CN107142109A - Terbium-doped green fluorescent material by matrix of vanadate and preparation method thereof - Google Patents
Terbium-doped green fluorescent material by matrix of vanadate and preparation method thereof Download PDFInfo
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- CN107142109A CN107142109A CN201710509614.6A CN201710509614A CN107142109A CN 107142109 A CN107142109 A CN 107142109A CN 201710509614 A CN201710509614 A CN 201710509614A CN 107142109 A CN107142109 A CN 107142109A
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- vanadate
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- terbium
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
- C09K11/7751—Vanadates; Chromates; Molybdates; Tungstates
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Abstract
The invention discloses the terbium-doped green fluorescent material using vanadate as matrix, using vanadate as matrix, chemical general formula is KBa1‑xVO4:XTb, wherein 0.01≤x≤0.08, passes through the active ions Tb that adulterates3+, the terbium-doped green fluorescent material using vanadate as matrix is prepared, is adapted near ultraviolet or blue light is excited, the main excitation peak 312nm of the green emitting phosphor, its emission spectrum is in 400nm~620nm, and main peak is near 488nm and 545nm, chemical property is stable, good luminous performance；The invention also discloses its preparation method, by K2CO3、BaCO3、V2O5And Tb4O7Calcined under mixed grinding, air atmosphere, insulation is ground, finally obtains the terbium-doped green fluorescent material using vanadate as matrix, prepared based on solid-phase synthesis again after furnace cooling, and temperature-rise period is simple, and method is simple and easy to apply, favorable reproducibility, short preparation period.
Description
Technical field
The invention belongs to LED fluorescent material preparing technical fields, and in particular to the terbium-doped green using vanadate as matrix is glimmering
Light powder, the invention further relates to the preparation method of terbium-doped green fluorescent material.
Background technology
Light emitting diode (Light Emitting Diode, LED) is acknowledged as the new light sources of 21st century, has
Many advantages, such as energy-conservation, fast response, environmental protection, long lifespan, small volume and high luminous efficiency, have in illumination and display field
Huge application prospect.In recent years, white light LEDs cause the extensive concern of people as energy-conserving light source of new generation.At present, with
The white emitting fluorescent powder that black light tube core matches lacks, generally using the method system of mixing three kinds of primary colours fluorescent material of red, green, blue
, luminescent properties are undesirable.Therefore, cost can not only be reduced by developing single matrix white emitting fluorescent powder, can also improve fluorescent material
Luminescent properties, tool is of great significance.
Red, green, blue color fluorescent material is excited as ultraviolet-near ultraviolet LED chip, because green emitting phosphor luminous efficiency is relative
Luminous efficiency is than relatively low for the fluorescent material of other two kinds of colors, so influencing whether whole LED luminous flux.Thus may be used
See, it is with researching value, Tb to seek a kind of green emitting phosphor of new system3+In the activator side as green emitting phosphor
Face, with very big potentiality.
The content of the invention
It is high, chemical with luminous efficiency it is an object of the invention to provide the terbium-doped green fluorescent material using vanadate as matrix
The characteristics of property stabilization and high luminous intensity.
It is a further object to provide the preparation method of the terbium-doped green fluorescent material using vanadate as matrix.
The technical solution adopted in the present invention is, the terbium-doped green fluorescent material by matrix of vanadate, using vanadate as base
Matter, chemical general formula is KBa1-xVO4:XTb, wherein 0.01≤x≤0.08.
Another technical scheme of the present invention is, the preparation side of the terbium-doped green fluorescent material by matrix of vanadate
Method, it is characterised in that specifically implement according to following steps：
Step 1, by chemical general formula KBa1-xVO4:XTb mol ratio, wherein 0.01≤x≤0.08, is weighed containing K respectively
Compound, compound containing Ba, compound containing V and compound containing Tb are used as raw material；
Step 2, will all raw materials that weighed in step 1 mix after grind, formed compound；
Step 3, by the compound obtained through step 2 under air atmosphere calcine 3h~9h, calcining heat be 1000 DEG C~
1200 DEG C, cool to room temperature after the completion of calcining with the furnace, obtain calcined product；
Step 4, the calcined product that step 3 is obtained is ground, obtains the terbium-doped green fluorescence using vanadate as matrix
Powder.
The characteristics of another technical scheme of the invention, also resides in,
In step 1：Compound containing K is K2CO3, compound containing Ba be BaCO3, compound containing V be V2O5And containing Tbization
Compound is Tb4O7。
Milling time is 20min~60min in step 2.
Heating rate is 3 DEG C/min~10 DEG C/min in step 3.
Milling time is 20min~60min in step 4.
The beneficial effects of the invention are as follows terbium-doped green fluorescent material of the present invention by matrix of vanadate, using vanadate as base
Matter, passes through the active ions Tb that adulterates3+, the terbium-doped green fluorescent material using vanadate as matrix can be prepared, be adapted near ultraviolet or
Blue light is excited, and the excitation spectrum of the green emitting phosphor is in 300nm~500nm, and main excitation peak 312nm, its emission spectrum exists
400nm~620nm, main peak near 488nm and 545nm, with chemical property stabilization, good luminous performance, luminous intensity it is high and
The good advantage of colour rendering；The preparation method of terbium-doped green fluorescent material of the present invention by matrix of vanadate, wherein being closed based on solid phase
Cheng Fa, strong operability is mainly prepared in air atmosphere, and temperature-rise period is simple, and whole method is simple and easy to apply, favorable reproducibility and system
The standby cycle is short.
Brief description of the drawings
Fig. 1 is the KBa that embodiment 4 is prepared0.99VO4:The X ray diffracting spectrum of 0.01Tb green emitting phosphors with
KBaVO4Standard card (PDF#31-0979) comparison diagram；
Fig. 2 is the KBa that embodiment 6 is prepared0.96VO4:The excitation spectrum and emission spectrum of 0.04Tb green emitting phosphors
Figure；
Fig. 3 is the KBa that embodiment 6 is prepared0.96VO4:The CIE chromaticity coordinates figures of 0.04Tb green emitting phosphors.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
Terbium-doped green fluorescent material of the present invention by matrix of vanadate, using vanadate as matrix, chemical general formula is KBa1- xVO4:XTb, wherein 0.01≤x≤0.08.
The preparation method of terbium-doped green fluorescent material of the present invention by matrix of vanadate, specifically implements according to following steps：
Step 1, by chemical general formula KBa1-xVO4:XTb mol ratio, wherein 0.01≤x≤0.08, is weighed respectively
K2CO3、BaCO3、V2O5And Tb4O7It is used as raw material；
Step 2, will all raw materials that weighed in step 1 mix after grind 20min~60min, it is to be mixed it is uniform after, formed
Compound；
Step 3, by the compound obtained through step 2 under air atmosphere calcine 3h~9h, calcining heat be 1000 DEG C~
1200 DEG C, heating rate is 3 DEG C/min~10 DEG C/min, cools to room temperature with the furnace after the completion of calcining, obtains calcined product；
Wherein, synthesized during calcining according to following chemical equation：
K2CO3+(1-x)BaCO3+V2O5+x/4Tb4O7→KBaVO4+CO2；
Step 4, the calcined product for obtaining step 3 grind 20min~60min, obtain mixing terbium by matrix of vanadate
Green emitting phosphor.
Embodiment 1
X=0.01 is taken, by chemical formula KBa0.99VO4:0.01Tb stoichiometric, is weighed respectively with electronic balance
K2CO3、BaCO3、V2O5And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Weighed above-mentioned
The mixing of all raw materials after grind 20min, make to be well mixed between raw material, obtain compound；Obtained compound is loaded firm
In beautiful crucible, and the corundum crucible is placed in be rapidly heated in resistance furnace, in being calcined under air atmosphere, during which with 3 DEG C/min's
Heating rate rises to 1000 DEG C, and calcination time is 3h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, is calcined
Product；The product regrinding 20min after calcining is taken out, that is, obtains the terbium-doped green fluorescent material using vanadate as matrix.
Embodiment 2
X=0.01 is taken, by chemical formula KBa0.99VO4:0.01Tb stoichiometric, is weighed respectively with electronic balance
K2CO3、BaCO3、V2O5And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Weighed above-mentioned
All raw mill 30min, make to be well mixed between raw material, obtain compound；Obtained compound is loaded into corundum crucible,
And the corundum crucible is placed in be rapidly heated in resistance furnace, in being calcined under air atmosphere, risen to 5 DEG C/min heating rate
1050 DEG C, calcination time is 5h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, obtains calcined product；Take out calcining
Product regrinding 30min afterwards, that is, obtain the terbium-doped green fluorescent material using vanadate as matrix.
Embodiment 3
X=0.01 is taken, by chemical formula KBa0.99VO4:0.01Tb stoichiometric, is weighed respectively with electronic balance
K2CO3、BaCO3、V2O5And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Weighed above-mentioned
All raw materials be ground 60min, make to be well mixed between raw material, obtain compound；Obtained compound is loaded into corundum
Crucible, and the corundum crucible is placed in be rapidly heated in resistance furnace, in being calcined under air atmosphere, with 10 DEG C/min heating rate
1200 DEG C are risen to, calcination time is 9h, wait furnace cooling after the completion of calcining, until being cooled to room temperature, obtain calcined product；Take out
Product regrinding 60min after calcining, that is, obtain the terbium-doped green fluorescent material using vanadate as matrix.
Embodiment 4
X=0.01 is taken, by chemical formula KBa0.99VO4:0.01Tb stoichiometric, is weighed respectively with electronic balance
K2CO3、BaCO3、V2O5And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Weighed above-mentioned
All raw materials be ground 40min, make to be well mixed between raw material, obtain compound；Obtained compound is loaded into corundum
Crucible, and the corundum crucible is placed in be rapidly heated in resistance furnace, in calcining the heating rate liter with 5 DEG C/min under air atmosphere
To 1050 DEG C, calcination time is 5h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, obtains calcined product；Taking-up is forged
Product regrinding 50min after burning, that is, obtain the terbium-doped green fluorescent material using vanadate as matrix.
The KBa that Fig. 1 is prepared using the preparation method in embodiment 40.99VO4:The X-ray of 0.01Tb green emitting phosphors
Diffracting spectrum and KBaVO4Standard card (PDF#31-0979) comparison diagram, as can be seen from Figure 1：Its thing phase purity is high, crystallinity
It is good.
Embodiment 5
X=0.02 is taken, by chemical formula KBa0.98VO4:0.02Tb stoichiometric, is weighed respectively with electronic balance
K2CO3、BaCO3、V2O5And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Weighed above-mentioned
All raw materials be ground 45min, make to be well mixed between raw material, obtain compound；Obtained compound is loaded into corundum
Crucible, the corundum crucible is placed in and is rapidly heated in resistance furnace, in being calcined under air atmosphere, with 6 DEG C/min heating rate liter
To 1050 DEG C, calcination time is 5h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, obtains calcined product；Taking-up is forged
Product regrinding 40min after burning, that is, obtain the terbium-doped green fluorescent material using vanadate as matrix.
Embodiment 6
X=0.04 is taken, by chemical formula KBa0.96VO4:0.04Tb stoichiometric, is weighed respectively with electronic balance
K2CO3、BaCO3、V2O5And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；By above-mentioned raw materials
It is ground after 30min, makes to be well mixed between raw material, obtain compound；Obtained compound is fitted into corundum crucible, and
The corundum crucible is placed in and is rapidly heated in resistance furnace, in being calcined under air atmosphere, is during which risen to 7 DEG C/min heating rate
1050 DEG C, calcination time is 5h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, obtains calcined product；Take out calcining
Product regrinding 50min afterwards, that is, obtain the terbium-doped green fluorescent material using vanadate as matrix.
Fig. 2 is the KBa prepared using the preparation method in embodiment 60.96VO4:0.04Tb green emitting phosphors are excited
Spectrum and emission spectrum, its main excitation peak is near 312nm as seen from Figure 2, and main emission peak is near 488nm and 545nm；
As can be seen here, the fluorescent material can effectively be excited by black light and blue light and send green glow, can be applied to white light LEDs.
Fig. 3 utilizes the KBa prepared by the preparation method in embodiment 60.96VO4:The CIE colors of 0.04Tb green emitting phosphors are sat
Mark on a map, as can be seen from Figure 3：The CIE chromaticity coordinates of the green emitting phosphor is (x=0.282, y=0.587).
Embodiment 7
X=0.06 is taken, by chemical formula KBa0.94VO4:0.06Tb stoichiometric, is weighed respectively with electronic balance
K2CO3、BaCO3、V2O5And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；By above-mentioned raw materials
It is ground after 40min, makes to be well mixed between raw material, obtain compound；Obtained compound is fitted into corundum crucible, and
The corundum crucible is placed in and is rapidly heated in resistance furnace, in being calcined under air atmosphere, is during which risen to 8 DEG C/min heating rate
1200 DEG C, calcination time is 9h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, obtains calcined product；Take out calcining
Product regrinding 45min afterwards, that is, obtain the terbium-doped green fluorescent material using vanadate as matrix.
Embodiment 8
X=0.08 is taken, by chemical formula KBa0.92VO4:0.08Tb stoichiometric, is weighed respectively with electronic balance
K2CO3、BaCO3、V2O5And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；By above-mentioned raw materials
It is ground after 60min, makes to be well mixed between raw material, obtain compound；Obtained compound is loaded into corundum crucible, and will
The corundum crucible, which is placed in, to be rapidly heated in resistance furnace, and in being calcined under air atmosphere, 1150 are risen to 5 DEG C/min heating rate
DEG C, calcination time is 8h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, obtains calcined product；Take out after calcining
Product regrinds 35min, that is, obtains the terbium-doped green fluorescent material using vanadate as matrix.
Terbium-doped green fluorescent material of the present invention by matrix of vanadate, using vanadate as matrix, adulterate active ions Tb3+,
Ion cluster VO in vanadate luminescent material4 3-There is strong absorption in ultraviolet region, the energy of absorption can be effectively transferred to
Activator ion, the energy that matrix vanadic acid radical ion absorbs is divided into two parts, and a portion passes through V5+On -2nAnd V5+On -2n+1It
Between energy level transition produce broadband VISIBLE LIGHT EMISSION, also another part is then to pass to activator ion Tb3+, so as to induce it
Generation energy level transition produces red emission.Pass through the active ions Tb that adulterates3+, prepare the terbium-doped green using vanadate as matrix
Fluorescent material, is adapted near ultraviolet or blue light is excited, and the excitation spectrum of the green emitting phosphor is in 300nm~500nm, main excitation peak
312nm, its emission spectrum is in 400nm~620nm, and main peak is near 488nm and 545nm, and chemical property is stable, luminescent properties
Good, luminous intensity is high, and colour rendering is good；The preparation method of terbium-doped green fluorescent material by matrix of vanadate, based on synthesis in solid state
Prepared by method, strong operability is prepared in air atmosphere, and temperature-rise period is simple, and method is simple and easy to apply, favorable reproducibility, prepares week
Phase is short.
Claims (6)
1. the terbium-doped green fluorescent material by matrix of vanadate, it is characterised in that using vanadate as matrix, chemical general formula is
KBa1-xVO4:XTb, wherein 0.01≤x≤0.08.
2. a kind of preparation method of the terbium-doped green fluorescent material as claimed in claim 1 by matrix of vanadate, its feature exists
In specifically implementing according to following steps：
Step 1, by chemical general formula KBa1-xVO4:XTb mol ratio, wherein 0.01≤x≤0.08, weighs chemical combination containing K respectively
Thing, compound containing Ba, compound containing V and compound containing Tb are used as raw material；
Step 2, will all raw materials that weighed in step 1 mix after grind, formed compound；
Step 3, by the compound obtained through step 2 under air atmosphere calcine 3h~9h, calcining heat be 1000 DEG C~1200
DEG C, cool to room temperature after the completion of calcining with the furnace, obtain calcined product；
Step 4, the calcined product that step 3 is obtained is ground, obtains the terbium-doped green fluorescent material using vanadate as matrix.
3. the preparation method of the terbium-doped green fluorescent material according to claim 2 using vanadate as matrix, it is characterised in that
In the step 1：Compound containing K is K2CO3, compound containing Ba is BaCO3, compound containing V is V2O5, compound containing Tb is
Tb4O7。
4. the preparation method of the terbium-doped green fluorescent material according to claim 2 using vanadate as matrix, it is characterised in that
In the step 2：Milling time is 20min~60min.
5. the preparation method of the terbium-doped green fluorescent material according to claim 2 using vanadate as matrix, it is characterised in that
In the step 3：Heating rate is 3 DEG C/min~10 DEG C/min in calcination process.
6. the preparation method of the terbium-doped green fluorescent material according to claim 2 using vanadate as matrix, it is characterised in that
In the step 4：Milling time is 20min~60min.
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| CN102399558A (en) * | 2011-11-24 | 2012-04-04 | 苏州大学 | Vanadate red phosphor, preparation method and application |
| CN102618270A (en) * | 2012-03-19 | 2012-08-01 | 湖南信多利新材料有限公司 | Vanadate substrate fluorescent powder for white light LED (light-emitting diode) and preparation method thereof |
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2017
- 2017-06-28 CN CN201710509614.6A patent/CN107142109A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| CN101624521A (en) * | 2009-07-03 | 2010-01-13 | 成都理工大学 | Vanadate garnet type fluorescent material as well as preparation method and application thereof |
| CN102344804A (en) * | 2011-07-27 | 2012-02-08 | 中国科学院宁波材料技术与工程研究所 | Vanadate fluorescent powder material and preparation method thereof |
| CN102399558A (en) * | 2011-11-24 | 2012-04-04 | 苏州大学 | Vanadate red phosphor, preparation method and application |
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Application publication date: 20170908 |