CN106381144A - Green phosphor and preparation method thereof - Google Patents
Green phosphor and preparation method thereof Download PDFInfo
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- CN106381144A CN106381144A CN201610804712.8A CN201610804712A CN106381144A CN 106381144 A CN106381144 A CN 106381144A CN 201610804712 A CN201610804712 A CN 201610804712A CN 106381144 A CN106381144 A CN 106381144A
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- emitting phosphor
- green
- phosphate
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- powder
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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
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
- C09K11/7752—Phosphates
- C09K11/7753—Phosphates with alkaline earth metals
Abstract
The invention discloses green phosphor. The chemical characteristic expression is Sr9-xMg1.5(PO4)7:xTb<3+>, wherein x is more than 0 and less than or equal to 0.3. The invention also provides a method for preparing the green phosphor. The method comprises the following steps of: weighing compounds corresponding to Sr, Mg and Tb and phosphate according to a molar ratio, uniformly mixing, grinding for 50-120 minutes, adding the powder into a reaction container, calcining in a high temperature furnace at the temperature of 1100-1300 DEG C in a CO or nitrogen-hydrogen mixed atmosphere for 5-10 hours, naturally cooling, and grinding into powder, thereby obtaining single-matrix phosphate green-emitting phosphor. The phosphor prepared by the method disclosed by the invention is high in quantum efficiency, adjustable in green light and simple in method, and the related process is mature, stable and low in cost.
Description
Technical field
The invention belongs to materialogy field, be related to a kind of rare earth luminescent material, specifically a kind of green emitting phosphor and
Its preparation method.
Background technology
Current energy source problem is severe, and energy-conserving and environment-protective become the major issue of various countries' care, and some countries prohibit the use of and progressively wash in a pan
Eliminate incandescent lamp, promote power saving fluorescent lamp.In recent years, the compact of energy-conservation and straight pipe type fluorescent lamp obtained bigger sending out in China
Exhibition.White light emitting diode (white light-emitting diodes, WLEDs) White-light LED illumination light source and incandescent lamp,
Fluorescent lamp is compared with long service life, efficiency high, anti-adverse environment, spectral region width, visual range be remote, environmental protection is no dirty
Dye, energy-conservation, safety, colour rendering be good, no stroboscopic and the remarkable advantage such as the advantages of small volume, has wide in illumination and display field
Application prospect, be referred to as lighting source of new generation.
RE phosphate material is mainly used as green emitting phosphor and blue colour fluorescent powder at present, also has a small amount of red fluorescence
Powder.Peak luminous wavelength due to green emitting phosphor is almost consistent with the peak wavelength regarding curve of sensitivity, to three primary colors fluorescent powder
Luminous efficiency impact maximum, therefore study the problem that efficient green emitting phosphor is always people's extremely attention.LED green
Fluorescent material is broadly divided into several big systems：Sulphide fluorescent material, aluminate-series fluorescent material, phosphate-based fluorescent material, borate fluorescence
Powder, silicate fluorescent material and silicon substrate nitrogen（Oxygen）Compound system.In all many body system fluorescent material, phosphate is that class luminescent properties are excellent
Good host material, the substitute as aluminate fluorescent powder occurs, and phosphate preparation temperature is lower than aluminate, and particle compares aluminic acid
Salt is thin, and luminosity is high, luminous efficiency is high and physicochemical properties are stable.Instead of aluminates system fluorescent material in Japan simultaneously
It is applied in lamp processed, also have discrete units to be engaged in this pilot study at home, but fail practicality.
Chinese patent " a kind of RE phosphate presoma green emitting phosphor, green emitting phosphor and preparation method thereof "（CN
101767780 A）Disclose a kind of method that liquid phase method prepares novel green fluorescent material, there is provided a kind of heat endurance is good, grain
Spend the preparation method of moderate high-efficiency fluorescence powder, but the problem being primarily present is luminous efficiency, brightness do not reach practical will
Ask, and technique is wayward.
Chinese patent " a kind of RE phosphate green emitting phosphor and preparation method thereof "（CN 105733582 A）Disclose
A kind of preparation method of RE phosphate green emitting phosphor, gained powder has purity height, advantages of good crystallization, epigranular, lights surely
Fixed feature, but fluorescent material quantum efficiency is relatively low, and preparation temperature requires higher.
Content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of green emitting phosphor and preparation method, institute
This green emitting phosphor stated and preparation method will solve green emitting phosphor luminous efficiency of the prior art, brightness does not reach
Real requirement, and the uppity technical problem of technique；Fluorescent material quantum efficiency to be solved relatively low, preparation temperature requires simultaneously
Higher technical problem.
The invention provides a kind of green emitting phosphor, its chemical feature expression formula is Sr9-xMg1.5(PO4)7:xTb3+, wherein
0<x≤0.3.
The invention provides a kind of preparation method of above-mentioned green emitting phosphor, weigh Sr, Mg, Tb according to mol ratio and correspond to
Compound and phosphate, mix, after grinding 50-120min, add a reaction vessel, in 1100-1300 DEG C of CO or
Calcine 5-10 hour, natural cooling grind into powder in the high temperature furnace of nitrogen and hydrogen mixture atmosphere, that is, obtain single matrix phosphate
Green-emitting phosphor, chemical feature expression formula is Sr9-xMg1.5(PO4)7:xTb3+, wherein 0<x≤0.3.
Further, described Sr2+、Mg2+Compound be selected from its carbonate, nitrate, any one in oxide
Plant or more than one combination；Containing PO4 2-Compound be selected from triammonium phosphate, diammonium hydrogen phosphate, appointing in ammonium dihydrogen phosphate
The combination of meaning one or more than one；Containing Tb3+Compound be selected from oxide or nitrate any one.
Phosphate is the good host material of class luminescent properties, and its preparation temperature is low, luminous efficiency is high, physical chemistry
Stable in properties, can effectively absorb UV photon energy.Therefore, for obtaining, synthesis temperature is low, luminous efficiency is high, physical chemistry
Performance is more stable, and the green emitting phosphor of preparation process is simple has very important significance.
The present invention compares with prior art, and its technological progress is significant.The present invention solves fluorescence of the prior art
The relatively low problem of powder quantum efficiency, the fluorescent material quantum efficiency prepared by the method for the present invention is higher, and green glow is adjustable, method letter
Single, related process is ripe, stable, low cost, and the fluorescent material function admirable prepared of the present invention is it is adaptable to batch steady production
Go out fluorescent material product.
Brief description
Fig. 1 is the Sr of the present invention9-xMg1.5(PO4)7: 0.1Tb3+X-ray diffraction spectrogram.
Fig. 2 is the Sr of the present invention9-xMg1.5(PO4)7: 0.3Tb3+Emission spectrum.
Fig. 3 is the Sr of the present invention9-xMg1.5(PO4)7: 0.01Tb3+Chromaticity coordinate figure.
Specific embodiment
Embodiment 1：
A kind of green emitting phosphor Sr9-xMg1.5(PO4)7: xTb3+（x=0.01）Preparation method, comprise the steps：
A. strontium carbonate 3.2032 g, basic magnesium carbonate 0.3446 g, terbium oxide 0.0064 g, ammonium dihydrogen phosphate 0.5602 are weighed
G, is placed in mortar；
B. a gained mixture is ground 50min, be subsequently adding alcohol and grind 60min；
C. b gained mixture is put in crucible boat and crucible is placed in double temperature-area tubular furnaces, 1300 DEG C under CO reducing atmosphere
After calcining 9 hours, natural cooling grind into powder, that is, obtain single matrix phosphate green-emitting phosphor.
Sr9-xMg1.5(PO4)7: xTb3+（x=0.01）Under the exciting of 230nm ultraviolet light, the transmitting main peak of emission spectrum
Positioned at 544nm, green emission is strong and pure.Accompanying drawing 3 is Sr in this embodiment9-xMg1.5(PO4)7: 0.01Tb3+Colourity
Coordinate diagram, as seen from the figure the chromaticity coordinate of prepared green emitting phosphor be（0.271,0.409）.
Embodiment 2：
A kind of green emitting phosphor Sr9-xMg1.5(PO4)7: xTb3+（x=0.05）Preparation method, comprise the steps：
A. strontium carbonate 3.1766 g, basic magnesium carbonate 0.3558 g, terbium nitrate 0.1329 g, ammonium dihydrogen phosphate 0.5790 are weighed
G, is placed in mortar；
B. a gained mixture is ground 120min, be subsequently adding alcohol and grind 50min again；
D. b gained mixture is put into and be placed in crucible boat in double temperature-area tubular furnaces, 1200 DEG C of calcinings under CO reducing atmosphere
After 8 hours, natural cooling grind into powder, that is, obtain single matrix phosphate green-emitting phosphor.
Sr9-xMg1.5(PO4)7: xTb3+（x=0.05）Under the exciting of 230nm ultraviolet light, the transmitting main peak of emission spectrum
Positioned at 544nm, green emission is strong and pure, and the chromaticity coordinate of prepared green emitting phosphor is（0.276,0.423）.
Embodiment 3：
A kind of green emitting phosphor Sr9-xMg1.5(PO4)7: xTb3+（x=0.1）Preparation method, comprise the steps：
A. strontium carbonate 3.1407 g, basic magnesium carbonate 0.3708 g, terbium oxide 0.0693 g, ammonium dihydrogen phosphate 0.6042 are weighed
G, is placed in mortar；
B. a gained mixture is ground 70 min, be subsequently adding acetone and grind 50 min；
C. b gained mixture is put into and be placed in crucible boat in double temperature-area tubular furnaces, 1100 DEG C of calcinings under CO reducing atmosphere
After 10 hours, natural cooling grind into powder.
Accompanying drawing 1 is the X ray diffracting spectrum of this embodiment, and all spectral lines of emission are all and Sr9Mg1.5(PO4)7Standard goes out peak position
Put consistent.The crystal of gained is single Sr9Mg1.5(PO4)7: Tb3+Three square crystals, Tb3+Sr is instead of in crystal3+Position
Put, its structure does not change, without other dephasigns.Sr9-xMg1.5(PO4)7: xTb3+（x=0.1）Swashing in 230nm ultraviolet light
Give, the transmitting main peak of emission spectrum is located at 544nm, green emission is strong and pure, the colourity of prepared green emitting phosphor
Coordinate is（0.278,0.456）.
Embodiment 4：
A kind of green emitting phosphor Sr9-xMg1.5(PO4)7: xTb3+（x=0.2）Preparation method, comprise the steps：
A. strontium 2.0573 g, magnesium carbonate 0.2471 g, terbium oxide 0.0797 g, ammonium dihydrogen phosphate 1.2157 g, are placed in mortar；
B. a gained mixture is ground 110min, be subsequently adding acetone and grind 40min；
C. b gained mixture is put into and be placed in crucible boat in double temperature-area tubular furnaces, 1300 DEG C of calcinings 5 under CO reducing atmosphere
After hour, natural cooling grind into powder, that is, obtain single matrix phosphate green-emitting phosphor.
Sr9-xMg1.5(PO4)7: xTb3+（x=0.2）Under the exciting of 230nm ultraviolet light, the transmitting main peak position of emission spectrum
In 544nm, green emission is strong and pure, and the chromaticity coordinate of prepared green emitting phosphor is（0.281,0.473）.
Embodiment 5：
A kind of green emitting phosphor Sr9-xMg1.5(PO4)7: xTb3+（x=0.3）Preparation method, comprise the steps：
A. strontium carbonate 2.9590 g, magnesium carbonate 0.4024 g, terbium oxide 0.2519 g, ammonium dihydrogen phosphate 0.7319 g, are placed in and grind
In alms bowl；
B. a gained mixture is ground 120min, be subsequently adding acetone and grind 60min；
C. b gained mixture is put into and be placed in crucible boat in double temperature-area tubular furnaces, 1300 DEG C of calcinings 6 under CO reducing atmosphere
After hour, natural cooling grind into powder, that is, obtain single matrix phosphate green-emitting phosphor.
Accompanying drawing 2 is Sr in this embodiment9-xMg1.5(PO4)7: 0.3Tb3+Emission spectrum, in exciting of 230nm ultraviolet light
Under, there is very high luminous intensity, obtain the fluorescent material that launch wavelength is 545nm.The chromaticity coordinate of prepared green emitting phosphor
For（0.283,0.491）.
Claims (3)
1. a kind of green emitting phosphor it is characterised in that：Chemical feature expression formula is Sr9-xMg1.5(PO4)7:xTb3+, wherein 0<x≤
0.3.
2. a kind of green emitting phosphor described in claim 1 preparation method it is characterised in that：According to mol ratio weigh Sr, Mg,
The corresponding compound of Tb and phosphate, mix, and add a reaction vessel, at 1100-1300 DEG C after grinding 50-120min
CO or nitrogen and hydrogen mixture atmosphere high temperature furnace in calcine 5-10 hour, natural cooling grind into powder, that is, obtain single matrix
Phosphate green-emitting phosphor, chemical feature expression formula is Sr9-xMg1.5(PO4)7:xTb3+, wherein 0<x≤0.3.
3. a kind of green emitting phosphor according to claim 2 preparation method it is characterised in that：Described Sr2+、Mg2+'s
Compound is selected from its carbonate, nitrate, any one or more than one combination in oxide；Containing PO4 2-Chemical combination
Thing is selected from triammonium phosphate, diammonium hydrogen phosphate, any one or more than one combination in ammonium dihydrogen phosphate；Containing Tb3+'s
Compound is selected from any one in oxide or nitrate.
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| CN201610804712.8A CN106381144B (en) | 2016-09-06 | 2016-09-06 | A kind of green emitting phosphor and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587622A (en) * | 2018-05-03 | 2018-09-28 | 惠州学院 | A kind of improved green phosphor for white light LED |
Citations (5)
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|---|---|---|---|---|
| CN101818064A (en) * | 2010-03-12 | 2010-09-01 | 兰州大学 | Vacuum ultraviolet-excited green light emitting material |
| WO2014133374A1 (en) * | 2013-02-28 | 2014-09-04 | Vilnius University | Solid-state sources of light for preferential colour rendition |
| CN105018085A (en) * | 2015-07-02 | 2015-11-04 | 沈阳师范大学 | Rare earth-doped phosphate phosphor used for UV-LED and preparation method thereof |
| CN105087003A (en) * | 2015-09-02 | 2015-11-25 | 中国科学院长春应用化学研究所 | Orange LED fluorescent powder as well as preparation method and application thereof |
| CN105131951A (en) * | 2015-09-02 | 2015-12-09 | 中国科学院长春应用化学研究所 | Red light LED fluorescent powder and preparation method and application thereof |
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2016
- 2016-09-06 CN CN201610804712.8A patent/CN106381144B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101818064A (en) * | 2010-03-12 | 2010-09-01 | 兰州大学 | Vacuum ultraviolet-excited green light emitting material |
| WO2014133374A1 (en) * | 2013-02-28 | 2014-09-04 | Vilnius University | Solid-state sources of light for preferential colour rendition |
| CN105018085A (en) * | 2015-07-02 | 2015-11-04 | 沈阳师范大学 | Rare earth-doped phosphate phosphor used for UV-LED and preparation method thereof |
| CN105087003A (en) * | 2015-09-02 | 2015-11-25 | 中国科学院长春应用化学研究所 | Orange LED fluorescent powder as well as preparation method and application thereof |
| CN105131951A (en) * | 2015-09-02 | 2015-12-09 | 中国科学院长春应用化学研究所 | Red light LED fluorescent powder and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| WENZHI SUN等: "Sr9Mg1.5(PO4)7:Eu2+: A Novel Broadband Orange-Yellow-Emitting Phosphor for Blue Light-Excited Warm White LEDs", 《ACS APPL. MATER. INTERFACES》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587622A (en) * | 2018-05-03 | 2018-09-28 | 惠州学院 | A kind of improved green phosphor for white light LED |
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Granted publication date: 20181012 Termination date: 20210906 |