CN107033891B - A kind of white light LEDs red light material and preparation method thereof based on fluozirconate - Google Patents

A kind of white light LEDs red light material and preparation method thereof based on fluozirconate Download PDF

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CN107033891B
CN107033891B CN201710442847.9A CN201710442847A CN107033891B CN 107033891 B CN107033891 B CN 107033891B CN 201710442847 A CN201710442847 A CN 201710442847A CN 107033891 B CN107033891 B CN 107033891B
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zrf
fluozirconate
white light
aqueous solution
red light
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CN107033891A (en
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潘跃晓
席陆青
刘桂
张磊
潘鑫
侯喜梅
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Wenzhou University
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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
    • C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
    • C09K11/674—Halogenides
    • C09K11/675—Halogenides with alkali or alkaline earth metals
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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

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  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)
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Abstract

The invention discloses a kind of white light LEDs red light material and preparation method thereof based on fluozirconate.The chemical composition of the material is Na5Zr2‑2xF13:xMn4+, wherein x=0.1~8.0mol%, with solid NaF, K2MnF6With HF, H2ZrF6Aqueous solution is raw material, is stirred to react at normal temperature 3~12 hours, is filtered, and naturally dry obtains white powder.Product sends out bright red in the UV lamp, and maximum excitation band is located at blue region, can be used for GaN blue chip, and the spike that emission spectrum is located at red area by 6 forms.The material may be applied to two primary colours white light LEDs, to improve its colour rendering index.Product is free of rare earth, and preparation method is simple, is suitable for industrial production.

Description

A kind of white light LEDs red light material and preparation method thereof based on fluozirconate
Technical field
The present invention relates to LED red light materials, more particularly to a kind of white light LEDs red light material based on fluozirconate And preparation method thereof；The material excitation wavelength is located at blue region, and launch wavelength is located at red light region.
Background technique
White light-emitting diodes (W-LED, white-light-emitting diode) solid state lighting is relative to traditional illumination Technology has the advantages that low energy consumption, luminous efficiency is high, pollution-free, has become the research hotspot of people.Countries in the world are studied at present Comparing active realization white light approach is mainly fluorescent conversion type, i.e., is shone with single led chip and phosphor combination.Current quotient The white light LEDs of industry excite yellow fluorescent powder YAG:Ce with GaN base LED chip, but this kind of white light LEDs are because it lacks red light district The spectrum in domain causes its colour rendering index lower, and usually less than 70, it is unable to satisfy large-scale high-end lighting demand.
In order to improve its colour rendering index, it is glimmering that an effective method exactly adds feux rouges appropriate in white light LED part Light powder enhances the red emission of device.Therefore, United States Patent (USP) 6649946 is disclosed using nitride as red fluorescence material, should The chemical formula of nitride is M2Si5N8: Eu and MSi7N10: Eu can be excited by the blue violet light of 420-470nm, and launch feux rouges. Currently, the white light LEDs of better performances are mainly rear-earth-doped nitride material, such as M with red light fluorescent powder2Si5N8:Eu2+(M= Ca, Sr, Ba), MSiN2:Eu2+(M=Sr, Ba, Mg) and CaAlSiN3:Eu2+Deng.But such red light fluorescent powder is emitted as Broadband emission, quite a few emission spectrum is in dark red (> 650nm) range, and it is extremely insensitive that human eye, which shines to this part, So that the radiation luminous efficacy (Luminous Efficacy of Radiation, LER) of device be greatly reduced and cost compared with It is high.Mn4+When ion is in the lattice environment of eight-coordinate, emission spectrum is peak value in the narrow emission of 630nm or so, can Blue chip is effectively matched applied to white light LEDs.
Previous Mn4+The red light material of doping is mostly aluminate, the oxygenatedchemicals such as germanate [M.Y.Peng, X.W.Yin, P.A.Tanner,M.G.Brik,P.F.Li,“Site Occupancy Preference,Enhancement Mechanism, and Thermal Resistance of Mn4+Red Luminescence in Sr4Al14O25:Mn4+for Warm WLEDs",Chem.Mater.27(2015)2938-2945；S.S.Liang,M.M.Shang,H.Z.Liang,Y.Zhang, J.Lin,“Deep red MGe4O9:Mn4+(M=Sr, Ba) phosphors:structure, luminescence properties and application in warm white light emitting diodes”, J.Mater.Chem.C 4 (2016) 6409-6416.] its high temperature solid-state method sintering temperature is higher, the time is long, or need to be specific It is synthesized under atmosphere, obtained fluorescent powder particle is larger, needs to grind for a long time, and industrial production application is limited.Mn4+The fluorine of doping Compound feux rouges material increasingly arouse people's interest [H.Zhu, C.C.Lin, W.Luo, S.Shu, Z.Liu, Y.Liu, J.Kong, E.Ma,Y.Cao,R.S.Liu,and X.Chen,"Highly efficient non-rare-earth red emitting phosphor for warm white light-emitting diodes,"Nat.Commun.,5(2014)4312；L.Lv, X.Jiang,S.Huang,X.a.Chen,and Y.Pan,"The formation mechanism,improved photoluminescence and LED applications of red phosphor K2SiF6:Mn4+," J.Mater.Chem.C, 2 (2014) 3879-84.], mainly due to its simple production process, production cost is low, powder granule grain Diameter is evenly distributed, and meets white light LEDs to feux rouges demand, not only both topographically controllably, but also to have high luminous efficiency, high Photochromic purity, thermal stability is good, the feature that physical and chemical performance is stablized etc., can further satisfaction existing market to fluorescence point Demand condition.But the technology uses the metal simple-substances raw materials such as expensive zirconium, germanium, titanium, and needs to carry out under hydrothermal conditions.
Summary of the invention
Present invention aims to overcome that existing Mn4+The fluozirconate red light material synthesis condition of doping limits, avoid using Expensive zirconium metal simple-substance synthesizes red light material Na under normal temperature conditions5Zr2F13:Mn4+；The method of the present invention is using inexpensively The raw material of source abundance, it is easy to accomplish batch production.
The purpose of the present invention is achieved through the following technical solutions:
A kind of white light LEDs red light material based on fluozirconate, it is characterised in that: the material is with Na5Zr2F13For base Matter, with Mn4+As activator, chemical composition Na5Zr2F13:Mn4+。Mn4+Part replaces Zr4+As the centre of luminescence, Mn4+Rub Your doping concentration is Zr4+0.1~8.0%.The material is powder white, is shone uniformly, excitation spectrum maximum absorption band is located at Blue region and be in broad band, launch wavelength is located at red light region, emission spectrum by positioned at 603nm, 607nm, 616nm, The narrow peak composition of six of 626nm, 629nm and 642nm.
The preparation method of the two primary colours white light LEDs red light material: by solid NaF, K2MnF6It is dissolved in HF aqueous solution, so After H is added2ZrF6Aqueous solution is stirred to react 3~12 hours at normal temperature in polytetrafluoroethylene beaker, is filtered, naturally dry, Obtain white powder.The raw material NaF and H2ZrF6Feed concentrations in the reaction system be respectively as follows: 0.5~5.0mol/L, with 0.4~4.0mol/L, K2MnF6Concentration be 0.1~8.0mol% (relative to H2ZrF6Calculate), the concentration of HF aqueous solution is 4 ~30wt%.
To further realize the object of the invention, the reaction time is preferably 6-10 hours.
K2MnF6Concentration in the reaction system is preferably 1.0~5.0mol% (relative to H2ZrF6It calculates).
The concentration of HF in the reaction system is preferably 10~20wt%..
In the present invention, K2MnF6With H2ZrF6It is partly dissolved in HF solution, dissociate the [MnF of going out6]2-With [ZrF6]2-From Son is since radius similar charge is identical, under agitation, ion exchange occurs, as anion [MnF6]2-、[ZrF6]2-With sun Ion Na+In conjunction with the red light material Na crystallized after recrystallization5Zr2F13:Mn4+, product matrix Na5Zr2F13Be equivalent to by NaF-Na2ZrF6-Na2ZrF6Unit three are constituted, and the XRD of product is shown as the Na of single pure phase5Zr2F13Structure.The essence of reaction Process are as follows: dissolution-ion exchange-recrystallization.Na in reaction system+With [ZrF6]2-Ratio is about 5:4, and Na in product+With [ZrF6]2-Ratio is 5:2, i.e. H2ZrF6It is excessive, and excessive H2ZrF6It has stayed in solution, it is reusable.With [ZrF6]2- It compares, [MnF6]2-Substitution amount it is less, therefore [MnF6]2-Substitution fail to crystal structure generate significantly affect.The present invention uses H2ZrF6As zirconium source, avoid not only increasing formation efficiency, and production cost is greatly saved using zirconium metal simple-substance.
Compared with the existing technology, the invention has the advantages that and effect:
(1) for the present invention compared with the aluminate of known tetravalence additive Mn, the luminous efficiency in the region of blue light is more preferable, and Material morphology is evenly dispersed, and the feux rouges of transmitting is purer, synthesizes at normal temperature, and synthesis temperature is far below CaAl12O19:Mn4+ (1500 DEG C) and nitride rouge and powder (1200 DEG C).
(2) present invention H2ZrF6As zirconium source, avoid using expensive zirconium metal simple-substance, and a step at normal temperatures and pressures Synthesis, not only increases formation efficiency, and production cost is greatly saved.
(3) preparation process of the present invention is conducive to the generation of work industry without heating woth no need to special atmosphere.
Detailed description of the invention
Fig. 1 Na5Zr2F13:Mn4+The XRD standard card data of (embodiment 1) and the XRD diagram of embodiment product.
Fig. 2 Na5Zr2F13:Mn4+The excitation spectrum (monitoring wavelength is 626nm) of (embodiment 1).
Fig. 3 Na5Zr2F13:Mn4+The emission spectrum (excitation wavelength 467nm) of (embodiment 1).
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described, but the scope of protection of present invention is not It is confined to the range of embodiment expression.
Embodiment 1
In polytetrafluoroethylene beaker, by solid NaF, K2MnF6It is dissolved in HF aqueous solution, H is then added2ZrF6Aqueous solution, The feed concentrations of raw material in the reaction system are respectively as follows: 1.5mol/L NaF, 1.2mol/L H2ZrF6, K2MnF6Concentration be 5.0mol% is (relative to H2ZrF6Calculate), the concentration of HF aqueous solution is 20wt%.It is stirred to react 10 hours, filters at normal temperature, Naturally dry obtains white powder.The white powder product sends out bright red in the UV lamp.Its XRD (Bruker D8 The detection of Advance X-ray diffractometer) as shown in Figure 1, XRD shows that product is pure Na5Zr2F13Phase, with its standard card 49- 0107 is completely the same.Using Fluoromax-4 Fluorescence Spectrometer (HORIBA Jobin Yvon Inc.), examine at room temperature The luminescent properties for surveying product, as shown in Fig. 2, the excitation spectrum of the white powder product is located at 350nm and 460nm by two Broadband composition, the blue light that maximum excitation band (460nm) and GaN blue chip are sent out exactly match, emission spectrum be located at by The narrow peak composition of six of 603nm, 607nm, 616nm, 626nm, 629nm and 642nm, top is located at 626nm.With known four The aluminate of valence additive Mn is compared, and luminous efficiency of the present embodiment in the region of blue light is more preferable, and material morphology is evenly dispersed, hair The feux rouges penetrated is purer, synthesizes at normal temperature, and synthesis temperature is far below CaAl12O19:Mn4+(1500 DEG C) and nitride rouge and powder (1200℃)。
The embodiment product is free of rare earth, and preparation method is simple, is suitable for industrial production.Embodiment H2ZrF6As zirconium Source avoids not only increasing formation efficiency, Er Qie great using expensive zirconium metal simple-substance, and one-step synthesis at normal temperatures and pressures Production cost is saved greatly.
Embodiment 2
In polytetrafluoroethylene beaker, by solid NaF, K2MnF6It is dissolved in HF aqueous solution, H is then added2ZrF6Aqueous solution, The feed concentrations of raw material in the reaction system are respectively as follows: 2.0mol/L NaF, 1.6mol/L H2ZrF6, K2MnF6Concentration be 8.0mol% is (relative to H2ZrF6Calculate), the concentration of HF aqueous solution is 30wt%.It is stirred to react 2 hours, filters at normal temperature, Naturally dry obtains white powder.The white powder product sends out bright red in the UV lamp.Product is invented bright in the UV lamp Feux rouges.The XRD diagram of the white powder material, excitation spectrum and emission spectrum are essentially identical with Fig. 1-3 respectively.
Embodiment 3
In polytetrafluoroethylene beaker, by solid NaF, K2MnF6It is dissolved in HF aqueous solution, H is then added2ZrF6Aqueous solution, The feed concentrations of raw material in the reaction system are respectively as follows: 0.5mol/L NaF, 0.4mol/L H2ZrF6, K2MnF6Concentration be 0.1mol% is (relative to H2ZrF6Calculate), the concentration of HF aqueous solution is 4wt%.It is stirred to react 3 hours, filters at normal temperature, from It so dries, obtains white powder.The white powder product sends out bright red in the UV lamp.Product invention azarin in the UV lamp Light.The XRD diagram of the white powder material, excitation spectrum and emission spectrum are essentially identical with Fig. 1-3 respectively.
Embodiment 4
In polytetrafluoroethylene beaker, by solid NaF, K2MnF6It is dissolved in HF aqueous solution, H is then added2ZrF6Aqueous solution, The feed concentrations of raw material in the reaction system are respectively as follows: 5.0mol/L NaF, 4.0mol/L H2ZrF6, K2MnF6Concentration be 1.0mol% is (relative to H2ZrF6Calculate), the concentration of HF aqueous solution is 10wt%.It is stirred to react 6 hours, filters at normal temperature, Naturally dry obtains white powder.The white powder product sends out bright red in the UV lamp.Product is invented bright in the UV lamp Feux rouges.The XRD diagram of the white powder material, excitation spectrum and emission spectrum are essentially identical with Fig. 1-3 respectively.
Embodiment 5
In polytetrafluoroethylene beaker, by solid NaF, K2MnF6It is dissolved in HF aqueous solution, H is then added2ZrF6Aqueous solution, The feed concentrations of raw material in the reaction system are respectively as follows: 1.0mol/L NaF, 0.8mol/L H2ZrF6, K2MnF6Concentration be 2.0mol% is (relative to H2ZrF6Calculate), the concentration of HF aqueous solution is 15wt%.It is stirred to react 12 hours, filters at normal temperature, Naturally dry obtains white powder.The white powder product sends out bright red in the UV lamp.Product is invented bright in the UV lamp Feux rouges.The XRD diagram of the white powder material, excitation spectrum and emission spectrum are essentially identical with Fig. 1-3 respectively.
Embodiment 6
In polytetrafluoroethylene beaker, by solid NaF, K2MnF6It is dissolved in HF aqueous solution, H is then added2ZrF6Aqueous solution, The feed concentrations of raw material in the reaction system are respectively as follows: 3.0mol/L NaF, 2.4mol/L H2ZrF6, K2MnF6Concentration be 6.0mol% is (relative to H2ZrF6Calculate), the concentration of HF aqueous solution is 25wt%.It is stirred to react 10 hours, filters at normal temperature, Naturally dry obtains white powder.The white powder product sends out bright red in the UV lamp.Product is invented bright in the UV lamp Feux rouges.The XRD diagram of the white powder material, excitation spectrum and emission spectrum are essentially identical with Fig. 1-3 respectively.
Embodiment 7
In polytetrafluoroethylene beaker, by solid NaF, K2MnF6It is dissolved in HF aqueous solution, H is then added2ZrF6Aqueous solution, The feed concentrations of raw material in the reaction system are respectively as follows: 4.0mol/L NaF, 3.2mol/L H2ZrF6, K2MnF6Concentration be 3.0mol% is (relative to H2ZrF6Calculate), the concentration of HF aqueous solution is 20wt%.It is stirred to react 8 hours, filters at normal temperature, Naturally dry obtains white powder.The white powder product sends out bright red in the UV lamp.Product is invented bright in the UV lamp Feux rouges.The XRD diagram of the white powder material, excitation spectrum and emission spectrum are essentially identical with Fig. 1-3 respectively.
Embodiment 8
In polytetrafluoroethylene beaker, by solid NaF, K2MnF6It is dissolved in HF aqueous solution, H is then added2ZrF6Aqueous solution, The feed concentrations of raw material in the reaction system are respectively as follows: 3.0mol/L NaF, 2.4mol/L H2ZrF6, K2MnF6Concentration be 7.0mol% is (relative to H2ZrF6Calculate), the concentration of HF aqueous solution is 30wt%.It is stirred to react 3 hours, filters at normal temperature, Naturally dry obtains white powder.The white powder product sends out bright red in the UV lamp.Product is invented bright in the UV lamp Feux rouges.The XRD diagram of the white powder material, excitation spectrum and emission spectrum are essentially identical with Fig. 1-3 respectively.
From above-described embodiment as it can be seen that the embodiment of the present invention is compared with the aluminate of known tetravalence additive Mn, in blue light The luminous efficiency in region is more preferable, and material morphology is evenly dispersed, and the feux rouges of transmitting is purer, synthesizes at normal temperature, synthesis temperature Far below the aluminate (1500 DEG C) and nitride rouge and powder (1200 DEG C) of tetravalence additive Mn.Meanwhile H of the embodiment of the present invention2ZrF6 As zirconium source, avoid not only increasing formation efficiency, and production cost is greatly saved using zirconium metal simple-substance, it is each to implement Example preparation process is conducive to the generation of work industry without heating woth no need to special atmosphere.

Claims (5)

1. a kind of white light LEDs red light material based on fluozirconate, it is characterised in that: the material is with Na5Zr2F13For matrix, with Mn4+As activator, chemical composition Na5Zr2F13:Mn4+；Mn4+Part replaces Zr4+As the centre of luminescence, Mn4+Mole mix Miscellaneous concentration is Zr4+0.1 ~ 8.0%.
2. the white light LEDs red light material based on fluozirconate according to claim 1, it is characterised in that: excitation spectrum is most Big absorption peak is located at blue region and in broad band, and emission spectrum is by being located at 603 nm, 607 nm, 616 nm, 626 nm, 629 The narrow peak composition of six of nm and 642 nm.
3. the preparation method of the white light LEDs red light material as claimed in claim 1 or 2 based on fluozirconate, it is characterised in that: In polytetrafluoroethylene beaker, by solid NaF, K2MnF6It is dissolved in HF aqueous solution, H is then added2ZrF6Aqueous solution stirs at normal temperature It mixes reaction 3 ~ 12 hours, filters, naturally dry obtains white powder.
4. the preparation method of the white light LEDs red light material according to claim 3 based on fluozirconate, it is characterised in that: described Raw material NaF and H2ZrF6Feed concentrations in the reaction system are respectively as follows: 0.5 ~ 5.0 mol/L and 0.4 ~ 4.0 mol/L；Relatively In H2ZrF6It calculates, K2MnF6Concentration be 0.1 ~ 8.0 mol%, the concentration of HF aqueous solution is 4 ~ 30 wt%.
5. the preparation method of the white light LEDs red light material according to claim 3 based on fluozirconate, it is characterised in that: described It is stirred to react whole normal pressure under room temperature, carries out in air.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN106433637A (en) * 2015-08-04 2017-02-22 云南民族大学 Novel Mn<4+> activated high color purity fluoride red light emitting material preparation method
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