CN107033903A - A kind of single matrix phosphate white fluorescent powder of rare earth ion and doped transition metal ionses and preparation method thereof - Google Patents
A kind of single matrix phosphate white fluorescent powder of rare earth ion and doped transition metal ionses and preparation method thereof Download PDFInfo
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- CN107033903A CN107033903A CN201710433241.9A CN201710433241A CN107033903A CN 107033903 A CN107033903 A CN 107033903A CN 201710433241 A CN201710433241 A CN 201710433241A CN 107033903 A CN107033903 A CN 107033903A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7795—Phosphates
- C09K11/7796—Phosphates with alkaline earth metals
Abstract
The invention discloses a kind of rare earth ion and single matrix phosphate white fluorescent powder of doped transition metal ionses, its chemical general formula is：Ca8.78‑x‑ySrxBayEu0.06Mn0.16Ce(PO4)7, wherein 0≤x≤1.0,0≤y≤1.0, and x it is different with y when be 0.Its preparation method includes：a）Mol ratio according to each element of the chemical general formula of fluorescent material is weighed containing Ca, Sr, Ba, Eu, Mn, Ce, the oxide of P element, carbonate or phosphate, is mixed, and is stirred, and grinding obtains mixture；b）Mixture is placed in reducing atmosphere, heat temperature raising roasting obtains sintered body；c）Sintered body is cooled to be fully ground after room temperature and produced.White fluorescent powder excitation wavelength range prepared by the present invention is wide, luminous intensity is high, can effectively be excited by specific UV wavelength, send bright white light, it is good by heat endurance, and the high temperature solid-state method used, preparation technology is simple, it is easy to operational control, it is safe, preparation time is short, and production efficiency is high, suitable for industrialization large-scale production and application.
Description
Technical field
The present invention relates to luminescent material and preparation method, specifically a kind of rare earth ion and doped transition metal ionses
Single matrix phosphate white fluorescent powder and preparation method thereof.
Background technology
White light LEDs (Light Emitting Diode, light emitting diode) are considered as the traditional incandescent lamp of substitution, fluorescence
The forth generation solid light source of lamp and high-intensity gas discharge lamp.LED component have energy-conservation, efficiently, environmental protection, small volume, make
With long lifespan, reliability it is high, can intelligent manipulation the advantages of, be widely used in various illuminations and display field.
At present, LED realizes that the approach of white light emission mainly has four kinds：(1) LED of feux rouges, green glow and blue light is launched respectively
Chip portfolio together, makes three kinds of optical superposition of RGB together, forms white light；(2) black light or purple LED chip are excited
Launch feux rouges, green glow, three kinds of fluorescent material of blue light respectively, red, green, blue is mixed into white light；(3) blue-light LED chip excites Huang
Color fluorescent material, blue light and gold-tinted are mixed into white light；(4) the single substrate fluorescent powder of UV LED chip excited white light transmitting.The first reality
Existing mode is different due to driving voltage needed for three kinds of LED of red, green, blue, and circuit is complicated, and cost is higher, narrower using scope.Second
, there is sink effect by blue colour fluorescent powder glows to red fluorescence powder so that the white light formed is in reality in the scheme of kind
Color drift phenomenon is produced during use.Current most popular technical scheme is the third, and used blue-ray LED is
Gallium nitride diode, the ripe yellow fluorescent powder of Technical comparing is YAG:Ce3+, it can be by 440-480nm blue-light LED chip
Effectively excite, with blue light formation white light, its advantage is that luminosity is high, electro-optical efficiency is high, heat endurance is strong, still
Also have in some obvious shortcomings, such as spectrum and lack red color components, cause colour temperature higher, glow color is colder, colour rendering compared with
Difference, the fluorescent material particle size of reaction synthesis is difficult to control.4th kind of scheme increasingly attracts attention in recent years, single base of matrix three
Color fluorescent material possesses many advantages, for example, it is possible to prevente effectively from self-absorption phenomenon, colour rendering index height, color and adjustable color etc..
Therefore, it is the problem that research staff tries to explore in current industry to continually develop a greater variety of single matrix three primary colors fluorescent powders.
The content of the invention
It is an object of the invention to provide a kind of single matrix phosphate of rare earth ion and doped transition metal ionses white
Fluorescent material and its preparation method, the selection of more market demands is provided for white fluorescent powder.
The purpose of the present invention is achieved through the following technical solutions：A kind of rare earth ion and doped transition metal ionses
Single matrix phosphate white fluorescent powder, it is characterised in that its chemical general formula is：
Ca8.78-x-ySrxBayEu0.06Mn0.16Ce(PO4)7, wherein 0≤x≤1.0,0≤y≤1.0, and x it is different with y when be
0。
Preferably, x=0.2 in chemical general formula, during y=0.2, the heat endurance of prepared fluorescent material is best.
The invention also discloses a kind of rare earth ion and single matrix phosphate white fluorescent powder of doped transition metal ionses
Preparation method, comprise the following steps：
(a) according to the chemical general formula Ca of fluorescent material8.78-x-ySrxBayEu0.06Mn0.16Ce(PO4)7The mol ratio of middle each element
Weigh containing Ca, Sr, Ba, Eu, Mn, Ce, the oxide of P element, carbonate or phosphate, mix, stir, grinding must be mixed
0 ＜ x≤1.0,0 ＜ y≤1.0 in thing, the chemical general formula, and x it is different with y when be 0；
(b) mixture is placed in reducing atmosphere, is heated to 1150-1250 DEG C of roasting 7-8h, obtains sintered body；
(c) gained sintered body is cooled to after room temperature and be fully ground, obtain rare earth ion and doped transition metal ionses
Phosphate white fluorescent powder.
Step (a) milling time is 20-30min.
The chemical formula of fluorescent material described in step (a) is Ca8.38Sr0.2Ba0.2Eu0.06Mn0.16Ce(PO4)7, the fluorescent material
Heat endurance is best.
Heating rate described in step (b) is 2-5 DEG C/min.
Step (b) reducing atmosphere refers to big particle diameter carbon dust embedding or H2With N2The reducing atmosphere of mixed gas formation.
Step (b) is described to be heated to 1150-1250 DEG C of roasting 8h, preferably 1200 DEG C roasting 8h.
In the prior art, transmitting feux rouges, green can not be produced in most of fluorescent material of single host doped element simultaneously
The centre of luminescence of light and blue light, so that the spectral content of the white light obtained not enough enriches, display property is poor, limits this kind of
The application of white emitting fluorescent powder.The fluorescent material that the present invention is provided is by by the rare earth ion Eu of special ratios2+And transition metal ions
Mn2+It is doped in single-matrix as activator and sensitizer, forms the centre of luminescence, come from matrix sensitized luminescence mechanism, success
Described technology barrier is overcome, while by Sr and Ba and the specific Sr/Ba doping ratios of adulterating, obtaining bright, heat
The strong single phosphate matrix white fluorescent powder of stability.Fluorescent material prepared by the present invention has very strong broadband in 280-350nm
Absorb, launch wavelength scope 360-750nm, in this wave-length coverage, full spectral emissions can be achieved, meet near ultraviolet LED chip
Excite requirement.And white fluorescent powder excitation wavelength range prepared by the present invention is wide, luminous intensity is high, can be by specific UV ripple
Length is effectively excited, and sends bright white light, especially, luminous intensity subtracts the fluorescent material of some existing single host dopeds at high temperature
Weak, bad stability, the present invention significantly improves the fluorescent material by adulterate Sr and Ba and specific Sr/Ba doping ratio
Luminous intensity under the high temperature conditions.The high temperature solid-state method that the white fluorescent powder that the present invention is provided is used, its preparation technology is simple,
Easily operated control, safe, preparation time is short, and production efficiency is high, suitable for industrialization large-scale production and application.
Brief description of the drawings
Fig. 1 is the XRD spectrum and the comparison diagram of standard diagram of fluorescent material prepared by embodiment 1 and embodiment 6.
Fig. 2 is exciting and launching collection of illustrative plates for fluorescent material prepared by embodiment 3.
Fig. 3 is the chromaticity coordinates of fluorescent material prepared by the embodiment of the present invention 1,5,6,10 and 12.
Fig. 4 is the alternating temperature spectrum of fluorescent material prepared by the embodiment of the present invention 1,6,12 and comparative example 1.
Embodiment
Example below is used to the present invention is further described, but the invention is not limited in any way.
Embodiment 1
(1) each raw material is weighed by following weight：1.139g CaCO3, 0.039g SrCO3, 0.014g Eu2O3、
0.024g MnCO3, 1.068g NH4H2PO4, 0.228g CeO2, it is well mixed, stirring grinds 20min, obtains mixture；
(2) mix powder after grinding is placed in small crucible, and in H2With N2(H2With N2Volume ratio be 9:1)
It is calcined in reducing atmosphere, is warming up to 1200 DEG C by 2 DEG C/min of the rate of heat addition, 8h is sintered at such a temperature, naturally cool to room
Temperature, obtains sintered body；
(3) gained sintered body is cooled to after room temperature and be fully ground, obtain rare earth ion and doped transition metal ionses
Single matrix phosphate white fluorescent powder Ca8.58Sr0.2Eu0.06Mn0.16Ce(PO4)7。
Embodiment 2-5
Embodiment 2-5 preparation method be the same as Example 1, only raw material proportioning is different, and it matches somebody with somebody when prepared fluorescence
Powder chemical formula is as follows：
| Project | The fluorescent material of preparation | CaCO3/g | SrCO3/g | Eu2O3/g | MnCO3/g | NH4H2PO4/g | CeO2/g |
| Embodiment 2 | Ca8.38Sr0.4Eu0.06Mn0.16Ce(PO4)7 | 1.112 | 0.078 | 0.014 | 0.024 | 1.068 | 0.228 |
| Embodiment 3 | Ca8.18Sr0.6Eu0.06Mn0.16Ce(PO4)7 | 1.086 | 0.117 | 0.014 | 0.024 | 1.068 | 0.228 |
| Embodiment 4 | Ca7.98Sr0.8Eu0.06Mn0.16Ce(PO4)7 | 1.059 | 0.157 | 0.014 | 0.024 | 1.068 | 0.228 |
| Embodiment 5 | Ca7.78Sr1.0Eu0.06Mn0.16Ce(PO4)7 | 1.033 | 0.196 | 0.014 | 0.024 | 1.068 | 0.228 |
Embodiment 6
(1) each raw material is weighed by following weight：1.139g CaCO3, 0.052g BaCO3, 0.014g Eu2O3、
0.024g MnCO3, 1.068g NH4H2PO4、0.228g CeO2, it is well mixed, stirring grinds 20min, obtains mixture；
(2) mix powder after grinding is placed in small crucible, and in H2With N2(H2With N2Volume ratio be 9:1)
It is calcined in reducing atmosphere, is warming up to 1200 DEG C by 2 DEG C/min of the rate of heat addition, 8h is sintered at such a temperature, naturally cool to room
Temperature, obtains sintered body；
(3) gained sintered body is cooled to after room temperature and be fully ground, obtain rare earth ion and doped transition metal ionses
Single matrix phosphate white fluorescent powder Ca8.58Ba0.2Eu0.06Mn0.16Ce(PO4)7。
Embodiment 7-10
Embodiment 7-10 preparation method be the same as Example 6, only raw material proportioning is different, and it matches somebody with somebody when prepared fluorescence
Powder chemical formula is as follows：
| Project | The phosphate phosphor of preparation | CaCO3/g | BaCO3/g | Eu2O3/g | MnCO3/g | NH4H2PO4/g | CeO2/g |
| Embodiment 7 | Ca8.38Ba0.4Eu0.06Mn0.16Ce(PO4)7 | 1.112 | 0.105 | 0.014 | 0.024 | 1.068 | 0.228 |
| Embodiment 8 | Ca8.18Ba0.6Eu0.06Mn0.16Ce(PO4)7 | 1.086 | 0.157 | 0.014 | 0.024 | 1.068 | 0.228 |
| Embodiment 9 | Ca7.98Ba0.8Eu0.06Mn0.16Ce(PO4)7 | 1.059 | 0.209 | 0.014 | 0.024 | 1.068 | 0.228 |
| Embodiment 10 | Ca7.78Ba1.0Eu0.06Mn0.16Ce(PO4)7 | 1.033 | 0.262 | 0.014 | 0.024 | 1.068 | 0.228 |
Embodiment 11
(1) each raw material is weighed by following weight：1.123g CaCO3, 0.039g SrCO3, 0.026g BaCO3、
0.014g Eu2O3, 0.024g MnCO3, 1.065g NH4H2PO4, 0.228g CeO2, it is well mixed, stirs, grinding
20min, obtains mixture；
(2) mix powder after grinding is placed in small crucible, and in H2With N2(H2With N2Volume ratio be 9:1)
It is calcined in reducing atmosphere, is warming up to 1200 DEG C by 2 DEG C/min of the rate of heat addition, 8h is sintered at such a temperature, naturally cool to room
Temperature, obtains sintered body；
(3) gained sintered body is cooled to after room temperature and be fully ground, obtain rare earth ion and doped transition metal ionses
Single matrix phosphate white fluorescent powder Ca8.48Sr0.2Ba0.1Eu0.06Mn0.16Ce(PO4)7。
Embodiment 12-14
Embodiment 12-14 preparation method be the same as Example 11, only raw material proportioning is different, and it is with when prepared glimmering
Light powder chemical formula is as follows：
| Project | The phosphate phosphor of preparation | CaCO3/g | SrCO3/g | BaCO3/g | Eu2O3/g | MnCO3/g | NH4H2PO4/g | CeO2/g |
| Embodiment 12 | Ca8.38Sr0.2Ba0.2Eu0.06Mn0.16Ce(PO4)7 | 1.110 | 0.039 | 0.052 | 0.014 | 0.024 | 1.065 | 0.228 |
| Embodiment 13 | Ca8.28Sr0.4Ba0.1Eu0.06Mn0.16Ce(PO4)7 | 1.097 | 0.078 | 0.026 | 0.014 | 0.024 | 1.065 | 0.228 |
| Embodiment 14 | Ca8.18Sr0.4Ba0.2Eu0.06Mn0.16Ce(PO4)7 | 1.083 | 0.078 | 0.052 | 0.014 | 0.024 | 1.065 | 0.228 |
Comparative example 1
(1) each raw material is weighed by following weight：1.165g CaCO3, 0.014g Eu2O3, 0.024g MnCO3、
1.068g NH4H2PO4, 0.228g CeO2, it is well mixed, stirring grinds 20min, obtains mixture；
(2) mix powder after grinding is placed in small crucible, and in H2With N2(H2With N2Volume ratio be 9:1)
It is calcined in reducing atmosphere, is warming up to 1200 DEG C by 2 DEG C/min of the rate of heat addition, 8h is sintered at such a temperature, naturally cool to room
Temperature, obtains sintered body；
(3) gained sintered body is cooled to after room temperature and be fully ground, obtain rare earth ion and doped transition metal ionses
Single matrix phosphate white fluorescent powder Ca8.78Eu0.06Mn0.16Ce(PO4)7。
The optics and other performances of fluorescent material prepared by the detection embodiment of embodiment 15 and comparative example.
Experimental method：
Detect Ca prepared by embodiment 1 and 68.58Sr0.2Eu0.06Mn0.16Ce(PO4)7And Ca8.58Ba0.2Eu0.06Mn0.16Ce
(PO4)7, the X ray diffracting spectrum for obtaining the fluorescent material is as shown in Figure 1.
Detect Ca prepared by embodiment 38.18Sr0.6Eu0.06Mn0.16Ce(PO4)7, obtain its excitation and emission spectra, such as Fig. 2
It is shown, excitation wavelength lambda in figureex=320nm, transmitting band obtains recombined white light transmitting, successfully prepares nearly purple from 360nm to 750nm
The white light emission fluorescent material that outer LED is excited.
The fluorescent material that detection embodiment 1, embodiment 5, embodiment 6, embodiment 10 and embodiment 12 are prepared respectively
Ca8.58Sr0.2Eu0.06Mn0.16Ce(PO4)7、Ca7.78Sr1.0Eu0.06Mn0.16Ce(PO4)7、Ca8.58Ba0.2Eu0.06Mn0.16Ce
(PO4)7、Ca7.78Ba1.0Eu0.06Mn0.16Ce(PO4)7And Ca8.38Sr0.2Ba0.2Eu0.06Mn0.16Ce(PO4)7Chromaticity coordinates, such as
Shown in Fig. 3；Illustrate that the fluorescent material of synthesis on the basis of white light emission, realizes Color tunable, colour temperature is controllable.
The Ca that detection embodiment 1, embodiment 6, embodiment 12 and comparative example 1 are prepared respectively8.58Sr0.2Eu0.06Mn0.16Ce
(PO4)7、Ca8.58Ba0.2Eu0.06Mn0.16Ce(PO4)7、Ca8.38Sr0.2Ba0.2Eu0.06Mn0.16Ce(PO4)7、
Ca8.78Eu0.06Mn0.16Ce(PO4)7Alternating temperature spectrum, individually doping Sr or Ba after, the luminance temperature stability of material has been carried
It is high.When adulterate simultaneously Sr and Ba after, the luminance temperature stability of material have (a) in further raising, such as Fig. 4, (b),
(c), shown in (d).
Preparation method described in description of the invention can prepare fluorescent material to be protected of the invention, in disclosed technique
The fluorescent material prepared under parameter is respectively provided with the substantially similar experiment effect of part fluorescent material of the detection of embodiment 15.
Claims (6)
1. single matrix phosphate white fluorescent powder of a kind of rare earth ion and doped transition metal ionses, it is characterised in that it is changed
Learning formula is：
Ca8.78-x-ySrxBayEu0.06Mn0.16Ce(PO4)7, wherein 0≤x≤1.0,0≤y≤1.0, and x it is different with y when be 0.
2. single matrix phosphate white fluorescent powder of rare earth ion according to claim 1 and doped transition metal ionses,
Characterized in that, x=0.2, y=0.2.
3. a kind of preparation method of single matrix phosphate white fluorescent powder of rare earth ion and doped transition metal ionses, its feature
It is, comprises the following steps：
（a）According to the chemical general formula Ca of fluorescent material8.78-x-ySrxBayEu0.06Mn0.16Ce(PO4)7The mol ratio of middle each element is weighed
Containing Ca, Sr, Ba, Eu, Mn, Ce, the oxide of P element, carbonate or phosphate, mix, stir, grinding obtains mixture, institute
State 0≤x≤1.0,0 in chemical general formula≤y≤1.0, and x it is different with y when be 0；
（b）The mixture is placed in reducing atmosphere, 1150-1250 DEG C of roasting 7-8h is heated to, obtains sintered body；
（c）Gained sintered body is cooled to after room temperature and is fully ground, single base of rare earth ion and doped transition metal ionses is obtained
Matter phosphate white fluorescent powder.
4. single matrix phosphate white fluorescent powder of rare earth ion according to claim 3 and doped transition metal ionses
Preparation method, it is characterised in that step（a）The milling time is 20-30min.
5. single matrix phosphate white fluorescent powder of rare earth ion according to claim 3 and doped transition metal ionses
Preparation method, it is characterised in that step（b）Described heating rate is 2-5 DEG C/min.
6. single matrix phosphate white fluorescent powder of rare earth ion according to claim 3 and doped transition metal ionses
Preparation method, it is characterised in that step（b）The reducing atmosphere refers to big particle diameter carbon dust embedding or H2With N2Mixed gas is formed
Reducing atmosphere.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217621A (en) * | 2018-03-02 | 2018-06-29 | 西北大学 | A kind of phosphate and the synthesis and application using its fluorescent powder as matrix |
| CN109679653A (en) * | 2019-01-14 | 2019-04-26 | 惠州学院 | A kind of single-substrate white LED white fluorescent powder |
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| CN103589424A (en) * | 2013-09-24 | 2014-02-19 | 厦门通士达新材料有限公司 | Yellow orange-orange red fluorescent material and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103589424A (en) * | 2013-09-24 | 2014-02-19 | 厦门通士达新材料有限公司 | Yellow orange-orange red fluorescent material and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| CHAO WANG ET AL.: "Crystal structure, luminescence properties, energy transfer and thermal properties of a novel color-tunable, white light-emitting phosphor Ca9-x-yCe(PO4)7:xEu2+,yMn2+", 《PHYS. CHEM. CHEM. PHYS.》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217621A (en) * | 2018-03-02 | 2018-06-29 | 西北大学 | A kind of phosphate and the synthesis and application using its fluorescent powder as matrix |
| CN109679653A (en) * | 2019-01-14 | 2019-04-26 | 惠州学院 | A kind of single-substrate white LED white fluorescent powder |
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