CN105038791A - Preparation method of spherical red phosphor powder capable of being excited by ultraviolet-blue light - Google Patents

Preparation method of spherical red phosphor powder capable of being excited by ultraviolet-blue light Download PDF

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CN105038791A
CN105038791A CN201510351113.0A CN201510351113A CN105038791A CN 105038791 A CN105038791 A CN 105038791A CN 201510351113 A CN201510351113 A CN 201510351113A CN 105038791 A CN105038791 A CN 105038791A
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excited
fluorescent material
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赵西成
李兆
徐克�
江元汝
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Xian University of Architecture and Technology
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Abstract

The invention discloses a preparation method of spherical red phosphor powder capable of being excited by ultraviolet-blue light. According to the preparation method, a hydrothermal method in a high-temperature and high-pressure environment is adopted to synthesize the spherical NaY(MoO4)2-based red phosphor powder capable of being excited by ultraviolet-blue light, the defect that the morphology of phosphor powder is agglomerated as a conventional high-temperature solid-phase method is adopted for sintering is overcome, and the growth morphology of the NaY(MoO4)2-based red phosphor powder is controlled through adjusting the pH value of the system to successfully prepare the spherical red phosphor powder.

Description

A kind of preparation method of the spherical red fluorescent material that can be excited by UV-blue
[technical field]
The invention belongs to chemical field, be specifically related to a kind of preparation method of the spherical red fluorescent material that can be excited by UV-blue.
[background technology]
Rear-earth-doped molybdate fluorescent material has very important application prospect in white light LEDs field, and the research tendency for molybdate fluorescent material is also carrying out constantly improvement relative to traditional molybdate.Research contents also from single ionic activate or single-matrix to compound molybdate system expanding, increase its width in excitation spectrum and near ultraviolet and blue region and intensity by compound system matrix or ion doping.
Research at present for compound system molybdate fluorescent material has been reported, and have also been obtained some good red light materials.Guan Li etc. are by high-temperature Solid phase synthesis LiGd (MoO 4) 2: Sm 3+, under ultraviolet excitation, this phosphor emission spectrum can 564,606,648nm has peak value, being wherein positioned at 648nm place red emission the strongest, is a kind of red fluorescence powder that effectively can be excited by UV-light and near-ultraviolet light.Xie An etc. utilize high temperature solid-state method to pass through at KEu (MoO 4) 2introduce appropriate wolframic acid, under the emmission spectrum shape not changing sample and emission peak positions prerequisite, strengthen the luminous intensity of sample.Yang Zhi equality adopts high temperature solid-state method to prepare NaY (MoO 4) 2: Sm 3+red fluorescence powder, and to Sm 3+at NaY (MoO 4) 2the characteristics of luminescence in matrix is studied, and has inquired into different Sm 3+doping content is on the impact of sample luminous intensity.For fluorescent material, optimal fluorescent material should be that pattern is regular, size is homogeneous, and the spherical phosphor of regular shape has very high tap density, can reduce scattering of light, obtains higher luminous efficiency.And the spherical fluorescent material of class has minimum stressed area, makes irregular luminescent layer minimize, therefore has longer luminescent lifetime.But how obtaining spherical molybdate fluorescent material in research is at present a technical barrier, and relevant report is uncommon.
[summary of the invention]
The object of the invention is to overcome above-mentioned deficiency, a kind of preparation method of the spherical red fluorescent material that can be excited by UV-blue is provided, by controlling the conditions such as the pH of solution reaction system, having prepared spherical NaY (MoO 4) 2base red fluorescent powder.
In order to achieve the above object, the present invention includes following steps:
Step one: by 1:(2-8) volume ratio by the Y (NO of 0.1mol/L 3) 3solution mixes with deionized water, obtains solution A;
Step 2: by (2-9): the volume ratio of 1 is by the Eu (NO of solution A and 0.5mol/L 3) 3solution mixes, and obtains solution B;
Step 3: by (2-6): the volume ratio of 1 is by the Na of 0.1mol/L 2moO 4solution mixes with deionized water, obtains solution C;
Step 4: solution C is added dropwise to solution B, stirs, and makes pH value of solution=6.5-11.5, obtains solution D;
Step 5: solution D be transferred in reactor, reacts under 140 DEG C of-280 DEG C of hydrothermal conditions, dry after centrifugation, obtains a kind of spherical red fluorescent material that can be excited by UV-blue.
In described step 2, Eu (NO 3) 3solution can replace with Sm (NO 3) 3solution.
In described step 4, stir and adopt magnetic agitation 10-50min.
In described step 5, reactor adopts stainless steel tetrafluoroethylene reactor.
In described step 5, the hydro-thermal reaction time is 12-48h.
In described step 5, drying is dry 6-36h at 50 DEG C-85 DEG C.
Compared with prior art, the present invention adopts the water heat transfer of high temperature and high pressure environment to go out the spherical NaY (MoO that can be excited by UV-blue 4) 2base red fluorescent powder, overcomes conventional high temperature solid phase method and sinters the shortcoming that fluorescent material pattern is reunited, and by regulation system pH value, controls NaY (MoO 4) 2the growth morphology of base red fluorescent powder, successfully prepares spherical red fluorescent material.
[accompanying drawing explanation]
Fig. 1 is doping Eu 3+, Sm 3+rare earth ion prepares NaY (MoO 4) 2the XRD spectrum of fluorescent material; Wherein a is 4%Eu 3+, b is 4%Sm 3+;
Fig. 2 is different pH value NaY (MoO 4) 2: Eu 3+the SME collection of illustrative plates of matrix; Wherein a is pH=7.0, b be pH=9.0, c be ph=11, d is pH=13.0;
Fig. 3 is NaY (MoO 4) 2: Eu 3+the fluorescence spectrum of fluorescent material; Wherein a is excitation spectrum, and b is emmission spectrum;
Fig. 4 is NaY (MoO 4) 2: Sm 3+the fluorescence spectrum of fluorescent material; Wherein a is excitation spectrum, and b is emmission spectrum;
Fig. 5 is NaY (MoO 4) 2the emmission spectrum of doping different content rare earth ion; Wherein a is doping Eu 3+, b is doping Sm 3+.
[embodiment]
Below in conjunction with drawings and Examples, the present invention will be further described.
Embodiment 1:
Step one: by the volume ratio of 1:2 by the Y (NO of 0.1mol/L 3) 3solution mixes with deionized water, obtains solution A;
Step 2: by the volume ratio of 2:1 by the Eu (NO of solution A and 0.5mol/L 3) 3solution mixes, and obtains solution B;
Step 3: by the volume ratio of 2:1 by the Na of 0.1mol/L 2moO 4solution mixes with deionized water, obtains solution C;
Step 4: solution C is added dropwise to solution B, magnetic agitation 10min, makes pH value of solution=6.5, obtains solution D;
Step 5: solution D is transferred in stainless steel tetrafluoroethylene reactor, reacts 48h under 140 DEG C of hydrothermal conditions, after centrifugation at 50 DEG C dry 36h, obtain a kind of spherical red fluorescent material that can be excited by UV-blue.
Embodiment 2:
Step one: by the volume ratio of 1:8 by the Y (NO of 0.1mol/L 3) 3solution mixes with deionized water, obtains solution A;
Step 2: by the volume ratio of 9:1 by the Eu (NO of solution A and 0.5mol/L 3) 3solution mixes, and obtains solution B;
Step 3: by the volume ratio of 6:1 by the Na of 0.1mol/L 2moO 4solution mixes with deionized water, obtains solution C;
Step 4: solution C is added dropwise to solution B, magnetic agitation 50min, makes pH value of solution=11.5, obtains solution D;
Step 5: solution D is transferred in stainless steel tetrafluoroethylene reactor, reacts 12h under 280 DEG C of hydrothermal conditions, after centrifugation at 85 DEG C dry 6h, obtain a kind of spherical red fluorescent material that can be excited by UV-blue.
Embodiment 3:
Step one: by the volume ratio of 1:5 by the Y (NO of 0.1mol/L 3) 3solution mixes with deionized water, obtains solution A;
Step 2: by the volume ratio of 5:1 by the Eu (NO of solution A and 0.5mol/L 3) 3solution mixes, and obtains solution B;
Step 3: by the volume ratio of 4:1 by the Na of 0.1mol/L 2moO 4solution mixes with deionized water, obtains solution C;
Step 4: solution C is added dropwise to solution B, magnetic agitation 30min, makes pH value of solution=9, obtains solution D;
Step 5: solution D is transferred in stainless steel tetrafluoroethylene reactor, reacts 30h under 210 DEG C of hydrothermal conditions, after centrifugation at 70 DEG C dry 21h, obtain a kind of spherical red fluorescent material that can be excited by UV-blue.
Embodiment 4:
Step one: by the volume ratio of 1:2 by the Y (NO of 0.1mol/L 3) 3solution mixes with deionized water, obtains solution A;
Step 2: by the volume ratio of 2:1 by the Sm (NO of solution A and 0.5mol/L 3) 3solution mixes, and obtains solution B;
Step 3: by the volume ratio of 2:1 by the Na of 0.1mol/L 2moO 4solution mixes with deionized water, obtains solution C;
Step 4: solution C is added dropwise to solution B, magnetic agitation 10min, makes pH value of solution=6.5, obtains solution D;
Step 5: solution D is transferred in stainless steel tetrafluoroethylene reactor, reacts 48h under 140 DEG C of hydrothermal conditions, after centrifugation at 50 DEG C dry 36h, obtain a kind of spherical red fluorescent material that can be excited by UV-blue.
Embodiment 5:
Step one: by the volume ratio of 1:8 by the Y (NO of 0.1mol/L 3) 3solution mixes with deionized water, obtains solution A;
Step 2: by the volume ratio of 9:1 by the Sm (NO of solution A and 0.5mol/L 3) 3solution mixes, and obtains solution B;
Step 3: by the volume ratio of 6:1 by the Na of 0.1mol/L 2moO 4solution mixes with deionized water, obtains solution C;
Step 4: solution C is added dropwise to solution B, magnetic agitation 50min, makes pH value of solution=11.5, obtains solution D;
Step 5: solution D is transferred in stainless steel tetrafluoroethylene reactor, reacts 12h under 280 DEG C of hydrothermal conditions, after centrifugation at 85 DEG C dry 6h, obtain a kind of spherical red fluorescent material that can be excited by UV-blue.
Embodiment 6:
Step one: by the volume ratio of 1:5 by the Y (NO of 0.1mol/L 3) 3solution mixes with deionized water, obtains solution A;
Step 2: by the volume ratio of 5:1 by the Sm (NO of solution A and 0.5mol/L 3) 3solution mixes, and obtains solution B;
Step 3: by the volume ratio of 4:1 by the Na of 0.1mol/L 2moO 4solution mixes with deionized water, obtains solution C;
Step 4: solution C is added dropwise to solution B, magnetic agitation 30min, makes pH value of solution=9, obtains solution D;
Step 5: solution D is transferred in stainless steel tetrafluoroethylene reactor, reacts 30h under 210 DEG C of hydrothermal conditions, after centrifugation at 70 DEG C dry 21h, obtain a kind of spherical red fluorescent material that can be excited by UV-blue.
See Fig. 1, wherein Fig. 1 a, b is respectively doping Eu 3+, Sm 3+rare earth ion prepares NaY (MoO 4) 2the XRD spectrum of fluorescent material, warp and the comparative analysis of JCPDS standard card, result shows: the diffraction peak of prepared product is consistent with JCPDS52-1802, does not have other impurity peaks to occur, illustrate that synthesized structure is sheelite tetragonal crystalline structure, and synthesized sample is pure phase NaY (MoO 4) 2, because the Eu of a small amount of doping 3+, Sm 3+do not cause sample diffraction peak shift, do not change the crystalline structure of sample.NaY (MoO 4) 2belong to rhombic system, space group structure I 41/a (88), lattice parameter is a=b=5.199nm, c=11.33nm; α=β=γ=90 °.
As seen from Figure 2, the pH value of solution is to synthesized NaY (MoO 4) 2pattern has remarkably influenced.As pH=7.0, obtained product is spherical, is evenly distributed, and particle diameter is 2 microns; Along with pH value in solution raises, as pH=9.0, obtained shape of product changes, and to become irregular class spherical from spherical for product; As pH=11.0, product presents sheet, and it is comparatively obvious to reunite; When pH value of solution continues to be increased to 13, product is needle-like.
As seen from Figure 2, in reaction system, pH value has impact clearly to obtained product pattern, when in solution during pH=7, in electric neutrality in solution, the charged character of the different crystal faces of nucleus is consistent, and crystal plane surface can be identical, and namely different crystal face growth velocity is identical, nucleus self-sow (isotropy), the spherical morphology that final formation particle is less; Improve pH value in solution, along with OH in solution -concentration increases, and different in the adsorptive power of different crystal face, the different crystal plane surface energy of final impact, cause oriented crystal growth, crystal morphology changes, along with solution ph constantly raises, crystal length-to-diameter ratio constantly increases, and as pH=13.0, product finally presents needle-like.
Fig. 3 a is NaY (MoO 4) 2: Eu 3+monitor the excitation spectrum that obtains of light at 616nm, mainly comprise two peak positions: the blue visible light district being positioned near ultraviolet region near 395nm and 465nm place, they correspond respectively to Eu 3+'s 7f 0- 5l 6with 7f 0- 5d 2transition, this interpret sample possesses can well mate with ultraviolet or blue chip LED.From Fig. 3 b, excite the transmitting spectrogram of lower sample at 465nm blue light, dominant emission peak position is positioned at 595nm, 616nm, 650nm, 700nm place, corresponds respectively to 7d 0- 7f 1, 7d 0- 7f 2, 7d 0- 7f 3, 7d 0- 7f 4transition.Wherein dominant emission peak position is set to 616nm, and this is due to Eu 3+non-centrosymmetrical Y is occupied in structure cell 3+4b lattice, and and Y 3+not isometrical replacement enhance the deformity of this crystal case, thus more depart from symmetrical environment, electric dipole transition environment improved further, thus launches the red light of 616nm.From map analysis, sample NaY (MoO 4) 2: Eu 3+a kind of there is the red fluorescence powder that researching value is applied near ultraviolet and blue-ray LED very much.
Shown in Fig. 4 a, its main excitation peak be positioned at 403nm ( 6h 5/2→ 4f 7/2), in one group of wide range of 450 ~ 500nm, 480nm place corresponds to Sm 3+'s 6h 5/2→ 4i 9/2characteristic transition peak, this shows, NaY (MoO 4) 2: Sm 3+effectively can be excited by near-ultraviolet light and blue light.Fig. 4 b is sample NaY (MoO 4) 2: Sm 3+emmission spectrum under 403nm ultraviolet excitation, by 564nm ( 4g 5/2→ 6h 5/2), 600nm and 607nm ( 4g 5/2→ 6h 7/2), 647nm ( 4g 5/2→ 6h 9/2) group peak formation, maximum emission peak is positioned at 647nm place.From transition rule, be positioned at 600nm and 607nm ( 4g 5/2→ 6h 7/2) be emitted as magnetic dipole transition, smaller by crystal field environmental influence; Be positioned at 647nm ( 4g 5/2→ 6h 9/2) be emitted as electric dipole transition, be comparatively subject to crystal field impact.Therefore, in different substrates, luminosity is different.From Fig. 4 b, NaY (MoO 4) 2: Sm 3+main emission peak is positioned at 647nm, presents stronger red emission, and this illustrates NaY (MoO 4) 2: Sm 3+red color components in white light LEDs three primary colors fluorescent powder or indigo plant can be applied to and add red compensating component in yellow pattern, that is: Sm 3+for a kind of red fluorescence powder getting a good eye value [71].
Fig. 5 a gives NaY (MoO 4) 2: Eu 3+series of samples excites lower red light emitting intensity and different doping Eu at 465nm blue light 3+relation.As seen from the figure, along with doping increases gradually, sample emission intensity first increases rear reduction, works as Eu 3+when doping is 0.04, emitted luminescence intensity is maximum.This is because luminescence center cross relaxation causes energy trasfer to arrive center of energy and the result of quencher.Occur that the reason of this kind of phenomenon can be summed up as: Eu 3+the increase of concentration increase and luminescence center, the transition probability of useful energy transfer and energy level increases, and therefore intensity concentration increases and increases; Work as Eu 3+concentration reaches 4mol%, Eu 3+be covered with parent lattice uniformly, intensity reaches maximum; Eu 3+concentration more than 4%, unnecessary Eu 3+ion is randomly dispersed in local lattice, and make on this position between luminescence center and luminescence center, and the probability that energy trasfer occurs between luminescence center and non-luminescent matrix increases, intensity reduces on the contrary.
Fig. 5 b is NaY (MoO 4) 2: Sm 3+the transmitting spectrogram of different levels of doping, works as Sm 3+when concentration is 0.04, sample luminous intensity reaches maximum, and continuing increases doping concentration of rare earth ion, and sample luminous intensity declines.This is because, on the one hand, along with rare earth ion Sm 3+the increase of concentration, interionic distance reduces, interionic Interaction enhanced, thus generate energy transfer.On the other hand, due to the cross relaxation of energy inter-stage, wherein Sm 3+→ Sm 3+between mainly with 4g 5/2+ 6h 5/2→ 6f 9/2+ 6f 9/2mode generation cross relaxation, thus cause fluorescent emission by golden quencher.

Claims (6)

1. a preparation method for the spherical red fluorescent material that can be excited by UV-blue, is characterized in that, comprise the following steps:
Step one: by 1:(2-8) volume ratio by the Y (NO of 0.1mol/L 3) 3solution mixes with deionized water, obtains solution A;
Step 2: by (2-9): the volume ratio of 1 is by the Eu (NO of solution A and 0.5mol/L 3) 3solution mixes, and obtains solution B;
Step 3: by (2-6): the volume ratio of 1 is by the Na of 0.1mol/L 2moO 4solution mixes with deionized water, obtains solution C;
Step 4: solution C is added dropwise to solution B, stirs, and makes pH value of solution=6.5-11.5, obtains solution D;
Step 5: solution D be transferred in reactor, reacts under 140 DEG C of-280 DEG C of hydrothermal conditions, dry after centrifugation, obtains a kind of spherical red fluorescent material that can be excited by UV-blue.
2. the preparation method of a kind of spherical red fluorescent material that can be excited by UV-blue according to claim 1, is characterized in that, in described step 2, and Eu (NO 3) 3solution can replace with Sm (NO 3) 3solution.
3. the preparation method of a kind of spherical red fluorescent material that can be excited by UV-blue according to claim 1, is characterized in that, in described step 4, stirs and adopts magnetic agitation 10-50min.
4. the preparation method of a kind of spherical red fluorescent material that can be excited by UV-blue according to claim 1, is characterized in that, in described step 5, reactor adopts stainless steel tetrafluoroethylene reactor.
5. the preparation method of a kind of spherical red fluorescent material that can be excited by UV-blue according to claim 1, it is characterized in that, in described step 5, the hydro-thermal reaction time is 12-48h.
6. the preparation method of a kind of spherical red fluorescent material that can be excited by UV-blue according to claim 1, is characterized in that, in described step 5, drying is dry 6-36h at 50 DEG C-85 DEG C.
CN201510351113.0A 2015-06-23 2015-06-23 Preparation method of spherical red phosphor powder capable of being excited by ultraviolet-blue light Pending CN105038791A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN106381145A (en) * 2016-08-20 2017-02-08 伊犁师范学院 Preparation method of NaY(MoO4)2:Eu<3+>, Tb<3+> series fluorescent powder
CN106520117A (en) * 2016-10-31 2017-03-22 陕西科技大学 A preparing method of LiLa(MoO4)2:Eu<3+> fluorescent powder
CN108531181A (en) * 2018-06-21 2018-09-14 东台市天源光电科技有限公司 A kind of rare earth doping fluorescent powder of anti-bombardment and preparation method thereof
CN110295044A (en) * 2019-07-22 2019-10-01 通化师范学院 A kind of very high rare earth Eu of luminous intensity3+Ion doping gadolinium molydbate lithium red fluorescence powder, preparation method thereof

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QI WU等: "Investigation of the Structure and Photoluminescence Properties of Ln3+(Eu3+, Dy3+, Sm3+) Ion-Doped NaY(MoO4)2", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 *
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106381145A (en) * 2016-08-20 2017-02-08 伊犁师范学院 Preparation method of NaY(MoO4)2:Eu<3+>, Tb<3+> series fluorescent powder
CN106520117A (en) * 2016-10-31 2017-03-22 陕西科技大学 A preparing method of LiLa(MoO4)2:Eu<3+> fluorescent powder
CN108531181A (en) * 2018-06-21 2018-09-14 东台市天源光电科技有限公司 A kind of rare earth doping fluorescent powder of anti-bombardment and preparation method thereof
CN110295044A (en) * 2019-07-22 2019-10-01 通化师范学院 A kind of very high rare earth Eu of luminous intensity3+Ion doping gadolinium molydbate lithium red fluorescence powder, preparation method thereof

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