CN103788953B - A kind of europkium-activated tellurate red fluorescence powder and preparation method thereof - Google Patents
A kind of europkium-activated tellurate red fluorescence powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of europkium-activated tellurate red fluorescence powder and preparation method thereof, belong to rare earth luminescent material technical field.Red fluorescence powder chemical general formula of the present invention is ALa
1 – xeu
xmgTeO
6, wherein, A represents element Na or K, and the doping content scope of active ions Eu is 0 & lt; X≤1.The preparation process of red fluorescence powder of the present invention is: (1), according to the mol ratio in described chemical general formula, accurately takes corresponding raw material, and mixed by raw mill; (2) by the high-temperature roasting in atmosphere of the uniform raw material of step (1) ground and mixed; (3) product of roasting that step (2) obtains is carried out aftertreatment, the red fluorescence powder described in acquisition.Red fluorescence powder of the present invention can launch stronger red light under the exciting of near-ultraviolet light or blue light, and peak wavelength is about 619nm, and red light color purity is high, can be used for manufacturing white light LEDs, to improve the colour rendering index of white light LEDs and to reduce colour temperature.
Description
Technical field
The present invention relates to rare earth luminescent material technical field, more particularly, relate to a kind of effectively can be excited by near-ultraviolet light and blue-ray LED be active ions with trivalent europium, take tellurate as red fluorescence powder of matrix and preparation method thereof.
Background technology
White light emitting diode (LED) is a kind of semiconducting solid illumination new light sources of efficient, less energy-consumption, and its advantage comprises: current consumption is little, is only 10 – 20% of same intensity incandescent bulb; 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, the one " green illumination light source " most possibly entering general lighting field is considered to.
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 and developed comparatively early and realized the fluorescent conversion type white light LEDs of industrialization present stage, i.e. coating fluorescent powder on LED chip, utilize the utilizing emitted light excitated fluorescent powder of LED chip thus send visible ray, and combination produces white light.
Fluorescent conversion type LED has the advantage that structure is simple, light efficiency is high and cost is low, is the main path obtaining now white light LEDs.Fluorescent material plays decisive role in fluorescent conversion type White light LED technology, and its performance determines the critical technical parameters such as the luminescent spectrum of white light LEDs, luminous efficiency, colour rendering index, colour temperature and work-ing life.So development white light LEDs high-efficiency fluorescence powder is significant.
Current commercialization white light LEDs adopts maximum, most typical method to be exactly " blue LED die+yellow fluorescent powder ", namely can by blue-light excited yellow fluorescent powder (YAG:Ce in the upper coating of GaN base blue LED die (420 – 480nm)
3+), the blue light that chip sends and the gold-tinted that fluorescent material sends complementation form white light.Its shortcoming is exactly that this fluorescent material lacks red light region spectrum and causes colour rendering index on the low side, is difficult to the requirement meeting the illumination of low colour temperature.Commercial red fluorescence powder is as Y
2o
2s:Eu
3+, CaS:Eu
2+near ultraviolet or blue-light excited lower luminous efficiency low, 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 in tricolor powder is maximum, price is the most expensive, and modulating the colour temperature of white light and improving 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, and invention and created name is: a kind of LED red fluorescence powder and preparation method thereof; This application case discloses a kind of trivalent europkium-activated telluric acid calcium 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, through pulverizing, cleaning removal of impurities, oven dry aftertreatment is made.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 be that this just causes part Te by synthesis material roasting at 600 ~ 800 DEG C in atmosphere in the preparation process of fluorescent material
4+element is oxidized to more stable Te
6+, the thing phase purity of the fluorescent material thus prepared and luminescent properties can be affected.
Summary of the invention
1. invent the technical problem that will solve
The object of the invention is to overcome the defect of existing red fluorescence powder in use properties, provide a kind of europkium-activated tellurate red fluorescence powder and preparation method thereof, 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 with stable Te
6+exist, the fluorescent material prepared is single pure phase, effectively can 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, and 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, and 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, the compound containing La, the compound containing Eu, the compound containing Mg and the compound containing Te, and is mixed by raw mill;
(2) by uniform for step (1) ground and mixed raw material high-temperature roasting;
(3) product of roasting that step (2) obtains is carried out aftertreatment, the red fluorescence powder described in acquisition.
Preparation method as red fluorescence powder of the present invention further improves, and is containing the oxide compound of A, nitrate, carbonate, vitriol or oxyhydroxide containing the compound of A described in step (1); Compound containing La is containing the oxide compound of La, nitrate or organic acid salt; Compound containing Eu is containing the oxide compound of Eu, nitrate or organic acid salt; Compound containing Mg is containing the oxide compound of Mg, nitrate, carbonate, vitriol or oxyhydroxide; Compound containing Te is containing the oxide compound of Te, oxygen acid or oxysalt.
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) adds volatile solvent ethanol or acetone in grinding operation process.
Preparation method as red fluorescence powder of the present invention further improves, and the high-temperature roasting described in step (2) operates in air or oxygen atmosphere to be carried out, and maturing temperature is 600 ~ 1200 DEG C, and roasting time is 10 ~ 48 hours.
Preparation method as red fluorescence powder of the present invention further improves, high-temperature roasting described in step (2) is divided into two-step sintering: first pre-burning 5 ~ 20 hours under 600 ~ 800 DEG C of conditions, by sintered powder mixed grinding again after cooling down, then 900 ~ 1200 DEG C of roasting temperatures 5 ~ 28 hours.
Preparation method as red fluorescence powder of the present invention further improves, the aftertreatment described in step (3) comprises fragmentation, selects powder, removal of impurities, oven dry and classification; Described except miscellaneous operation select in pickling, alkali cleaning, washing one or more; Described progressive operation adopt in settling process, method of sieving, hydraulic elutria-tion method, air classification method one or more.
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 for preparing of the present invention, at ALa
1 – xeu
xmgTeO
6in lattice, Eu
3+be in highly asymmetric micro, theoretical according to rare-earth spectrum, 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 for preparing of the present invention, applicable near ultraviolet and blue-light LED chip excite, can the near-ultraviolet light of about 398nm and about 467nm blue-light excited under launch stronger wavelength and be positioned at the higher ruddiness of the purity of color of about 619nm, the encapsulation requirement of white light LEDs can well be met, improve the colour rendering index of white light LEDs and reduce colour temperature;
(3) the europkium-activated tellurate red fluorescence powder for preparing of the present invention, its physicochemical property are stablized, nontoxic, nuisanceless, expose in atmosphere for a long time, also can not react with the oxygen in environment, carbonic acid gas and steam;
(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 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, and ordinate zou represents relative diffracted intensity;
Fig. 2 is 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, determined wavelength is that in 619nm, figure, X-coordinate represents excitation wavelength, and ordinate zou represents relative intensity;
Fig. 3 is 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 that in 398nm and 467nm, figure, X-coordinate represents excitation wavelength, and ordinate zou represents relative intensity;
Fig. 4 is 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, and ordinate zou represents relative diffracted intensity.
Embodiment
For understanding content of the present invention further, 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 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 prepares NaLa
0.5eu
0.5mgTeO
6the concrete steps of red fluorescence powder are:
Precise 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 get according to the molecular weight calculating of the mol ratio in red fluorescence powder chemical formula and employing raw material.Above-mentioned raw materials is ground 1 hour in agate mortar, in process of lapping, adds volatile solvent ethanol, to promote grinding effect, raw material is mixed, particle diminish be applicable to sintering, for follow-up acquisition better roasting effect lay the foundation.Put into alumina crucible after being mixed by raw mill, carry out pre-burning 20 hours in atmosphere under 600 DEG C of temperature condition, after cooling down, grinding is even again, and under 1200 DEG C of conditions, roasting reacts fully for 5 hours in atmosphere.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., often to the fluorescent material obtaining excellent properties, vital effect is played to the optimization of processing parameter.The present embodiment adopts two-step sintering method, moisture in raw material is first removed in the pre-burning stage, raw material is impelled to decompose better, strengthen the reactive behavior of raw material, through again grinding after cooling down, control the presintering powder roasting longer time at a higher temperature more further, and the roasting effect that every one-phase all can make material reach desirable to the control of temperature and time, research shows that the steps intensification roasting that the present embodiment adopts can obtain roasting effect better compared to constant temperature disposable roasting, compared to multistep roasting (being more than or equal to three steps), greatly preparation cost can be saved under the prerequisite obtaining same sintering effect, save time.It is also simultaneously the key factor that red fluorescence powder that the present embodiment prepares can obtain ideal effect.
Fragmentation is carried out to the sintered product obtained, selects powder, pickling, washing, drying operation, finally cross 200 mesh sieves carry out stage treatment, namely obtaining component is NaLa
0.5eu
0.5mgTeO
6red fluorescence powder.
What deserves to be explained is, the valency of the Te element adulterated in the present embodiment red fluorescence powder is+6 valencys, compared to the fluorescent material of Traditional dopant+4 valency Te, the present embodiment, by coordinating air atmosphere downstairs sinter process, makes Te element in the red fluorescence powder product prepared can with stable Te
6+exist, the fluorescent material prepared is single pure phase, and again because contriver has carried out further optimization in the chemical composition of fluorescent material, the red fluorescence powder performance that the present embodiment is prepared is 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+be in highly asymmetric micro, theoretical according to rare-earth spectrum, 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 see Fig. 1, as seen from Figure 1, red fluorescence powder diffraction peak intensity is high and comparatively sharp-pointed, illustrates that the fluorescent material crystal property of synthesis is good, the XRD spectra of the present embodiment and JCPDS (JCPDS) standard card (NaLaMgTeO
6, No.82-2366) substantially identical, prove the NaLa that the present embodiment is obtained
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 excites is shown in Fig. 3.Emmission spectrum is made up of a series of spike, 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), and this illustrates, the ruddiness monochromaticity that the red fluorescence powder of the present embodiment is launched is good.
It can thus be appreciated that, the red fluorescence powder that the present embodiment prepares is applicable near ultraviolet and blue-light LED chip excites, can the near-ultraviolet light of about 398nm and about 467nm blue-light excited under launch stronger wavelength and be positioned at the higher ruddiness of the purity of color of about 619nm, the encapsulation requirement of white light LEDs can well be met, 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 stablized, nontoxic, nuisanceless, this red fluorescence powder exposes in atmosphere by contriver for a long time, and powder diffraction analysis shows that it does not react with the oxygen in environment, carbonic acid gas and steam.
Embodiment 2
The present embodiment preparative chemistry formula is NaLa
0.8eu
0.2mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing, substantially with embodiment 1, to be now summarized as follows preparation process:
Precise 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 1.5 hours in agate mortar, alumina crucible is put into after being mixed by raw mill, carry out under 700 DEG C of temperature condition in oxygen atmosphere pre-burning 10 hours removing moisture, impel feed material degradation, intensified response is active, after cooling down, grinding is even again, and under 1000 DEG C of conditions, roasting reacts fully for 20 hours in atmosphere.The sintered product obtained is carried out fragmentation, selects powder, pickling, washing, oven dry, air classification, namely obtaining component is NaLa
0.8eu
0.2mgTeO
6red fluorescence powder.
Embodiment 3
The present embodiment preparative chemistry formula is NaLa
0.3eu
0.7mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing, substantially with embodiment 1, to be now summarized as follows preparation process:
Precise 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 0.8 hour in agate mortar, alumina crucible is put into after mixing, carry out under 800 DEG C of temperature condition in atmosphere pre-burning 5 hours removing moisture, impel feed material degradation, intensified response is active, after cooling down, grinding is even again, and under 900 DEG C of conditions, roasting reacts fully for 28 hours in atmosphere.The sintered product obtained is carried out fragmentation, selects powder, pickling, washing, oven dry, cross 200 mesh sieves, namely obtaining component is NaLa
0.3eu
0.7mgTeO
6red fluorescence powder.
Embodiment 4
The present embodiment preparative chemistry formula is NaEuMgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing, substantially with embodiment 1, to be now summarized as follows preparation process:
Precise 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 process of lapping, adds proper amount of acetone in ball mill.Alumina crucible is put into after being mixed by raw mill, in oxygen atmosphere 650 DEG C carry out pre-burning 12 hours removing moisture, impel feed material degradation, intensified response is active, after cooling down, grinding is even again, and in oxygen atmosphere, under 1100 DEG C of conditions, roasting reacts fully for 18 hours.The sintered product obtained is carried out fragmentation, selects powder, washing, oven dry, hydraulic classification, namely obtaining component is NaEuMgTeO
6red fluorescence powder.
Embodiment 5
The present embodiment preparative chemistry formula is NaLa
0.5eu
0.5mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing, substantially with embodiment 1, to be now summarized as follows preparation process:
Precise 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, alumina crucible is put into after being mixed by raw mill, in atmosphere 700 DEG C carry out pre-burning 15 hours removing moisture, impel feed material degradation, intensified response is active, after cooling down, grinding is even again, and under 1000 DEG C of conditions, roasting reacts fully for 23 hours in atmosphere.The sintered product obtained is carried out fragmentation, selects powder, pickling, washing, oven dry, cross 200 mesh sieves, namely obtaining component is NaLa
0.5eu
0.5mgTeO
6red fluorescence powder.
Embodiment 6
The present embodiment preparative chemistry formula is KLa
0.6eu
0.4mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing, substantially with embodiment 1, to be now summarized as follows preparation process:
Precise 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 ethanol in proper amount and grind 1 hour, alumina crucible is put into after mixing, in atmosphere 650 DEG C carry out pre-burning 10 hours removing moisture, impel feed material degradation, intensified response is active, after cooling down, grinding is even again, and under 1100 DEG C of conditions, roasting reacts fully for 24 hours in atmosphere.The sintered product obtained is carried out fragmentation, selects powder, pickling, alkali cleaning, washing, oven dry, cross 200 mesh sieves, namely 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 prepared with embodiment 1
0.5eu
0.5mgTeO
6xRD diffractogram coincide, both explanations structure is identical, good without dephasign, crystal property, can effectively be excited by near-ultraviolet light and blue light and send ruddiness equally, and ruddiness monochromaticity is better, can be applicable to white light LEDs.
Embodiment 7
The present embodiment preparative chemistry formula is KLa
0.6eu
0.4mgTeO
6red fluorescence powder, preparation method and the red fluorescence powder performance for preparing, substantially with embodiment 1, to be now summarized as follows preparation process:
Precise 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 is ground 12 hours with the rotating speed of 180 revs/min in ball mill, alumina crucible is put into after mixing, in atmosphere 750 DEG C carry out pre-burning 8 hours removing moisture, impel feed material degradation, intensified response is active, after cooling down, grinding is even again, and under 1100 DEG C of conditions, roasting reacts fully for 18 hours in atmosphere.The sintered product obtained is carried out fragmentation, selects powder, pickling, washing, oven dry, cross 200 mesh sieves, namely obtaining component is KLa
0.6eu
0.4mgTeO
6red fluorescence powder.
Embodiment 1 ~ 7 in the process of the europkium-activated tellurate red fluorescence powder of preparation just preferred one or more compounds of each component of red fluorescence powder (as the compound containing Eu has only used Eu
2o
3with Eu (NO
3)
36H
2o), in view of length limit, the Usable compounds that claim is enumerated all is not enumerated, it should be noted that, use the classes of compounds that claim is enumerated can obtain the fluorescent material identical with embodiment 1 ~ 7 performance equally.
Claims (1)
1. 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, and 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 oxide compound of A, nitrate, carbonate, vitriol or oxyhydroxide; Compound containing La is containing the oxide compound of La, nitrate or organic acid salt; Containing the oxide compound of Eu, nitrate or organic acid salt; Containing the oxide compound of Mg, nitrate, carbonate, vitriol or oxyhydroxide and the compound containing Te, wherein, the compound containing Te is tellurium dioxide, the oxygen acid of Te or oxysalt, and is mixed by raw mill; In grinding operation process, add volatile solvent ethanol or acetone, and raw material used is analytical pure or is better than analytical pure;
(2) by uniform for step (1) ground and mixed raw material high-temperature roasting, described high-temperature roasting operates in air or oxygen atmosphere to be carried out, and be divided into two-step sintering: first pre-burning 20 hours under 600 DEG C of conditions, by sintered powder mixed grinding again after cooling down, then 1200 DEG C of roasting temperatures 5 hours;
(3) product of roasting that step (2) obtains carried out fragmentation, select powder, removal of impurities, oven dry and classification aftertreatment, described except miscellaneous operation select in pickling, alkali cleaning, washing one or more; Described progressive operation adopt in settling process, method of sieving, hydraulic elutria-tion method, air classification method one or more; Red fluorescence powder described in acquisition.
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| CN108587627B (en) * | 2018-06-01 | 2020-03-17 | 苏州大学 | Eu3+Ion-activated bismuth fluorochlorotelluroate and preparation method and application thereof |
| CN113717724B (en) * | 2021-09-28 | 2023-03-17 | 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 |
| 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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