CN1876757B - 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 PDF

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CN1876757B
CN1876757B CN2006101034180A CN200610103418A CN1876757B CN 1876757 B CN1876757 B CN 1876757B CN 2006101034180 A CN2006101034180 A CN 2006101034180A CN 200610103418 A CN200610103418 A CN 200610103418A CN 1876757 B CN1876757 B CN 1876757B
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luminescent material
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heating
dissolving
sulfide
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CN1876757A (en
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卢利平
张希艳
柏朝晖
米晓云
刘全生
王晓春
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Changchun University of Science and Technology
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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

The low temperature combustion synthesis method of converting luminescent material of sulfide
Technical field
The invention belongs to non-oxide system up-conversion luminescent material preparation technology, particularly a kind of preparation method of converting luminescent material of sulfide belongs to optical function material Technology field.
Background technology
Up-conversion luminescent material can change infrared light invisible to the human eye into visible light, plays crucial effect in fields such as upconversion laser, 3 D stereo demonstration, anti-counterfeit recognitions.The up-conversion luminescent material of sulfide system has the outstanding feature of wide spectrum, low threshold value infrared response, has very important using value in infrared acquisition fields such as the adjusting of infrared laser light path, spot detection, light beam check and correction, the demonstration of emission light and the tracking of emission light.
On the 296th～298 page of the 30th the 3rd phase of volume of " optical technology " (China) that publication was published in May, 2004, be entitled as " CaS:Eu by what people such as Zhang Xiyan write 2+, Sm 3+Preparation and sign " one piece of article, a kind of preparation method of converting luminescent material of sulfide is disclosed, this method belongs to a kind of high-temperature solid phase reaction method.Adopt this method need be with material calcination long period under comparatively high temps, and, also need in the activated carbon powder reducing atmosphere, can finish preparation process, calcination temperature is 700～1200 ℃, and calcination time is 0.5～3.0h, and the product granularity is a micron order.
Low-temperature combustion synthesis (Low-temperature Combustion Synthesis is abbreviated as LCS) is to utilize metal nitrate and organic-fuel when heating strong oxidation-reduction reaction to take place and the high-energy that discharges is finished the synthetic of product.The outstanding advantage of this method is that Heating temperature is low, preparation time short, and reaction atmosphere is not required, thereby energy-conservation, convenient, prepared product granularity can reach nano level.At present, the material system aspect from by LCS method preparation also is confined to oxide compound and composite oxides substantially, and for example, people such as J.J.Kingsley 1988 are at " Materials Letters " 6 (11/12): reported Al on 427～432 pages 2O 3The LCS method preparation of superfine powder; People such as Zhimin Zhong nineteen ninety-five is at " Journal of Materials Research " 10 (1): reported BaTiO on 945～952 pages 3The LCS method preparation of superfine powder.And from material function aspect, relate to the numerous areas that comprises luminescent material by LCS method preparation, as Lee east equality people 2004 at " rare metal " 28 (4): 62～665 pages of LCS methods preparations of having reported long persistence luminescent silicate material.
Summary of the invention
The outstanding shortcoming of high-temperature solid phase reaction method is temperature of reaction height and long reaction time, also needs to control reaction atmosphere, and the product granularity is big in addition.If make product have higher infrared conversion luminescence intensity, generally will be under 1050 ℃ of temperature calcination 1 hour, the product granularity often needs long-time grinding at micron order when second stage employ, cause luminous intensity to descend.
And existing low-temperature combustion synthesis is not applied to the preparation of sulfide system up-conversion luminescent material as yet, and, adopt low-temperature combustion synthesis to prepare sulfide system up-conversion luminescent material and also exist the technical barrier that sulphur is insoluble to reaction mass.
In order to realize adopting low-temperature combustion synthesis to prepare sulfide system up-conversion luminescent material, we have invented a kind of low temperature combustion synthesis method of converting luminescent material of sulfide.
The present invention is achieved in that this method synthetic product is a converting luminescent material of sulfide, and its chemical expression is MS:D 1 M+, D 2 N+, wherein, M=Ca or Sr; D 1=Eu or Ce; D 2=Sm.Synthesis step is:
1, takes by weighing each rare earth oxide Eu by stoichiometric ratio 2O 3Perhaps CeO 2And Sm 2O 3, be dissolved in HNO respectively 3In be made into corresponding rare earth nitrate solution, be mixed with mixing solutions again;
2, with alkine earth metal nitrate Ca (NO 3) 24H 2O or Sr (NO 3) 2Be dissolved in the above-mentioned rare earth nitrate mixed solution with organic-fuel, treat the clarification of this solution after, in solution, add the sulphur powder, through miscible, promptly get the slip that burns;
Perhaps above-mentioned rare earth nitrate mixed solution heating is concentrated, again with alkine earth metal nitrate Ca (NO 3) 24H 2O or Sr (NO 3) 2, organic-fuel and sulphur powder mix, and grinds through mixing repeatedly, promptly gets the material base that burns;
3, will burn slip or burning material base places and is preheating to 500～600 ℃ furnace chamber in advance, reacts very fast being lighted, and burns, discharge the gentle body of big energy simultaneously, whole combustion reactions finishes in 3～5min, and take out the cooling back, and product is fluffy multilayer chip powder.
Compared to the prior art, can prepare converting luminescent material of sulfide, although ignition temperature is lower according to aforesaid method, but temperature of reaction can be up to 1600 ℃, so the product crystalline state is good, infrared conversion luminescence intensity height, its luminosity can reach 5.4cd/m 2Reactant at high temperature, under the effect of the reaction gas that moment produced, be the fine droplet shape, and calcination time is very short, and the products therefrom quality is loose, particle is tiny, and granularity can reach nano level and even, as particle diameter is 20～40nm, so the luminescent material of granularity can directly be used, need not secondary processing.The infrared response threshold value is low, as 1 μ w, and has the infrared transition effects of going up of wide spectrum, has versatility for the detection of infrared light in 810～1550nm scope.Short, simple synthetic method of whole process of preparation time.Miscible or the mixed step of grinding of being established has solved the sulphur powder that existing low temperature combustion synthesis method did not run into and the mixed problem of other reactants.
Description of drawings
Fig. 1 is the last switching emission spectrogram of the embodiment of the invention 1 prepared converting luminescent material of sulfide.The double accompanying drawing that makes an abstract of this figure.Fig. 2 is the last switching emission spectrogram of the embodiment of the invention 5 prepared converting luminescent material of sulfide.Fig. 3 is the last switching emission spectrogram of the embodiment of the invention 9 prepared converting luminescent material of sulfide.
Embodiment
This method synthetic product is a converting luminescent material of sulfide, and its chemical expression is MS:D 1 M+, D 2 N+, wherein, M=Ca or Sr; D 1=Eu or Ce; D 2=Sm, alkaline earth sulfide MS be as matrix, variable valence rare earth ion D 1, D 2As dopant ion.Synthesis step is:
1, takes by weighing each rare earth oxide Eu by stoichiometric ratio 2O 3Or CeO 2And Sm 2O 3, be dissolved in HNO respectively 3In be made into corresponding rare earth nitrate solution, be mixed with mixing solutions again.Selected rare earth oxide purity is 99.99%, selected HNO 3Purity is spectroscopically pure.Introduce dopant ion in the product by this step.
2, with alkine earth metal nitrate Ca (NO 3) 24H 2O or Sr (NO 3) 2Be dissolved in the above-mentioned rare earth nitrate mixed solution with organic-fuel, treat the clarification of this solution after, in solution, add the sulphur powder, through miscible, promptly get the slip that burns;
Perhaps above-mentioned rare earth nitrate mixed solution heating is concentrated, again with alkine earth metal nitrate Ca (NO 3) 24H 2O or Sr (NO 3) 2, organic-fuel and sulphur powder mix, and grinds through mixing repeatedly, promptly gets the material base that burns.
The purity of selected alkine earth metal nitrate is analytical pure; The sulphur powder is the sublimed sulphur powder; Introduce each element in the product matrix by this step.Select urea CO (NH 2) 2, glycine C 2H 5NO 2With citric acid C 6H 8O 7H 2One of O is analytical pure as organic-fuel, plays the reductive agent effect in combustion reactions.Miscible method is for adopting the magnetic stirring apparatus heating and stirring 8～10min, ultrasonic vibration 30～60min afterwards.Mixing the method for grinding is earlier with alkine earth metal nitrate Ca (NO 3) 24H 2O or Sr (NO 3) 2, after organic-fuel and sulphur powder place the agate mortar mixed grinding evenly, the more spissated rare earth nitrate mixed solution of above-mentioned heating is poured into, mix repeatedly afterwards and grind until evenly.
By Eu ionic mole doping content in the above-mentioned steps control product is 0.02～0.5%; Ce ionic mole doping content is 0.02～0.6%; Sm ionic mole doping content is 0.04～1.0%; All for 1 mol alkali earth metals sulfide M S.
3, will burn slip or burning material base places and is preheating to 500～600 ℃ furnace chamber in advance, reacts very fast being lighted, and burns, discharge the gentle body of big energy simultaneously, whole combustion reactions finishes in 3～5min, and take out the cooling back, and product is fluffy multilayer chip powder.
Alkine earth metal nitrate can be used formula M (NO 3) 2Following chemical reaction takes place in this step in (M=Ca or Sr) expression, when adopting urea to make fuel:
6M(NO 3) 2+10CO(NH 2) 2+9S＝＝＝6MS+10CO 2↑+20H 2O↑+16N 2↑+3SO 2↑
When adopting glycine to make fuel:
18M(NO 3) 2+20C 2H 5NO 2+27S＝＝＝18MS+40CO 2↑+50H 2O↑+28N 2↑+9SO 2↑
When adopting citric acid to make fuel:
18M(NO 3) 2+10C 6H 8O 7·H 2O+27S＝＝＝18MS+60CO 2↑+50H 2O↑+18N 2↑+9SO 2↑
Further illustrate the present invention below, embodiment 1: under the room temperature, with Eu 2O 3And Sm 2O 3With concentration respectively rare HNO of 6mol/L 3Heating for dissolving treats that rare earth oxide all after the dissolving, pours in the volumetric flask, adds the Eu (NO that deionized water is mixed with 0.00003mol/mL 3) 3Sm (the NO of solution and 0.00003mol/mL 3) 3Solution.Measure above-mentioned Eu (NO respectively with injection needle 3) 3And Sm (NO 3) 3Solution 1.3mL and 0.65mL mix.In mixing solutions, add 4.723g Ca (NO 3) 24H 2O and 2.002g urea, heating for dissolving, treat solution clarification after, add 0.96g sublimed sulphur powder, heating and magnetic agitation 10min, ultrasonic vibration 30min places the burning slip that obtains to be preheating to 520 ℃ retort furnace in advance, takes out behind the 5min.Gained up-conversion luminescent material particle diameter is 20～40nm, under 810～1550nm is infrared ray excited, sends red visible light, sees shown in Figure 1.
Embodiment 2: under the room temperature, with Eu 2O 3And Sm 2O 3With concentration respectively rare HNO of 6mol/L 3Heating for dissolving treats that rare earth oxide all after the dissolving, pours in the volumetric flask, adds the Eu (NO that deionized water is mixed with 0.00003mol/mL 3) 3Sm (the NO of solution and 0.00003mol/mL 3) 3Solution.Measure above-mentioned Eu (NO respectively with injection needle 3) 3And Sm (NO 3) 3Solution 1.3mL and 0.65mL mix, and the mixing solutions heating is concentrated into 1mL.Take by weighing 4.723g Ca (NO 3) 24H 2O, 1.3344g glycine and 0.96g sublimed sulphur powder, after placing the agate mortar mixed grinding evenly, the heating concentrated solution of above-mentioned 1mL rare earth nitrate is poured into, mixed repeatedly and grind evenly, the burning material base that obtains placed be preheating to 540 ℃ retort furnace in advance, take out behind the 3min.The gained up-conversion luminescent material is infrared ray excited down at 810～1550nm, sends red visible light.
Embodiment 3: under the room temperature, with Eu 2O 3And Sm 2O 3With concentration respectively rare HNO of 6mol/L 3Heating for dissolving treats that rare earth oxide all after the dissolving, pours in the volumetric flask, adds the Eu (NO that deionized water is mixed with 0.00003mol/mL 3) 3Sm (the NO of solution and 0.00003mol/mL 3) 3Solution.Measure above-mentioned Eu (NO respectively with injection needle 3) 3And Sm (NO 3) 3Solution 0.3mL and 0.65mL mix.In mixing solutions, add 2.3615g Ca (NO 3) 24H 2O, 2.335g citric acid and 50mL deionized water, after the dissolving, mixed solution is placed on the magnetic stirring apparatus heating and stirs 40～60min, change in 70～90 ℃ of waters bath with thermostatic control, after treating that solution forms light yellow gel, put into the dry 8～15h of 100～120 ℃ of baking ovens, take out the back and pulverize with agate mortar, add 0.96g sublimed sulphur powder again, mix repeatedly and grind evenly.Ground burning material base placed be preheating to 600 ℃ retort furnace in advance, take out behind the 5min.The gained up-conversion luminescent material is infrared ray excited down at 810～1550nm, sends red visible light.
Embodiment 4: under the room temperature, take by weighing 0.00688g CeO 2With 0.00698g Sm 2O 3, use the dense HNO of 10mL respectively 3With 1mL concentration be rare HNO of 6mol/L 3Heating for dissolving treats that rare earth oxide all after the dissolving, mixes, and adds 4.723g Ca (NO in mixing solutions 3) 24H 2O and 1.001g urea, heating for dissolving, treat solution clarification after, add 0.96g sublimed sulphur powder, heating and magnetic agitation 8min, ultrasonic vibration 60min places the burning slip that obtains to be preheating to 560 ℃ retort furnace in advance, takes out behind the 4min.The gained up-conversion luminescent material is infrared ray excited down at 810～1550nm, sends the light green visible light.
Embodiment 5: under the room temperature, take by weighing 0.0103g CeO 2With 0.00698g Sm 2O 3, use the dense HNO of 15mL respectively 3With 1mL concentration be rare HNO of 6mol/L 3Heating for dissolving treats that rare earth oxide all after the dissolving, mixes, and the mixing solutions heating is concentrated into 1mL.Take by weighing 4.723g Ca (NO 3) 24H 2O, 1.6016g urea and 0.96g sublimed sulphur powder, after placing the agate mortar mixed grinding evenly, the heating concentrated solution of above-mentioned 1mL rare earth nitrate is poured into, mixed repeatedly and grind evenly, the burning material base that obtains placed be preheating to 540 ℃ retort furnace in advance, take out behind the 4min.The gained up-conversion luminescent material sends the light green visible light under 810～1550nm is infrared ray excited, see shown in Figure 2.
Embodiment 6: under the room temperature, take by weighing 0.0103g CeO 2With 0.00698g Sm 2O 3, use the dense HNO of 15mL respectively 3With 1mL concentration be rare HNO of 6mol/L 3Heating for dissolving treats that rare earth oxide all after the dissolving, mixes, and adds 4.723g Ca (NO in mixing solutions 3) 24H 2O and 1.668g glycine, heating for dissolving, treat solution clarification after, add 0.96g sublimed sulphur powder, heating and magnetic agitation 10min, ultrasonic vibration 40min places the burning slip that obtains to be preheating to 560 ℃ retort furnace in advance, takes out behind the 5min.The gained up-conversion luminescent material is infrared ray excited down at 810～1550nm, sends the light green visible light.
Embodiment 7: under the room temperature, take by weighing 0.00703g Eu 2O 3With 0.00698g Sm 2O 3, be respectively rare HNO of 6mol/L with 1mL concentration 3Heating for dissolving treats that rare earth oxide all dissolves the back and mixes, and adds 8.4652g Sr (NO in mixing solutions 3) 2With 2.002g urea, heating for dissolving, treat solution clarification after, add 1.9236g sublimed sulphur powder, heating and magnetic agitation 10min, ultrasonic vibration 40min places the burning slip that obtains to be preheating to 580 ℃ retort furnace in advance, takes out behind the 3min.The gained up-conversion luminescent material is infrared ray excited down at 810～1550nm, sends orange red visible light.
Embodiment 8: under the room temperature, take by weighing 0.00703g Eu 2O 3With 0.00698g Sm 2O 3, be respectively rare HNO of 6mol/L with 1mL concentration 3Heating for dissolving treats that rare earth oxide all dissolves the back and mixes, and adds 3.1208g NH in mixing solutions 4NO 3, 8.4652g Sr (NO 3) 2With 3.2032g urea, heating for dissolving, treat solution clarification after, add 2.8854g sublimed sulphur powder, heating magnetic agitation 10min, ultrasonic vibration 40min places the burning slip that obtains to be preheating to 540 ℃ retort furnace in advance, takes out behind the 3min.The gained up-conversion luminescent material is infrared ray excited down at 810～1550nm, sends orange red visible light.The NH that is added 4NO 3Be secondary oxidizer, replenish the nitrate radical that loses owing to pyrolytic decomposition.
Embodiment 9: under the room temperature, take by weighing 0.01406g Eu 2O 3With 0.01396g Sm 2O 3, be respectively rare HNO of 6mol/L with 2mL concentration 3Heating for dissolving treats that rare earth oxide all dissolves the back and mixes, and the mixing solutions heating is concentrated into 2mL.Take by weighing 6.1826g NH 4NO 3, 8.4652g Sr (NO 3) 2, 3.336g glycine and 3.8472g sublimed sulphur powder, after placing the agate mortar mixed grinding evenly, the heating concentrated solution of above-mentioned 2mL rare earth nitrate is poured into, mixed repeatedly and grind evenly, the burning material base that obtains placed be preheating to 520 ℃ retort furnace in advance, take out behind the 5min.Gained up-conversion luminescent material particle diameter is 20nm, under 810～1550nm is infrared ray excited, sends orange red visible light, sees shown in Figure 3.
Embodiment 10: under the room temperature, take by weighing 0.01406g Eu 2O 3With 0.01396g Sm 2O 3, be respectively rare HNO of 6mol/L with 2mL concentration 3Heating for dissolving treats that rare earth oxide all after the dissolving, mixes, and the mixing solutions heating is concentrated into 2mL.Take by weighing 8.4652g Sr (NO 3) 2, 5.004g glycine and 5.7708g sublimed sulphur powder, after placing the agate mortar mixed grinding evenly, the heating concentrated solution of above-mentioned 2mL rare earth nitrate is poured into, mixed repeatedly and grind evenly, the burning material base that obtains placed be preheating to 500 ℃ retort furnace in advance, take out behind the 4min.The gained up-conversion luminescent material is infrared ray excited down at 810～1550nm, sends orange red visible light.
Embodiment 11: under the room temperature, take by weighing 0.0103g CeO 2With 0.00698g Sm 2O 3, use the dense HNO of 15mL respectively 3With 1mL concentration be rare HNO of 6mol/L 3Heating for dissolving treats that rare earth oxide all after the dissolving, mixes, and the mixing solutions heating is concentrated into 2mL.Take by weighing 8.4652g Sr (NO 3) 2, 3.2032g urea and 2.8854g sublimed sulphur powder, after placing the agate mortar mixed grinding evenly, the heating concentrated solution of above-mentioned 2mL rare earth nitrate is poured into, mixed repeatedly and grind evenly, the burning material base that obtains placed be preheating to 500 ℃ retort furnace in advance, take out behind the 4min.The gained up-conversion luminescent material is infrared ray excited down at 810～1550nm, sends orange red visible light.

Claims (1)

1. a low temperature combustion synthesis method is characterized in that, this method synthetic product is a converting luminescent material of sulfide, and synthesis step is:
(1) under the room temperature, with Eu 2O 3And Sm 2O 3With concentration respectively rare HNO of 6mol/L 3Heating for dissolving treats that rare earth oxide all after the dissolving, pours in the volumetric flask, adds the Eu (NO that deionized water is mixed with 0.00003mol/mL 3) 3Sm (the NO of solution and 0.00003mol/mL 3) 3Solution;
(2) measure above-mentioned Eu (NO respectively with injection needle 3) 3And Sm (NO 3) 3Solution 0.3mL and 0.65mL mix, and add 2.3615g Ca (NO in mixing solutions 3) 24H 2O, 2.335g citric acid and 50mL deionized water, after the dissolving, mixed solution is placed on the magnetic stirring apparatus heating and stirs 40～60min, change in 70～90 ℃ of waters bath with thermostatic control, after treating that solution forms light yellow gel, put into the dry 8～15h of 100～120 ℃ of baking ovens, take out the back and pulverize with agate mortar, add 0.96g sublimed sulphur powder again, mix repeatedly and grind evenly;
(3) ground burning material base is placed be preheating to 600 ℃ retort furnace in advance, take out behind the 5min;
The gained up-conversion luminescent material is infrared ray excited down at 810～1550nm, sends red visible light.
CN2006101034180A 2006-07-20 2006-07-20 Low temperature combustion synthesis method for converting luminescent material of sulfide Expired - Fee Related CN1876757B (en)

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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
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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