CN107033901A - A kind of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder and preparation method thereof - Google Patents
A kind of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder and preparation method thereof Download PDFInfo
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- CN107033901A CN107033901A CN201710388153.1A CN201710388153A CN107033901A CN 107033901 A CN107033901 A CN 107033901A CN 201710388153 A CN201710388153 A CN 201710388153A CN 107033901 A CN107033901 A CN 107033901A
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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
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Abstract
The invention discloses the terbium doped three boric acid lanthanum-strontium base green light fluorescent powder of one kind, with Sr3La(BO3)3For matrix, chemical general formula is Sr3La1‑x(BO3)3:XTb, wherein 0.01≤x≤0.10, passes through the active ions Tb that adulterates3+, terbium doped three boric acid lanthanum-strontium base green light fluorescent powder is prepared, transmitting peak position is located at 490nm, 547nm, 585nm, 625nm respectively, chromaticity coordinates is located at green wavelength, and chemical property is stable, good luminous performance, luminous intensity is high, and colour rendering is good, is a kind of green light fluorescent powder of good luminescence property；The invention also discloses its preparation method, by SrCO3、La2O3、H3BO3And Tb4O7Mixed grinding, 5%H2Calcined under+95%Ar reducing atmospheres, insulation is ground, finally obtains terbium doped three boric acid lanthanum-strontium base green light fluorescent powder again after furnace cooling, prepared based on solid-phase synthesis, strong operability, temperature-rise period is simple, 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 a kind of terbium doped three boric acid lanthanum-strontium base green glow
Fluorescent material, the invention further relates to the preparation method of the terbium doped three boric acid lanthanum-strontium base green light fluorescent powder.
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, high luminous efficiency, have in illumination and display field
Huge application prospect；Rare earth ion has good physical and chemical stability and the characteristics of luminescence, and its luminescent material adulterated exists
The fields such as green illumination, short wavelength laser, presentation of information, bioluminescence mark and photoelectronics have before wide application
Scape.
At present, commercial white light LEDs produce white light and mainly excite YAG by the blue light of GaIn bases chip generation:Ce3+Fluorescence
Powder, but the white light produced lacks red color components, causes the relatively low (Ra of its color rendition index<80), the higher (CCT of correlated colour temperature>
7000K), common lighting requirement can only be met.Redgreenblue fluorescent material is coated near ultraviolet LED chip, near ultraviolet
Light excitated blue, green, red fluorescence powder formation blue and green light, feux rouges combination can also send white light.This method not only may be used
To overcome the problem of conventional white light LED is present, the luminous color of control is also easy to.Tb3+Through swashing frequently as a kind of green emission
Agent living, can excite lower transmitting green glow near ultraviolet wavelength.Therefore, research can effectively be excited by black light, luminous intensity height,
The good terbium doped three boric acid lanthanum-strontium base green light fluorescent powder of purity has good actual application value.
The content of the invention
It is an object of the invention to provide the terbium doped three boric acid lanthanum-strontium base green light fluorescent powder of one kind, existing white light LEDs phase is solved
Close the problem of colour temperature is high, display index is low.
It is a further object to provide a kind of preparation method of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder.
The technical solution adopted in the present invention is, with Sr3La(BO3)3For matrix, chemical general formula is Sr3La1-x(BO3)3:
XTb, wherein 0.01≤x≤0.10.
Another technical scheme of the present invention is, a kind of preparation of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder
Method, it is characterised in that specifically implement according to following steps：
Step 1, by chemical general formula Sr3La1-x(BO3)3:XTb mol ratio, wherein 0.01≤x≤0.10, is weighed respectively
Compound containing Sr, compound containing La, boride alloy and compound containing Tb, which contain, is used as raw material；
Step 2, the raw mill for being weighed step 1 are simultaneously well mixed；
Step 3, by well mixed raw material in 5%H23h~5h is calcined under+95%Ar reducing atmospheres, temperature is 1250 DEG C
~1300 DEG C, cool to room temperature with the furnace；
Step 4, the calcined product for obtaining step 3 are ground, and obtain terbium doped three boric acid lanthanum-strontium base green light fluorescent powder.
The features of the present invention is also resided in,
Compound containing Sr is SrCO in step 13, compound containing La be La2O3, boride alloy be H3BO3And chemical combination containing Tb
Thing is Tb4O7。
Milling time is 20min~60min in step 2.
Calcining uses SGQ-5-14 tube type resistance furnaces in step 3, and heating rate is 8 DEG C/min~10 DEG C/min.
Milling time is 20min~60min in step 4.
The beneficial effects of the invention are as follows the terbium doped three boric acid lanthanum-strontium base green light fluorescent powder of the present invention, with Sr3La(BO3)3For
Matrix, matrix cost is low, stability is good, it is easy prepare, have a very strong excitation peak near ultraviolet region, suitable UV is excited, can
Applied to LED；
Pass through the active ions Tb that adulterates3+, terbium doped three boric acid lanthanum-strontium base green light fluorescent powder is prepared, is adapted near ultraviolet and swashs
Hair, transmitting peak position is located at 490nm, 547nm, 585nm, 625nm respectively, and chromaticity coordinates is located at green wavelength (x=0.277, y=
0.411), the light emitting diode near ultraviolet chip is matched, and illustrates that fluorescent material prepared by the present invention is a kind of good luminescence property
Green emitting phosphor；
The preparation method of the terbium doped three boric acid lanthanum-strontium base green light fluorescent powder of the present invention, is prepared based on solid-phase synthesis, is grasped
The property made is strong, and temperature-rise period is simple, and method is simple and easy to apply, favorable reproducibility, short preparation period.
Brief description of the drawings
Fig. 1 is the Sr that embodiment 2 is prepared3La0.97(BO3)3:0.03Tb fluorescent material and Sr3La(BO3)3The X of matrix is penetrated
Ray diffraction diagram is composed.
Fig. 2 is the Sr that embodiment 3 is prepared3La0.95(BO3)3:The excitation spectrum and emission spectrum of 0.05Tb fluorescent material.
Fig. 3 is the Sr that embodiment 3 is prepared3La0.95(BO3)3:The CIE chromaticity coordinates figures of 0.05Tb fluorescent material.
Embodiment
With reference to the accompanying drawings and detailed description to terbium doped three boric acid lanthanum-strontium base green light fluorescent powder of the invention a kind of and
Its preparation method is described in detail.
A kind of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder of the invention, with Sr3La(BO3)3For matrix, chemical general formula is
Sr3La1-x(BO3)3:XTb, wherein 0.01≤x≤0.10.
A kind of preparation method of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder, it is characterised in that specifically according to following step
It is rapid to implement：
Step 1, by chemical general formula Sr3La1-x(BO3)3:XTb mol ratio, wherein 0.01≤x≤0.10, is weighed respectively
Containing SrCO3、La2O3、H3BO3And Tb4O7It is used as raw material；
Step 2, the raw mill 20min~60min for being weighed step 1 are simultaneously well mixed；
Step 3, by well mixed raw material using SGQ-5-14 tube type resistance furnaces in 5%H2Under+95%Ar reducing atmospheres
3h~5h is calcined, temperature is 1250 DEG C~1300 DEG C, and heating rate is 8 DEG C/min~10 DEG C/min, cools to room temperature with the furnace；
Wherein, synthesized during calcining according to following chemical equation：
3SrCO3+(1-x)/2La2O3+3H3BO3+x/4Tb4O7→Sr3La1-x(BO3)3:xTb+9/2H2O+3CO2
Step 4, the calcined product for obtaining step 3 grind 20min~60min, obtain terbium doped three boric acid lanthanum-strontium base green
Emitting phosphor.
Embodiment 1
X=0.01 is taken, by chemical formula Sr3La0.99(BO3)3:0.01Tb stoichiometric, it is accurate respectively with electronic balance
Really weigh SrCO3、La2O3、H3BO3And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Will
Above-mentioned raw materials are ground after 20min, are loaded corundum crucible, are placed in high temperature process furnances, in 5%H2+ 95%Ar reducing atmospheres
Under rise to 1250 DEG C with 8 DEG C/min heating rate, 3h, then furnace cooling are incubated, until being cooled to room temperature；Take out after calcining
Sample regrinding 20min, that is, obtain terbium doped three boric acid lanthanum-strontium base green light fluorescent powder.
Embodiment 2
X=0.03 is taken, by chemical formula Sr3La0.97(BO3)3:0.03Tb stoichiometric, it is accurate respectively with electronic balance
Really weigh SrCO3、La2O3、H3BO3And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Will
Above-mentioned raw materials are ground after 40min, are loaded corundum crucible, are placed in high temperature process furnances, in 5%H2+ 95%Ar reducing atmospheres
Under rise to 1270 DEG C with 9 DEG C/min heating rate, 4h, then furnace cooling are incubated, until being cooled to room temperature；Take out after calcining
Sample regrinding 50min, that is, obtain terbium doped three boric acid lanthanum-strontium base green light fluorescent powder.
Fig. 1 is Sr prepared by the present embodiment 23La0.97(BO3)3:0.03Tb fluorescent material and Sr3La(BO3)3The X-ray of matrix
Diffracting spectrum.Without discovery Sr in current PDF card bases3La(BO3)3Standard card, but Rietveld fitting result with
Sr3La(BO3)3The XRD results of matrix are consistent.It is seen that thing phase purity is high, and better crystallinity degree, the front and rear principal crystalline phase of doping is not
Generation significant change.
Embodiment 3
X=0.05 is taken, by chemical formula Sr3La0.99(BO3)3:0.05Tb stoichiometric, it is accurate respectively with electronic balance
Really weigh SrCO3、La2O3、H3BO3And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Will
Above-mentioned raw materials are ground after 60min, are loaded corundum crucible, are placed in high temperature process furnances, in 5%H2+ 95%Ar reducing atmospheres
Under rise to 1300 DEG C with 10 DEG C/min heating rate, 5h, then furnace cooling are incubated, until being cooled to room temperature；Take out calcining
Sample regrinding 60min afterwards, that is, obtain terbium doped three boric acid lanthanum-strontium base green light fluorescent powder.
Fig. 2 is Sr prepared by the present embodiment 33La0.99(BO3)3:The excitation spectrum and emission spectrum of 0.05Tb fluorescent material.Should
The excitation spectrum of fluorescent material in 310nm~400nm, main excitation peak near 376nm, its emission spectrum 450nm~
650nm, transmitting peak position is located at 490nm, 547nm, 585nm, 625nm respectively, and main peak is near 547nm.As can be seen here, the fluorescence
Powder can effectively be excited by black light and send green glow, can be applied to white light LEDs.
Fig. 3 is r prepared by the present embodiment 33La0.99(BO3)3:The CIE chromaticity coordinates figures of 0.05Tb fluorescent material, chromaticity coordinates is located at
Green wavelength (x=0.277, y=0.411) illustrates that fluorescent material prepared by the present invention is a kind of green-emitting fluorescent of good luminescence property
Powder.
Embodiment 4
X=0.08 is taken, by chemical formula Sr3La0.99(BO3)3:0.08Tb stoichiometric, it is accurate respectively with electronic balance
Really weigh SrCO3、La2O3、H3BO3And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Will
Above-mentioned raw materials are ground after 50min, are loaded corundum crucible, are placed in high temperature process furnances, in 5%H2+ 95%Ar reducing atmospheres
Under rise to 1280 DEG C with 9 DEG C/min heating rate, 4h, then furnace cooling are incubated, until being cooled to room temperature；Take out after calcining
Sample regrinding 40min, that is, obtain terbium doped three boric acid lanthanum-strontium base green light fluorescent powder.
Embodiment 5
X=0.10 is taken, by chemical formula Sr3La0.99(BO3)3:0.10Tb stoichiometric, it is accurate respectively with electronic balance
Really weigh SrCO3、La2O3、H3BO3And Tb4O7, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Will
Above-mentioned raw materials are ground after 40min, are loaded corundum crucible, are placed in high temperature process furnances, in 5%H2+ 95%Ar reducing atmospheres
Under rise to 1300 DEG C with 10 DEG C/min heating rate, 5h, then furnace cooling are incubated, until being cooled to room temperature；Take out calcining
Sample regrinding 50min afterwards, that is, obtain terbium doped three boric acid lanthanum-strontium base green light fluorescent powder.
Claims (6)
1. a kind of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder, it is characterised in that with Sr3La(BO3)3For matrix, chemical general formula
For Sr3La1-x(BO3)3:XTb, wherein 0.01≤x≤0.10.
2. a kind of preparation method of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder as claimed in claim 1, it is characterised in that
Specifically implement according to following steps：
Step 1, by chemical general formula Sr3La1-x(BO3)3:XTb mol ratio, wherein 0.01≤x≤0.10, is weighed containing Sr respectively
Compound, compound containing La, boride alloy and compound containing Tb, which contain, is used as raw material；
Step 2, the raw mill for being weighed step 1 are simultaneously well mixed；
Step 3, by well mixed raw material in 5%H2Under+95%Ar reducing atmospheres calcine 3h~5h, temperature be 1250 DEG C~
1300 DEG C, cool to room temperature with the furnace；
Step 4, the calcined product for obtaining step 3 are ground, and obtain terbium doped three boric acid lanthanum-strontium base green light fluorescent powder.
3. the preparation method of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder according to claim 2, it is characterised in that step
Compound containing Sr described in rapid 1 is SrCO3, compound containing La be La2O3, boride alloy be H3BO3And compound containing Tb is
Tb4O7。
4. the preparation method of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder according to claim 3, it is characterised in that step
Milling time described in rapid 2 is 20min~60min.
5. the preparation method of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder according to claim 4, it is characterised in that step
Calcining described in rapid 3 uses SGQ-5-14 tube type resistance furnaces, and heating rate is 8 DEG C/min~10 DEG C/min.
6. the preparation method of terbium doped three boric acid lanthanum-strontium base green light fluorescent powder according to claim 5, it is characterised in that step
Milling time described in rapid 4 is 20min~60min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0358278A1 (en) * | 1988-09-07 | 1990-03-14 | Koninklijke Philips Electronics N.V. | Luminescent terbium-activated borate, luminescent screen provided with such a borate and low-pressure mercury vapour discharge lamp provided with such a screen |
| CN102115667A (en) * | 2009-12-30 | 2011-07-06 | 海洋王照明科技股份有限公司 | Borate green luminescent material and preparation method thereof |
| CN102352246A (en) * | 2011-08-25 | 2012-02-15 | 福建富顺电子有限公司 | High-brightness borate-based green fluorescent powder for white light-emitting diode (LED) and high-temperature reduction preparation method thereof |
| CN102838989A (en) * | 2012-09-25 | 2012-12-26 | 中国地质大学（武汉） | Ultraviolet excited borate-based white fluorescent powder and preparation method thereof |
-
2017
- 2017-05-27 CN CN201710388153.1A patent/CN107033901A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0358278A1 (en) * | 1988-09-07 | 1990-03-14 | Koninklijke Philips Electronics N.V. | Luminescent terbium-activated borate, luminescent screen provided with such a borate and low-pressure mercury vapour discharge lamp provided with such a screen |
| CN102115667A (en) * | 2009-12-30 | 2011-07-06 | 海洋王照明科技股份有限公司 | Borate green luminescent material and preparation method thereof |
| CN102352246A (en) * | 2011-08-25 | 2012-02-15 | 福建富顺电子有限公司 | High-brightness borate-based green fluorescent powder for white light-emitting diode (LED) and high-temperature reduction preparation method thereof |
| CN102838989A (en) * | 2012-09-25 | 2012-12-26 | 中国地质大学（武汉） | Ultraviolet excited borate-based white fluorescent powder and preparation method thereof |
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