CN108641715B - A kind of fluorine gallic acid barium sodium red light material and preparation method thereof for white light LEDs - Google Patents
A kind of fluorine gallic acid barium sodium red light material and preparation method thereof for white light LEDs Download PDFInfo
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- CN108641715B CN108641715B CN201810341509.0A CN201810341509A CN108641715B CN 108641715 B CN108641715 B CN 108641715B CN 201810341509 A CN201810341509 A CN 201810341509A CN 108641715 B CN108641715 B CN 108641715B
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- 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
- C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
- C09K11/626—Halogenides
- C09K11/628—Halogenides with alkali or alkaline earth metals
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- Y—GENERAL 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
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The fluorine gallic acid barium sodium red light material and preparation method thereof that the invention discloses a kind of for white light LEDs.The chemical composition of the material is NaF-BaF2‑Ga(1‑x)F3:xMn4+, by main matrix NaBaGaF6Molar ratio computing, wherein 0.001%≤x≤1.0%.The present invention is prepared at normal temperatures and pressures, and the specific method is as follows: weighing solid material NaF, BaF2、Ga2O3With K2MnF6Raw material puts into the HF aqueous solution of 5~40wt%, stirs 0.5~3 hour at normal temperatures and pressures, filters, and naturally dry obtains faint yellow powder.Product sends out bright red in the UV lamp, can be applied to the colour rendering index for improving two primary colours white light LEDs, and product of the present invention is free of rare earth, and preparation method simple process, synthesis condition is mild, easy mass production, has industry application value.
Description
Technical field
The present invention relates to inoganic solids luminescent material technical fields, and in particular to a kind of red light material, in particular to it is a kind of
Fluorine gallic acid barium sodium red light material and preparation method thereof for white light LEDs.
Background technique
Blue GaN chip and the solid-state of YAG:Ce bloom manufacture are in illuminating device, because they show superior advantage,
It such as low energy consumption, long service life, mercury-free, therefore is considered as the illumination of a new generation.The white light LEDs of present business application are by indigo plant
Color blue GaN chip and YAG:Ce bloom composition, colour rendering index is low (<70), correlated colour temperature height (>6000K), this is because it is electric
Photoluminescence spectrum lacks red color light component.[Chen,D.Q.；Zhou,Y.；Zhong,J.S.A Review on Mn4+
Activators in Solids for Warm White Light-Emitting Diodes.RSC Adv.2016,6,
86285-86296；Xia,Z.G.；Liu,Q.L.Progress in Discovery and Structural Design of
Color Conversion Phosphors for LEDs.Prog.Mater.Sci.2016,84,59-117.]。
There to be the red fluorescence powder of suitable match spectrum and sufficiently high luminous efficiency mixed, acquisition can apply
The warm white LED of backlight in room lighting and display device.Eu2+The nitride of doping has in blue region due to them
There is strong absorption, there is high-quantum efficiency and comparatively ideal thermal stability in red area, therefore can be used to improve white light LEDs
Performance.[P.Pust,V.Weiler,C.Hecht,A.Tücks,A.S.Wochnik,A.K.Henβ,D.Wiechert,
C.Scheu,P.J.Schmidt,W.Schnick,Narrow-band red-emitting Sr[LiAl3N4]:Eu2+ as a
Next-generation LED-phosphor material, Nat.Mater.13 (9) (2014) 891-896.] however, nitridation
The wide excitation band of object is Chong Die in the transmitting band of green area with YAG:Ce, therefore whole luminous efficiency can be made to reduce.This
Outside, the synthesis condition of this nitride is harsher, and starting material price is also somewhat expensive, so that synthesis cost is expensive.Tetravalent manganese
Ion Mn4+The red fluorescence powder of the centre of luminescence as octahedron crystallization site shows to absorb by force in blue region, in red
Region has sharp emission peak, by the way that coating can obtain high-performance together after mixing them with YAG:Ce bloom after optimization
White light LEDs.
Mn4+The red fluorescence powder of doping can perfectly and Spectral matching, and synthesis process is simple, therefore it is in white light LEDs
Field has potential application.Mn4+The composite oxides of doping are dived as aluminate, titanate and germanate show white light LEDs
Application, but its emission spectrum is expanded to the insensitive near infrared region of naked eyes, and their synthesis temperature is higher than
1000℃.[Wang,B.；Lin,H.；Xu,J.；Chen,H.；Wang,Y.S.CaMg2Al16O27:Mn4+-Based Red
Phosphor:A Potential Color Converter for High-Powered Warm W-LED.ACS
Appl.Mater.Inter.2014,6,22905-22913；Chen,H.；Lin,H.；Huang,Q.M.；Huang,F.；Xu,J.；
Wang,B.；Lin,Z.B.；Zhou,J.C.；Wang,Y.S.A Novel Double-Perovskite Gd2ZnTiO6:Mn4+
Red Phosphor for UV-Based w-LEDs:Structure and Luminescence
Properties.J.Mater.Chem.C 2016,4,2374-2381.]Mn4+The hexafluoride of doping is in blue region Qiang Erkuan
Absorption band it is Chong Die with the electroluminescent spectrum of GaN chip, Mn4+Between the excitation and emission spectra of the fluorination matter fluorescent powder of doping
Since Stokes is displaced, when they and YAG:Ce bloom being caused to coat jointly, basically will not produce self-absorption.
Summary of the invention
The present invention is in order to overcome Mn in the prior art4+The fluorine gallic acid of doping receives the photochromic not ideal enough problem of red light material,
And provide a kind of preparation method of fluorine gallic acid barium sodium red light material for white light LEDs.
Second object of the present invention is to provide for a kind of fluorine gallic acid barium sodium red light material for white light LEDs.
To realize first purpose, the technical solution of the present invention is as follows:
A kind of preparation method of the fluorine gallic acid barium sodium red light material for white light LEDs includes the following steps: to weigh solid original
Expect NaF, BaF2、Ga2O3With K2MnF6Raw material puts into HF aqueous solution, stirs at normal temperatures and pressures, reaches dynamic chemical balance, takes out
Filter, naturally dry obtain faint yellow powder, and product sends out bright red in the UV lamp, can be applied to improve two primary colours white light LEDs
Colour rendering index.NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5, K2MnF6Feed ratio is Ga3+0.001%~
1.0%, the Na+、Ba2+With Ga3+Concentration range in the reaction system is 0.1-1.0mol/L, HF aqueous solution mass concentration
For 5-40wt%.Reaction is that normal temperature and pressure whole process carries out in plastic containers, and product is in dissolution-ion exchange-crystallization dynamic
Obtained in process, reaction carries out in air, and the time of reaction is 0.5-3 hours.
The K2MnF6It is preferred that feed ratio is Ga3+0.01%-0.5%.
The HF aqueous solution mass concentration is preferably 20-30wt%.
The Na+、Ba2+With Ga3+Concentration range in the reaction system is preferably 0.5-0.8mol/L.
The reaction time of the reaction is preferably 2-3 hours.
A kind of fluorine gallic acid barium sodium red light material for white light LEDs, the chemical composition of the fluogermanic acid barium red light material are
NaF-BaF2-Ga(1-x)F3:xMn4+, wherein 0.001%≤x≤1.0%, product main matrix ingredient is NaBaGaF6Crystalline phase,
Micro constitutent is Na3GaF6Crystalline phase.
Further, the maximum excitation wavelength of material is swashed in blue region with the blue-ray LED that wavelength is 440~470nm
Hair, obtains the feux rouges of pure color；Chromaticity coordinates is located at: x=0.67, y=0.33 (consistent with colour TV feux rouges international standard), than
There is feux rouges technology Na3GaF6:Mn4+Closer to ideal feux rouges (Na3GaF6:Mn4+Chromaticity coordinates be x=0.66, y=0.32), mainly
The reason is that Mn4+In NaBaGaF6In locating environment symmetry it is weak, make NaBaGaF6:Mn4+It is relatively strong in zero photon line of 617nm
Spend stronger, present invention can apply to two primary colours white light LEDs, to improve white light LEDs colour rendering index.
Compared with the existing technology, the invention has the advantages that and effect:
Red light material and reported K of the invention2SiF6:Mn4+、BaGeF6:Mn4+Equal red light materials are compared, K2SiF6:
Mn4+It needs simple substance Si crystalline substance to do raw material and needs hydrothermal condition ability optimized emission performance, BaGeF6:Mn4+It needs to use noble metal
Ge, the present invention and whole process carry out at normal temperatures and pressures, raw materials used cheap sufficient and nontoxic, the production cost being greatly lowered,
Moreover, mixed-cation Na and Ba coexisting structure in invention product, not only increase the stability of material (because containing water solubility
The alkaline-earth metal ions of difference), and ideal feux rouges (x=0.67, the y=of photochromic and international standard more importantly of the invention
0.33) when unanimously, using white light LEDs, better than existing feux rouges technology Na3GaF6:Mn4+。
Product of the present invention is free of rare earth, and preparation method simple process, synthesis condition is mild, easy mass production, has industry
Application value.
Detailed description of the invention
Product XRD diagram and NaBaGaF obtained in Fig. 1 comparative example 16The standard card data of phase compare.
Product XRD diagram and Na obtained in Fig. 2 comparative example 13GaF6The standard card data of phase compare.
Excitation spectrum of the product obtained in Fig. 3 comparative example 1 under 620nm monitoring.
Emission spectrum of the product obtained in Fig. 4 comparative example 1 under 467nm excitation.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but the scope of protection of present invention
It is not limited to the range of embodiment expression.
Comparative example 1
Accurate NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5 solid material NaF, BaF2、Ga2O3Put into 100mL matter
Measuring concentration is to make Na in 30wt%HF aqueous solution+、Ba2+With Ga3+Concentration in the reaction system is 0.5mol/L, then plus
Enter K2MnF6Raw material makes K2MnF6Concentration in the reaction system is Ga3+0.5%, persistently stir 2 hours under normal temperature and pressure, reach
It balances, filters to dynamic chemical, naturally dry obtains faint yellow powder, and product sends out bright red in the UV lamp.
As shown in Figures 1 and 2, it is NaBaGaF that XRD, which shows that product wants ingredient,6Phase and a small amount of Na3GaF6Phase carefully compares
The spectrum of this product and public technology Na3GaF6:Mn4+Spectrum discovery, the feux rouges in this product is mainly from NaBaGaF6:
Mn4+(spectral signature and Na3GaF6:Mn4+It is different), and chromaticity coordinates is better than Na3GaF6:Mn4+,Because of Mn4+Doping down to
1.0mol% is with respect to NaBaGaF6), it can't be to NaBaGaF6It mutually generates and significantly affects.
As shown in figure 3, using Fluoromax-4 Fluorescence Spectrometer (HORIBA Jobin Yvon Inc.), in room temperature item
The luminescent properties of testing product under part, for the product in the case where the feux rouges of 620nm monitors wavelength, obtained excitation spectrum is located at blue light region
Domain (460nm), and bands of a spectrum are very wide, can effectively absorb the light of blue chip；As shown in figure 4, being used in same Fluorescence Spectrometer
The light of 467nm xenon lamp excites, and obtains NaBaGaF6:Mn4+Emission spectrum, be computed chromaticity coordinates be (x=0.67, y=0.33)
Embodiment 1
Accurate NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5 solid material NaF, BaF2、Ga2O3Put into 100mL matter
Measuring concentration is to make Na in 5wt%HF aqueous solution+、Ba2+With Ga3+Concentration in the reaction system is 0.6mol/L, is then added
K2MnF6Raw material makes K2MnF6Concentration in the reaction system is Ga3+0.001%, persistently stir 2 hours under normal temperature and pressure, reach
It balances, filters to dynamic chemical, naturally dry obtains faint yellow powder, and product sends out bright red in the UV lamp.Product
XRD is similar to comparative example to spectrum.
Embodiment 2
Accurate NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5 solid material NaF, BaF2、Ga2O3Put into 100mL matter
Measuring concentration is to make Na in 15wt%HF aqueous solution+、Ba2+With Ga3+Concentration in the reaction system is 0.7mol/L, then plus
Enter K2MnF6Raw material makes K2MnF6Concentration in the reaction system is Ga3+0.01%, persistently stir 1 hour under normal temperature and pressure,
Reach dynamic chemical balance, filter, naturally dry obtains faint yellow powder, and product sends out bright red in the UV lamp.Product
XRD is similar to comparative example to spectrum.
Embodiment 3
Accurate NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5 solid material NaF, BaF2、Ga2O3Put into 100mL matter
Measuring concentration is to make Na in 20wt%HF aqueous solution+、Ba2+With Ga3+Concentration in the reaction system is 0.8mol/L, then plus
Enter K2MnF6Raw material makes K2MnF6Concentration in the reaction system is Ga3+0.1%, persistently stir 1.5 hours under normal temperature and pressure,
Reach dynamic chemical balance, filter, naturally dry obtains faint yellow powder, and product sends out bright red in the UV lamp.Product
XRD is similar to comparative example to spectrum.
Embodiment 4
Accurate NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5 solid material NaF, BaF2、Ga2O3Put into 100mL matter
Measuring concentration is to make Na in 25wt%HF aqueous solution+、Ba2+With Ga3+Concentration in the reaction system is 0.1mol/L, then plus
Enter K2MnF6Raw material makes K2MnF6Concentration in the reaction system is Ga3+0.2%, persistently stir 0.5 hour under normal temperature and pressure,
Reach dynamic chemical balance, filter, naturally dry obtains faint yellow powder, and product sends out bright red in the UV lamp.Product
XRD is similar to comparative example to spectrum.
Embodiment 5
Accurate NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5 solid material NaF, BaF2、Ga2O3Put into 100mL matter
Measuring concentration is to make Na in 30wt%HF aqueous solution+、Ba2+With Ga3+Concentration in the reaction system is 0.2mol/L, then plus
Enter K2MnF6Raw material makes K2MnF6Concentration in the reaction system is Ga3+0.3%, persistently stir 2.5 hours under normal temperature and pressure,
Reach dynamic chemical balance, filter, naturally dry obtains faint yellow powder, and product sends out bright red in the UV lamp.Product
XRD is similar to comparative example to spectrum.
Embodiment 6
Accurate NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5 solid material NaF, BaF2、Ga2O3Put into 100mL matter
Measuring concentration is to make Na in 40wt%HF aqueous solution+、Ba2+With Ga3+Concentration in the reaction system is 1.0mol/L, then plus
Enter K2MnF6Raw material makes K2MnF6Concentration in the reaction system is Ga3+0.5%, persistently stir 3 hours under normal temperature and pressure, reach
It balances, filters to dynamic chemical, naturally dry obtains faint yellow powder, and product sends out bright red in the UV lamp.Product
XRD is similar to comparative example to spectrum.
Embodiment 7
Accurate NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5 solid material NaF, BaF2、Ga2O3Put into 100mL matter
Measuring concentration is to make Na in 30wt%HF aqueous solution+、Ba2+With Ga3+Concentration in the reaction system is 10.8mol/L, then plus
Enter K2MnF6Raw material makes K2MnF6Concentration in the reaction system is Ga3+1%, persistently stir 2.5 hours under normal temperature and pressure, reach
It balances, filters to dynamic chemical, naturally dry obtains faint yellow powder, and product sends out bright red in the UV lamp.Product
XRD is similar to comparative example to spectrum.
As can be seen from the above embodiments, product of the present invention luminous efficiency is high, and photochromic purity is high, crystallization temperature is low, preparation process
Simply, equipment requirement is low, does not generate waste liquid exhaust gas, it is easy to accomplish large-scale production.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, therefore equivalent changes made in accordance with the claims of the present invention, is still within the scope of the present invention.
Claims (8)
1. a kind of fluorine gallic acid barium sodium red light material for white light LEDs, it is characterised in that: the change of the fluogermanic acid barium red light material
Group becomes NaF-BaF2-Ga(1-x)F3:xMn4+, wherein 0.001%≤x≤1.0%, product main matrix ingredient are
NaBaGaF6Crystalline phase, micro constitutent Na3GaF6Crystalline phase.
2. a kind of preparation method of the fluorine gallic acid barium sodium red light material according to claim 1 for white light LEDs, feature
It is: weighs solid material NaF, BaF2、Ga2O3With K2MnF6Raw material puts into HF aqueous solution, stirs at normal temperatures and pressures, reaches dynamic
State chemical balance filters, and naturally dry obtains faint yellow powder, and product sends out bright red in the UV lamp, can be applied to improve
The colour rendering index of two primary colours white light LEDs.
3. the white light LEDs according to claim 2 preparation method of fluorine gallic acid barium sodium red light material, it is characterised in that:
NaF:BaF2:Ga2O3Mole charge ratio is 1:1:0.5, K2MnF6Feed ratio is Ga3+0.001%~1.0%, the Na+、Ba2 +With Ga3+Concentration range in the reaction system is 0.1~1.0mol/L.
4. the white light LEDs according to claim 2 preparation method of fluorine gallic acid barium sodium red light material, it is characterised in that: HF
Aqueous solution mass concentration is 5~40wt%.
5. the white light LEDs according to claim 2 preparation method of fluorine gallic acid barium sodium red light material, it is characterised in that: institute
Stating reaction is that normal temperature and pressure whole process carries out in plastic containers.
6. the white light LEDs according to claim 2 preparation method of fluorine gallic acid barium sodium red light material, it is characterised in that: institute
Stating product is obtained in dissolution-ion exchange-crystallization dynamic process.
7. the white light LEDs according to claim 2 preparation method of fluorine gallic acid barium sodium red light material, it is characterised in that: institute
Reaction is stated to carry out in air.
8. the white light LEDs according to claim 2 preparation method of fluogermanic acid barium red light material, it is characterised in that: described
The time of reaction is 0.5~3 hour.
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Application publication date: 20181012 Assignee: ZHEJIANG YONGGUANG ELECTRIC APPLIANCES Co.,Ltd. Assignor: Wenzhou University Contract record no.: X2020330000082 Denomination of invention: A red light material of sodium barium gallinate for white LED and its preparation method Granted publication date: 20191025 License type: Common License Record date: 20201028 |
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