CN105038787A - Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder and preparation method thereof - Google Patents
Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder and preparation method thereof Download PDFInfo
- Publication number
- CN105038787A CN105038787A CN201510376253.3A CN201510376253A CN105038787A CN 105038787 A CN105038787 A CN 105038787A CN 201510376253 A CN201510376253 A CN 201510376253A CN 105038787 A CN105038787 A CN 105038787A
- Authority
- CN
- China
- Prior art keywords
- coactivated
- terbium
- temperature
- phosphor powder
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention discloses Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder. A general formula of the Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder is Ba2(1-x-y-z)Mg(PO4)2: xCe<3+>, yTb<3+>, zMn<2+>, wherein x is greater than 0 and is smaller than or equal to 0.2, y is greater than 0 and is smaller than or equal to 0.2, and z is greater than 0 and is smaller than or equal to 0.4. The invention also discloses a preparation method of the white phosphor powder. The preparation method comprises the following steps: uniformly mixing carbonates and ammonium dihydrogen phosphates corresponding to Ba, Mg and Mn with oxides or nitrates of Ce and Tb according to a stoichiometric ratio, and performing grinding to obtain a mixture; putting the mixture into a crucible boat, and placing the crucible boat into a double-temperature-zone tubular furnace quartz tube; calcining the mixture at a high temperature by using aluminum powder as a reducing agent, and cooling and grinding the mixture into powder namely the single-matrix phosphate white phosphor powder. Under the ultraviolet excitation, the phosphor powder emits white light composed of 380nm of blue light, 550nm of green light and 600nm of red light by regulating the concentrations of doped Ce, Tb and Mn ions.
Description
Technical field
The invention belongs to materialogy field, relate to a kind of rare earth luminescent material, specifically a kind of cerium, terbium, the coactivated single matrix phosphoric acid salt white emitting fluorescent powder of manganese and preparation method.
Background technology
White light emitting diode (whitelight-emittingdiodes, WLEDs), the remarkable advantage such as energy consumption low, pollution-free, efficiency high, volume little long with its life-span, have broad application prospects in illumination and display field, be called as lighting source of new generation.
At present, the emphasis of current WLEDs industry development is become by the preparation scheme that ultraviolet-near ultraviolet chip excites three primary colors fluorescent powder to realize white light.Because vision is to the insensitivity of ultraviolet-near-ultraviolet light, the color of this kind of white light LEDs is only determined by fluorescent material, therefore such a scheme overcomes the shortcomings such as " champac " combined white light LED color temperature is higher, colour rendering index is poor, luminous efficiency is low.But, absorb and the problems such as proportioning regulation and control owing to there is color between heterogeneous phosphor mixture, luminous efficiency and color rendition performance are a greater impact, in addition again, the coating processes of several fluorescent material mixing too increases the difficulty of manufacture process of white light LED, adds production cost.
Therefore, development of new efficient single-matrix white luminescent material tool is of great significance, and becomes the study hotspot of White-light LED illumination of new generation.Have some novel single-matrix white fluorescent powder systems of bibliographical information in recent years, mostly concentrate on silicate substrate.Such as Eu
2+/ Tb
3+/ Mn
2+coactivated silicate BaMg
2al
6si
9o
30, Ce
3+/ Tb
3+/ Mn
2+coactivated silicate CaScAlSiO
6white light emission is obtained etc. in system.But silicate systems preparation temperature is high, and due to SiO
2inertia is comparatively strong, thing phase and structural confirmation more difficult.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of cerium, terbium, the coactivated single matrix phosphoric acid salt white emitting fluorescent powder of manganese and preparation method, the coactivated single matrix phosphoric acid salt white emitting fluorescent powder of described this cerium, terbium, manganese and preparation method solve that white emitting fluorescent powder preparation temperature of the prior art is high, thing phase and the more difficult technical problem of structural confirmation.
The present invention a kind of cerium, terbium, the coactivated single matrix phosphoric acid salt white emitting fluorescent powder of manganese, its combination matching general formula is Ba
2 (1-x-y-z)mg (PO
4)
2: xCe
3+, yTb
3+, zMn
2+, wherein 0<x≤0.2,0<y≤0.2,0<z≤0.4.
Present invention also offers the preparation method of above-mentioned a kind of cerium, terbium, the coactivated single matrix phosphoric acid salt white emitting fluorescent powder of manganese,
(1) barium carbonate is taken according to mol ratio, magnesium basic carbonate, primary ammonium phosphate, cerium oxide or cerous nitrate, terbium sesquioxide or Terbium trinitrate, manganous carbonate, barium carbonate, magnesium basic carbonate, primary ammonium phosphate, cerium oxide or cerous nitrate, terbium sesquioxide or Terbium trinitrate, the mass ratio of manganous carbonate is 2 (1-x-y-z): 1:2:x:y:z, above-mentioned substance is mixed, then grind, the mixture obtained after grinding is put into crucible boat and is placed in one end of pair temperature-area tubular furnace silica tube, the crucible boat that aluminium powder is housed is placed in the other end of two temperature-area tubular furnace silica tube,
(2) under above-mentioned pair of temperature-area tubular furnace being placed in vacuum environment, one end sintering temperature of mixture is 1000-1300 DEG C, and calcination time is 3-10 hour, and one end sintering temperature of aluminium powder is 700-900 DEG C, and calcination time is 3-10 hour; Be cooled to after room temperature until tube furnace, close vacuum pump, take out sinter grinding and namely obtain cerium, terbium, the coactivated single matrix phosphoric acid salt white emitting fluorescent powder of manganese.
The present invention is fluorescent material prepared by reductive agent with aluminium powder, under the exciting of 307nm light source, and Ce
3+→ Tb
3+energy trasfer, increased substantially the green emission intensity that emission peak wavelength is 550nm, simultaneously Ce
3+sensitization Mn
2+transmitting, improve the red light emitting intensity that emission peak wavelength is 600nm, obtain tristimulus coordinates for the white emitting fluorescent powder of (0.263,0.240).Fluorescent material of the present invention is under ultraviolet excitation, the concentration of the cerium adulterated by adjustment, terbium, mn ion, and sample sends the white light combined by 380nm blue light, 550nm green glow and 600nm ruddiness.
The present invention compares with prior art, and its technical progress is significant.Phosphoric acid salt is the substrate material that a class luminescent properties is good, and its preparation temperature is low, luminous efficiency is high, physicochemical property are stable, effectively can absorb UV photon energy.Therefore, acquisition synthesis temperature is low, luminous efficiency is high, physical and chemical performance is more stable, and preparation technology's simple single-matrix phosphoric acid salt white emitting fluorescent powder has very important significance.
Accompanying drawing explanation
Fig. 1 is Ba of the present invention
1.88mg (PO
4)
2: 0.04Ce
3+, 0.01Tb
3+, 0.01Mn
2+emmission spectrum.
Fig. 2 is Ba of the present invention
1.88mg (PO
4)
2: 0.04Ce
3+, 0.01Tb
3+, 0.01Mn
2+tristimulus coordinates figure.
Embodiment
embodiment 1:
Preparation Ba
1.92mg (PO
4)
2: 0.04Ce
3+, 0.01Tb
3+, 0.01Mn
2+.
Take barium carbonate 2.0668g, magnesium basic carbonate 0.5411g, cerium oxide 0.0767g, terbium sesquioxide 0.0208, manganous carbonate 0.0128, primary ammonium phosphate 1.2817g, be placed in mortar ground and mixed 120min, after then adding alcohol grinding 60min, obtain mixture, mixture put into crucible boat and be placed in two temperature-area tubular furnace, under aluminium reducing atmosphere, 1100 DEG C of calcinings are after 5 hours, naturally cooling grind into powder.
embodiment 2:
Preparation Ba
1.74mg (PO
4)
2: 0.04Ce
3+, 0.03Tb
3+, 0.06Mn
2+.
Take barium carbonate 1.9193g, magnesium basic carbonate 0.5429g, cerous nitrate 0.1458g, Terbium trinitrate 0.0289, manganous carbonate 0.0771g, primary ammonium phosphate 1.2859g, be placed in mortar ground and mixed 120min, after then adding alcohol grinding 60min, obtain mixture, mixture put into crucible boat and be placed in two temperature-area tubular furnace, under aluminium reducing atmosphere, 1100 DEG C of calcinings are after 5 hours, naturally cooling grind into powder.
embodiment 3:
Preparation Ba
1.72mg (PO
4)
2: 0.2Ce
3+, 0.1Tb
3+, 0.3Mn
2+.
Take barium carbonate 0.9564g, magnesium basic carbonate 0.5884g, cerium oxide 0.4171g, terbium sesquioxide 0.2265g, manganous carbonate 0.4178g, primary ammonium phosphate 1.3937g, be placed in mortar ground and mixed 120min, after then adding acetone grinding 10min, obtain mixture, mixture put into crucible boat and be placed in two temperature-area tubular furnace, under aluminium reducing atmosphere, 1000 DEG C of calcinings are after 10 hours, naturally cooling grind into powder.
embodiment 4:
Preparation Ba
1.72mg (PO
4)
2: 0.2Ce
3+, 0.2Tb
3+, 0.4Mn
2+.
Take barium carbonate 0.4921g, magnesiumcarbonate 0.6055g, cerium oxide 0.4291g, terbium sesquioxide 0.4661g, manganous carbonate 0.5732g, primary ammonium phosphate 1.4341g, be placed in mortar ground and mixed 120min, after then adding acetone grinding 10min, obtain mixture, mixture put into crucible boat and be placed in two temperature-area tubular furnace, under aluminium reducing atmosphere, 1300 DEG C of calcinings are after 3 hours, naturally cooling grind into powder.
Claims (2)
1. cerium, terbium, the coactivated single matrix phosphoric acid salt white emitting fluorescent powder of manganese, is characterized in that: its combination matching general formula is Ba
2 (1-x-y-z)mg (PO
4)
2: xCe
3+, yTb
3+, zMn
2+, wherein 0<x≤0.2,0<y≤0.2,0<z≤0.4.
2. the preparation method of a kind of cerium according to claim 1, terbium, the coactivated single matrix phosphoric acid salt white emitting fluorescent powder of manganese, is characterized in that:
(1) barium carbonate, magnesium basic carbonate, primary ammonium phosphate, cerium oxide (cerous nitrate), terbium sesquioxide (Terbium trinitrate), manganous carbonate is taken according to the mol ratio of 2 (1-x-y-z): 1:2:x:y:z, mix after grinding, put into crucible boat and be placed in one end of two temperature-area tubular furnace silica tube, the crucible boat that aluminium powder is housed being placed in the other end of two temperature-area tubular furnace silica tube;
(2) under above-mentioned pair of temperature-area tubular furnace being placed in vacuum environment, one end sintering temperature of mixture is 1000-1300 DEG C, and calcination time is 3-10 hour, and one end sintering temperature of aluminium powder is 700-900 DEG C, and calcination time is 3-10 hour; Be cooled to after room temperature until tube furnace, close vacuum pump, take out sinter grinding and namely obtain cerium, terbium, the coactivated single matrix phosphoric acid salt white emitting fluorescent powder of manganese.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510376253.3A CN105038787A (en) | 2015-07-01 | 2015-07-01 | Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510376253.3A CN105038787A (en) | 2015-07-01 | 2015-07-01 | Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105038787A true CN105038787A (en) | 2015-11-11 |
Family
ID=54445765
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510376253.3A Pending CN105038787A (en) | 2015-07-01 | 2015-07-01 | Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105038787A (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957653A (en) * | 2017-03-30 | 2017-07-18 | 上海应用技术大学 | One kind enhancing YAG:The method of Ce fluorescent material yellow emission intensity |
| CN106995698A (en) * | 2017-03-30 | 2017-08-01 | 上海应用技术大学 | A kind of preparation method for launching enhanced fluorescent material |
| CN107880885A (en) * | 2016-09-29 | 2018-04-06 | 有研稀土新材料股份有限公司 | Carbuncle type aluminosilicate fluorescent powder and preparation method thereof and the luminescent device for including it |
| CN105740629B (en) * | 2016-02-01 | 2018-05-08 | 南京航空航天大学 | A kind of method that shock-wave spot is determined according to Flow Field Numerical Calculation result |
| CN108059446A (en) * | 2018-01-10 | 2018-05-22 | 上海应用技术大学 | A kind of white fluorescence ceramics and preparation method thereof |
| CN110591712A (en) * | 2018-06-13 | 2019-12-20 | 广州航海学院 | Single-matrix multicolor fluorescent powder for ultraviolet LED and preparation method thereof |
| CN110791291A (en) * | 2019-09-29 | 2020-02-14 | 贺州学院 | Synthesis method of phosphosilicate white light emitting fluorescent powder |
| CN111653657A (en) * | 2020-07-08 | 2020-09-11 | 泉州市康电光电科技有限公司 | Illumination process for plant solar photosynthesis |
| CN111944527A (en) * | 2020-07-10 | 2020-11-17 | 贺州学院 | Synthesis method of ultraviolet light excited multicolor emission fluorescent powder |
| CN111978960A (en) * | 2020-07-10 | 2020-11-24 | 贺州学院 | Synthesis method of broadband excitation phosphate red fluorescent powder |
| CN112125659A (en) * | 2020-10-15 | 2020-12-25 | 贵州赛义光电科技有限公司 | Fluorescent ceramic for warm white lighting and preparation method thereof |
| CN113403076A (en) * | 2021-04-30 | 2021-09-17 | 南京林业大学 | Cerium-manganese activated single-matrix fluorescent powder with ultra-wideband emission and multifunctional 1-pc-LED device applying same |
| CN116333739A (en) * | 2023-03-27 | 2023-06-27 | 河北工业大学 | Activator-free matrix luminous red fluorescent powder and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597493A (en) * | 2009-07-10 | 2009-12-09 | 孙德春 | A kind of alkaline-earth metal silicophosphate fluorescent material and manufacture method and application |
| CN103881703A (en) * | 2014-03-25 | 2014-06-25 | 陕西科技大学 | Preparation method of single-substrate fluorescent powder for white-light LED |
-
2015
- 2015-07-01 CN CN201510376253.3A patent/CN105038787A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597493A (en) * | 2009-07-10 | 2009-12-09 | 孙德春 | A kind of alkaline-earth metal silicophosphate fluorescent material and manufacture method and application |
| CN103881703A (en) * | 2014-03-25 | 2014-06-25 | 陕西科技大学 | Preparation method of single-substrate fluorescent powder for white-light LED |
Non-Patent Citations (1)
| Title |
|---|
| ZHIJUN WANG ET AL: "A white emitting phosphor BaMg2(PO4)2 Ce3+, Mn2+, Tb3+ Luminescence and energy transfer", 《CERAMICS INTERNATIONAL》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105740629B (en) * | 2016-02-01 | 2018-05-08 | 南京航空航天大学 | A kind of method that shock-wave spot is determined according to Flow Field Numerical Calculation result |
| CN107880885A (en) * | 2016-09-29 | 2018-04-06 | 有研稀土新材料股份有限公司 | Carbuncle type aluminosilicate fluorescent powder and preparation method thereof and the luminescent device for including it |
| CN106957653A (en) * | 2017-03-30 | 2017-07-18 | 上海应用技术大学 | One kind enhancing YAG:The method of Ce fluorescent material yellow emission intensity |
| CN106995698A (en) * | 2017-03-30 | 2017-08-01 | 上海应用技术大学 | A kind of preparation method for launching enhanced fluorescent material |
| CN108059446A (en) * | 2018-01-10 | 2018-05-22 | 上海应用技术大学 | A kind of white fluorescence ceramics and preparation method thereof |
| CN110591712A (en) * | 2018-06-13 | 2019-12-20 | 广州航海学院 | Single-matrix multicolor fluorescent powder for ultraviolet LED and preparation method thereof |
| CN110791291A (en) * | 2019-09-29 | 2020-02-14 | 贺州学院 | Synthesis method of phosphosilicate white light emitting fluorescent powder |
| CN111653657A (en) * | 2020-07-08 | 2020-09-11 | 泉州市康电光电科技有限公司 | Illumination process for plant solar photosynthesis |
| CN111944527A (en) * | 2020-07-10 | 2020-11-17 | 贺州学院 | Synthesis method of ultraviolet light excited multicolor emission fluorescent powder |
| CN111978960A (en) * | 2020-07-10 | 2020-11-24 | 贺州学院 | Synthesis method of broadband excitation phosphate red fluorescent powder |
| CN112125659A (en) * | 2020-10-15 | 2020-12-25 | 贵州赛义光电科技有限公司 | Fluorescent ceramic for warm white lighting and preparation method thereof |
| CN113403076A (en) * | 2021-04-30 | 2021-09-17 | 南京林业大学 | Cerium-manganese activated single-matrix fluorescent powder with ultra-wideband emission and multifunctional 1-pc-LED device applying same |
| CN116333739A (en) * | 2023-03-27 | 2023-06-27 | 河北工业大学 | Activator-free matrix luminous red fluorescent powder and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105038787A (en) | Ce, Tb and Mn-coactivated single-matrix phosphate white phosphor powder and preparation method thereof | |
| CN101768441B (en) | Rare earth borate luminescent material and preparation material thereof | |
| CN102660276A (en) | Near ultraviolet stimulated borophosphate white light fluorescent powder and preparation method | |
| CN105199728A (en) | Novel Eu<3+> and Mn<2+> co-doped tungstate red fluorescent material and preparation method thereof | |
| WO2013074158A1 (en) | Green and yellow aluminate phosphors | |
| CN102732251A (en) | Single-phase white light phosphor for near-ultraviolet light excitation and preparation method thereof | |
| CN103881705B (en) | Cerium, terbium or europium silico-aluminate blue-green fluorescent powder mixing activation altogether and preparation method thereof | |
| CN102199429B (en) | Fluophosphate-based light-emitting material and preparation method thereof | |
| CN103740364B (en) | A kind of yellow orange-orange red orthosilicate fluorescent material and preparation method thereof | |
| CN103275713A (en) | Rare earth molybdate red phosphor, and preparation method and application thereof | |
| CN102286281B (en) | Aluminate-based red fluorescent material and preparation method thereof | |
| CN102952546B (en) | Molybdate red phosphor powder applicable to white-light LED (Light-Emitting Diode) and preparation method thereof | |
| CN104962286A (en) | Garnet-structure multiphase fluorescent material and preparation method thereof | |
| CN102127441A (en) | Eu<2+> activated strontium pyrophosphate photoluminescence material and preparation method thereof | |
| CN108276998B (en) | Trivalent samarium ion doped barium gadolinium titanate red fluorescent powder and preparation method thereof | |
| CN107163934B (en) | Quadrivalent manganese ion doped fluorine aluminum oxide lithium red fluorescent powder and preparation method thereof | |
| CN102492422A (en) | Green emitting phosphor for white-light LEDs and preparation method thereof | |
| CN103396798B (en) | A kind of near ultraviolet excitated nitric oxide fluorescent powder and preparation method thereof | |
| CN103131415B (en) | Yellow long-lasting phosphor material and preparation method thereof | |
| CN106929016A (en) | A kind of blueness arrives adjustable silicate fluorescent powder of green color and preparation method thereof | |
| CN104974756B (en) | Cerium and terbium mono-doped/codoped yttrium sodium phosphate fluorescent powder, and preparation method thereof | |
| CN109294583B (en) | Cerium ion doped barium gadolinium titanate blue fluorescent powder for white light LED and preparation method thereof | |
| CN102533268A (en) | Blue light-emitting material and preparation method thereof | |
| CN102127442B (en) | Zirconium phosphate-based luminescent material as well as preparation method and application thereof | |
| CN106867524B (en) | A kind of preparation and application of alkaline earth aluminate blue fluorescent material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20151111 |
|
| RJ01 | Rejection of invention patent application after publication |