CN102477298B - Luminescent material and preparation method thereof - Google Patents
Luminescent material and preparation method thereof Download PDFInfo
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- CN102477298B CN102477298B CN201010562500.6A CN201010562500A CN102477298B CN 102477298 B CN102477298 B CN 102477298B CN 201010562500 A CN201010562500 A CN 201010562500A CN 102477298 B CN102477298 B CN 102477298B
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Abstract
The invention belongs to the field of luminescent materials, and discloses a luminescent material and a preparation method thereof. The chemical general formula of the luminescent material is La1-xRexAO3, wherein A refers to at least one of Al, In and Ga, Re refers to at least one of Tm, Tb, Eu, Sm, Gd, Dy, Ce and Pr, and the value of the x ranges from 0.001 to 0.3. The luminous intensity of the luminescent material can exceed that of LaGaO3 prepared by a solid-phase method, and commercial ZnS: Ag, Cl luminous intensity can be achieved. Furthermore, preparation temperature of the La1-xRexAO3 can be greatly reduced by the preparation method, and the luminescent material and the preparation method thereof are simple in operation, free of pollution, simple in process, easy in preparation, low in equipment requirements, beneficial to industrial production and widely applicable to the field of luminescent material preparation.
Description
Technical field
The present invention relates to field of photovoltaic materials, relate in particular to the luminescent material of the sour lanthanum doped with rare-earth elements of a kind of aluminium (or indium or gallium).The invention still further relates to the preparation method of luminescent material.
Background technology
Aluminium (gallium, indium) salt luminescent material is under cathode-ray exciting, and its luminescent properties is better than commercial luminescent material ZnS:Ag, Cl and LaGaO
3: the luminescent properties of Tm, has great application prospect.Yet, our experiment shows, the aluminium of preparing by high temperature solid-state method, sol-gel method, coprecipitation method (gallium, indium) salt luminescent material, not only sintering temperature is at 1300～1600 ℃, temperature of reaction is high, granule-morphology and the size of sample are inhomogeneous, and color sample is not easy control, easy ash and then the reduction luminous intensity of becoming.
Summary of the invention
In order to address the above problem, the invention provides a kind of luminescent material, there is following chemical general formula: La
1-xre
xaO
3; Wherein,
A is at least one in Al (aluminium), In (indium) or Ga (gallium);
Re is at least one in Tm (thulium), Tb (terbium), Eu (europium), Sm (samarium), Gd (gadolinium), Dy (dysprosium), Ce (cerium) or Pr (praseodymium);
The span of x is 0.001≤x≤0.3.
The present invention also provides the preparation method of above-mentioned luminescent material, and preparation flow is as follows:
According to chemical general formula La
1-xre
xaO
3in the stoichiometric ratio of each element, the source compound of the source compound of La, the source compound of Re and A is provided, grind to form mixed powder together with melting salt; Wherein, A is at least one in Al, In or Ga; Re is at least one in Tm, Tb, Eu, Sm, Gd, Dy, Ce or Pr; The span of x is 0.001≤x≤0.3;
Above-mentioned mixed powder is placed in and at 700～1300 ℃, carries out calcination processing 1～24h, the powder after cooling, washing calcining;
Powder drying after washing is placed at 500～950 ℃ and carries out secondary clacining 0.5～5h, and cooling, grinding, makes described luminescent material.
Compared with prior art, the present invention has the following advantages:
1, the present invention is by molten salt process, the La of preparation
1-xre
xaO
3luminescent material is white, and luminous intensity can surpass LaGaO prepared by solid phase method
3: Tm, reaches commercial ZnS:Ag, the luminous intensity of Cl;
2, the present invention, by molten-salt growth method, can reduce La greatly
1-xre
xaO
3the preparation temperature of luminescent material;
3, the present invention is simple to operate, pollution-free, and technique is simple, is easy to preparation, and equipment requirements is low, is beneficial to suitability for industrialized production, can be widely used in the preparation field of luminescent material.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of luminescent material of the present invention;
Fig. 2 is that the luminescent material of the embodiment of the present invention 1 preparation is the luminescent spectrum comparison diagram under the cathode-ray exciting under 3.0kV at acceleration voltage, and wherein, curve a is La prepared by this example molten-salt growth method
0.99tm
0.01al
0.95in
0.05o
3the luminescent spectrum of luminescent material; Curve b is commercial LaGaO
3: the luminescent spectrum of Tm luminescent material.Curve c is commercial powder ZnS:Ag, the luminescent spectrum of Cl luminescent material;
Fig. 3 is the luminescent material La of the embodiment of the present invention 2 preparations
0.99tm
0.01alO
3and La
0.99tm
0.01al
0.95in
0.05o
3at acceleration voltage, be the luminescent spectrum under the cathode-ray exciting under 5.0kV, be expressed as curve d and e.
Embodiment
The invention provides a kind of luminescent material, it is characterized in that, this luminescent material has following chemical general formula: La
1-xre
xaO
3; Wherein,
A is at least one in Al, In or Ga;
Re is at least one in Tm, Tb, Eu, Sm, Gd, Dy, Ce or Pr;
The span of x is 0.001≤x≤0.3.
Manufacture the method for above-mentioned luminescent material, as shown in Figure 1, preparation flow is as follows:
Step S1, according to chemical general formula La
1-xre
xaO
3in the stoichiometric ratio of each element, the source compound of the source compound of La, the source compound of Re and A is provided, grind to form mixed powder together with melting salt; Wherein, A is at least one in Al, In or Ga; Re is at least one in Tm, Tb, Eu, Sm, Gd, Dy, Ce or Pr; The span of x is 0.001≤x≤0.3;
Step S2, described mixed powder is placed in to calcining furnace, by the heat-up rate of 1～10 ℃/min, is warming up at 700～1300 ℃, carry out calcination processing 1～24h, the powder after cooling, washing calcining;
Step S3, the powder after washing is put into loft drier and at 100～200 ℃, carried out drying treatment, with being placed on, at 500～950 ℃, carry out secondary clacining 0.5～5h, cooling, grind, make described luminescent material.
In above-mentioned preparation method's step S1, according to La
1-xre
xaO
3molar weight be 1: 1～1: 15 with the ratio that melts the integral molar quantity of salt, accurately take the source compound of La, the source compound of the source compound of Re, A and the source compound that respectively melts salt, and the source compound lanthanum trioxide of La, the oxide compound that the source compound of Re is Re, as Re
2o
3(Re is Tm, Tb, Eu, Sm, Gd, Dy, Ce, Pr); The source compound of A is the oxide compound of A, as Al
2o
3, In
2o
3, Ga
2o
3in at least one; Melt salt and be LiCl-KCl (mol ratio is 5: 41) mixing salt, KCl-NaCl (mol ratio is 5: 50) mixing salt, LiNO
3-KNO3 (mol ratio is 4: 57) mixing salt, a kind of in LiF-NaF-KF (mol ratio is 16.: 11.: 42 or 4: 1: 41) mixing salt or KCl-KF (mol ratio is 53.3: 46.7) mixing salt.
In above-mentioned preparation method's step S2, need the powder after calcining be handled as follows, with the salt ion that melts in filtering powder as far as possible:
With the powder after hot-water soak, dissolving, washing calcining, subsequently washed powder transferred in beaker, boil 1～5h, filter, wash; Repeatedly carry out above washing operation.
In above-mentioned preparation method's step S3, secondary clacining is processed and is carried out under reducing atmosphere or air atmosphere, and required reducing atmosphere is: the 1) gas mixture of nitrogen and hydrogen, and its volume ratio is 95: 5 or 90: 10; 2) pure hydrogen; 3) carbon monoxide.
In conjunction with the advantage of molten-salt growth method, (fused salt is as a kind of ion melt that just can melting at lower temperature, and it not only can provide starting material to react required high-temperature liquid state environment in the present invention; Meanwhile, also will have influence on build environment and the speed of material, play the effect of controlling pattern and particle diameter; There is use temperature scope widely) prepare that a kind of color is white, aluminium (gallium, the indium) salt luminescent material of good luminous performance.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1:
According to La
0.99tm
0.01al
0.95in
0.05o
3with the ratio of melting salt KCl-KF (mol ratio, 53.3: 46.7) integral molar quantity be 1: 3, accurately take 3.2255g La
2o
3, 0.0386g Tm
2o
3, 0.9686gAl
2o
3, 0.1388g In
2o
3, 2.3841g KCl and 2.6365g KF2H
2o is placed in agate mortar, grinds 30min; Put it in corundum crucible, be warmed up to 900 ℃, insulation 5h, 3 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 2h, filtration washing; Repeatedly carry out above operation, with AgNO3 solution check Cl, whether wash completely, until unnecessary Cl ion be washed complete after; Completely dry in the baking oven of 120 ℃; At 850 ℃, in air atmosphere, secondary clacining 3h obtains required luminescent material La again
0.99tm
0.01al
0.95in
0.05o
3.
Fig. 2 is that the luminescent material of the embodiment of the present invention 1 preparation is the luminescent spectrum comparison diagram under the cathode-ray exciting under 3.0kV at acceleration voltage, and wherein, curve a is La prepared by this example molten-salt growth method
0.99tm
0.01al
0.95in
0.05o
3the luminescent spectrum of luminescent material; Curve b is commercial LaGaO
3: the luminescent spectrum of Tm luminescent material; Curve c is commercial powder ZnS:Ag, the luminescent spectrum of Cl luminescent material.
As seen from Figure 2, the La preparing by molten salt process
0.99tm
0.01al
0.95in
0.05o
3the luminous intensity of luminescent material can surpass LaGaO
3: the luminous intensity of Tm, reaches commercial ZnS:Ag, the luminous intensity of Cl.
Embodiment 2:
According to La
0.99tm
0.01alO
3with the ratio of melting salt KCl-KF (mol ratio, 53.3: 46.7) integral molar quantity be 1: 5, accurately take 3.2255g La
2o
3, 0.0386g Tm
2o
3, 1.0196g Al
2o
3, 3.9735g KCl and 4.3943g KF2H
2o is placed in agate mortar, grinds 5min; Put it in corundum crucible, be warmed up to 1100 ℃, insulation 5h, 5 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 3h, filtration washing; Repeatedly carry out above operation, use AgNO
3whether solution check Cl washs completely, until unnecessary Cl ion be washed complete after; Completely dry in the baking oven of 150 ℃; At 800 ℃, in air atmosphere, secondary clacining 3h obtains required luminescent material La again
0.99tm
0.01alO
3.Same condition is prepared luminescent material La
0.99tm
0.01al
0.95in
0.05o
3.
Fig. 3 is the luminescent material La of the embodiment of the present invention 2 preparations
0.99tm
0.01alO
3and La
0.99tm
0.01al
0.95in
0.05o
3at acceleration voltage, be the luminescent spectrum under the cathode-ray exciting under 5.0kV, be expressed as curve d and e.
Embodiment 3:
According to La
0.999eu
0.001gaO
3with the ratio of melting salt KCl-KF (mol ratio, 53.3: 46.7) integral molar quantity be 1: 1, accurately take 1.6274g La
2o
3, 0.0018g Eu
2o
3, 0.9372g Ga
2o
3, 0.3974g KCl and 0.4395g KF2H
2o is placed in agate mortar, grinds 60min; Put it in corundum crucible, be warmed up to 1300 ℃, insulation 1h, 10 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 1h, filtration washing; Repeatedly carry out above operation, use AgNO
3whether solution check Cl washs completely, until unnecessary Cl ion be washed complete after; Completely dry in the baking oven of 100 ℃; At 500 ℃, in air atmosphere, secondary clacining 0.5h obtains required luminescent material La again
0.999eu
0.001gaO
3.
Embodiment 4:
According to La
0.70gd
0.05tb
0.25alO
3with the ratio of melting salt KCl-KF (mol ratio, 53.3: 46.7) integral molar quantity be 1: 15, accurately take 1.1403g La
2o
3, 0.0906g Gd
2o
3, 0.4673gTb
4o
7, 0.5098g Al
2o
3, 5.9602g KCl and 6.5915g KF2H
2o is placed in agate mortar, grinds 30min; Put it in corundum crucible, be warmed up to 1000 ℃, insulation 24h, 1 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 5h, filtration washing; Repeatedly carry out above operation, use AgNO
3whether solution check Cl washs completely, until unnecessary Cl ion be washed complete after; Completely dry in the baking oven of 200 ℃; At 950 ℃, in reducing atmosphere, (gas mixture of nitrogen and hydrogen, its volume ratio is 95: 5) secondary clacining 5h obtains required luminescent material La again
0.70gd
0.05tb
0.25alO
3.
Embodiment 5:
According to La
0.95ce
0.05alO
3with the ratio of melting salt LiCl-KCl (mol ratio, 59: 41) integral molar quantity be 1: 6, accurately take 1.5476g La
2o
3, 0.0861g CeO
2, 0.5098gAl
2o
3, 1.5007gLiCl and 1.8340g KCl are placed in agate mortar, grind 40min; Put it in corundum crucible, be warmed up to 700 ℃, insulation 12h, 1 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 4h, filtration washing; Repeatedly carry out above operation, use AgNO
3whether solution check Cl washs completely, until unnecessary Cl ion be washed complete after; Completely dry in the baking oven of 200 ℃; At 500 ℃, in reducing atmosphere, (gas mixture of nitrogen and hydrogen, its volume ratio is 90: 10) secondary clacining 5h obtains required luminescent material La again
0.95ce
0.05alO
3.
Embodiment 6:
According to La
0.85pr
0.05eu
0.10alO
3with the ratio of melting salt KCl-NaCl (mol ratio, 50: 50) integral molar quantity be 1: 8, accurately take 1.3847g La
2o
3, 0.0851g Pr
6o
11, 0.1760g Eu
2o
3, 0.5098g Al
2o
3, 2.9820g KCl and 2.3377g NaCl are placed in agate mortar, grind 20min; Put it in corundum crucible, be warmed up to 1200 ℃, insulation 4h, 3 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 4h, filtration washing; Repeatedly carry out above operation, use AgNO
3whether solution check Cl washs completely, until unnecessary Cl ion be washed complete after; Completely dry in the baking oven of 180 ℃; At 850 ℃, in reducing atmosphere, (carbon monoxide) secondary clacining 2h obtains required luminescent material La again
0.85pr
0.05eu
0.10alO
3.
Embodiment 7:
According to La
0.95dy
0.05ga
0.98in
0.02o
3with melt salt LiNO
3-KNO
3the ratio of (mol ratio, 43: 57) integral molar quantity is 1: 5, accurately takes 1.5476g La
2o
3, 0.0872g Sm
2o
3, 0.91858gGa
2o
3, 0.0278g In
2o
3, 1.4824g LiNO
3with 2.8814g KNO
3be placed in agate mortar, grind 30min; Put it in corundum crucible, be warmed up to 900 ℃, insulation 8h, 2 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 4h, filtration washing; Repeatedly carry out above operation, washing completely; Completely dry in the baking oven of 150 ℃; At 800 ℃, in air atmosphere, secondary clacining 5h obtains required luminescent material La again
0.95sm
0.05ga
0.98in
0.02o
3.
Embodiment 8:
According to La
0.90dy
0.10alO
3with the ratio of melting salt LiF-NaF-KF (mol ratio, 16.5: 11.5: 42) integral molar quantity be 1: 11, accurately take 1.4661g La
2o
3, 0.1865g Dy
2o
3, 0.5098gAl
2o
3, 0.4708g LiF, 0.5312g NaF and 4.3472g KF2H
2o is placed in agate mortar, grinds 30min; Put it in corundum crucible, be warmed up to 1000 ℃, insulation 10h, 3 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 5h, filtration washing; Repeatedly carry out above operation, washing completely; Completely dry in the baking oven of 200 ℃; At 800 ℃, in air atmosphere, secondary clacining 5h obtains required luminescent material La again
0.70gd
0.05tb
0.25alO
3.
Embodiment 9:
According to La
0.85gd
0.02ce
0.05tb
0.08alO
3with the ratio of melting salt LiF-NaF-KF (mol ratio, 47: 12: 41) integral molar quantity be 1: 11, accurately take 1.3847g La
2o
3, 0.0362g Gd
2o
3, 0.0861gCeO
2, 0.1495g Tb
4o
7, 0.5098g Al
2o
3, 0.4708g LiF, 0.5312g NaF and 4.3472gKF2H
2o is placed in agate mortar, grinds 30min; Put it in corundum crucible, be warmed up to 1000 ℃, insulation 8h, 4 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 5h, filtration washing; Repeatedly carry out above operation, completely dry in the baking oven of 200 ℃ after washing completely; At 850 ℃, in reducing atmosphere, (H2) secondary clacining 5h obtains required luminescent material La again
0.85gd
0.02ce
0.05tb
0.08alO
3.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (2)
1. a luminescent material, is characterized in that, this luminescent material has following chemical general formula:
La
0.99Tm
0.01Al
0.95In
0.05O
3。
2. a preparation method for luminescent material, comprises the steps:
According to La
0.99tm
0.01al
0.95in
0.05o
3with the ratio of melting salt KCl-KF integral molar quantity be 1:3, described in melt KCL in salt KCl-KF and the mol ratio of KF is 53.3:46.7, accurately take 3.2255gLa
2o
3, 0.0386g Tm
2o
3, 0.9686g Al
2o
3, 0.1388g In
2o
3, 2.3841g KCl and 2.6365gKF2H
2o is placed in agate mortar, grinds 30min; Put it in corundum crucible, be warmed up to 900 ℃, insulation 5h, 3 ℃/min of temperature speed; Cool to room temperature, with after hot-water soak, dissolving, washing, transfers in beaker, boils 2h, filtration washing; Repeatedly carry out above operation, use AgNO
3whether solution check Cl washs completely, until unnecessary Cl ion be washed complete after; Completely dry in the baking oven of 120 ℃; At 850 ℃, in air atmosphere, secondary clacining 3h obtains luminescent material La again
0.99tm
0.01al
0.95in
0.05o
3.
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| CN106753379A (en) * | 2016-11-10 | 2017-05-31 | 哈尔滨理工大学 | A kind of preparation method of terbium ion doping fluoride solid luminescent material |
| CN116064036A (en) * | 2023-01-16 | 2023-05-05 | 海南大学 | Up-conversion luminescent material and preparation method thereof |
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