CN104830338A - Preparation method of spherical YAG (yttrium aluminum garnet):Ce - Google Patents
Preparation method of spherical YAG (yttrium aluminum garnet):Ce Download PDFInfo
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- CN104830338A CN104830338A CN201510249803.5A CN201510249803A CN104830338A CN 104830338 A CN104830338 A CN 104830338A CN 201510249803 A CN201510249803 A CN 201510249803A CN 104830338 A CN104830338 A CN 104830338A
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Abstract
The invention relates to the field of preparation of YAG (yttrium aluminum garnet), particularly a preparation method of spherical YAG:Ce. The preparation method comprises the following steps: S1) dissolving aluminum nitrate, yttrium nitrate and cerium nitrate in an anhydrous ethanol solvent according to the stoichiometric proportion to form a mixed solution A; S2) adding triethylenetetramine into the mixed solution A, and stirring at room temperature for 6-10 hours to form a precursor; S3) dispersing the obtained precursor in a triethylenetetramine solvent to form a mixed solution B; and S4) transferring the mixed solution B into a hydrothermal reaction kettle, reacting under the solvothermal condition of 250 DEG C, and cooling to room temperature to obtain the spherical YAG:Ce. Compared with the existing synthesis technique, the method prepares the uniform-shape spherical YAG:Ce by a simple solvothermal synthesis process, and has the characteristics of no need of high-temperature roasting, high yield and favorable repetitiveness. The obtained material has the advantages of high luminescent intensity and high luminescence efficiency when being used as fluorescent powder.
Description
Technical field
The present invention relates to the preparation field of YAG, particularly the preparation method of a kind of spherical YAG:Ce.
Background technology
Rare-earth cerium ion doped yttrium aluminum garnet (YAG) is that one is rich in long history and widely used luminescent material.In recent years, because of its application in the white light emitting diode (LED), people are made to have rekindled high interest to this material.YAG belongs to carbuncle type isometric system, and its lattice parameter is 12.002.Its structural formula can be written as: L
3b
2(AO
4)
3, wherein L, A, B represent three kinds of cases respectively.Eight Y are had in unit cell
3al
5o
12molecule, comprises 24 ruthenium ions altogether, 40 aluminum ions, 96 oxonium ions.Wherein, each ruthenium ion is in the dodecahedral L case by 8 oxonium ion coordinations, and 16 aluminum ions are in by octahedral B case of 6 oxonium ion coordinations, and other 24 aluminum ions are on the tetrahedral A case by 4 oxonium ion coordinations.Octahedral aluminum ion becomes body-centered cubic structure, and tetrahedral aluminum ion and dodecahedral ruthenium ion are in cubical bisector, and octahedral and tetrahedral is all distortion.
1991, the people such as Inoue adopted BDO to do reaction solvent 300
oin the closed reactor of C, isothermal reaction obtains the YAG of pure phase, and this method is referred to as alcoholysis method again.Subsequently, the people such as Isobe also report and utilize BDO to prepare the nanocrystal of about 10nm as reaction solvent, and adopt polyoxyethylene glycol to modify to strengthen its luminescent properties to its surface.By the inspiration of the research of Isobe, the people such as Nyman also adopt similar synthetic route 225
o4 ~ 14 days preparation YAG:Ce nanocrystals are reacted under C.But the YAG:Ce how synthesizing specific morphology remains one of difficult problem of the prior art.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of a kind of spherical YAG:Ce.
A preparation method of spherical YAG:Ce, comprises the following steps:
S1) according to stoichiometric ratio aluminum nitrate, Yttrium trinitrate and cerous nitrate be dissolved in anhydrous ethanol solvent and form mixed liquor A;
S2) in mixed liquor A, add triethylene tetramine, then at room temperature stir 6 ~ 10h and form precursor;
S3) precursor of gained is scattered in triethylene tetramine solvent forms mixed liquid B;
S4) then described mixed liquid B is proceeded in hydrothermal reaction kettle and react at solvent thermal 250 DEG C, be down to room temperature with 2 DEG C/h ~ 5 DEG C/h after reaction and obtain described spherical YAG:Ce.
Further, in the triethylene tetramine added in described S2 step and S1 step, the volume ratio of dehydrated alcohol is 0.5 ~ 4:15.
Further, the compactedness that the triethylene tetramine added in described S3 step accounts for hydrothermal reaction kettle is 25% ~ 75%.
Further, the described solvent thermal reaction time is 8 ~ 120 hours.
The present invention has following beneficial effect:
Compared with existing synthetic technology, the present invention has following outstanding feature: the present invention adopts simple solvent-thermal process method, prepare the spherical YAG:Ce that pattern is homogeneous, this method is without the need to high-temperature roasting, productive rate is high, reproducible, when the material obtained uses as fluorescent material, the luminous intensity of this sample is large, and luminous efficiency is high.
Accompanying drawing explanation
Fig. 1 is the XRD diffractogram of spherical YAG:Ce of the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of spherical YAG:Ce of the present invention.
Fig. 3 is the fluorescence spectrum figure of spherical YAG:Ce of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be described in detail.Embodiment is only the preferred embodiment of the present invention, is not limitation of the invention.
embodiment 1
By Y
3-xal
5o
12: Ce
x(x=0.02). stoichiometric ratio, accurately take aluminum nitrate (Al (NO with electronic analytical balance
3)
39H
2o, 99%), Yttrium trinitrate (Y (NO
3)
36H
2o, 99.99%), cerous nitrate (Ce (NO
3)
36H
2o, 99%), wherein Al (NO
3)
39H
2o 0.9379g.Above-mentioned nitrate is dissolved in 15 mL dehydrated alcohols and forms mixed liquor A; Then add 4 mL triethylene tetramines in mixed liquor A, at room temperature stir 8h and form precursor; Then first for this presoma decompress filter is rinsed three times to remove remaining foreign ion with dehydrated alcohol, then it puts into reactor by gained presoma, add compactedness be 25% triethylene tetramine (being 10 mL in the present embodiment) do reaction solvent; Reactor is positioned in constant temperature blast drying oven, 250
oisothermal reaction 72h under C, is down to room temperature with 3 DEG C/h after reaction, rinses three times and 80 by its first decompress filter and with dehydrated alcohol
obe incubated 12h in loft drier under C, required yellow YAG:Ce fluorescent material can be obtained.The XRD spectra of YAG:Ce fluorescent material as shown in Figure 1, in 2 θ=18.1
o, 27.6
o, 29.7
o, 33.3
o, 36.4
o, 41.0
o, 46.6
o, 55.1
oand 57.4
ounder diffraction peak completely the same with the standard P DF card (JCPDS card No.33-0040) of cube phase YAG.Material morphology is obtained by scanning electron microscope result, as shown in Figure 2, as figure can find out that material is uniform globosity.And the fluorescence spectrum figure of this YAG:Ce fluorescent material as shown in Figure 3, excitation wavelength is 455 nm, records the wide cutting edge of a knife or a sword that emmission spectrum is visible region, and the highest emission peak positions is at 525nm, and corresponding color is yellow-green colour.
embodiment 2
By Y
3-xal
5o
12: Ce
x(x=0.08). stoichiometric ratio, accurately take aluminum nitrate (Al (NO with electronic analytical balance
3)
39H
2o, 99%), Yttrium trinitrate (Y (NO
3)
36H
2o, 99.99%), cerous nitrate (Ce (NO
3)
36H
2o, 99%), wherein Al (NO
3)
39H
2o 0.9379g.Above-mentioned nitrate is dissolved in 15 mL dehydrated alcohols and forms mixed liquor A; Then add 0.5 mL triethylene tetramine in mixed liquor A, at room temperature stir 6h and form precursor; Then first for this presoma decompress filter is rinsed three times to remove remaining foreign ion with dehydrated alcohol, then it puts into reactor by gained presoma, add compactedness be 50% triethylene tetramine (being 20 mL in the present embodiment) do reaction solvent; Reactor is positioned in constant temperature blast drying oven, 250
oisothermal reaction 24h under C, is down to room temperature with 2 DEG C/h after reaction, rinses three times and 80 by its first decompress filter and with dehydrated alcohol
obe incubated 12h in loft drier under C, required yellow YAG:Ce fluorescent material can be obtained.Products therefrom is X-ray powder diffraction, scanning electron microscope and fluorescence spectrum figure (collection of illustrative plates prepared with embodiment 1 is similar) after characterizing.
embodiment 3
By Y
3-xal
5o
12: Ce
x(x=0.04). stoichiometric ratio, accurately take aluminum nitrate (Al (NO with electronic analytical balance
3)
39H
2o, 99%), Yttrium trinitrate (Y (NO
3)
36H
2o, 99.99%), cerous nitrate (Ce (NO
3)
36H
2o, 99%), wherein Al (NO
3)
39H
2o 0.9379g.Above-mentioned nitrate is dissolved in 15 mL dehydrated alcohols and forms mixed liquor A; Then add 1 mL triethylene tetramine in mixed liquor A, at room temperature stir 10h and form precursor; Then first for this presoma decompress filter is rinsed three times to remove remaining foreign ion with dehydrated alcohol, then it puts into reactor by gained presoma, add compactedness be 4% triethylene tetramine (being 12.5 mL in the present embodiment) do reaction solvent; Reactor is positioned in constant temperature blast drying oven, 250
oisothermal reaction 120h under C, is down to room temperature with 5 DEG C/h after reaction, rinses three times and 80 by its first decompress filter and with dehydrated alcohol
obe incubated 12h in loft drier under C, required yellow YAG:Ce fluorescent material can be obtained.Products therefrom is X-ray powder diffraction, scanning electron microscope and fluorescence spectrum figure (collection of illustrative plates prepared with embodiment 1 is similar) after characterizing.
embodiment 4
By Y
3-xal
5o
12: Ce
x(x=0.06). stoichiometric ratio, accurately take aluminum nitrate (Al (NO with electronic analytical balance
3)
39H
2o, 99%), Yttrium trinitrate (Y (NO
3)
36H
2o, 99.99%), cerous nitrate (Ce (NO
3)
36H
2o, 99%), wherein Al (NO
3)
39H
2o 0.9379g.Above-mentioned nitrate is dissolved in 15 mL dehydrated alcohols and forms mixed liquor A; Then add 2 mL triethylene tetramines in mixed liquor A, at room temperature stir 8h and form precursor; Then first for this presoma decompress filter is rinsed three times to remove remaining foreign ion with dehydrated alcohol, then it puts into reactor by gained presoma, add compactedness be 4% triethylene tetramine (being 12.5 mL in the present embodiment) do reaction solvent; Reactor is positioned in constant temperature blast drying oven, 250
oisothermal reaction 120h under C, is down to room temperature with 4 DEG C/h after reaction, rinses three times and 80 by its first decompress filter and with dehydrated alcohol
obe incubated 12h in loft drier under C, required yellow YAG:Ce fluorescent material can be obtained.Products therefrom is X-ray powder diffraction, scanning electron microscope and fluorescence spectrum figure (collection of illustrative plates prepared with embodiment 1 is similar) after characterizing.
The above embodiment only have expressed embodiments of the present invention; it describes comparatively concrete and detailed; but therefore can not be interpreted as the restriction to the scope of the claims of the present invention; in every case the technical scheme adopting the form of equivalent replacement or equivalent transformation to obtain, all should drop within protection scope of the present invention.
Claims (4)
1. a preparation method of spherical YAG:Ce, is characterized in that, comprises the following steps:
S1) according to stoichiometric ratio aluminum nitrate, Yttrium trinitrate and cerous nitrate be dissolved in anhydrous ethanol solvent and form mixed liquor A;
S2) in mixed liquor A, add triethylene tetramine, then at room temperature stir 6 ~ 10h and form precursor;
S3) precursor of gained is scattered in triethylene tetramine solvent forms mixed liquid B;
S4) then described mixed liquid B is proceeded in hydrothermal reaction kettle and react at solvent thermal 250 DEG C, be down to room temperature with 2 DEG C/h ~ 5 DEG C/h after reaction and obtain described spherical YAG:Ce.
2. the preparation method of a kind of spherical YAG:Ce according to claim 1, is characterized in that: in the triethylene tetramine added in described S2 step and S1 step, the volume ratio of dehydrated alcohol is 0.5 ~ 4:15.
3. the preparation method of a kind of spherical YAG:Ce according to claim 1, is characterized in that: the compactedness that the triethylene tetramine added in described S3 step accounts for hydrothermal reaction kettle is 25% ~ 75%.
4. the preparation method of a kind of spherical YAG:Ce according to claim 1, is characterized in that: the described solvent thermal reaction time is 8 ~ 120 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161889A (en) * | 2011-02-24 | 2011-08-24 | 中国计量学院 | Yttrium aluminum garnet (YAG) nano fluorescent powder and preparation method thereof |
| CN102181291A (en) * | 2011-03-23 | 2011-09-14 | 山东轻工业学院 | Method for preparing cerium doped yttrium aluminum garnet fluorescent powder |
-
2015
- 2015-05-18 CN CN201510249803.5A patent/CN104830338A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161889A (en) * | 2011-02-24 | 2011-08-24 | 中国计量学院 | Yttrium aluminum garnet (YAG) nano fluorescent powder and preparation method thereof |
| CN102181291A (en) * | 2011-03-23 | 2011-09-14 | 山东轻工业学院 | Method for preparing cerium doped yttrium aluminum garnet fluorescent powder |
Non-Patent Citations (1)
| Title |
|---|
| 王立开: "白光LED用YAG：Ce黄色荧光粉的湿化学法制备及其性能研究", 《中国优秀硕士学位论文全文数据库》 * |
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Application publication date: 20150812 |