CN107384398A - A kind of YAG fluorescent powder and preparation method thereof and YAG fluorescence ceramics prepared therefrom - Google Patents

A kind of YAG fluorescent powder and preparation method thereof and YAG fluorescence ceramics prepared therefrom Download PDF

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CN107384398A
CN107384398A CN201710595397.7A CN201710595397A CN107384398A CN 107384398 A CN107384398 A CN 107384398A CN 201710595397 A CN201710595397 A CN 201710595397A CN 107384398 A CN107384398 A CN 107384398A
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yag
fluorescent powder
yag fluorescent
fluorescence ceramics
preparation
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周有福
李小强
张云峰
洪茂椿
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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Priority to PCT/CN2017/114990 priority patent/WO2019015227A1/en
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Abstract

This application discloses a kind of YAG fluorescent powder and preparation method thereof and YAG fluorescence ceramics prepared therefrom, the luminescent center ion of the YAG fluorescent powder includes Ce3+With the M of transmitting red/green；Its preparation method includes：Each raw material is mixed, obtained mixture carries out high temperature process heat, produces.The YAG fluorescent powder improves the problem of original fluorescent material colour rendering index is relatively low, colour temperature is higher, and avoids the light decay problem that traditional LED lamp uses for a long time；The YAG fluorescent ceramic packages LED that the YAG fluorescent powder is prepared can produce the high-quality illumination effect of simulated solar irradiation.

Description

A kind of YAG fluorescent powder and preparation method thereof and YAG fluorescence ceramics prepared therefrom
Technical field
The application is related to a kind of YAG fluorescent powder and preparation method thereof and YAG fluorescence ceramics prepared therefrom, belongs to fluorescent material And fluorescence ceramics field.
Background technology
White light LEDs are as a kind of new solid state light emitter, and compared with the light sources such as traditional incandescent lamp and fluorescent lamp, it has Environmental protection, save, be efficient, responding the advantages that fast, being described as after three big light source of incandescent lamp, fluorescent lamp and high-voltage gas discharging light Forth generation green light source.In LED light source, the performance of fluorescent material determines LED luminous efficiencies, colour rendering index, colour temperature and made With technical indicators such as life-spans, therefore, fluorescent material has very important status in white light LEDs, receives significant attention.
YAG (yttrium-aluminium-garnet, Y3Al5O12) fluorescent material be in white light LED part commonly use a kind of luminescent material.Wherein with Ce3+YAG fluorescent powder for the centre of luminescence is one of material being most widely used at present, and its luminescent spectrum scope is wide, and light effect Rate is high, stable performance.Due to YAG:Ce3+Only contain yellow component in luminescent spectrum, lack feux rouges, green color components, cause white light LEDs Colour rendering index it is relatively low, the problems such as colour temperature is higher, it is impossible to meet the requirement of human eye comfort level, human eye is through long-term evolution to sunshine Feel comfortably cool, therefore the illumination of simulated solar irradiation is that the high-quality for meeting human eye health lights.
The content of the invention
According to the one side of the application, there is provided a kind of YAG fluorescent powder and preparation method thereof, the YAG fluorescent powder improve The problem of original fluorescent material colour rendering index is relatively low, colour temperature is higher, and avoid the light decay that traditional LED lamp uses for a long time and ask Topic.
The luminescent center ion of the YAG fluorescent powder includes Ce3+And M；Wherein, M launches red/green.
Preferably, the M is at least one of rare earth ion, transition metal ions.
Preferably, the rare earth metal is at least one of Pr, Tb, Eu, Dy, Nd, Sm；Transition metal be Cr, Ti, V, At least one of Ni, Cu.
It is further preferred that the rare earth metal is Pr or Tb；Transition metal is Cr or Ti.
Preferably, the M is Cr3+、Cr3+And Tb3+、Ti3+、Pr3+And Tb3+、Pr3+Or Tb3+。
It is further preferred that it is 1 that the M, which is mol ratio,:1 Cr3+And Tb3+Or mol ratio is 1:1 Pr3+And Tb3+。
Preferably, Ce and Y mol ratio is 0.002 in the YAG fluorescent powder:1~0.06:1, M and Al mol ratio is 0.001:1~0.01:1.
It is further preferred that the Ce and Y mol ratio is 0.02:1~0.06:1, M and Al mol ratio is 0.001:1 ~0.005:1.
It is further preferred that the Ce and Y mol ratio is 0.02:1、0.03:1 or 0.06:1；M and Al mol ratio For 0.001:1、0.002:1、0.003:1、0.005:1 or 0.01:1.
The preparation method of the YAG fluorescent powder, including：
Silicon source, yttrium source and luminescent center ion source are mixed in organic solvent, dries, obtains mixture；Then flowing Under dynamic protection of reducing atmosphere, obtained mixture is subjected to high temperature process heat, obtains YAG fluorescent powder.
Preferably, source of aluminium is aluminum oxide；Yttrium source is at least one of yittrium oxide, yttrium carbonate；Luminescent center ion Source is oxide, carbonate corresponding to luminescent center ion；The boiling point of the organic solvent is no more than 120 DEG C at ambient pressure；Institute State dry for first organic solvent is boiled off in Rotary Evaporators, then move in 70 DEG C~90 DEG C of drying box continue drying out 4h~ 6h；The reducing atmosphere is N2/H2Mixed atmosphere；The temperature of the high temperature process heat is that the time is no less than not less than 1500 DEG C 2h。
Preferably, heated up during high temperature process heat for the stage, be warming up to 900 first with 8~10 DEG C/min speed DEG C~1100 DEG C, reaction temperature is then warming up to 4 DEG C/min~5 DEG C/min speed.
It is further preferred that being heated up during high temperature process heat for the stage, it is warming up to first with 10 DEG C/min speed 1000 DEG C, reaction temperature is then warming up to 5 DEG C/min speed.
Preferably, the temperature of the high temperature process heat is 1500 DEG C~1700 DEG C, and the time is 2h~6h.
Preferably, particle diameter≤20 μm of the aluminum oxide, purity >=99.9%；The μ of the particle diameter of yittrium oxide and yttrium carbonate≤20 M, purity >=99.9%；Particle diameter≤20 μm in luminescent center ion source, purity >=99.9%.
Preferably, particle diameter≤15 μm in the luminescent center ion source, purity >=99.9%.
Preferably, source of aluminium is at least one of Alpha-alumina, beta-alumina, gama-alumina；
The boiling point of organic solvent is no more than 100 DEG C at ambient pressure；The temperature of the high temperature process heat be 1500 DEG C~ 1600 DEG C, the time is 4h~5h.
Preferably, the aluminum oxide is at least one of Alpha-alumina and gama-alumina；Organic solvent is acetone, second At least one of ether, petroleum ether, ethanol.
Preferably, source of aluminium, yttrium source and luminescent center ion source are powder.
Preferably, raw material is sufficiently mixed uniformly by the organic solvent by wet-mixing.
Preferably, the addition of the organic solvent for silicon source, yttrium source and luminescent center ion source quality sum 5~ 99%.
It is further preferred that the addition of the organic solvent for silicon source, yttrium source and luminescent center ion source quality it The 10~50% of sum.
A kind of YAG fluorescence ceramics that the application provides again, the fluorescence ceramics are by the YAG fluorescent powder and/or described The YAG fluorescent powder that method is prepared obtains by broken, shaping, sintering, post processing.
Preferably, it is described to be broken for ball mill crushing；Being shaped to will be first dry-pressing formed then cold etc. by the YAG powders of ball milling Hydrostatic profile, obtain YAG biscuits；It is sintered in the temperature not less than 1750 DEG C and carries out vacuum-sintering；Post-process and thrown for grinding Light.
It is further preferred that the ball mill crushing is：The YAG powders are mixed with appropriate sintering aid, using height Pure alumina abrading-ball, absolute ethyl alcohol are that medium carries out ball milling.
Preferably, the sintering aid is calcirm-fluoride (CaF2) and tetraethyl orthosilicate (TEOS).
Preferably, it is described it is broken after the obtained particle diameter of YAG fluorescent powder be no more than 1mm.
It is further preferred that it is described it is broken after the obtained particle diameter of YAG fluorescent powder be no more than 0.01mm.
Preferably, generation under the exciting of at least one section glistening light of waves of the YAG fluorescence ceramics in 320nm~480nm (450nm~800nm) high-quality lights.
Preferably, the light of blue-light LED chip of the YAG fluorescence ceramics in 465nm is sent out under exciting in 480~750nm Light (high-quality of simulated solar irradiation lights).
Preferably, the temperature of the sintering is 1750~1800 DEG C, and the time is 7h~8h.
Preferably, the straight line transmittance of the YAG fluorescence ceramics is 50%~80%.
Preferably, the preparation method of the YAG fluorescence ceramics, including：
(1) dispensing：Using alumina powder, yittrium oxide, cerium oxide, chrome green as reaction raw materials；Wherein, alumina powder Particle diameter≤20 μm, purity >=99.9%；Particle diameter≤20 μm of yittrium oxide, purity >=99.9%；Particle diameter≤20 μm of cerium oxide, it is pure Degree >=99.9%；Particle diameter≤15 μm of chrome green, purity >=99.9%.
(2) batch mixing：Using lower boiling organic solvent of the boiling point under normal pressure not higher than 120 DEG C as medium, pass through material by wet type mixing So that aluminum oxide, yittrium oxide, cerium oxide, chrome green are sufficiently mixed, uniform slurry is obtained；
(3) dry：By slurry drying obtained by step (2), sieving, mixed powder is obtained；
(4) high―temperature nuclei：The mixed powder that step (3) obtains is fitted into crucible, is placed in high temperature furnace, is passed through flowing N2/H2Gaseous mixture, soak, synthesize high-purity YAG powders；
(5) ball mill crushing：The YAG powders of step (4) synthesis are sieved, ball milling, appropriate sintering aid is added, dries To component homogenous superfine YAG powders；
(6) it is molded：The ultra-fine YAG powders that step (5) obtains obtain YAG biscuit of ceramics through shaping；
(7) sinter：YAG biscuits are fitted into crucible, are placed in vacuum tungsten coil furnace, are incubated under high temperature, vacuum-sintering is made YAG ceramics；
(8) post-process：The YAG ceramics that step (7) obtains are ground polishing, obtain high-quality YAG fluorescence ceramics.
Preferably, the YAG fluorescence ceramics are applied to LED.
The present invention is for YAG in the prior art:Ce3+The shortcomings that fluorescent material feux rouges, green portions deficiency, in common YAG: Ce3+Fluorescent material, which introduces, to glow, the luminescent center ion M of green glow, and YAG is made:Ce3+, M crystalline ceramics is as white Light LED encapsulating material, the problem of original fluorescent material colour rendering index is relatively low, colour temperature is higher is not only improved, and avoid biography LED of uniting uses for a long time, light decay problem caused by packaging silicon rubber is thermally decomposed.Furthermore, it is possible to concentration and class by adjusting M Type, the luminous parameters such as colour temperature luminous regulation and control LED and spectrum, lights so as to obtain the high-quality of simulated solar irradiation.
Beneficial effect caused by the application energy includes：
1) introduced in YAG fluorescent powder provided herein it is one or more can launch red/green it is luminous in Heart ion, obtained in the case where the blue light of blue-light LED chip excites and the high-quality of the simulated solar irradiation of human eye health is lighted (480nm~750nm).
2) LED of YAG fluorescent ceramic packages provided herein, heated point of traditional LED lamp packaging silicon rubber is avoided Light decay problem caused by solution, while the advantage that the high-quality for obtaining simulated solar irradiation lights.
3) method raw material provided herein be easy to get extensively, technique it is simple, be adapted to large-scale production, be prepared for purity The high YAG fluorescent powder body of height, better crystallinity degree, luminescent quality, the YAG fluorescent ceramic packages LED of preparation can produce simulated solar irradiation High-quality illumination effect.
Brief description of the drawings
Fig. 1 is the XRD spectrum of P1 in embodiment 1；
Fig. 2 is the XRD spectrum of C1 in embodiment 2；
Fig. 3 is the emission spectrum that C1 is packaged into LED lamp with blue-light LED chip in embodiment 2；
Fig. 4 is the emission spectrum that D1 is packaged into LED lamp with blue-light LED chip in comparative example 1.
Embodiment
The application is described in detail with reference to embodiment, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material in embodiments herein, solvent and auxiliary agent are bought by commercial sources, are not entered Row processing.
Analysis method is as follows in embodiments herein：
XRD spectrum analyses are carried out using X-ray diffractometer (Miniflex-600, Rigaku Japan)；Using spectrum analysis System (PMS-80, Hangzhou distant place photoelectricity company) carries out LED emission spectrographic analysis.
The method of testing of colour rendering index, colour temperature and heat endurance is as follows in embodiments herein：
The test of colour rendering index calculates analysis emission spectrum from tape program using PMS-80 systems and obtained.
The test of colour temperature is using HASS-2000 spectrometers band integrating sphere (Hangzhou distant place photoelectricity company).
Embodiment 1
The preparation of YAG fluorescent powder.
Obtain mixing different Ce and M mol ratio according to plan, calculate the mixed proportion of silicon source, yttrium source, cerium and M powders, Powder is placed in same container；Appropriate organic solvent is added into the container equipped with powder, is mixed by mechanical agitation Powder is sufficiently mixed, and mixed slurry is placed in Rotary Evaporators and quickly boils off organic solvent, and 5 are dried in 80 DEG C of drying box Sieved after hour；Mixture loads crucible after sieving, in flowing N2/H2In atmosphere, in tube furnace first with 10 DEG C/min heating Speed is warming up to 1000 DEG C, then is warming up to reaction temperature with 5 DEG C/min heating rate, reacts natural cooling after a period of time, Obtain the high-quality YAG fluorescent powder body.
The relation of sample number into spectrum and raw material type, proportioning, specific preparation condition is as shown in table 1.
Table 1
The thing of 1~P6 of sample P obtained by the present embodiment is mutually analyzed using method of X-ray diffraction, the results showed that powder 1~P6 of sample P is pure YAG phases (PDF NO.33-40), the XRD spectrums of sample P 1 in Typical Representative such as Fig. 1,2~P6's of sample P XRD spectrum results approach with Fig. 1, are pure YAG phases.
Embodiment 2
The preparation of YAG fluorescence ceramics (transparent).
After 1~P6 of sample P prepared by embodiment 1 crosses 150 mesh sieves respectively, with appropriate calcirm-fluoride (CaF2) and silicic acid four Ethyl ester (TEOS) complex sintering aids mix, using high purity aluminium oxide abrading-ball, ratio of grinding media to material 10：1, absolute ethyl alcohol is medium, ball Mill 12 hours, drying obtain the sample P 1 ' by ball milling~P6 ' (particle diameter 0.001mm)；By by ball milling sample P 1 '~ P6 ' is first dry-pressing formed under 10MPa respectively, then the cold isostatic compaction under 200MPa, obtains YAG biscuits；YAG biscuits are loaded Crucible, it is placed in vacuum tungsten coil furnace, vacuumizes, be warming up to 1800 DEG C with 6 DEG C/min heating rate, be incubated 8 hours, carries out true Sky sintering, obtain YAG ceramics；Polishing is ground to YAG ceramics, obtains diameter about 10mm, thickness about 1.0mm fluorescence pottery Porcelain, ceramic C1~C6 is designated as respectively.
Material phase analysis is carried out to ceramic C1~C6 obtained above.As a result show, ceramics sample C1~C6 is in sintering procedure Middle thing is mutually without significant change.Sample C1 XRD spectrums in Typical Representative such as Fig. 2, sample C2~C6 XRD spectrum results approach with Fig. 2, For pure YAG phases.
Ceramic C1 obtained above and blue-light LED chip are packaged into LED lamp C11, the simulation of its emission spectrum (such as Fig. 3) Sunshine (480~750nm), luminescent quality is high, beneficial to human eye health.
Comparative example 1
The preparation of common YAG fluorescence ceramics.
In the comparative example in the preparation process of YAG fluorescent powder, M is added without；Wherein, the addition of silicon source, yttrium source and cerium with And preparation condition is identical with P1~P6 respectively, common YAG fluorescent powder Q1~Q6 is obtained.
Using Q1~Q6 obtained above, prepare common YAG fluorescence ceramics D1~D6, preparation condition with embodiment 2 It is identical.
D1 obtained above and blue-light LED chip are packaged into LED lamp D11, its emission spectrum is Fig. 4.
C11 and D11 colour rendering index, colour temperature data are as shown in table 2.
Table 2
Can be seen that sample in embodiment from the data in table 2 improves the colour rendering index of sample in comparative example well The problem of relatively low and colour temperature is higher.
It is described above, only it is several embodiments of the application, any type of limitation is not done to the application, although this Shen Please with preferred embodiment disclose as above, but and be not used to limit the application, any person skilled in the art, do not taking off In the range of technical scheme, make a little variation using the technology contents of the disclosure above or modification is equal to Case study on implementation is imitated, is belonged in the range of technical scheme.

Claims (10)

1. a kind of YAG fluorescent powder, it is characterised in that the luminescent center ion of the YAG fluorescent powder includes Ce3+And M；Wherein, M is sent out Penetrate red/green.
2. YAG fluorescent powder according to claim 1, it is characterised in that the M be rare earth ion, transition metal from At least one of son.
Preferably, the rare earth metal is at least one of Pr, Tb, Eu, Dy, Nd, Sm；Transition metal be Cr, Ti, V, Ni, At least one of Cu.
3. YAG fluorescent powder according to claim 1 or 2, it is characterised in that Ce and Y mol ratio in the YAG fluorescent powder For 0.002:1~0.06:1, M and Al mol ratio is 0.001:1~0.01:1.
Preferably, the mol ratio of the Ce and Y are 0.02~0.06:1, M and Al mol ratio is 0.001~0.005:1.
4. a kind of preparation method of YAG fluorescent powder as described in any one of claims 1 to 3, including：
Silicon source, yttrium source and luminescent center ion source are mixed in organic solvent, dries, obtains mixture；Then in flowing also Under former atmosphere protection, obtained mixture is subjected to high temperature process heat, obtains YAG fluorescent powder.
5. the preparation method of YAG fluorescent powder according to claim 4, it is characterised in that source of aluminium is aluminum oxide；It is described Yttrium source is at least one of yittrium oxide, yttrium carbonate；Luminescent center ion source is oxide, carbonic acid corresponding to luminescent center ion Salt；
The boiling point of the organic solvent is no more than 120 DEG C at ambient pressure；
The temperature of the high temperature process heat is 1500 DEG C~1700 DEG C, and the time is 2h~6h.
6. the preparation method of YAG fluorescent powder according to claim 4, it is characterised in that source of aluminium be Alpha-alumina, β- At least one of aluminum oxide, gama-alumina；
The boiling point of organic solvent is no more than 100 DEG C at ambient pressure；
The temperature of the high temperature process heat is 1500 DEG C~1600 DEG C, and the time is 4h~5h.
7. a kind of YAG fluorescence ceramics, it is characterised in that the YAG fluorescence ceramics are as described in any one of claims 1 to 3 The YAG fluorescent powder that any one of YAG fluorescent powder and/or claim 4 to 6 methods described are prepared is by broken, shaping, burning Knot, post processing obtain.
8. YAG fluorescence ceramics according to claim 7, it is characterised in that the YAG fluorescence ceramics are in 320nm~480nm In at least one section glistening light of waves exciting under produce 450nm~800nm light；
The temperature of the sintering is 1750~1800 DEG C.
9. YAG fluorescence ceramics according to claim 7, it is characterised in that blue light of the YAG fluorescence ceramics in 465nm The light of LED chip excites down to light in 480nm~750nm.
10. YAG fluorescence ceramics according to claim 9, it is characterised in that the YAG fluorescence ceramics are applied to LED.
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