CN107722983A - L ED fluorescent powder and preparation method thereof - Google Patents
L ED fluorescent powder and preparation method thereof Download PDFInfo
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- CN107722983A CN107722983A CN201710854426.7A CN201710854426A CN107722983A CN 107722983 A CN107722983 A CN 107722983A CN 201710854426 A CN201710854426 A CN 201710854426A CN 107722983 A CN107722983 A CN 107722983A
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- 239000000843 powder Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 55
- 239000000126 substance Substances 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims description 88
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 29
- 239000004254 Ammonium phosphate Substances 0.000 claims description 29
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 29
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 29
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical group [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 29
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 21
- 238000002604 ultrasonography Methods 0.000 claims description 21
- 238000000227 grinding Methods 0.000 claims description 20
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 18
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 18
- 239000004744 fabric Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000009413 insulation Methods 0.000 claims description 10
- 238000012805 post-processing Methods 0.000 claims description 9
- 229910020187 CeF3 Inorganic materials 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 230000001795 light effect Effects 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 abstract 1
- 238000010792 warming Methods 0.000 description 8
- 238000005286 illumination Methods 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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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
- C09K11/7792—Aluminates
-
- 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)
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
the invention belongs to the technical field of luminescent materials, and particularly relates to an L ED fluorescent powder and a preparation method thereof, which solve the problems of low luminous efficiency, low flexibility, narrow application range, high roasting temperature and long roasting time of L ED white light in the prior art, wherein the L ED fluorescent powder has a chemical general formula of Sr0.4AaMbAl3O12:(Tb3+ xEu2+ y) the fluorescent powder provided by the invention has the advantages of reasonable structure, wide spectrum range, strong light effect, high flexibility, wide application range, simple preparation method, mild conditions and short time consumption.
Description
Technical field
The present invention relates to luminescent material technical field, more particularly to a kind of LED fluorescent powder and preparation method thereof.
Background technology
Incandescent lamp and halogen tungsten lamp are that two kinds of the most frequently used light sources were once illuminated in family, and the light efficiency of incandescent lamp and halogen tungsten lamp is big
About 12~24lm/W, and the light efficiency of the white light LEDs of rising in recent years is gradually increased to 50lm/W from earliest 5lm/W.
The illumination mode of existing white light LEDs can be divided into monocrystalline type and polymorphic two types, and wherein polymorphic is to make
With two or more 2 complementary color LED light emitting diodes or 3 primary colors LED light emitting diodes are done mixed light and formed
White light, but the realization of this illumination mode needs multiple light emitting diodes to coordinate jointly, and the driving of each light emitting diode
Voltage, temperature characterisitic, service life differ, therefore the complexity of polymorphic illumination mode is higher, and maintenance difficulties are larger.
Compared to polymorphic illumination mode, monocrystalline type illumination mode complexity is relatively low, so application is wider.At present, it is single
It is exactly to pass through blue light or ultraviolet leds light emitting diode excitated fluorescent powder that crystal formation, which produces the most frequently used method of white light,.
White light LED fluorescent powder disclosed in the B of China Patent No. CN 102634341 can match with UV LED core
Produce white light；White light LED fluorescent powder disclosed in the B of China Patent No. CN 101391803 can be 440~475nm with launch wavelength
Blue-light LED chip collocation be made diameter 5mm, 20mA white light LEDs, but fluorescent material flexibility ratio made from above two method compared with
Difference, it is only capable of being matched with specific LED chip, narrow application range, and light efficiency highest is only capable of reaching 80lm/W.Above-mentioned two disclosure
Patent also proposes the preparation method of fluorescent material respectively, but two kinds of preparation methods are time-consuming longer, needs in roasting process
Sintering temperature is higher.Based on above statement, the present invention proposes a kind of LED fluorescent powder and preparation method thereof.
The content of the invention
The invention aims to solve present in prior art, LED white lights light efficiency is low, flexibility ratio is low, the scope of application
The shortcomings that narrow, and sintering temperature is high, and roasting time is long, and a kind of LED fluorescent powder proposed and preparation method thereof.
A kind of LED fluorescent powder, the chemical general formula of the fluorescent material is Sr0.4AaMbAl3O12:(Tb3+ xEu2+ y), wherein M is
Any one element in La, Lu, Y, any one element in A Ca, Ba, Zn, Mg, 1.5≤a≤5,0.04≤b≤3,0
≤ x≤3,0.01≤y≤0.1.
Preferably, the x is 0,1,2 or 3.
Preferably, the Eu2+From the compound containing Eu, wherein the preferably oxides, divalent of europium.
Preferably, the one kind of the A in A oxide, carbonate or subcarbonate, the Sr are containing Srization
Compound, the M are the compound containing M, and the Tb is the compound containing Tb, and the Al is oxide or salt containing Al.
Preferably, when the Tb is not 0, A and Tb mol ratio are 0.5~5：1
The invention also provides a kind of preparation method of LED fluorescent powder, comprise the following steps：
S1, raw material mixing and pretreatment：According to the chemical general formula Sr of fluorescent material0.4AaMbAl3O12:(Tb3+ xEu2+ y) claim
Raw material is taken, and adds fluxing agent, it is well mixed to produce mixture A, mixture A is placed in mill and is ground, crosses 100 mesh
Screen cloth above, the mixture A after grinding is produced, the combination of ammonium phosphate and sodium hypophosphite is added into the mixture A after grinding
Thing, and progress 10~20min of ultrasound in Ultrasound Instrument is transferred to, produce mixture B；
S2, mixture roasting and reduction：Mixture after S1 step process is added in high temperature furnace, and in 30min
Inside it is warming up to 550~650 DEG C, keeps 20~30min, then the temperature of high temperature furnace is risen to 750~950 DEG C, while to high temperature furnace
Inside be passed through carbon monoxide, after carbon monoxide be passed through the time rise to 750~950 DEG C more than 30min and temperature after start timing insulation
Time is 60~100min, and insulation is cooled to room temperature after terminating；
S3, post processing：The mixture reduced is transferred in pulverizer and crushed, transfers to ultrasonic powder in Ultrasound Instrument
It is broken, finally it is transferred in mill and grinds, and the screen cloth crossed more than 200 mesh, produce LED fluorescent powder.
Preferably, the cosolvent in the S1 steps is chloric metal-salt, NH4F and B2O3Mixture, the chloric metal-salt,
NH4F and B2O3Mass ratio be 0.5~1.5：3~5：10~25.
Preferably, the chloric metal-salt is CeF3、BiF3、PbF2In the mixing of any one or two kinds.
Preferably, the addition quality of the fluxing agent is the 1~4% of the total compound of fluorescent material.
Preferably, the addition quality of ammonium phosphate and the sodium hypophosphite composition is the 0.5~5% of fluorescent material gross mass,
And the mass ratio of ammonium phosphate and sodium hypophosphite is 2~5：1.
Fluorescent material proposed by the present invention, rational in infrastructure, spectral range is wide, and light efficiency is strong, can reach more than 80lm/W, prepares
Fluorescent material can carry out that collocation is luminous, and flexibility ratio is high, applied widely with blue light or UV chip, and preparation method letter
It is single, the mixture after helping reducing agent will be added in preparation process and carries out ultrasound, phosphor raw material, fluxing agent can be accelerated and helped also
Mixing efficiency between former agent, the uniformity of mixture is improved, added with chloric metal-salt, NH4F and B2O3For the fluxing agent of combination
Compared to the fluxing agent used in the prior art, fluxing effect is more preferable, can significantly reduce temperature and the roasting of fluorescent material roasting
Time, then coordinate using ammonium phosphate and sodium hypophosphite as the addition for helping reducing agent of combination, the preparation condition of fluorescent material can be made more
It is time-consuming short to be gentle, and then improve the production efficiency of fluorescent material；And used when the fluorescent material to preparation post-processes
The mode that pulverizer crushing, Ultrasonic Pulverization and grinding are combined, can significantly improve the treatment effeciency of fluorescent material, make fluorescent material
Granularity is small, and surface area is big, and action effect is good.
Embodiment
The present invention is made with reference to specific embodiment further to explain.
Embodiment one
A kind of LED fluorescent powder proposed by the present invention, the chemical formula of the fluorescent material is Sr0.4A4M3Al3O12:Eu2+ 0.1。
Its preparation method, comprise the following steps：
S1, raw material mixing and pretreatment：According to the chemical general formula Sr of fluorescent material0.4A4M3Al3O12:Eu2+ 0.1Weigh original
Material, and mass ratio is added as 1：4：15 CeF3、NH4F and B2O3, it is well mixed to produce mixture A, mixture A is placed in grinding
It is ground in device, the screen cloth crossed more than 100 mesh, produces the mixture A after grinding, phosphorus is added into the mixture A after grinding
The composition of sour ammonium and sodium hypophosphite, and be transferred in Ultrasound Instrument and carry out ultrasonic 15min, produce mixture B；
S2, mixture roasting and reduction：Mixture after S1 step process is added in high temperature furnace, and in 30min
600 DEG C are inside warming up to, keeps 25min, then the temperature of high temperature furnace is risen to 850 DEG C, while carbon monoxide is passed through into high temperature furnace,
After carbon monoxide be passed through the time rise to 850 DEG C more than 30min and temperature after to start timing soaking time be 90min, insulation terminates
After be cooled to room temperature；
S3, post processing：The mixture reduced is transferred in pulverizer and crushed, transfers to ultrasonic powder in Ultrasound Instrument
It is broken, finally it is transferred in mill and grinds, and the screen cloth crossed more than 200 mesh, produce LED fluorescent powder.
In the present invention, the addition quality of fluxing agent is the 2% of the total compound of fluorescent material；Ammonium phosphate and the sodium hypophosphite group
The addition quality of compound is the 4% of fluorescent material gross mass, and the mass ratio of ammonium phosphate and sodium hypophosphite is 3：1.
Embodiment two
A kind of LED fluorescent powder proposed by the present invention, the chemical formula of the fluorescent material is Sr0.4A2.55M0.04Al3O12:(Tb3+ 3Eu2+ 0.01)。
Its preparation method, comprise the following steps：
S1, raw material mixing and pretreatment：According to the chemical general formula Sr of fluorescent material0.4A2.55M0.04Al3O12:(Tb3+ 3Eu2 + 0.01) raw material is weighed, and mass ratio is added as 1：4：15 CeF3、NH4F and B2O3, it is well mixed to produce mixture A, it will mix
Thing A, which is placed in mill, to be ground, and the screen cloth crossed more than 100 mesh, the mixture A after grinding is produced, to the mixing after grinding
The composition of ammonium phosphate and sodium hypophosphite is added in thing A, and is transferred in Ultrasound Instrument and carries out ultrasonic 15min, produces mixture B；
S2, mixture roasting and reduction：Mixture after S1 step process is added in high temperature furnace, and in 30min
600 DEG C are inside warming up to, keeps 25min, then the temperature of high temperature furnace is risen to 850 DEG C, while carbon monoxide is passed through into high temperature furnace,
After carbon monoxide be passed through the time rise to 850 DEG C more than 30min and temperature after to start timing soaking time be 90min, insulation terminates
After be cooled to room temperature；
S3, post processing：The mixture reduced is transferred in pulverizer and crushed, transfers to ultrasonic powder in Ultrasound Instrument
It is broken, finally it is transferred in mill and grinds, and the screen cloth crossed more than 200 mesh, produce LED fluorescent powder.
In the present invention, the addition quality of fluxing agent is the 2% of the total compound of fluorescent material；Ammonium phosphate and the sodium hypophosphite group
The addition quality of compound is the 4% of fluorescent material gross mass, and the mass ratio of ammonium phosphate and sodium hypophosphite is 3：1.
Embodiment three
A kind of LED fluorescent powder proposed by the present invention, the chemical formula of the fluorescent material is Sr0.4A1.5M2.5Al3O12:(Tb3+ 2Eu2+ 0.1)。
Its preparation method, comprise the following steps：
S1, raw material mixing and pretreatment：According to the chemical general formula Sr of fluorescent material0.4A1.5M2.5Al3O12:(Tb3+ 2Eu2 + 0.1) raw material is weighed, and mass ratio is added as 1：4：15 CeF3、NH4F and B2O3, it is well mixed to produce mixture A, by mixture
A is placed in mill and is ground, and the screen cloth crossed more than 100 mesh, the mixture A after grinding is produced, to the mixture A after grinding
It is middle to add the composition of ammonium phosphate and sodium hypophosphite, and be transferred in Ultrasound Instrument and carry out ultrasonic 15min, produce mixture B；
S2, mixture roasting and reduction：Mixture after S1 step process is added in high temperature furnace, and in 30min
600 DEG C are inside warming up to, keeps 25min, then the temperature of high temperature furnace is risen to 850 DEG C, while carbon monoxide is passed through into high temperature furnace,
After carbon monoxide be passed through the time rise to 850 DEG C more than 30min and temperature after to start timing soaking time be 90min, insulation terminates
After be cooled to room temperature；
S3, post processing：The mixture reduced is transferred in pulverizer and crushed, transfers to ultrasonic powder in Ultrasound Instrument
It is broken, finally it is transferred in mill and grinds, and the screen cloth crossed more than 200 mesh, produce LED fluorescent powder.
In the present invention, the addition quality of fluxing agent is the 2% of the total compound of fluorescent material；Ammonium phosphate and the sodium hypophosphite group
The addition quality of compound is the 4% of fluorescent material gross mass, and the mass ratio of ammonium phosphate and sodium hypophosphite is 3：1.
Example IV
A kind of LED fluorescent powder proposed by the present invention, the chemical formula of the fluorescent material is Sr0.4A5M0.5Al3O12:(Tb3+Eu2 + 0.1)。
Its preparation method, comprise the following steps：
S1, raw material mixing and pretreatment：According to the chemical general formula Sr of fluorescent material0.4A5M0.5Al3O12:(Tb3+Eu2+ 0.1)
Raw material is weighed, and adds mass ratio as 1：4：15 CeF3、NH4F and B2O3, it is well mixed to produce mixture A, mixture A is put
It is ground in mill, the screen cloth crossed more than 100 mesh, the mixture A after grinding is produced, into the mixture A after grinding
The composition of ammonium phosphate and sodium hypophosphite is added, and is transferred in Ultrasound Instrument and carries out ultrasonic 15min, produces mixture B；
S2, mixture roasting and reduction：Mixture after S1 step process is added in high temperature furnace, and in 30min
600 DEG C are inside warming up to, keeps 25min, then the temperature of high temperature furnace is risen to 850 DEG C, while carbon monoxide is passed through into high temperature furnace,
After carbon monoxide be passed through the time rise to 850 DEG C more than 30min and temperature after to start timing soaking time be 90min, insulation terminates
After be cooled to room temperature；
S3, post processing：The mixture reduced is transferred in pulverizer and crushed, transfers to ultrasonic powder in Ultrasound Instrument
It is broken, finally it is transferred in mill and grinds, and the screen cloth crossed more than 200 mesh, produce LED fluorescent powder.
In this present invention, the addition quality of fluxing agent is the 2% of the total compound of fluorescent material；The ammonium phosphate and sodium hypophosphite
The addition quality of composition is the 4% of fluorescent material gross mass, and the mass ratio of ammonium phosphate and sodium hypophosphite is 3：1.
Embodiment five
A kind of LED fluorescent powder proposed by the present invention, the chemical formula of the fluorescent material is Sr0.4A5M0.5Al3O12:(Tb3+Eu2 + 0.1)。
Its preparation method, comprise the following steps：
S1, raw material mixing and pretreatment：According to the chemical general formula Sr of fluorescent material0.4A5M0.5Al3O12:(Tb3+Eu2+ 0.1)
Raw material is weighed, and adds mass ratio as 1.5：3：25 BiF3、NH4F and B2O3, it is well mixed to produce mixture A, by mixture A
It is placed in mill and is ground, the screen cloth crossed more than 100 mesh, the mixture A after grinding is produced, to the mixture A after grinding
It is middle to add the composition of ammonium phosphate and sodium hypophosphite, and be transferred in Ultrasound Instrument and carry out ultrasonic 15min, produce mixture B；
S2, mixture roasting and reduction：Mixture after S1 step process is added in high temperature furnace, and in 30min
600 DEG C are inside warming up to, keeps 30min, then the temperature of high temperature furnace is risen to 850 DEG C, while carbon monoxide is passed through into high temperature furnace,
After carbon monoxide be passed through the time rise to 850 DEG C more than 30min and temperature after to start timing soaking time be 90min, insulation terminates
After be cooled to room temperature；
S3, post processing：The mixture reduced is transferred in pulverizer and crushed, transfers to ultrasonic powder in Ultrasound Instrument
It is broken, finally it is transferred in mill and grinds, and the screen cloth crossed more than 200 mesh, produce LED fluorescent powder.
In the present invention, the addition quality of fluxing agent is the 2% of the total compound of fluorescent material；Ammonium phosphate and the sodium hypophosphite group
The addition quality of compound is the 4% of fluorescent material gross mass, and the mass ratio of ammonium phosphate and sodium hypophosphite is 3：1.
Embodiment six
A kind of LED fluorescent powder proposed by the present invention, the chemical formula of the fluorescent material is Sr0.4A5M0.5Al3O12:(Tb3+Eu2 + 0.1)。
Its preparation method, comprise the following steps：
S1, raw material mixing and pretreatment：According to the chemical general formula Sr of fluorescent material0.4A5M0.5Al3O12:(Tb3+Eu2+ 0.1)
Raw material is weighed, and adds mass ratio as 1.5：3：25 BiF3、NH4F and B2O3, it is well mixed to produce mixture A, by mixture A
It is placed in mill and is ground, the screen cloth crossed more than 100 mesh, the mixture A after grinding is produced, to the mixture A after grinding
It is middle to add the composition of ammonium phosphate and sodium hypophosphite, and be transferred in Ultrasound Instrument and carry out ultrasonic 15min, produce mixture B；
S2, mixture roasting and reduction：Mixture after S1 step process is added in high temperature furnace, and in 30min
600 DEG C are inside warming up to, keeps 30min, then the temperature of high temperature furnace is risen to 850 DEG C, while carbon monoxide is passed through into high temperature furnace,
After carbon monoxide be passed through the time rise to 850 DEG C more than 30min and temperature after to start timing soaking time be 90min, insulation terminates
After be cooled to room temperature；
S3, post processing：The mixture reduced is transferred in pulverizer and crushed, transfers to ultrasonic powder in Ultrasound Instrument
It is broken, finally it is transferred in mill and grinds, and the screen cloth crossed more than 200 mesh, produce LED fluorescent powder.
In the present invention, the addition quality of fluxing agent is the 4% of the total compound of fluorescent material；Ammonium phosphate and the sodium hypophosphite group
The addition quality of compound is the 4% of fluorescent material gross mass, and the mass ratio of ammonium phosphate and sodium hypophosphite is 3：1.
Embodiment seven is identical with the chemical formula of the fluorescent material of example IV；Its preparation method, comprise the following steps：
S1, raw material mixing and pretreatment：According to the chemical general formula Sr of fluorescent material0.4A5M0.5Al3O12:(Tb3+Eu2+ 0.1)
Raw material is weighed, and adds mass ratio as 1：4：15 CeF3、NH4F and B2O3, it is well mixed to produce mixture A, mixture A is put
It is ground in mill, the screen cloth crossed more than 100 mesh, the mixture A after grinding is produced, into the mixture A after grinding
The composition of ammonium phosphate and sodium hypophosphite is added, and is transferred in Ultrasound Instrument and carries out ultrasonic 15min, produces mixture B；
S2, mixture roasting and reduction：Mixture after S1 step process is added in high temperature furnace, and in 30min
550 DEG C are inside warming up to, keeps 25min, then the temperature of high temperature furnace is risen to 750 DEG C, while carbon monoxide is passed through into high temperature furnace,
After carbon monoxide be passed through the time rise to 750 DEG C more than 30min and temperature after to start timing soaking time be 60min, insulation terminates
After be cooled to room temperature；
S3, post processing：The mixture reduced is transferred in pulverizer and crushed, transfers to ultrasonic powder in Ultrasound Instrument
It is broken, finally it is transferred in mill and grinds, and the screen cloth crossed more than 200 mesh, produce LED fluorescent powder.
In this present invention, the addition quality of fluxing agent is the 2% of the total compound of fluorescent material；The ammonium phosphate and sodium hypophosphite
The addition quality of composition is the 4% of fluorescent material gross mass, and the mass ratio of ammonium phosphate and sodium hypophosphite is 5：It is real unlike 1
It is the 5% of fluorescent material gross mass to apply the addition of ammonium phosphate and sodium hypophosphite composition in example seven.
Light efficiency detection is carried out to fluorescent material prepared by embodiment one~seven, it is as a result as follows：
| Embodiment | One | Two | Three | Four | Five | Six | Seven |
| Light efficiency lm/W | 83 | 82 | 83 | 84 | 83 | 88 | 84 |
Experimental result shows that the light efficiency test result of fluorescent material prepared by embodiment one~seven is similar, and light efficiency can reach
To 82lm/W, embodiment six is even up to 88lm/W, and compared to below the 80lm/W of prior art, light efficiency significantly improves；Implement
The fluorescent material chemical formula of example one~tetra- is different, but obtained light efficiency result is basically identical, shows the fluorescent material formula in the present invention
Rationally, and favorable reproducibility；The light efficiency result of example IV, embodiment five and embodiment six shows, the species and dosage of fluxing agent
Also the size of preparation that can be to fluorescer and light efficiency has an impact, and CeF3、NH4F and B2O3Combined effect than BiF3、
NH4F and B2O3Combine；The light efficiency result of example IV and embodiment seven shows, using ammonium phosphate and sodium hypophosphite as combination
Help reducing agent to reduce sintering temperature on the premise of light efficiency is kept, shorten roasting time, and then show to help adding for reducing agent
Enter to make reaction condition more gentle.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of LED fluorescent powder, it is characterised in that the chemical general formula of the fluorescent material is Sr0.4AaMbAl3O12:(Tb3+ xEu2+ y),
Wherein M is any one element in La, Lu, Y, any one element in A Ca, Ba, Zn, Mg, 1.5≤a≤5,0.04
≤ b≤3,0≤x≤3,0.01≤y≤0.1.
2. a kind of LED fluorescent powder according to claim 1, it is characterised in that the x is 0,1,2 or 3.
A kind of 3. LED fluorescent powder according to claim 1, it is characterised in that the Eu2+From the compound containing Eu,
Wherein it is preferably the oxides, divalent of europium.
4. a kind of LED fluorescent powder according to claim 1, it is characterised in that the A derives from A oxide, carbonate
Or one kind in subcarbonate, the Sr are compound containing Sr, the M is the compound containing M, and the Tb is the chemical combination containing Tb
Thing, the Al are oxide or salt containing Al.
A kind of 5. LED fluorescent powder according to claim 1, it is characterised in that when the Tb is not 0, A and Tb mol ratio
For 0.5~5：1.
6. a kind of preparation method of LED fluorescent powder, it is characterised in that comprise the following steps：
S1, raw material mixing and pretreatment：According to the chemical general formula Sr of fluorescent material0.4AaMbAl3O12:(Tb3+ xEu2+ y) weigh original
Material, and fluxing agent is added, it is well mixed to produce mixture A, mixture A is placed in mill and is ground, is crossed more than 100 mesh
Screen cloth, produce the mixture A after grinding, the composition of ammonium phosphate and sodium hypophosphite added into the mixture A after grinding, and
Progress 10~20min of ultrasound in Ultrasound Instrument is transferred to, produces mixture B；
S2, mixture roasting and reduction：Mixture after S1 step process is added in high temperature furnace, and risen in 30min
Temperature keeps 20~30min to 550~650 DEG C, then the temperature of high temperature furnace is risen into 750~950 DEG C, while leads into high temperature furnace
Enter carbon monoxide, after carbon monoxide be passed through the time rise to 750~950 DEG C more than 30min and temperature after start timing soaking time
For 60~100min, insulation is cooled to room temperature after terminating；
S3, post processing：The mixture reduced is transferred in pulverizer and crushed, transfers to Ultrasonic Pulverization in Ultrasound Instrument, most
After be transferred in mill and grind, and the screen cloth crossed more than 200 mesh produces LED fluorescent powder.
A kind of 7. preparation method of LED fluorescent powder according to claim 6, it is characterised in that helping in the S1 steps
Solvent is chloric metal-salt, NH4F and B2O3Mixture, the chloric metal-salt, NH4F and B2O3Mass ratio be 0.5~1.5：3~
5：10~25.
8. the preparation method of a kind of LED fluorescent powder according to claim 7, it is characterised in that the chloric metal-salt is
CeF3、BiF3、PbF2In the mixing of any one or two kinds.
A kind of 9. preparation method of LED fluorescent powder according to claim 6, it is characterised in that the addition of the fluxing agent
Quality is the 1~4% of the total compound of fluorescent material.
10. the preparation method of a kind of LED fluorescent powder according to claim 6, it is characterised in that the ammonium phosphate and time phosphorus
The addition quality of sour composition of sodium be fluorescent material gross mass 0.5~5%, and the mass ratio of ammonium phosphate and sodium hypophosphite be 2~
5：1.
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