CN109437900A - A kind of fluorescence ceramics block, preparation method and its application in laser lighting - Google Patents

A kind of fluorescence ceramics block, preparation method and its application in laser lighting Download PDF

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CN109437900A
CN109437900A CN201811516205.XA CN201811516205A CN109437900A CN 109437900 A CN109437900 A CN 109437900A CN 201811516205 A CN201811516205 A CN 201811516205A CN 109437900 A CN109437900 A CN 109437900A
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fluorescence ceramics
source
ceramics block
powder
sample
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孙鹏
刘永福
蒋俊
江浩川
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

This application discloses a kind of fluorescence ceramics block, preparation method and its application in laser lighting, which is selected from least one of the compound with chemical formula shown in formula 1.The thermal stability and high colour rendering index that the fluorescence ceramics block has had compared with conventional powder material.The preparation method of fluorescence ceramics block provided herein, the available fluorescence ceramics block haveing excellent performance, to meet its application in laser lighting.Application in laser lighting provided herein, colour rendering index is 80 or so, with YAG:Ce3+The made laser lighting device of fluorescence ceramics is obviously improved compared to (colour rendering index is less than 70), in illumination and display field, there is good application prospect.

Description

A kind of fluorescence ceramics block, preparation method and its application in laser lighting
Technical field
This application involves a kind of fluorescence ceramics block, preparation method and its applications in laser lighting, belong to ceramic material Expect technical field.
Background technique
Traditional LD illuminating device mainly synthesizes white light in such a way that blue light LD excites yellow fluorescent powder, which needs Yellow fluorescent powder is blended in silica gel and is packaged into illuminating device again, but it is about 0.1-0.4W/mK that silica gel thermal conductivity is lower, it is higher Laser power easily cause silica gel aging, and the thermal stability of phosphor material powder is also poor, both phenomenons can cause to shine Funerary objects part optical property decline, reduced service life the problems such as.For example, Zhou in 2017 et al. is reported for the first time Lu2Mg2Al2Si2O12:Ce3+Orange fluorescent powder (please refers to document A broad-band orange-yellow-emitting Lu2Mg2Al2Si2O12:Ce3+phosphor for application in warm white light-emitti ng Diodes, RSC Adv., 2017,7,46713-46720), emission peak of the fluorescent powder under the excitation of 436nm blue light is wider, and half Gao Kuanwei 144nm, emission peak range are 475-750nm, and it includes red spectral band abundant, with the material that most strong transmitting, which is located at 575nm, Expect the white light LEDs of production, colour rendering index is up to 84.5, however the thermal stability of the phosphor material powder is poor, at 150 DEG C, Luminous intensity falls to the 75% of green strength.Pan in 2015 et al. reports Mg2Y2Al2Si2O12:Ce3+Luminescent material (please join Examine document Combination cation substitution tuning of yellow-orange emitting phosphor Mg2Y2Al2Si2O12:Ce3+, RSC Adv., 2015,5,9489-9496), the material under the excitation of 460nm blue light, Its emission spectrum range is 500-800nm, is emitted for wide range, and most strong transmitting is located at 600nm, the white light LEDs made of the material, Colour rendering index is up to 84.7, and the thermal stability of the same fluorescent powder is also poor, and at 160 DEG C, luminous intensity falls to original The 84.7% of intensity.Above-mentioned reported two kinds of materials are powder body material, are obtained by high temperature solid-state method, still need to make in the application With traditional organic packages mode, high temperature ageing problem caused by weak heat-dissipating not can avoid, be difficult to apply in laser lighting device In.
At this stage, it proposes in the industry old using silica gel high temperature in the high thermal conductivity materials such as fluorescence ceramics solution conventional package mode Change problem, and fluorescence ceramics can be coupled directly with blue light LD, eliminate mixed glue and dispensing process, simplified illuminating device and made work Skill.Since fluorescence ceramics are directly synthesized by raw material through high temperature solid-state method, material is uniform, is more suitable for making laser lighting device.It grinds Study carefully that more and what is applied is the laser lighting device made using YAG:Ce fluorescence ceramics, however, since YAG:Ce fluorescence is made pottery Lack red light wave band in the emission spectrum of porcelain, gained illuminating device color developing is poor, and colour rendering index is serious to make less than 70 About its application and development in high colour developing illumination and display field.
It is asked so providing and becoming technology urgently to be resolved with the fluorescence ceramics block that thermal stability is good and colour rendering index is high Topic.
Summary of the invention
According to the one aspect of the application, a kind of fluorescence ceramics block is provided, which has excellent heat steady Qualitative and high colour rendering index.
The fluorescence ceramics block, selected from least one of the compound with chemical formula as shown in Equation 1,
A2-xQxM2L2D2O12Formula I
Wherein, A is selected from least one of Y element, Lu element, La element, Sc element, Gd element;
Eu element, Ce element, Pr element, Sm element, Dy element, Tm element, Tb element, Nd of the Q in rare earth element At least one of element;
M is selected from least one of Mg element, Ca element, Sr element, Ba element, Zn element;
L is selected from least one of Al element, Ga element;
D is selected from least one of Ti element, Si element, Ge element;
0.0001≤x≤0.3。
The upper limit of the value range of x is that the lower limit of the value range of 0.06,0.1,0.3, x is 0.0001,0.06,0.1.
Preferably, A is selected from Lu element and/or Y element.
Preferably, Q is selected from Ce element and/or Dy element.
Preferably, M is selected from Mg element and/or Ca element.
Preferably, D is selected from Si element and/or Ge element.
Present invention also provides a kind of methods for preparing above-mentioned fluorescence ceramics block, include at least step:
(1) powder will be prepared into containing the source A, the source Q, the source M, the source L, the mixture in the source D and additive;
(2) powder calcined, formed, obtain biscuit of ceramics;
(3) biscuit of ceramics is sintered, obtains fluorescence ceramics block.
Optionally, the source A is selected from least one of the oxide of A, salt of A;
The source Q is selected from least one of the oxide of Q, salt of Q;
The source M is selected from least one of the oxide of M, salt of M;
The source L is selected from least one of the oxide of L, salt of L;
The source D is selected from least one of the oxide of D, salt of D;
The additive includes MgO, SiO2、ZrO2、B2O3At least one of.
Specifically, the salt of A includes villaumite, carbonate, acetate etc.
The salt of Q includes villaumite, carbonate, acetate etc.
The salt of M includes villaumite, carbonate, acetate etc.
The salt of L includes villaumite, carbonate, acetate etc.
The salt of D includes villaumite, carbonate, acetate etc..
Additive is that technical field often uses sintering aid, such as: MgO, SiO2、ZrO2、B2O3Include Deng, the application but unlimited In above-mentioned additive, those skilled in the art can select according to needs of production.
In this application, it can use ball-milling method to mix the source A, the source Q, the source M, the source L, the source D.
Optionally, the partial size of powder is less than 10 microns.Preferably, the partial size of powder is less than 2 microns.
Optionally, the calcination process in step (2) are as follows: be warming up to 600~1200 DEG C, keep the temperature 1~10 hour.
In this application, considered critical is not done to molding mode, those skilled in the art can be according to needs of production Select suitable molding mode.
Optionally, the molding includes any one in dry-pressing formed, injection moulding, tape casting.
Specifically, the upper limit of calcination temperature is selected from 700 DEG C, 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C, 1200 DEG C, calcining The lower limit of temperature be selected from 600 DEG C, 700 DEG C, 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C.
The upper limit of soaking time in calcination process is in 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10h, calcination process Soaking time lower limit be selected from 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h.
After being calcined to powder, can using tape casting, injection moulding, isometric unidirectional, isometric bidirectional pressing and The forming methods such as isostatic cool pressing make biscuit of ceramics.
Optionally, the sintering process in step (3) are as follows: be warming up to I: 1000~1300 DEG C of sintering temperature, heat preservation 1~24 is small When, later it is further heated up to II: 1400~1500 DEG C of sintering temperature, keep the temperature 2~24 hours.
Specifically, the upper limit of sintering temperature I is selected from 1100 DEG C, 1250 DEG C, 1300 DEG C, and the lower limit of sintering temperature I is selected from 1000℃、1100℃、1250℃。
The upper limit of soaking time under sintering temperature I is selected from 2h, 4h, 10h, 16h, for 24 hours, the guarantor under sintering temperature I The lower limit of warm time is selected from 1h, 2h, 4h, 10h, 16h.
The upper limit of sintering temperature II is selected from 1450 DEG C, 1500 DEG C, and the lower limit of sintering temperature II is selected from 1400 DEG C, 1450 DEG C.
The upper limit of soaking time under sintering temperature II is selected from 4h, 10h, 16h, for 24 hours, the heat preservation under sintering temperature II The lower limit of time is selected from 2h, 4h, 10h, 16h.
The heating rate of sintering process be 0.1~200 DEG C/min, it is preferable that heating rate be 1 DEG C/min, 200 DEG C/ min。
When being sintered to biscuit of ceramics, can using discharge plasma sintering or vacuum-sintering or atmosphere sintering, Or the modes such as hot pressed sintering or HIP sintering are sintered.
It optionally, further include annealing after being sintered to biscuit of ceramics.
Preferably, annealing temperature is 900~1300 DEG C, and soaking time is 2~20h.
Preferably, annealing atmosphere is air atmosphere, oxidizing atmosphere or reducing atmosphere.
The upper limit of annealing temperature is selected from 1000 DEG C, 1100 DEG C, 1200 DEG C, 1300 DEG C, and the lower limit of annealing temperature is selected from 900 ℃、1000℃、1100℃、1200℃。
The upper limit of the soaking time of annealing is selected from 4h, 5h, 10h, 20h, the lower limit of the soaking time of annealing be selected from 2h, 4h, 5h、10h。
It optionally, after an annealing treatment, further include that fluorescence ceramics are processed by shot blasting, to control fluorescence ceramics Thickness and smoothness.
Present invention also provides a kind of laser lighting devices, by fluorescence ceramics block described above, any of the above-described side At least one of the fluorescence ceramics block that method is prepared, in conjunction with optical lens, with blue light laser diode with transmission-type light Road or reflection type optical path are obtained through Automatic manual transmission.
Fluorescence ceramics block provided by the present application can be any appropriate shape.Preferably, fluorescence ceramics block is side Shape block, cylindric block, round sheet body, rectangular sheet body etc..
Optionally, fluorescence ceramics block with a thickness of 0.1~10mm.Preferably, the fluorescence ceramics block with a thickness of 1mm。
Optionally, the emission peak of the blue light laser diode is 440~480nm.Preferably, the blue laser two The emission peak that pole pipe issues is 455nm.
Specifically, fluorescence ceramics block is from the blue light laser diode assembly production of different wattages at laser lighting device. The power of blue light laser diode is not specifically limited in the application, those skilled in the art can be according to needs of production Select the blue light laser diode of appropriate power.Preferably, the electrical power of the blue light laser diode is 1~20W, such as blue Ray laser diode can be 2W or may be 10W or can also be 20W.
Present invention also provides application of the above-mentioned laser lighting device in illumination or display field.
The beneficial effect that the application can generate includes:
1) fluorescence ceramics block provided herein has excellent thermal stability, while mechanical and mechanical property Also more prominent, hardness is up to 12GPa after tested.Gained fluorescence ceramics block can be assembled directly with blue light LD, and substitution is glimmering at present Light powder adds the encapsulation mode of organic material, efficiently solves organic packaging materials weak heat-dissipating, and light efficiency caused by continuous high temperature reduces And the problems such as color drift, it can significantly extend the service life of illuminating device.
2) fluorescence ceramics block provided herein, compared with phosphor material powder form, fluorescence ceramics have better Light-emitting uniformity improves the optical quality of illuminating device.
3) laser lighting device provided herein, colour rendering index is 80 or so, with YAG:Ce3+Fluorescence ceramics are made Laser lighting device is obviously improved compared to (colour rendering index is less than 70), in illumination and display field, there is good application Prospect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of sample C-5#;
Fig. 2 is the excitation-emission spectrogram of sample C-2#;
Fig. 3 is the thermostabilization curve of sample C-1#;
Fig. 4 is the device spectral figure of sample L-C-3#.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material in embodiments herein and additive are bought by commercial sources.
Embodiment 1 prepares fluorescence ceramics block Lu1.9999Ce0.0001Mg2Al2Si2O12
(1) Lu is stoichiometrically weighed2O3: 9.9478g, CeO2: 0.0004g, MgO:2.0152g, Al2O3: 2.5490g SiO2: 3.0042g and additive B2O3: 0.0017g;It is grinding with dehydrated alcohol with grinding pot plus zirconia ball Medium is ground and is mixed, until powder average grain diameter is less than 2 μm;
(2) gained slurry is dry and be sieved, by the 600 DEG C of heat preservation 10h in air of the powder after sieving, in removal powder Organic matter;2min will be kept using isometric unidirectional application 10Mpa pressure after gained calcining powder sieving, it is dry-pressing formed, by it Biscuit of ceramics, pressure 200MPa, dwell time 2min are pressed into isostatic cool pressing equipment;
(3) gained biscuit of ceramics is sintered, 1 DEG C/min of heating rate in a vacuum furnace, is kept the temperature at 1000 DEG C for 24 hours, It is kept the temperature at 1400 DEG C for 24 hours, completes solid phase reaction, excluded stomata and reach densification;
(4) sample after vacuum-sintering is being contained into 5vol.%H2And 95vol.%N2Reducing atmosphere it is lower 900 DEG C heat preservation 20h restores rare earth element;
(5) the fluorescence ceramics block after step (4) annealing is processed by shot blasting, is obtained Lu1.9999Ce0.0001Mg2Al2Si2O12Fluorescence ceramics piece, with a thickness of 1mm.It is denoted as sample C-1#.
Embodiment 2 prepares fluorescence ceramics block Lu1.9Ce0.1Mg2Al2Si2O12
(1) Lu is stoichiometrically weighed2O3: 9.4509g, CeO2: 0.4303g, MgO:2.0152g, Al2O3: 2.5490g SiO2: 3.0042g;With grinding pot plus zirconia ball, is ground and mixed using dehydrated alcohol as abrasive media, directly To powder average grain diameter less than 1 μm;
(2) gained slurry is dry and be sieved, by the 1200 DEG C of heat preservation 1h in air of the powder after sieving, in removal powder Organic matter;It will be formed in a mold in the way of injection molding after the sieving of gained powder, and carry out ungrease treatment, made pottery Porcelain biscuit;
(3) gained biscuit of ceramics is sintered, 1 DEG C/min of heating rate in hot isostatic pressing furnace, is kept the temperature at 1300 DEG C 1h completes solid phase reaction in 1500 DEG C of heat preservation 2h, excludes stomata and reaches densification;
(4) sample 1200 DEG C of heat preservation 2h annealing in air after being sintered;
(5) the fluorescence ceramics block after step (4) annealing is processed by shot blasting, obtains Lu1.9Ce0.1Mg2Al2Si2O12It is glimmering Light ceramic piece, with a thickness of 1mm.It is denoted as sample C-2#.
Embodiment 3 prepares fluorescence ceramics block Lu1.94Ce0.06Mg2Al2Si2O12
(1) Lu is stoichiometrically weighed2O3: 9.6499g, CeO2: 0.2582g, MgO:2.0152g, Al2O3: 2.5490g SiO2: 3.0042g;With grinding pot plus zirconia ball, is ground and mixed using dehydrated alcohol as abrasive media, directly To powder average grain diameter less than 5 μm;
(2) gained slurry is dry and be sieved, by the 900 DEG C of heat preservation 2h in air of the powder after sieving, in removal powder Organic matter;2min will be kept using isometric two-way application 5Mpa pressure after the sieving of gained powder, it is dry-pressing formed, by it cold etc. Biscuit, pressure 200MPa, dwell time 2min are pressed into static pressure equipment;
(3) gained biscuit of ceramics is sintered in discharge plasma sintering furnace, 200 DEG C/min of heating rate, 1100 DEG C of heat preservation 1h complete solid phase reaction in 1450 DEG C of heat preservation 2h, exclude stomata and reach densification;
(4) sample after sintering is being contained into 5vol.%H2And 95vol.%N2Reducing atmosphere lower 1000 DEG C of heat preservations 4h, it is right Rare earth element is restored;
(5) the fluorescence ceramics block after step (4) annealing is processed by shot blasting, is obtained Lu0.94YCe0.06Mg2Al2Si2O12Fluorescence ceramics piece, with a thickness of 1mm.It is denoted as sample C-3#.
Embodiment 4 prepares fluorescence ceramics block Lu1.94Ce0.06Mg2AlGaSi2O12
(1) Lu is stoichiometrically weighed2O3: 9.6499g, CeO2: 0.2582g, MgO:2.0152g, Al2O3: 1.2745g Ga2O3: 2.3430g, SiO2: 3.0042g;With grinding pot plus zirconia ball, carried out by abrasive media of dehydrated alcohol It grinds and mixes, until powder average grain diameter is less than 1 μm;
(2) gained slurry is dry and be sieved, by the 900 DEG C of heat preservation 2h in air of the powder after sieving, in removal powder Organic matter;Biscuit will be made using doctor-blade casting process after the sieving of gained powder, biscuit is with a thickness of 2mm;
(3) gained biscuit of ceramics is sintered in oxygen atmosphere, 1 DEG C/min of heating rate, in 1250 DEG C of heat preservation 4h, 1450 DEG C of heat preservation 10h complete solid phase reaction, exclude stomata and reach densification;
(4) sample after sintering is being contained into 5vol.%H2And 95vol.%N2Reducing atmosphere lower 1100 DEG C of heat preservations 5h, it is right Rare earth element is restored;
(5) the fluorescence ceramics block after step (4) annealing is processed by shot blasting, is obtained Lu1.94Ce0.06Mg2AlGaSi2O12Fluorescence ceramics piece, with a thickness of 1mm.It is denoted as sample C-4#.
Embodiment 5 prepares fluorescence ceramics block Lu1.7Ce0.3Mg2Al2SiGeO12
(1) Lu is stoichiometrically weighed2O3: 8.4561g, CeO2: 1.2909g, MgO:2.0152g, Al2O3: 2.5490g SiO2: 1.5021g, GeO2: 2.6160g;With grinding pot plus zirconia ball, carried out by abrasive media of dehydrated alcohol It grinds and mixes, until powder average grain diameter is less than 3 μm;
(2) gained slurry is dry and be sieved, by the 1200 DEG C of heat preservation 1h in air of the powder after sieving, in removal powder Organic matter;It will be formed in a mold in the way of injection molding after the sieving of gained powder, and carry out ungrease treatment, made pottery Porcelain biscuit;
(3) gained biscuit of ceramics is sintered, 1 DEG C/min of heating rate in hot isostatic pressing furnace, is kept the temperature at 1300 DEG C 1h completes solid phase reaction in 1500 DEG C of heat preservation 2h, excludes stomata and reaches densification;
(4) sample 1300 DEG C of heat preservation 2h annealing in oxygen after being sintered;
(5) the fluorescence ceramics block after step (4) annealing is processed by shot blasting, obtains Lu1.7Ce0.3Mg2Al2SiGeO12 Fluorescence ceramics piece, with a thickness of 1mm.It is denoted as sample C-5#.
Embodiment 6 prepares fluorescence ceramics block Lu0.94YCe0.05Dy0.01CaMgAl2Si2O12
(1) Lu is stoichiometrically weighed2O3: 4.6757g, Y2O3: 2.8226g, CeO2: 0.2151g, Dy2O3: 0.0466g, CaCO3: 2.5022g, MgO:1.0076g, Al2O3: 2.5490g, SiO2: 3.0042g;With grinding pot plus zirconium oxide Ball is ground and is mixed using dehydrated alcohol as abrasive media, until powder average grain diameter is less than 10 μm;
(2) gained slurry is dry and be sieved, by the 1000 DEG C of heat preservation 2h in air of the powder after sieving, in removal powder Organic matter and volatile substance;By gained powder using isometric unidirectional dry-pressing formed, biscuit is obtained;
(3) gained biscuit of ceramics is placed in graphite jig, is sintered in hot-pressed sintering furnace, 1 DEG C of heating rate/ Min completes solid phase reaction in 1450 DEG C of heat preservations 4h, pressure 40MPa, pressure maintaining 4h in 1250 DEG C of heat preservation 2h, excludes stomata and reach To densification;
(4) sample after sintering is annealed in oxygen, 900 DEG C of heat preservation 10h eliminate stress;
(5) the fluorescence ceramics block after step (4) annealing is processed by shot blasting, obtains Lu0.94YCe0.05Dy0.01CaMg Al2Si2O12Fluorescence ceramics piece, with a thickness of 1mm.It is denoted as sample C-6#.
7 morphology microstructure of embodiment characterization
Morphology characterization is carried out to the powder after ball milling in sample C-1#~C-6# preparation process respectively.
Test method: pattern test is carried out to the powder of sample C-1#~C-6# respectively using scanning electron microscope.
Test result: the average grain diameter of the powder of sample C-1#~C-6# is less than 10 microns.
Using the powder of sample C-5# as Typical Representative, Fig. 1 is the scanning electron microscope (SEM) photograph of the powder of sample C-5#, can be with by Fig. 1 Find out, the average grain diameter of powder is 2 microns, and diameter of particle is respectively less than 10 microns after gained calcining as can be seen from Figure 1, average Partial size is about 2 microns, which ensure that the high-compactness of gained fluorescence ceramics.
The excitation-emission spectrum test of 9 fluorescence ceramics block of embodiment
Test method: excitation-emission spectrum is carried out with the F4600 spectrometer of Hitachi, Ltd respectively to sample C-1#~C-6# Test tests emission spectrum by excitation wavelength of 455nm, is monitoring wavelength measurement excitation spectrum with 565nm.After tested, own The excitation spectrum of sample covers blue region, can effectively be excited by blue light, and emission spectrum is wide range transmitting, and range is 470nm to 800nm.
Using sample C-2# as Typical Representative, Fig. 2 is the excitation-emission spectrogram of sample C-2#, is excited as seen from Figure 2 Peak value is located at 450nm or so, can effectively be excited by blue light, and emission spectrum includes red spectral band abundant, and emission peak is located at 570nm or so can make low color temperature height colour developing illuminating device of the fluorescence ceramics.
The heat stability testing of 10 fluorescence ceramics block of embodiment
Test method: heat stability testing, specific method are carried out respectively to sample C-1#~C-6# are as follows: in Horiba public affairs The Fluorescence Spectrometer FL3-111 of department is warming up to 300 DEG C from 25 DEG C under 455nm excitation, emits light every 25 DEG C of test samples Spectrum.
Test result: sample C-1#~C-6# all has high thermal stability, and at 125 DEG C, luminous intensity is most strong, At 225 DEG C, luminous intensity begins lower than room temperature luminous intensity.
Using sample C-1# as Typical Representative, Fig. 3 is the thermostabilization curve of sample C-1#, as can be seen from Figure 3 sample C- 1# luminous intensity highest at 125 DEG C, at 225 DEG C, luminous intensity starts to be less than room temperature luminous intensity, and conventional fluorescent powder is usual At 150 DEG C, luminous intensity is generally below the 90% of room temperature luminous intensity, made compared with the thermal stability of conventional fluorescent powder The thermal stability of fluorescence ceramics, which has, significantly to be promoted.
The measuring mechanical property of 11 fluorescence ceramics block of embodiment
Test method: with the hardness of fluorescence ceramics after indentation method test polishing;
Test result: the fluorescence ceramics block has good mechanical performance;
Using sample C-2# as Typical Representative, after tested, hardness 12GPa.
Embodiment 12 prepares laser lighting device
The 455nm blue light laser diode of sample C-1# combination 20W is made into laser lighting device using transmission-type optical path, The corresponding laser lighting device of sample C-1# is denoted as sample L-C-1#.
The 455nm blue light laser diode of sample C-2# combination 8W is made into laser lighting device using transmission-type optical path, The corresponding laser lighting device of sample C-2# is denoted as sample L-C-2#.
The 455nm blue light laser diode of sample C-3# combination 5W is made into laser lighting device using transmission-type optical path, The corresponding laser lighting device of sample C-3# is denoted as sample L-C-3#.
The 455nm blue light laser diode of sample C-4# combination 10W is made into laser lighting device using transmission-type optical path, The corresponding laser lighting device of sample C-4# is denoted as sample L-C-4#.
The 455nm blue light laser diode of sample C-5# combination 8W is made into laser lighting device using transmission-type optical path, The corresponding laser lighting device of sample C-5# is denoted as sample L-C-5#.
The 455nm blue light laser diode of sample C-6# combination 2W is made into laser lighting device using transmission-type optical path, The corresponding laser lighting device of sample C-6# is denoted as sample L-C-6#.
The optical performance test of 13 illuminating device of embodiment
Test method: spectrum test, specific method are as follows: will illuminate are carried out to sample L-C-1#~sample L-C-6# respectively Device is placed in integrating sphere, tests its optical property using the Fluorescence Spectrometer FL3-111 of Horiba company, including light efficiency, aobvious Colour index, colour temperature etc..
Test result: optical property is as shown in table 1.The fluorescence ceramics of different component and indigo plant it can be seen from test result Ray laser assembly, obtains a series of illuminating devices haveing excellent performance, light efficiency is in 100lm/W or more, and colour rendering index is obvious Laser lighting device (colour rendering index is less than 70) higher than traditional YAG:Ce, the colour temperature of made illuminating device from 4500K to 6500K covers wider application range.
Using sample L-C-3# as Typical Representative, Fig. 4 is the device spectral figure of sample L-C-3#, as seen from Figure 4 the photograph The razor-edge and the wide range emission peak after fluorescence ceramics converting blue light that the spectrogram of funerary objects part includes blue laser.
Table 1
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to Case study on implementation is imitated, is belonged in technical proposal scope.

Claims (10)

1. a kind of fluorescence ceramics block, which is characterized in that at least one in the compound with chemical formula shown in formula I Kind,
A2-xQxM2L2D2O12Formula I
Wherein, A is selected from least one of Y element, Lu element, La element, Sc element, Gd element;
Eu element, Ce element, Pr element, Sm element, Dy element, Tm element, Tb element, Nd element of the Q in rare earth element At least one of;
M is selected from least one of Mg element, Ca element, Sr element, Ba element, Zn element;
L is selected from least one of Al element, Ga element;
D is selected from least one of Ti element, Si element, Ge element;
0.0001≤x≤0.3。
2. a kind of method for preparing fluorescence ceramics block described in claim 1, which is characterized in that include at least step:
(1) powder will be prepared into containing the source A, the source Q, the source M, the source L, the mixture in the source D and additive;
(2) powder calcined, formed, obtain biscuit of ceramics;
(3) biscuit of ceramics is sintered, obtains the fluorescence ceramics block.
3. according to the method described in claim 2, it is characterized in that, in the salt of oxide of the source A selected from A, A at least one Kind;
The source Q is selected from least one of the oxide of Q, salt of Q;
The source M is selected from least one of the oxide of M, salt of M;
The source L is selected from least one of the oxide of L, salt of L;
The source D is selected from least one of the oxide of D, salt of D;
The additive includes MgO, SiO2、ZrO2、B2O3At least one of.
4. according to the method described in claim 2, it is characterized in that, the partial size of the powder is less than 10 microns.
5. according to the method described in claim 2, it is characterized in that, calcination process in the step (2) are as follows: be warming up to 600 ~1200 DEG C, keep the temperature 1~10 hour;
The molding includes any one in dry-pressing formed, injection moulding, tape casting.
6. according to the method described in claim 2, it is characterized in that, sintering process in the step (3) are as follows: be warming up to sintering I: 1000~1300 DEG C of temperature, 1~24 hour is kept the temperature, later it is further heated up to II: 1400~1500 DEG C of sintering temperature, heat preservation 2~24 hours.
7. according to the method described in claim 2, it is characterized in that, being sintered in the step (3) to the biscuit of ceramics After further include annealing, polishing treatment.
8. the method according to the description of claim 7 is characterized in that annealing temperature be 900~1300 DEG C, soaking time be 2~ 20h;
Preferably, annealing atmosphere is air atmosphere, oxidizing atmosphere or reducing atmosphere.
9. a kind of laser lighting device, which is characterized in that by fluorescence ceramics block described in claim 1, claim 2 to 8 At least one of the fluorescence ceramics block that any one method is prepared assembles to obtain with blue light laser diode;
Preferably, the emission peak of the blue light laser diode is 440~480nm;
Preferably, the electrical power of the blue light laser diode is 1~20W;
Preferably, the fluorescence ceramics block with a thickness of 1mm.
10. application of the laser lighting device as claimed in claim 9 in illumination or display field.
CN201811516205.XA 2018-12-12 2018-12-12 A kind of fluorescence ceramics block, preparation method and its application in laser lighting Pending CN109437900A (en)

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Application publication date: 20190308