CN107338050A - Rare earth samarium activation molybdate base red fluorescent powder and preparation method thereof - Google Patents
Rare earth samarium activation molybdate base red fluorescent powder and preparation method thereof Download PDFInfo
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- CN107338050A CN107338050A CN201710508798.4A CN201710508798A CN107338050A CN 107338050 A CN107338050 A CN 107338050A CN 201710508798 A CN201710508798 A CN 201710508798A CN 107338050 A CN107338050 A CN 107338050A
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- 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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7776—Vanadates; Chromates; Molybdates; Tungstates
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Abstract
The invention discloses rare earth samarium to activate molybdate base red fluorescent powder, using molybdate as matrix, chemical general formula K5Y1‑x(MoO4)4:xSm3+, wherein 0.01≤x≤0.2, by adulterating active ions Sm3+, rare earth samarium activation molybdate base red fluorescent powder is prepared, can be effectively matched with existing light emitting diode, and luminous efficiency is high, stability is good, the red light composition being suitable as in white light LEDs, and chemical property is stable, and colour rendering is good；The invention also discloses its preparation method, by K2CO3、Y2O3、MoO3And Sm2O3Mixed grinding, calcine under air atmosphere, be incubated, be ground again after furnace cooling, finally obtain rare earth samarium activation molybdate base red fluorescent powder, prepared based on solid-phase synthesis, method is simple and easy, favorable reproducibility, short preparation period.
Description
Technical field
The invention belongs to rare earth luminescent material preparing technical field, and in particular to rare earth samarium activates molybdic acid alkali red fluorescence
Powder, the invention further relates to the preparation method of the red fluorescence powder.
Background technology
Light emitting diode (Light Emitting Diode, LED) is acknowledged as the light source of new generation of 21st century,
With consume energy low, fast, the green, long lifespan of response, high small volume and luminous efficiency many advantages, such as, illuminating and showing neck
There is huge application prospect in domain.At present, obtained more using europium ion as activator in white light for illumination LED red fluorescence powder
Red light composition is obtained, it is more single.Therefore the rare earth ion for developing new burn red has certain realistic meaning, and samarium from
The light (~565nm ,~600nm and~646nm) at three peaks can be launched after son absorption ultraviolet light, so as to show red
Light, this feature have good application value in the colour temperature for reducing white light LEDs.
The content of the invention
It is an object of the invention to provide rare earth samarium to activate molybdate base red fluorescent powder, can have with existing light emitting diode
Effect matching, and luminous efficiency is high, stability is good, the red light composition being suitable as in white light LEDs.
It is a further object to provide the preparation method of rare earth samarium activation molybdate base red fluorescent powder.
The technical solution adopted in the present invention is, using molybdate as matrix, chemical general formula K5Y1-x(MoO4)4:xSm3+, its
In 0.01≤x≤0.2.
Another technical scheme of the present invention is that rare earth samarium activates the preparation side of molybdate base red fluorescent powder
Method, specifically implement according to following steps：
Step 1, by chemical general formula K5Y1-x(MoO4)4:xSm3+Mol ratio, wherein 0.01≤x≤0.2, is weighed respectively
Solid chemical compound containing K element, the solid chemical compound containing Y element, the solid chemical compound containing Mo elements and contain Sm elements
Solid chemical compound is as raw material；
Step 2, the raw mill for being weighed step 1 are simultaneously well mixed, and obtain raw mixture；
Step 3, the raw mixture for obtaining step 2 calcine 3h~6h in air atmosphere, and calcining heat is 600 DEG C~
850 DEG C, cool to room temperature after the completion of calcining with the furnace, obtain calcined product；
Step 4, the calcined product for obtaining step 3 are ground, and obtain rare earth samarium activation molybdate base red fluorescent powder.
The features of the present invention also resides in,
The solid chemical compound containing K element is K in step 12CO3, the solid chemical compound containing Y element is Y2O3, contain Mo elements
Solid chemical compound be MoO3, the solid chemical compound containing Sm elements is Sm2O3。
Milling time is 30min~60min in step 2.
Using the resistance furnace that is rapidly heated, heating rate is 5 DEG C/min~8 DEG C/min for calcining in step 3.
Milling time is 10min~30min in step 4.
The invention has the advantages that
Rare earth samarium of the present invention activates molybdate base red fluorescent powder, using molybdate as matrix, by adulterating active ions Sm3 +, rare earth samarium activation molybdate base red fluorescent powder is prepared, excitation wavelength is 350nm~500nm, launch wavelength 550nm
~680nm, main emission peak are located at 646nm, belong to red optical range, can be effectively matched with existing light emitting diode, and luminous
Efficiency high, stability is good, the red light composition being suitable as in white light LEDs, and chemical property is stable, good luminous performance, lights strong
Degree is high, and colour rendering is good；
The preparation method of rare earth samarium activation molybdate base red fluorescent powder of the present invention, using high temperature solid-state method, does not add and helps
Flux, calcine at the temperature in air atmosphere, relatively low, technological process apparatus requirement is simple, and experiment condition easily reaches, production week
Phase is short, and favorable reproducibility can be used for industrialized production.
Brief description of the drawings
Fig. 1 is the K that embodiment 2 is prepared5Y0.98(MoO4)4:0.02Sm3+The XRD spectrum of red fluorescence powder；
Fig. 2 is the K that embodiment 4 is prepared5Y0.94(MoO4)4:0.06Sm3+The excitation spectrum of red fluorescence powder and transmitting
Spectrum；
Fig. 3 is the K that embodiment 6 is prepared5Y0.9(MoO4)4:0.1Sm3+The CIE chromaticity coordinates figures of red fluorescence powder.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
Rare earth samarium of the present invention activates molybdate base red fluorescent powder, using molybdate as matrix, chemical general formula K5Y1-x
(MoO4)4:xSm3+, wherein 0.01≤x≤0.2.
The preparation method of rare earth samarium activation molybdate base red fluorescent powder of the present invention, specifically implements according to following steps：
Step 1, by chemical general formula K5Y1-x(MoO4)4:xSm3+Mol ratio, wherein 0.01≤x≤0.2, is weighed respectively
K2CO3、Y2O3、MoO3And Sm2O3As raw material；
Step 2, will all raw materials that weighed in step 1 mix after grind 30min~60min it is to be mixed uniformly after, formed
Compound；
Step 3, the compound obtained through step 2 calcined to 3h~6h under air atmosphere, heating rate be 5 DEG C/min~
8 DEG C/min, calcining heat is 600 DEG C~850 DEG C, cools to room temperature after the completion of calcining with the furnace, obtains calcined product；
Wherein, synthesized during calcining according to following chemical equation：
5/2K2CO3+(1-x)/2Y2O3+4MoO3+x/2Sm2O3=K5Y(MoO4)4:xSm3++5/2CO2；
Step 4, the calcined product for obtaining step 3 grind 10min~30min, and it is red to obtain rare earth samarium activation molybdic acid alkali
Color fluorescent material.
Embodiment 1
X=0.01 is taken, by chemical formula K5Y0.99(MoO4)4:0.01Sm3+Stoichiometric, claimed respectively with electronic balance
Take K2CO3、Y2O3、MoO3And Sm2O3As raw material, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；
30min is ground after the above-mentioned all raw materials weighed are mixed, makes to be well mixed between raw material, obtains compound；It is mixed by what is obtained
Close material to be fitted into corundum crucible, and the corundum crucible be placed in and is rapidly heated in resistance furnace, calcined under air atmosphere, during which with
5 DEG C/min heating rate rises to 600 DEG C, is incubated 3h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, is forged
Burn product；The product regrinding 10min after calcining is taken out, that is, it is K to obtain chemical formula5Y0.99(MoO4)4:0.01Sm3+Rare earth samarium
Activate molybdate base red fluorescent powder.
Embodiment 2
X=0.02 is taken, by chemical formula K5Y0.98(MoO4)4:0.02Sm3+Stoichiometric, claimed respectively with electronic balance
Take K2CO3、Y2O3、MoO3And Sm2O3As raw material, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；
40min is ground after the above-mentioned all raw materials weighed are mixed, makes to be well mixed between raw material, obtains compound；It is mixed by what is obtained
Close material to be fitted into corundum crucible, and the corundum crucible be placed in and is rapidly heated in resistance furnace, calcined under air atmosphere, during which with
7 DEG C/min heating rate rises to 750 DEG C, is incubated 5h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, is forged
Burn product；The product regrinding 20min after calcining is taken out, that is, it is K to obtain chemical formula5Y0.98(MoO4)4:0.02Sm3+Rare earth samarium
Activate molybdate base red fluorescent powder.
Fig. 1 is the K obtained using the preparation method in embodiment 25Y0.98(MoO4)4:0.02Sm3+X-ray diffractogram
Spectrum, as can see from Figure 1：The test result of the present embodiment matches with standard PDF cards 47-0898, prepared by this explanation
Fluorescent material it is purer, it is hexagonal structure, space group R-3m.
Embodiment 3
X=0.04 is taken, by chemical formula K5Y0.96(MoO4)4:0.04Sm3+Stoichiometric, claimed respectively with electronic balance
Take K2CO3、Y2O3、MoO3And Sm2O3As raw material, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；
60min is ground after the above-mentioned all raw materials weighed are mixed, makes to be well mixed between raw material, obtains compound；It is mixed by what is obtained
Close material to be fitted into corundum crucible, and the corundum crucible be placed in and is rapidly heated in resistance furnace, calcined under air atmosphere, during which with
8 DEG C/min heating rate rises to 850 DEG C, is incubated 6h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, is forged
Burn product；The product regrinding 30min after calcining is taken out, that is, it is K to obtain chemical formula5Y0.96(MoO4)4:0.04Sm3+Rare earth samarium
Activate molybdate base red fluorescent powder.
Embodiment 4
X=0.06 is taken, by chemical formula K5Y0.94(MoO4)4:0.06Sm3+Stoichiometric, claimed respectively with electronic balance
Take K2CO3、Y2O3、MoO3And Sm2O3As raw material, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；
55min is ground after the above-mentioned all raw materials weighed are mixed, makes to be well mixed between raw material, obtains compound；It is mixed by what is obtained
Close material to be fitted into corundum crucible, and the corundum crucible be placed in and is rapidly heated in resistance furnace, calcined under air atmosphere, during which with
7 DEG C/min heating rate rises to 800 DEG C, is incubated 5.5h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, obtains
Calcined product；The product regrinding 15min after calcining is taken out, that is, it is K to obtain chemical formula5Y0.94(MoO4)4:0.06Sm3+Rare earth
Samarium activates molybdate base red fluorescent powder.
Fig. 2 is the K being prepared using the preparation method in embodiment 45Y0.94(MoO4)4:0.06Sm3+Fluorescent material swashs
Luminous spectrum and emission spectrum, as can be seen from Fig. 2：Main excitation peak 405nm, can be existing positioned at ultraviolet light to blue region
LED chip effectively excites, and its main emission peak is located at 646nm, launches bright feux rouges, can be as the red in white light LEDs
Light composition.
Embodiment 5
X=0.08 is taken, by chemical formula K5Y0.92(MoO4)4:0.08Sm3+Stoichiometric, claimed respectively with electronic balance
Take K2CO3、Y2O3、MoO3And Sm2O3As raw material, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；
35min is ground after the above-mentioned all raw materials weighed are mixed, makes to be well mixed between raw material, obtains compound；It is mixed by what is obtained
Close material to be fitted into corundum crucible, and the corundum crucible be placed in and is rapidly heated in resistance furnace, calcined under air atmosphere, during which with
5 DEG C/min heating rate rises to 650 DEG C, is incubated 3.5h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, obtains
Calcined product；The product regrinding 30min after calcining is taken out, that is, it is K to obtain chemical formula5Y0.92(MoO4)4:0.08Sm3+Rare earth
Samarium activates molybdate base red fluorescent powder.
Embodiment 6
X=0.1 is taken, by chemical formula K5Y0.9(MoO4)4:0.1Sm3+Stoichiometric, weighed respectively with electronic balance
K2CO3、Y2O3、MoO3And Sm2O3As raw material, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Will
30min is ground after the above-mentioned all raw materials mixing weighed, makes to be well mixed between raw material, obtains compound；The mixing that will be obtained
Material is fitted into corundum crucible, and the corundum crucible is placed in and is rapidly heated in resistance furnace, is calcined under air atmosphere, during which with 7
DEG C/min heating rate rises to 800 DEG C, 5h is incubated, waits furnace cooling after the completion of calcining, until being cooled to room temperature, is calcined
Product；The product regrinding 25min after calcining is taken out, that is, it is K to obtain chemical formula5Y0.9(MoO4)4:0.1Sm3+Rare earth samarium activates
Molybdate base red fluorescent powder.
Fig. 3 is the K being prepared using the preparation method in embodiment 65Y0.9(MoO4)4:0.1Sm3+The CIE colors of fluorescent material
Coordinate diagram, as can see from Figure 3：K5Y0.9(MoO4)4:0.1Sm3+The chromaticity coordinates of fluorescent material sample is (0.611,0.387), is shown
It is shown as red light.
Embodiment 7
X=0.15 is taken, by chemical formula K5Y0.85(MoO4)4:0.15Sm3+Stoichiometric, claimed respectively with electronic balance
Take K2CO3、Y2O3、MoO3And Sm2O3As raw material, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；
30min is ground after the above-mentioned all raw materials weighed are mixed, makes to be well mixed between raw material, obtains compound；It is mixed by what is obtained
Close material to be fitted into corundum crucible, and the corundum crucible be placed in and is rapidly heated in resistance furnace, calcined under air atmosphere, during which with
5 DEG C/min heating rate rises to 800 DEG C, is incubated 6h, waits furnace cooling after the completion of calcining, until being cooled to room temperature, is forged
Burn product；The product regrinding 15min after calcining is taken out, that is, it is K to obtain chemical formula5Y0.85(MoO4)4:0.15Sm3+Rare earth samarium
Activate molybdate base red fluorescent powder.
Embodiment 8
X=0.2 is taken, by chemical formula K5Y0.8(MoO4)4:0.2Sm3+Stoichiometric, weighed respectively with electronic balance
K2CO3、Y2O3、MoO3And Sm2O3As raw material, the purity of its middle rare earth is 99.99%, and remaining is that analysis is pure；Will
35min is ground after the above-mentioned all raw materials mixing weighed, makes to be well mixed between raw material, obtains compound；The mixing that will be obtained
Material is fitted into corundum crucible, and the corundum crucible is placed in and is rapidly heated in resistance furnace, is calcined under air atmosphere, during which with 7
DEG C/min heating rate rises to 850 DEG C, 6h is incubated, waits furnace cooling after the completion of calcining, until being cooled to room temperature, is calcined
Product；The product regrinding 20min after calcining is taken out, that is, it is K to obtain chemical formula5Y0.8(MoO4)4:0.2Sm3+Rare earth samarium activates
Molybdate base red fluorescent powder.
Rare earth samarium of the present invention activates molybdate base red fluorescent powder, using molybdate as matrix, by adulterating active ions Sm3 +, rare earth samarium activation molybdate base red fluorescent powder, the MoO in molybdate is prepared4 2-The special nature having due to itself,
The ultraviolet light to blue region can be effectively absorbed, and transfers energy to Doped ions, so as to very high luminous strong
Degree；Rare earth samarium activation molybdate base red fluorescent powder is prepared, excitation wavelength is 350nm~500nm, and launch wavelength is
550nm~680nm, main emission peak are located at 646nm, belong to red optical range, can be effectively matched with existing light emitting diode, and
Luminous efficiency is high, and stability is good, the red light composition being suitable as in white light LEDs, and chemical property is stable, good luminous performance, hair
Luminous intensity is high, and colour rendering is good；
The preparation method of rare earth samarium activation molybdate base red fluorescent powder of the present invention, using high temperature solid-state method, does not add and helps
Flux, calcine at the temperature in air atmosphere, relatively low, technological process apparatus requirement is simple, and experiment condition easily reaches, production week
Phase is short, and favorable reproducibility can be used for industrialized production.
Claims (6)
1. rare earth samarium activates molybdate base red fluorescent powder, it is characterised in that using molybdate as matrix, chemical general formula K5Y1-x
(MoO4)4:xSm3+, wherein 0.01≤x≤0.2.
A kind of 2. preparation method of rare earth samarium activation molybdate base red fluorescent powder as claimed in claim 1, it is characterised in that
Specifically implement according to following steps：
Step 1, by chemical general formula K5Y1-x(MoO4)4:xSm3+Mol ratio, wherein 0.01≤x≤0.2, weigh respectively containing K members
Solid chemical compound, the solid chemical compound containing Y element, the solid chemical compound containing Mo elements and the solidification containing Sm elements of element
Compound is as raw material；
Step 2, the raw mill for being weighed step 1 are simultaneously well mixed, and obtain raw mixture；
Step 3, the raw mixture for obtaining step 2 calcine 3h~6h in air atmosphere, and calcining heat is 600 DEG C~850
DEG C, cool to room temperature after the completion of calcining with the furnace, obtain calcined product；
Step 4, the calcined product for obtaining step 3 are ground, and obtain rare earth samarium activation molybdate base red fluorescent powder.
3. the preparation method of rare earth samarium activation molybdate base red fluorescent powder according to claim 2, it is characterised in that
In the step 1：Solid chemical compound containing K element is K2CO3, the solid chemical compound containing Y element is Y2O3, contain Mo elements
Solid chemical compound is MoO3, the solid chemical compound containing Sm elements is Sm2O3。
4. the preparation method of rare earth samarium activation molybdate base red fluorescent powder according to claim 2, it is characterised in that institute
It is 30min~60min to state milling time in step 2.
5. the preparation method of rare earth samarium activation molybdate base red fluorescent powder according to claim 2, it is characterised in that institute
Stating calcining in step 3, using the resistance furnace that is rapidly heated, heating rate is 5 DEG C/min~8 DEG C/min.
6. the preparation method of rare earth samarium activation molybdate base red fluorescent powder according to claim 2, it is characterised in that institute
It is 10min~30min to state milling time in step 4.
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| CN109463547A (en) * | 2018-11-30 | 2019-03-15 | 深圳农畉食品开发集团有限公司 | It is a kind of for treating the feed addictive and preparation method thereof of pig perosis |
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| CN112898975A (en) * | 2021-03-10 | 2021-06-04 | 旦宇科技江苏有限公司 | Preparation method and application of samarium ion activated phosphate luminescent ceramic |
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