CN106318381A - Mn<4+>-doped sodium bifluoride red light material and method for preparing same - Google Patents
Mn<4+>-doped sodium bifluoride red light material and method for preparing same Download PDFInfo
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Abstract
The invention discloses a Mn<4+>-doped sodium bifluoride red light material and a method for preparing the same. Chemical composition of the Mn<4+>-doped sodium bifluoride red light material is NaHF<2>:Mn<4+>. The Mn<4+>-doped sodium bifluoride red light material is made of raw materials including 15-30 mL of HF (with the concentration of wt 40%), 1*10<-4>-9*10<-4> mol of K<2>MnF<6> solid and 0.01-0.1 mol of NaF. The method includes adding the raw materials into deionized water to obtain liquid with the total volume of 40 mL; carrying out stirring reaction on the liquid at the normal temperature for 0.5-2 hours; carrying out suction filtration on reaction products; naturally drying the reaction products at the normal temperature to obtain white powder. The Mn<4+>-doped sodium bifluoride red light material and the method have the advantages that bright red light can be emitted by the Mn<4+>-doped sodium bifluoride red light material under ultraviolet lamps, the maximum excitation bands of the Mn<4+>-doped sodium bifluoride red light material can be completely matched with spectra of blue light emitted by blue light chips of white light LEDs, and an emission spectrum of the Mn<4+>-doped sodium bifluoride red light material comprises seven red light emission peaks positioned at four locations of 595-643 nm; the Mn<4+>-doped sodium bifluoride red light material can be possibly applied to a white light LED with two fundamental colors, so that color rendering indexes of the white light LED can be increased; the Mn<4+>-doped sodium bifluoride red light material does not contain rare earth, the method is simple, and accordingly the Mn<4+>-doped sodium bifluoride red light material and the method are applicable to industrial production.
Description
Technical field
The present invention relates to luminescent material, particularly relate to a kind of can the red light material that be used for white light LEDs and preparation method thereof；
It is specifically related to a kind of excitation wavelength and is positioned at blue region, launch wavelength and be positioned at the Mn of red light region4+The fluohydric acid gas of doping receives luminescence
Material and preparation method thereof.
Background technology
White light LEDs is the forth generation light source after electric filament lamp, fluorescent lamp, is the new light sources generally acknowledged 21 century.Yin Qigao
Imitate the advantages such as energy-conservation, environmental protection, life-span length and volume are little, be widely used in the multiple fields such as illumination, communication and display, no
It is only manufacturer and provides perfect backlighting scheme, the light source of economic high-quality is also provided for general lighting.Nowadays leading market
White light LEDs product is to be encapsulated with blue-ray LED by yellow fluorescent powder YAG:Ce, obtains color white light LEDs by champac complementation color matching, with
Traditional energy-saving lamp is compared, and this type of white LEDs is relatively low at low colour temperature district color rendering index, it is impossible to meet large-scale lighting demand, former
Cause is to only have gold-tinted and blue light ingredient in its white light, and the composition of redness is less.
In order to improve the white light LEDs color rendering index being made up of yellow fluorescent powder YAG:Ce with blue chip, in YAG:Ce
It is mixed into nitride red fluorescent material, the most effectively the method for reality.Two primary colours that commercial applications is to be handed over can be reached at present
The Nitride systems of WLED red light material commonly used divalent europium doping, such as Sr2‐x‐yBaxCaySi5N8:Eu2+, its substrate is stable
Property height, Absorber Bandwidth, excitation is high, luminous efficiency high, temperature quenching is inconspicuous, the colour developing that can effectively optimize two primary colours WLED refers to
Number and colour temperature, the quantum efficiency under 465nm excites reaches 80%, and luminous intensity only reduces a few percent at 150 DEG C
[X.Q.Piao,T.Horikawa,H.Hanzawa,K.Machida,“Characterization and luminescence
properties of Sr2Si5N8:Eu2+phosphor for white light‐emitting‐diode
illumination”,Appl.Phys.Lett.88(2006)161908.Y.Q.Li,De With G,H.T.Hintzen,“The
effect of replacement of Sr by Ca on the structural and luminescence
properties of the red‐emitting Sr2Si5N8:Eu2+LED conversion phosphor”,J.Solid
State Chem.181(2008)515‐524.].Owing to being used for preparing the alkaline earth nitride of this system red light material, silicon nitride etc.
Raw material is much more expensive, and the overall process of batch mixing and preparation need to be kept away water and be kept away oxygen so that the price of nitride red light material is high.Mn4+
The red light material of doping is given birth to because of fortune, causes the great interest carrying out people, is because it is in clad aluminum hydrochlorate with composite fluoride
Excitation wavelength be positioned near ultraviolet to blue region, just mate with the electroluminescence wavelength of blue-ray LED with semiconductor-based purple light, energy
Effectively absorb purple light and the blue light of LED chip, and its emission spectrum to be sharp peak be positioned at red light region, the HONGGUANG of efficient transmission can have
Effect improves the color rendering index of WLED, it is thus achieved that the warm white of low colour temperature height colour developing.Mn4+Possessed this has Broad excitation band with narrow
Launch what illumination was especially advantageously applied by the luminosity carried.Therefore, LED industry expects Mn4+The red light material of doping can take
The business nitride Hydrargyri Oxydum Rubrum harsh for synthesis condition, raw material is rare.
The Mn of Philips company the '20s in last century invention4+The fluogermanate red light emitting phosphor efficiency of doping is high,
Excitation high [G.Kemeny, C.H.Haake, " Activator center in magnesium fluorogermanate
Phosphors ", J.Chem.Phys.33 (1960) 783.], but expensive (because raw material is containing GeO2), therefore, this Hydrargyri Oxydum Rubrum is current
It is only applied to special fluorescent lamp to improve its color rendering index, and its excitation spectrum is positioned at black light district, is not suitable for market master
The blue chip base LED led.Fluorescent material CaAl12O19:Mn4+HONGGUANG can be launched, from reason under the black light the exciting with blue light
Saying on Lun, this powder potential can be applied to LED, but its luminous efficiency still have much room for improvement [T.Murata, T.Tanoue,
M.Iwasaki,K.Morinaga,T.Hase,“Fluorescence properties of Mn4+in
CaAl12O19compounds as red‐emitting phosphor for white LED”,J.Lumin.114(2005)
207；Y.X.Pan,G.K.Liu,“Enhancement of phosphor efficiency via composition
Modification ", Opt.Lett.33 (2008) 1], utilize anion exchange method recently, efficiently synthesize and have studied HONGGUANG material
Material K2TiF6:Mn4+, its light efficiency is up to 98%, by K2TiF6:Mn4+Blue-ray LED jointly it is packaged in yellowish green fluorescent powder YAG:Ce
After chip, obtain low colour temperature (3088K), high-color rendering (CRI=90), high efficiency (82%) warm white WLED [H.M.Zhu,
C.C.Lin,W.Q.Luo,S.T.Shu,Z.G.Liu,Y.S.Liu,J.T.Kong,E.Ma,Y.G.Cao,R.S.Liu,
X.Y.Chen,"Highly efficient non‐rare‐earth red emitting phosphor for warm
white light‐emitting diodes",Nat.Commun.5(2014)4312.].Japanese researchers has synthesized a series of
Mn4+The composite fluoride red light material of doping also studies its luminosity, but synthetic method is more complicated, and raw materials used costliness
(simple metal), etching liquid used dense (40%HF aqueous solution), KMnO4Concentration height (non-luminous by-product easily occurs, as
MnO2)[S.Adachi,T.Takahashi,"A yellow phosphor K2SiF6activated by Mn2+ion",
J.Appl.Phys.108(2010)063506；R.Kasa,S.Adachi,"Mn‐activated K2ZrF6and
Na2ZrF6phosphors:Sharp red and oscillatory blue‐green emissions",
J.Appl.Phys.112(2012)013506.；S.Adachi,T.Takahashi,"Photoluminescence and
Raman scattering spectroscopies of Ba SiF6:Mn4+red phosphor",J.Appl.Phys.106
(2009)013516.]。
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art, it is provided that a kind of can effectively be excited by the blue light of GaN chip,
And the two inorganic primary colours white light LEDs red light materials launching HONGGUANG and preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions:
A kind of Mn4+The fluohydric acid gas of doping receives red light material: this material is with NaHF2For substrate, with Mn4+As the centre of luminescence,
Chemical composition is NaHF2:Mn4+, Mn4+Mole doping content be NaHF20.1%～1.0%；Mn4+Part replaces Na+With H+, and form negatron hole and make in crystal electric charge keep neutrality.
The most described Mn4+Mole doping content be NaHF20.4%～0.6%.
It is white powder that this fluohydric acid gas receives red light material, luminous uniformly, maximum excitation wavelength, in blue region, launches wavelength
Accompany in red light region.Specifically product issues bright red at uviol lamp, and this material emitted light spectrum is laid respectively at by three
250nm, 350nm, 460nm broadband forms, complete of the blue spectrum that the excitation band of its maximum and White LED Blue Light chip are sent out
Joining, emission spectrum is positioned at by 7 spikes laying respectively at 593nm, 605nm, 608nm, 616nm, 626nm, 630nm and 642nm
Composition, summit is positioned at 626nm.The photochromic coordinate of described transmitting is positioned at: x=0.66；Y=0.33, is in close proximity to CIE standard red
The chromaticity coordinates of light.
Described Mn4+The fluohydric acid gas of doping receives the preparation method of red light material: by K2MnF6Solid is dissolved in HF aqueous solution, adds
NaF solid, adds deionized water, stirring reaction at normal temperatures 0.5～2 hour, sucking filtration, and room temperature dries naturally, obtains white powder
Body target material；K2MnF6It is 0.001～0.09:1 with the mol ratio of NaF.
For realizing the object of the invention further, it is preferable that the mass concentration of described HF solution is 40%.
Preferably, the consumption of the every 0.01～0.1mol NaF HF aqueous solution added is 15～30mL.
Preferably, the described response time is 1～2 hour.
Preferably, the described every 0.01～0.1mol NaF deionized water added is 10 25mL.
In the present invention, this material with researched and developed Mn4+The composite fluoride A of doping2XF6:Mn4+(A=K, Na, Cs；X=
Si, Ge, Zr, Ti) difference of red light material, the substrate of these red light materials all has and Mn4+It is all the sun of+4 valencys from such as Si4+,
Ge4+,Zr4+,Ti4+, Mn4+Part replaces sun sublattice position and sends HONGGUANG, and prepares these materials and it is frequently necessary to (add in hydro-thermal
Heat pressurization) condition just carries out.Base NaHF2In there is no+4 valency cationes, but NaHF2:Mn4+But can be luminous, luminous efficiency reaches 88%.
Mn can be speculated4+Part replaces Na+With H+, and form negatron hole and make in crystal electric charge keep neutrality, reaction is omnidistance in room temperature
Under carry out.
Relative to prior art, the invention have the advantages that and effect:
(1) present invention is compared with the aluminate that known tetravalent manganese is adulterated, it is not necessary to high temperature sintering, because whole process is at air
In carry out at normal temperatures, material because without sintering and pattern is dispersed；Emission maximum mother-in-law's length of the present invention is in the region of blue light, therefore
Can more effectively absorb blue light, and because of Mn4+Narrowed emission, makes HONGGUANG purer.
(2) with the Mn researched and developed4+The composite fluoride A of doping2XF6:Mn4+Red light material is compared, and the present invention has only to 3 kinds
Raw material: K2MnF6, HF and NaF, it is not necessary to positive tetravalent metal raw material, therefore raw material is simple, and synthesis technique whole process is entered at normal temperatures
OK, can be mass-produced.
(3) because material is without rare earth, preparation process keeps away oxygen without keeping away water, it is not necessary to high temperature sintering, and therefore, cost is far below business
Industry nitride Hydrargyri Oxydum Rubrum.
Accompanying drawing explanation
Fig. 1 NaHF2:Mn4+The XRD standard card data of (embodiment 1) and the XRD figure of embodiment product.
Fig. 2 NaHF2:Mn4+EDS (spectral distribution) figure of (embodiment 1).
Fig. 3 NaHF2:Mn4+The excitation spectrum (a: monitoring wavelength is 626nm) of (embodiment 1) and emission spectrum (b: excite
Wavelength is 460nm).
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but the scope of protection of present invention is not
It is confined to the scope that embodiment represents.
Embodiment 1
In plastic containers, by 0.1235g (5 × 10‐4mol)K2MnF6Solid material is dissolved in 20mL HF, and (concentration is
Wt40%), being subsequently adding 2.1g (0.05mol) NaF is raw material, adds deionized water and makes cumulative volume be 40mL, stirs at normal temperatures
Reacting 1.5 hours, sucking filtration, room temperature dries naturally, obtains white powder.Product issues bright red at uviol lamp.Its XRD
(detection of Bruker D8Advance X-ray diffractometer) is as it is shown in figure 1, XRD display product is pure NaHF2Phase, trace doped
Mn4+And have no significant effect thing phase.As in figure 2 it is shown, energy spectrum analysis records on Nova NanoSEM 200, at electron beam
Under effect, energy spectrum analysis display element: Na, F and Mn, and H cannot show owing to quality is the least, it is seen that products obtained therefrom composition is
NaHF2:Mn4+.As it is shown on figure 3, utilize Fluoromax 4 fluorescence spectrophotometer (HORIBA Jobin Yvon Inc.), in room temperature
Under the conditions of detect the luminescent properties of product, the excitation spectrum of this white powder product by three lay respectively at 250nm, 350nm,
460nm broadband forms, and the blue light that the excitation band (460nm) of its maximum is sent out with GaN blue chip mates completely, emission spectrum position
Form in being laid respectively at the spike being positioned at 593nm, 605nm, 608nm, 616nm, 626nm, 630nm and 642nm by 7, the highest
Peak is positioned at 626nm.The granule of product is more uniform, and its particle size size and scope distribution are also suitable for being coated with pipe application.Product does not contains
Rare earth, preparation method is simple, is suitable to commercial production.
Embodiment 2
In plastic containers, by 0.0988g (4 × 10‐4mol)K2MnF6Solid material is dissolved in 30mL HF, and (concentration is
Wt40%), being subsequently adding 0.42g (0.01mol) NaF is raw material, adds deionized water and makes cumulative volume be 40mL, stirs at normal temperatures
Reacting 0.5 hour, sucking filtration, room temperature dries naturally, obtains white powder.Product issues bright red at uviol lamp.This white powder
The XRD figure of body material, surface sweeping Electronic Speculum figure and fluorescence spectrum are essentially identical with Fig. 13.
Embodiment 3
In plastic containers, by 0.1482g (6 × 10‐4mol)K2MnF6Solid material is dissolved in 15mL HF, and (concentration is
Wt40%), being subsequently adding 3.36g (0.08mol) NaF is raw material, adds deionized water and makes cumulative volume be 40mL, stirs at normal temperatures
Reacting 1 hour, sucking filtration, room temperature dries naturally, obtains white powder.Product issues bright red at uviol lamp.This white powder
The XRD figure of material, surface sweeping Electronic Speculum figure and fluorescence spectrum are essentially identical with Fig. 13.
Embodiment 4
In plastic containers, by 0.0247g (1 × 10‐4mol)K2MnF6Solid material is dissolved in 18mL HF, and (concentration is
Wt40%), being subsequently adding 2.52g (0.06mol) NaF is raw material, adds deionized water and makes cumulative volume be 40mL, stirs at normal temperatures
Reacting 2 hours, sucking filtration, room temperature dries naturally, obtains white powder.Product issues bright red at uviol lamp.This white powder
The XRD figure of material, surface sweeping Electronic Speculum figure and fluorescence spectrum are essentially identical with Fig. 13.
Embodiment 5
In plastic containers, by 0.2223g (9 × 10‐4mol)K2MnF6Solid material is dissolved in 25mL HF, and (concentration is
Wt40%), being subsequently adding 4.2g (0.1mol) NaF is raw material, adds deionized water and makes cumulative volume be 40mL, and stirring is anti-at normal temperatures
Answering 1.8 hours, sucking filtration, room temperature dries naturally, obtains white powder.Product issues bright red at uviol lamp.This white powder
The XRD figure of material, surface sweeping Electronic Speculum figure and fluorescence spectrum are essentially identical with Fig. 13.
Embodiment 6
In plastic containers, by 0.1235g (5 × 10‐4mol)K2MnF6Solid material is dissolved in 25mL HF, and (concentration is
Wt40%), being subsequently adding 2.94g (0.07mol) NaF is raw material, adds deionized water and makes cumulative volume be 40mL, stirs at normal temperatures
Reacting 1.6 hours, sucking filtration, room temperature dries naturally, obtains white powder.Product issues bright red at uviol lamp.This white powder
The XRD figure of body material, surface sweeping Electronic Speculum figure and fluorescence spectrum are essentially identical with Fig. 13.
From above-described embodiment, the present invention is compared with the aluminate that known tetravalent manganese is adulterated, it is not necessary to high temperature sintering,
Because whole process is carried out the most at normal temperatures, material is because without sintering, pattern is dispersed；Emission maximum mother-in-law's length of the present invention exists
The region of blue light, therefore can more effectively absorb blue light, and because of Mn4+Narrowed emission, makes HONGGUANG purer.
With the Mn researched and developed4+The composite fluoride A of doping2XF6:Mn4+Red light material is compared, the present invention have only to 3 kinds former
Material: K2MnF6, HF and NaF, it is not necessary to positive tetravalent metal raw material, therefore raw material is simple, and synthesis technique whole process is entered at normal temperatures
OK, can be mass-produced.
Because material is without rare earth, preparation process whole process is carried out in atmosphere, it is not necessary to keeps away water and keeps away oxygen, it is not necessary to high temperature sintering, because of
This, cost is far below business nitride Hydrargyri Oxydum Rubrum.
Claims (8)
1. a Mn4+The fluohydric acid gas of doping receives red light material, it is characterised in that: this material is with NaHF2For substrate, with Mn4+As
The centre of luminescence, chemical composition is NaHF2:Mn4+, Mn4+Mole doping content be NaHF20.1%～1.0%；Mn4+Part takes
For Na+With H+, and form negatron hole and make in crystal electric charge keep neutrality.
Mn the most according to claim 14+The fluohydric acid gas of doping receives red light material, it is characterised in that: described Mn4+Mole doping
Concentration is NaHF20.4%～0.6%.
Mn the most according to claim 14+The fluohydric acid gas of doping receives red light material, it is characterised in that: this fluohydric acid gas receives HONGGUANG material
Material is white powder, luminous uniform, and maximum excitation wavelength, in blue region, is launched wavelength and is positioned at red light region；Described transmitting light
Chromaticity coordinates is positioned at: x=0.66, y=0.33, is in close proximity to the chromaticity coordinates of CIE standard HONGGUANG.
4. Mn described in claim 14+The fluohydric acid gas of doping receives the preparation method of red light material, it is characterised in that: by K2MnF6Solid
Being dissolved in HF aqueous solution, add NaF solid, add deionized water, stirring reaction at normal temperatures 0.5～2 hour, sucking filtration, room temperature is certainly
So dry, obtain white powder target material；K2MnF6It is 0.001～0.09:1 with the mol ratio of NaF.
Mn the most according to claim 44+The fluohydric acid gas of doping receives the preparation method of red light material, it is characterised in that: described
The mass concentration of HF solution is 40%.
Mn the most according to claim 54+The fluohydric acid gas of doping receives the preparation method of red light material, it is characterised in that: every
The consumption of the HF aqueous solution that 0.01～0.1mol NaF adds is 15～30mL.
Mn the most according to claim 44+The fluohydric acid gas of doping receives the preparation method of red light material, it is characterised in that: institute
Stating the response time is 1～2 hour.
Mn the most according to claim 44+The fluohydric acid gas of doping receives the preparation method of red light material, it is characterised in that: institute
The deionized water stating every 0.01～0.1mol NaF addition is 10 25mL.
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Cited By (2)
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| CN109179481A (en) * | 2018-10-26 | 2019-01-11 | 温州大学 | A kind of fluorine scandium acid barium red light material of tetravalence manganese ion doping and preparation method thereof |
| CN111978955A (en) * | 2020-08-24 | 2020-11-24 | 重庆文理学院 | Red fluorescent powder and preparation method and application thereof |
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Cited By (3)
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| CN109179481A (en) * | 2018-10-26 | 2019-01-11 | 温州大学 | A kind of fluorine scandium acid barium red light material of tetravalence manganese ion doping and preparation method thereof |
| CN109179481B (en) * | 2018-10-26 | 2020-09-01 | 温州大学 | Quadrivalent manganese ion doped barium fluoscandate red light-emitting material and preparation method thereof |
| CN111978955A (en) * | 2020-08-24 | 2020-11-24 | 重庆文理学院 | Red fluorescent powder and preparation method and application thereof |
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Application publication date: 20170111 Assignee: INSTITUTE OF NEW MATERIALS & INDUSTRIAL TECHNOLOGY, WENZHOU University Assignor: Wenzhou University Contract record no.: X2020330000095 Denomination of invention: A Mn4 +doped sodium hydrogen fluoride red light material and its preparation method Granted publication date: 20180619 License type: Common License Record date: 20201112 |