CN102504800A - 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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- CN102504800A CN102504800A CN2011103844395A CN201110384439A CN102504800A CN 102504800 A CN102504800 A CN 102504800A CN 2011103844395 A CN2011103844395 A CN 2011103844395A CN 201110384439 A CN201110384439 A CN 201110384439A CN 102504800 A CN102504800 A CN 102504800A
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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-converting 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 making.Light-converting agent can convert sunlight medium ultraviolet light and green glow to the needed blue light of plant-growth and ruddiness, improves the 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 is fertile).Various dissimilar light-converting agents are added in the different resins, can process 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 north that weather is cold usually, can regulate temperature of shed, and temperature promotes the canopy temperature to rise when low.When temperature is high, reduce the canopy temperature; Promote plant growth, can make the farm crop well developed root system, the photosynthesis amount strengthens, premature ripening; Optimize crop quality, can make VITAMINs, the sugar part significantly increase of agricultural-food; 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 the market can be divided into three types of organic ligand rare-earth light-converting material, optical dye and inorganic alkaline earth sulfide light-converting agents.Organic ligand and optical dye price are high, and the rate of decay is also very fast, can not be synchronous with the canopy membrane lifetime, and it is extensively promoted be restricted.Sulfide is met water and is prone to decompose, and emits H
2S gas contamination environment.Therefore, people are devoted to develop the more superior agricultural light-converting agent material of new performance always.In recent years, the performance of stratiform earth alkali metal oxysulfide water insoluble and anti-weak acid alkali with it has caused investigator's extensive concern.
At present, being used for synthetic stratiform oxysulfide light conversion agent method mainly is high temperature solid-state method.Yet this conventional type of heating synthesis temperature is high, and sintering time is long, and power consumption is big, production efficiency is low, and the preparation or the production cost of material are higher; And temperature rise rate is slow, and the product particle diameter is big, and granule-morphology is irregular, finally causes the commentaries on classics optical property of material wayward.
Summary of the invention
The object of the present invention is to provide a kind of high-light-energy light-converting agent, it has the commentaries on classics optical property that green glow abundant in the sunshine is transferred to the absorbable blood orange light of plant.
Another object of the present invention is to provide a kind of microwave carbothermic method to prepare the method for above-mentioned high-light-energy light-converting agent, and this method adopts microwave method to heat-treat, and not only the preparation method is simple, and production cost is low, efficient energy-saving.
The technical scheme that the present invention adopted is:
A kind of high-light-energy light-converting agent, its composition formula is: Ca
1-mM
mZn
1-nW
nOS, in the 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 among Mn, Pb, Sn, Sb, the Co.
The preparation method of above-mentioned high-light-energy light-converting agent comprises the steps:
1) raw material is weighed, pulverize, mix, place crucible;
2) above-mentioned crucible is placed in the reaction vessel that gac is housed, in microwave oven, carry out microwave sintering;
3) product that obtains of sintering through cooling, pulverize, clean, oven dry obtains light-converting agent.
Preferably, step 2) microwave frequency of said microwave sintering is 15～28GHz, and temperature is 900 ~ 1000 ℃, and the time is 10 ~ 180 minutes.
Preferably, also can add fusing assistant in the said raw material of step 1), said fusing assistant is at least a in boric acid, barium fluoride, bariumchloride, Sodium Fluoride, sodium-chlor, the lithium fluoride.
Preferably, the mixing of step 1) raw material can be adopted dry mixed.
Preferably, the mixing of step 1) raw material can be adopted wet-mixed, and the wet-mixed agent is absolute ethyl alcohol or water.
Beneficial effect of the present invention is:
1) high-light-energy light-converting agent of the present invention has the commentaries on classics optical property that green glow abundant in the sunshine is transferred to the absorbable blood orange light of plant;
2) it is once sintered that preparation method of the present invention adopts the high temperature microwave technology; Sintering time is short, is merely 10-180 minute, has prevented growing up of crystal grain preferably; With the activated carbon of cheapness as inhaling ripple carrier and protective atmosphere; Greatly reduce the building-up process energy consumption, prevented that oxysulfide is oxidized, improved the purity of light-converting agent material.
Description of drawings
The XRD figure of the light conversion agent that Fig. 1 obtains for embodiment 1;
Excitation spectrum (the λ of the light conversion agent that Fig. 2 obtains for embodiment 2
Em=650nm);
Emmission spectrum (the λ of the light conversion agent that Fig. 3 obtains for embodiment 2
Ex=530nm);
The SEM figure of the light conversion agent that Fig. 4 obtains for embodiment 3.
Embodiment
A kind of high-light-energy light-converting agent, its composition formula is: Ca
1-mM
mZn
1-nW
nOS, in the 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 among Mn, Pb, Sn, Sb, the Co.
The preparation method of above-mentioned high-light-energy light-converting agent comprises the steps:
1) raw material is weighed, pulverize, mix, place crucible;
2) above-mentioned crucible is placed in the reaction vessel that gac is housed, in microwave oven, carry out microwave sintering;
3) product that obtains of sintering through cooling, pulverize, clean, oven dry obtains light-converting agent.
Preferably, step 2) microwave frequency of said microwave sintering is 15～28GHz, and temperature is 900 ~ 1000 ℃, and the time is 10 ~ 180 minutes.
Preferably, also can add fusing assistant in the said raw material of step 1), said fusing assistant is at least a in boric acid, barium fluoride, bariumchloride, Sodium Fluoride, sodium-chlor, the lithium fluoride.
Below in conjunction with embodiment the present invention is further described, but is not limited thereto.
Embodiment 1 Ca
0.999
ZnO
0.999
S:Eu
0.001
With quicklime, zinc sulphide, europium sesquioxide mixed in molar ratio, carry out dry ball milling (rotating speed is 400rppm, ball milling time 3h, ball-to-powder weight ratio is 10:1) with 0.999:1:0.001.Behind the ball milling powder is placed microwave oven, microwave frequency is 25GHz, and 1000 ℃ of following constant temperature sintering 150 minutes naturally cool to room temperature, broken, grind, clean, 100 ℃ of oven dry obtain high-light-energy light-converting agent Ca
0.999ZnO
0.999S:Eu
0.001
With quicklime, zinc sulphide, europium sesquioxide mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is an absolute ethyl alcohol) with 0.999:1:0.001.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 20GHz, 900 ℃ of following thermostatically heating 120 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 100 ℃ of oven dry obtain high-light-energy light-converting agent Ca
0.999ZnO
0.999S:Eu
0.001
Embodiment 3 Ca
0.999
ZnO
0.999
S:Eu
0.001
, B
0.1
With quicklime, zinc sulphide, europium sesquioxide, fusing assistant boric acid mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is an absolute ethyl alcohol) with 0.999:1:0.001:0.1.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 25GHz, 1000 ℃ of following thermostatically heating 120 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 100 ℃ of oven dry obtain high-light-energy light-converting 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
With quicklime, zinc sulphide, europium sesquioxide, fusing assistant Sodium Fluoride mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is an absolute ethyl alcohol) with 0.999:1:0.001:0.1.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 25GHz, 1000 ℃ of following thermostatically heating 120 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 100 ℃ of oven dry obtain high-light-energy light-converting 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
With quicklime, zinc sulphide, europium sesquioxide, cupric chloride, fusing assistant boric acid mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is an absolute ethyl alcohol) with 0.998:1:0.001:0.001:0.1.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 25GHz, 1000 ℃ of following thermostatically heating 120 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 80 ℃ of oven dry obtain high-light-energy light-converting 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
With quicklime, zinc sulphide, manganous carbonate, boric acid mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is an absolute ethyl alcohol) with 1:0.9:0.1:0.1.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 25GHz, 1000 ℃ of following thermostatically heating 120 minutes; 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
With quicklime, zinc sulphide, manganous carbonate, europium sesquioxide, boric acid mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is an absolute ethyl alcohol) with 1:1:0.1:0.001:0.1.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 25GHz, 1000 ℃ of following thermostatically heating 120 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 100 ℃ of oven dry obtain high-light-energy light-converting 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
With quicklime, zinc sulphide, manganous carbonate, europium sesquioxide, cupric chloride, boric acid mixed in molar ratio 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, the wet-mixed agent is an absolute ethyl alcohol).Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 20GHz, 900 ℃ of following thermostatically heating 120 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 100 ℃ of oven dry obtain high-light-energy light-converting 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
With quicklime, zinc sulphide, manganous carbonate, europium sesquioxide, White tin oxide, boric acid mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is a water) with 0.999:0.895:0.1:0.001:0.005:0.1.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 26GHz, 950 ℃ of following thermostatically heating 150 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 80 ℃ of oven dry obtain high-light-energy light-converting 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
With quicklime, zinc sulphide, manganous carbonate, trioxide, fusing assistant bariumchloride mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is a water) with 1:0.899:0.1:0.001:0.1.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 15GHz, 900 ℃ of following thermostatically heating 100 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 100 ℃ of oven dry obtain high-light-energy light-converting 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
With quicklime, zinc sulphide, plumbous oxide, cerium oxide, fusing assistant sodium-chlor mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is an absolute ethyl alcohol) with 1:0.895:0.1:0.005:0.1.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 18GHz, 900 ℃ of following thermostatically heating 120 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 100 ℃ of oven dry obtain high-light-energy light-converting 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
With quicklime, zinc sulphide, weisspiessglanz, Erbium trioxide, fusing assistant boric acid mixed in molar ratio, carry out mechanical wet-mixed (rotating speed is 200rppm, mixing time 3h, the wet-mixed agent is an absolute ethyl alcohol) with 1:0.897:0.1:0.003:0.1.Place loft drier at 100 ℃ of dry 2h in mixture, put into alumina crucible to mixture then, again alumina crucible is placed in the reaction vessel that gac is housed; Cover lid; Place microwave oven, microwave frequency is 20GHz, 900 ℃ of following thermostatically heating 120 minutes; Naturally cool to room temperature, fragmentation, grinding, cleaning, 100 ℃ of oven dry obtain high-light-energy light-converting agent CaZn
0.897OS
0.897: Sb
0.1, Er
0.003, B
0.1
Above embodiment is merely and introduces preferred case of the present invention, and to those skilled in the art, any conspicuous variation and the improvement in the scope that does not deviate from spirit of the present invention, carried out all should be regarded as a part of the present invention.
Claims (6)
1. high-light-energy light-converting agent, its composition formula is: Ca
1-mM
mZn
1-nW
nOS, in the 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 among Mn, Pb, Sn, Sb, the Co.
2. the preparation method of the described high-light-energy light-converting agent of claim 1 comprises the steps:
1) raw material is weighed, pulverize, mix, place crucible;
2) above-mentioned crucible is placed in the reaction vessel that gac is housed, in microwave oven, carry out microwave sintering;
3) product that obtains of sintering through cooling, pulverize, clean, oven dry obtains light-converting agent.
3. the preparation method of high-light-energy light-converting agent according to claim 2 is characterized in that step 2) microwave frequency of said microwave sintering is 15～28GHz, and temperature is 900 ~ 1000 ℃, and the time is 10 ~ 180 minutes.
4. the preparation method of high-light-energy light-converting agent according to claim 2 is characterized in that, also can add fusing assistant in the said raw material of step 1), and said fusing assistant is at least a in boric acid, bariumchloride, Sodium Fluoride, barium fluoride, sodium-chlor, the lithium fluoride.
5. the preparation method of high-light-energy light-converting agent according to claim 2 is characterized in that, the mixing of step 1) raw material can be adopted dry mixed.
6. the preparation method of high-light-energy light-converting agent according to claim 2 is characterized in that, the mixing of step 1) raw material can be adopted wet-mixed, and the wet-mixed agent is absolute ethyl alcohol or water.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899033A (en) * | 2012-11-16 | 2013-01-30 | 湖南师范大学 | Method for preparing red fluorescent powder containing divalent europium ions |
| CN104073256A (en) * | 2014-03-20 | 2014-10-01 | 王海容 | Sulfoborate phosphor and application thereof |
| 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 |
| WO2021097977A1 (en) * | 2019-11-21 | 2021-05-27 | 山东森博斯特塑胶科技有限公司 | Light conversion film, and preparation method for multi-layer light conversion film |
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|---|---|
| CN102504800B (en) | 2014-08-20 |
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