CN108148592A - One kind has phase separation structure rare earth eutectic fluorescent material and its preparation method and application - Google Patents
One kind has phase separation structure rare earth eutectic fluorescent material and its preparation method and application Download PDFInfo
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- 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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7774—Aluminates
Abstract
The present invention relates to one kind to have phase separation structure rare earth eutectic fluorescent material and its preparation method and application, and the chemical formula of the rare earth eutectic fluorescent material is RE3‑xCexAl5‑yGayO12/Al2O3, wherein, RE is one or more of Rare Earth Y, Gd, Lu, and the value range of x is 0.0005 ＜ x ＜ 0.08, and the value range of y is 0 ＜ y ＜ 5；The preparation method of the rare earth eutectic fluorescent material is as follows：S1：It weighs aluminium oxide, gallium oxide, cerium oxide and rare earth oxide and is uniformly mixed, be then placed in high temperature furnace the calcination under reducing atmosphere, pre-burning raw material is crushed to obtain after cooling；S2：Pre-burning raw material is put into bottom to open in foraminate Iridium Crucible, Iridium Crucible is placed in micro- drop-down crystal growing furnace, makes melting sources by Medium frequency induction heating；S3：With mounted seed crystal contact Iridium Crucible bottom in advance, by micro- drop-down seed crystal directional solidification melt growth eutectic, cooling down is up to the fluorescent material after having grown.Rare earth eutectic fluorescent material provided by the invention in the detection and laser display of high-energy ray to that can significantly improve imaging resolution, available for high-energy ray detection imaging and technical field of laser display.
Description
Technical field
The present invention relates to rare earth luminescent material fields, and in particular, to one kind has phase separation structure rare earth eutectic fluorescence
Material and its preparation method and application.
Background technology
Rare earth garnet type fluorescent material due to the special crystal structure of garnet and unique photochemical properties, makes
It becomes a kind of very important phosphor.The matrix of carbuncle type fluorescent material is mainly Y3Al5O12(YAG) and
Lu3Al5O12(LuAG), this is because in rare earth ion, Y3+And La3+4f electronic shell in without electronics, Gd3+And Lu3+4f it is sub-
The electronics of layer is respectively half state for being full of and being full of entirely, and all has closed shell, they have optics inertia, are suitable for
Make host material.Due to La3+And Gd3+Garnet structure there is thermal instability, therefore generally use YAG and LuAG conduct
Matrix.The rare earth garnet type fluorescent material of developmental research at present, since form existing for different preparation methods has powder respectively
Body, film, ceramics, monocrystalline etc..
Rare earth garnet type powder fluorescent material is mainly used in light emitting diode（LED）, commercialization preferably sending out
Coating can be stimulated by blue light out the fluorescent powder of yellow light on the InGaN/GaN chips of blue light（Use YAG more：Ce3+Fluorescent powder）With glue
The mixture of body, so as to match white light.Because it is uneven, scattered that dotting glue method is unfavorable for the heat dissipation of LED chip, the white light matched
It is more serious to penetrate phenomenon.Therefore thin-film material is subsequently developed, there is high light-emitting uniformity, thermostabilization compared with powder body material
Property and array package and the heat dissipation for being conducive to LED chip.Pass through the R and D to material, rare earth garnet type ceramics
With single crystal fluorescent material relative to gluey mixed fluorescent powder YAG:Ce has higher fusing point（Up to 1950 DEG C）It is dissipated with higher
Hot coefficient, therefore it is more suitable for the light excitation of high power density zonule area；Rare earth garnet type ceramics and monocrystalline are glimmering simultaneously
Luminescent material has the characteristics that high density, small, physical and chemical performance and scintillation properties are excellent, in nuclear medicine, nuclear physics and high energy object
The fields such as reason, environmental monitoring, safety random check, oil well exploration are widely used.But ceramics are internal generally to have a large amount of gas
The non-uniform microstructure such as hole, crystal boundary and impurity can cause strong scattering and refraction effect to light；It is primarily present in monocrystalline
The defects of core, growth striation, wrappage, dislocation, reduces the scintillation properties of crystal.
Less to the research of rare earth garnet type eutectic fluorescent material at present, therefore, necessary research and development are a kind of to have phase
The rare earth eutectic fluorescent material of separated structure.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide one kind to have phase separation structure rare earth eutectic fluorescence
Material.
Rare earth eutectic fluorescent material RE provided by the invention3-xCexAl5-y GayO12/Al2O3Rare earth eutectic fluorescent material is
The trivalent rare earth cerium ion being prepared by the growth of micro- glass tube down-drawing（Ce3+）Garnet crystal form aluminate/aluminium oxide of activation is common
Crystalline substance, under high-energy ray or laser irradiation, the RE in eutectic fluorescent material3-xCexAl5-y GayO12Crystalline phase sends out visible fluorescence,
Al2O3Crystalline phase does not fluoresce, and each fluorescent emission unit is mutually isolated, avoids scattering of the fluorescence signal in material internal,
To imaging resolution can be significantly improved in the detection and laser display of high-energy ray, available for high-energy ray detection imaging and laser
Display technology field.
Another object of the present invention is to provide it is above-mentioned have phase separation structure rare earth eutectic fluorescent material in high-energy ray
Application in detection imaging field or technical field of laser display.
To achieve the above object, the present invention adopts the following technical scheme that：
One kind has phase separation structure rare earth eutectic fluorescent material, and the chemical formula of the rare earth eutectic fluorescent material is RE3- xCexAl5-yGayO12/Al2O3, wherein, RE is Rare Earth Y, one or more of Gd, Lu, Ce3+For rare-earth luminescent center, Ga originals
Son substitution Al atoms, the value range of x is 0.0005 ＜ x ＜ 0.08, and the value range of y is 0 ＜ y ＜ 5；The rare earth eutectic is glimmering
The preparation method of luminescent material is as follows：
S1：It weighs aluminium oxide, gallium oxide, cerium oxide and rare earth oxide and is uniformly mixed, be then placed in high temperature furnace in reduction
Calcination under atmosphere crushes to obtain pre-burning raw material after cooling；
S2：Pre-burning raw material is put into bottom to open in foraminate Iridium Crucible, Iridium Crucible is placed in micro- drop-down crystal growing furnace
In, melting sources are made by Medium frequency induction heating；
S3：With mounted seed crystal contact Iridium Crucible bottom in advance, seed crystal directional solidification melt growth eutectic is pulled down by micro-,
Cooling down is up to the fluorescent material after having grown；
Wherein, the micro- drop-down growth rate of eutectic is 0.1~8 mm/min；The rare earth oxide for yttrium oxide, gadolinium oxide or
One or more of luteium oxide.
The present invention is by selecting micro- glass tube down-drawing to grow the trivalent rare earth cerium ion being prepared（Ce3+）The garnet of activation is brilliant
Type aluminate/aluminium oxide eutectic, expression formula RE3-xCexAl5-y GayO12/Al2O3Eutectic contains stratiform in the fluorescent material
Two kinds of crystalline phases being orderly distributed, and both crystalline phases have different refractive index.Under high-energy ray irradiation, RE3-xCexAl5-y
GayO12/Al2O3In RE3-xCexAl5-y GayO12Crystalline phase absorbs high-energy ray, sends out yellow fluorescence, and passed inside this crystalline phase
It broadcasts, reduces the scattering of fluorescence in the material, so as to improve the imaging resolution detected to high-energy ray and laser display intensity.
Preferably, the value range of the x is 0.005 ＜ x ＜ 0.06, and the value range of the y is 0 ＜ y ＜ 1.
Preferably, the x is 0.03, and the RE is rare earth lutetium.
Preferably, the micro- drop-down growth rate of eutectic is 0.3~5 mm/min.
Preferably, the micro- drop-down growth rate of eutectic is 1.5 mm/mins.
Preferably, the gas of the reducing atmosphere is CO, H2、N2Or one or more of Ar.
Preferably, the % of the purity of the aluminium oxide, gallium oxide cerium oxide and rare earth oxide >=99.995.
What deserves to be explained is above-mentioned rare earth eutectic fluorescent material is in high-energy ray detection imaging field and laser display technology
Application in field is also within protection scope of the present invention.
Compared with prior art, the present invention has the advantages that：
Containing two crystalline phases that refractive index is different in rare earth eutectic fluorescent material provided by the invention with phase separation structure, and
Orderly layered arrangement is presented, garnet crystalline phase is the phase that shines, and phase is isolated for fluorescence in alumina crystalline phase.Under high-energy ray irradiation,
RE3-xCexAl5-y GayO12Crystalline phase generates yellow fluorescence and is propagated in this phase, reduces fluorescence dissipating in scintillator material
It penetrates, can significantly improve to the imaging resolution of high-energy ray detectable signal and laser display intensity.The present invention selects micro- drop-down life
Regular way prepares fluorescent material, CCD observation Material growth processes can be selected, and using raw material is few, the speed of growth is fast, noble metal earthenware
Crucible is small, fibre diameter from micron to millimeter it is adjustable the advantages that.
Description of the drawings
Lu is prepared for embodiment 12 in Fig. 10.99Ce0.01Al5O12/Al2O3The EDS energy spectrum diagrams of eutectic sample；
Lu is prepared for embodiment 12 in Fig. 20.99Ce0.01Al5O12/Al2O3Fluorescence lifetime spectrum of the eutectic sample under different casting
Figure；
Lu is prepared for embodiment 12 in Fig. 30.99Ce0.01Al5O12/Al2O3Cross section SEM of the eutectic sample under different casting
Figure；
Lu is prepared for embodiment 12 in Fig. 40.99Ce0.01Al5O12/Al2O3Eutectic sample longitudinal section SEM under different casting schemes；
Lu is prepared for embodiment 12 in Fig. 50.99Ce0.01Al5O12/Al2O3Fluorescence emission spectrum of the eutectic sample under different casting
Figure.
Specific embodiment
Further illustrated the present invention below in conjunction with specific embodiments and the drawings, but embodiment the present invention is not done it is any
The restriction of form.Unless stated otherwise, the reagent of the invention used, method and apparatus is the art conventional reagent, methods
And equipment.
Unless stated otherwise, agents useful for same and material of the present invention are purchased in market.
1 Y of embodiment0.9995Ce0.0005Al4GaO12/Al2O3Rare earth eutectic fluorescent material
A kind of rare earth eutectic fluorescent material with phase separation structure, the chemical expression of the fluorescent material are
Y0.9995Ce0.0005Al4GaO12/Al2O3, the preparation method of the fluorescent material is as follows：
（1）Weigh raw material yttrium oxide（Y2O3）2.1103g, cerium oxide（CeO2）0.0008g, aluminium oxide（Al2O3）3.3158g, oxygen
Change gallium（Ga2O3）1.5239g adds raw materials into absolute ethyl alcohol as dispersant, and oxidation is put into after being fully ground in agate mortar
Crucible is put into box Muffle furnace by aluminium crucible, and with 4 DEG C/min heating rates in 1400 DEG C, 10 are sintered in CO reducing atmospheres
After sample is cooled to room temperature, eutectic powder pre-burning raw material is obtained after being ground to powdery by h；
（2）Pre-burning raw material is put into the foraminate Iridium Crucible in bottom, Iridium Crucible is placed in micro- drop-down crystal growing furnace,
Stove is installed, leads to inert gas, intermediate frequency power supply, Iridium Crucible sensing heating heating, by pre-burning melting sources are controlled through program；
（3）Under CCD observations, advance mounted seed crystal is slowly risen from bottom, touching Iridium Crucible bottom is drawn molten
Body, by adjusting the EF power of crystal growing furnace, after the meniscus stability of melt, with the drop-down rate of 0.1 mm/min
Eutectic is grown, after having grown, cooling obtains Y0.9995Ce0.0005Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
2 Y of embodiment0.995Ce0.005Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）2.1008g, cerium oxide（CeO2）0.0080g, aluminium oxide（Al2O3）3.3158g, oxidation
Gallium（Ga2O3）1.5239g by method same as Example 1, is obtained with the drop-down rate of 0.1 mm/min
Y0.995Ce0.005Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
3 Y of embodiment0.99Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）2.0902g, cerium oxide（CeO2）0.0161g, aluminium oxide（Al2O3）3.3158g, oxidation
Gallium（Ga2O3）1.5239g by method same as Example 1, is obtained with the drop-down rate of 0.5 mm/min
Y0.99Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
4 Y of embodiment0.97Ce0.03Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）2.0480g, cerium oxide（CeO2）0.0483g, aluminium oxide（Al2O3）3.3158g, oxidation
Gallium（Ga2O3）1.5239g by method same as Example 1, is obtained with the drop-down rate of 0.5 mm/min
Y0.97Ce0.03Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
5 Y of embodiment0.94Ce0.06Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）1.9846g, cerium oxide（CeO2）0.0966g, aluminium oxide（Al2O3）3.3158g, oxidation
Gallium（Ga2O3）1.5239g by method same as Example 1, is obtained with the drop-down rate of 1.0 mm/mins
Y0.94Ce0.06Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
6 Y of embodiment0.92Ce0.08Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）1.9424g, cerium oxide（CeO2）0.1287g, aluminium oxide（Al2O3）3.3158g, oxidation
Gallium（Ga2O3）1.5239g by method same as Example 1, is obtained with the drop-down rate of 1.0 mm/mins
Y0.92Ce0.08Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
7 Y of embodiment0.99Ce0.01Al5O12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）2.0902g, cerium oxide（CeO2）0.0161g, aluminium oxide（Al2O3）4.1447g pass through
Method same as Example 1 obtains Y with the drop-down rate of 2.0 mm/mins0.99Ce0.01Al5O12/Al2O3Rare earth eutectic is glimmering
Luminescent material.
8 Y of embodiment0.99Ce0.01Al3Ga2O12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）2.0902g, cerium oxide（CeO2）0.0161g, aluminium oxide（Al2O3）2.4868g, oxidation
Gallium（Ga2O3）3.0478g by method same as Example 1, is obtained with the drop-down rate of 2.0 mm/mins
Y0.99Ce0.01Al3Ga2O12/Al2O3Rare earth eutectic fluorescent material.
9 Y of embodiment0.99Ce0.01Al2Ga3O12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）2.0902g, cerium oxide（CeO2）0.0161g, aluminium oxide（Al2O3）1.6579g, oxidation
Gallium（Ga2O3）4.5718g by method same as Example 1, is obtained with the drop-down rate of 3.0 mm/mins
Y0.99Ce0.01Al2Ga3O12/Al2O3Rare earth eutectic fluorescent material.
10 Y of embodiment0.99Ce0.01AlGa4O12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）2.0902g, cerium oxide（CeO2）0.0161g, aluminium oxide（Al2O3）0.8289g, oxidation
Gallium（Ga2O3）6.0957g by method same as Example 1, is obtained with the drop-down rate of 3.0 mm/mins
Y0.99Ce0.01AlGa4O12/Al2O3Rare earth eutectic fluorescent material.
11 Y of embodiment0.99Ce0.01Ga5O12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）2.0902g, cerium oxide（CeO2）0.0161g, gallium oxide（Ga2O3）7.6196g pass through
Method same as Example 1 obtains Y with the drop-down rate of 4.0 mm/mins0.99Ce0.01Ga5O12/Al2O3Rare earth eutectic is glimmering
Luminescent material.
12 Lu of embodiment0.99Ce0.01Al5O12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material luteium oxide（Lu2O3）3.6835g, cerium oxide（CeO2）0.0161g, aluminium oxide（Al2O3）4.1447g pass through
Method same as Example 1 obtains Lu with the drop-down rate of 2.0 mm/mins0.99Ce0.01Al5O12/Al2O3Rare earth eutectic
Fluorescent material.
13 Lu of embodiment0.99Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material luteium oxide（Lu2O3）3.6835g, cerium oxide（CeO2）0.0161g, aluminium oxide（Al2O3）3.3158g, oxidation
Gallium（Ga2O3）1.5239g by method same as Example 1, is obtained with the drop-down rate of 4.0 mm/mins
Lu0.99Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
14 Y of embodiment0.89Lu0.1Ce0.01Al5O12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）1.8791g, luteium oxide（Lu2O3）0.3721g, cerium oxide（CeO2）0.0161g, oxidation
Aluminium（Al2O3）4.1447g by method same as Example 1, is obtained with the drop-down rate of 5.0 mm/mins
Y0.89Lu0.1Ce0.01Al5O12/Al2O3Rare earth eutectic fluorescent material.
15 Y of embodiment0.89Lu0.1Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）1.8791g, luteium oxide（Lu2O3）0.3721g, cerium oxide（CeO2）0.0161g, oxidation
Aluminium（Al2O3）3.3158g, gallium oxide（Ga2O3）1.5239g, by method same as Example 1, with 5.0 mm/mins
Drop-down rate obtains Lu0.99Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
16 Y of embodiment0.89Gd0.1Ce0.01Al5O12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）1.8791g, gadolinium oxide（Gd2O3）0.3389g, cerium oxide（CeO2）0.0161g, oxidation
Aluminium（Al2O3）4.1447g by method same as Example 1, is obtained with the drop-down rate of 6.0 mm/mins
Y0.89Gd0.1Ce0.01Al5O12/Al2O3Rare earth eutectic fluorescent material.
17 Y of embodiment0.89Gd0.1Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）1.8791g, gadolinium oxide（Gd2O3）0.3389g, cerium oxide（CeO2）0.0161g, oxidation
Aluminium（Al2O3）3.3158g, gallium oxide（Ga2O3）1.5239g, by method same as Example 1, with 6.0 mm/mins
Drop-down rate obtains Y0.89Gd0.1Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
18 Lu of embodiment0.89Gd0.1Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material luteium oxide（Lu2O3）3.3114g, gadolinium oxide（Gd2O3）0.3389g, cerium oxide（CeO2）0.0161g, oxidation
Aluminium（Al2O3）4.1447g by method same as Example 1, is obtained with the drop-down rate of 7.0 mm/mins
Lu0.89Gd0.1Ce0.01Al5O12/Al2O3Rare earth eutectic fluorescent material.
19 Lu of embodiment0.89Gd0.1Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material luteium oxide（Lu2O3）3.3114g, gadolinium oxide（Gd2O3）0.3389g, cerium oxide（CeO2）0.0161g, oxidation
Aluminium（Al2O3）3.3158g, gallium oxide（Ga2O3）1.5239g, by method same as Example 1, with 7.0 mm/mins
Drop-down rate obtains Lu0.89Gd0.1Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
20 Y of embodiment0.79Lu0.1Gd0.1Ce0.01Al5O12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）1.6679g, luteium oxide（Lu2O3）0.3721g, gadolinium oxide（Gd2O3）0.3389g, oxidation
Cerium（CeO2）0.0161g, aluminium oxide（Al2O3）4.1447g, by method same as Example 1, with 8.0 mm/mins
Drop-down rate obtains Y0.79Gd0.1Lu0.1Ce0.01Al5O12/Al2O3Rare earth eutectic fluorescent material.
21 Y of embodiment0.79Lu0.1Gd0.1Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material
Weigh raw material yttrium oxide（Y2O3）1.6679g, luteium oxide（Lu2O3）0.3721g, gadolinium oxide（Gd2O3）0.3389g, oxidation
Cerium（CeO2）0.0161g, aluminium oxide（Al2O3）3.3158g, gallium oxide（Ga2O3）1.5239g passes through side same as Example 1
Method obtains Y with the drop-down rate of 8.0 mm/mins0.79Gd0.1Lu0.1Ce0.01Al4GaO12/Al2O3Rare earth eutectic fluorescent material.
Lu is prepared for embodiment 12 in Fig. 10.99Ce0.01Al5O12/Al2O3The EDS energy spectrum diagrams of eutectic sample are shown in collection of illustrative plates
It is Lu to show white area0.99Ce0.01Al5O12Crystalline phase, black region Al2O3Crystalline phase, it is two-phase eutectic to illustrate gained sample；
Lu is prepared for embodiment 12 in Fig. 20.99Ce0.01Al5O12/Al2O3Fluorescence lifetime spectrum of the eutectic sample under different casting
Scheme, the life curve under each pulling rate coincide substantially, and influence of the pulling rate to the service life is smaller；
Lu is prepared for embodiment 12 in Fig. 30.99Ce0.01Al5O12/Al2O3Cross section SEM of the eutectic sample under different casting
Figure；
Lu is prepared for embodiment 12 in Fig. 40.99Ce0.01Al5O12/Al2O3Eutectic sample longitudinal section SEM under different casting schemes,
With reference to Fig. 3, the distribution of eutectic two-phase layered；
Lu is prepared for embodiment 12 in Fig. 50.99Ce0.01Al5O12/Al2O3Fluorescence emission spectrum of the eutectic sample under different casting
Scheme, luminous intensity is different under different casting, and under certain pulling rate, structure is more uniform, and luminous intensity is higher.
Above-described specific embodiment has carried out the purpose of the present invention, technical solution and advantageous effect further
It is described in detail, it should be understood that the foregoing is merely the specific embodiment of the present invention, is not intended to limit the present invention
Protection domain, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (8)
1. one kind has phase separation structure rare earth eutectic fluorescent material, which is characterized in that the change of the rare earth eutectic fluorescent material
Formula is RE3-xCexAl5-yGayO12/Al2O3, wherein, RE is one or more of Rare Earth Y, Gd, Lu, and the value range of x is
The value range of 0.0005 ＜ x ＜ 0.08, y are 0 ＜ y ＜ 5；The preparation method of the rare earth eutectic fluorescent material is as follows：
S1：It weighs aluminium oxide, gallium oxide, cerium oxide and rare earth oxide and is uniformly mixed, be then placed in high temperature furnace in reduction
Calcination under atmosphere crushes to obtain pre-burning raw material after cooling；
S2：Pre-burning raw material is put into bottom to open in foraminate Iridium Crucible, Iridium Crucible is placed in micro- drop-down crystal growing furnace
In, melting sources are made by Medium frequency induction heating；
S3：With mounted seed crystal contact Iridium Crucible bottom in advance, seed crystal directional solidification melt growth eutectic is pulled down by micro-,
Cooling down is up to the fluorescent material after having grown；
Wherein, the micro- drop-down growth rate of eutectic is 0.1~8 mm/min；The rare earth oxide for yttrium oxide, gadolinium oxide or
One or more of luteium oxide.
2. there is phase separation structure rare earth eutectic fluorescent material according to claim 1, which is characterized in that the value of the x
The value range of ranging from 0.005 ＜ x ＜ 0.06, the y are 0 ＜ y ＜ 1.
3. there is phase separation structure rare earth eutectic fluorescent material according to claim 1, which is characterized in that the x is 0.03,
The RE is rare earth lutetium.
4. there is phase separation structure rare earth eutectic fluorescent material according to claim 1, which is characterized in that the micro- drop-down life of eutectic
Long rate is 0.3~5 mm/min.
5. there is phase separation structure rare earth eutectic fluorescent material according to claim 4, which is characterized in that the micro- drop-down life of eutectic
Long rate is 1.5 mm/mins.
6. there is phase separation structure rare earth eutectic fluorescent material according to claim 1, which is characterized in that the reducing atmosphere
Gas be CO, H2、N2Or one or more of Ar.
7. there is phase separation structure rare earth eutectic fluorescent material according to claim 1, which is characterized in that the aluminium oxide,
The % of the purity of gallium oxide cerium oxide and rare earth oxide >=99.995.
Described in 8. claim 1~7 is any there is phase separation structure rare earth eutectic fluorescent material to be led in high-energy ray detection imaging
Application in domain or technical field of laser display.
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| CN110331443A (en) * | 2019-07-09 | 2019-10-15 | 同济大学 | A kind of rare earth ion doped germanate eutectic material and preparation method thereof |
| CN110331444A (en) * | 2019-07-09 | 2019-10-15 | 同济大学 | A kind of rare earth ion doped silicate eutectic material and preparation method thereof |
| CN110983433A (en) * | 2019-11-28 | 2020-04-10 | 中国科学院包头稀土研发中心 | Process for producing rare earth eutectic fluorophor by guide mode method |
| CN111235629A (en) * | 2020-03-09 | 2020-06-05 | 西北工业大学深圳研究院 | Preparation method of alumina-YAG eutectic melt growth composite material |
| CN111423128A (en) * | 2020-05-11 | 2020-07-17 | 奕瑞新材料科技（太仓）有限公司 | GGAG fluorescent glass ball and preparation method thereof |
| CN112552038A (en) * | 2020-11-13 | 2021-03-26 | 浙江大学 | Green fluorescent composite ceramic and preparation method and application thereof |
| CN115142130A (en) * | 2022-06-30 | 2022-10-04 | 同济大学 | Method and device for growing flaky gallium oxide crystal by micro pull-down zone melting method |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110331443A (en) * | 2019-07-09 | 2019-10-15 | 同济大学 | A kind of rare earth ion doped germanate eutectic material and preparation method thereof |
| CN110331444A (en) * | 2019-07-09 | 2019-10-15 | 同济大学 | A kind of rare earth ion doped silicate eutectic material and preparation method thereof |
| CN110331443B (en) * | 2019-07-09 | 2021-09-03 | 同济大学 | Rare earth ion doped germanate eutectic material and preparation method thereof |
| CN110983433A (en) * | 2019-11-28 | 2020-04-10 | 中国科学院包头稀土研发中心 | Process for producing rare earth eutectic fluorophor by guide mode method |
| CN111235629A (en) * | 2020-03-09 | 2020-06-05 | 西北工业大学深圳研究院 | Preparation method of alumina-YAG eutectic melt growth composite material |
| CN111423128A (en) * | 2020-05-11 | 2020-07-17 | 奕瑞新材料科技（太仓）有限公司 | GGAG fluorescent glass ball and preparation method thereof |
| CN112552038A (en) * | 2020-11-13 | 2021-03-26 | 浙江大学 | Green fluorescent composite ceramic and preparation method and application thereof |
| CN115142130A (en) * | 2022-06-30 | 2022-10-04 | 同济大学 | Method and device for growing flaky gallium oxide crystal by micro pull-down zone melting method |
| CN115142130B (en) * | 2022-06-30 | 2024-02-27 | 同济大学 | Method and device for growing flaky gallium oxide crystals by micro-pull-down zone melting method |
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Application publication date: 20180612 |