CN107033883A - A kind of green luminescent material and preparation method thereof - Google Patents
A kind of green luminescent material and preparation method thereof Download PDFInfo
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Abstract
A kind of green luminescent material and preparation method thereof, the chemical structural formula of the green luminescent material is：M2+y/2‑x A1‑y C y O4:xD, wherein, 0 ＜xThe ＜ of ＜ 0.03,0y＜ 0.5.By the stoichiometric proportion of each chemical composition in chemical structural formula; each raw material is weighed respectively; taken each raw mill is well mixed; 1000 °C~1500 °C are warming up in tube furnace under conditions of protective atmosphere is passed through, 3~8h is calcined, is then cooled to 500 °C; turn off heating system; cool to room temperature with the furnace, sintered product is pulverized into powder sieving, green luminescent material is obtained.The green luminescent material luminosity and luminous efficiency are high, better heat stability.And simple easily repetition is made, with low cost, process window is wide, is adapted to large-scale industrial production.
Description
Technical field
The invention belongs to luminescent material technical field, it is related to a kind of green luminescent material, the invention further relates to a kind of hair
The preparation method of luminescent material.
Background technology
White light LEDs are described as the forth generation light source after incandescent lamp, fluorescent lamp, high-voltage gas discharging light.At this stage
Main implementation method is fluorescence conversion method.For visual angle, blue light+gold-tinted or blue light+green glow+red can be perceived as
White light.Based on principles above, the implementation method of white light LEDs mainly has：1）Blue-light LED chip+yellow fluorescent material combination transmitting
White light.Wherein, the patent of YAG powder and LuAG powder is that Japanese day is sub- chemical all, the patent No.：US5998925.The patent of TAG powder
All, patent No. for German Ou Silang：US6669866.RAG:Ce3+, (R is Y, Lu, Gd, Sc, La, one kind or several in Sm
Kind）All, patent No. for Chinese You Yan rare earth materials limited company：02130949.3.2）Ultraviolet/near ultraviolet LED chip+
Red, green, blue fluorescent material with three basic colour launches white light.Due to there is the leakage hidden danger of ultraviolet/black light, the combination is not by city
Welcome field.3）Blue-light LED chip synthesizes white light LEDs with red+green fluorescent material.Blue chip base white light LEDs are considered as peace
Entirely, save, efficient lighting source.The leading mode of production is still by modified (Y, Gd) at present3(Al, Ga)5O12:Ce3 +（YAG）Yellow fluorescent powder is coated on GaInN blue chips.With the Ce that can be effectively excited by blue chip3+/ Eu2+Doping
The discovery of nitrogen (oxygen) compound green/red fluorescent material and update.Blue-light LED chip is synthesized in vain with red+green fluorescent material
Light LED technology path is more and more concerned.The white light of combination synthesis is aobvious with the colour temperature and Geng Gao adjusted extensively
Colour index.The green emitting phosphor that can be effectively excited by blue chip at present has MSi2O2N2:Eu2+(M=Ca, Sr, Ba) and
β-SiAlON:Eu2+.But MSi2O2N2：Eu2+The patent of (M=Ca, Sr, Ba) is all for Germany Ou Silang, Patent No.：
EP1413618）.β-SiAlON:Eu2+The patent of fluorescent material is all for Japanese state-run material science research institute, U.S. Patent number：
US6632379.In China native country, the green emitting phosphor that can be effectively excited by blue chip lacks.
The content of the invention
It is an object of the invention to provide a kind of green luminescent material that can be effectively excited by blue chip.
It is a further object to provide a kind of preparation method of above-mentioned green luminescent material.
To achieve the above object, the technical solution adopted in the present invention is：A kind of green luminescent material, its chemical structural formula
For：M2+y/2-x A1-y C y O4:xD, wherein, 0 ＜xThe ＜ of ＜ 0.03,0y＜ 0.5；M is Ca, Sr or Ba；A is B, P or Si；C be Al or
Ga；D is Mn, Ce, Pr, Eu, Sm, Dy, Nd, Gd, Tb, Ho, Er or Tm.
Another technical scheme of the present invention is：A kind of preparation method of above-mentioned green luminescent material, be specially：
By chemical structural formula M2+y/2-x A1-y C y O4:xThe stoichiometric proportion of each chemical composition in D, weighs each raw material respectively, by taken each original
Abrasive lapping is well mixed, and is warming up to 1000 °C~1500 °C in tube furnace under conditions of protective atmosphere is passed through, and is calcined 3~8h,
Then 500 °C are cooled to, turns off heating system, room temperature is cooled to the furnace, sintered product is pulverized into powder sieving, green emitting is obtained
Material.
Green luminescent material luminosity of the present invention and luminous efficiency are high, better heat stability.And the simple easily repetition of making,
With low cost, process window is wide, is adapted to large-scale industrial production.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram of green luminescent material made from embodiment 1.
Fig. 2 is exciting and launching light spectrogram for green luminescent material made from embodiment 1.
Fig. 3 is barium silicate (Ba2SiO4:Eu2+) and alumina silicate barium (Ba2-x Si1-y Al y O4:xEu2+)Excitation spectrum model
Enclose comparison（Intensity normalized）Figure.
Fig. 4 is barium silicate (Ba2SiO4:Eu2+) and alumina silicate barium (Ba2-x Si1-y Al y O4:xEu2+) emission spectrum hair
Penetrate intensity comparison chart.
Fig. 5 is the emission spectrum variation with temperature figure of green luminescent material made from embodiment 1.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The chemical structural formula for the green luminescent material that the present invention is provided is：M2+y/2-x A1-y C y O4:xD, wherein, 0 ＜x＜
0.03,0 ＜y＜ 0.5；M is Ca, Sr or Ba；A is B, P or Si；C is Al or Ga；D be Mn, Ce, Pr, Eu, Sm, Dy, Nd,
Gd, Tb, Ho, Er or Tm.
Present invention also offers a kind of preparation method of above-mentioned green luminescent material, it is specially：By chemical structural formula
M2+y/2-x A1-y C y O4:xThe stoichiometric proportion of each chemical composition in D, weighs each raw material respectively, and M therein passes through its carbonate, oxygen
Compound or fluoride are introduced, and A is introduced by its oxide, and C is introduced with its oxide, and D is introduced with its oxide；By taken each original
Material is placed in agate mortar, adds alcohol, and ground and mixed is uniform, in tube furnace under conditions of protective atmosphere is passed through with 5 DEG C/
Min heating rate is warming up to 1000 °C~1500 °C, is calcined 3~8h, is then cooled to 500 ° with 5 DEG C/min rate of temperature fall
C, turns off heating system, cools to room temperature with the furnace, and sintered product is pulverized into powder sieving, green luminescent material is obtained.
The control of temperature concentrates on final sintering temperature in whole preparation process（The formation temperature of solid solution）And insulation
Time（Ensure that the formation of solid solution is completely carried out）.
Protective atmosphere is made up of by percent by volume 5~10% hydrogen and 95~90% nitrogen.
Green luminescent material provided by the present invention can be by 300~400nm ultraviolet chip and 420~460nm indigo plant
Optical chip is effectively excited, and then is launched peak wavelength and be located at~520nm broadband green glow.
The green emitting phosphor Ba that preparation method of the present invention is effectively excited to conventional ultra-violet2SiO4:Eu2+Carry out cation substitution
It is modified.Rare-Earth Ce3+ /Eu2+Excite and launch and influenceed very big by crystalline field environment around, therefore by changing Ce3+ /
Eu2+ Surrounding coordination environment, and then adjust the main method of modifying that luminescent properties are fluorescent material.Traditional green emitting phosphor
Ba2SiO4:Eu2+, can effectively be excited by ultraviolet/near ultraviolet, and launch high-intensity, narrow-band band blue green light.That is Eu2+ In Ba2SiO4
Under crystalline field ambient influnence, effective excites scope corresponding to the splitting degree of 5d energy levels is 350nm~410nm, transmitting boundary
For 475nm~560nm, and most strong transmitting is located at~500nm.Al is mixed, causes lattice distortion, 5d energy is further increased
The splitting degree of level, causes corresponding effective excites scope to expand to 350nm~460nm, transmitting boundary be 460nm~
580nm, and most strong transmitting is located at~520 nm.Under same doping concentration, Al incorporation causes Eu2+Valid density increase,
And then emissive porwer is dramatically increased.In addition, wide absorption band shows that the absorption to projectile energy is more efficient, high emissive porwer and
Wide transmitting boundary shows to launch outgoing efficiency high.Therefore relative to Ba2SiO4:Eu2+, green luminescent material of the present invention it is luminous
Efficiency is significantly improved.
Embodiment 1
Weigh BaCO3 0.9617g、SiO2 0.1957g、Al2O3 0.0553g、Eu2O30.0020g, adds wine in agate mortar
Essence is transferred to corundum crucible after being fully ground, be then placed in tube furnace, is passed through by percent by volume by 95% nitrogen and 5%
The protective atmosphere of hydrogen composition, 1340 DEG C are warming up to 5 DEG C/min heating rate, 3 hours are incubated, then with 5 DEG C/min's
Rate of temperature fall is cooled to 500 DEG C, turns off heating system, cools to room temperature with the furnace；Product after sintering is pulverized into powder sieving, obtained
Structural formula is Ba2-x Si1-y Al y O4:xEu2+（0.019<x< 0.021, 0.19< y< 0.21）Luminescent material.
In being operated in actual experiment, the raw material of fixed mass is weighed, repeats real under metastable reaction condition
Test three times, the product luminescent properties difference finally given less, does not influence application performance.But the content of each element must be different
, simply by strict control, the change of content, which should be reduced to, does not influence performance.
The X-ray diffraction spectrogram of sample made from embodiment 1, as shown in figure 1, as can be seen from the figure prepared sample is
The preferable single phase solid solution of crystallinity, and single-phase purpose is prepared, it is in order to repeatable.The loss of the high then luminescent properties of crystallinity
It is few.
The excitation-emission spectrogram of sample made from embodiment 1 in figure as shown in Fig. 2 show, gained sample has very wide
Excitation band（300~470nm）.Excites scope from ultraviolet to blue light region, effective blue light excites scope be 420nm~
460nm, in the case where 450nm blue lights are excited, launches high intensity green glow, illustrate embodiment 1 made from sample be green emitting material
Material.
Fig. 3 is barium silicate (Ba2SiO4:Eu2+) and alumina silicate barium (Ba2-x Si1-y Al y O4:xEu2+)Excitation spectrum model
Enclose comparison（Intensity normalized）Figure.Illustrate that the excitation spectrum broadening of green luminescent material made from embodiment 1 has arrived blue light
Area, modified fluorescent material can effectively be excited by blue chip.Fig. 4 is barium silicate (Ba2SiO4:Eu2+) and alumina silicate barium
(Ba2-x Si1-y Al y O4:xEu2+) emission spectrum emissive porwer compare.Ba2SiO4:Eu2+ Most excite by force as ~ 365
Nm, Ba2-x Si1-y Al y O4:xEu2+Most excite by force as ~ 400nm.The conventional blue chip of industry is 450nm, therefore
Give Ba2-x Si1-y Al y O4:xEu2+Intensity in the case where 450 nm are excited.Green luminescent material made from embodiment 1 is excited
Intensity afterwards is much larger than Ba2SiO4:Eu2+Intensity after exciting.
The thermal quenching performance plot of sample made from embodiment 1, as shown in figure 3, as can be seen from Figure 3 when temperature reaches 150 DEG C
（The operating temperature of great power LED）, more than 70% when emissive porwer is initial.Show that the sample has good heat endurance
Embodiment 2
By chemical structural formula Ca1.463B0.505Ga0.495O4:The stoichiometric proportion of each chemical composition, is weighed respectively in 0.295Mn
CaO、BO、Ga3O2And Mn2O3；It is placed in agate mortar and adds alcohol to be transferred to corundum crucible after being fully ground, is then placed in tubular type
In stove, the protective atmosphere being made up of by percent by volume 90% nitrogen and 10% hydrogen is passed through, with 5 DEG C/min heating rate
1000 DEG C are warming up to, 8 hours is incubated, is then cooled to 500 DEG C with 5 DEG C/min rate of temperature fall, turns off heating system, it is cold with stove
But to room temperature；Product after sintering is pulverized into powder sieving, green luminescent material is obtained.
Embodiment 3
By chemical structural formula Sr1.134P0.75Ga0.25O4:The stoichiometric proportion of each chemical composition in 0.015Ce, weigh respectively SrO,
P2O5、Ga3O2And Ce2O3；It is placed in agate mortar and adds alcohol to be transferred to corundum crucible after being fully ground, is then placed in tube furnace
It is interior, the protective atmosphere being made up of by percent by volume 92.5% nitrogen and 7.5% hydrogen is passed through, with 5 DEG C/min heating speed
Rate is warming up to 1025 DEG C, is incubated 5.5 hours, is then cooled to 500 DEG C with 5 DEG C/min rate of temperature fall, turns off heating system, with
Stove is cooled to room temperature；Product after sintering is pulverized into powder sieving, green luminescent material is obtained.
Embodiment 4
By chemical structural formula Sr1.008P0.99Al0.01O4:The stoichiometric proportion of each chemical composition, is weighed respectively in 0.005Sm
SrCO3、P2O5、Al3O2And Sm2O3；Then green luminescent material is made as described in Example 1.
Embodiment 5
By chemical structural formula Ca1.011B0.998Al0.002O4:The stoichiometric proportion of each chemical composition, is weighed respectively in 0.02Dy
CaCO3、B2O5、Al3O2And Dy2O3；Then green luminescent material is made as described in Example 2.
Embodiment 6
By chemical structural formula Ba1.018Si0.97Ga0.03O4:The stoichiometric proportion of each chemical composition, is weighed respectively in 0.005Nd
BaCO3、SiO2、Ga3O2And Nd2O3；Then green luminescent material is made as described in Example 3.
Embodiment 7
By chemical structural formula Ba1.025Si0.96Ga0.04O4:The stoichiometric proportion of each chemical composition, weighs BaF respectively in 0.01Gd2、
SiO2、Ga3O2And Gd2O3；Then green luminescent material is made as described in Example 4.
Embodiment 8
By chemical structural formula Sr1.191P0.975Al0.025O4:The stoichiometric proportion of each chemical composition, is weighed respectively in 0.2999Ho
SrF2、P2O5、Al3O2And Ho2O3；Then green luminescent material is made as described in Example 2.
Embodiment 9
By chemical structural formula Ca1.178B0.65Ga0.35O4:The stoichiometric proportion of each chemical composition, weighs CaF respectively in 0.005Er2、
B2O5、Ga3O2And Er2O3；Then green luminescent material is made as described in Example 3.
Embodiment 10
By chemical structural formula Ca1.288B0.55Ga0.45O4:The stoichiometric proportion of each chemical composition, weighs CaF respectively in 0.02Tm2、
B2O5、Ga3O2And Tm2O3；Then green luminescent material is made as described in Example 2.
Embodiment 11
By chemical structural formula Ca1.104P0.875Ga0.125O4:The stoichiometric proportion of each chemical composition, is weighed respectively in 0.075Pr
CaCO3、P2O5、Al3O2And Pr2O3；Then green luminescent material is made as described in Example 3.
Embodiment 12
By chemical structural formula Ca1.104P0.875Ga0.125O4:The stoichiometric proportion of each chemical composition, is weighed respectively in 0.075Tb
CaCO3、P2O5、Al3O2And Tb2O3；Then green luminescent material is made as described in Example 4.
Claims (4)
1. a kind of green luminescent material, it is characterised in that its chemical structural formula is：M2+y/2-x A1-y C y O4:xD, wherein, 0 ＜x＜
0.03,0 ＜y＜ 0.5；M is Ca, Sr or Ba；A is one kind in B, P, Si；C is one kind in Al, Ga；D be Mn, Ce, Pr,
One kind in Eu, Sm, Dy, Nd, Gd, Tb, Ho, Er, Tm.
2. a kind of preparation method of the green luminescent material described in claim 1, it is characterised in that the preparation method is specially：
By chemical structural formula M2+y/2-x A1-y C y O4:xThe stoichiometric proportion of each chemical composition in D, weighs each raw material respectively, by taken each original
Abrasive lapping is well mixed, and is warming up to 1000 °C~1500 °C in tube furnace under conditions of protective atmosphere is passed through, and is calcined 3~8h,
Then 500 °C are cooled to, turns off heating system, room temperature is cooled to the furnace, sintered product is pulverized into powder sieving, green emitting is obtained
Material.
3. the preparation method of green luminescent material according to claim 2, it is characterised in that when weighing each raw material, wherein
M introduced by its carbonate, oxide or fluoride, A introduced by its oxide, and C is introduced with its oxide, and D is with its oxygen
Compound is introduced.
4. the preparation method of green luminescent material according to claim 2, it is characterised in that during heating, with 5 DEG C/min speed
Rate heats up；During cooling, cooled with 5 DEG C/min speed.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2013227527A (en) * | 2012-03-26 | 2013-11-07 | Mitsubishi Chemicals Corp | Phosphor and light emitting device using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2013227527A (en) * | 2012-03-26 | 2013-11-07 | Mitsubishi Chemicals Corp | Phosphor and light emitting device using the same |
Non-Patent Citations (1)
| Title |
|---|
| ZHIYONG MAO等: "Tunable Luminescent Eu2+-Doped Dicalcium Silicate Polymorphs Regulated by Crystal Engineering", 《JOURNAL OF MATERIALS CHEMISTRY C》 * |
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