CN108503352A - A kind of garnet-base red fluorescence ceramic material and preparation method thereof - Google Patents
A kind of garnet-base red fluorescence ceramic material and preparation method thereof Download PDFInfo
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Abstract
A kind of garnet-base red fluorescence ceramic material of present invention offer and preparation method thereof, the chemical formula of the garnet-base red fluorescence ceramics is：RE3Al5‑x‑yMnxRyO12, wherein RE is at least one of Y, Lu, La, Ga, and one kind in R Mg, Ca, K, Li, 0.001≤x≤0.05,0≤y≤0.1, x is light emitting ionic Mn4+The molar fraction of doping.
Description
Technical field
The present invention relates to a kind of garnet-base red fluorescence ceramic materials and preparation method thereof, belong to luminescent material technology neck
Domain.
Background technology
High-power WLEDs and laser lighting technology have the advantages that high efficiency, high brightness, long lifespan, low energy consumption, environmental protection,
It is the research hotspot of current solid-state lighting display field.Commercialized WLEDs is by blue-light LED chip and YAG:The yellow fluorescence of Ce
Powder combines to obtain, technology of preparing maturation and lower cost, but fluorescent powder needs to use resin-encapsulated, and resin is easy to aging, heat
Conductance is low, seriously affects and is used for a long time performance, therefore the ceramic phosphor with higher heat-conductivity and without encapsulation comes into being,
The Y/LuAG of mainstream at present：Ce yellow green fluorescence ceramics have achieved some achievements.But it is mixed to get by blue light and yellow light
White light because lacking red color light component in spectrum, however it remains that colour temperature is higher, the relatively low problem of colour rendering index.It is red by being added
Fluorophor is to solve the problems, such as one of this effective ways, therefore we are ceramic there is an urgent need for preparing the red fluorescence of high efficient and reliable.Currently,
Report about red fluorescence ceramics is considerably less, mainly nitride etc. the non-oxide systems delivered, but these systems are glimmering
Light ceramic preparation condition is harsh, cost is higher.
Invention content
In view of the above-mentioned problems, the purpose of the present invention is to provide a kind of garnet-bases simple for process, at low cost, efficient
Red fluorescence ceramic material and preparation method thereof.
On the one hand, the present invention provides a kind of garnet-base red fluorescence ceramics, the garnet-base red fluorescence ceramics
Chemical formula be：RE3Al5-x-yMnxRyO12, wherein RE is at least one of Y, Lu, La, Ga, one in R Mg, Ca, K, Li
Kind, 0.001≤x≤0.05,0≤y≤0.1, x are light emitting ionic Mn4+The molar fraction of doping.
In the disclosure, garnet-base red fluorescence ceramics (RE3Al5-x-yMnxRyO12) in Mn elements be contain higher oxygen
Change state Mn4+, so that garnet-base red fluorescence ceramics can be sent out under the excitation of the ultraviolet or blue light of 230~500nm wavelength
The feux rouges of 600~750nm wave bands.Further, since its intact crystal property and stomata scattering process, to exciting light absorption
By force, luminous intensity is high, and quantum efficiency is high.
Preferably, 0.001≤x≤0.01 or/and 0.04≤y≤0.08.
Also, preferably, the consistency of the garnet-base red fluorescence ceramics be ＞ 75%, preferably greater than 97%.
In the disclosure, the stomata in garnet-base red fluorescence ceramics needs suitable amount, if stomata is too many, ceramic translucency is poor, hair
Light is weak.If stomata is very little, incident light is directed through, and light conversion efficiency is low, and consistency is preferably ＞ 97%.
Preferably, under ultraviolet light or blue light of the garnet-base red fluorescence ceramics within the scope of 230~500nm effectively
Inspire the feux rouges of 600~750nm wave bands.
On the other hand, the present invention also provides a kind of preparation method of garnet-base red fluorescence ceramics as described above,
Including：
According to stoichiometric ratio RE3Al5-x-yMnxRyO12The sources RE, the sources Al, the sources Mn, the sources R are weighed, is mixed, obtains mixed powder
Body；
It after gained mixed powder compression moulding, is placed in oxidizing atmosphere, is sintered 2~15 hours, obtains at 1500~1700 DEG C
To garnet-base red fluorescence ceramics.
In the disclosure, according to stoichiometric ratio RE3Al5-x-yMnxRyO12The sources RE, the sources Al, the sources Mn, the sources R are weighed, is mixed
It closes, obtains mixed powder.Then (1500~1700 DEG C) certain time is sintered directly in oxidizing atmosphere, in the process the sources R
(oxide containing R or/and carbonate), which serves not only as valence state compensation, to be existed or sintering aid, which promote sintering process,
Fluorescence ceramics are made to obtain higher consistency.
Preferably, the sources RE are the oxide of RE, preferably Y2O3、Lu2O3、La2O3、Ga2O3At least one of；Institute
It is Al to state the sources Al2O3；The sources Mn are MnO, MnCO3、Mn2O3At least one of；The sources R be the oxide containing R or/and
Carbonate, preferably MgO, MgCO3、CaO、CaCO3、K2CO3、Li2CO3At least one of.
Preferably, the mode of the compression moulding includes dry-pressing formed or/and cold isostatic compaction, preferably first dry-pressing at
Cold isostatic compaction after type.
Also, preferably, the dry-pressing formed pressure is 10~15MPa, the dwell time is 0.5~5min, described cold etc.
The pressure of hydrostatic profile is 180~200MPa, and the dwell time is 1~10min.
Preferably, the oxidizing atmosphere is air atmosphere or oxygen atmosphere.
Advantageous effect：
In the disclosure, garnet-base red fluorescence ceramics have higher consistency, and due to intact crystal property and gas
Hole scattering process, strong to excitation light absorption, luminous intensity is high, and quantum efficiency is high；
In the disclosure, garnet-base red fluorescence ceramics dissipate light by it using its internal remaining stomata as scattering center
The effect of penetrating enhances the absorption to exciting light, improves luminous intensity, obtains higher quantum efficiency, in 250~500nm models
Under ultraviolet light or the blue light excitation enclosed, emitting bright feux rouges；
In the disclosure, garnet-base red fluorescence ceramics are because be garnet system, therefore be easy to and the Y of mainstream (Lu) AG：Ce
Yellow-green fluorescence ceramics be packaged, difference is small, and permanent stability is good；
In the disclosure, garnet-base red fluorescence ceramics are combined with garnet-base yellow green fluorescence ceramics can generate white light, energy
Colour temperature is effectively reduced, colour rendering index is improved；
In the disclosure, garnet-base red fluorescence ceramics have high luminous efficiency, can be applied to WLEDs, laser lighting is shown
Other illumination fields such as show；
In the disclosure, fine and close garnet-base red fluorescence ceramics are made using high temperature solid state reaction one-step method, it is simple for process, at
This is low, suitable for mass production；
In the disclosure, use isostatic cool pressing in forming method, suitable sintering aid content (y be preferably 0.04≤y≤
0.08), higher sintering temperature (>=1600 DEG C) can obtain the garnet-base red fluorescence ceramics of higher-density.
Description of the drawings
Fig. 1 is the XRD spectrum of garnet-base red fluorescence ceramics prepared by 6-9 of the embodiment of the present invention；
Fig. 2 is the SEM spectrum of garnet-base red fluorescence ceramic (x=0.003) prepared by the embodiment of the present invention 8；
Fig. 3 is the excitation spectrum of garnet-base red fluorescence ceramics prepared by 6-9 of the embodiment of the present invention；
Fig. 4 is transmitting of the garnet-base red fluorescence ceramic (x=0.003) of the preparation of the embodiment of the present invention 8 under 460nm excitations
Spectrum；
Fig. 5 is the quantum efficiency of garnet-base red fluorescence ceramic (x=0.003) prepared by the embodiment of the present invention 8；
Fig. 6 is the pictorial diagram of garnet-base red fluorescence ceramics prepared by 6-9 of the embodiment of the present invention.
Specific implementation mode
It is further illustrated the present invention below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
In the disclosure, the chemical formula of garnet-base red fluorescence ceramics can be：RE3Al5-x-yMnxRyO12, wherein RE are
Y, at least one of Lu, La, Ga, one kind in R Mg, Ca, K, Li, 0.001≤x≤0.05 (preferably 0.001≤x≤
0.01), 0≤y≤0.1 (preferably 0.04≤y≤0.08), x are light emitting ionic Mn4+The molar fraction of doping, y be R ions (such as
Mg2+) doping molar fraction.Garnet-base red fluorescence ceramics can by within the scope of 230~500nm ultraviolet light and blue light have
Effect excitation, launches the bright feux rouges of 600~750nm wave bands.In addition, by adjusting x values, different excitations can be prepared
The red fluorescence ceramics of wave band.
The garnet-base red fluorescence ceramics (Mn of the present invention4+The garnet-base red fluorescence ceramics of doping) preparation process letter
It is single, it is at low cost, it can not only solve the problems, such as that fluorescent powder encapsulates, more due to its intact crystal property and stomata scattering process
And has higher quantum efficiency so that it can preferably be applied to illumination display field.In one embodiment of the disclosure, stone
Garnet base red fluorescence ceramics can be directly made by high temperature solid state reaction one-step method.Illustrate that garnet-base is red to following exemplary
The preparation method of color fluorescence ceramics.
According to stoichiometric ratio RE3Al5-x-yMnxRyO12The sources RE, the sources Al, the sources Mn, the sources R are weighed, is mixed, is mixed
Powder.In alternative embodiments, the sources RE can be the oxide (RE of RE2O3), such as Y2O3、Lu2O3、La2O3、Ga2O3Deng.
In alternative embodiments, the sources Al can be Al2O3Deng.In alternative embodiments, the sources Mn can be MnO, MnCO3、Mn2O3
Deng.In alternative embodiments, the sources R can be oxide or/and carbonate containing R, such as MgO, MgCO3、CaO、CaCO3、
K2CO3、Li2CO3Deng, can provide make valence state compensation cation, while as sintering aid exist.As an example, it presses
According to RE3Al5-x-yMnxRyO12(0.001≤x≤0.05,0 y≤0.1 ＜) stoichiometric ratio weighs RE2O3Powder, Al2O3Powder,
MnO powders, the oxide powder containing R, are mixed, are ground up, sieved, obtain mixed powder.Above-mentioned all raw materials (sources RE, Al
Source, the sources Mn, the sources R) purity be not less than 99.5%.
By mixed powder compression moulding, biscuit is obtained.Wherein, the mode of compression moulding includes dry-pressing formed or/and cold etc.
Hydrostatic profile, preferably first dry-pressing formed rear cold isostatic compaction.In alternative embodiments, dry-pressing formed pressure can be
10~15Mpa, dwell time are 0.5~5min.In alternative embodiments, the pressure of the cold isostatic compaction can be
180~200MPa, dwell time are 1~10min.
Biscuit is placed in oxidizing atmosphere, 2~15 hours (preferably 3~15 hours) are sintered at 1500~1700 DEG C, are obtained
To garnet-base red fluorescence ceramics.Wherein, oxidizing atmosphere can be oxygen atmosphere or air atmosphere.Then by garnet-base red
Fluorescence ceramics carry out plane lapping polishing treatment to suitable thickness.
The example of preparation method as the garnet-base red fluorescence ceramics described in one, including it is as follows：
(1) according to RE3Al5-x-yMnxMgyO12The stoichiometric ratio of (0.001≤x≤0.01,0≤y≤0.1) weighs RE2O3Powder
Body, Al2O3Powder, MgO powders, the sources Mn powder, are mixed, are ground up, sieved, while wherein MgO powders are sintering aid also
The Mg for making valence state compensation is provided2+；(2) mixture is dry-pressing formed and carry out isostatic cool pressing processing；(3) by biscuit in Muffle furnace
High temperature sintering is carried out, red fluorescence ceramics are obtained.RE in step (1)2O3Powder is Y2O3、Lu2O3、La2O3、Ga2O3In extremely
Few one kind, the sources Mn powder are MnO, MnCO3、Mn2O3In one kind.The purity of all material powders is not less than 99.5%.Step
(3) high temperature solid phase reaction need to carry out under oxidizing atmosphere, the direct sintering preferably in air atmosphere, sintering temperature be 1550~
1700 DEG C, soaking time is 3~15 hours.
In the disclosure, garnet-base red fluorescence ceramics ceramic crystalline grain development it is more complete, crystal property is good, defect compared with
Few, luminescent properties can higher.Moreover, there are still some stomatas in garnet-base red fluorescence ceramics, due to the scattering of stomata
Effect increases extraction of the ceramic body to the absorption of incident light and to emitting light, is beneficial to improve quantum efficiency.
Embodiment is enumerated further below so that the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.
Its chemical formula of prepared garnet-base red fluorescence ceramics is in following embodiments：Lu3Al5-x- yMnxMgyO12, 0.001≤x≤0.01,0≤y≤0.1.What follows any embodiment is handled in accordance with the following steps：According to change
Metering ratio is learned, Lu is accurately weighed with four figures balance2O3、Al2O3、MgO、MnCO3It is mixed to be added to ball milling in ball grinder for material powder
Expect 12h, dry in an oven to be then sieved for 24 hours with 200 mesh screens, obtained powder is pressed into punching block under 12MPa pressure
The disk of diameter 20mm, progress isostatic cool pressing handles to obtain biscuit at 200MPa；Biscuit is placed in alumina crucible, in height
It is sintered in warm Muffle furnace；By the ceramic twin grinding of gained to 0.2mm thickness.
Embodiment 1
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.001.Sintering temperature is 1600 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 97.85%, under the excitation of ultraviolet or blue light
Emit feux rouges.
Embodiment 2
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.002.Sintering temperature is 1600 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 97.88%, under the excitation of ultraviolet or blue light
Emit feux rouges.
Embodiment 3
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.003.Sintering temperature is 1600 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 97.86%, under the excitation of ultraviolet or blue light
Emit feux rouges, emits feux rouges under the excitation of ultraviolet or blue light.
Embodiment 4
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.005.Sintering temperature is 1600 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 97.74%, under the excitation of ultraviolet or blue light
Emit feux rouges.
Embodiment 5
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.008.Sintering temperature is 1600 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 97.87%, under the excitation of ultraviolet or blue light
Emit feux rouges.
Embodiment 6
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.001.Sintering temperature is 1650 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 98.95%, under the excitation of ultraviolet or blue light
Emit feux rouges.
Embodiment 7
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.002.Sintering temperature is 1650 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 99.29%, under the excitation of ultraviolet or blue light
Emit feux rouges.
Embodiment 8
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.003.Sintering temperature is 1650 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 99.19%, under the excitation of ultraviolet or blue light
Emit feux rouges.
Embodiment 9
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.005.Sintering temperature is 1650 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 98.65%, under the excitation of ultraviolet or blue light
Emit feux rouges.
It is shown in Figure 1, the XRD spectrum of garnet-base red fluorescence ceramics prepared by embodiment 6-9, with standard card pair
Than being Lu3Al5O12Phase shows Mn ion dopings on matrix structure without influence；
SEM figures in Fig. 2 show that the crystallinity of garnet-base red fluorescence ceramics prepared by embodiment 8 is good, and there are a small amount of gas
Hole and the second phase measure its consistency through Archimedes method and reach 99.19%；
As shown in figure 3, the garnet-base red fluorescence ceramics that are prepared of embodiment 6-9 within the scope of 230~500nm there are two
Stronger excitation peak, and with the increase of Mn contents, there is the phenomenon that apparent broadening in the excitation peak of ultra-violet (UV) band；
Fig. 4 shows the garnet-base red fluorescence ceramics prepared by embodiment 8 under 460nm excitations, electromagnetic radiation 600~
The feux rouges of 750nm wave bands；
Fig. 5 is the light that ceramic (x=0.003) integrated ball of garnet-base red fluorescence that embodiment 8 is prepared is tested
Spectrum, is computed its quantum efficiency (QE) and is up to 47.8%；
Fig. 6 is the pictorial diagram for the garnet-base red fluorescence ceramics that embodiment 6-9 is prepared, and sample can be indistinctly seen from figure
Writing below product illustrates that sample has certain translucency.Sample launches bright feux rouges under 365nm ultra violet lamps.
Embodiment 10
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.001.Sintering temperature is 1700 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Sample manufactured in the present embodiment, primary structure pattern, excitation spectrum and transmitting light
Spectrum is similar to embodiment 6~9.
Embodiment 11
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.002.Sintering temperature is 1700 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Sample manufactured in the present embodiment, primary structure pattern, excitation spectrum and transmitting light
Spectrum is similar to embodiment 6~9.
Embodiment 12
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.003.Sintering temperature is 1700 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Sample manufactured in the present embodiment, primary structure pattern, excitation spectrum and transmitting light
Spectrum is similar to embodiment 6~9.
Embodiment 13
The content of fixed Mg, chemical formula Lu3Al5-x-0.04MnxMg0.04O12, wherein x=0.005.Sintering temperature is 1700 DEG C,
Time is 5 hours, and atmosphere is air atmosphere.Sample manufactured in the present embodiment, primary structure pattern, excitation spectrum and transmitting light
Spectrum is similar to embodiment 6~9.
Embodiment 14
The content of fixed light emitting ionic Mn, chemical formula Lu3Al5-0.003-yMn0.003MgyO12, wherein y=0.Sintering temperature is fixed
It it is 1650 DEG C, the time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 78.47%.
Embodiment 15
The content of fixed light emitting ionic Mn, chemical formula Lu3Al5-0.003-yMn0.003MgyO12, wherein y=0.02.Sintering temperature is solid
It is set to 1650 DEG C, the time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 88.36%.
Embodiment 16
The content of fixed light emitting ionic Mn, chemical formula Lu3Al5-0.003-yMn0.003MgyO12, wherein y=0.06.Sintering temperature is solid
It is set to 1650 DEG C, the time is 5 hours, and atmosphere is air atmosphere.Its obtained ceramic body relative density is 98.58%.
Embodiment 17
The content of fixed light emitting ionic Mn, chemical formula Lu3Al5-0.003-yMn0.003MgyO12, wherein y=0.08.Sintering temperature is solid
It is set to 1650 DEG C, the time is 5 hours, and atmosphere is air atmosphere.Obtained ceramic body relative density is 98.87%.
Sample prepared by embodiment 14-17, primary structure pattern, excitation spectrum and emission spectrum and 6~9 phase of embodiment
Seemingly.Wherein, sample obtained by embodiment 15-17 and no doping Mg in embodiment 142+Sample compare, adulterate Mg2+Sample cause
Density and luminous efficiency significantly improve.
Table 1 is the composition and performance parameter of garnet-base red fluorescence ceramics prepared by 1-17 of the embodiment of the present invention：
Claims (9)
1. a kind of garnet-base red fluorescence ceramics, which is characterized in that the chemical formula of the garnet-base red fluorescence ceramics is：
RE3Al5-x-yMnxRyO12, wherein RE is at least one of Y, Lu, La, Ga, one kind in R Mg, Ca, K, Li, 0.001≤x
≤ 0.05,0≤y≤0.1, x are light emitting ionic Mn4+The molar fraction of doping.
2. garnet-base red fluorescence according to claim 1 ceramics, which is characterized in that 0.001≤x≤0.01 or/and
0.04≤y≤0.08。
3. garnet-base red fluorescence ceramics according to claim 1 or 2, which is characterized in that the garnet-base is red
The consistency of fluorescence ceramics is more than 75%, preferably greater than 97%.
4. garnet-base red fluorescence ceramics according to any one of claim 1-3, which is characterized in that the garnet
Base red fluorescence ceramics effectively inspire the red of 600~750nm wave bands under the ultraviolet light or blue light within the scope of 230~500nm
Light.
5. a kind of preparation method of garnet-base red fluorescence ceramics as described in any one of claim 1-4, feature exist
In, including：
According to stoichiometric ratio RE3Al5-x-yMnxRyO12The sources RE, the sources Al, the sources Mn, the sources R are weighed, is mixed, obtains mixed powder；
It after gained mixed powder compression moulding, is placed in oxidizing atmosphere, is sintered 2~15 hours, obtains at 1500~1700 DEG C
To garnet-base red fluorescence ceramics.
6. preparation method according to claim 5, which is characterized in that the sources RE are the oxide of RE, preferably Y2O3、
Lu2O3、La2O3、Ga2O3At least one of；The sources Al are Al2O3；The sources Mn are MnO, MnCO3、Mn2O3In at least one
Kind；The sources R are oxide or/and carbonate containing R, preferably MgO, MgCO3、CaO、CaCO3、K2CO3、Li2CO3In
It is at least one.
7. preparation method according to claim 5 or 6, which is characterized in that the mode of the compression moulding include dry-pressing at
Type or/and cold isostatic compaction, preferably first dry-pressing formed rear cold isostatic compaction.
8. preparation method according to claim 7, which is characterized in that the dry-pressing formed pressure is 10~15Mpa, is protected
It is 0.5~5 minute to press the time；The pressure of the cold isostatic compaction is 180~200MPa, and the dwell time is 1~10 minute.
9. according to the preparation method described in any one of claim 5-8, which is characterized in that the oxidizing atmosphere is air atmosphere
Or oxygen atmosphere.
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