CN107189779A - A kind of white light LEDs adjustable phosphate phosphor of spectrum and preparation method thereof - Google Patents
A kind of white light LEDs adjustable phosphate phosphor of spectrum and preparation method thereof Download PDFInfo
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- CN107189779A CN107189779A CN201710408192.3A CN201710408192A CN107189779A CN 107189779 A CN107189779 A CN 107189779A CN 201710408192 A CN201710408192 A CN 201710408192A CN 107189779 A CN107189779 A CN 107189779A
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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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7737—Phosphates
- C09K11/7738—Phosphates with alkaline earth metals
Abstract
The present invention relates to rare earth luminescent material technical field.A kind of white light LEDs adjustable phosphate phosphor of spectrum, the fluorescent material has following chemical representation：Ca9‑xM1.5(PO4)7：xEu2+, wherein, M is any one in Zn and Mg, and x is 0.001~0.10.The adjustable phosphate phosphor of white light LEDs spectrum has chemical stability and good thermal stability, the low advantage of the inexpensive production cost of raw material.
Description
Technical field
The present invention relates to rare earth luminescent material technical field, more particularly, to a kind of white light LEDs adjustable phosphate of spectrum
Fluorescent material and preparation method thereof.
Background technology
White light LEDs are a kind of solid-state semiconductor devices for converting electrical energy into white light, with energy-conserving and environment-protective, it is easy to use,
Safety, long lifespan, luminous efficiency are high, small volume the advantages of, it is considered to be after incandescent lamp, fluorescent lamp, high-voltage gas discharging light it
Forth generation lighting source afterwards, widely using for it opens the New Times of " green illumination ".
From the point of view of the synthetic method of white light LEDs and the current situation of fluorescent material, realizing the major way of white light LEDs is
The body fluorescence conversion technology of LED chip+fluorescent material.Therefore, the performance of fluorescent material directly determines the quality of white light LEDs.At present, it is real
Existing white light LEDs mainly have following three kinds of modes：(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 drive circuit design is simple, good process repeatability, at present the preparation method as most ripe commercialization white light LEDs.
But it is due to lack red color light component in yellow fluorescent powder, the partially narrow white light colour rendering for causing synthesis of spectrum is poor, and colour rendering index is paid no attention to
Think.Simultaneously because the influence of driving current and temperature, causes white light as aging occurs in the increase of use time and causes white light
Drift.
With the development of technology, semi-conductor LED chips develop into ultraviolet region from blue light, and increasingly to energy
The high, direction of short wavelength is developed.Therefore, the base of red, green, blue three for purple LED chip+can effectively be excited by ultraviolet and purple light is utilized
Color phosphor combination realizes that the transmitting of white light is considered as replacing the former new method.The energy ratio blue light of UV photons is high, fits
Fluorescent material system for ultraviolet excitation is more, so the selectivity of fluorescent material is consequently increased.In addition, in this mixed light mistake
Cheng Zhong, ultraviolet light is not involved in mixed light in itself, and obtained white light is all from fluorescent material, and the white light synthesized in this way shows
Colour index is high, and adjustable color is the main flow of following white light LEDs.At present, this obtained the obvious of white light LEDs presence that combine is asked
Topic is that the efficiency of ultraviolet LED is relatively low, and cost is slightly higher.In addition, often there is color reabsorption with matching somebody with somebody after a variety of fluorescent component mixing
The problem of than hardly possible regulation and control, and it is relatively low by the red fluorescence powder efficiency of burst of ultraviolel.Therefore, we can be glimmering by improving three primary colours
The luminous efficiency of light powder, so as to be combined with purple light chip, develops the adjustable fluorescent material of spectrum to make up in synthesis white light process
Middle color reabsorption and the low problem of rouge and powder efficiency.
The content of the invention
It is an object of the invention to provide a kind of chemical stability and heat endurance are good, the low white light LEDs of production cost are used up
Compose adjustable phosphate phosphor.It is a further object to provide the above-mentioned white light LEDs adjustable phosphate phosphor of spectrum
Preparation method.
To achieve the above object, the technical solution used in the present invention is：A kind of white light LEDs are glimmering with the adjustable phosphate of spectrum
Light powder, the fluorescent material has following chemical representation：Ca9-xM1.5(PO4)7：xEu2+, wherein, M is any one in Zn and Mg, x
For 0.001~0.10.
A kind of white light LEDs preparation method of the adjustable phosphate phosphor of spectrum, comprises the following steps：(1) with calcium carbonate,
Compound containing M, containing [PO4]3-Compound and europium oxide, by chemical expression Ca9-xM1.5(PO4)7：xEu2+Obtain mixture；
(2) mixture is loaded into crucible, sintered 2~4 hours under the conditions of under reducing atmosphere 1300~1400 DEG C in high temperature furnace, after
It is cooled to room temperature and obtains the adjustable phosphate phosphor of the spectrum.
Further, the compound containing M is one kind in magnesium carbonate and zinc oxide.
Further, it is described to contain [PO4]3-Compound is one kind in diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
Further, the reducing atmosphere is nitrogen and hydrogen mixture or CO atmosphere.
Compared with prior art, the beneficial effects of the invention are as follows：(1) fluorescent material of the invention is using phosphate as matrix material
Material, good with chemical stability, heat endurance is good, low in raw material price, rich reserves, the low advantage of sintering temperature.Compared to sulphur
Compound fluorescent material, heat endurance of the present invention is 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 material, synthesis technique 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 luminosity and luminous efficiency are high, and physics
Stable chemical performance；(2) present invention compares other phosphate phosphors (such as LiSrPO4：Eu2+、KSrPO4：Eu2+、Ca10K
(PO4)7：Eu3+), it is to avoid with deliquescent alkali carbonate in decomposition temperature height, exposure air.
Brief description of the drawings
Fig. 1 is fluorescent powder excitation spectrum figure prepared by the embodiment 1 that the present invention is provided.
Fig. 2 is phosphor emission spectrogram prepared by the embodiment 1 that the present invention is provided.
Fig. 3 is fluorescent material XRD spectrum prepared by the embodiment 1 that the present invention is provided.
Embodiment
Embodiment 1
According to Ca8.999Zn1.5(PO4)7：0.001Eu2+Weigh CaCO3、ZnO、(NH4)2HPO4And Eu2O3, between them
Mol ratio is 8.999：1.5：7：0.0005, be fully ground it is well mixed after, place in corundum crucible, place into high temperature furnace in
5%H2+ 95%N2It is calcined 2 hours at 1400 DEG C under the nitrogen and hydrogen mixture atmosphere of (volume ratio), is subsequently cooled to room temperature, obtains white light
The LED adjustable phosphate phosphors of spectrum.
Fig. 1 is the adjustable phosphate phosphor exciting light spectrogram of above-mentioned white light LEDs spectrum, 467 nanometers of supervisory wavelength, from figure
As can be seen that the fluorescent material PLE of the present embodiment is a wide range in 1, ultraviolet and violet region is covered, excitation peak is located at
Near 291nm and 425nm, spectrum peak is high, illustrates the fluorescent material of the present embodiment and can effectively be excited by ultraviolet and purple light chip.
Fig. 2 is phosphor emission spectrogram, 360 nanometers of excitation wavelength, when the excitation wavelength of emission spectrum is 360nm, can be with from Fig. 2
Find out, the broadband blue light for the being emitted as divalent europium transmitting of the fluorescent material of the present embodiment and the arrowband red emission of trivalent europium, hair
Penetrate peak to be respectively located near 413nm and 614nm, illustrate that the fluorescent material of the present embodiment is adapted to do ultraviolet and purple light excited fluorescence
Powder.From figure 3, it can be seen that the fluorescent material XRD spectrum of the present embodiment shows the d values and relative intensity variation tendency and mark of product
Accurate Ca9Cu1.5(PO4)7Standard card (JCPDF：51592) unanimously, illustrate that the fluorescence powder purity of the present embodiment synthesis is higher.From
As can be seen that in the case where the light of different wave length (360-380nm) is excited in table 1, the purple of the fluorescent material of the present embodiment changes to red
Color (chromaticity coordinates from (0.2439,0.1294)-(0.4540,0.2425)), illustrates that the present embodiment fluorescent material can realize glow color
It is adjustable.
Table 1 is chromaticity coordinates of the fluorescent powder of the preparation of the embodiment of the present invention 1 under different excitation wavelengths.
Table 1
| Excitation wavelength (nm) | Launch peak-to-peak value (nm) | Chromaticity coordinates |
| 360 | 413、614 | (0.2439,0.1294) |
| 365 | 413、614 | (0.2237,0.1163) |
| 370 | 413、614 | (0.2279,0.1160) |
| 375 | 413、614 | (0.4089,0.2180) |
| 380 | 413、614 | (0.4540,0.2425) |
Embodiment 2
According to Ca8.99Zn1.5(PO4)7：0.01Eu2+Weigh CaCO3、ZnO、(NH4)2HPO4And Eu2O3, rubbing between them
You are than being 8.99：1.5：7：0.005, it is fully ground after being well mixed, places in corundum crucible, place into high temperature furnace in 5%
H2+ 95%N2It is calcined 3 hours at 1350 DEG C under the nitrogen and hydrogen mixture atmosphere of (volume ratio), is subsequently cooled to room temperature, obtains spectrum adjustable
Phosphate phosphor.
The fluorescent material PLE of the present embodiment is a wide range, covers ultraviolet and violet region, excitation peak be located at 291nm and
Near 425nm, spectrum peak is high, illustrates the fluorescent material of the present embodiment and can effectively be excited by ultraviolet and purple light chip.Work as transmitting
The excitation wavelength of spectrum is 360nm, the broadband blue light for the being emitted as divalent europium transmitting of the fluorescent material of the present embodiment and trivalent europium
Arrowband red emission, emission peak respectively be located at 413nm and 614nm near, illustrate that the fluorescent material of the present embodiment is adapted to do ultraviolet
With purple light excited fluorescent material.The fluorescent material XRD spectrum of the present embodiment shows the d values and relative intensity variation tendency and mark of product
Accurate Ca9Cu1.5(PO4)7Standard card (JCPDF：51592) unanimously, illustrate that the fluorescence powder purity of the present embodiment synthesis is higher.
The light of different wave length (360-380nm) is excited down, and the purple of the fluorescent material of the present embodiment changes to red, illustrates that the present embodiment is glimmering
Light powder can realize that glow color is adjustable.
Embodiment 3
According to Ca8.9Zn1.5(PO4)7：0.1Eu2+Weigh CaCO3、ZnO、NH4H2PO4And Eu2O3, the mol ratio between them
For 8.9：1.5：7：0.05, be fully ground it is well mixed after, place in corundum crucible, place into high temperature furnace under CO atmosphere
1300 DEG C are calcined 4 hours, are subsequently cooled to room temperature, obtain the adjustable phosphate phosphor of spectrum.
The fluorescent material PLE of the present embodiment is a wide range, covers ultraviolet and violet region, excitation peak be located at 291nm and
Near 425nm, spectrum peak is high, illustrates the fluorescent material of the present embodiment and can effectively be excited by ultraviolet and purple light chip.Work as transmitting
The excitation wavelength of spectrum is 360nm, the broadband blue light for the being emitted as divalent europium transmitting of the fluorescent material of the present embodiment and trivalent europium
Arrowband red emission, emission peak respectively be located at 413nm and 614nm near, illustrate that the fluorescent material of the present embodiment is adapted to do ultraviolet
With purple light excited fluorescent material.The fluorescent material XRD spectrum of the present embodiment shows the d values and relative intensity variation tendency and mark of product
Accurate Ca9Cu1.5(PO4)7Standard card (JCPDF：51592) unanimously, illustrate that the fluorescence powder purity of the present embodiment synthesis is higher.
The light of different wave length (360-380nm) is excited down, and the purple of the fluorescent material of the present embodiment changes to red, illustrates that the present embodiment is glimmering
Light powder can realize that glow color is adjustable.
Embodiment 4
According to Ca8.999Mg1.5(PO4)7：0.001Eu2+Weigh CaCO3、MgCO3、(NH4)2HPO4And Eu2O3, between them
Mol ratio be 8.999：1.5：7：0.0005, it is fully ground after being well mixed, places in corundum crucible, place into high temperature furnace
In 5%H2+ 95%N2It is calcined 2 hours at 1400 DEG C under the nitrogen and hydrogen mixture atmosphere of (volume ratio), is subsequently cooled to room temperature, obtains light
Compose adjustable phosphate phosphor.
The fluorescent material PLE of the present embodiment is a wide range, covers ultraviolet and violet region, excitation peak be located at 291nm and
Near 425nm, spectrum peak is high, illustrates the fluorescent material of the present embodiment and can effectively be excited by ultraviolet and purple light chip.Work as transmitting
The excitation wavelength of spectrum is 360nm, the broadband blue light for the being emitted as divalent europium transmitting of the fluorescent material of the present embodiment and trivalent europium
Arrowband red emission, emission peak respectively be located at 413nm and 614nm near, illustrate that the fluorescent material of the present embodiment is adapted to do ultraviolet
With purple light excited fluorescent material.The fluorescent material XRD spectrum of the present embodiment shows the d values and relative intensity variation tendency and mark of product
Accurate Ca9Cu1.5(PO4)7Standard card (JCPDF：51592) unanimously, illustrate that the fluorescence powder purity of the present embodiment synthesis is higher.
The light of different wave length (360-380nm) is excited down, and the purple of the fluorescent material of the present embodiment changes to red, illustrates that the present embodiment is glimmering
Light powder can realize that glow color is adjustable.
Embodiment 5
According to Ca8.99Mg1.5(PO4)7：0.01Eu2+Weigh CaCO3、MgCO3、(NH4)2HPO4And Eu2O3, between them
Mol ratio is 8.99：1.5：7：0.005, be fully ground it is well mixed after, place in corundum crucible, place into high temperature furnace in
5%H2+ 95%N2It is calcined 3 hours at 1350 DEG C under the nitrogen and hydrogen mixture atmosphere of (volume ratio), is subsequently cooled to room temperature, obtains spectrum
Adjustable phosphate phosphor.
The fluorescent material PLE of the present embodiment is a wide range, covers ultraviolet and violet region, excitation peak be located at 291nm and
Near 425nm, spectrum peak is high, illustrates the fluorescent material of the present embodiment and can effectively be excited by ultraviolet and purple light chip.Work as transmitting
The excitation wavelength of spectrum is 360nm, the broadband blue light for the being emitted as divalent europium transmitting of the fluorescent material of the present embodiment and trivalent europium
Arrowband red emission, emission peak respectively be located at 413nm and 614nm near, illustrate that the fluorescent material of the present embodiment is adapted to do ultraviolet
With purple light excited fluorescent material.The fluorescent material XRD spectrum of the present embodiment shows the d values and relative intensity variation tendency and mark of product
Accurate Ca9Cu1.5(PO4)7Standard card (JCPDF：51592) unanimously, illustrate that the fluorescence powder purity of the present embodiment synthesis is higher.
The light of different wave length (360-380nm) is excited down, and the purple of the fluorescent material of the present embodiment changes to red, illustrates that the present embodiment is glimmering
Light powder can realize that glow color is adjustable.
Embodiment 6
According to Ca8.9Zn1.5(PO4)7：0.1Eu2+Weigh CaCO3、MgCO3、NH4H2PO4And Eu2O3, mole between them
Than for 8.9：1.5：7：0.05, it is fully ground after being well mixed, places in corundum crucible, place into high temperature furnace under CO atmosphere
It is calcined 4 hours at 1300 DEG C, is subsequently cooled to room temperature, obtains the adjustable phosphate phosphor of spectrum.
The fluorescent material PLE of the present embodiment is a wide range, covers ultraviolet and violet region, excitation peak be located at 291nm and
Near 425nm, spectrum peak is high, illustrates the fluorescent material of the present embodiment and can effectively be excited by ultraviolet and purple light chip.Work as transmitting
The excitation wavelength of spectrum is 360nm, the broadband blue light for the being emitted as divalent europium transmitting of the fluorescent material of the present embodiment and trivalent europium
Arrowband red emission, emission peak respectively be located at 413nm and 614nm near, illustrate that the fluorescent material of the present embodiment is adapted to do ultraviolet
With purple light excited fluorescent material.The fluorescent material XRD spectrum of the present embodiment shows the d values and relative intensity variation tendency and mark of product
Accurate Ca9Cu1.5(PO4)7Standard card (JCPDF：51592) unanimously, illustrate that the fluorescence powder purity of the present embodiment synthesis is higher.
The light of different wave length (360-380nm) is excited down, and the purple of the fluorescent material of the present embodiment changes to red, illustrates that the present embodiment is glimmering
Light powder can realize that glow color is adjustable.
Above-described embodiment is used for illustrating the present invention, rather than limits the invention, the present invention spirit and
In scope of the claims, any modifications and changes made to the present invention both fall within protection scope of the present invention.
Claims (5)
1. a kind of white light LEDs adjustable phosphate phosphor of spectrum, it is characterised in that the fluorescent material has following chemical representation：
Ca9-xM1.5(PO4)7：xEu2+, wherein, M is any one in Zn and Mg, and x is 0.001~0.10.
2. the preparation method of the white light LEDs adjustable phosphate phosphor of spectrum described in a kind of claim 1, it is characterised in that including
Following steps：(1) compound with calcium carbonate, containing M, containing [PO4]3-Compound and europium oxide, by chemical expression Ca9-xM1.5
(PO4)7：xEu2+Obtain mixture；(2) mixture is loaded into crucible, in 1300~1400 under reducing atmosphere in high temperature furnace
Sintered 2~4 hours under the conditions of DEG C, after be cooled to room temperature and obtain the adjustable phosphate phosphor of the spectrum.
3. the white light LEDs as claimed in claim 2 preparation method of the adjustable phosphate phosphor of spectrum, it is characterised in that described to contain
It is one kind in magnesium carbonate and zinc oxide to have M compound.
4. the white light LEDs as claimed in claim 2 preparation method of the adjustable phosphate phosphor of spectrum, it is characterised in that described to contain
[PO4]3-Compound is one kind in diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
5. the white light LEDs as claimed in claim 2 preparation method of the adjustable phosphate phosphor of spectrum, it is characterised in that described to go back
Primordial Qi atmosphere is nitrogen and hydrogen mixture or CO atmosphere.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109957401A (en) * | 2018-05-28 | 2019-07-02 | 吉林大学 | A kind of ultraviolet LED single-phase warm white fluorescent powder and preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105087003A (en) * | 2015-09-02 | 2015-11-25 | 中国科学院长春应用化学研究所 | Orange LED fluorescent powder as well as preparation method and application thereof |
| CN105131951A (en) * | 2015-09-02 | 2015-12-09 | 中国科学院长春应用化学研究所 | Red light LED fluorescent powder and preparation method and application thereof |
-
2017
- 2017-06-02 CN CN201710408192.3A patent/CN107189779A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105087003A (en) * | 2015-09-02 | 2015-11-25 | 中国科学院长春应用化学研究所 | Orange LED fluorescent powder as well as preparation method and application thereof |
| CN105131951A (en) * | 2015-09-02 | 2015-12-09 | 中国科学院长春应用化学研究所 | Red light LED fluorescent powder and preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109957401A (en) * | 2018-05-28 | 2019-07-02 | 吉林大学 | A kind of ultraviolet LED single-phase warm white fluorescent powder and preparation method |
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Application publication date: 20170922 |