CN108659825A - A kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof - Google Patents
A kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof Download PDFInfo
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- CN108659825A CN108659825A CN201810641808.6A CN201810641808A CN108659825A CN 108659825 A CN108659825 A CN 108659825A CN 201810641808 A CN201810641808 A CN 201810641808A CN 108659825 A CN108659825 A CN 108659825A
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- 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7734—Aluminates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a kind of white light LEDs silicate single-substrate white emitting fluorescent powders and preparation method thereof, which is characterized in that includes the following steps：S1. raw material are chosen and accurately weigh raw material according to stoicheiometry：BaCO3, CaCO3, SiO2, ZnO, Eu2O3, MnCO3, La2O3, Sm2O3, BaCl22H2O；S2. load weighted raw material are placed in mortar and are ground, be uniformly mixed addition absolute ethyl alcohol and further grind；S3. with the micro- dry abrasive material mortar of absolute ethyl alcohol will be put into vacuum drying chamber dry half an hour；S4. removing pharmaceutical producs mortar, by mixture scrape and it is finely ground after be fitted into calcination kettle；S5. it is placed in tube furnace, heats up in calcination kettle；S6. nitrogen and hydrogen are opened and roasts sample as reducing atmosphere；S7. persistently overheating, it is then down to room temperature automatically；S8. silicate single-substrate white emitting fluorescent powder is obtained after ball milling, washing, drying.Invention has the characteristics that safe and pollution-free, simple production process, at low cost, easy temperature control system, can guarantee to form good crystal structure.
Description
Technical field
The present invention relates to phosphor technologies field more particularly to a kind of white light LEDs silicate single-substrate white emitting fluorescent powders
And preparation method thereof.
Background technology
Fluorescent powder is commonly called as luminescent powder, is generally divided into two class of photo-induced energy storage luminescent powder and luminescent powder with radionuclide.It is photic
Energy storage luminescent powder is fluorescent powder after by irradiations such as natural light, daylight light, ultraviolet lights, and luminous energy is stored, is being stopped
It after light irradiation, then slowly releases in a manner of fluorescence, so at night or dark, remains to see luminous, continue
Time is up to a few houres to ten a few houres.
In real life, using the characteristic that luminescent powder is luminous for a long time, weak illumination light source is made, in military service in people
There is special use, this material is coated in instrument, clock and watch, window, various switch signs on machine, the handle etc. of door
Place, it is also possible to which various light-passing plastics are pressed into various symbols, component, articles for use (such as power switch, socket, fishhook) together.
These luminous components get up etc. it still in continuous illumination, keep people distinguishable not after light irradiates after night or accidental power failure, lightning
Peripheral direction, to work and life is brought convenience.Noctilucent material ultrafine particle is mixed in textile, keeps color more bright-coloured, it is small
There is the textile of noctilucence in child wear, traffic accident can be reduced.
The prior art is mostly using three primary colours [blue, red and green (yellow) fluorescent powder, since it is optional glimmering
Light powder type is more, and the white light LEDs of different-colour are adjusted out in the proportioning for changing three primary colours, and flexibility greatly improves.It loses
Regret be three primary colours proportioning adjusting difficulty it is larger, there are feux rouges or green lights to the re-absorption phenomenon of blue light, and for purple light
The defects of rouge and powder of activation is less efficient.However, single-substrate white or single sintering multiphase white emitting fluorescent powder can be good at gram
Take this defect.
Invention content
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of white light LEDs silicic acid proposed
Salt single-substrate white fluorescent powder and preparation method thereof.
To achieve the goals above, present invention employs following technical solutions：
A kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof, which is characterized in that including following step
Suddenly：S1. raw material are chosen and accurately weigh raw material according to stoicheiometry：BaCO3, CaCO3, SiO2, ZnO, Eu2O3,
MnCO3, La2O3, Sm2O3, BaCl22H2O；S2. load weighted raw material are placed in mortar and are ground, be uniformly mixed and be added
Absolute ethyl alcohol is further ground；S3. it is small dry half will to be put into vacuum drying chamber with the micro- dry abrasive material mortar of absolute ethyl alcohol
When；S4. removing pharmaceutical producs mortar, by mixture scrape and it is finely ground after be fitted into calcination kettle；S5. it is placed in tube furnace in calcination kettle,
Heating；S6. nitrogen and hydrogen are opened and roasts sample as reducing atmosphere；S7. persistently overheating, it is then down to room temperature automatically；S8. it passes through
Silicate single-substrate white emitting fluorescent powder is obtained after crossing ball milling, washing, drying.
Preferably, in the S1, each raw material proportioning calculating is carried out by its molecular composition, i.e.,：BaCO3:CaCO3:ZnO:
Eu2O3:MnCO3:Re2O3:SiO2 molar ratios are 1.3:(0.46-x):0.2:(0.02/2):0.02:(x/2):1.
Preferably, in the S8, silicate single-substrate white emitting fluorescent powder chemical equation structure is Ba1.3Ca0.46-x
Zn0.2SiO4:0.02Eu2+, excitation spectrum are wide range wavestrip of the wave-length coverage in 320~450nm.
Preferably, in the S2, grinding body is preferably agate mortar, grinds 15-30min.
Preferably, in the S4, calcination kettle is preferably porcelain pot.
Preferably, in the S6, after temperature reaches 300-600 DEG C, nitrogen and hydrogen are opened.
Preferably, in the S7, temperature is kept for 1-3 hours at 800-1200 DEG C.
Preferably, in the S8, ball milling is preferably hyperfine sphere grinding machine, and washing preferably first washing and pickling are done
Dry process is carried out in dryer at 60-80 DEG C.
Preferably, it is needed to take different x values (x=2%~12%) according to actual conditions.
Preferably, in the S2, use the BaCl22H2O of 2-10% (molar ratio) as fluxing agent.
Compared with prior art, the beneficial effects of the invention are as follows：
1. the present invention is preferably agate mortar by grinding body, calcination kettle is preferably porcelain pot so that in production process, product
It will not be chemically contaminated, will not be oxidized, substantially increase the quality and purity of product.
2. Ba1.3Ca0.46-x Zn0.2SiO4 of the present invention:0.02Eu2+ luminous intensities are strong, and colour rendering index is relatively high.
3. the present invention has the characteristics that safe and pollution-free, simple production process, at low cost, easy temperature control system can guarantee shape
At good crystal structure.
In the present invention, it is not directed to part in the device and is the same as those in the prior art or can be realized by using the prior art,
The present invention has the characteristics that safe and pollution-free, simple production process, at low cost, easy temperature control system, can guarantee to form good crystalline substance
Body structure.
Description of the drawings
Fig. 1 is a kind of swashing for white light LEDs silicate single-substrate white emitting fluorescent powder proposed by the present invention and preparation method thereof
The structural schematic diagram for the emission spectrum given.
Fig. 2 is a kind of swashing for white light LEDs silicate single-substrate white emitting fluorescent powder proposed by the present invention and preparation method thereof
The structural schematic diagram for the emission spectrum given.
Fig. 3 is a kind of XRD of white light LEDs silicate single-substrate white emitting fluorescent powder proposed by the present invention and preparation method thereof
The structural schematic diagram of collection of illustrative plates.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that, term "upper", "lower", "front", "rear", "left", "right", "top",
The orientation or positional relationship of the instructions such as "bottom", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, merely to just
In the description present invention and simplify description, do not indicate or imply the indicated device or element must have a particular orientation, with
Specific azimuth configuration and operation, therefore be not considered as limiting the invention.
Embodiment 1：
A kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof, which is characterized in that including following step
Suddenly：S1. raw material are chosen and accurately weigh raw material according to stoicheiometry：BaCO3, CaCO3, SiO2, ZnO, Eu2O3,
MnCO3, La2O3, Sm2O3, BaCl22H2O；S2. load weighted raw material are placed in mortar and are ground, be uniformly mixed and be added
Absolute ethyl alcohol is further ground；S3. it is small dry half will to be put into vacuum drying chamber with the micro- dry abrasive material mortar of absolute ethyl alcohol
When；S4. removing pharmaceutical producs mortar, by mixture scrape and it is finely ground after be fitted into calcination kettle；S5. it is placed in tube furnace in calcination kettle,
Heating；S6. nitrogen and hydrogen are opened and roasts sample as reducing atmosphere；S7. persistently overheating, it is then down to room temperature automatically；S8. it passes through
Silicate single-substrate white emitting fluorescent powder is obtained after crossing ball milling, washing, drying.
In the S1, each raw material proportioning calculating is carried out by its molecular composition, i.e.,：BaCO3:CaCO3:ZnO:Eu2O3:
MnCO3:Re2O3:SiO2 molar ratios are,
1.3:(0.46-x):0.2:(0.02/2):0.02:(x/2):1。
In the S8, silicate single-substrate white emitting fluorescent powder chemical equation structure is Ba1.3Ca0.46-x Zn0.2SiO4:
0.02Eu2+, excitation spectrum are wide range wavestrip of the wave-length coverage in 320~450nm.
In the S2, grinding body is preferably agate mortar, grinds 20min.
In the S4, calcination kettle is preferably porcelain pot.
In the S6, after temperature reaches 350 DEG C, nitrogen and hydrogen are opened.
In the S7, temperature is kept for 1 hour at 900 DEG C.
In the S8, ball milling is preferably hyperfine sphere grinding machine, and preferably first washing and pickling, drying process are for washing
It is carried out in dryer at 65 DEG C.
It is needed to take different x values (x=6%) according to actual conditions.
In the S2, use the BaCl22H2O of 6% (molar ratio) as fluxing agent.
In order to improve luminous intensity, we tried to replace Ca with Zn on former Research foundation.Ba1.3Ca0.68-
xZnxSiO4:The excitation spectrum and emission spectrum of 0.02Eu2+ (x=0.1~0.68) is respectively such as Fig. 3 .2a, (λ em=shown in b
460nm, λ ex=365nm).Fig. 1 shows that the excitation spectrum of the fluorescent powder of preparation is width of the wave-length coverage in 320~450nm
Wavestrip is composed, excitation band broadens after adding Zn2+, in especially 330~420nm wave-length coverages.They illustrate that ultraviolet light can be had
Effect absorbs, and wherein maximum excitation wavelength is located at 368nm.Show as feature jumps of the Eu2+ in silicate substrate between 4f-5d configurations
Move excitation peak.Match with purple light for InGaN chip (340~420nm).
Fig. 2 is Ba1.3Ca0.68-xZnxSiO4:0.02Eu2+ (x=0.1~0.68) is under 365nm ultraviolet excitations
Emission spectrum.As can be seen from Figure, the addition of Zn2+ effectively enhances the luminous intensity of green light band.With Zn2+ ion concentrations
Increase, the emission peak positions of sample are substantially change, and emissive porwer increases.As x=0.1~0.4, emission spectrum covering
The blue-green wavestrip of 430~560nm, maximum emission wavelength 460nm and 500nm, curve are in mal-distribution, belong to Eu2+ and take
For the 5d-4f transition characteristics transmitting of Ba2+ (Ca2+) case；With the increase of x, 504nm transmitting peak intensities gradually increase, 460nm
Transmitting peak intensity gradually weakens, and as x=0.5~0.68, emission spectrum covers the green wavestrip of 450~560nm, emission maximum
Wavelength 504nm, belongs to the 5d-4f transition characteristics transmitting of Eu2+ substitution Ba2+ (Zn2+) cases, and transmitting peak intensity is dense with Zn2+
The increase of degree gradually increases.Electromagnetic radiation peak intensity is more than Ba1.98SiO4 when x=0.68:The transmitting peak intensity of 0.02Eu2+.
The luminescent properties of Eu2+ and host crystal structure are closely related, and multiple cases of alkali metal cation provide for luminescent center ion
Different case environment.
Embodiment 2：
A kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof, which is characterized in that including following step
Suddenly：S1. raw material are chosen and accurately weigh raw material according to stoicheiometry：BaCO3, CaCO3, SiO2, ZnO, Eu2O3,
MnCO3, La2O3, Sm2O3, BaCl22H2O；S2. load weighted raw material are placed in mortar and are ground, be uniformly mixed and be added
Absolute ethyl alcohol is further ground；S3. it is small dry half will to be put into vacuum drying chamber with the micro- dry abrasive material mortar of absolute ethyl alcohol
When；S4. removing pharmaceutical producs mortar, by mixture scrape and it is finely ground after be fitted into calcination kettle；S5. it is placed in tube furnace in calcination kettle,
Heating；S6. nitrogen and hydrogen are opened and roasts sample as reducing atmosphere；S7. persistently overheating, it is then down to room temperature automatically；S8. it passes through
Silicate single-substrate white emitting fluorescent powder is obtained after crossing ball milling, washing, drying.
In the S1, each raw material proportioning calculating is carried out by its molecular composition, i.e.,：BaCO3:CaCO3:ZnO:Eu2O3:
MnCO3:Re2O3:SiO2 molar ratios are,
1.3:(0.46-x):0.2:(0.02/2):0.02:(x/2):1。
In the S8, silicate single-substrate white emitting fluorescent powder chemical equation structure is Ba1.3Ca0.46-x Zn0.2SiO4:
0.02Eu2+, excitation spectrum are wide range wavestrip of the wave-length coverage in 320~450nm.
In the S2, grinding body is preferably agate mortar, grinds 25min.
In the S4, calcination kettle is preferably porcelain pot.
In the S6, after temperature reaches 500 DEG C, nitrogen and hydrogen are opened.
In the S7, temperature is kept for 3 hours at 850 DEG C.
In the S8, ball milling is preferably hyperfine sphere grinding machine, and preferably first washing and pickling, drying process are for washing
It is carried out in dryer at 75 DEG C.
It is needed to take different x values (x=10%) according to actual conditions.
In the S2, use the BaCl22H2O of 5.5% (molar ratio) as fluxing agent.
Ba1.3Ca0.5-x-yZn0.2SiO4:The crystal phase structure of xEu2+, yMn2+ are analyzed：
Fig. 3 is Ba1.3Ca0.46Zn0.2SiO4:The XRD spectrum of 0.02Eu2+, 0.02Mn2+ system, by with JCPDS#
48-0210 standard cards compare, and can be good at matching, and illustrate that the sample of synthesis is Ba1.3Ca0.7SiO4 crystal phase structures, few
The doping of amount Eu2+, Mn2+ do not generate dephasign.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof, which is characterized in that including following step
Suddenly：
S1. raw material are chosen and accurately weigh raw material according to stoicheiometry：BaCO3, CaCO3, SiO2, ZnO, Eu2O3, MnCO3,
La2O3, Sm2O3, BaCl2·2H2O。
S2. load weighted raw material are placed in mortar and are ground, be uniformly mixed addition absolute ethyl alcohol and further grind.
S3. with the micro- dry abrasive material mortar of absolute ethyl alcohol will be put into vacuum drying chamber dry half an hour.
S4. removing pharmaceutical producs mortar, by mixture scrape and it is finely ground after be fitted into calcination kettle.
S5. it is placed in tube furnace, heats up in calcination kettle.
S6. nitrogen and hydrogen are opened and roasts sample as reducing atmosphere.
S7. persistently overheating, it is then down to room temperature automatically.
S8. silicate single-substrate white emitting fluorescent powder is obtained after ball milling, washing, drying.
2. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof according to claim 1, special
Sign is, in the S1, carries out each raw material proportioning calculating by its molecular composition, i.e.,：BaCO3:CaCO3:ZnO:Eu2O3:MnCO3:
Re2O3:SiO2Molar ratio is 1.3:(0.46-x):0.2:(0.02/2):0.02:(x/2):1.
3. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof according to claim 1, special
Sign is, in the S8, silicate single-substrate white emitting fluorescent powder chemical equation structure is Ba1.3Ca0.46-x Zn0.2SiO4:
0.02Eu2+, excitation spectrum are wide range wavestrip of the wave-length coverage in 320~450nm.
4. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof according to claim 1, special
Sign is, in the S2, grinding body is preferably agate mortar, grinds 15-30min.
5. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof according to claim 1, special
Sign is, in the S4, calcination kettle is preferably porcelain pot.
6. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof according to claim 1, special
Sign is, in the S6, after temperature reaches 300-600 DEG C, opens nitrogen and hydrogen.
7. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof according to claim 1, special
Sign is, in the S7, temperature is kept for 1-3 hours at 800-1200 DEG C.
8. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof according to claim 1, special
Sign is, in the S8, ball milling is preferably hyperfine sphere grinding machine, and preferably first washing and pickling, drying process are for washing
It is carried out in dryer at 60-80 DEG C.
9. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof according to claim 2, special
Sign is, is needed to take different x values (x=2%~12%) according to actual conditions.
10. a kind of white light LEDs silicate single-substrate white emitting fluorescent powder and preparation method thereof according to claim 1,
It is characterized in that, in the S2, uses the BaCl22H2O of 2-10% (molar ratio) as fluxing agent.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101868515A (en) * | 2007-11-22 | 2010-10-20 | 默克专利有限公司 | Surface-modified phosphors |
| JP4661419B2 (en) * | 2005-07-14 | 2011-03-30 | 三菱化学株式会社 | Phosphor and light emitting device using the same |
-
2018
- 2018-06-21 CN CN201810641808.6A patent/CN108659825A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4661419B2 (en) * | 2005-07-14 | 2011-03-30 | 三菱化学株式会社 | Phosphor and light emitting device using the same |
| CN101868515A (en) * | 2007-11-22 | 2010-10-20 | 默克专利有限公司 | Surface-modified phosphors |
Non-Patent Citations (3)
| Title |
|---|
| WENZHEN LV ET AL.,: ""Ba1.3Ca0.7SiO4:Eu2+,Mn2+: A Promising Single-Phase, Color-Tunable Phosphor for Near-Ultraviolet White-Light-Emitting Diodes"", 《INORGANIC CHEMISTRY》 * |
| 陈永杰 等: ""单一基质白光荧光粉Ba1.31Ca0.64-xSiO4:0.02Eu2+,0.03Mn2+,xRe3+( Re3+=La3+,Sm3+)的研究"", 《沈阳化工大学学报》 * |
| 陈琳 等: ""蓝绿色荧光粉Ba1.3Ca0.7-x-yZnxSiO4:yEu2+的晶体结构和光谱性能"", 《硅酸盐学报》 * |
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Application publication date: 20181016 |