1000 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 3 hours under 1000 ℃.The sintering synthesis step is with example one.
Example seven
1. the preparation of blue colour fluorescent powder
1. material chooses according to its chemical structural formula
M 0.6 N 3.33 Si 3 O 8 Cl 4 : R 0.07 , when M is the Mg element, when N is the Sr element, when R is the Eu element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：24.02％ SrCl
2.6H
2O：53.72％
SiO
2：19.20％ Eu
2O
3：1.61％
MgO：1.45％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 2 hours under 1100 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 2 hours under 900 ℃.The sintering synthesis step is with example one.
2. the preparation of yellow fluorescent powder
1. material chooses according to its chemical structural formula
W 0.6 S 3.15 Si 3 O 8 Cl 4 : Y 0.07 T 0.18 , when W is the Ca element, when S is the Sr element, when Y is the Eu element, when T is the Mn element, take by weighing the following material of following high purity by its weight percent:
SrCO
3：20.24％ SrCl
2.6H
2O：55.77％
SiO
2：18.07％ Eu
2O
3：1.89％
CaCO
3：2.03％ MnCO
3：2.0％
2. put it in the High Temperature Furnaces Heating Apparatus and calcined 2 hours under 1100 ℃, put it into then in the High Temperature Furnaces Heating Apparatus and calcined 2 hours under 900 ℃.The sintering synthesis step is with example one.
Example eight
Can realize the white emitting fluorescent powder (from warm white to cold white) of different-colour after blueness that makes according to example one to example seven methods and yellow fluorescent powder the mixed by 3: 4,1: 1 or 2: 1.
Claims (2)
1. LED conversion of white light into purple light is characterized in that step is as follows with the preparation method of rare earth two primary colours luminescent materials:
1), the preparation method of blue colour fluorescent powder:
1. material chooses according to its chemical structural formula M
xN
4-x-ySi
3O
8Cl
4: R
y, when M was the Mg element, when N was the Sr element, when R was the Eu element, its weight percent took by weighing the following material of high purity:
SrCO
3：17.56％-26.44％ SrCl
2.6H
2O：53.67％-56.64％
SiO
2：18.36％-19.37％ Eu
2O
3：0.69％-3.5％
MgO：0.79％-3.07％；
2. after the above-mentioned improved grinding that takes by weighing being mixed, the aluminum oxide of packing into monkey is added a cover, and monkey is packed in the big crucible, with gac monkey is buried and is added a cover, and puts it in the High Temperature Furnaces Heating Apparatus 900 ℃～1100 ℃ calcinings 2 hours～4 hours down then;
3. " porphyrize is taken out in sample cooling back; reinstall the aluminum oxide monkey and add a cover; monkey is packed in the big crucible; with gac monkey is buried and added a cover; put it in the High Temperature Furnaces Heating Apparatus 900 ℃～1100 ℃ calcinings 1 hour～3 hours down then, the cooling back is taken out porphyrize and obtained giving the crystal powder that sends brilliant blue light at the purple light of λ=400nm;
2), the preparation method of yellow fluorescent powder:
1. material chooses according to its chemical structural formula W
xS
4-x-ySi
3O
8Cl
4: Y
yWhen T was the Ca element as W, when S was the Sr element, when Y was the Eu element, when T was the Mn element, its weight percent took by weighing the following material of high purity:
SrCO
3：16.83％-28.02％ SrCl
2.6H
2O：47.25％-58.57％
SiO
2：15.96％-19.78％ Eu
2O
3：0.63％-2.59％
CaCO
3：1.87％-8.24％ MnCO
3：0-2.5％；
2. after the above-mentioned improved grinding that takes by weighing being mixed, the aluminum oxide of packing into monkey is added a cover, and monkey is packed in the big crucible, with gac monkey is buried and is added a cover, and puts it in the High Temperature Furnaces Heating Apparatus 900 ℃～1100 ℃ calcinings 2 hours～4 hours down then;
3. porphyrize is taken out in sample cooling back, reinstalling the aluminum oxide monkey adds a cover, monkey is packed in the big crucible, with gac monkey is buried and added a cover, put it in the High Temperature Furnaces Heating Apparatus 900 ℃～1100 ℃ calcinings 1 hour～3 hours down then, the cooling back is taken out porphyrize and is obtained the purple light excited crystal powder that sends bright sodium yellow down at λ=400nm;
3), the blueness that will make and yellow fluorescent powder be by 3: 4, obtains the white emitting fluorescent powder from warm white to cold white light different-colour after the mixed of 3: 3 or 2: 1,
Span 0.1≤x≤1 of x in the structural formula, span 0.02≤y≤0.08 of y, span 0≤z≤0.2 of z.
2. by the purple LED conversion of white light into purple light that the prepares rare earth two primary colours luminescent materials of the method for claim 1.
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| CN110433744A (en) * | 2019-07-30 | 2019-11-12 | 广州珠江光电新材料有限公司 | Fluorescent powder preparation facilities and preparation method |
| CN113004891A (en) * | 2021-02-02 | 2021-06-22 | 深圳大学 | Fluorescent powder and LED light source |
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| CN102766462A (en) * | 2012-07-26 | 2012-11-07 | 常州金凯照明电器有限公司 | Color temperature-tunable, universal and high performance fluorescent powder |
| CN102766462B (en) * | 2012-07-26 | 2015-03-25 | 常州金凯照明电器有限公司 | Color temperature-tunable, universal and high performance fluorescent powder |
| CN107634132A (en) * | 2017-09-28 | 2018-01-26 | 苏州轻光材料科技有限公司 | A kind of burst of ultraviolel white light LEDs containing Two Colour Fluorescence powder and preparation method thereof |
| CN110433744A (en) * | 2019-07-30 | 2019-11-12 | 广州珠江光电新材料有限公司 | Fluorescent powder preparation facilities and preparation method |
| CN113004891A (en) * | 2021-02-02 | 2021-06-22 | 深圳大学 | Fluorescent powder and LED light source |
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Application publication date: 20111102 |