CN110669519A - Samarium-zirconium co-doped tin oxide fluorescent powder and soft chemical preparation method thereof - Google Patents
Samarium-zirconium co-doped tin oxide fluorescent powder and soft chemical preparation method thereof Download PDFInfo
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Abstract
The invention discloses samarium-zirconium co-doped tin oxide fluorescent powder and a soft chemical preparation method thereof, wherein the fluorescent powder has the following chemical general formula: SnO2：xSm3+,yZr4+Wherein x is 0.01 to 0.5, and y is 0 to 2. The soft chemical preparation method comprises the following steps: (1) weighing raw material SnCl4·2H2O、Sm2O3、ZrO(NO3)2·xH2O; (2) dissolving the raw materials in water or acid to prepare a solution; (3) mixing and stirring the mixture until the pH value is alkaline; fully stirring, standing and cleaning; (4) drying, grinding, adding a fluxing agent, sintering and grinding to obtain the samarium-zirconium codoped tin oxide fluorescent powder. The tin oxide fluorescent powder prepared by adopting a soft chemical method has the advantages of uniform phase components, good particle dispersibility, easily controllable particle size and morphology, uniform particle size, good luminous performance, simple process and lower calcination temperature.
Description
Technical Field
The invention relates to the field of fluorescent materials, in particular to samarium-zirconium co-doped tin oxide fluorescent powder and a soft chemical preparation method thereof.
Background
In order to prepare a high-efficiency phosphor, attention has been paid to exploring crystals of superior structure, wherein a novel phosphor is developed by doping rare earth metals or/and other chemical elements in different crystals. Tin dioxide is a wide bandgap semiconductor (3.6 eV), and has the chemical formula SnO2Tin dioxide is also an n-type semiconductor, having a rutile crystal structure. The elements constituting tin oxide are 51 (Sn) th and the first most abundant element (O) in the earth's crust. Tin is a malleable silver metallic element and is a cheap and safe material. The materials are widely used in commercial, industrial and biological applications, including transparent conductive oxides, oxidation catalysts, solid state gas sensors (piezoresistors), as well as glass coatings, ceramic glazes and polishing powders.
Generally, the existing method for synthesizing tin oxide phosphor mainly adopts a solid phase method, but since the solid phase method is difficult to synthesize a product with a uniform phase component, the luminous effect and intensity thereof are seriously affected.
The tin oxide fluorescent powder prepared by adopting a soft chemical method has the advantages of uniform phase components, good particle dispersibility, easily controllable particle size and morphology, uniform particle size, good luminous performance, simple process and lower calcination temperature (the trend is promising, the synthesis and property research of rare earth doped semiconductor nanocrystals and panchromatic fluorescent powder [ D ] Shantou university, 2010 ].
In addition, the samarium-zirconium co-doped tin oxide fluorescent powder can effectively enhance the luminous intensity of single samarium-doped tin oxide fluorescent powder, and is favorable for improving the energy utilization efficiency.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide samarium-zirconium co-doped tin oxide fluorescent powder and a soft chemical preparation method thereof.
The purpose of the invention is realized by one of the following technical schemes.
The invention provides samarium-zirconium co-doped tin oxide fluorescent powder which has the following chemical general formulaFormula (II): SnO2：xSm3+,yZr4+Wherein x is 0.01 to 0.5, and y is 0 to 2.
The invention also provides a method for preparing the samarium-zirconium co-doped tin oxide fluorescent powder, which comprises the following steps:
(1) according to the formula SnO2：xSm3+,yZr4+SnCl is weighed according to the stoichiometric ratio of each element4·2H2O、Sm2O3、ZrO(NO3)2·xH2O, wherein x is 0.01-0.5, and y is 0-2;
(2) SnCl4·2H2Dissolving O in water to prepare a solution 1; mixing Sm2O3Dissolving in an acid solution 1 to prepare a solution 2; ZrO (NO)3)2·xH2Dissolving O in water, and adding an acid solution 2 to prepare a solution 3;
(3) mixing and stirring the solution 1, the solution 2 and the solution 3 to obtain a mixed solution, and adding an alkaline solution to adjust the pH value of the mixed solution to be alkaline; fully stirring, standing to obtain a precipitate, and cleaning the precipitate to be neutral;
(4) drying the cleaned precipitate, grinding the dried precipitate into a precursor, and adding a fluxing agent to obtain a mixture; and sintering and grinding the mixture in a tubular furnace protected by atmosphere to obtain the samarium-zirconium co-doped tin oxide fluorescent powder.
Preferably, the acid solution 1 or the acid solution 2 in step (2) comprises nitric acid or hydrochloric acid; the pH value of the acid solution 1 is 1-6; the pH of the acid solution 2 is 1-6.
Preferably, the alkaline solution in the step (3) comprises ammonia water or sodium hydroxide solution, and the pH value of the mixed solution is 7-14 after the alkaline solution is added for adjustment.
Preferably, the stirring speed in the step (3) is 100-2000 r/min; the stirring time is 1-5 hours.
Preferably, the standing time in the step (4) is 1-24 hours, and the washing liquid used for washing the precipitate is distilled water and absolute ethyl alcohol.
Preferably, the drying temperature in the step (4) is 60-120 ℃.
Preferably, the sintering temperature of the mixture in the step (4) in a tube furnace is 600-1400 ℃; the sintering time is 0.5-12 hours.
Preferably, the cosolvent in the step (4) comprises more than one of boric acid, sodium carbonate or fluorite; the content of the cosolvent in the mixture is 0.001-20 wt%.
Preferably, the atmosphere in step (4) comprises air or oxygen.
Compared with the prior art, the invention has the following technical effects and advantages:
(1) the samarium-zirconium co-doped tin oxide fluorescent powder provided by the invention has strong luminous intensity and is not easy to absorb water;
(2) in the photoluminescence spectrum of the samarium-zirconium co-doped tin oxide fluorescent powder provided by the invention, the fluorescent powder can be excited to emit orange light by ultraviolet light (262 nm) short-wave radiation;
(3) the synthesis process of the precursor in the preparation process of the preparation method is carried out in solution, and the wastewater generated in the washing and precipitating process is environment-friendly.
Drawings
FIG. 1 is an XRD diagram of a samarium zirconium co-doped tin oxide fluorescent powder material prepared in example 6;
FIG. 2 is a Photoluminescence (PL) diagram of samarium and zirconium co-doped tin oxide fluorescent powder materials prepared in examples 1 to 4;
FIG. 3 is a Photoluminescence (PL) diagram of samarium and zirconium co-doped tin oxide phosphor materials prepared in examples 4 to 7.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The embodiment provides samarium-zirconium co-doped tin oxide fluorescent powder, which has the following chemical general formula: SnO2：xSm3+,yZr4 +Wherein x is 0.02 and y is 0.
The embodiment also provides a preparation method of the fluorescent powder, which comprises the following steps:
commercial tin chloride (8.765 g; 0.025 mol) was dissolved in 50ml of deionized water, and Sm was added2O3(0.087 g; 0.00025 mol) and 1.500mL of nitric acid (1mol/L) were prepared as 5mL (0.100mol/L) standard solutions. The prepared solution was mixed according to the ratio and stirred for 1 hour. Then, the solution was titrated with aqueous ammonia to a pH of 9, and the solution was stirred to precipitate for 1 hour and then allowed to stand for 24 hours. Washing and precipitating by centrifugation, wherein the washing liquid is firstly deionized water and then absolute ethyl alcohol. After the washing and precipitation are finished, the precipitate is dried at the temperature of 60 ℃. And drying, grinding and precipitating to obtain a precursor, adding a fluxing agent to obtain a mixture, wherein the fluxing agent is boric acid, and the addition amount is 5wt%, so that the mixture is obtained. And the mixture was placed in a tube furnace and heated to 1400 deg.c (air atmosphere) for 4 hours. And grinding the sintered product to obtain the designed fluorescent powder, and detecting and verifying the optical performance.
Example 2
The embodiment provides samarium-zirconium co-doped tin oxide fluorescent powder, which has the following chemical general formula: SnO2：xSm3+,yZr4 +Wherein x is 0.02 and y is 0.1.
The embodiment also provides a preparation method of the fluorescent powder, which comprises the following steps:
commercial tin chloride (8.765 g; 0.025 mol) was dissolved in 50mL of deionized water, the purchased zirconyl nitrate (0.578 g; 0.575 mol) and concentrated nitric acid (0.346 mL; 0.005 mol) were dissolved to make up a 12.500mL (0.200mol/L) standard solution, and Sm was added2O3(0.087 g; 0.00025 mol) and 1.500mL of nitric acid (1mol/L) were prepared as 5mL (0.100mol/L) standard solutions. The prepared solution was mixed according to the ratio and stirred for 1 hour. Then, the solution was titrated with aqueous ammonia to a pH of 9, and the solution was stirred to precipitate for 1 hour and then allowed to stand for 24 hours. Washing and precipitating by centrifugation, wherein the washing liquid is firstly deionized water and then absolute ethyl alcohol. After the washing and precipitation are finished, the precipitate is dried at the temperature of 60 ℃. And drying, grinding and precipitating to obtain a precursor, adding a fluxing agent to obtain a mixture, wherein the fluxing agent is boric acid, and the addition amount is 5wt%, so that the mixture is obtained. And placing the mixture into a tube furnace, heating to 1400 deg.C (air atmosphere), and keeping the temperature for 4 hrThen (c) is performed. And grinding the sintered product to obtain the designed fluorescent powder, and detecting and verifying the optical performance.
Example 3
The embodiment provides samarium-zirconium co-doped tin oxide fluorescent powder, which has the following chemical general formula: SnO2：xSm3+,yZr4 +Wherein x is 0.02 and y is 0.2.
The embodiment also provides a preparation method of the fluorescent powder, which comprises the following steps:
commercial tin chloride (8.765 g; 0.025 mol) was dissolved in 50mL of deionized water, the commercially available zirconyl nitrate (1.156 g; 1.150 mol) and concentrated nitric acid (0.692 mL; 0.010 mol) were dissolved to make up a 25mL (0.200mol/L) standard solution, and Sm was added2O3(0.087 g; 0.00025 mol) and 1.500mL of nitric acid (1mol/L) were prepared as 5mL (0.100mol/L) standard solutions. The prepared solution was mixed according to the ratio and stirred for 1 hour. Then, the solution was titrated with aqueous ammonia to a pH of 9, and the solution was stirred to precipitate for 1 hour and then allowed to stand for 24 hours. Washing and precipitating by centrifugation, wherein the washing liquid is firstly deionized water and then absolute ethyl alcohol. After the washing and precipitation are finished, the precipitate is dried at the temperature of 60 ℃. And drying, grinding and precipitating to obtain a precursor, adding a fluxing agent to obtain a mixture, wherein the fluxing agent is boric acid, and the addition amount is 5wt%, so that the mixture is obtained. And the mixture was placed in a tube furnace and heated to 1400 deg.c (air atmosphere) for 4 hours. And grinding the sintered product to obtain the designed fluorescent powder, and detecting and verifying the optical performance.
Example 4
The embodiment provides samarium-zirconium co-doped tin oxide fluorescent powder, which has the following chemical general formula: SnO2：xSm3+,yZr4 +Wherein x is 0.02 and y is 0.4.
The embodiment also provides a preparation method of the fluorescent powder, which comprises the following steps:
commercial tin chloride (8.765 g; 0.025 mol) was dissolved in 50mL of deionized water, and the purchased zirconyl nitrate (2.312 g; 2.301 mol) and concentrated nitric acid (2.770 mL; 0.020 mol) were dissolved to prepare a 50mL (0.200mol/L) standard solutionSm is2O3(0.087 g; 0.00025 mol) and 1.500mL of nitric acid (1mol/L) were prepared as 5mL (0.100mol/L) standard solutions. The prepared solution was mixed according to the ratio and stirred for 1 hour. Then, the solution was titrated with aqueous ammonia to a pH of 9, and the solution was stirred to precipitate for 1 hour and then allowed to stand for 24 hours. Washing and precipitating by centrifugation, wherein the washing liquid is firstly deionized water and then absolute ethyl alcohol. After the washing and precipitation are finished, the precipitate is dried at the temperature of 60 ℃. And drying, grinding and precipitating to obtain a precursor, adding a fluxing agent to obtain a mixture, wherein the fluxing agent is boric acid, and the addition amount is 5wt%, so that the mixture is obtained. And the mixture was placed in a tube furnace and heated to 1400 deg.c (air atmosphere) for 4 hours. And grinding the sintered product to obtain the designed fluorescent powder, and detecting and verifying the optical performance.
Example 5
The embodiment provides samarium-zirconium co-doped tin oxide fluorescent powder, which has the following chemical general formula: SnO2：xSm3+,yZr4 +Wherein x is 0.02 and y is 0.8.
The embodiment also provides a preparation method of the fluorescent powder, which comprises the following steps:
commercial tin chloride (8.765 g; 0.025 mol) was dissolved in 50mL of deionized water, the commercially available zirconyl nitrate (4.625 g; 4.602 mol) and concentrated nitric acid (5.540 mL; 0.040 mol) were dissolved to make 100mL (0.200mol/L) of standard solution, and Sm was added2O3(0.087 g; 0.00025 mol) and 1.500mL of nitric acid (1mol/L) were prepared as 5mL (0.100mol/L) standard solutions. The prepared solution was mixed according to the ratio and stirred for 1 hour. Then, the solution was titrated with aqueous ammonia to a pH of 9, and the solution was stirred to precipitate for 1 hour and then allowed to stand for 24 hours. Washing and precipitating by centrifugation, wherein the washing liquid is firstly deionized water and then absolute ethyl alcohol. After the washing and precipitation are finished, the precipitate is dried at the temperature of 60 ℃. And drying, grinding and precipitating to obtain a precursor, adding a fluxing agent to obtain a mixture, wherein the fluxing agent is boric acid, and the addition amount is 5wt%, so that the mixture is obtained. And the mixture was placed in a tube furnace and heated to 1400 deg.c (air atmosphere) for 4 hours. And grinding the sintered product to obtain the designed fluorescent powder, and detecting and verifying the optical performance.
Example 6
The embodiment provides samarium-zirconium co-doped tin oxide fluorescent powder, which has the following chemical general formula: SnO2：xSm3+,yZr4 +Wherein x is 0.02 and y is 0.9.
The embodiment also provides a preparation method of the fluorescent powder, which comprises the following steps:
commercial tin chloride (8.765 g; 0.025 mol) was dissolved in 50mL of deionized water, the commercially available zirconyl nitrate (5.203 g; 5.178 mol) and concentrated nitric acid (3.116 mL; 0.045 mol) were dissolved to prepare 112.500mL (0.200mol/L) of standard solution, and Sm was added2O3(0.088 g; 0.00025 mol) and 1.500mL of nitric acid (1mol/L) were prepared as 5mL (0.100mol/L) standard solutions. The prepared solution was mixed according to the ratio and stirred for 1 hour. Then, the solution was titrated with aqueous ammonia to a pH of 9, and the solution was stirred to precipitate for 1 hour and then allowed to stand for 24 hours. Washing and precipitating by centrifugation, wherein the washing liquid is firstly deionized water and then absolute ethyl alcohol. After the washing and precipitation are finished, the precipitate is dried at the temperature of 60 ℃. And drying, grinding and precipitating to obtain a precursor, adding a fluxing agent to obtain a mixture, wherein the fluxing agent is boric acid, and the addition amount is 5wt%, so that the mixture is obtained. And the mixture was placed in a tube furnace and heated to 1400 deg.c (air atmosphere) for 4 hours. And grinding the sintered product to obtain the designed fluorescent powder, and detecting and verifying the optical performance.
Example 7
The embodiment provides samarium-zirconium co-doped tin oxide fluorescent powder, which has the following chemical general formula: SnO2：xSm3+,yZr4 +Wherein x is 0.02 and y is 1.0.
The embodiment also provides a preparation method of the fluorescent powder, which comprises the following steps:
commercial tin chloride (8.765 g; 0.025 mol) was dissolved in 50mL of deionized water, the commercially available zirconyl nitrate (5.781 g; 5.753 mol) and concentrated nitric acid (3.462 mL; 0.050 mol) were dissolved to make 125mL (0.200mol/L) of standard solution, and Sm was added2O3(0.0872 g; 0.00025 mol) and nitric acid (1mol/L)1.500mL5mL (0.100mol/L) of the standard solution. The prepared solution was mixed according to the ratio and stirred for 1 hour. Then, the solution was titrated with aqueous ammonia to a pH of 9, and the solution was stirred to precipitate for 1 hour and then allowed to stand for 24 hours. Washing and precipitating by centrifugation, wherein the washing liquid is firstly deionized water and then absolute ethyl alcohol. After the washing and precipitation are finished, the precipitate is dried at the temperature of 60 ℃. And drying, grinding and precipitating to obtain a precursor, adding a fluxing agent to obtain a mixture, wherein the fluxing agent is boric acid, and the addition amount is 5wt%, so that the mixture is obtained. And the mixture was placed in a tube furnace and heated to 1400 deg.c (air atmosphere) for 4 hours. And grinding the sintered product to obtain the designed fluorescent powder, and detecting and verifying the optical performance.
The crystal structure of the prepared material was determined using an X' Pert Pro X-ray diffractometer, model number PANALytial, Netherlands. The fluorescence emission properties of the prepared materials were tested using a TRIA-320 fluorescence spectrometer, manufactured by Edinburgh, England.
FIG. 1 is an XRD (X-ray diffraction) diagram of samarium-zirconium co-doped tin oxide fluorescent powder prepared in example 6, and as can be seen from FIG. 1, the obtained product SnO2：xSm3+,yZr4+Is a tin oxide crystal of tetragonal phase structure;
as can be seen from FIG. 2, SnO2:0.02Sm3+The emission peak of (A) is 600-625 nm (orange light); SnO2:0.02Sm3+,0.1Zr4+The emission peak of (A) is 575-600 nm (yellow light) and 650-700 nm (red light); SnO2:0.02Sm3+,0.2Zr4+And SnO2:0.02Sm3+,0.4Zr4+The emission peak is 575-600 nm (yellow light) and 600-615 nm (orange light) 650-700 nm (red light).
SnO can be seen from FIG. 32:0.02Sm3+,0.4Zr4+， SnO2:0.02Sm3+,0.8Zr4+SnO2:0.02Sm3+,0.9Zr4+， SnO2:0.02Sm3+,1.0Zr4+The fluorescent material has the same emission peak, but the emission peaks have different intensities, and the emission peaks are respectively 575-600 nm (yellow light) and 600-615 nm (orange light) 650-700 nm (red light).
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any equivalent alterations, modifications or improvements made by those skilled in the art to the above-described embodiments using the technical solutions of the present invention are still within the scope of the technical solutions of the present invention.
Claims (10)
1. A samarium and zirconium co-doped tin oxide fluorescent powder is characterized by having the following chemical general formula: SnO2：xSm3+,yZr4+Wherein x is 0.01 to 0.5, and y is 0 to 2.
2. The method for preparing the samarium-zirconium co-doped tin oxide fluorescent powder of claim 1, which is characterized by comprising the following steps of:
(1) according to the formula SnO2：xSm3+,yZr4+SnCl is weighed according to the stoichiometric ratio of each element4·2H2O、Sm2O3、ZrO(NO3)2·xH2O, wherein x is 0.01-0.5, and y is 0-2;
(2) SnCl4·2H2Dissolving O in water to prepare a solution 1; mixing Sm2O3Dissolving in an acid solution 1 to prepare a solution 2; ZrO (NO)3)2·xH2Dissolving O in water, and adding an acid solution 2 to prepare a solution 3;
(3) mixing and stirring the solution 1, the solution 2 and the solution 3 to obtain a mixed solution, and adding an alkaline solution to adjust the pH value of the mixed solution to be alkaline; fully stirring, standing to obtain a precipitate, and cleaning the precipitate to be neutral;
(4) drying the cleaned precipitate, grinding the dried precipitate into a precursor, and adding a fluxing agent to obtain a mixture; and sintering and grinding the mixture in a tubular furnace protected by atmosphere to obtain the samarium-zirconium co-doped tin oxide fluorescent powder.
3. The method for preparing samarium and zirconium co-doped tin oxide phosphor according to claim 2, wherein the acid solution 1 or the acid solution 2 in the step (2) comprises nitric acid or hydrochloric acid; the pH value of the acid solution 1 is 1-6; the pH of the acid solution 2 is 1-6.
4. The method for preparing the samarium and zirconium co-doped tin oxide fluorescent powder according to claim 2, wherein the alkaline solution in the step (3) comprises ammonia water or sodium hydroxide solution, and the pH value of the mixed solution is 7-14 after the alkaline solution is added.
5. The method for preparing the samarium and zirconium co-doped tin oxide fluorescent powder according to claim 2, wherein the stirring speed in the step (3) is 100-2000 r/min; the stirring time is 1-5 hours.
6. The method for preparing the samarium and zirconium co-doped tin oxide fluorescent powder according to claim 2, wherein the standing time in the step (4) is 1-24 hours, and washing liquids used for washing the precipitate are distilled water and absolute ethyl alcohol.
7. The method for preparing samarium and zirconium co-doped tin oxide fluorescent powder according to claim 2, wherein the drying temperature in the step (4) is 60-120 ℃.
8. The method for preparing the samarium and zirconium co-doped tin oxide fluorescent powder according to claim 2, wherein the sintering temperature of the mixture in the step (4) in a tubular furnace is 600-1400 ℃; the sintering time is 0.5-12 hours.
9. The method for preparing samarium and zirconium co-doped tin oxide fluorescent powder according to claim 2, wherein the cosolvent in the step (4) comprises one or more of boric acid, sodium carbonate or fluorite; the content of the cosolvent in the mixture is 0.001-20 wt%.
10. The method for preparing samarium and zirconium co-doped tin oxide phosphor according to claim 2, wherein the atmosphere in step (4) comprises air or oxygen.
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| CN105600815A (en) * | 2014-11-12 | 2016-05-25 | 天津科技大学 | Doped nanometer zinc oxide light conversion agent preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105600815A (en) * | 2014-11-12 | 2016-05-25 | 天津科技大学 | Doped nanometer zinc oxide light conversion agent preparation method |
Non-Patent Citations (3)
| Title |
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| JIACHI ZHANG ET AL.: "The synthesis and afterglow luminescence properties of a novel red afterglow phosphor: SnO2:Sm3+, Zr4+", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| TAO LIN ET AL.: "Size-Dependent Optical Properties of SnO2 Nanoparticles Prepared by Soft Chemical Technique", 《JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY》 * |
| 赵丹: "《新型磷酸盐晶体材料的合成与发光性能研究》", 31 December 2017, 西安交通大学出版社 * |
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