CN107033900A - Three boric acid lanthanum-strontium base green light fluorescent powders of a kind of europium doping and preparation method thereof - Google Patents

Three boric acid lanthanum-strontium base green light fluorescent powders of a kind of europium doping and preparation method thereof Download PDF

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Publication number
CN107033900A
CN107033900A CN201710388048.8A CN201710388048A CN107033900A CN 107033900 A CN107033900 A CN 107033900A CN 201710388048 A CN201710388048 A CN 201710388048A CN 107033900 A CN107033900 A CN 107033900A
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boric acid
green light
acid lanthanum
europium
light fluorescent
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武秀兰
焦叶辉
任强
海鸥
林飞
李欢欢
白文妮
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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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
    • 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
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7797—Borates

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses a kind of europium three boric acid lanthanum-strontium base green light fluorescent powders of doping, with Sr3La(BO3)3For matrix, chemical general formula is Sr3‑xLa(BO3)3:XEu, wherein 0.02≤x≤0.20, passes through the active ions Eu that adulterates3+Prepare europium three boric acid lanthanum-strontium base green light fluorescent powders of doping, excite lower acquisition main peak to be located at the feux rouges near 615nm near ultraviolet and blue light, be adapted near ultraviolet or blue light is excited, transmitting peak position is located at 594nm, 615nm, 625nm, 709nm respectively, chromaticity coordinates is located at red light region, chemical property is stable, good luminous performance, and luminous intensity is high, 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 Eu2O3Calcined under mixed grinding, air atmosphere, insulation is ground again after furnace cooling, europium three boric acid lanthanum-strontium base green light fluorescent powders of doping are finally obtained, are 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

Three boric acid lanthanum-strontium base green light fluorescent powders of a kind of europium doping and preparation method thereof
Technical field
The invention belongs to LED fluorescent material preparing technical fields, and in particular to a kind of three boric acid lanthanum-strontium base green glows of europium doping Fluorescent material, the preparation method for the three boric acid lanthanum-strontium base green light fluorescent powders that adulterated the invention further relates to the europium.
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 green glow 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 green glow, green glow, 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, colour rendering is good.Eu3+Through frequently as a kind of feux rouges The activator of transmitting, can excite lower acquisition main peak to be located near 615nm near ultraviolet (395nm) and blue light (465nm) and light by force The degree relatively higher feux rouges of strong, excitation.Eu3+The transmitting light of doping fluorescent powder can as white light LEDs red color components.Therefore, Research can effectively be excited by near ultraviolet, blue light, the europium doping three boric acid lanthanum-strontium base red light fluorescent powders tool that luminous intensity is high, purity is good There is good actual application value.
The content of the invention
It is an object of the invention to provide a kind of europium three boric acid lanthanum-strontium base green light fluorescent powders of doping, 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 europium three boric acid lanthanum-strontium base green light fluorescent powders of doping.
The technical solution adopted in the present invention is, with Sr3La(BO3)3For matrix, chemical general formula is Sr3-xLa(BO3)3: XEu, wherein 0.02≤x≤0.20.
Another technical scheme of the present invention is, a kind of europium adulterates the preparations of three boric acid lanthanum-strontium base green light fluorescent powders Method, it is characterised in that specifically implement according to following steps：
Step 1, by chemical general formula Sr3-xLa(BO3)3:XEu mol ratio, wherein 0.02≤x≤0.20, is weighed respectively Compound containing Sr, compound containing La, boride alloy and compound containing Eu, which contain, is used as raw material；
Step 2, the raw mill for being weighed step 1 are simultaneously well mixed；
Step 3, well mixed raw material is calcined to 3h~5h in air atmosphere, temperature is 1250 DEG C~1300 DEG C, with Stove is cooled to room temperature；
Step 4, the calcined product for obtaining step 3 are ground, and obtain europium three boric acid lanthanum-strontium base green light fluorescent powders of doping.
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 Eu Thing is Eu2O3。
Milling time is 20min~60min in step 2.
Calcining is rapidly heated resistance furnace using SX3-10-14 types in step 3, and heating rate is 5 DEG C/min~10 DEG C/min.
Milling time is 20min~60min in step 4.
The beneficial effects of the invention are as follows three boric acid lanthanum-strontium base green light fluorescent powders of europium doping 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 Eu that adulterates3+, europium three boric acid lanthanum-strontium base green light fluorescent powders of doping are prepared, is adapted near ultraviolet and swashs Hair, excites lower acquisition main peak to be located at luminous intensity relatively strong, excitation near 615nm near ultraviolet (395nm) and blue light (465nm) Higher feux rouges, is adapted near ultraviolet or blue light is excited, and transmitting peak position is located at 594nm, 615nm, 625nm, 709nm respectively, and color is sat Mark is in red light region (x=0.642, y=0.357), and this connects very much with NTSC standard chromaticity coordinates (x=0.63, y=0.34) Closely, the light emitting diode near ultraviolet chip and blue chip is matched, and illustrates that fluorescent material prepared by the present invention is a kind of photism The excellent red fluorescent powder for white radiation LED of energy；
The preparation method of three boric acid lanthanum-strontium base green light fluorescent powders of europium doping of the present invention, is prepared based on solid-phase synthesis, grasped The property made is strong, prepares in air atmosphere, 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 prepared2.96La(BO3)3:0.04Eu 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 prepared2.92La(BO3)3:The excitation spectrum and emission spectrum of 0.08Eu fluorescent material.
Fig. 3 is the Sr that embodiment 3 is prepared2.92La(BO3)3:The CIE chromaticity coordinates figures of 0.08Eu fluorescent material.
Embodiment
A kind of europium of the invention is adulterated with reference to the accompanying drawings and detailed description three boric acid lanthanum-strontium base green light fluorescent powders and Its preparation method is described in detail.
The present invention three boric acid lanthanum-strontium base green light fluorescent powders of a kind of europium doping, with Sr3La(BO3)3For matrix, chemical general formula is Sr3-xLa(BO3)3:XEu, wherein 0.02≤x≤0.20.
The preparation method of three boric acid lanthanum-strontium base green light fluorescent powders of a kind of europium doping, it is characterised in that specifically according to following step It is rapid to implement：
Step 1, by chemical general formula Sr3-xLa(BO3)3:XEu mol ratio, wherein 0.02≤x≤0.20, is weighed respectively SrCO3、La2O3、H3BO3And Eu2O3It is used as raw material；
Step 2, the raw mill 20min~60min for being weighed step 1 are simultaneously well mixed；
Step 3, well mixed raw material is placed in SX3-10-14 types be rapidly heated in resistance furnace, forge in air atmosphere 3h~5h is burnt, temperature is 1250 DEG C~1300 DEG C, cools to room temperature with the furnace；
Wherein, synthesized during calcining according to following chemical equation：
(3-x)SrCO3+1/2La2O3+3H3BO3+x/2Eu2O3→Sr3-xLa(BO3)3:xEu+9/2H2O+3CO2
Step 4, the calcined product for obtaining step 3 grind 20min~60min, obtain europium three boric acid lanthanum-strontium bases of doping green Emitting phosphor.
Embodiment 1
X=0.02 is taken, by chemical formula Sr2.98La(BO3)3:0.02Eu stoichiometric, it is accurate respectively with electronic balance Really weigh SrCO3、La2O3、H3BO3And Eu2O3, 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 SX3-10-14 types and are rapidly heated in resistance furnace, in air gas Calcined under atmosphere and rise to 1250 DEG C with 5 DEG C/min heating rate, be incubated 3h, then furnace cooling, until being cooled to room temperature；Take out Sample regrinding 20min after calcining, that is, obtain europium three boric acid lanthanum-strontium base green light fluorescent powders of doping.
Embodiment 2
X=0.04 is taken, by chemical formula Sr2.96La(BO3)3:0.04Eu stoichiometric, it is accurate respectively with electronic balance Really weigh SrCO3、La2O3、H3BO3And Eu2O3, 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 30min, are loaded corundum crucible, are placed in SX3-10-14 types and are rapidly heated in resistance furnace, in air gas Calcined under atmosphere and rise to 1270 DEG C with 6 DEG C/min heating rate, be incubated 4h, then furnace cooling, until being cooled to room temperature；Take out Sample regrinding 50min after calcining, that is, obtain europium three boric acid lanthanum-strontium base green light fluorescent powders of doping.
Fig. 1 is Sr prepared by the present embodiment 22.96La(BO3)3:0.04Eu 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=0.08 is taken, by chemical formula Sr2.92La(BO3)3:0.08Eu stoichiometric, it is accurate respectively with electronic balance Really weigh SrCO3、La2O3、H3BO3And Eu2O3, 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 SX3-10-14 types and are rapidly heated in resistance furnace, in air gas Calcined under atmosphere and rise to 1300 DEG C with 10 DEG C/min heating rate, be incubated 5h, then furnace cooling, until being cooled to room temperature；Take The sample regrinding 60min gone out after calcining, that is, obtain europium three boric acid lanthanum-strontium base green light fluorescent powders of doping.
Fig. 2 is Sr prepared by embodiment 32.92La(BO3)3:The excitation spectrum and emission spectrum of 0.08Eu fluorescent material.This is glimmering The excitation spectrum of light powder in 330nm~500nm, main excitation peak near 393nm, its emission spectrum in 550nm~730nm, Launch peak position and be located at 594nm, 615nm, 625nm, 709nm respectively, main peak is near 615nm.As can be seen here, the fluorescent material can quilt Black light effectively excites and sends feux rouges, can be applied to white light LEDs.
Fig. 3 is Sr prepared by embodiment 32.92La(BO3)3:The CIE chromaticity coordinates figures of 0.08Eu fluorescent material.Chromaticity coordinates is located at red Light region (x=0.642, y=0.357), illustrates that fluorescent material prepared by the present invention is a kind of red fluorescence of good luminescence property Powder.
Embodiment 4
X=0.15 is taken, by chemical formula Sr2.85La(BO3)3:0.15Eu stoichiometric, it is accurate respectively with electronic balance Really weigh SrCO3、La2O3、H3BO3And Eu2O3, 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 SX3-10-14 types and are rapidly heated in resistance furnace, in air gas Calcined under atmosphere and rise to 1280 DEG C with 9 DEG C/min heating rate, be incubated 4h, then furnace cooling, until being cooled to room temperature；Take out Sample regrinding 40min after calcining, that is, obtain europium three boric acid lanthanum-strontium base green light fluorescent powders of doping.
Embodiment 5
X=0.20 is taken, by chemical formula Sr2.80La(BO3)3:0.20Eu stoichiometric, it is accurate respectively with electronic balance Really weigh SrCO3、La2O3、H3BO3And Eu2O3, 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 45min, are loaded corundum crucible, are placed in SX3-10-14 types and are rapidly heated in resistance furnace, in air gas Calcined under atmosphere and rise to 1300 DEG C with 10 DEG C/min heating rate, be incubated 5h, then furnace cooling, until being cooled to room temperature；Take The sample regrinding 45min gone out after calcining, that is, obtain europium three boric acid lanthanum-strontium base green light fluorescent powders of doping.

Claims (6)

  1. The three boric acid lanthanum-strontium base green light fluorescent powders 1. a kind of europium adulterates, it is characterised in that with Sr3La(BO3)3For matrix, chemical general formula For Sr3-xLa(BO3)3:XEu, wherein 0.02≤x≤0.20.
  2. The preparation method of three boric acid lanthanum-strontium base green light fluorescent powders 2. a kind of europium as claimed in claim 1 adulterates, it is characterised in that Specifically implement according to following steps：
    Step 1, by chemical general formula Sr3-xLa(BO3)3:XEu mol ratio, wherein 0.02≤x≤0.20, is weighed containing Sr respectively Compound, compound containing La, boride alloy and compound containing Eu, which contain, is used as raw material；
    Step 2, the raw mill for being weighed step 1 are simultaneously well mixed；
    Step 3, well mixed raw material is calcined to 3h~5h in air atmosphere, temperature is 1250 DEG C~1300 DEG C, cold with stove But to room temperature；
    Step 4, the calcined product for obtaining step 3 are ground, and obtain europium three boric acid lanthanum-strontium base green light fluorescent powders of doping.
  3. The preparation method of three boric acid lanthanum-strontium base green light fluorescent powders 3. europium according to claim 2 adulterates, 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 Eu is Eu2O3。
  4. The preparation method of three boric acid lanthanum-strontium base green light fluorescent powders 4. europium according to claim 3 adulterates, it is characterised in that step Milling time described in rapid 2 is 20min~60min.
  5. The preparation method of three boric acid lanthanum-strontium base green light fluorescent powders 5. europium according to claim 4 adulterates, it is characterised in that step Calcining described in rapid 3 is rapidly heated resistance furnace using SX3-10-14 types, and heating rate is 5 DEG C/min~10 DEG C/min.
  6. The preparation method of three boric acid lanthanum-strontium base green light fluorescent powders 6. europium according to claim 5 adulterates, it is characterised in that step Milling time described in rapid 4 is 20min~60min.
CN201710388048.8A 2017-05-27 2017-05-27 Three boric acid lanthanum-strontium base green light fluorescent powders of a kind of europium doping and preparation method thereof Pending CN107033900A (en)

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CN109021972A (en) * 2018-05-31 2018-12-18 杭州电子科技大学 A kind of white light LEDs borate blue fluorescent powder and preparation method thereof
CN109021976A (en) * 2018-09-21 2018-12-18 陕西科技大学 Three strontium yttrium borate base red fluorescent powders of a kind of europium doping and preparation method thereof
CN109181694A (en) * 2018-09-21 2019-01-11 陕西科技大学 Three strontium yttrium borate base blue colour fluorescent powders of a kind of divalent europium doping and preparation method thereof
CN114686225A (en) * 2020-12-25 2022-07-01 中国科学院江西稀土研究院 Near-infrared fluorescent powder and preparation method and application thereof

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CN109181694A (en) * 2018-09-21 2019-01-11 陕西科技大学 Three strontium yttrium borate base blue colour fluorescent powders of a kind of divalent europium doping and preparation method thereof
CN114686225A (en) * 2020-12-25 2022-07-01 中国科学院江西稀土研究院 Near-infrared fluorescent powder and preparation method and application thereof

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Application publication date: 20170811