CN110156036A - A kind of monoclinic crystal RE3BO6The preparation method of spheric granules - Google Patents
A kind of monoclinic crystal RE3BO6The preparation method of spheric granules Download PDFInfo
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- CN110156036A CN110156036A CN201910460056.8A CN201910460056A CN110156036A CN 110156036 A CN110156036 A CN 110156036A CN 201910460056 A CN201910460056 A CN 201910460056A CN 110156036 A CN110156036 A CN 110156036A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/127—Borates of heavy metals
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7712—Borates
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/774—Borates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Abstract
The invention belongs to materials science fields, are related to a kind of monoclinic crystal RE3BO6The preparation method of spheric granules the steps include: that H is added in beaker3BO3And urea (CO (NH2)2) powder, RE (NO is stirring evenly and then adding under room temperature3)3Solution and ethylene glycol (EG), wherein RE is one of Eu-Yb or Y element；It is stirred evenly after constant volume；Clear solution is kept the temperature in heating water bath, after reaction, precipitated product is centrifugated after suspension natural cooling, is cleaned, obtain amorphous precursor body powder after dry.Amorphous precursor body obtained is calcined under oxygen atmosphere, obtains final RE3BO6Spheric granules.The present invention prepares RE by homogeneous precipitation method3BO6, monodispersed borate spheric granules is obtained by control boric acid and urea content and rare earth ion concentration, improves product fluorescence property, and realize the spheroidization engineering of Eu-Yb and Y for the first time.
Description
Technical field
The invention belongs to materials science fields, and in particular to a kind of monoclinic crystal RE3BO6The preparation method of spheric granules.
Background technique
Luminescent material is by the compound (matrix) as body of material and to select a small amount of down to micro impurity of incorporation
Ion-activated dose is formed.Rare earth borate luminescent material has that synthesis temperature is low, chemical stability is good, the spies such as many kinds of
Therefore point is considered as luminous host of great practical value, and be widely used in FPD, illumination, medical radioactive figure
As etc..Micro-nano spherical fluorescent grain of uniform size is easy to line up fine and close fluorescence coating, to reduce to the maximum extent
To the scattering of exciting light to be presented optimal luminescent efficiency, thus monodisperse spherical particle is prepared into fluorescent material pattern control
Make the hot spot of research.
There are particle size distribution unevenness, reaction products to be easy agglomeration for the RE borate prepared by traditional handicraft solid phase method
And pattern it is irregular the disadvantages of, it is difficult to monodispersed spheric granules is prepared, to influence product fluorescence property.Homogeneous precipitation method can
Accurately to control content, purity, granular size, grain size, dispersibility and the phase composition of each component, reach controllable preparation boric acid
Salt spheric granules.
Summary of the invention
The present invention provides a kind of monoclinic crystal RE3BO6The preparation method of spheric granules, before preparing amorphous using homogeneous precipitation method
Drive body, thermally treated acquisition monoclinic crystal RE3BO6Spheric granules, wherein RE is one of Eu-Yb or Y element, wherein Eu-Yb
Including Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, the spheroidization engineering of Eu-Yb and Y is realized.
Technical solution of the present invention:
A kind of monoclinic crystal RE3BO6Spheric granules the preparation method is as follows:
Step 1: by H3BO3And urea powder, it is scattered in deionized water, is stirred evenly under room temperature, mixed solution A is made；
Step 2: by RE (NO3)3It is added with ethylene glycol in the mixed solution A that step 1 obtains, stirs evenly, obtain under room temperature
The molar concentration of rare earth ion is 0.001~0.01mol/L in mixed solution B, mixed solution B, and the molar concentration of borate is
0.01~0.3mol/L, the molar concentration of carbanion are 0.015~0.45mol/L, ethylene glycol volume fraction is 3%~
The pH of 10%, mixed solution B are 3~6；Wherein, RE is one of Eu-Yb or Y element；
Step 3: the mixed solution B that step 2 obtains being heated to 85~95 DEG C under water bath, micro- indigo plant occurs from solution
Start timing, to suspension natural cooling, precipitated product is centrifugated after reaction, cleans, is transferred to 60 by 2~3h of heat preservation
It is completely dried in DEG C thermostatic drying chamber below, obtains amorphous precursor body powder；
Step 4: by amorphous precursor body powder made from step 3 under oxygen atmosphere, with the rate of heat addition of 8~12 DEG C/min
In 600~1100 DEG C of 2~4h of calcining, final monoclinic crystal RE is obtained3BO6Spheric granules.
Further, above-mentioned steps 2, the molar concentration of rare earth ion is 0.004~0.008mol/L in mixed solution B.
Further, above-mentioned steps 2, it is 4%~6% that the volume fraction of ethylene glycol, which is concentration, in mixed solution B.
Further, above-mentioned steps 2, pH is 4~5 in mixed solution B.
Further, the bath temperature in above-mentioned steps 3 is 90~95 DEG C.
Further, the calcination temperature in above-mentioned steps 4 is 900~1000 DEG C.
Beneficial effects of the present invention:
Homogeneous precipitation method prepares RE3BO6, list is obtained by control boric acid and urea content and rare earth ion concentration
The borate spheric granules of dispersion, and the spheroidization engineering of Eu-Yb and Y is realized for the first time.
Detailed description of the invention
Fig. 1 is the FE-SEM figure of presoma product prepared by the embodiment of the present invention 1；
Fig. 2 is the XRD spectrum of presoma product prepared by the embodiment of the present invention 1；
Fig. 3 is the FE-SEM figure that the embodiment of the present invention 1 prepares final products；
Fig. 4 is the XRD spectrum of final products prepared by the embodiment of the present invention 1；
Fig. 5 is the FE-SEM figure of presoma product prepared by the embodiment of the present invention 2；
Fig. 6 is the XRD spectrum of presoma product prepared by the embodiment of the present invention 2；
Fig. 7 is the FE-SEM figure that the embodiment of the present invention 2 prepares final products；
Fig. 8 is the XRD spectrum of final products prepared by the embodiment of the present invention 2；
Fig. 9 is the FE-SEM figure of presoma product prepared by the embodiment of the present invention 3；
Figure 10 is the XRD spectrum of presoma product prepared by the embodiment of the present invention 3；
Figure 11 is the FE-SEM figure that the embodiment of the present invention 3 prepares final products；
Figure 12 is the XRD spectrum of final products prepared by the embodiment of the present invention 3；
Figure 13 is the FE-SEM figure of presoma product prepared by the embodiment of the present invention 4；
Figure 14 is the XRD spectrum of presoma product prepared by the embodiment of the present invention 4；
Figure 15 is the FE-SEM figure that the embodiment of the present invention 4 prepares final products；
Figure 16 is the XRD spectrum of final products prepared by the embodiment of the present invention 4；
Figure 17 is the FE-SEM figure of presoma product prepared by the embodiment of the present invention 5；
Figure 18 is the XRD spectrum of presoma product prepared by the embodiment of the present invention 5；
Figure 19 is the FE-SEM figure that the embodiment of the present invention 5 prepares final products；
Figure 20 is the XRD spectrum of final products prepared by the embodiment of the present invention 5.
Specific embodiment
Specific embodiments of the present invention are described in detail below in conjunction with technical solution and attached drawing.
Boric acid employed in present example is excellent pure grade grade product, remaining chemical reagent is the pure grade product of analysis.
Embodiment 1 (RE=Eu)
By excellent pure grade H3BO3And urea (CO (NH2)2) powder, it is scattered in deionized water, is stirred evenly under room temperature.By Eu
(NO3)3Solution and ethylene glycol are added in above-mentioned solution, and deionized water is added by solution constant volume, stir evenly, mix under room temperature
In solution, Eu3+The molar concentration of ion is 0.001mol/L, and the molar concentration of borate is 0.01mol/L, carbanion
Molar concentration is 0.015mol/L, and ethylene glycol volume fraction is 3%, and final pH is maintained at 3.Clear solution after homogenization is existed
85 DEG C are heated under water bath, timing there is micro- basket since solution keeps the temperature 3h, after reaction, naturally cold to suspension
But, precipitated product is centrifugated, cleans, is transferred in 60 DEG C of thermostatic drying chambers below and is completely dried, obtain amorphous precursor body
Powder.Presoma obtained is transferred in alumina crucible, using temperature programming resistance batch-type furnace under oxygen atmosphere, with 8
DEG C/rate of heat addition of min in 600 DEG C of calcining 4h, taken out after cooling, grind, obtain final Eu3BO6Spheric granules final product.
Embodiment 2 (RE=Ho)
By excellent pure grade H3BO3And (CO (NH2)2) powder, it is scattered in deionized water, is stirred evenly under room temperature.By Ho
(NO3)3Solution and ethylene glycol (EG) are added in above-mentioned solution, and deionized water is added by solution constant volume, stir evenly under room temperature,
In mixed solution, Ho3+The molar concentration of ion is 0.003mol/L, and the molar concentration of borate is 0.06mol/L, carbonate from
The molar concentration of son is 0.08mol/L, and ethylene glycol volume fraction is 5%, and final pH is maintained at 4.5.By the clarification after homogenization
Solution is heated to 90 DEG C under water bath, and timing there is micro- basket since solution keeps the temperature 2.5h, after reaction, to suspended
Liquid natural cooling, precipitated product is centrifugated, and cleaning is transferred in 60 DEG C of thermostatic drying chambers below and is completely dried, and is obtained non-
Brilliant precursor powder.Presoma obtained is transferred in alumina crucible, using temperature programming resistance batch-type furnace in oxygen gas
Under atmosphere, with the rate of heat addition of 10 DEG C/min in 800 DEG C of calcining 3h, is taken out after cooling, grind, obtain final Ho3BO6Spheric granules
Final product.
Embodiment 3 (RE=Yb)
By excellent pure grade H3BO3And (CO (NH2)2) powder, it is scattered in deionized water, is stirred evenly under room temperature.By Yb
(NO3)3Solution and ethylene glycol (EG) are added in above-mentioned solution, and deionized water is added by solution constant volume, stir evenly under room temperature,
In mixed solution, Yb3+The molar concentration of ion is 0.006mol/L, and the molar concentration of borate is 0.2mol/L, carbonate from
The molar concentration of son is 0.25mol/L, and ethylene glycol volume fraction is 6%, and final pH is maintained at 5.5.By the clarification after homogenization
For heat to 92 DEG C, timing there is micro- basket since solution keeps the temperature 2h, after reaction, certainly to suspension to solution under water bath
It is so cooling, precipitated product is centrifugated, is cleaned, is transferred in 60 DEG C of thermostatic drying chambers below and is completely dried, before obtaining amorphous
Drive body powder.Presoma obtained is transferred in alumina crucible, using temperature programming resistance batch-type furnace under oxygen atmosphere,
It with the rate of heat addition of 11 DEG C/min in 900 DEG C of calcining 2h, is taken out after cooling, grinds, obtain final Yb3BO6Spheric granules produces eventually
Object.
Embodiment 4 (RE=Y)
By excellent pure grade H3BO3And (CO (NH2)2) powder, it is scattered in deionized water, is stirred evenly under room temperature.By Y (NO3)3
Solution and ethylene glycol (EG) are added in above-mentioned solution, and deionized water is added by solution constant volume, stir evenly, mix molten under room temperature
In liquid, Y3+The molar concentration of ion is 0.01mol/L, and the molar concentration of borate is 0.3mol/L, mole of carbanion
Concentration is 0.45mol/L, and ethylene glycol volume fraction is 10%, and final pH is maintained at 6.By the clear solution after homogenization in water-bath
To 95 DEG C, timing there is micro- basket since solution, heat preservation 2h's heat to suspension natural cooling, will sink after reaction under environment
The centrifuge separation of shallow lake product, cleaning are transferred in 60 DEG C of thermostatic drying chambers below and are completely dried, and obtain amorphous precursor body powder.It will
Presoma obtained is transferred in alumina crucible, using temperature programming resistance batch-type furnace under oxygen atmosphere, with 12 DEG C/min
The rate of heat addition in 1100 DEG C of calcining 2h, taken out after cooling, grind, obtain final Y3BO6Spheric granules final product.
Embodiment 5 (RE=Er)
By excellent pure grade H3BO3And (CO (NH2)2) powder, it is scattered in deionized water, is stirred evenly under room temperature.By Er
(NO3)3Solution and ethylene glycol (EG) are added in above-mentioned solution, and deionized water is added by solution constant volume, stir evenly under room temperature,
In mixed solution, Er3+The molar concentration of ion is 0.005mol/L, and the molar concentration of borate is 0.07mol/L, carbonate from
The molar concentration of son is 0.2mol/L, and ethylene glycol volume fraction is 5%, and final pH is maintained at 4.5.Clarification after homogenization is molten
Heat is to 92 DEG C under water bath for liquid, and timing there is micro- basket since solution keeps the temperature 2h, after reaction, to suspension nature
It is cooling, precipitated product is centrifugated, is cleaned, is transferred in 60 DEG C of thermostatic drying chambers below and is completely dried, amorphous precursor is obtained
Body powder.Presoma obtained is transferred in alumina crucible, using temperature programming resistance batch-type furnace under oxygen atmosphere, with
The rate of heat addition of 10 DEG C/min is taken out after cooling in 950 DEG C of calcining 2h, grinds, obtains final Er3BO6Spheric granules final product.
Claims (6)
1. a kind of monoclinic crystal RE3BO6The preparation method of spheric granules, which comprises the steps of:
Step 1: by H3BO3And urea powder, it is scattered in deionized water, is stirred evenly under room temperature, mixed solution A is made；
Step 2: by RE (NO3)3It is added with ethylene glycol in the mixed solution A that step 1 obtains, stirs evenly, mixed under room temperature
Solution B, the molar concentration of rare earth ion is 0.001~0.01mol/L in mixed solution B, and the molar concentration of borate is 0.01
~0.3mol/L, the molar concentration of carbanion are 0.015~0.45mol/L, and ethylene glycol volume fraction is 3%~10%,
The pH of mixed solution B is 3~6；Wherein, RE is one of Eu-Yb or Y element；
Step 3: the mixed solution B that step 2 obtains being heated to 85~95 DEG C under water bath, since micro- basket occurs in solution
Timing, heat preservation 2~3h to suspension natural cooling, precipitated product is centrifugated after reaction, clean, be transferred to 60 DEG C with
Under thermostatic drying chamber in be completely dried, obtain amorphous precursor body powder；
Step 4: by amorphous precursor body powder made from step 3 under oxygen atmosphere, with the rate of heat addition of 8~12 DEG C/min in
600~1100 DEG C of 2~4h of calcining, obtain final monoclinic crystal RE3BO6Spheric granules.
2. monoclinic crystal RE according to claim 13BO6The preparation method of spheric granules, which is characterized in that step 2, mixing
The molar concentration of rare earth ion is 0.004~0.008mol/L in solution B.
3. monoclinic crystal RE according to claim 13BO6The preparation method of spheric granules, which is characterized in that step 2, mixing
It is 4%~6% that the volume fraction of ethylene glycol, which is concentration, in solution B.
4. monoclinic crystal RE according to claim 13BO6The preparation method of spheric granules, which is characterized in that step 2, mixing
PH is 4~5 in solution B.
5. monoclinic crystal RE according to claim 13BO6The preparation method of spheric granules, which is characterized in that the water in step 3
Bath temperature is 90~95 DEG C.
6. monoclinic crystal RE according to claim 13BO6The preparation method of spheric granules, which is characterized in that forging in step 4
Burning temperature is 900~1000 DEG C.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1633718A (en) * | 2001-09-03 | 2005-06-29 | 松下电器产业株式会社 | Semiconductor light-emitting device, light-emitting apparatus and manufacturing method of semiconductor light-emitting device |
| WO2005073146A1 (en) * | 2004-01-30 | 2005-08-11 | Murata Manufacturing Co., Ltd. | Composition for ceramic substrate, ceramic substrate, process for producing ceramic substrate and glass composition |
| CN101215469A (en) * | 2008-01-10 | 2008-07-09 | 同济大学 | Method for preparing fluorescent powder used for plasma display |
| WO2010018418A1 (en) * | 2008-08-12 | 2010-02-18 | Novatech D.O.O. | Formulation based on micronized clinoptilolite as therapeutic agent providing highly bioavailable silicon |
| CN108384544A (en) * | 2018-01-05 | 2018-08-10 | 东北大学 | A kind of tetragonal YPO4:Ln3+Spherical fluorescent grain and preparation method |
-
2019
- 2019-05-30 CN CN201910460056.8A patent/CN110156036B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1633718A (en) * | 2001-09-03 | 2005-06-29 | 松下电器产业株式会社 | Semiconductor light-emitting device, light-emitting apparatus and manufacturing method of semiconductor light-emitting device |
| WO2005073146A1 (en) * | 2004-01-30 | 2005-08-11 | Murata Manufacturing Co., Ltd. | Composition for ceramic substrate, ceramic substrate, process for producing ceramic substrate and glass composition |
| CN101215469A (en) * | 2008-01-10 | 2008-07-09 | 同济大学 | Method for preparing fluorescent powder used for plasma display |
| WO2010018418A1 (en) * | 2008-08-12 | 2010-02-18 | Novatech D.O.O. | Formulation based on micronized clinoptilolite as therapeutic agent providing highly bioavailable silicon |
| CN108384544A (en) * | 2018-01-05 | 2018-08-10 | 东北大学 | A kind of tetragonal YPO4:Ln3+Spherical fluorescent grain and preparation method |
Non-Patent Citations (1)
| Title |
|---|
| CHONG WANG等: "Sol–gel synthesis and photoluminescence of RE3BO6: Eu3+/Tb3+", 《JOURAL OF NON-CRYSTALLINE SOLIDS》 * |
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