CN108003874B - Single-matrix negative thermal expansion white fluorescent powder and sintering synthesis method thereof - Google Patents
Single-matrix negative thermal expansion white fluorescent powder and sintering synthesis method thereof Download PDFInfo
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Abstract
The present invention belongs to inorganic non-metal materialThe field specifically discloses single-matrix negative thermal expansion white fluorescent powder, and the molecular formula is as follows: zr0.3Sc1.7Mo2.7V0.3O12(ii) a Two sintering methods are disclosed: solid phase methods and sol gel methods. The invention provides single-matrix negative thermal expansion white light fluorescent powder Zr0.3Sc1.7Mo2.7V0.3O12The material has stable negative thermal expansion property within the range of room temperature to 400 ℃; and emits white light fluorescence under ultraviolet excitation, wherein the white light color coordinate (0.3420, 0.3404) excited at 370nm is close to the standard white light color coordinate (0.330 ), indicating Zr0.3Sc1.7Mo2.7V0.3O12Is a good single-matrix white light fluorescent powder under the excitation of near ultraviolet light and has engineering application value.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials, and particularly relates to single-matrix negative thermal expansion white fluorescent powder and a sintering synthesis method thereof.
Background
Most materials in nature have the characteristics of expansion with heat and contraction with cold, but the abnormal phenomenon of thermal contraction and cold expansion, namely the negative thermal expansion phenomenon, also exists in nature. Both thermal expansion and contraction of the material and mismatch in expansion coefficients between the materials can affect device performance and even permanent failure. With regard to negative thermal expansion materials, the problem to be solved urgently is to actively search a novel negative thermal expansion material and explore an effective preparation method for unknown materials; the method implements effective performance regulation on the existing negative thermal expansion material, such as properly reducing the temperature phase change point, realizing zero expansion and controllable expansion coefficient and the like. But the negative thermal expansion material with excellent performance and engineering application value is few. For example, the commonly studied negative thermal expansion oxide materials include ZrW2O8, a common AM2O 8The material is similar to the prior art, but the application problem of the material is that ZrW2O8 is at room temperatureThe lower part is a metastable phase material, which has phase change at about 150 ℃ and is easy to decompose when being compounded with other materials. Another common class of negative expansion materials A2M3O12(A is trivalent cation, can be transition metal or rare earth element, A can also be substituted by a quadrivalent cation and a divalent cation; M is W or Mo) series has to be converted from monoclinic phase to orthorhombic phase to show negative thermal expansion performance, and the series of materials have the problems of phase change, water absorption or poor mechanical property and the like.
The white light LED is called as a new generation of lighting source and has wide application prospect. The single-substrate white light fluorescent powder for the ultraviolet-near ultraviolet excited white light LED has unique advantages, and becomes a research hotspot of the current light conversion material for the white light LED. Therefore, the research and development of the single-matrix white light fluorescent powder with stable negative expansion performance has important application value.
Disclosure of Invention
In view of the above-mentioned drawbacks and disadvantages of the prior art, an object of the present invention is to provide a single-matrix negative thermal expansion white phosphor and a sintering synthesis method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a single-matrix negative thermal expansion white light fluorescent powder has a molecular formula as follows: zr0.3Sc1.7Mo2.7V0.3O12。
The invention relates to single-matrix negative thermal expansion white light fluorescent powder Zr0.3Sc1.7Mo2.7V0.3O12Two sintering synthesis methods are provided, which respectively adopt a solid phase method and a sol-gel method, and specifically comprise the following steps:
the solid phase method comprises the following steps: in terms of mole ratio, based on zirconium dioxide ZrO2Sc of scandia trioxide2O3Molybdenum trioxide (MoO)3Vanadium pentoxide V2O5Weighing raw materials in a ratio of = 0.3: 0.85: 2.7: 0.15, grinding and mixing uniformly, sintering and synthesizing the uniformly mixed raw materials directly or after tabletting, and naturally cooling to obtain the target product Zr0.3Sc1.7Mo2.7V0.3O12(ii) a Wherein, the sintering conditions are as follows: the temperature is 700-800 ℃, the time is 3-4 h, the pressure is normal pressure, and the atmosphere is air.
Preferably, in order to fully grind, the raw materials are preferably weighed, and then the grinding is started after the absolute ethyl alcohol is added.
② the sol-gel method, comprising the following steps:
(1) in terms of molar ratio, as ZrN2O7∶Sc(NO3)3∶(NH4)6Mo7O24·4H2O∶NH4VO3Weighing raw materials according to the ratio of = 0.3: 1.7: (2.7/7): 0.3, and mixing (NH)4)6Mo7O24·4H2O and NH4VO3Dispersing in water to form solution A, and adding ZrN2O7And Sc (NO)3)3Dispersing in water to form a solution B;
(2) adding the solution A into the solution B while stirring, stirring at constant temperature of 80 + -10 deg.C, and adding citric acid C6H8O7As a complexing agent, adjusting the pH of the system to 11-12 by using ammonia water, and continuously stirring until sol is obtained; citric acid C in terms of molar ratio6H8O7Is ZrN2O7、Sc(NO3)3、(NH4)6Mo7O24·4H2O and NH4VO30.01-0.03 times of the total molar weight;
(3) drying the obtained sol at 100-110 ℃ to form gel;
(4) sintering the obtained gel for 3-4 h at the temperature of 700-800 ℃ under normal pressure and air atmosphere, and naturally cooling to room temperature to obtain the target product Zr0.3Sc1.7Mo2.7V0.3O12。
The invention has no strict requirement on the dosage of water, so long as the raw materials can be dispersed, but when the dosage of water is large, the sol can be obtained after long stirring time. Therefore, in the step (1), the amount of water used in the solution A is preferably (NH)4)6Mo7O24·4H2O and NH4VO320-30 times of the total mass, and the amount of water in the solution B is (NH)4)6Mo7O24·4H2O and NH4VO320-30 times of the total mass.
The product can be repeatedly sintered, other tests are convenient for obtaining blocks, the taking is convenient and better, in the step (4), after the temperature is naturally reduced to the room temperature, the obtained product is ground and pressed into sheets, the obtained product is sintered for 3-4 hours at the temperature of 700-800 ℃ under the normal pressure and the air atmosphere, and the temperature is naturally reduced to the room temperature, so that the target product is obtained.
Has the advantages that:
1. the invention provides single-matrix negative thermal expansion white light fluorescent powder Zr0.3Sc1.7Mo2.7V0.3O12The material has stable negative thermal expansion property within the range of room temperature to 400 ℃; and emits white light fluorescence under ultraviolet excitation, wherein the white light color coordinate (0.3420, 0.3404) excited at 370nm is close to the standard white light color coordinate (0.330 ), indicating Zr0.3Sc1.7Mo2.7V0.3O12The fluorescent powder is a good single-matrix white-light fluorescent powder under the excitation of near ultraviolet light, and has engineering application value;
2. the solid phase method and the sol-gel method provided by the invention are used for sintering synthesis, the raw materials are fully reacted, the reaction process is simple, and the prepared product has uniform granularity, smooth surface and very dense crystallization.
Drawings
FIG. 1: XRD pattern of the product of example 1 (solid phase method 770 ℃ sintering for 3 h);
FIG. 2: XRD pattern of the product of example 2 (solid phase method 770 ℃ sintering for 4 h);
FIG. 3: XRD pattern of the product of comparative example 1 (solid phase method 770 ℃ sintering for 4 h);
FIG. 4: XRD pattern of the product of example 3 (sol-gel method);
FIG. 5: XRD spectrum (sol-gel method) of the product of comparative example 2;
FIG. 6: XRD spectrum (sol-gel method) of the product of comparative example 3;
FIG. 7: XRD spectrum (sol-gel method) of the product of comparative example 4;
FIG. 8: the change curve of the relative length of the product in the example 2 along with the testing temperature (-120-400 ℃);
FIG. 9: the change curve of the relative length of the product of example 3 along with the test temperature (RT-400 ℃);
FIG. 10: the fluorescence spectrum (left graph) and the color coordinate graph (right graph) of the product of the example 2 under the excitation of ultraviolet light with the wavelength of 370 nm;
FIG. 11: the fluorescence spectrum (left graph) and the color coordinate graph (right graph) of the product of the example 3 under the excitation of ultraviolet light with the wavelength of 370 nm;
FIG. 12: scanning electron micrographs of the product of example 2 wherein (a) (b) are 2000 and 12000 times magnification, respectively;
FIG. 13: scanning electron micrographs of the product of example 3 wherein (a) and (b) were at 2000 and 12000 magnifications, respectively.
Detailed Description
In order to make the invention clearer and clearer, the invention is further described in detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Sintering by solid phase method
Example 1
ZrO to be analytically pure2、Sc2O3、MoO3、V2O5Weighing and taking materials according to the mol ratio of 0.3: 0.85: 2.7: 0.15, uniformly mixing in an agate mortar, adding absolute ethyl alcohol, and grinding for 2 hours; pressing the sample into a cylindrical sample with the diameter of 10 mm and the height of about 6 mm under the uniaxial pressure of 300 MPa; setting a low-temperature tube furnace at 770 ℃, putting the corundum crucible with the sample into the tube furnace at the sintering temperature, sintering for 3 hours in normal-pressure air, and naturally cooling to room temperature in the air to obtain the product. The corresponding XRD pattern phase analysis of the product is shown in figure 1, and the XRD result of figure 1 shows that pure-phase Zr is formed0.3Sc1.7Mo2.7V0.3O12And after structure refinement, determining that the prepared material is an orthorhombic structure with a space group of Pbcn (60).
Example 2
The difference from example 1 is that: the sintering time is 4 h; the other steps are the same as in example 1.
The corresponding XRD pattern phase analysis of the product is shown in figure 2, and the XRD result of figure 2 shows that pure-phase Zr is formed0.3Sc1.7Mo2.7V0.3O12And after structure refinement, determining that the prepared material is an orthorhombic structure with a space group of Pbcn (60).
In the course of the research and development of the present inventors, the inventors found that the molar ratio between the raw materials has a very important influence on the phase composition of the product when sintering by the solid phase method, and the examples are given by way of example, but not by way of exhaustive list.
Comparative example 1
The difference from the embodiment 1 is that: MoO3And V2O5Nine percent excess of molar ratio; the other steps are the same as in example 1.
The corresponding XRD pattern phase analysis of the product is shown in figure 3, and the XRD result of figure 3 shows that the main body structure is Zr0.3Sc1.7Mo2.7V0.3O12But contains a small amount of ZrMo2O8。
Sol gel process
Example 3
(1) In terms of molar ratio, as ZrN2O7∶Sc(NO3)3∶(NH4)6Mo7O24·4H2O∶NH4VO3Weighing raw materials according to the ratio of = 0.3: 1.7: (2.7/7): 0.3, and mixing (NH)4)6Mo7O24·4H2O and NH4VO3Placing in A beaker, ZrN2O7And Sc (NO)3)3Placing the mixture into a beaker B, adding deionized water with the mass being 25 times of the mass of the raw materials in each beaker into A, B beakers respectively, and stirring for 3 hours by using a magnetic stirrer;
(2) slowly adding the uniformly stirred solution in the beaker A into the solution in the beaker B while stirring, stirring at the constant temperature of 80 ℃ for 3 hours, and adding ZrN with the molar weight2O7、Sc(NO3)3、(NH4)6Mo7O24·4H2O and NH4VO3Citric acid C with a molar weight of 0.02 times of the total6H8O7As complexing agent, use is made of concentrated NH3·H2Adjusting the pH value of the system to 11 by O (the mass concentration is 30 percent), and continuously stirring for 24 hours at 80 ℃ to obtain transparent colloid (namely sol);
(3) drying the obtained transparent colloid in an air drying oven at 100 ℃ for 12 h, wherein the original sol is converted into gel;
(4) putting the obtained gel into a muffle furnace, sintering for 4 hours at 770 ℃ under normal pressure and air atmosphere, and naturally cooling to room temperature; grinding the obtained product, tabletting under the pressure of 5MPa, and sintering at 770 ℃ for 4h under normal pressure and air atmosphere to obtain the product.
The XRD pattern corresponding to the product is shown in figure 4, and no raw material peak and possible intermediate product peak appear in the XRD pattern given in figure 4, which indicates that the prepared sample is Zr with a pure cross-phase structure0.3Sc1.7Mo2.7V0.3O12。
In the research and development process of the inventor, the inventor finds that the material adding sequence, the system pH and the drying temperature of the gel have very important influence on the phase composition of the product when sintering by the sol-gel method, and the three comparative examples are listed for illustration but are not exhaustive.
Comparative example 2
The difference from example 3 is that: will be (NH)4)6Mo7O24·4H2O and NH4VO3Respectively dispersing the mixture in water, and then respectively adding the mixture into a beaker B, wherein the specific process comprises the following steps:
(1) in terms of molar ratio, as ZrN2O7∶Sc(NO3)3∶(NH4)6Mo7O24·4H2O∶NH4VO3Weighing raw materials according to the ratio of = 0.3: 1.7: (2.7/7): 0.3, and mixing (NH)4)6Mo7O24·4H2O in A1 beaker, NH4VO3Placing in A2 beaker, ZrN2O7And Sc (NO)3)3Placing the mixture into a beaker B, adding deionized water with the mass being 25 times of the total mass of the raw materials in the beaker A1, the beaker A2 and the beaker B respectively, and stirring the mixture for 3 hours by using a magnetic stirrer;
(2) slowly adding the uniformly stirred solution of the A1 beaker into the solution of the B beaker while stirring, then slowly adding the uniformly stirred solution of the A2 beaker into the solution of the B beaker while stirring, stirring at the constant temperature of 80 ℃ for 3 hours, and then adding the solution with the molar weight of ZrN2O7、Sc(NO3)3、(NH4)6Mo7O24·4H2O and NH4VO3Citric acid C with a molar weight of 0.02 times of the total6H8O7As complexing agent, use is made of concentrated NH3·H2Adjusting the pH value of the system to 11 by O (the mass concentration is 30 percent), and continuously stirring for 24 hours at 80 ℃ to obtain transparent colloid (namely sol);
steps (3) to (4) were the same as in example 3.
The XRD pattern corresponding to the product is shown in figure 5, and Zr with main phase of orthorhombic structure in the XRD pattern shown in figure 50.3Sc1.7Mo2.7V0.3O12And more intermediate product peaks ZrMo2O8。
Comparative example 3
The difference from example 3 is that: in the step (2), adjusting the pH value of the system to 7; the other steps are the same as in example 3.
The XRD pattern corresponding to the product is shown in figure 6, the XRD pattern shown in figure 6 has no raw material peak, and the main phase is Zr with an orthogonal phase structure0.3Sc1.7Mo2.7V0.3O12And having an intermediate peak ZrMo2O8。
Comparative example 4
The difference from example 3 is that: in the step (3), the drying temperature of the gel is 120 ℃; the other steps are the same as in example 3.
The XRD pattern corresponding to the product is shown in figure 7, and no raw material peak appears in the XRD pattern shown in figure 7, mainlyZr of quadrature phase structure0.3Sc1.7Mo2.7V0.3O12And having an intermediate peak ZrMo2O8。
Performance detection
FIGS. 8 and 9 are Zr prepared in example 2 and example 3, respectively0.3Sc1.7Mo2.7V0.3O12The relative length as a function of the test temperature shows that Zr prepared in example 2 and example 30.3Sc1.7Mo2.7V0.3O12The relative length decreased with increasing temperature, indicating that the material prepared was a negative thermal expansion material. The linear expansion coefficient is calculated to be about-2.68 x 10-6 ℃-1(25-400 ℃), which shows that the material has stable negative thermal expansion property in the range of room temperature-400 ℃.
FIG. 10 is Zr prepared in example 20.3Sc1.7Mo2.7V0.3O12A fluorescence spectrogram (left picture) and a color coordinate graph (right picture) obtained by excitation of ultraviolet light with the wavelength of 370nm on a fluorescence spectrometer; FIG. 11 is Zr prepared in example 30.3Sc1.7Mo2.7V0.3O12The obtained fluorescence spectrum (left graph) and the color coordinate graph (right graph) are excited by ultraviolet light with the wavelength of 370nm on a fluorescence spectrometer. As shown in FIGS. 10 and 11, Zr prepared in examples 2 and 30.3Sc1.7Mo2.7V0.3O12The Zr prepared in example 2 emits white light fluorescence with color coordinates of (0.3420, 0.3404) and (0.3183, 0.4538) broad spectrum under the excitation of ultraviolet light with the wavelength of 370nm on a fluorescence spectrometer0.3Sc1.7Mo2.7V0.3O12The white light color coordinate (0.3420, 0.3404) excited at 370nm is close to the standard white light color coordinate (0.330 ), and the LED white light fluorescent powder has application value.
Electron scanning electron microscope testing
FIGS. 12 and 13 show Zr prepared in examples 2 and 3, respectively0.3Sc1.7Mo2.7V0.3O12Watch (A)The surface scanning electron micrographs, wherein the magnifications (a) and (b) are 2000 and 12000 respectively, as can be seen from fig. 12 and 13, the phosphor prepared by the solid phase sintering method has the advantages of uniform particle size distribution, smooth surface, very dense crystallization and finer phosphor prepared by the sol-gel method.
Claims (6)
1. A single-matrix negative thermal expansion white light fluorescent powder is characterized in that the molecular formula is as follows: zr0.3Sc1.7Mo2.7V0.3O12。
2. A method for synthesizing the single-matrix negative thermal expansion white phosphor of claim 1, wherein: the method is a solid phase method and comprises the following steps: in terms of mole ratio, based on zirconium dioxide ZrO2Sc of scandia trioxide2O3Molybdenum trioxide (MoO)3Vanadium pentoxide V2O5Weighing raw materials in a ratio of = 0.3: 0.85: 2.7: 0.15, grinding and mixing uniformly, sintering and synthesizing the uniformly mixed raw materials directly or after tabletting, and naturally cooling to obtain the target product Zr0.3Sc1.7Mo2.7V0.3O12(ii) a Wherein, the sintering conditions are as follows: the temperature is 700-800 ℃, the time is 3-4 h, the pressure is normal pressure, and the atmosphere is air.
3. The sintering synthesis method of single-matrix negative thermal expansion white light fluorescent powder as claimed in claim 2, characterized in that: after the raw materials are weighed, firstly, absolute ethyl alcohol is added, and then, grinding is started.
4. A method for synthesizing the single-matrix negative thermal expansion white phosphor of claim 1, wherein: the method is a sol-gel method and comprises the following steps:
(1) in terms of molar ratio, as ZrN2O7∶Sc(NO3)3∶(NH4)6Mo7O24·4H2O∶NH4VO3Weighing raw materials according to the ratio of = 0.3: 1.7: (2.7/7): 0.3, and mixing (NH)4)6Mo7O24·4H2O and NH4VO3Dispersing in water to form solution A, and adding ZrN2O7And Sc (NO)3)3Dispersing in water to form a solution B;
(2) adding the solution A into the solution B while stirring, stirring at constant temperature of 80 + -10 deg.C, and adding citric acid C6H8O7As a complexing agent, adjusting the pH of the system to 11-12 by using ammonia water, and continuously stirring until sol is obtained; citric acid C in terms of molar ratio6H8O7Is ZrN2O7、Sc(NO3)3、(NH4)6Mo7O24·4H2O and NH4VO30.01-0.03 times of the total molar weight;
(3) drying the obtained sol at 100-110 ℃ to form gel;
(4) sintering the obtained gel for 3-4 h at the temperature of 700-800 ℃ under normal pressure and air atmosphere, and naturally cooling to room temperature to obtain the target product Zr0.3Sc1.7Mo2.7V0.3O12。
5. The method for synthesizing single-matrix negative thermal expansion white light fluorescent powder of claim 4, wherein: in the step (1), the amount of water in the solution A is (NH) by mass ratio4)6Mo7O24·4H2O and NH4VO320-30 times of the total mass, and the amount of water in the solution B is (NH)4)6Mo7O24·4H2O and NH4VO320-30 times of the total mass.
6. The method for synthesizing single-matrix negative thermal expansion white light fluorescent powder of claim 4, wherein: and (4) naturally cooling to room temperature, grinding and tabletting the obtained product, sintering for 3-4 hours at the temperature of 700-800 ℃ under normal pressure and air atmosphere, and naturally cooling to room temperature to obtain the target product.
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| CN102115597A (en) * | 2009-12-31 | 2011-07-06 | 三星电机株式会社 | Composite material for substrate containing inorganic filling material and liquid crystal thermosetting oligomer with negative thermal expansion coefficient |
| CN104291822A (en) * | 2014-09-29 | 2015-01-21 | 郑州大学 | Novel negative thermal expansion material ZrScMo2VO12 and solid phase sintering synthesis method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102115597A (en) * | 2009-12-31 | 2011-07-06 | 三星电机株式会社 | Composite material for substrate containing inorganic filling material and liquid crystal thermosetting oligomer with negative thermal expansion coefficient |
| CN104291822A (en) * | 2014-09-29 | 2015-01-21 | 郑州大学 | Novel negative thermal expansion material ZrScMo2VO12 and solid phase sintering synthesis method thereof |
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| Title |
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| Negative thermal expansion and broad band photoluminescence in a novel material of ZrScMo2VO12;Xianghong Ge et al.;《Scientific Reports》;20160421;第6卷;第1-8页 * |
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