CN103788953A - Europium-activated tellurate red phosphor and preparation method thereof - Google Patents
Europium-activated tellurate red phosphor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses europium-activated tellurate red phosphor and a preparation method of the europium-activated tellurate red phosphor and belongs to the technical field of rare earth luminescent materials. The chemical general formula of the red phosphor is Ala1-xEuxMgTeO6, wherein A refers to the element Na or K, the doping concentration range of the active ion Eu is 0 to 1, and x is less than or equal to 1. The preparation method of the red phosphor comprises the steps that (1) according to the molar ratio in the chemical general formula, corresponding raw materials are weighed accurately and ground and mixed uniformly; (2) the raw materials which are ground and mixed uniformly in the step (1) are roasted at a high temperature in the air; (3) a roasted product obtained in the step (2) is post-processed, and then the red phosphor is obtained. The red phosphor can emit strong red light after being motivated by near ultraviolet light or blue light, and the peak wavelength is about 619 nm; besides, since the red light is high in color purity, the red phosphor can be used for manufacturing of a white LED, the color rendering index of the white LED can be improved, and the color temperature of the white LED can be lowered.
Description
Technical field
The present invention relates to rare earth luminescent material technical field, more particularly, relate to a kind of red fluorescence powder take trivalent europium as active ions, take tellurate as matrix that can effectively be excited by near-ultraviolet light and blue-ray LED and preparation method thereof.
Background technology
White light emitting diode (LED) is a kind of semi-conductor solid state lighting new light sources of efficient, less energy-consumption, and its advantage comprises: current consumption is little, is only 10 – 20% of same brightness incandescent light; Low voltage, low current start, fast response time (only 60ns); Volume is little, safe and reliable, and the life-span is 100,000 hours; Thermal value is low, without ir radiation, is convenient to hidden and non-environmental-pollution (without electromagnetic interference, without mercury pollution, without broken quarrel etc.).Therefore, be considered to most possibly enter the one " green illumination light source " in general lighting field.
White light LEDs generally can be divided into following three classes: fluorescent conversion type, multi-chip are combined, single-chip Multiple Quantum Well type.Consider based on factors such as technique, cost and the states of the art, research emphasis still concentrated on exploitation early and realized the fluorescent conversion type white light LEDs of industrialization present stage, i.e. coating fluorescent powder on LED chip, thereby utilize the utilizing emitted light excitated fluorescent powder of LED chip to send visible ray, and combination results white light.
That fluorescent conversion type LED has advantages of is simple in structure, light efficiency is high and cost is low, is the main path that obtains now white light LEDs.Fluorescent material plays decisive role in fluorescent conversion type white light LEDs technology, and its performance determines the critical technical parameters such as luminescent spectrum, luminous efficiency, colour rendering index, colour temperature and the work-ing life of white light LEDs.So development white light LEDs is significant with high-efficiency fluorescence powder.
Maximum, the most typical method of commercialization white light LEDs employing is at present exactly " blue led chip+yellow fluorescent powder ", can be by blue-light excited yellow fluorescent powder (YAG:Ce in the upper coating of GaN base blue led chip (420 – 480nm)
3+), the complementary white light that forms of gold-tinted that the blue light that chip sends and fluorescent material send.Its shortcoming is exactly that this fluorescent material lacks ruddiness region spectrum and causes colour rendering index on the low side, is difficult to meet the requirement of low colour temperature illumination.Commercial red fluorescence powder is as Y
2o
2s:Eu
3+, CaS:Eu
2+low near ultraviolet or blue-light excited lower luminous efficiency, its luminous intensity only has 1/8th of blue colour fluorescent powder and green emitting phosphor brightness.In addition, under the exciting of near-ultraviolet light or blue light sulfide red fluorescent material chemical property unstable, easily decompose and produce harmful SO
2gas.The red fluorescence powder of other type has their own characteristics each, and also respectively has shortcoming, in general, not yet reaches the target that current LED technology is expected red fluorescence powder.
In view of red fluorescence powder proportion maximum, price in tricolor powder are the most expensive, and in the colour temperature of modulation white light and improve the important roles such as its color developing, the exploitation of red fluorescence powder has become the bottleneck place of white light LEDs development.Therefore, the red fluorescent powder for white radiation LED that development of new is efficient, physical and chemical performance is stable, becomes a urgent task.
Chinese Patent Application No. 201210185657.0, the applying date is on June 7th, 2012, invention and created name is: red fluorescence powder and preparation method thereof for a kind of LED; This application case discloses the europkium-activated telluric acid calcium of a kind of trivalent fluorescent material, and its chemical expression is (Ca
1-2xeu
xa
x) TeO
3.Wherein A is at least one in Li, Na, K; 0<x<0.5, this application case also discloses the preparation method of this fluorescent material: by the compound of the simple substance of Ca, Te, Eu, compound or corresponding salt and A or corresponding salt, after mix grinding is even, by high-temperature roasting, make through pulverizing, cleaning removal of impurities, oven dry aftertreatment.The fluorescent material of this application case has the features such as excitation wavelength range is wide, efficient, stable, but the Te in this application case fluorescent material chemical formula is+4 valencys, and in the preparation process of fluorescent material, be that this just causes part Te by synthesis material roasting at 600～800 ℃ in air
4+element is oxidized to more stable Te
6+, thereby the thing phase purity of the fluorescent material preparing and luminescent properties can be affected.
Summary of the invention
1. the technical problem that invention will solve
The object of the invention is to overcome the defect of existing red fluorescence powder aspect use properties, a kind of europkium-activated tellurate red fluorescence powder and preparation method thereof is provided, the chemical general formula of red fluorescence powder provided by the invention is: ALa
1 – xeu
xmgTeO
6, wherein, the valency of Te is+6 valencys; The present invention adopts high temperature solid-state method to prepare red fluorescence powder under air or oxygen atmosphere, and in product, Te element can be with stable Te
6+exist, the fluorescent material preparing is single pure phase, can effectively be excited by near-ultraviolet light or blue light, have the features such as good luminous performance, ruddiness ideal color purity and physical and chemical performance be stable, and preparation method is simple, convenient operation and realize suitability for industrialized production.
2. technical scheme
For achieving the above object, technical scheme provided by the invention is:
The europkium-activated tellurate red fluorescence powder of one of the present invention, its chemical general formula is: ALa
1 – xeu
xmgTeO
6, wherein, A represents element Na or K, the doping content scope of active ions Eu is 0<x≤1.
The preparation method of a kind of europkium-activated tellurate red fluorescence powder of the present invention, described red fluorescence powder chemical general formula is: ALa
1 – xeu
xmgTeO
6, wherein, A represents element Na or K, the doping content scope of active ions Eu is 0<x≤1; The preparation process of this red fluorescence powder is:
(1) according to the mol ratio in described chemical general formula, accurately take corresponding raw material, described raw material is containing the compound of A, containing the compound of La, containing the compound of Eu, containing the compound of Mg with containing the compound of Te, and by even raw material ground and mixed;
(2) by the uniform raw material high-temperature roasting of step (1) ground and mixed;
(3) product of roasting step (2) being obtained carries out aftertreatment, obtains described red fluorescence powder.
Preparation method as red fluorescence powder of the present invention further improves, and described in step (1), is oxide compound, nitrate, carbonate, vitriol or the oxyhydroxide containing A containing the compound of A; Be oxide compound, nitrate or the organic acid salt containing La containing the compound of La; Be oxide compound, nitrate or the organic acid salt containing Eu containing the compound of Eu; Be oxide compound, nitrate, carbonate, vitriol or the oxyhydroxide containing Mg containing the compound of Mg; Be oxide compound, oxygen acid or the oxysalt containing Te containing the compound of Te.
Preparation method as red fluorescence powder of the present invention further improves, and in step (1), raw material used is analytical pure or is better than analytical pure.
Preparation method as red fluorescence powder of the present invention further improves, and step (1) has added volatile solvent ethanol or acetone in grinding operation process.
Preparation method as red fluorescence powder of the present invention further improves, and the described high-temperature roasting of step (2) operates in air or oxygen atmosphere to be carried out, and maturing temperature is 600～1200 ℃, and roasting time is 10～48 hours.
Preparation method as red fluorescence powder of the present invention further improves, the described high-temperature roasting of step (2) is divided into two-step sintering: first pre-burning 5～20 hours under 600～800 ℃ of conditions, after cooling down by sintered powder mixed grinding again, then 900～1200 ℃ of roasting temperatures 5～28 hours.
Preparation method as red fluorescence powder of the present invention further improves, and the described aftertreatment of step (3) comprises fragmentation, selects powder, removal of impurities, oven dry and classification; Described select one or more in pickling, alkali cleaning, washing except miscellaneous operation; Described progressive operation adopts one or more in settling process, method of sieving, hydraulic elutria-tion method, air classification method.
3. beneficial effect
Adopt technical scheme provided by the invention, compared with existing known technology, there is following unusual effect:
(1) the europkium-activated tellurate red fluorescence powder that the present invention prepares, at ALa
1 – xeu
xmgTeO
6in lattice, Eu
3+in highly asymmetric micro, according to rare-earth spectrum theory, this kind of constitutional features is very beneficial for obtaining the red emission that intensity is large, purity of color is high;
(2) the europkium-activated tellurate red fluorescence powder that the present invention prepares, being applicable near ultraviolet and blue-light LED chip excites, can under the near-ultraviolet light of about 398nm and 467nm left and right blue-light excited, launch stronger wavelength and be positioned at the higher ruddiness of purity of color of 619nm left and right, can well meet the encapsulation requirement of white light LEDs, improve the colour rendering index of white light LEDs and reduce colour temperature;
(3) the europkium-activated tellurate red fluorescence powder that the present invention prepares, its physicochemical property are stable, nontoxic, nuisanceless, be exposed to for a long time in air, also not can with environment in oxygen, carbonic acid gas and steam react;
(4) preparation method of the europkium-activated tellurate red fluorescence powder of the present invention, simple for process, preparation cost is low, easy handling and realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is that chemical formula prepared by the embodiment of the present invention 1 is NaLa
0.5eu
0.5mgTeO
6x-ray powder diffraction (XRD) spectrogram of red fluorescence powder, in figure, X-coordinate represents angle of diffraction, ordinate zou represents relative diffracted intensity;
Fig. 2 is that chemical formula prepared by the embodiment of the present invention 1 is NaLa
0.5eu
0.5mgTeO
6the exciting light spectrogram of red fluorescence powder, detection wavelength is 619nm, and in figure, X-coordinate represents excitation wavelength, and ordinate zou represents relative intensity;
Fig. 3 is that chemical formula prepared by the embodiment of the present invention 1 is NaLa
0.5eu
0.5mgTeO
6the utilizing emitted light spectrogram of red fluorescence powder, excitation wavelength is 398nm and 467nm, and in figure, X-coordinate represents excitation wavelength, and ordinate zou represents relative intensity;
Fig. 4 is that chemical formula prepared by the embodiment of the present invention 6 is KLa
0.6eu
0.4mgTeO
6x-ray powder diffraction (XRD) spectrogram of red fluorescence powder, in figure, X-coordinate represents angle of diffraction, ordinate zou represents relative diffracted intensity.
Embodiment
For further understanding content of the present invention, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.
Embodiment 1
By reference to the accompanying drawings, the europkium-activated tellurate red fluorescence powder of the one of the present embodiment, the chemical formula of this red fluorescence powder is: NaLa
0.5eu
0.5mgTeO
6, the doped parameterx of Eu equals 0.5.
The present embodiment is prepared NaLa
0.5eu
0.5mgTeO
6the concrete steps of red fluorescence powder are:
Accurately weigh Eu
2o
3(99.99%) 1.073g, La
2o
3(99.99%) 0.994g, Na
2cO
3(analytical pure) 0.667g, MgO (analytical pure) 0.492g, TeO
2(99.99%) 1.986g, weighing quality is to calculate and get according to the molecular weight of the mol ratio in red fluorescence powder chemical formula and employing raw material.Above-mentioned raw materials is ground in agate mortar 1 hour, in process of lapping, adds volatile solvent ethanol, to promote grinding effect, raw material is mixed, the particle applicable sintering that diminishes, for follow-up acquisition better roasting effect lay the foundation.After raw material ground and mixed is even, put into alumina crucible, in air, under 600 ℃ of temperature condition, carry out pre-burning 20 hours, after cooling down, again grind evenly, in air, under 1200 ℃ of conditions, roasting reacts fully for 5 hours.Contriver points out, in the preparation process of fluorescent material, variation is a lot, as sintering number, sintering atmosphere, sintering temperature, sintering time, whether add fusing assistant (kind of fusing assistant, content) etc., the optimization of processing parameter is often played to vital effect to obtaining the fluorescent material of excellent properties.The present embodiment adopts two-step sintering method, moisture in first removing raw material in the pre-burning stage, impel raw material to decompose better, strengthen the reactive behavior of raw material, after cooling down through again grind, further control again presintering powder roasting longer time under higher temperature, and every one-phase all can make material reach desirable roasting effect to the control of temperature and time, research shows that the ladder intensification roasting that the present embodiment adopts can obtain roasting effect better than constant temperature disposable roasting, than multistep roasting (being more than or equal to three steps), under the prerequisite that obtains same sintering effect, can greatly save preparation cost, save time.It is also simultaneously the key factor that red fluorescence powder that the present embodiment prepares can obtain ideal effect.
To the sintered product obtaining carry out fragmentation, select powder, pickling, washing, drying operation, finally cross 200 mesh sieves and carry out stage treatment, obtaining component is NaLa
0.5eu
0.5mgTeO
6red fluorescence powder.
What deserves to be explained is, the valency of the Te element adulterating in the present embodiment red fluorescence powder is+6 valencys, than the fluorescent material of tradition doping+4 valency Te, the present embodiment is by coordinating air atmosphere downstairs sinter process, and in the red fluorescence powder product that makes to prepare, Te element can be with stable Te
6+exist, the fluorescent material preparing is single pure phase, again because contriver has carried out further optimization in the chemical composition of fluorescent material, makes the red fluorescence powder performance that the present embodiment prepares be much better than conventional commercial red fluorescence powder, specific as follows:
The europkium-activated tellurate red fluorescence powder that the present embodiment prepares, at NaLa
0.5eu
0.5mgTeO
6in lattice, Eu
3+in highly asymmetric micro, according to rare-earth spectrum theory, this kind of constitutional features is very beneficial for obtaining the red emission that intensity is large, purity of color is high.Its XRD spectra is referring to Fig. 1, as seen from Figure 1, red fluorescence powder diffraction peak intensity is high and more sharp-pointed, illustrates that synthetic fluorescent material crystal property is good, the standard card (NaLaMgTeO of the XRD spectra of the present embodiment and JCPDS (JCPDS)
6, No.82-2366) substantially identical, prove the NaLa that the present embodiment makes
0.5eu
0.5mgTeO
6red fluorescence powder is without dephasign.
The excitation spectrum of the red fluorescence powder that the present embodiment prepares as shown in Figure 2.This red fluorescence powder can belong to Eu-O charge transfer band at the broadband excitation peak of 200～350nm, and the sharp line of 350～500nm to excite be by Eu
3+4f → 4f transition of electron cause.Two main excitation peaks lay respectively at 396nm and 467nm, mate well with the output wavelength of near ultraviolet LED chip and blue-light LED chip.
The emmission spectrum of the red fluorescence powder that the present embodiment prepares under 396nm and 367nm wavelength light excite is shown in Fig. 3.Emmission spectrum is made up of a series of spikes, corresponding Eu
3+characteristic spectral line.Main emission peak is positioned at 619nm, and luminous intensity is far away higher than the emission peak at other wavelength place (as 596nm), this explanation, and the ruddiness monochromaticity of the red fluorescence powder transmitting of the present embodiment is good.
Hence one can see that, the red fluorescence powder that the present embodiment prepares is applicable near ultraviolet and blue-light LED chip excites, can under the near-ultraviolet light of about 398nm and 467nm left and right blue-light excited, launch stronger wavelength and be positioned at the higher ruddiness of purity of color of 619nm left and right, can well meet the encapsulation requirement of white light LEDs, improve the colour rendering index of white light LEDs and reduce colour temperature.
Another very outstanding being also advantageous in that of the red fluorescence powder that the present embodiment prepares, its physicochemical property are stable, nontoxic, nuisanceless, contriver is exposed to this red fluorescence powder in air for a long time, powder diffraction analysis show its not with environment in oxygen, carbonic acid gas and steam react.
It is NaLa that the present embodiment is prepared chemical formula
0.8eu
0.2mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing be substantially with embodiment 1, existing preparation process is summarized as follows:
Accurately weigh Eu
2o
3(99.99%) 0.429g, La
2o
3(99.99%) 1.590g, Na
2cO
3(analytical pure) 0.667g, MgO (analytical pure) 0.492g, TeO
2(99.99%) 1.986g, above-mentioned raw materials is ground in agate mortar 1.5 hours, after raw material ground and mixed is even, put into alumina crucible, in oxygen atmosphere, under 700 ℃ of temperature condition, carry out pre-burning 10 hours removing moisture, impel that raw material decomposes, intensified response activity, after cooling down, again grind evenly, in air, under 1000 ℃ of conditions, roasting reacts fully for 20 hours.By the sintered product obtaining carry out fragmentation, select powder, pickling, washing, oven dry, air classification, obtaining component is NaLa
0.8eu
0.2mgTeO
6red fluorescence powder.
Embodiment 3
It is NaLa that the present embodiment is prepared chemical formula
0.3eu
0.7mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing be substantially with embodiment 1, existing preparation process is summarized as follows:
Accurately weigh Eu
2o
3(99.99%) 1.503g, La
2o
3(99.99%) 0.596g, Na
2cO
3(analytical pure) 0.667g, MgO (analytical pure) 0.492g, TeO
2(99.99%) 1.986g, above-mentioned raw materials is ground in agate mortar 0.8 hour, after mixing, put into alumina crucible, in air, under 800 ℃ of temperature condition, carry out pre-burning 5 hours removing moisture, impel that raw material decomposes, intensified response activity, after cooling down, again grind evenly, in air, under 900 ℃ of conditions, roasting reacts fully for 28 hours.By the sintered product obtaining carry out fragmentation, select powder, pickling, washing, oven dry, cross 200 mesh sieves, obtaining component is NaLa
0.3eu
0.7mgTeO
6red fluorescence powder.
Embodiment 4
It is NaEuMgTeO that the present embodiment is prepared chemical formula
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing be substantially with embodiment 1, existing preparation process is summarized as follows:
Accurately weigh Eu
2o
3(99.99%) 2.147g, Na
2cO
3(analytical pure) 0.667g, MgO (analytical pure) 0.492g, TeO
2(99.99%) 1.986g grinds above-mentioned raw materials 3 hours with 200 revs/min in ball mill, adds proper amount of acetone in process of lapping.After raw material ground and mixed is even, put into alumina crucible, in oxygen atmosphere 650 ℃ carry out pre-burning 12 hours removing moisture, impel that raw material decomposes, intensified response activity, after cooling down, again grind evenly, in oxygen atmosphere, under 1100 ℃ of conditions, roasting reacts fully for 18 hours.By the sintered product obtaining carry out fragmentation, select powder, washing, oven dry, hydraulic classification, obtaining component is NaEuMgTeO
6red fluorescence powder.
Embodiment 5
It is NaLa that the present embodiment is prepared chemical formula
0.5eu
0.5mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing be substantially with embodiment 1, existing preparation process is summarized as follows:
Accurately weigh Eu (NO
3)
36H
2o (99.99%) 2.721g, La
2o
3(99.99%) 0.994g, Na
2cO
3(analytical pure) 0.667g, Mg
2(OH)
2cO
3(analytical pure) 0.988g, TeO
2(99.99%) 1.986g, above-mentioned raw materials is ground 6 hours with 220 revs/min in ball mill, after raw material ground and mixed is even, put into alumina crucible, in air 700 ℃ carry out pre-burning 15 hours removing moisture, impel that raw material decomposes, intensified response activity, after cooling down, again grind evenly, in air, under 1000 ℃ of conditions, roasting reacts fully for 23 hours.By the sintered product obtaining carry out fragmentation, select powder, pickling, washing, oven dry, cross 200 mesh sieves, obtaining component is NaLa
0.5eu
0.5mgTeO
6red fluorescence powder.
Embodiment 6
It is KLa that the present embodiment is prepared chemical formula
0.6eu
0.4mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing be substantially with embodiment 1, existing preparation process is summarized as follows:
Accurately weigh Eu (NO
3)
36H
2o (99.99%) 2.095g, La
2o
3(99.99%) 1.147g, K
2cO
3(analytical pure) 0.836g, Mg
2(OH)
2cO
3(analytical pure) 0.950g, TeO
2(99.99%) 1.911g, above-mentioned raw materials is added in agate mortar appropriate ethanol grind 1 hour, after mixing, put into alumina crucible, in air 650 ℃ carry out pre-burning 10 hours removing moisture, impel that raw material decomposes, intensified response activity, after cooling down, again grind evenly, in air, under 1100 ℃ of conditions, roasting reacts fully for 24 hours.By the sintered product obtaining carry out fragmentation, select powder, pickling, alkali cleaning, washing, oven dry, cross 200 mesh sieves, obtaining component is KLa
0.6eu
0.4mgTeO
6red fluorescence powder.
The XRD spectra of the red fluorescence powder that the present embodiment prepares is shown in Fig. 4, the NaLa preparing with embodiment 1
0.5eu
0.5mgTeO
6xRD diffractogram coincide, illustrate that the two structure is identical, good without dephasign, crystal property, can effectively be excited and send ruddiness by near-ultraviolet light and blue light equally, and ruddiness monochromaticity be better, can be applicable to white light LEDs.
Embodiment 7
It is KLa that the present embodiment is prepared chemical formula
0.6eu
0.4mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing be substantially with embodiment 1, existing preparation process is summarized as follows:
Accurately weigh Eu
2o
3(99.99%) 0.826g, La
2o
3(99.99%) 1.147g, K
2cO
3(analytical pure) 0.836g, MgO (analytical pure) 0.473g, TeO
2(99.99%) 1.911g, above-mentioned raw materials rotating speed with 180 revs/min in ball mill is ground 12 hours, after mixing, put into alumina crucible, in air 750 ℃ carry out pre-burning 8 hours removing moisture, impel that raw material decomposes, intensified response activity, after cooling down, again grind evenly, in air, under 1100 ℃ of conditions, roasting reacts fully for 18 hours.By the sintered product obtaining carry out fragmentation, select powder, pickling, washing, oven dry, cross 200 mesh sieves, obtaining component is KLa
0.6eu
0.4mgTeO
6red fluorescence powder.
Embodiment 1～7 one or more compounds of the each component of red fluorescence powder that are preferred in the process of the europkium-activated tellurate red fluorescence powder of preparation are (as the compound containing Eu has only been used Eu
2o
3and Eu (NO
3)
36H
2o), limit in view of length, the available compound that claim is enumerated is not all enumerated, and it should be noted that, right to use requires the classes of compounds of enumerating can make equally the fluorescent material identical with embodiment 1～7 performance.
Claims (8)
1. an europkium-activated tellurate red fluorescence powder, is characterized in that: its chemical general formula is: ALa
1 – xeu
xmgTeO
6, wherein, A represents element Na or K, the doping content scope of active ions Eu is 0<x≤1.
2. a preparation method for europkium-activated tellurate red fluorescence powder, is characterized in that: described red fluorescence powder chemical general formula is: ALa
1 – xeu
xmgTeO
6, wherein, A represents element Na or K, the doping content scope of active ions Eu is 0<x≤1; The preparation process of this red fluorescence powder is:
(1) according to the mol ratio in described chemical general formula, accurately take corresponding raw material, described raw material is containing the compound of A, containing the compound of La, containing the compound of Eu, containing the compound of Mg with containing the compound of Te, and by even raw material ground and mixed;
(2) by the uniform raw material high-temperature roasting of step (1) ground and mixed;
(3) product of roasting step (2) being obtained carries out aftertreatment, obtains described red fluorescence powder.
3. the preparation method of a kind of europkium-activated tellurate red fluorescence powder according to claim 2, is characterized in that: described in step (1), be oxide compound, nitrate, carbonate, vitriol or the oxyhydroxide containing A containing the compound of A; Be oxide compound, nitrate or the organic acid salt containing La containing the compound of La; Be oxide compound, nitrate or the organic acid salt containing Eu containing the compound of Eu; Be oxide compound, nitrate, carbonate, vitriol or the oxyhydroxide containing Mg containing the compound of Mg; Be oxide compound, oxygen acid or the oxysalt containing Te containing the compound of Te.
4. the preparation method of a kind of europkium-activated tellurate red fluorescence powder according to claim 3, is characterized in that: in step (1), raw material used is analytical pure or is better than analytical pure.
5. the preparation method of a kind of europkium-activated tellurate red fluorescence powder according to claim 4, is characterized in that: step (1) has added volatile solvent ethanol or acetone in grinding operation process.
6. the preparation method of a kind of europkium-activated tellurate red fluorescence powder according to claim 3, it is characterized in that: the described high-temperature roasting of step (2) operates in air or oxygen atmosphere to be carried out, maturing temperature is 600～1200 ℃, and roasting time is 10～48 hours.
7. the preparation method of a kind of europkium-activated tellurate red fluorescence powder according to claim 6, it is characterized in that: the described high-temperature roasting of step (2) is divided into two-step sintering: first pre-burning 5～20 hours under 600～800 ℃ of conditions, after cooling down by sintered powder mixed grinding again, then 900～1200 ℃ of roasting temperatures 5～28 hours.
8. the preparation method of a kind of europkium-activated tellurate red fluorescence powder according to claim 7, is characterized in that: the described aftertreatment of step (3) comprises fragmentation, selects powder, removal of impurities, oven dry and classification; Described select one or more in pickling, alkali cleaning, washing except miscellaneous operation; Described progressive operation adopts one or more in settling process, method of sieving, hydraulic elutria-tion method, air classification method.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694127A (en) * | 2014-12-25 | 2015-06-10 | 陕西科技大学 | Red fluorescent powder and preparation method thereof |
| CN108587627A (en) * | 2018-06-01 | 2018-09-28 | 苏州大学张家港工业技术研究院 | Eu3+Ion-activated fluorine chlorine telluric acid bismuth and its preparation method and application |
| CN113717724A (en) * | 2021-09-28 | 2021-11-30 | 常州工程职业技术学院 | Eu (Eu)3+Doped transition metal tellurium oxide fluorescent powder and preparation method and application thereof |
| CN115710507A (en) * | 2022-11-17 | 2023-02-24 | 广东工业大学 | Tellurate near-infrared fluorescent material and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694127A (en) * | 2014-12-25 | 2015-06-10 | 陕西科技大学 | Red fluorescent powder and preparation method thereof |
| CN108587627A (en) * | 2018-06-01 | 2018-09-28 | 苏州大学张家港工业技术研究院 | Eu3+Ion-activated fluorine chlorine telluric acid bismuth and its preparation method and application |
| CN113717724A (en) * | 2021-09-28 | 2021-11-30 | 常州工程职业技术学院 | Eu (Eu)3+Doped transition metal tellurium oxide fluorescent powder and preparation method and application thereof |
| CN115710507A (en) * | 2022-11-17 | 2023-02-24 | 广东工业大学 | Tellurate near-infrared fluorescent material and preparation method and application thereof |
| CN115710507B (en) * | 2022-11-17 | 2023-10-31 | 广东工业大学 | Tellurate near infrared fluorescent material and preparation method and application thereof |
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| CN103788953B (en) | 2016-02-24 |
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