CN108192614A - A kind of white light LEDs full spectral emissions fluorescent powder and preparation method thereof - Google Patents

A kind of white light LEDs full spectral emissions fluorescent powder and preparation method thereof Download PDF

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Publication number
CN108192614A
CN108192614A CN201810019680.XA CN201810019680A CN108192614A CN 108192614 A CN108192614 A CN 108192614A CN 201810019680 A CN201810019680 A CN 201810019680A CN 108192614 A CN108192614 A CN 108192614A
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fluorescent powder
present
full spectral
spectral emissions
white light
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吴铭
邓德刚
黄飞飞
田颖
张军杰
华有杰
徐时清
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China Jiliang University
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China Jiliang University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7715Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
    • C09K11/7723Phosphates
    • C09K11/7724Phosphates with alkaline earth metals
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02BCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

Abstract

The present invention relates to rare earth luminescent material technical fields.A kind of full spectral emissions fluorescent powder of white light LEDs, the fluorescent powder have following chemical representation:(M19‑yMgy)Ce1‑x(PO4)14:xSn4+, in formula, x=0.001~0.1, y=1~5, any one in M Ca, Sr and Ba.The fluorescent powder good dispersion, uniform granularity, chemical stability are good, thermal stability is good, luminous efficiency is high, and excitation band covers ultraviolet, purple light and blue region, can be used as white light LEDs single-matrix fluorescent powder.

Description

A kind of white light LEDs full spectral emissions fluorescent powder and preparation method thereof
Technical field
The present invention relates to rare earth luminescent material technical field, more particularly, to a kind of full spectral emissions fluorescence of white light LEDs Powder and preparation method thereof.
Background technology
White light LEDs are a kind of solid-state semiconductor devices for converting electrical energy into white light, have energy conservation and environmental protection, it is easy to use, The advantages that safety, long lifespan, luminous efficiency are high, small, it is considered to be after incandescent lamp, fluorescent lamp, high-voltage gas discharging light it Forth generation lighting source afterwards, being widely used for it open the new era of " green illumination ".
From the point of view of the synthetic method of white light LEDs and the current situation of fluorescent powder, realizing the major way of white light LEDs is The body fluorescence conversion technology of LED chip+fluorescent powder.Therefore, the performance of fluorescent powder directly determines the quality of white light LEDs.At present, it is real Existing white light LEDs mainly have three ways, such as following:(1) blue-light LED chip is combined with yellow fluorescent material;Blue-light LED chip with it is red Color and green fluorescent material combination;(3) purple LED chip is combined with fluorescent material with three basic colour.The first combination operation is simple, into This is low, and driving circuit design is simple, and good process repeatability has become the preparation method of most ripe commercialization white light LEDs at present. But due to lacking red color light component in yellow fluorescent powder, the partially narrow white light colour rendering for leading to synthesis of spectrum is poor, and colour rendering index is paid no attention to Think.Simultaneously because the influence of driving current and temperature, leads to white light as aging occurs in the increase of usage time and causes white light Drift.
With the development of technology, semi-conductor LED chips develop to ultraviolet region from blue light, and increasingly to energy High, short wavelength direction is developed.Therefore, purple LED chip+can be by three base of red, green, blue that ultraviolet and purple light effectively excites is utilized Color phosphor combination realizes that the transmitting of white light is considered as the new method for replacing the former.The energy ratio blue light of UV photons is high, fits It is more for the fluorescent powder system of ultraviolet excitation, so the selectivity of fluorescent powder is consequently increased.In addition, in this mixed light mistake Cheng Zhong, ultraviolet light are not involved in mixed light in itself, and all from fluorescent powder, the white light synthesized in this way is shown obtained white light Colour index is high, adjustable color, is the mainstream of following white light LEDs.At present, this combine significantly is asked existing for obtained white light LEDs Topic is that the efficiency of ultraviolet LED is relatively low, and cost is slightly higher.In addition, then existing color is reabsorbed and is matched between phosphor mixture Regulation and control problem can make the luminous efficiency of LED and color reducibility be a greater impact, and use ultraviolet-near ultraviolet chip excitation single The full spectral emissions fluorescent powder of matrix realizes that white light emission can then avoid these problems, therefore, the single full spectral emissions fluorescence of matrix Powder becomes the research hotspot of current illumination field.
Invention content
It is an object of the present invention to provide a kind of physical and chemical performance stabilizations, can realize the white of visible light full spectrum transmitting The full spectral emissions fluorescent powders of light LED;It is a further object to provide the full spectral emissions fluorescent powders of above-mentioned white light LEDs Preparation method.
To achieve the above object, the technical solution used in the present invention:A kind of full spectral emissions fluorescent powder of white light LEDs, The fluorescent powder has following chemical representation:(M19-yMgy)Ce1-x(PO4)14:xSn4+, in formula, x=0.001~0.1, y=1~ Any one in 5, M Ca, Sr and Ba.
A kind of white light LEDs preparation method of full spectral emissions fluorescent powder, includes the following steps:(1) with magnesium carbonate, containing M Compound, ceria, containing [PO4]3-Compound and stannic oxide, by chemical expression (M19-yMgy)Ce1-x(PO4)14: xSn4+, wherein, x=0.001~0.1, y=1~5, any one in M Ca, Sr and Ba obtain mixture;(2) by mixture Crucible is packed into, is sintered 2~4 hours under the conditions of 1300~1400 DEG C under air atmosphere in high temperature furnace, postcooling is obtained to room temperature To the full spectral emissions fluorescent powder.
Preferably, the compound containing M is any one in calcium carbonate, strontium carbonate and barium carbonate.
Preferably, containing [PO4]3-Compound is a kind of in diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
Compared with prior art, the beneficial effects of the invention are as follows:(1) fluorescent powder of the invention is using phosphate as matrix material Material has the advantages such as chemical stability is good, and thermal stability is good, low in raw material price, rich reserves, and sintering temperature is low.Compared to sulphur Compound fluorescent powder, thermal stability of the present invention are good.Compared to silicate fluorescent powder, grain graininess of the present invention is uniform, and sintering temperature is relatively low. Compared to silicon substrate nitrogen (oxygen) compound fluorescent powder, synthesis technology of the present invention is simple, and sintering temperature is low and low in raw material price, reserves are rich It is rich.Compared to aluminate fluorescent powder, preparation temperature of the present invention is low, and grain diameter is smaller, and light emission luminance and luminous efficiency are high, and physics Stable chemical performance.(2) fluorescent powder of the invention is without the rare earth element of price costly, and preparation condition is mild, is not required to Want high temperature and reducing atmosphere.(3) fluorescent powder of the invention can realize that visible light full spectrum emits.The fluorescent powder good dispersion, Epigranular, chemical stability are good, thermal stability is good, luminous efficiency is high, and excitation band covers ultraviolet, purple light and blue region, White light LEDs single-matrix fluorescent powder can be used as.
Description of the drawings
Fig. 1 is fluorescent powder exciting light spectrogram prepared by the embodiment of the present invention 1.
Fig. 2 is fluorescent powder launching light spectrogram prepared by the embodiment of the present invention 1.
Fig. 3 is fluorescent powder XRD spectrum and Ca prepared by the embodiment of the present invention 119Ce(PO4)14Standard diagram.
Specific embodiment
Embodiment 1
A kind of white light LEDs are with full spectral emissions fluorescent powder, chemical representation:(Ca18Mg)Ce0.999(PO4)14: 0.001Sn4+
According to (Ca18Mg)Ce0.999(PO4)14:0.001Sn4+Weigh CaCO3、MgCO3、CeO2、(NH4)2HPO4And SnO2, Molar ratio between them is 18:1:0.999:14:0.001, it is fully ground after mixing, places in corundum crucible, then put Enter in high temperature furnace and roasted 2 hours at 1400 DEG C under air atmosphere, be subsequently cooled to room temperature, obtain full spectral emissions fluorescent powder.
Fig. 1 is fluorescent powder exciting light spectrogram manufactured in the present embodiment, and 610 nanometers of supervisory wavelength can from Fig. 1 Go out, the fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak be located at 275nm, Near 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can effectively be excited by ultraviolet and purple light chip. Fig. 2 is fluorescent powder launching light spectrogram manufactured in the present embodiment, 300 nanometers of excitation wavelength, when the excitation wavelength of emission spectrum is 300nm, from figure 2 it can be seen that the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak be located at respectively 400nm, Near 500nm and 614nm, illustrate that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light activated full spectral emissions are glimmering Light powder.Fig. 3 is fluorescent powder XRD spectrum manufactured in the present embodiment and Ca19Ce(PO4)14Standard diagram (ICSD-83401), from As can be seen that the fluorescent powder XRD spectrum of the present embodiment shows the d values of product and relative intensity variation tendency and standard in Fig. 3 Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 2
According to (Ca18Mg)Ce0.9(PO4)14:0.1Sn4+Weigh CaCO3、MgCO3、CeO2、NH4H2PO4And SnO2, they it Between molar ratio be 18:1:0.9:14:0.1, it is fully ground after mixing, places in corundum crucible, place into high temperature furnace It is roasted 4 hours at 1300 DEG C under air atmosphere, is subsequently cooled to room temperature, obtains full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 3
According to (Ca16Mg3)Ce0.99(PO4)14:0.01Sn4+Weigh CaCO3、MgCO3、CeO2、(NH4)2HPO4And SnO2, it Between molar ratio be 16:3:0.99:14:0.001, it is fully ground after mixing, places in corundum crucible, place into height It is roasted 3 hours at 1350 DEG C under air atmosphere in warm stove, is subsequently cooled to room temperature, obtains full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 4
According to (Ca14Mg5)Ce0.95(PO4)14:0.05Sn4+Weigh CaCO3、MgCO3、CeO2、NH4H2PO4And SnO2, they Between molar ratio be 14:5:0.95:14:0.05, it is fully ground after mixing, places in corundum crucible, place into high temperature It is roasted 3 hours at 1350 DEG C under air atmosphere in stove, is subsequently cooled to room temperature, obtains full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 5
According to (Sr18Mg)Ce0.999(PO4)14:0.001Sn4+Weigh SrCO3、MgCO3、CeO2、(NH4)2HPO4And SnO2, Molar ratio between them is 18:1:0.999:14:0.001, it is fully ground after mixing, places in corundum crucible, then put Enter in high temperature furnace and roasted 2 hours at 1400 DEG C under air atmosphere, be subsequently cooled to room temperature, obtain full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 6
According to (Sr18Mg)Ce0.9(PO4)14:0.1Sn4+Weigh SrCO3、MgCO3、CeO2、NH4H2PO4And SnO2, they it Between molar ratio be 18:1:0.9:14:0.1, it is fully ground after mixing, places in corundum crucible, place into high temperature furnace It is roasted 4 hours at 1300 DEG C under air atmosphere, is subsequently cooled to room temperature, obtains full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 7
According to (Sr16Mg3)Ce0.99(PO4)14:0.01Sn4+Weigh SrCO3、MgCO3、CeO2、(NH4)2HPO4And SnO2, it Between molar ratio be 16:3:0.99:14:0.001, it is fully ground after mixing, places in corundum crucible, place into height It is roasted 3 hours at 1350 DEG C under air atmosphere in warm stove, is subsequently cooled to room temperature, obtains full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 8
According to (Sr14Mg5)Ce0.95(PO4)14:0.05Sn4+Weigh SrCO3、MgCO3、CeO2、NH4H2PO4And SnO2, they Between molar ratio be 14:5:0.95:14:0.05, it is fully ground after mixing, places in corundum crucible, place into high temperature It is roasted 3 hours at 1350 DEG C under air atmosphere in stove, is subsequently cooled to room temperature, obtains full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 9
According to (Ba18Mg)Ce0.999(PO4)14:0.001Sn4+Weigh BaCO3、MgCO3、CeO2、(NH4)2HPO4And SnO2, Molar ratio between them is 18:1:0.999:14:0.001, it is fully ground after mixing, places in corundum crucible, then put Enter in high temperature furnace and roasted 2 hours at 1400 DEG C under air atmosphere, be subsequently cooled to room temperature, obtain full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 10
According to (Ba18Mg)Ce0.9(PO4)14:0.1Sn4+Weigh BaCO3、MgCO3、CeO2、NH4H2PO4And SnO2, they it Between molar ratio be 18:1:0.9:14:0.1, it is fully ground after mixing, places in corundum crucible, place into high temperature furnace It is roasted 4 hours at 1300 DEG C under air atmosphere, is subsequently cooled to room temperature, obtains full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 11
According to (Ba16Mg3)Ce0.99(PO4)14:0.01Sn4+Weigh BaCO3、MgCO3、CeO2、(NH4)2HPO4And SnO2, it Between molar ratio be 16:3:0.99:14:0.001, it is fully ground after mixing, places in corundum crucible, place into height It is roasted 3 hours at 1350 DEG C under air atmosphere in warm stove, is subsequently cooled to room temperature, obtains full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Embodiment 12
According to (Ba14Mg5)Ce0.95(PO4)14:0.05Sn4+Weigh CaCO3、MgCO3、CeO2、NH4H2PO4And SnO2, they Between molar ratio be 14:5:0.95:14:0.05, it is fully ground after mixing, places in corundum crucible, place into high temperature It is roasted 3 hours at 1350 DEG C under air atmosphere in stove, is subsequently cooled to room temperature, obtains full spectral emissions fluorescent powder.
The fluorescent powder excitation spectrum of the present embodiment is a wide range, covers ultraviolet, purple light and blue region, excitation peak is located at Near 275nm, 300nm and 400nm, spectrum peak is high, illustrates the fluorescent powder of the present embodiment and can be had by ultraviolet and purple light chip Effect excitation.When the excitation wavelength of emission spectrum is 300nm, the fluorescent powder of the present embodiment is emitted as full spectral emissions, emission peak It is located near 400nm, 500nm and 614nm respectively, illustrates that the fluorescent powder of the present embodiment is suitble to do ultraviolet, purple light and blue light excitation Full spectral emissions fluorescent powder.The d values and relative intensity variation tendency and mark of the fluorescent powder XRD spectrum display product of the present embodiment Accurate Ca19Ce(PO4)14Standard card (ICSD-83401) unanimously, illustrates that the fluorescence powder purity of the present embodiment synthesis is higher.
Above-described embodiment be used for illustrate the present invention rather than limit the invention, the present invention spirit and In scope of the claims, to any modifications and changes that the present invention makes, protection scope of the present invention is both fallen within.

Claims (4)

1. the full spectral emissions fluorescent powder of a kind of white light LEDs, it is characterised in that the fluorescent powder has following chemical representation:(M19- yMgy)Ce1-x(PO4)14:xSn4+, in formula, x=0.001~0.1, y=1~5, any one in M Ca, Sr and Ba.
2. a kind of white light LEDs preparation method of full spectral emissions fluorescent powder, it is characterised in that include the following steps:(1) with carbon Sour magnesium, compound, ceria containing M, containing [PO4]3-Compound and stannic oxide, by chemical expression (M19-yMgy)Ce1-x (PO4)14:xSn4+, wherein, x=0.001~0.1, y=1~5, any one in M Ca, Sr and Ba obtain mixture;(2) Crucible is filled this blend into, is sintered 2~4 hours under the conditions of 1300~1400 DEG C under air atmosphere in high temperature furnace, postcooling The full spectral emissions fluorescent powder is obtained to room temperature.
3. the white light LEDs as claimed in claim 2 preparation method of full spectral emissions fluorescent powder, it is characterised in that described to contain M Compound be any one in calcium carbonate, strontium carbonate and barium carbonate.
4. the white light LEDs as claimed in claim 2 preparation method of full spectral emissions fluorescent powder, it is characterised in that described to contain [PO4 ]3-Compound is a kind of in diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
CN201810019680.XA 2018-01-09 2018-01-09 A kind of white light LEDs full spectral emissions fluorescent powder and preparation method thereof Pending CN108192614A (en)

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