CN102504800B - High-light-energy light conversion agent and preparation method thereof - Google Patents
High-light-energy light conversion agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-light-energy light conversion agent, wherein the compositional formula of the light conversion agent is Ca1-mMmZn1-nWnOS; and in the formula, m is greater than or equal to 0 and is less than or equal to 1, n is greater than or equal to 0 and is less than or equal to 1, M is one or more elements of Eu, Cu, Sm, Pr, Ce, Ho, Er, Tm, Lu, Yb and Tb, and W is one or more elements of Mn, Pb, Sn, Sb and Co. A preparation method of the high-light-energy light conversion agent comprises the following steps of: (1) weighing raw materials, crushing, uniformly mixing and placing in a crucible; (2) placing the crucible in a reaction container filled with active carbon and performing microwave sintering in a microwave oven; and (3) cooling, crushing, cleaning and drying a product obtained by sintering to obtain the light conversion agent. The high-light-energy light conversion agent has light conversion performance of converting rich green light in sunshine into red orange light capable of being absorbed by plants; one-time sintering of a high-temperature microwave technology is adopted; the sintering time is short; crystal grains are excellently prevented from growing; the active carbon is used as a wave absorbing carrier and protective atmosphere; the energy consumption in a synthesis process is greatly reduced; sulfur oxide is prevented from being oxidized; and the purity of the light conversion agent material is improved.
Description
Technical field
The invention belongs to the preparation field of agricultural light-converting film light-converting agent.Relate to a kind of high-light-energy light conversion agent and preparation method thereof.
Background technology
Photosynthesis is the prerequisite that green plants grows.Different plants has the chlorophyllous ability that absorbs different wave length light of manufacturing.Light-converting agent can convert sunlight medium ultraviolet light and green glow to the needed blue light of plant-growth and ruddiness, improves crop illumination condition, makes full use of sun power, reduces and uses agricultural chemicals and chemical fertilizer, is called as third generation physical fertilizer (light fertilizer).Various dissimilar light-converting agents are added in different resins, can make the multi-functional plastic sheeting for farm use that promotes different plant-growths, i.e. light conversion film.This functional type plastic sheeting for farm use is applicable to the colder north of weather conventionally, can regulate temperature of shed, promotes canopy temperature to rise when temperature is lower.When temperature is high, reduce canopy temperature; Promote plant growth, can make the prosperity of farm crop root system, photosynthesis amount strengthens, premature ripening; Optimize crop quality, can make the VITAMIN of agricultural-food, sugar part significantly increase; Increase output.Therefore light-converting agent has become a kind of valuable cargo of modern high technology agricultural.
Present stage, the light conversion agent on market can be divided into organic ligand rare-earth light-converting material, fluorescence dye and inorganic alkaline earth sulfide light-converting agent three classes.Organic ligand and fluorescence dye price are high, and the rate of decay is also very fast, can not synchronize with canopy membrane lifetime, make it extensively promote and be restricted.Sulfide is met water and is easily decomposed, and emits H
2s gas contamination environment.Therefore, people are devoted to develop the agricultural light-converting agent material that new performance is more superior always.In recent years, stratiform alkaline-earth metal oxysulfide performance water insoluble with it and anti-weak acid alkali has caused investigator's extensive concern.
At present, be mainly high temperature solid-state method for the synthesis of stratiform oxysulfide light conversion agent method.But this conventional heating mode synthesis temperature is high, sintering time is long, and power consumption is large, production efficiency is low, and preparation or the production cost of material are higher; And temperature rise rate is slow, particle size were is large, and granule-morphology is irregular, finally cause material to turn optical property wayward.
Summary of the invention
The object of the present invention is to provide a kind of high-light-energy light conversion agent, it has the optical property that turns that green glow abundant in sunlight is transferred to the absorbable blood orange light of plant.
Another object of the present invention is to provide a kind of microwave carbothermal reduction method to prepare the method for above-mentioned high-light-energy light conversion agent, and the method adopts microwave method to heat-treat, and not only preparation method is simple, and production cost is low, efficient energy-saving.
The technical solution adopted in the present invention is:
A kind of high-light-energy light conversion agent, its composition formula is: Ca
1-mm
mzn
1-nw
noS, in formula, 0≤m≤1,0≤n≤1, M be Eu, Cu, Sm, Pr, Ce, Ho, Er, Tm, Lu, Yb, Tb, in one or more elements, W is one or more elements in Mn, Pb, Sn, Sb, Co.
The preparation method of above-mentioned high-light-energy light conversion agent, comprises the steps:
1) raw material is weighed, pulverize, mix, be placed in crucible;
2) above-mentioned crucible is placed in the reaction vessel that gac is housed, in microwave oven, carries out microwave sintering;
3) product that sintering obtains obtains light-converting agent through cooling, pulverizing, cleaning, oven dry.
Preferably, step 2) microwave frequency of described microwave sintering is 15～28GHz, and temperature is 900 ~ 1000 DEG C, and the time is 10 ~ 180 minutes.
Preferably, also can add fusing assistant described in step 1) in raw material, described fusing assistant is at least one in boric acid, barium fluoride, bariumchloride, Sodium Fluoride, sodium-chlor, lithium fluoride.
Preferably, the mixing of step 1) raw material can adopt dry mixed.
Preferably, the mixing of step 1) raw material can adopt wet-mixed, and wet-mixed agent is dehydrated alcohol or water.
Beneficial effect of the present invention is:
1) high-light-energy light conversion agent of the present invention has the optical property that turns that green glow abundant in sunlight is transferred to the absorbable blood orange light of plant;
2) it is once sintered that preparation method of the present invention adopts high temperature microwave technology; sintering time is short; be only 10-180 minute; prevent preferably growing up of crystal grain; using cheap activated carbon as inhaling ripple carrier and protective atmosphere; greatly reduce building-up process energy consumption, prevented that oxysulfide is oxidized, improved the purity of light-converting agent material.
Brief description of the drawings
Fig. 1 is the XRD figure of the light conversion agent that obtains of example example 1;
Fig. 2 is the excitation spectrum (λ of the light conversion agent that obtains of embodiment 2
em=650nm);
Fig. 3 is the emmission spectrum (λ of the light conversion agent that obtains of embodiment 2
ex=530nm);
Fig. 4 is the SEM figure of the light conversion agent that obtains of embodiment 3.
Embodiment
A kind of high-light-energy light conversion agent, its composition formula is: Ca
1-mm
mzn
1-nw
noS, in formula, 0≤m≤1,0≤n≤1, M be Eu, Cu, Sm, Pr, Ce, Ho, Er, Tm, Lu, Yb, Tb, in one or more elements, W is one or more elements in Mn, Pb, Sn, Sb, Co.
The preparation method of above-mentioned high-light-energy light conversion agent, comprises the steps:
1) raw material is weighed, pulverize, mix, be placed in crucible;
2) above-mentioned crucible is placed in the reaction vessel that gac is housed, in microwave oven, carries out microwave sintering;
3) product that sintering obtains obtains light-converting agent through cooling, pulverizing, cleaning, oven dry.
Preferably, step 2) microwave frequency of described microwave sintering is 15～28GHz, and temperature is 900 ~ 1000 DEG C, and the time is 10 ~ 180 minutes.
Preferably, also can add fusing assistant described in step 1) in raw material, described fusing assistant is at least one in boric acid, barium fluoride, bariumchloride, Sodium Fluoride, sodium-chlor, lithium fluoride.
Below in conjunction with embodiment, the present invention is further illustrated, but be not limited to this.
embodiment 1 Ca
0.999
znO
0.999
s:Eu
0.001
Mixed in molar ratio by calcium oxide, zinc sulphide, europium sesquioxide with 0.999:1:0.001, carries out dry ball milling (rotating speed is 400rppm, Ball-milling Time 3h, ratio of grinding media to material is 10:1).After ball milling, powder is placed in to microwave oven, microwave frequency is 25GHz, and constant temperature sintering 150 minutes, naturally cools to room temperature at 1000 DEG C, broken, grind, clean, 100 DEG C of oven dry obtain high-light-energy light conversion agent Ca
0.999znO
0.999s:Eu
0.001.
embodiment 2 Ca
0.999
znO
0.999
s:Eu
0.001
Mixed in molar ratio by calcium oxide, zinc sulphide, europium sesquioxide with 0.999:1:0.001, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is dehydrated alcohol).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 20GHz, thermostatically heating 120 minutes at 900 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 100 DEG C of oven dry obtain high-light-energy light conversion agent Ca
0.999znO
0.999s:Eu
0.001.
embodiment 3 Ca
0.999
znO
0.999
s:Eu
0.001
, B
0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, europium sesquioxide, fusing assistant boric acid with 0.999:1:0.001:0.1, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is dehydrated alcohol).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 25GHz, thermostatically heating 120 minutes at 1000 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 100 DEG C of oven dry obtain high-light-energy light conversion agent Ca
0.999znO
0.999s:Eu
0.001, B
0.1.
embodiment 4?
ca 0.999 znO 0.999 s:Eu 0.001 , Na 0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, europium sesquioxide, fusing assistant Sodium Fluoride with 0.999:1:0.001:0.1, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is dehydrated alcohol).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 25GHz, thermostatically heating 120 minutes at 1000 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 100 DEG C of oven dry obtain high-light-energy light conversion agent Ca
0.999znO
0.999s:Eu
0.001, Na
0.1.
embodiment 5 Ca
0.998
znO
0.998
s:Eu
0.001
, Cu
0.001
, B
0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, europium sesquioxide, cupric chloride, fusing assistant boric acid with 0.998:1:0.001:0.001:0.1, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is dehydrated alcohol).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 25GHz, thermostatically heating 120 minutes at 1000 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 80 DEG C of oven dry obtain high-light-energy light conversion agent Ca
0.998znO
0.998s:Eu
0.001, Cu
0.001, B
0.1.
embodiment 6?
caZn 0.9 oS 0.9 : Mn 0.1 , B 0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, manganous carbonate, boric acid with 1:0.9:0.1:0.1, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is dehydrated alcohol).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 25GHz, thermostatically heating 120 minutes at 1000 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, oven dry CaZn
0.9oS
0.9: Mn
0.1, B
0.1.
embodiment 7?
ca 0.999 zn 0.9 o 0.999 s 0.9 : Mn 0.1 , Eu 0.001 , B 0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, manganous carbonate, europium sesquioxide, boric acid with 1:1:0.1:0.001:0.1, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is dehydrated alcohol).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 25GHz, thermostatically heating 120 minutes at 1000 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 100 DEG C of oven dry obtain high-light-energy light conversion agent Ca
0.999zn
0.9o
0.999s
0.9: Mn
0.1, Eu
0.001, B
0.1.
embodiment 8?
ca 0.997 zn 0.9 o 0.997 s 0.9 : Mn 0.1 , Eu 0.001 , Cu 0.002 , B 0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, manganous carbonate, europium sesquioxide, cupric chloride, boric acid with 0.997:0.9:0.1:0.001:0.002:0.1, (rotating speed is 200rppm to carry out mechanical wet-mixed, mixing time 3h, wet-mixed agent is dehydrated alcohol).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 20GHz, thermostatically heating 120 minutes at 900 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 100 DEG C of oven dry obtain high-light-energy light conversion agent Ca
0.997zn
0.9o
0.997s
0.9: Mn
0.1, Eu
0.001, Cu
0.002, B
0.1.
embodiment 9?
ca 0.999 zn 0.895 o 0.999 s 0.895 : Mn 0.1 , Eu 0.001 , Sn 0.005 , B 0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, manganous carbonate, europium sesquioxide, stannic oxide, boric acid with 0.999:0.895:0.1:0.001:0.005:0.1, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is water).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 26GHz, thermostatically heating 150 minutes at 950 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 80 DEG C of oven dry obtain high-light-energy light conversion agent Ca
0.999zn
0.895o
0.999s
0.895: Mn
0.1, Eu
0.001, Sn
0.005, B
0.1.
embodiment 10 CaZn
0.899
oS
0.899
: Mn
0.1
, Tm
0.001
, Ba
0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, manganous carbonate, trioxide, fusing assistant bariumchloride with 1:0.899:0.1:0.001:0.1, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is water).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 15GHz, thermostatically heating 100 minutes at 900 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 100 DEG C of oven dry obtain high-light-energy light conversion agent CaZn
0.899oS
0.899: Mn
0.1, Tm
0.001, B
0.1.
embodiment 11 CaZn
0.895
oS
0.895
: Pb
0.1
, Ce
0.005
, Na
0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, plumbous oxide, cerium oxide, fusing assistant sodium-chlor with 1:0.895:0.1:0.005:0.1, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is dehydrated alcohol).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 18GHz, thermostatically heating 120 minutes at 900 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 100 DEG C of oven dry obtain high-light-energy light conversion agent CaZn
0.895oS
0.895: Pb
0.1, Ce
0.005, B
0.1.
embodiment 12 CaZn
0.897
oS
0.897
: Sb
0.1
, Er
0.003
, B
0.1
Mixed in molar ratio by calcium oxide, zinc sulphide, weisspiessglanz, Erbium trioxide, fusing assistant boric acid with 1:0.897:0.1:0.003:0.1, carries out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, wet-mixed agent is dehydrated alcohol).Mixture is placed in to loft drier at 100 DEG C of dry 2h, then mixture is put into alumina crucible, again alumina crucible is placed in the reaction vessel that gac is housed, cover lid, be placed in microwave oven, microwave frequency is 20GHz, thermostatically heating 120 minutes at 900 DEG C, naturally cool to room temperature, fragmentation, grinding, cleaning, 100 DEG C of oven dry obtain high-light-energy light conversion agent CaZn
0.897oS
0.897: Sb
0.1, Er
0.003, B
0.1.
Above embodiment is only for introducing preferred case of the present invention, and to those skilled in the art, any apparent changes and improvements of carrying out in the scope that does not deviate from spirit of the present invention, all should be regarded as a part of the present invention.
Claims (4)
1. a preparation method for high-light-energy light conversion agent, comprises the steps:
1) raw material is weighed, pulverize, mix, be placed in crucible;
2) above-mentioned crucible is placed in the reaction vessel that gac is housed, in microwave oven, carries out microwave sintering;
3) product that sintering obtains obtains light-converting agent through cooling, pulverizing, cleaning, oven dry;
The composition formula of described high-light-energy light conversion agent is: Ca
1-mm
mzn
1-nw
noS, in formula, 0≤m≤1,0≤n≤1, M be Eu, Cu, Sm, Pr, Ce, Ho, Er, Tm, Lu, Yb, Tb, in one or more elements, W is one or more elements in Mn, Pb, Sn, Sb, Co;
Step 2) microwave frequency of described microwave sintering is 15～28GHz, and temperature is 900～1000 DEG C, and the time is 10～180 minutes.
2. the preparation method of high-light-energy light conversion agent according to claim 1, is characterized in that, also can add fusing assistant described in step 1) in raw material, and described fusing assistant is at least one in boric acid, bariumchloride, Sodium Fluoride, barium fluoride, sodium-chlor, lithium fluoride.
3. the preparation method of high-light-energy light conversion agent according to claim 1, is characterized in that, the mixing of step 1) raw material can adopt dry mixed.
4. the preparation method of high-light-energy light conversion agent according to claim 1, is characterized in that, the mixing of step 1) raw material can adopt wet-mixed, and wet-mixed agent is dehydrated alcohol or water.
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| CN102899033B (en) * | 2012-11-16 | 2014-11-26 | 湖南师范大学 | Method for preparing red fluorescent powder containing divalent europium ions |
| CN104073256B (en) * | 2014-03-20 | 2016-11-09 | 王海容 | A kind of thioborate fluorophor and application thereof |
| CN108607601A (en) * | 2018-05-15 | 2018-10-02 | 中国石油大学(华东) | Iron catalyst for Catalytic Decomposition of Hydrogen Peroxide prepares and reaction process |
| CN108686701A (en) * | 2018-05-15 | 2018-10-23 | 中国石油大学(华东) | Iron catalyst for destruction of phenol prepares and reaction process |
| CN110978697A (en) * | 2019-11-21 | 2020-04-10 | 徐蕾 | Light conversion film, multilayer light conversion film and preparation method of multilayer light conversion film |
| CN116443917A (en) * | 2023-03-13 | 2023-07-18 | 江南大学 | Preparation of mechanoluminescence CaZnOS: mn by microwaves 2+ Method of material |
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| KR100806734B1 (en) * | 2005-10-17 | 2008-02-27 | 루시미아 주식회사 | Luminescent material for emitting white light, preparation method thereof, and white light emitting diode using the material |
| EP2100943B1 (en) * | 2008-03-06 | 2013-07-10 | Leuchtstoffwerk Breitungen GmbH | ABOS:M-based phosphors and light sources containing these phosphors |
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