CN1876757A - Low temperature combustion synthesis method for converting luminescent material of sulfide - Google Patents
Low temperature combustion synthesis method for converting luminescent material of sulfide Download PDFInfo
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Abstract
The invention relates the low-temperature burning synthesis of transform luminescent material on sulphide. The high-temperature solid state reaction method is used to prepare transform luminescent material on sulphide, and low-temperature burning synthesis is used to prepare oxidate and composite oxides materials. The defects of the high-temperature solid state reaction method are high reaction temperature, long reaction time and big graininess. The invention uses low-temperature burning synthesis method, overcoming the defects. The invention mixes the sulfur powder and other reactant. The invention has the advantages of highly effective, energy conservation, and low threshold of response value. The invention possesses the broad frequency spectrum conversion effect.
Description
Technical Field
The invention belongs to a preparation process of an up-conversion luminescent material of a non-oxide system, in particular to a preparation method of a sulfide up-conversion luminescent material, and belongs to the technical field of optical functional material processes.
Background
The up-conversion luminescent material can convert infrared light invisible to human eyes into visible light, and plays an important role in the fields of up-conversion lasers, three-dimensional display, anti-counterfeiting identification and the like. The up-conversion luminescent material of the sulfide system has the outstanding characteristics of wide frequency spectrum and low threshold infrared response, and has very important application value in the infrared detection fields of infrared laser light path adjustment, light spot detection, light beam correction, emitted light display, emitted light tracking and the like.
Published in optics technologies (China) volume 30, No. 3, pages 296 to 298, published in 2004, month 5, and entitled "CaS: Eu", by Zhang Xiyan et al2+，Sm3+The article "preparation and characterization" discloses a method for preparing a sulfide up-conversion luminescent material, which belongs to a high-temperature solid-phase reaction method. The method needs to burn the material at a high temperature for a long time, and also needs to complete the preparation process in an activated carbon powder reducing atmosphere, wherein the burning temperature is 700-1200 ℃, the burning time is 0.5-3.0 h, and the granularity of the product is micron.
Low-temperature Combustion Synthesis (LCS) is a Synthesis of products using high energy released by strong oxidation-reduction reactions of metal nitrates with organic fuels when heated. The method has the outstanding advantages of low heating temperature, short preparation time and no requirement on reaction atmosphere, thereby saving energy, being convenient and fast, and the granularity of the prepared product can reach the nanometer level. At present, from the point of view of material systems prepared by the LCS method, there are also fundamental limitations to oxides and complex oxides, for example, J.J.Kingsley et al, Materials Letters 6(11/12) 1988: al is reported on pages 427-4322O3LCS method for preparing superfine powder(ii) a Zhimin Zhong et al, Journal of Materials Research 10(1) in 1995: BaTiO is reported on pages 945 to 9523LCS method for preparing superfine powder. However, from the aspect of the function of materials prepared by the LCS method, it relates to many fields including luminescent materials, such as rare metals 28(4) in 2004 by luotoping et al: the LCS method preparation of the silicate long-afterglow luminescent material is reported on pages 62 to 665.
Disclosure of Invention
The high-temperature solid-phase reaction method has the outstanding disadvantages of high reaction temperature, long reaction time, reaction atmosphere control and large product particle size. If the product is requiredto have higher infrared conversion luminous intensity, the product is generally burnt at 1050 ℃ for 1 hour, the particle size of the product is micron-sized, and long-time grinding is often required during secondary utilization, so that the luminous intensity is reduced.
The existing low-temperature combustion synthesis method is not applied to the preparation of the sulfur-containing matter up-conversion luminescent material, and the technical problem that sulfur is insoluble in reaction materials exists in the preparation of the sulfur-containing matter up-conversion luminescent material by adopting the low-temperature combustion synthesis method.
In order to realize the preparation of the sulfide up-conversion luminescent material by adopting a low-temperature combustion synthesis method, a low-temperature combustion synthesis method of the sulfide up-conversion luminescent material is invented.
The method is realized by synthesizing a product which is a sulfide up-conversion luminescent material, and the chemical expression of the product is MS: d1 m+，D2 n+Wherein M ═ Ca or Sr; d1Eu or Ce; d2Sm. The synthesis steps are as follows:
1. weighing each rare earth oxide Eu according to stoichiometric ratio2O3Or CeO2And Sm2O3Separately dissolved in HNO3Preparing corresponding rare earth nitrate solution, and preparing mixed solution;
2. alkaline earth metal nitrate Ca (NO)3)2·4H2O or Sr (NO)3)2Dissolving the organic fuel and the rare earth nitrate mixed solution in water, adding sulfur powder into the solution after the solution is clarified, and mixing and dissolving to obtain combustion slurry;
or heating and concentrating the mixed solution of the rare earth nitrate, and mixing with alkaline earth metal nitrate Ca (NO)3)2·4H2O or Sr (NO)3)2Mixing the organic fuel and the sulfur powder, and repeatedly mixing and grinding to obtain a combustion blank;
3. and (2) placing the combustion slurry or the combustion blank in a furnace chamber preheated to 500-600 ℃ in advance, igniting the combustion slurry or the combustion blank quickly to perform combustion, releasing a large amount of energy and gas, finishing the whole combustion reaction within 3-5 min, cooling and taking out the combustion slurry or the combustion blank to obtain a fluffy multi-layer sheet-shaped powder product.
Compared with the prior art, the sulfide up-conversion luminescent material can be prepared by the method, although the ignition temperature is lower, the reaction temperature can reach 1600 ℃, so the product has good crystallization state and high infrared conversion luminescent intensity, and the luminescent brightness can reach 5.4cd/m2. The reactant is in the shape of tiny drops under the action of gas generated at the moment of reaction at high temperature, the burning time is short, the obtained product has loose texture and fine particles, the particle size can reach the nanometer level and be uniform, for example, the particle size is 20-40 nm, and the luminescent material with the particle size can be directly applied without secondary processing. The infrared response threshold is low, such as 1 mu w, the wide-spectrum infrared upconversion effect is achieved, and the universality is achieved for detection of infrared light in the range of 810-1550 nm. The whole preparation process is short in time and the synthesis method is simple and convenient. The established mixing and mixing or grinding step solves the problem of mixing of sulfur powder and other reactants which is not met bythe existing low-temperature combustion synthesis method.
Drawings
FIG. 1 is an upconversion emission spectrum of a sulfide upconversion luminescent material prepared in example 1 of the present invention. This figure is also taken as an abstract figure. FIG. 2 is an upconversion emission spectrum of the sulfide upconversion luminescent material prepared in example 5 of the present invention. FIG. 3 is an upconversion emission spectrum of the sulfide upconversion luminescent material prepared in example 9 of the present invention.
Detailed Description
The synthesized product is a sulfide up-conversion luminescent material, and the chemical expression of the synthesized product is MS: d1 m+，D2 n+Wherein M ═ Ca or Sr; d1Eu or Ce; d2Sm, sulfide of alkaline earth metal MS as matrix, variable valence rare earth ion D1、D2As dopant ions. The synthesis steps are as follows:
1. weighing each rare earth oxide Eu according to stoichiometric ratio2O3Or CeO2And Sm2O3Separately dissolved in HNO3Preparing corresponding rare earth nitrate solution, and preparing mixed solution. The purity of the selected rare earth oxide is 99.99 percentHNO3The purity is spectral purity. The dopant ions in the product are introduced by this step.
2. Alkaline earth metal nitrate Ca (NO)3)2·4H2O or Sr (NO)3)2Dissolving the organic fuel and the rare earth nitrate mixed solution in water, adding sulfur powder into the solution after the solution is clarified, and mixing and dissolving to obtain combustion slurry;
or heating and concentrating the mixed solution of the rare earth nitrate, and mixing with alkaline earth metal nitrate Ca (NO)3)2·4H2O or Sr (NO)3)2Mixing with organic fuel and sulfur powder, and repeatedly grinding to obtain the combustion blank.
The purity of the selected alkaline earth metal nitrate is analytical purity; the sulfur powder is sublimed sulfur powder; the elements introduced into the product matrix by this step. Selection of Urea CO (NH)2)2Glycine C2H5NO2And citric acid C6H8O7·H2One of the O is analytically pure as an organic fuel and acts as a reducing agent in the combustion reaction. The mixing and dissolving method comprises the steps of heating and stirring by a magnetic stirrer for 8-10 min, and then ultrasonically vibrating for 30-60 min. The mixing grinding method comprises the steps of firstly, alkaline earth metal nitrate Ca (NO)3)2·4H2O or Sr (NO)3)2And the organic fuel and the sulfur powder are put into an agate mortar to be mixed and ground uniformly, then the heated and concentrated rare earth nitrate mixed solution is poured in, and then the mixture is repeatedly mixed and ground until the mixture is uniform.
Controlling the molar doping concentration of Eu ions in the product to be 0.02-0.5% through the steps; the molar doping concentration of Ce ions is 0.02-0.6%; the molar doping concentration of Sm ions is 0.04-1.0%; both with respect to 1 mole of alkaline earth metal sulfide MS.
3. And (2) placing the combustion slurry or the combustion blank in a furnace chamber preheated to 500-600 ℃ in advance, igniting the combustion slurry or the combustion blank quickly to perform combustion, releasing a large amount of energy and gas, finishing the whole combustion reaction within 3-5 min, cooling and taking out the combustion slurry or the combustion blank to obtain a fluffy multi-layer sheet-shaped powder product.
The alkaline earth metal nitrate can be represented by the general formula M (NO)3)2(M ═ Ca or Sr), in which the following chemical reaction takes place, when urea is used as fuel:
the invention is further illustrated below, example 1: at room temperature, Eu is added2O3And Sm2O3Respectively using diluted HNO with the concentration of 6mol/L3Heating to dissolve, pouring into a volumetric flask after the rare earth oxide is completely dissolved, adding deionized water to prepare Eu (NO) of 0.00003mol/mL3)3Solution and 0.00003mol/mL of Sm (NO)3)3And (3) solution. Measuring the Eu (NO) with the injection needle tube3)3And Sm (NO)3)3The solutions were mixed at 1.3mL and 0.65 mL. 4.723g Ca (NO) was added to the mixed solution3)2·4H2Heating and dissolving O and 2.002g of urea, adding 0.96g of sublimed sulfur powder after the solution is clarified, heating and magnetically stirring for 10min, ultrasonically vibrating for 30min, placing the obtained combustion slurry in a muffle furnace preheated to 520 ℃, and taking out after 5 min. The particle size of the obtained up-conversion luminescent material is 20-40 nm, and the up-conversion luminescent material emits red visible light under the excitation of infrared light of 810-1550 nm, as shown in figure 1As shown.
Example 2: at room temperature, Eu is added2O3And Sm2O3Respectively using diluted HNO with the concentration of 6mol/L3Heating to dissolve, pouring into a volumetric flask after the rare earth oxide is completely dissolved, adding deionized water to prepare Eu (NO) of 0.00003mol/mL3)3Solution and 0.00003mol/mL of Sm (NO)3)3And (3) solution. Measuring the Eu (NO) with the injection needle tube3)3And Sm (NO)3)3The solution 1.3mL and 0.65mL were mixed, and the mixed solution was concentrated to 1mL by heating. Weighing 4.723g Ca (NO)3)2·4H2Placing O, 1.3344g of glycine and 0.96g of sublimed sulfur powder in an agate mortar, mixing and grinding uniformly, pouring 1mL of the heated concentrated solution of the rare earth nitrate, mixing and grinding uniformly repeatedly, placing the obtained combustion blank in a muffle furnace preheated to 540 ℃, and taking out after 3 min. The obtained up-conversion luminescent material emits red visible light under the excitation of infrared light of 810-1550 nm.
Example 3: at room temperature, Eu is added2O3And Sm2O3Respectively using diluted HNO with the concentration of 6mol/L3Heating to dissolve, pouring into a volumetric flask after the rare earth oxide is completely dissolved, adding deionized water to prepare Eu (NO) of 0.00003mol/mL3)3Solution and 0.00003mol/mL of Sm (NO)3)3And (3) solution. Measuring the Eu (NO) with the injection needle tube3)3And Sm (NO)3)3Solutions 0.3mL and 0.65mL were mixed. 2.3615g Ca (NO) was added to the mixed solution3)2·4H2Dissolving O, 2.335g of citric acid and 50mL of deionized water, placing the mixed solution on a magnetic stirrer, heating and stirring for 40-60 min, transferring into a constant-temperature water bath at 70-90 ℃, and waiting for dissolutionAnd (3) after the liquid forms light yellow gel, drying the light yellow gel in an oven at the temperature of 100-120 ℃ for 8-15 h, taking out the light yellow gel, grinding the light yellow gel into powder by using an agate mortar, adding 0.96g of sublimed sulfur powder, and repeatedly and uniformly mixing and grinding the powder. And placing the ground combustion blank in a muffle furnace preheated to 600 ℃ in advance, and taking out after 5 min. The obtained up-conversion luminescent material emits red visible light under the excitation of infrared light of 810-1550 nm.
Example 4: 0.00688g of CeO were weighed out at room temperature2And 0.00698g Sm2O3Respectively using 10mL of concentrated HNO3And 1mL of diluted HNO with a concentration of 6mol/L3Heating to dissolve, mixing after the rare earth oxide is completely dissolved, adding 4.723g Ca (NO) into the mixed solution3)2·4H2Heating and dissolving O and 1.001g of urea, adding 0.96g of sublimed sulfur powder after the solution is clarified, heating and magnetically stirring for 8min, ultrasonically vibrating for 60min, placing the obtained combustion slurry in a muffle furnace preheated to 560 ℃ in advance, and taking out after 4 min. The obtained up-conversion luminescent material emits light green visible light under the excitation of 810-1550 nm infrared light.
Example 5: at room temperature, 0.0103g CeO was weighed2And 0.00698g Sm2O3Respectively using 15mL of concentrated HNO3And 1mL of diluted HNO with a concentration of 6mol/L3Heating to dissolve, mixingafter the rare earth oxide is completely dissolved, and heating and concentrating the mixed solution to 1 mL. Weighing 4.723g Ca (NO)3)2·4H2O, 1.6016g of urea and 0.96g of sublimed sulfur powder are put into an agate mortar to be mixed and ground uniformly, then 1mL of the heated concentrated solution of the rare earth nitrate is poured into the mortar to be mixed and ground uniformly repeatedly, and the obtained combustion blank is put into a muffle furnace preheated to 540 ℃ in advance and taken out after 4 min. The obtained up-conversion luminescent material emits light green visible light under the excitation of 810-1550 nm infrared light, which is shown in figure 2.
Example 6: at room temperature, 0.0103g CeO was weighed2And 0.00698g Sm2O3Respectively using 15mL of concentrated HNO3And 1mL of diluted HNO with a concentration of 6mol/L3Heating to dissolve, mixing after the rare earth oxide is completely dissolved, adding 4.723g Ca (NO) into the mixed solution3)2·4H2O and 1668g glycine, heating to dissolve, adding 0.96g sublimed sulfur powder after the solution is clarified, heating and magnetically stirring for 10min, ultrasonically vibrating for 40min, placing the obtained combustion slurry in a muffle furnace preheated to 560 deg.CAnd taking out after 5 min. The obtained up-conversion luminescent material emits light green visible light under the excitation of 810-1550 nm infrared light.
Example 7: weighing 0.00703g Eu at room temperature2O3And 0.00698g Sm2O31mL of diluted HNO with the concentration of 6mol/L is respectively used3Heating to dissolve, mixing after the rare earth oxide is completely dissolved, adding 8.4652g Sr (NO) into the mixed solution3)2And 2.002g of urea, heating for dissolving, adding 1.9236g of sublimed sulfur powder after the solution is clarified, heating and magnetically stirring for 10min, ultrasonically vibrating for 40min, placing the obtained combustion slurry in a muffle furnace preheated to 580 ℃ in advance, and taking out after 3 min. The obtained up-conversion luminescent material emits orange-red visible light under the excitation of 810-1550 nm infrared light.
Example 8: weighing 0.00703g Eu at room temperature2O3And 0.00698g Sm2O31mL of diluted HNO with the concentration of 6mol/L is respectively used3Heating to dissolve, mixing after the rare earth oxide is completely dissolved, adding 3.1208g NH into the mixed solution4NO3、8.4652g Sr(NO3)2And 3.2032g of urea, heating for dissolving, adding 2.8854g of sublimed sulfur powder after the solution is clarified, heating and magnetically stirring for 10min, ultrasonically vibrating for 40min, placing the obtained combustion slurry in a muffle furnace preheated to 540 ℃ in advance, and taking out after 3 min. The obtained up-conversion luminescent material emits orange-red visible light under the excitation of 810-1550 nm infrared light. NH added4NO3To assist the oxidant, the nitrate that is lost due to pyrolysis is replenished.
Example 9: weighing 0.01406g Eu at room temperature2O3And 0.01396g Sm2O32mL of diluted HNO with a concentration of 6mol/L are respectively used3Heating to dissolve, mixing after the rare earth oxide is completely dissolved, and heating and concentrating the mixed solution to 2 mL. Weighing 6.1826g NH4NO3、8.4652g Sr(NO3)23.336g of glycine and 3.8472g of sublimed sulfur powder are placed in an agate mortar to be mixed and ground uniformly, then 2mL of the heated concentrated solution of the rare earth nitrate is poured into the mortar to be mixed and ground uniformly repeatedly, the obtained combustion blank is placed in a muffle furnace preheated to 520 ℃ in advance, and the blank is taken out after 5 min. The particle size of the obtained up-conversion luminescent material is 20nm, and the up-conversion luminescent material emits orange-red visible light under the excitation of infrared light of 810-1550 nm, as shown in figure 3.
Example 10: weighing 0.01406g Eu at room temperature2O3And 0.01396g Sm2O32mL of diluted HNO with a concentration of 6mol/L are respectively used3Heating to dissolve, mixing after the rare earth oxide is completely dissolved, and heating and concentrating the mixed solution to 2 mL. Weighing 8.4652g Sr (NO)3)25.004g of glycine and 5.7708g of sublimed sulfur powder are placed in an agate mortar to be mixed and ground uniformly, then 2mL of the heated concentrated solution of the rare earth nitrate is poured into the mortar to be mixed and ground uniformly repeatedly, the obtained combustion blank is placed in a muffle furnace preheated to 500 ℃ in advance, and the blank is taken out after 4 min. The obtained up-conversion luminescent material emits orange-red visible light under the excitation of 810-1550 nm infrared light.
Example 11: at room temperature, 0.0103g CeO was weighed2And 0.00698g Sm2O3Respectively using 15mL of concentrated HNO3And 1mL of diluted HNO with a concentration of 6mol/L3Heating to dissolve, mixing after the rare earth oxide is completely dissolved, and heating and concentrating the mixed solution to 2 mL. Weighing 8.4652g Sr (NO)3)23.2032g of urea and 2.8854g of sublimed sulfur powder are put into an agate mortar to be mixed and ground uniformly, then 2mL of the heated concentrated solution of the rare earth nitrate is poured into the mortar to be mixed and ground uniformlyrepeatedly, and the obtained combustion blank is put into a muffle furnace preheated to 500 ℃ in advance and taken out after 4 min. The obtained up-conversion luminescent material emits orange-red visible light under the excitation of 810-1550 nm infrared light.
Claims (6)
1. A low-temperature combustion synthesis method is characterized in that the synthesized product is a sulfide up-conversion luminescent material, and the synthesis steps are as follows:
(1) weighing each rare earth oxide Eu according to stoichiometric ratio2O3Or CeO2And Sm2O3Separately dissolved in HNO3Preparing corresponding rare earth nitrate solution, and preparing mixed solution;
(2) alkaline earth metal nitrate Ca (NO)3)2·4H2O or Sr (NO)3)2Dissolving the organic fuel and the rare earth nitrate mixed solution in water, adding sulfur powder into the solution after the solution is clarified, and mixing and dissolving to obtain combustion slurry;
or heating and concentrating the mixed solution of the rare earth nitrate, and mixing with alkaline earth metal nitrate Ca (NO)3)2·4H2O or Sr (NO)3)2Mixing the organic fuel and the sulfur powder, and repeatedly mixing and grinding to obtain a combustion blank;
(3) and (2) placing the combustion slurry or the combustion blank in a furnace chamber preheated to 500-600 ℃ in advance, igniting the combustion slurry or the combustion blank quickly to perform combustion, releasing a large amount of energy and gas, finishing the whole combustion reaction within 3-5 min, cooling and taking out the combustion slurry or the combustion blank to obtain a fluffy multi-layer sheet-shaped powder product.
2. A synthesis method according to claim 1, characterized in that one of urea, glycine and citric acid is selected as organic fuel.
3. The synthesis method according to claim 1, wherein the mixing is performed by heating and stirring with a magnetic stirrer for 8-10 min, and then ultrasonically vibrating for 30-60 min.
4. The method according to claim 1, wherein the mixing is performed by first mixing the alkaline earth metal nitrate Ca (NO)3)2·4H2O or Sr (NO)3)2The organic fuel and the sulfur powder are put into an agate mortar to be mixed and ground uniformly, then the heated and concentrated rare earth nitrate mixed solution is poured in, and then the mixture is repeatedly mixed and ground until the mixture is uniform.
5. The method of synthesis according to claim 1, characterized in that NH is added to the reactants4NO3Nitrate radicals lost by pyrolysis are replenished as an auxiliary oxidizing agent.
6. The synthesis method according to claim 2 or 4, wherein when the organic fuel is citric acid and sulfur powder, the mixing method comprises mixing and grinding, the mixed solution is placed on a magnetic stirrer to be heated and stirred for 40-60 min, the mixed solution is transferred into a constant-temperature water bath at 70-90 ℃, after the solution forms light yellow gel, the mixed solution is placed into an oven at 100-120 ℃ to be dried for 8-15 h, the dried solution is taken out and ground into powder by an agate mortar, sublimed sulfur powder is added, and the mixture is repeatedly and uniformly mixed and ground.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103274695A (en) * | 2013-05-31 | 2013-09-04 | 哈尔滨工业大学 | Burning, synthesizing and casting method of non-oxide eutectic ceramics |
| CN103435351A (en) * | 2013-08-01 | 2013-12-11 | 长春理工大学 | Up-conversion luminescent sulfide ceramic |
| CN103601169A (en) * | 2013-06-13 | 2014-02-26 | 南昌大学 | Preparation method of carbon-hybrid nano belt |
| CN106701082A (en) * | 2017-02-16 | 2017-05-24 | 吉林大学 | Preparation method of up-conversion luminescence composite material based on Sm<2+> ion |
| CN106833626A (en) * | 2017-02-16 | 2017-06-13 | 吉林大学 | One kind is based on Sm2+The up-conversion luminescence composite of ion |
Family Cites Families (2)
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| CN1102170C (en) * | 1999-10-29 | 2003-02-26 | 重庆大学 | Combustion process for preparing long-afterglow phosphorescent powder |
| CN1632053A (en) * | 2004-11-08 | 2005-06-29 | 陕西科技大学 | Method for self-propagating combustion synthesis of strontium europium dysprosium aluminate long afterglow luminescent materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103274695A (en) * | 2013-05-31 | 2013-09-04 | 哈尔滨工业大学 | Burning, synthesizing and casting method of non-oxide eutectic ceramics |
| CN103274695B (en) * | 2013-05-31 | 2014-10-08 | 哈尔滨工业大学 | Burning, synthesizing and casting method of non-oxide eutectic ceramics |
| CN103601169A (en) * | 2013-06-13 | 2014-02-26 | 南昌大学 | Preparation method of carbon-hybrid nano belt |
| CN103435351A (en) * | 2013-08-01 | 2013-12-11 | 长春理工大学 | Up-conversion luminescent sulfide ceramic |
| CN106701082A (en) * | 2017-02-16 | 2017-05-24 | 吉林大学 | Preparation method of up-conversion luminescence composite material based on Sm<2+> ion |
| CN106833626A (en) * | 2017-02-16 | 2017-06-13 | 吉林大学 | One kind is based on Sm2+The up-conversion luminescence composite of ion |
| CN106701082B (en) * | 2017-02-16 | 2018-04-24 | 吉林大学 | A kind of preparation method based on Sm2+ ion up-conversion luminescence composite materials |
| CN106833626B (en) * | 2017-02-16 | 2018-04-24 | 吉林大学 | One kind is based on Sm2+The up-conversion luminescence composite material of ion |
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