CN103627393B - Tungsten molybdate red phosphor powder and preparation method and application thereof - Google Patents

Tungsten molybdate red phosphor powder and preparation method and application thereof Download PDF

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CN103627393B
CN103627393B CN201310586572.8A CN201310586572A CN103627393B CN 103627393 B CN103627393 B CN 103627393B CN 201310586572 A CN201310586572 A CN 201310586572A CN 103627393 B CN103627393 B CN 103627393B
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red phosphor
phosphor powder
compound
preparation
tungsten
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CN103627393A (en
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黄彦林
祁淑云
王婧
魏东磊
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Anhui Xiangneng Electric Power Technology Co ltd
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Suzhou University
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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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

Abstract

The invention discloses tungsten molybdate red phosphor powder. The tungsten molybdate red phosphor powder is characterized in that the chemical formula of the tungsten molybdate red phosphor powder is Cs[2-2x]Eu2xMg2M3O12, wherein M is Mo or W, x is the molar ratio of Eu<3+> substituting for Cs<+>, and x is greater than or equal to 0.001 and less than 0.25. The red phosphor powder prepared by the method has high degree of crystallinity and good luminous quality; preparation conditions are safe, a preparation method is simple, low in cost, safe and pollution-free. The excitation wavelength of the tungsten molybdate red phosphor powder is mainly in ultraviolet and blue light areas of a range of 250-490 nm; being excited by near ultraviolet, the red phosphor powder can emit high efficient and stable red light, which is completely matched with the radiation wavelength of a near ultraviolet InGaN chip, so that the red phosphor powder can be matched with proper amount of blue phosphor powder and green phosphor powder to be coated and packaged outside an InGaN diode to prepare white light LED (light emitting diode) lighting equipment, therefore, the tungsten molybdate red phosphor powder can be well applied to a near-ultraviolet white light LED. The invention also provides a preparation method for the red phosphor powder. The preparation method has simple processes, is easy to operate, and is safe and pollution-free, and the tungsten molybdate red phosphor powder product is easy to collect.

Description

A kind of tungsten molybdate red phosphor and its preparation method and application
Technical field
The present invention relates to a kind of inorganic fluorescent luminescent material and its preparation method and application, in particular to a kind of in ultraviolet to the tungsten hydrochlorate fluorescent material of blue-light excited lower transmitting red fluorescence, can apply and be packaged in outside InGaN diode, for the preparation of White-light LED illumination device, belong to phosphor technical field.
Background technology
LED (Light Emitting Diode) is as the green illumination light source of a new generation, be widely used in lighting field, especially white light LEDs, have that current consumption is few, long service life, operating voltage are low, stable performance, shock resistance is strong, the advantages such as volume is little, cost is low, luminescence response is fast, energy-conserving and environment-protective, thus obtain and pay attention to more and more widely and research, particularly the developing rapidly of blue, purple and near ultraviolet LED in recent years, makes LED replace incandescent light and luminescent lamp becomes possibility at lighting field.
Prepare white light LEDs and mostly be unable to do without fluorescent RE powder, realizing White light LED technology at present has a variety of method, has wherein obtained the mainly blue-light LED chip coating yellow fluorescent powder Y of commercial applications 3al 5o 12: Ce 3+the single-chip type white light LEDs be prepared from, another kind is that the near ultraviolet excitation three primary colors fluorescent powder utilizing near ultraviolet LED chip (GaN) to send obtains white light, but, because lack high efficiency red phosphor powder, cause color developing on the low side, terms of settlement obtains high colour rendering index by adding red fluorescence powder.Therefore, preparation utilizes ultraviolet or near ultraviolet LED chip to coordinate red, blue, green three primary colors fluorescent powder to be compounded to form white light, which can obtain higher color developing, and colour temperature is mated arbitrarily within 2500 ~ 10000K scope, thus has more wide application prospect.
At present, yellow both domestic and external and green emitting phosphor are very ripe in package application, and red fluorescence powder also exists poor stability, inefficient defect, becomes the bottleneck of white light LEDs luminescence.Report and the red fluorescence powder applied mainly contain Eu 3+the vanadic acid alkali excited, phosphate base, boric acid alkali, oxyfluoride base etc.But its ultraviolet, blue-light excited under, luminous efficiency is low, poor stability, and synthesis technique is complicated, cost is higher, can not meet actual requirement.Y 2o 3: Eu 3+it is a kind of conventional rare earth red fluorescent powder, this fluorescent material launches ruddiness under the exciting of UV-light, receptivity is strong, efficiency of conversion is high, but it is high to prepare this material preparation temperature, reaction times is longer, and the powder granule of preparation is uneven, complex process, energy consumption and cost are higher, easily absorb water in air and carbonic acid gas and cause luminous intensity to decline.Therefore, a kind of efficient stable long lifetime red fluorescence powder under ultraviolet is extremely blue-light excited and preparation method thereof is studied significant.
At Eu 3+in the red fluorescence powder activated, molybdate has many excellent properties as the fluorescent material of substrate material.Be a kind of molybdate red phosphor and preparation method thereof disclosed in Chinese invention patent CN101698798A, its structural formula is Na 0.5-yliyGd 0.5-xeu xmoO 4; Wherein, 0.05≤x≤0.5,0.05≤y≤0.5.This molybdate red phosphor can effectively be excited by near-ultraviolet light (396 nanometer) and blue light (466 nanometer) respectively, and emission peak is positioned at 615 nanometers, and luminosity is high, stable luminescent property.Be a kind of preparation method of molybdate red phosphor disclosed in Chinese invention patent CN103113889A, its chemical formula is MMoO 4: Eu 3+, R +, RE 3+; M=Ca, Sr, Ba; R=Li, Na, K; RE=Gd, Sm, Bi.The dispersiveness of the powder that this invention obtains is relatively good, particle fine uniform, and agglomeration traits is very significantly improved, and technical process is simple, even particle distribution, and has good luminous efficiency.But, Eu 3+the tungsten hydrochlorate sill Cs activated 2-2xeu 2xmg 2m 3o 12there is not been reported.
Summary of the invention
The present invention seeks to: low in ultraviolet, blue-light excited lower luminous efficiency for overcoming existing red fluorescence powder, poor stability, and the deficiency that synthesis technique is complicated, cost is higher, and provide that a kind of degree of crystallinity is high, luminous mass good, preparation condition safety, preparation technology are simple, cost is low, the tungsten molybdate red phosphor of safety non-pollution, its ultraviolet to blue-light excited lower can the red-emitting of efficient stable.
Technical scheme of the present invention is: a kind of tungsten molybdate red phosphor, it is characterized in that its chemical formula is: Cs 2-2xeu 2xmg 2m 3o 12, wherein M is Mo(molybdenum), W(tungsten) in one, x is Eu 3+replace Cs +mol ratio, 0.001≤x<0.25.
Further, fluorescent material described in the present invention at wavelength be the ultraviolet of 250 ~ 490 nanometers under blue-light excited, launch the red fluorescence that predominant wavelength is 612 nanometers.
The present invention provides a kind of preparation method of above-mentioned tungsten molybdate red phosphor simultaneously, and this preparation method's process is simple, easy handling; product easily collecting; and employing air atmosphere, without the need to rare gas element or protection of reducing atmosphere, preparation technology's safety; synthesis temperature lower (700 ~ 900 DEG C); can the energy be saved, reduce costs, pollution-free, discharge without waste water and gas; environmental friendliness, is especially applicable to continuous prodution.Concrete employing high temperature solid-state method, comprises the following steps:
(1) by chemical formula Cs 2-2xeu 2xmg 2m 3o 12in the mol ratio of each element, take containing cesium ion Cs +compound, containing europium ion Eu 3+compound, containing magnesium ion Mg 2+compound and containing the compound of M element as raw material, grind and mix, obtaining mixture, wherein x is Eu 3+replace Cs +mol ratio, 0.001≤x<0.25;
(2) by said mixture precalcining 1 ~ 2 time in air atmosphere, calcining temperature is 300 ~ 650 DEG C, and single calcination time is 2 ~ 12 hours;
(3) by step 2) calcining after product naturally cooling after, grind and mix, calcining in air atmosphere, calcining temperature is 700 ~ 900 DEG C, and calcination time is 6 ~ 15 hours, obtains required tungsten molybdate red phosphor after naturally cooling.
Further, described in the present invention containing cesium ion Cs +compound be one in cesium carbonate, cesium nitrate, cesium sulfate, Cs2O; Described contains magnesium ion Mg 2+compound be one in magnesium nitrate, magnesium sulfate, magnesium basic carbonate, magnesium oxide.
Further, the compound containing M element described in the present invention refers to containing molybdenum ion Mo 6+compound and containing tungsten ion W 6+compound in one, wherein said containing molybdenum ion Mo 6+compound be one in molybdenum oxide, molybdenum acid ammonia, containing tungsten ion W 6+compound be one in Tungsten oxide 99.999, wolframic acid ammonia.
Further, described in the present invention containing europium ion Eu 3+compound be one in europium sesquioxide, europium nitrate, europium sulfate.
Further, the calcining temperature in the present invention described in step (2) is 350 ~ 650 DEG C, and calcination time is 3 ~ 11 hours; Calcining temperature described in described step (3) is 700 ~ 850 DEG C, and calcination time is 7 ~ 14 hours.
The present invention also provides the application of above-mentioned tungsten molybdate red phosphor, excitation wavelength mainly in 250 ~ 490 nanometer ultraviolets to blue region, the red fluorescence that predominant wavelength is 612 nanometers is launched under near ultraviolet excitated, mate the radiation wavelength of near ultraviolet InGaN chip completely, the blueness that it can coordinate and green emitting phosphor, apply and be packaged in outside InGaN diode, preparing White-light LED illumination device, meet the application of near ultraviolet type white light LEDs preferably.
Advantage of the present invention is:
1, the tungsten molybdate red phosphor that prepared by the present invention has good chemical stability and thermostability, is also the fluorescent synthetic materials with high-luminous-efficiency simultaneously, has higher crystallinity and visible light permeability.
2, the excitation wavelength of tungsten molybdate red phosphor prepared of the present invention mainly in 250 ~ 490 nanometer ultraviolets to blue region, ruddiness is launched under near ultraviolet excitated, mate the radiation wavelength of near ultraviolet InGaN chip completely, it can coordinate appropriate blueness and green emitting phosphor, apply and be packaged in outside InGaN diode, White-light LED illumination equipment can be prepared, meet the application of near ultraviolet type white light LEDs preferably.
3, the preparation method of described tungsten molybdate red phosphor provided by the invention, its prepared atmosphere is air atmosphere, and without the need to rare gas element or protection of reducing atmosphere, preparation technology's safety, synthesis temperature lower (700 ~ 900 DEG C), can save the energy, reduce costs.
4, the preparation method of described tungsten molybdate red phosphor provided by the invention, its preparation process is simple, easy handling, product easily collecting, pollution-free, without waste water and gas discharge, environmental friendliness, especially applicable continuous prodution.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction pattern of the material sample prepared by the embodiment of the present invention 1 technical scheme;
Fig. 2 is the scanning electron microscope (SEM) photograph of the material sample prepared by the embodiment of the present invention 1 technical scheme;
Fig. 3 is the exciting light spectrogram of the ultraviolet that obtains under the light detection of 612 nanometers of the material sample prepared by the embodiment of the present invention 1 technical scheme to blue region;
Fig. 4 is the luminescent spectrum figure of material sample under the optical excitation of 395 nanometers prepared by the embodiment of the present invention 1 technical scheme;
Fig. 5 is the decay of luminescence graphic representation that the material sample prepared by the embodiment of the present invention 1 technical scheme obtains under the light of 612 nanometers detects;
Fig. 6 is the luminescent spectrum figure of material sample under the optical excitation of 395 nanometers prepared by the embodiment of the present invention 2 technical scheme;
Fig. 7 is the luminescent spectrum figure of material sample under the optical excitation of 395 nanometers prepared by the embodiment of the present invention 3 technical scheme.
Embodiment
Embodiment: technical solution of the present invention is further described below in conjunction with drawings and Examples.
Embodiment 1:
Preparation Cs 1.9eu 0.1mg 2mo 3o 12
According to chemical formula Cs 1.9eu 0.1mg 2mo 3o 12in the mol ratio of each element, take cesium carbonate Cs respectively 2cO 3: 1.548 grams, europium sesquioxide Eu 2o 3: 0.088 gram, ammonium molybdate (NH 4) 6mo 7o 244H 2o:2.649 gram, magnesium basic carbonate 4MgCO 3mg (OH) 25H 2o:0.971 gram, grinds in agate mortar and after mixing, select air atmosphere first time calcining, temperature is 350 DEG C, and calcination time 3 hours, is then cooled to room temperature, takes out sample; By the raw material of first time calcining, fully mixed grinding is even again, and again calcine in air atmosphere, temperature 550 DEG C, calcination time 7 hours, is then chilled to room temperature, takes out sample; Be placed on air calcination in retort furnace after finally it again fully being ground, calcining temperature is 850 DEG C, and calcination time is 14 hours, namely obtains tungsten molybdate red phosphor.
See accompanying drawing 1, it is the X-ray powder diffraction pattern of the sample prepared by the present embodiment technical scheme, and XRD test result shows, prepared material C s 1.9eu 0.1mg 2mo 3o 12for monophase materials, the impurity thing without any other exists mutually.
See accompanying drawing 2, it is the scanning electron microscope (SEM) photograph of the material sample prepared by the embodiment of the present invention 1 technical scheme, and SEM test result shows, prepared material granule particle diameter at 2 microns, complete crystallization.
See accompanying drawing 3, it is the exciting light spectrogram in ultraviolet blue region obtained material sample monitoring utilizing emitted light 612 nanometer prepared by the technology of the present invention, as can be seen from the figure, the emitting red light of this material excite the main ultraviolet between 250 ~ 490 nanometers in source to blue region, ultraviolet can be mated well and excite to blue-light LED chip.
See accompanying drawing 4, it is the luminescent spectrum that the sample prepared by the present embodiment technical scheme obtains under near-ultraviolet light 395 nanometer excites, the main center emission wavelength of this material is the emitting red light wave band of 612 nanometers, calculate through CIE simultaneously, learn that its coordinate is x=0.667, y=0.332, also just in time drops on red area.
See accompanying drawing 5, it is the decay of luminescence curve of the sample prepared by the present embodiment technical scheme, and this curve presents single exponent ring-down, and luminescent lifetime is 1288 μ s.
Embodiment 2:
Preparation Cs 1.5eu 0.5mg 2w 3o 12
According to chemical formula Cs 1.5eu 0.5mg 2w 3o 12in the mol ratio of each element, take cesium nitrate CsNO respectively 3: 0.731 gram, europium nitrate Eu (NO 3) 3: 0.558 gram, Tungsten oxide 99.999 WO 3: 1.739 grams, magnesium nitrate Mg (NO 3) 26H 2o:1.283 gram, grinds in agate mortar and after mixing, select air atmosphere first time calcining, temperature is 350 DEG C, and calcination time 4 hours, is then cooled to room temperature, takes out sample; By the raw material of first time calcining, fully mixed grinding is even again, and again calcine in air atmosphere, temperature 500 DEG C, calcination time 11 hours, is then chilled to room temperature, takes out sample; Be placed on air calcination in retort furnace after finally it again fully being ground, calcining temperature is 800 DEG C, and calcination time is 7 hours, namely obtains tungsten molybdate red phosphor.
The tungsten molybdate red phosphor obtained, its main structure properties, excitation spectrum, decay of luminescence are similar to embodiment 1.
Fig. 6 is the luminescent spectrum figure of material sample under the optical excitation of 395 nanometers prepared by the embodiment of the present invention 2 technical scheme, the main center emission wavelength of this material is the emitting red light wave band of 612 nanometers, calculate through CIE simultaneously, learn that its coordinate is x=0.667, y=0.332, also just in time drops on red area.
Embodiment 3:
Preparation Cs 1.6eu 0.4mg 2mo 3o 12
According to chemical formula Cs 1.6eu 0.4mg 2mo 3o 12in the mol ratio of each element, take cesium sulfate Cs respectively 2sO 4: 1.448 grams, europium sesquioxide Eu 2o 3: 0.352 gram, molybdenum oxide MoO 3: 2.160 grams, magnesium sulfate MgSO 4: 1.205 grams, to grind in agate mortar and after mixing, select air atmosphere first time calcining, temperature is 380 DEG C, and calcination time 5 hours, is then cooled to room temperature, takes out sample; By the raw material of first time calcining, fully mixed grinding is even again, and again calcine in air atmosphere, temperature 600 DEG C, calcination time 8 hours, is then chilled to room temperature, takes out sample; Be placed on air calcination in retort furnace after finally it again fully being ground, calcining temperature is 700 DEG C, and calcination time is 10 hours, namely obtains tungsten molybdate red phosphor.
The tungsten molybdate red phosphor obtained, its main structure properties, excitation spectrum, decay of luminescence are similar to embodiment 1.
Fig. 7 is the luminescent spectrum figure of material sample under the optical excitation of 395 nanometers prepared by the embodiment of the present invention 2 technical scheme, the main center emission wavelength of this material is the emitting red light wave band of 612 nanometers, calculate through CIE simultaneously, learn that its coordinate is x=0.667, y=0.332, also just in time drops on red area.
Embodiment 4:
Preparation Cs 1.8eu 0.2mg 2w 3o 12
According to chemical formula Cs 1.8eu 0.2mg 2w 3o 12in the mol ratio of each element, take cesium carbonate Cs respectively 2cO 4: 0.978 gram, europium sulfate Eu 2(SO 4) 3: 0.194 gram, ammonium tungstate (NH 4) 10w 12o 41: 2.536 grams, magnesium basic carbonate 4MgCO 3mg (OH) 25H 2o:0.648 gram, grinds in agate mortar and after mixing, select air atmosphere first time calcining, temperature is 360 DEG C, and calcination time 4 hours, is then cooled to room temperature, takes out sample; By the raw material of first time calcining, fully mixed grinding is even again, and again calcine in air atmosphere, temperature 650 DEG C, calcination time 10 hours, is then chilled to room temperature, takes out sample; Be placed on air calcination in retort furnace after finally it again fully being ground, calcining temperature is 820 DEG C, and calcination time is 11 hours, namely obtains tungsten molybdate red phosphor.
The tungsten molybdate red phosphor obtained, its main structure properties, excitation spectrum, luminescent spectrum are similar to embodiment 1 with decay of luminescence.
Embodiment 5:
Preparation Cs 1.7eu 0.3mg 2mo 3o 12
According to chemical formula Cs 1.7eu 0.3mg 2mo 3o 12in the mol ratio of each element, take cesium nitrate Cs respectively 2o:1.978 gram, europium sesquioxide Eu 2o 3: 0.264 gram, ammonium molybdate (NH 4) 6mo 7o 24: 2.648 grams, magnesium oxide MgO:0.4038 gram, grinds in agate mortar and after mixing, select air atmosphere first time calcining, temperature is 350 DEG C, and calcination time 5 hours, is then cooled to room temperature, takes out sample; By the raw material of first time calcining, fully mixed grinding is even again, and again calcine in air atmosphere, temperature 490 DEG C, calcination time 9 hours, is then chilled to room temperature, takes out sample; Be placed on air calcination in retort furnace after finally it again fully being ground, calcining temperature is 850 DEG C, and calcination time is 13 hours, namely obtains tungsten molybdate red phosphor.
The tungsten molybdate red phosphor obtained, its main structure properties, excitation spectrum, luminescent spectrum are similar to embodiment 1 with decay of luminescence.
Embodiment 6:
Preparation Cs 1.998eu 0.002mg 2w 3o 12
According to chemical formula Cs 1.998eu 0.002mg 2w 3o 12in the mol ratio of each element, take cesium carbonate Cs respectively 2cO 4: 1.086 grams, europium nitrate Eu (NO 3) 3: 0.003 gram, Tungsten oxide 99.999 WO 3: 2.318 grams, magnesium chloride Mg Cl 26H 2o:1.356 gram, grinds in agate mortar and after mixing, select air atmosphere first time calcining, temperature is 350 DEG C, and calcination time 6 hours, is then cooled to room temperature, takes out sample; By the raw material of first time calcining, fully mixed grinding is even again, and again calcine in air atmosphere, temperature 510 DEG C, calcination time 11 hours, is then chilled to room temperature, takes out sample; Be placed on air calcination in retort furnace after finally it again fully being ground, calcining temperature is 840 DEG C, and calcination time is 10 hours, namely obtains tungsten molybdate red phosphor.
The tungsten molybdate red phosphor obtained, its main structure properties, excitation spectrum, luminescent spectrum are similar to embodiment 1 with decay of luminescence.
Certain above-described embodiment is just exemplifying of illustrating that technical conceive of the present invention and feature do and non exhaustive, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All modifications done according to the spirit of main technical schemes of the present invention, all should be encompassed within protection scope of the present invention.

Claims (8)

1. a tungsten molybdate red phosphor, is characterized in that its chemical formula is: Cs 2-2xeu 2xmg 2m 3o 12, wherein M is the one in Mo, W, and x is Eu 3+replace Cs +mol ratio, 0.001≤x<0.25.
2. a kind of tungsten molybdate red phosphor according to claim 1, it is characterized in that described fluorescent material at wavelength be the ultraviolet of 250 ~ 490 nanometers under blue-light excited, launch the red fluorescence that predominant wavelength is 612 nanometers.
3. a preparation method for tungsten molybdate red phosphor as claimed in claim 1 or 2, is characterized in that adopting high temperature solid-state method, comprises the following steps:
(1) by chemical formula Cs 2-2xeu 2xmg 2m 3o 12in the mol ratio of each element, take containing cesium ion Cs +compound, containing europium ion Eu 3+compound, containing magnesium ion Mg 2+compound and containing the compound of M element as raw material, grind and mix, obtaining mixture, wherein x is Eu 3+replace Cs +mol ratio, 0.001≤x<0.25;
(2) by said mixture precalcining 1 ~ 2 time in air atmosphere, calcining temperature is 300 ~ 650 DEG C, and single calcination time is 2 ~ 12 hours;
(3) by step 2) calcining after product naturally cooling after, grind and mix, calcining in air atmosphere, calcining temperature is 700 ~ 900 DEG C, and calcination time is 6 ~ 15 hours, obtains required tungsten molybdate red phosphor after naturally cooling.
4. preparation method according to claim 3, is characterized in that: described contains cesium ion Cs +compound be one in cesium carbonate, cesium nitrate, cesium sulfate, Cs2O; Described contains magnesium ion Mg 2+compound be one in magnesium nitrate, magnesium sulfate, magnesium basic carbonate, magnesium oxide.
5. preparation method according to claim 3, is characterized in that: the described compound containing M element refers to containing molybdenum ion Mo 6+compound and containing tungsten ion W 6+compound in one, wherein said containing molybdenum ion Mo 6+compound be one in molybdenum oxide, ammonium molybdate, containing tungsten ion W 6+compound be one in Tungsten oxide 99.999, ammonium tungstate.
6. preparation method according to claim 3, is characterized in that: described contains europium ion Eu 3+compound be one in europium sesquioxide, europium nitrate, europium sulfate.
7. preparation method according to claim 3, is characterized in that: the calcining temperature described in step (2) is 350 ~ 650 DEG C, and calcination time is 3 ~ 11 hours; Calcining temperature described in described step (3) is 700 ~ 850 DEG C, and calcination time is 7 ~ 14 hours.
8. an application for tungsten molybdate red phosphor as claimed in claim 1 or 2, is characterized in that: coordinated blue and green emitting phosphor, apply and be packaged in outside InGaN diode, prepare White-light LED illumination device.
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