CN104845615A - Rare-earth doped beta-phase Sr2SiO4 nano-powder and preparation method therefor - Google Patents
Rare-earth doped beta-phase Sr2SiO4 nano-powder and preparation method therefor Download PDFInfo
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Abstract
The present invention discloses a rare-earth doped beta-phase Sr2SiO4 nano-powder and a preparation method therefor. Nano-powder meets composition formula of rare-earth doped beta-phase Sr2SiO4 shown as follows: (Sr1-X RE X) 2SiO4, wherein RE represents one kind of rare earth elements, and 0.001<=X<=0.05. The rare-earth doped beta-phase Sr2SiO4 nano-powder prepared in the method has a high phase purity, phase detection shows a pure beta phase, no fluxing agents is needed, fused salt and other foreign matters can be washed with water, and the method is concise and efficient. The preparation method needs low synthesis temperature which is only at 750-800 DEG C, and is at least 500 DEG C lower than that of common solid phase method, the energy saving effect is significant, and requirements for equipments are greatly reduced. The rare-earth doped beta-phase Sr2SiO4 nano-powder prepared in the method has a small particle size which is only 40-80 nm.
Description
Technical field
The present invention relates to advanced powder synthesis technical field, relate to a kind of molten-salt growth method that adopts and prepare rare-earth doped beta phase Sr
2siO
4raw powder's production technology, relates to a kind of with the meso-hole structure SiO of high-ratio surface or rather
2powder is Si source, with NaCl-KCl mixture for molten salt system, with NaNO
3for catalysts, under low calcining temperature, prepare pure β phase Sr
2siO
4the method of nano-powder.
Background technology
White light LEDs has played a significant role at road and the field such as Landscape Lighting, flat pannel display with its energy-saving and environmental protection, the advantage such as efficient as a kind of novel green illumination device, and it replaces incandescent light becomes lighting source of future generation and progressively come true.At present, the scheme of white light is produced with the main flow that its technique is simple, efficiency high is still current application and research based on the conversion of fluorescent material light.Mostly current commercialization white light LEDs is to adopt blue chip collocation Y
3al
5o
12: Ce
3+(YAG:Ce
3+) yellow fluorescent powder (Japanese Scientists Shuji Nakamura obtains the Nobel prize in 2014 because having invented this fluorescent material); although the program shows high-luminous-efficiency and chemical stability; but its red sector is launched shortcoming and is caused device colour rendering index on the low side, and there is patent protection.Therefore, all kinds of novel fluorescent material system obtains extensive research.Wherein, the positive strontium silicate Sr that adulterates of rare earth (especially Eu, Dy etc.)
2siO
4material system obtains more concern.Silicate-base material has higher chemical stability and thermostability, also has stronger ultraviolet light resistant ability, and in potting resin, has stronger weather resistance, Eu
2+the M of doping
2siO
4(M=Sr, Ca, Ba) system has also obtained preliminary commercial applications at present, and this substrate material has become important luminous host material.
But there are two kinds of crystalline phases in this substrate material, α '-Sr
2siO
4with β-Sr
2siO
4, and numerous documents and materials research shows, the rare earth ion being incorporated into two kinds of crystalline phase cases often has different luminescent properties, such as emission wavelength, emission peak halfwidth, emissive porwer and corresponding excitating performance.Based on this, the Sr of the not jljl phase of different rare earth ions doping
2siO
4luminescent powder has different application potentials and field.Wherein, β phase Sr
2siO
4powder is because coordination polyhedron and crystal field effects etc. are to Eu
3+, Tb
3+plasma is compared to α ' phase Sr
2siO
4there is the advantage such as higher luminous intensity and excitation wavelength coupling.
At present, rear-earth-doped Sr is prepared
2siO
4the main method of silicate powder material is solid phase method, and raw material is SrCO
3, SiO
2and rare earth oxide, its calcining temperature is at 1100-1300 DEG C, and usual β and α ' of thing phase composite of synthetic powder coexists, and often containing SrSiO
3dephasign, is difficult to obtain pure phase β-Sr by directly optimizing calcining temperature system
2siO
4powder.And well-known, the luminous intensity to luminescent material, efficiency of conversion are had material impact by compound type particularly foreign matter content, prepare pure β phase Sr
2siO
4powder is most important.
At present, document 1 (JAlloy Compd, 512 (2012) 5-11) is by optimizing fusing assistant NH in solid state reaction
4the add-on of Cl obtains pure β phase powder (as at 1.0wt%NH
4cl fusing assistant, obtains Dy when being incubated 4h at 1000 DEG C
3+adulterate pure β-Sr
2siO
4powder); Document 2 (J European Ceram Soc, 11 (1993) 291-298) defines principal phase β-Sr under the high temperature of 1400 DEG C
2siO
4powder, but be not single-phase; Document 3 (J Rare Earth, 26 (2008) 421-424) also obtain the higher β phase powder of purity (as during when Eu concentration x≤0.005 when attempting the different dopant ion concentration of preparation, powder principal phase is β phase, but powder consists of α ' phase when concentration increases to x>0.01).
In the above documents, although its principal phase is β phase in the powder that obtains of great majority, the α ' phase wherein containing a great deal of, and need up to the 1300 even calcining temperature of 1400 DEG C; When additionally adding fusing assistant, form appropriate liquid phase by fusing assistant, reduce calcining temperature in the mode of Liquid Phase Diffusion, optimize sintering process, but the chlorosilicate reaction by product formed under high temperature, can not be removed from luminescent powder by simple water washing process.When adopting different dopant ion concentration to replace, β-Sr
2siO
4powder all can not controlled syntheses, especially cannot systematic study different ions kind and concentration this thing mutually in luminescent properties.Above-mentioned preparation method and condition is made to be subject to huge restriction.
Summary of the invention
The object of the present invention is to provide a kind of molten-salt growth method that adopts to prepare rare-earth doped beta phase Sr
2siO
4the method of nano-powder, the method is with high-purity (99.99% and more than) high-specific-surface mesoporous structure SiO
2powder is Si raw material, with NaCl-KCl mixture for molten salt system, with NaNO
3for catalysts, under lower calcining temperature, (be only 750 ~ 800 DEG C) nanoparticle powder that thing phase composite is pure β phase can be obtained.
A kind of rare-earth doped beta phase Sr that the present invention proposes
2siO
4the molten salt preparation method of nano-powder a kind ofly adopts NaCl-KCl mixture to be molten salt system, with high-purity (99.99% and more than) high-specific-surface mesoporous structure SiO
2powder is Si raw material; At a lower temperature, molten salt system melting, Sr (NO also molten near 570 DEG C
3)
2the Sr formed
2+, O
2-plasma is diffused into the meso-hole structure SiO of high-ratio surface in this liquid medium with high rate of diffusion
2on powder, larger contact gear ratio surface and shorter thermal-diffusion length, cause fast nucleation and the growth of crystalline phase; Meanwhile, molten salt system can adopt washing just can remove after the reaction simply.Therefore, the method is a kind of simple, economy, high efficiency preparation method of preparing high-purity, single-phase crystal powder under lower calcining temperature and shorter soaking time.But in the method, the formation kind of target crystalline phase is subject to molten salt system kind and composition, temperature of reaction and time in molten salt react ion, the great effect of the many factors such as fused salt addition.Meanwhile, add catalysts wherein with its high reaction activity and Si forming reactions intermediate, greatly reduce the potential barrier that thing is formed mutually, but its catalyst type and the kind of addition to formation phase also play significant role.
The present invention adopts following technical scheme:
Rare-earth doped beta phase Sr of the present invention
2siO
4nano-powder meets the strontium silicate component shown in following formula:
(Sr
1-xRE
x)
2SiO
4
In formula, RE is the one in rare earth element, 0.001≤x≤0.05.
RE is the one in praseodymium, samarium, europium, terbium or dysprosium.
Described rear-earth-doped Sr
2siO
4the thing phase composite of powder is pure β phase, and particle mean size is 40 ~ 80nm.
Rare-earth doped beta phase Sr of the present invention
2siO
4the molten salt preparation method of nano-powder, concrete steps are as follows:
(1) raw material is chosen: Sr raw material choose analytical pure Sr (NO
3)
2powder; RE raw material choose high pure oxide RE
2o
3powder, its purity be 99.99% and more than; The high-purity high-specific-surface mesoporous structure SiO of Si raw material choose
2powder, its purity be 99.99% and more than; The pure NaCl-KCl mixture of fused salt kind Analysis about Selection; Analytical pure NaNO
3for catalysts;
(2) weighing and ball milling: by (Sr
1-xrE
x)
2siO
4material molar ratio raw materials weighing powder needed for composition, adds NaCl-KCl fused salt, NaNO
3catalyzer, and add solvent dehydrated alcohol configuration slurry; Ball milling mixing 2 ~ 4 hours on planetary ball mill, drum's speed of rotation is 100 ~ 200r/min;
(3) dry and calcining: after being mixed by ball milling, powder is placed in 60 ~ 80 DEG C of baking ovens, 8 ~ 12 hours dry out solvent, be placed in agate mortar grinding 10 ~ 20 minutes again, finally put into retort furnace and carry out high-temperature calcination, temperature is 750 ~ 800 DEG C, soaking time 4 ~ 8 hours;
(4) cleaning and oven dry: take out after calcining powder and naturally cooling to room temperature, be placed in deionized water for stirring cleaning, make fused salt be dissolved in deionized water, filter and obtain insolubles, repeatedly clean, filter repeatedly, until filtered liquid clarification, and detects without Cl
-ion exists (adopts AgNO
3solution titration produces without AgCl precipitation); Finally, filtration insolubles is placed in 100 ~ 120 DEG C of baking ovens and within 8 ~ 12 hours, dries and obtain rear-earth-doped strontium silicate powder.
In step (1), selected Si raw material is for having high-specific-surface mesoporous structure SiO
2powder, its specific surface is greater than 1000m
2/ g, hole mean sizes is less than 10nm.
In step (2), for avoiding impurity to be mixed into, abrading-ball selects high-purity agate ball, and ball grinder selects high-purity agate tank; Material powder: ball: mass ratio=1:(1 ~ 2 of solvent): (1 ~ 3).
Synthesized molten salt system needed for process is NaCl-KCl mixture, both mol ratios (0.5 ~ 1): 1, its molten salt mixture addition and preparation Sr
2siO
4the mol ratio of powder is (6 ~ 8): 1; Synthesized process adds NaNO
3for catalysts, its addition and preparation Sr
2siO
4the mol ratio of powder is (0.05 ~ 0.1): 1;
Positively effect of the present invention is as follows:
1. with rear-earth-doped Sr prepared by method provided by the invention
2siO
4it is high that powder has phase purity, and thing is detected as pure β phase mutually, and without the need to adding fusing assistant, the foreign matters such as fused salt can wash removing, succinct, efficient.
2. prepare rear-earth-doped Sr by method provided by the invention
2siO
4it is low that powder has synthesis temperature, only needs 750 ~ 800 DEG C, at least lower than common solid phase method more than 500 DEG C, and energy-saving effect is obvious, also greatly reduces the requirement of equipment etc.
3. with rear-earth-doped Sr prepared by method provided by the invention
2siO
4powder, its particle size is little, and being only is 40 ~ 80nm.
Accompanying drawing explanation
Fig. 1 is for prepare 1.0mol%Eu according to example 1
3+doping Sr
2siO
4the XRD figure of powder, schemes the diffraction peak that short-and-medium vertical line is standard β phase, known, and powder, without any dephasign diffraction peak, consists of pure β phase.
Fig. 2 is for prepare 0.1mol%Eu according to example 2
3+doping Sr
2siO
4the SEM figure of powder, show that particle size is little, morphology microstructure is needle-like or bar-shaped, and particle diameter length is all less than 100nm.Fig. 3 is for prepare 5.0mol%Pr according to example 3
3+doping Sr
2siO
4the emmission spectrum of powder, excitation wavelength is 395nm, and powder sends centre wavelength and is positioned at 565 gold-tinteds and 610nm ruddiness and the dark red light of 646nm, and Integral luminous color is reddish orange.
Embodiment
The following examples describe in further detail of the present invention.
Below in conjunction with embodiment (with 1.0mol%Eu
3+doping, 0.1mol%Eu
3+, 5.0mol%Pr
3+doping Sr
2siO
4component is representative instance) the present invention is further illustrated, but should not limit the scope of the invention with this.
The present invention adopts NaCl-KCl mixture to be molten salt system, with high-purity (99.99% and more than) high-specific-surface mesoporous structure SiO
2powder is Si raw material, with the Sr (NO of low melting point
3)
2for Sr raw material, with NaNO
3for catalysts, adopt molten-salt growth method, prepare pure β phase Sr
2siO
4nano-powder, 3 specific embodiment components as table 1, with theoretical yield 50g for standard.
Table 1
Embodiment 1
#((Sr
0.99eu
0.01)
2siO
4):
Form as in table 11
#shown in, concrete preparation method comprises the following steps:
1. weighing: by the composition raw materials weighing in table 1, fused salt and catalystic material;
2. ball milling: add NaCl-KCl fused salt, NaNO in above-mentioned mixed powder
3catalyzer, adds dehydrated alcohol configuration slurry; On planetary ball mill, ball milling mixes 2 hours, and drum's speed of rotation is 200r/min; For avoiding impurity to be mixed into, abrading-ball is high-purity agate ball, and ball grinder is high-purity agate tank; Material powder: ball: the mass ratio=1:1:3 of solvent;
3. dry and calcine with fused salt: after being mixed by ball milling, powder is placed in 70 DEG C of baking ovens, 10 hours dry out solvent, then be placed in agate mortar grinding 20 minutes, finally put into retort furnace and carry out high-temperature calcination, temperature is 750 DEG C, soaking time 8 hours;
4. cleaning and oven dry: take out after calcining powder and naturally cooling to room temperature, use deionized water stirring and washing, make fused salt be dissolved in deionized water, filter and obtain insolubles, repeatedly clean, filter repeatedly, until filtered liquid clarification after the 5th, and detects without Cl
-ion exists (adopts AgNO
3solution titration produces without AgCl precipitation); Finally, filtration insolubles 120 DEG C of baking ovens are dried and obtain rear-earth-doped strontium silicate powder for 10 hours;
4. the powder obtained is carried out XRD test (Bruker, D2), adopts Cu-K alpha-ray, walk wide 0.02 °, sweep velocity 10 °/min, its collection of illustrative plates is shown in that accompanying drawing illustrates 1, schemes the diffraction peak that short-and-medium vertical line is standard β phase, can see, powder, without any dephasign diffraction peak, is pure β phase; It is needle-like or bar-shaped that SEM (JSM-6510, JEOL, Japan) records pattern, and its mean length is about 57.3nm; Adopt fluorescence spectrophotometer (JOBIN YVON, FL3-221) under 395nm wavelength excites, its emission center wavelength is the ruddiness of 616nm.
Embodiment 2
#((Sr
0.999eu
0.001)
2siO
4):
Form as in table 12
#shown in, concrete preparation method comprises the following steps:
1. weighing: by the composition raw materials weighing in table 1, fused salt and catalystic material;
2. ball milling: add NaCl-KCl fused salt, NaNO in above-mentioned mixed powder
3catalyzer, adds dehydrated alcohol configuration slurry; On planetary ball mill, ball milling mixes 4 hours, and drum's speed of rotation is 150r/min; For avoiding impurity to be mixed into, abrading-ball is high-purity agate ball, and ball grinder is high-purity agate tank; Material powder: ball: the mass ratio=1:2:1 of solvent;
3. dry and calcine with fused salt: after being mixed by ball milling, powder is placed in 60 DEG C of baking ovens, 8 hours dry out solvent, then be placed in agate mortar grinding 10 minutes, finally put into retort furnace and carry out high-temperature calcination, temperature is 800 DEG C, soaking time 6 hours;
4. cleaning and oven dry: take out after calcining powder and naturally cooling to room temperature, be placed in deionized water for stirring cleaning, make fused salt be dissolved in deionized water, filter and obtain insolubles, repeatedly clean, filter repeatedly, until filtered liquid clarification after the 4th, and detects without Cl
-ion exists (adopts AgNO
3solution titration produces without AgCl precipitation); Finally, filtration insolubles is placed in 100 DEG C of baking ovens and dries and obtain strontium silicate powder in 12 hours;
4. the powder obtained is carried out XRD test (Bruker, D2), and powder is pure β phase; It is needle-like or bar-shaped that SEM (JSM-6510, JEOL, Japan) records pattern, and its mean length is about 72.1nm, sees accompanying drawing 2; Adopt fluorescence spectrophotometer (JOBIN YVON, FL3-221) under 395nm wavelength excites, its emission center wavelength is the ruddiness of 616nm.。
Embodiment 3# ((Sr
0.95pr
0.05)
2siO
4):
Composition is as shown in 3# in table 1, and concrete preparation method comprises the following steps:
1. weighing: by the composition raw materials weighing in table 1, fused salt and catalystic material;
2. ball milling: add NaCl-KCl fused salt, NaNO in above-mentioned mixed powder
3catalyzer, adds dehydrated alcohol configuration slurry; On planetary ball mill, ball milling mixes 3 hours, and drum's speed of rotation is 100r/min; For avoiding impurity to be mixed into, the preferred high-purity agate ball of abrading-ball, the preferred high-purity agate tank of ball grinder; Material powder: ball: the mass ratio=1:1.5:2 of solvent;
3. dry and calcine with fused salt: after being mixed by ball milling, powder is placed in 80 DEG C of baking ovens, 12 hours dry out solvent, then be placed in agate mortar grinding 15 minutes, finally put into retort furnace and carry out high-temperature calcination, temperature is 780 DEG C, soaking time 4 hours;
4. cleaning and oven dry: take out after calcining powder and naturally cooling to room temperature, use deionized water stirring and washing, make fused salt be dissolved in deionized water, filter and obtain insolubles, repeatedly clean, filter repeatedly, until filtered liquid clarification after the 5th, and detects without Cl
-ion exists (adopts AgNO
3solution titration produces without AgCl precipitation); Finally, filtration insolubles 105 DEG C of baking ovens are dried and obtain rear-earth-doped strontium silicate powder for 8 hours;
4. the powder obtained is carried out XRD test (Bruker, D2), adopts Cu-K alpha-ray, sampling step is wide 0.02 °, sweep velocity 10 °/min, and powder is pure β phase; It is needle-like or bar-shaped that SEM (JSM-6510, JEOL, Japan) records pattern, and its mean length is about 49.5nm; Adopt fluorescence spectrophotometer (JOBINYVON, FL3-221), excitation wavelength is 395nm, and powder sends centre wavelength and is positioned at 565 gold-tinteds and 610nm ruddiness and the dark red light of 646nm, and Integral luminous color is reddish orange, sees accompanying drawing 3.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (9)
1. a rare-earth doped beta phase Sr
2siO
4nano-powder, is characterized in that: described nano-powder meets the strontium silicate component shown in following formula:
(Sr
1-xRE
x)
2SiO
4
In formula, RE is the one in rare earth element, 0.001≤x≤0.05.
2. rare-earth doped beta phase Sr as claimed in claim 1
2siO
4nano-powder, is characterized in that: RE is the one in praseodymium, samarium, europium, terbium or dysprosium.
3. rare-earth doped beta phase Sr as claimed in claim 1
2siO
4nano-powder, is characterized in that: described rear-earth-doped Sr
2siO
4the thing phase composite of powder is pure β phase, and particle mean size is 40 ~ 80nm.
4. prepare the rare-earth doped beta phase Sr as described in any one of claim 1-3 for one kind
2siO
4the method of nano-powder, is characterized in that: adopt molten-salt growth method preparation, concrete steps are as follows:
(1) raw material is chosen: Sr raw material choose analytical pure Sr (NO
3)
2powder; RE raw material choose high pure oxide RE
2o
3powder, its purity be 99.99% and more than; The high-purity high-specific-surface mesoporous structure SiO of Si raw material choose
2powder, its purity be 99.99% and more than; The pure NaCl-KCl mixture of fused salt kind Analysis about Selection; Analytical pure NaNO
3for catalysts;
(2) weighing and ball milling: by (Sr
1-xrE
x)
2siO
4material molar ratio raw materials weighing powder needed for composition, adds NaCl-KCl fused salt, NaNO
3catalyzer, and add solvent dehydrated alcohol configuration slurry; Ball milling mixing 2 ~ 4 hours on planetary ball mill, drum's speed of rotation is 100 ~ 200r/min;
(3) oven dry is calcined with fused salt: after being mixed by ball milling, powder is placed in 60 ~ 80 DEG C of baking ovens, 8 ~ 12 hours dry out solvent, be placed in agate mortar grinding 10 ~ 20 minutes again, finally put into retort furnace and carry out high-temperature calcination, temperature is 750 ~ 800 DEG C, soaking time 4 ~ 8 hours;
(4) cleaning and oven dry: take out after calcining powder and naturally cooling to room temperature, be placed in deionized water for stirring cleaning, make fused salt be dissolved in deionized water, filter and obtain insolubles, repeatedly clean, filter repeatedly, until filtered liquid clarification, and detects without Cl
-ion exists; Finally, filtration insolubles is placed in 100 ~ 120 DEG C of baking ovens and within 8 ~ 12 hours, dries and obtain rear-earth-doped strontium silicate powder.
5. preparation method as claimed in claim 4, it is characterized in that: in step (1), selected Si raw material is for having high-specific-surface mesoporous structure SiO
2powder, its specific surface is greater than 1000m
2/ g, hole mean sizes is less than 10nm.
6. preparation method as claimed in claim 4, it is characterized in that: in step (2), for avoiding impurity to be mixed into, abrading-ball selects high-purity agate ball, and ball grinder selects high-purity agate tank; Material powder: ball: mass ratio=1:(1 ~ 2 of solvent): (1 ~ 3).
7. preparation method as claimed in claim 4, is characterized in that: in step (2), both mol ratios (0.5 ~ 1) in fused salt NaCl-KCl mixture: 1, its molten salt mixture addition and preparation Sr
2siO
4the mol ratio of powder is (6 ~ 8): 1.
8. preparation method as claimed in claim 4, is characterized in that: in step (2), NaNO
3catalyst loading and preparation Sr
2siO
4the mol ratio of powder is (0.05 ~ 0.1): 1.
9. preparation method as claimed in claim 4, is characterized in that: in step (3), detects without Cl
-there is employing AgNO in ion
3the method that solution titration produces without AgCl precipitation.
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| CN105062470A (en) * | 2015-08-24 | 2015-11-18 | 上海工程技术大学 | Molten-salt growth method for preparing manganese-doped zinc silicate green fluorescent powder |
| CN107043622A (en) * | 2016-12-30 | 2017-08-15 | 陕西科技大学 | A kind of europium doping strontium silicate blood orange emitting phosphor and preparation method thereof |
| CN110564408A (en) * | 2019-08-26 | 2019-12-13 | 昆明理工大学 | Samarium-doped silicate luminescent material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105062470A (en) * | 2015-08-24 | 2015-11-18 | 上海工程技术大学 | Molten-salt growth method for preparing manganese-doped zinc silicate green fluorescent powder |
| CN105062470B (en) * | 2015-08-24 | 2017-03-15 | 上海工程技术大学 | A kind of method that molten-salt growth method prepares the green willemite phosphor for mixing manganese |
| CN107043622A (en) * | 2016-12-30 | 2017-08-15 | 陕西科技大学 | A kind of europium doping strontium silicate blood orange emitting phosphor and preparation method thereof |
| CN110564408A (en) * | 2019-08-26 | 2019-12-13 | 昆明理工大学 | Samarium-doped silicate luminescent material and preparation method thereof |
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