CN104152143B - Rare earth-containing functional material and preparation method thereof - Google Patents
Rare earth-containing functional material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a rare earth-containing functional material and a preparation method, belongs to the technical field of the rare earth-doped functional materials and relates to the composition and a preparation method of the functional material. The chemical composition of the functional material is M＜3-a-x＞N＜a＞Si＜1+b＞O＜5+2b-0.5c＞X＜c＞: xEu, wherein M is one or a combination of more than one element selected from Mg, Ca, Si and Ba, N is one or a combination of two of Ti and Zr, and X is one or a combination of more than one element of F, Cl, Br and I; a, b, c and x are molar fractions, a is greater than 0 and less than or equal to 0.25, b is greater than or equal to 0 and less than or equal to 0.2, c is greater than or equal to 0 and less than or equal to 1.0 and x is greater than 0 and less than or equal to 0.3. The functional material is prepared through the steps of weighing corresponding raw materials according to the desired stoichiometric ratio, and then performing operations such as grinding, even mixing, roasting in reducing atmosphere, cooling, crushing, water washing and sieving. The functional material prepared by the method has excellent optical characteristics and stability.
Description
Technical field
The invention belongs to technical field of function materials, more particularly to a kind of chemical composition containing rear-earth-doped functional material
And preparation method thereof.
Background technology
White light emitting diode is known as after the forth generation lighting source after incandescent lamp, fluorescent lamp, high-intensity discharge lamp,
Have energy-conservation, long lifespan, pollution-free, efficiency high, small volume, fast response time, driving voltage low compared with conventional illumination sources
Etc. various advantages, mobile phone, the backlight of display, indicator lamp, various illuminations, billboard, traffic lights are widely applied to
Etc. aspect, be increasingly valued by people.
The method for generally making LED emit white light is combined with some fluorescent materials with luminous semiconductor chip, and the method is current
The main technology for using is to excite YAG yellow fluorescent materials with the blue light of 460nm, but because lacking red color light component in launching light,
And then limit application of the fluorescent material in high performance illumination field.Therefore, needing one kind badly can be stimulated by blue light, Neng Goufa
Orange light or feux rouges are penetrated, and more current YAG yellow fluorescent materials have the functional material of more excellent properties.With silicate as matrix
Functional material can be excited effectively by 460nm blue lights, launch orange light to orange light, improve colour rendering index；And silicic acid
Salt fluorescent material have it is wider excite wave band and emission band, but such material has that luminous intensity is not high and stability phase
To poor problem.This patent provides a kind of functional material containing rare earth that can be effectively excited by 460nm blue lights, and the material passes through
The spectral region that regulation chemical composition can launch is from orange light to orange light, and the functional material has luminous intensity higher
And stability.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided it is a kind of it is being stimulated by blue light, meat can be sent
The preparation method containing the new function material of rare earth and the functional material of the visible 570nm ~ 610nm light of eye.
To achieve the above object, the invention provides a kind of rear-earth-doped functional material, M is specifically comprised3-a-xNaSi1+ bO5+2b-0.5cXc﹕ xEu, wherein M are the combination selected from one or more elements in Mg, Ca, Sr or Ba, and N is in Ti or Zr
One or two elements combination, X be F, Cl, Br or I in one or more elements combination；Wherein a, b, c, x
It is molar fraction, and 0<A≤0.25,0≤b≤0.2,0≤c≤1.0,0<x≤0.3.
In the chemical composition of above-mentioned functional material, it is preferable that M be Sr or Ba or combinations thereof, N be Ti or Zr or it
Combination, X be F or Cl or combinations thereof；Or M at least contains Sr, N at least contains Zr, and X at least contains Cl；Or M is extremely
Contain Ba less, N at least contains Zr, and X at least contains Cl；Or M at least contains Sr, N at least contains Ti, and X at least contains Cl；Or
M at least contains Ba, and N at least contains Ti, and X at least contains Cl；A, b, c, x are molar fraction, wherein 0<A≤0.25,0≤b≤
0.2,0≤c≤1.0,0<x≤0.3.
The method for preparing above-mentioned functions material mainly comprises the following steps：
（1）By chemical formula metering than weighing corresponding raw material dosage, then weigh raw material gross mass 0.5 ~ 8% flux,
Mix and be fully ground；
（2）Above-mentioned raw materials are placed in high temperature furnace, under reducing atmosphere pre-burning, calcined temperature is 800 ~ 1200 DEG C, pre-burning
Time is 1 ~ 5 hour；Then temperature rises to 1300 ~ 1500 DEG C and carries out high-temperature roasting, and 3 ~ 10 hours high-temperature roasting time, control rises
5 ~ 10 DEG C/min of warm speed；
（3）Treat that above-mentioned sinter temperature in reducing atmosphere is down to room temperature, the sinter is crushed, be washed with deionized water
Wash, then dried at a temperature of 110 ~ 150 DEG C, obtain final product required function material.
In the step（1）In raw material used be the carbonate of respective element, nitrate, acetate, oxide or halogen
Compound.
In the step（1）In flux used be H3BO3, alkali halide, in alkali carbonate and ammonium halide
The combination of one or more, consumption for raw material gross mass 1 ~ 5%.
In the step（2）Middle reducing atmosphere is for carbon dust, CO atmosphere or containing H2Volume fraction is mixed for 60% ~ 100% hydrogen nitrogen
Close gas.
In the step（2）Middle calcined temperature is preferably 1000 ~ 1200 DEG C, and burn-in time is preferably 2 ~ 4 hours, high temperature roasting
Burn temperature and be preferably 1300 ~ 1400 DEG C, the high-temperature roasting time is preferably 4 ~ 8 hours.
In the composition that this patent is proposed, a kind of alkaline-earth metal is used（Such as Ba）A small amount of another alkaline-earth metal of substitution（Such as Sr）Can
Other crystal cases of host lattice case are different to be formed in lattice.The luminous meeting that a small amount of foreign crystal case is produced
Regulation oikocryst case lights, and brings it about slight red shift or blue shift, the ratio of the degree of red shift or blue shift doped chemical together
It is relevant.On the one hand the addition of halogen compounds can optimize Growing Process of Crystal Particles as flux reduction sintering temperature, and refinement is brilliant
Grain, makes granulation；The opposing party is bright can to influence lattice parameter, lattice is produced distortion, so as to adjust emission wavelength.Ti、Zr
Contour valent metal enters in lattice, and certain Lacking oxygen occurs in order to meet the charge balance around it, appropriate dense
The Lacking oxygen of degree can promote energy transfer as sensitizer, so as to improve luminous intensity.
Compared with prior art, beneficial effects of the present invention have：1st, preparation method is simple, and prepared functional material has
Good optical characteristics and stability；2nd, the functional material prepared can be excited by the light in the range of 430 ~ 490nm, especially by
The light of 450 ~ 470nm is efficiently excited, therefore may apply to blue light activated white light LEDs；3rd, by adjust Sr, Ba, Ca or
The content of Mg and halogen can adjust transmitting peak position from 570nm to 610nm in the range of change, being applied in white light LEDs can
To significantly improve colour rendering index；4th, the phase of the functional material can be obviously improved by adding Ti or Zr elements and adjusting its content
To luminous intensity.5th, excessive SiO2Emission peak red shift can be made, and luminous intensity can be improved.
Brief description of the drawings
Fig. 1 Sr2.76Ba0.2Zr0.01Si1.10O5.20The excitation spectrum of ﹕ 0.02Eu samples
Fig. 2 Sr2.76Ba0.2Zr0.01Si1.10O5.20The emission spectrum of ﹕ 0.02Eu samples（λex=460nm）
Specific embodiment
The following is embodiments of the invention, it will help a further understanding of the present invention, but the model that the present invention is protected
Enclose and be not restricted by the embodiments, the scope of the present invention is determined by claim.
Comparative example：
By chemical formula Sr2.98SiO5﹕ 0.02Eu prepare required sample.Take the relative luminous intensity of functional material under the composition
It is 100.Luminescence maintenance rate is 80 at 150 DEG C of the composition material.Luminescence maintenance rate is the fluorescent material at 150 DEG C at 150 DEG C Luminous intensity and material luminous intensity ratio at room temperature percentage.
The present invention is provided and a kind of contains Rare Earth Functional Materials, it is characterised in that the chemical composition of the functional material is：M3-a- xNaSi1+bO5+2b-0.5cXc﹕ xEu, wherein M are the combination selected from one or more elements in Mg, Ca, Sr or Ba, and N is Ti
Or the combination of one or two elements in Zr, X is the combination of one or more elements in F, Cl, Br or I；a、b、c、
X is molar fraction, wherein 0≤a≤0.25,0≤b≤0.2,0≤c≤1.0,0<x≤0.3.
Convenient in order to describe compound, wherein M, N, X are element code name, and specific M is selected from Mg, Ca, Sr or Ba
The combination of kind or more than one elements, N is the combination of one or two elements in Ti or Zr, and X is in F, Cl, Br or I
The combination of kind or more than one elements.Wherein, there is footmark in the element code name lower right corner, each element code name in representation compound composition
Molar ratio relation, specially a, b, c, x, such M3-a-xNaSi1+bO5+2b-0.5cXc﹕ xEu just represent a series of functional compounds.
In example below：Sr2.76Ba0.2Zr0.01Si1.10O5.19Cl0.02﹕ 0.02Eu.Wherein Si, O, Eu are in the periodic table of elements
Element, be well known to a person skilled in the art common technical knowledge.
Embodiment 1：
By chemical formula Sr2.97Zr0.005Si1.10O5.20﹕ 0.02Eu weigh analytically pure strontium carbonate（SrCO3）8.769g, oxidation
Zirconium（ZrO2）0.012g, silica（SiO2）1.322g, and high-purity europium oxide（Eu2O3）0.070g, and weigh 0.10g
Analytically pure Na2CO3Make flux.Load corundum crucible after load weighted raw mill is mixed, be in hydrogen nitrogen volume ratio
Under the reducing atmosphere of 60 ﹕ 40, prior to 1000 DEG C of pre-burnings 4 hours, then it is calcined 4 hours at 1400 DEG C, after cooling spends product
Ion is washed 3 times, is dried under the conditions of 110 DEG C after filtering, the functional material of composition needed for obtaining final product.
Embodiment 2：
By chemical formula Sr2.97Zr0.005Si1.10O5.19Cl0.02﹕ 0.02Eu weigh analytically pure strontium carbonate（SrCO3）
8.740g, zirconium oxide（ZrO2）0.012g, silica（SiO2）1.322g, strontium chloride（SrCl2）0.032g, and it is high-purity
Europium oxide（Eu2O3）0.070g, and weigh the analytically pure H of 0.505g3BO3Make flux.Load weighted raw mill is mixed
After load corundum crucible, under the reducing atmosphere of carbon dust, prior to 1200 DEG C of pre-burnings 2 hours, then be calcined 4 hours at 1300 DEG C, treat
Product is washed with deionized water 3 times after cooling, is dried under the conditions of 120 DEG C after filtering, the functional material of composition needed for obtaining final product.
Embodiment 3：
By chemical formula Sr2.76Ba0.2Zr0.01Si1.10O5.20﹕ 0.02Eu weigh analytically pure strontium carbonate（SrCO3）8.149g、
Barium carbonate（BaCO3）0.789g, zirconium oxide（ZrO2）0.024g, silica（SiO2）1.322g, and high-purity europium oxide
（Eu2O3）0.070g, and weigh the analytically pure Li of 0.303g2CO3Make flux.Filled after load weighted raw mill is mixed
Enter corundum crucible, under the reducing atmosphere of CO, prior to 1000 DEG C of pre-burnings 2 hours, then be calcined 8 hours at 1400 DEG C, after cooling
Product is washed with deionized water 3 times, is dried under the conditions of 150 DEG C after filtering, the functional material of composition needed for obtaining final product.The function material
Material can absorb the light of 430 ~ 490nm scopes, it is possible to send light of the main peak value positioned at 606nm.If Fig. 1 is the work(under the composition
The exciting light spectrogram of energy material；Fig. 2 is the luminescent spectrum figure of functional material under the composition under 460nm light irradiations.
Embodiment 4：
By chemical formula Sr2.76Ba0.2Zr0.01Si1.10O5.19Cl0.02﹕ 0.02Eu weigh analytically pure strontium carbonate（SrCO3）
8.149g, barium carbonate（BaCO3）0.750g, zirconium oxide（ZrO2）0.024g, silica（SiO2）1.322g, barium chloride
（BaCl2）0.042g, and high-purity europium oxide（Eu2O3）0.070g, and weigh the analytically pure H of 0.305g3BO3Do fluxing
Agent.Load corundum crucible after load weighted raw mill is mixed, under the reducing atmosphere of pure hydrogen, prior to 1000 DEG C of pre-burnings 2
Hour, then be calcined 8 hours at 1300 DEG C, product is washed with deionized water 3 times after cooling, dried under the conditions of 120 DEG C after filtering
It is dry, the functional material of composition needed for obtaining final product.
Embodiment 5：
By chemical formula Sr2.76Ba0.2Ti0.01Si1.10O5.20﹕ 0.02Eu weigh analytically pure strontium carbonate（SrCO3）8.149g、
Barium carbonate（BaCO3）0.789g, titanium dioxide（TiO2）0.016g, silica（SiO2）1.216g, and high-purity europium oxide
（Eu2O3）0.070g, and weigh the analytically pure Na of 0.305g2CO3Make flux.Filled after load weighted raw mill is mixed
Enter corundum crucible, under the reducing atmosphere that hydrogen nitrogen volume ratio is 80 ﹕ 20, prior to 1000 DEG C of pre-burnings 4 hours, then in 1300 DEG C of roastings
4 hours, product is washed with deionized water 3 times after cooling, is dried under the conditions of 120 DEG C after filtering, the work(of composition needed for obtaining final product
Can material.
Embodiment 6-44 is the example for meeting patent claims scope, as shown in table 1.Pass through as can be seen from the table
The content of regulation Sr, Ba, Ca or Mg and halogen can adjust transmitting peak position；Can by the doping for adjusting Ti, Zr or rare earth
Significantly improve the luminous intensity and stability of the functional material.
Table 1
| Embodiment | Fluorescent material chemical composition | Launching light main peak/nm | Relative luminous intensity | 150 DEG C of luminescence maintenance rates |
| Comparative example | Sr2.98SiO5﹕ 0.02Eu | 592 | 100 | 80 |
| 1 | Sr2.97Zr0.005Si1.10O5.20﹕ 0.02Eu | 594 | 147 | 86 |
| 2 | Sr2.97Zr0.005Si1.10O5.19Cl0.02﹕ 0.02Eu | 588 | 142 | 84 |
| 3 | Sr2.76Ba0.2Zr0.01Si1.10O5.20﹕ 0.02Eu | 606 | 149 | 86 |
| 4 | Sr2.76Ba0.2Zr0.01Si1.10O5.19Cl0.02﹕ 0.02Eu | 597 | 154 | 84 |
| 5 | Sr2.76Ba0.2Ti0.01Si1.10O5.20﹕ 0.02Eu | 605 | 142 | 84 |
| 6 | Sr2.97Zr0.005SiO5﹕ 0.02Eu | 590 | 138 | 83 |
| 7 | Sr2.97Zr0.005SiO4.99Cl0.02﹕ 0.02Eu | 582 | 136 | 83 |
| 8 | Sr2.76Ba0.2Zr0.01SiO5﹕ 0.02Eu | 604 | 143 | 84 |
| 9 | Sr2.76Ba0.2Zr0.01SiO4.99Cl0.02﹕ 0.02Eu | 594 | 150 | 86 |
| 10 | Sr2.97Ti0.005Si1.10O5.20﹕ 0.02Eu | 594 | 142 | 84 |
| 11 | Sr2.97Ti0.005Si1.10O5.19Cl0.02﹕ 0.02Eu | 595 | 141 | 84 |
| 12 | Sr2.76Ba0.2Ti0.01Si1.10O5.20﹕ 0.02Eu | 581 | 142 | 84 |
| 13 | Sr2.76Ba0.2Ti0.01Si1.10O5.19Cl0.02﹕ 0.02Eu | 590 | 140 | 83 |
| 14 | Sr2.94Zr0.01Ti0.01Si1.10O5.20﹕ 0.02Eu | 596 | 153 | 87 |
| 15 | Sr2.978Zr0.001Si1.10O5.20﹕ 0.02Eu | 593 | 143 | 84 |
| 16 | Sr2.88Zr0.05Si1.10O5.20﹕ 0.02Eu | 594 | 162 | 90 |
| 17 | Sr2.78Zr0.1Si1.10O5.20﹕ 0.02Eu | 595 | 158 | 88 |
| 18 | Sr2.48Zr0.25Si1.10O5.20﹕ 0.02Eu | 596 | 150 | 86 |
| 19 | Sr2.96Zr0.01Si1.10O5.19Cl0.02﹕ 0.02Eu | 583 | 157 | 88 |
| 20 | Sr2.74Ba0.2Zr0.02Si1.10O5.20﹕ 0.02Eu | 608 | 160 | 89 |
| 21 | Sr2.92Zr0.005Si1.10O5.20﹕ 0.07Eu | 596 | 157 | 88 |
| 22 | Sr2.87Zr0.005Si1.10O5.20﹕ 0.12Eu | 598 | 156 | 88 |
| 23 | Sr2.69Zr0.005Si1.10O5.20﹕ 0.3Eu | 601 | 153 | 87 |
| 24 | Sr2.71Ba0.2Zr0.01Si1.10O5.20﹕ 0.07Eu | 607 | 168 | 93 |
| 25 | Sr2.71Ba0.2Zr0.01Si1.10O5.19Cl0.02﹕ 0.07Eu | 597 | 166 | 91 |
| 26 | Sr2.83Zr0.05Si1.10O5.20﹕ 0.07Eu | 598 | 167 | 93 |
| 27 | Sr2.96Zr0.01Si1.10O5.19F0.02﹕ 0.02Eu | 585 | 149 | 86 |
| 28 | Sr2.96Zr0.01Si1.10O5.19Br0.02﹕ 0.02Eu | 582 | 146 | 85 |
| 29 | Sr2.96Zr0.01Si1.10O5.19I0.02﹕ 0.02Eu | 586 | 141 | 84 |
| 30 | Sr2.96Zr0.01Si1.10O5.18F0.02Cl0.02﹕ 0.02Eu | 580 | 150 | 87 |
| 31 | Sr2.96Zr0.01Si1.10O5.10Cl0.2﹕ 0.02Eu | 576 | 151 | 87 |
| 32 | Sr2.96Zr0.01Si1.10O4.95Cl0.5﹕ 0.02Eu | 574 | 139 | 83 |
| 33 | Sr2.96Zr0.01Si1.10O4.70Cl1.0﹕ 0.02Eu | 571 | 141 | 83 |
| 34 | Sr2.56Ba0.4Zr0.01Si1.10O5.20﹕ 0.02Eu | 609 | 145 | 85 |
| 35 | Sr2.76Ca0.2Zr0.01Si1.10O5.20﹕ 0.02Eu | 597 | 151 | 87 |
| 36 | Sr2.76Mg0.2Zr0.01Si1.10O5.20﹕ 0.02Eu | 603 | 147 | 85 |
| 37 | Sr2.56Ba0.2Ca0.2Zr0.01Si1.10O5.20﹕ 0.02Eu | 606 | 153 | 87 |
| 38 | Ba2.97Zr0.005Si1.10O5.20﹕ 0.02Eu | 603 | 157 | 88 |
| 39 | Ba2.97Zr0.005Si1.10O5.19Cl0.02﹕ 0.02Eu | 592 | 155 | 87 |
| 40 | Ba2.97Ti0.005Si1.10O5.19Cl0.02﹕ 0.02Eu | 593 | 153 | 87 |
| 41 | Ba2.97Ti0.005Si1.10O5.20﹕ 0.02Eu | 601 | 156 | 88 |
| 42 | Ba2.77Ca0.2Zr0.005Si1.10O5.20﹕ 0.02Eu | 582 | 149 | 85 |
| 43 | Ba2.77Mg0.2Zr0.005Si1.10O5.20﹕ 0.02Eu | 584 | 148 | 85 |
| 44 | Sr2.76Ba0.2Zr0.01Si1.20O5.40﹕ 0.02Eu | 608 | 150 | 86 |
Claims (8)
1. it is a kind of to contain Rare Earth Functional Materials, it is characterised in that the chemical composition of the functional material is：M3-a-xNaSi1+bO5+2b-0.5cXc﹕
XEu, wherein M are the combination selected from one or more elements in Mg, Ca, Sr or Ba, and at least contain Sr, N be Ti or
The combination of one or two elements in Zr, and at least contain Zr, X is one or more elements in F, Cl, Br or I
Combination, and when c is not 0, X at least contains Cl；A, b, c, x are molar fraction, wherein 0<A≤0.25,0≤b≤0.2,0≤c
≤ 1.0,0<x≤0.3.
2. it is a kind of to contain Rare Earth Functional Materials, it is characterised in that the chemical composition of the functional material is：M3-a-xNaSi1+bO5+2b-0.5cXc﹕
XEu, wherein M are the combination selected from one or more elements in Mg, Ca, Sr or Ba, and at least contain Ba, N be Ti or
The combination of one or two elements in Zr, and at least contain Zr, X is one or more elements in F, Cl, Br or I
Combination, and when c is not 0, X at least contains Cl；A, b, c, x are molar fraction, wherein 0<A≤0.25,0≤b≤0.2,0≤c
≤ 1.0,0<x≤0.3.
3. functional material as claimed in claim 1, it is characterised in that the chemical composition of the functional material is：M3-a-xNaSi1+ bO5+2b-0.5cXc﹕ xEu, wherein M are the combination selected from one or more elements in Mg, Ca, Sr or Ba, and are at least contained
Sr, N are the combination of Ti and Zr, and X is the combination of one or more elements in F, Cl, Br or I, and when c is not 0, X is extremely
Contain Cl less；A, b, c, x are molar fraction, wherein 0<A≤0.25,0≤b≤0.2,0≤c≤1.0,0<x≤0.3.
4. functional material as claimed in claim 2, it is characterised in that the chemical composition of the functional material is：M3-a-xNaSi1+ bO5+2b-0.5cXc﹕ xEu, wherein M are the combination selected from one or more elements in Mg, Ca, Sr or Ba, and are at least contained
Ba, N are the combination of Ti and Zr, and X is the combination of one or more elements in F, Cl, Br or I, and when c is not 0, X is extremely
Contain Cl less；A, b, c, x are molar fraction, wherein 0<A≤0.25,0≤b≤0.2,0≤c≤1.0,0<x≤0.3.
5. a kind of preparation method containing Rare Earth Functional Materials as described in claim any one of 1-4, it is characterised in that specific step
It is rapid as follows：
(1) by chemical formula metering than weighing corresponding raw material, then weigh raw material gross mass 0.5~8% flux, mix simultaneously
It is fully ground；
(2) above-mentioned raw materials are placed in high temperature furnace, under reducing atmosphere pre-burning, calcined temperature is 800~1200 DEG C, burn-in time
It is 1~5 hour；Then temperature rises to 1300~1500 DEG C and carries out high-temperature roasting, and 3~10 hours high-temperature roasting time, control rises
5~10 DEG C/min of warm speed；
(3) treat that above-mentioned sinter temperature in reducing atmosphere is down to room temperature, the sinter is crushed, be washed with deionized, so
Dried at a temperature of 110~150 DEG C afterwards, obtain final product required function material.
6. a kind of preparation method containing Rare Earth Functional Materials as claimed in claim 5, it is characterised in that used in step (1)
Raw material is the combination of the one or more than one in carbonate, nitrate, acetate, oxide, the halide of respective element；
The flux is H3BO3, alkali halide, the combination of one or more in alkali carbonate and ammonium halide, consumption is
The 1~5% of raw material gross mass.
7. a kind of preparation method containing Rare Earth Functional Materials as claimed in claim 5, it is characterised in that described in step (2)
Reducing atmosphere is for carbon dust, CO atmosphere or containing H2Volume fraction is 60%~100% hydrogen nitrogen mixed gas.
8. a kind of preparation method containing Rare Earth Functional Materials as claimed in claim 5, it is characterised in that described in step (2)
Calcined temperature is 1000~1200 DEG C, and burn-in time is 2~4 hours, and high-temperature roasting temperature is 1300~1400 DEG C, high-temperature roasting
Time is 4~8 hours.
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