CN106893584A - Rare-earth europium doped aluminium film and agricultural light conversion agent and preparation method thereof - Google Patents
Rare-earth europium doped aluminium film and agricultural light conversion agent and preparation method thereof Download PDFInfo
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- CN106893584A CN106893584A CN201710076850.3A CN201710076850A CN106893584A CN 106893584 A CN106893584 A CN 106893584A CN 201710076850 A CN201710076850 A CN 201710076850A CN 106893584 A CN106893584 A CN 106893584A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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Abstract
The present invention provides a kind of rare-earth europium doped aluminium film and agricultural light conversion agent and preparation method thereof.The molar content of aluminum oxide is 99.99~99.90% in the film, and the molar content of europium ion is 0.01%~0.10%.The agricultural light conversion agent includes matrix material and is arranged at the rare-earth europium doped aluminium film of substrate material surface.The preparation method of the agricultural light conversion agent is：Prepare boehmite sol；Prepare the boehmite sol of rare-earth europium doping；Substrate material surface is prepared using czochralski method and forms the aluminum oxide film that rare-earth europium is adulterated.It is aluminium isopropoxide as presoma that the present invention is used, rear-earth-doped oxidation aluminium film is prepared with sol-gal process, preparation process is simple, heat treatment temperature is low, the light converts the blood orange light required for the ultraviolet light of 280~400nm can be converted into plant by plastic film for agricultural use, is had broad application prospects in terms of greenhouse corps production.
Description
Technical field
The present invention relates to agricultural conversion film, more particularly to sol-gal process prepare rare-earth europium doped aluminium film and
Agricultural light conversion agent and preparation method thereof.
Background technology
With the continuous propulsion of building a knowledge-driven society, scientific and technological information and economic globalization, the strategy of sustainable development seems outstanding
For important.But the scarcity of resources and the hang-up of environmental pollution two for facing at present, this causes how to be provided using existing environmental protection
Source has far reaching significance.Sunshine is that plant carries out photosynthetic energy source, but plant is to the demand of solar energy, most
It is important that light quality, not only influences the photosynthetic efficiency of plant, the nutritional ingredient of each tissue of crops can also be regulated and controled.The sun
Blood orange light (600~700nm) and blue violet light (400~480nm) in light is particularly important to the photosynthesis of plant, and ultraviolet light
(200~400nm) is then easy to promote limb aging and germ reproduction, and remaining part is then mainly converted to the heat for improving temperature
Can, there is bad influence to the growth of plant.Chloroplaset is that plant carries out photosynthetic place, photochemical reaction in chloroplaset
Key substance be chlorophyll, have many photosynthetic pigments, such as chlorophyll a, chlorophyll b, carotenoid in green plants,
Although they are light absorbing very capable, actually plant carry out photosynthesis be mainly by chlorophyll complete, its allochromatic colour
The luminous energy that element absorbs can just cause photochemical reaction after can only passing to chlorophyll, and the most important property of chlorophyll is can selectivity
Ground absorbs light, and it has special absorption spectrum.The absorption spectrum of chlorophyll a and chlorophyll b is more similar, respectively there is 2 absorptions
Band, respectively blue zone and red tape, its most strong absorption band is respectively positioned at the blue violet light area of 400~480nm and 600~700nm
Blood orange light area, the ultraviolet light of below 400nm and the green glow of 500~580nm are not absorbed and are reflected substantially.
In the sunlight for impinging perpendicularly on ground, due to the influence of atmosphere, the blue light region beneficial to crop growth and
Red light district radiation intensity weakens, so manual simulation's plant optimum growh photoenvironment improves the illumination condition of crops, is allowed to
Significant to development high technological aqriculture in optimum growh state, therefore agricultural conversion film arises at the historic moment.Conversion film is
A kind of film that light conversion is realized by adding light conversion agent, it can convert ultraviolet light into the blue violet light useful to crop and red
Orange light, or green-yellow light is converted into blood orange light, so as to change the light quality through film, promote plant to nutrition such as nitrogen, phosphorus, potassium, zinc
The absorption of element, improves the blade area and expansion degree of plant, increases the plant height and petiole length of plant, thus increases blade and blade
The content of green element, raises the photosynthate content in blade, promotes plant growth.
Aluminum oxide film has excellent physical and chemical performance, and such as mechanical strength and hardness are high, heat endurance is good, taboo wide
Band, light transmission rate is high, insulating properties is splendid etc., is had a wide range of applications in many fields such as optics, machinery and microelectronics, and
And be a kind of good matrix material.Luminosity of the rare earth ion in different substrates is widely studied for many years, base after doping
The structure of material, optical property all make moderate progress, and have widened the application field of material.How will be unfavorable for planting crop growth
Ultraviolet light be converted into blue violet light and blood orange light, have become the focus of agricultural conversion film research.
The content of the invention
The technical problem to be solved in the present invention is：There is provided it is a kind of convert uv light into plant required for blood orange light
Rare-earth europium doped aluminium film and agricultural light conversion agent and preparation method thereof.
The present invention is for the solution technical scheme taken of above-mentioned technical problem：
A kind of rare-earth europium doped aluminium film, the Mole percent of aluminum oxide contains in the rare-earth europium doped aluminium film
It is 99.99~99.90mol% to measure, and the molar content of europium ion is 0.01%~0.10%.
In such scheme, when excitation wavelength is 200~400nm, the rare-earth europium doped aluminium film 610~
Occurs obvious characteristic radiation at 620nm.
A kind of agricultural light conversion agent, the agricultural light conversion agent includes matrix material and is arranged at described matrix material surface
Rare-earth europium doped aluminium film.
The preparation method of described agricultural light conversion agent, comprises the following steps：
Step one, prepare boehmite sol：Aluminium isopropoxide is added to the water and is sufficiently stirred for, hydrolyzed, be subsequently adding nitric acid, obtained
To boehmite sol；
Step 2, the boehmite sol for preparing rare-earth europium doping：The europium nitrate aqueous solution is added to boehmite sol, 85
DEG C~95 DEG C of refluxes in, be sufficiently stirred for 12~18h, obtain rare-earth europium doping boehmite sol；
Step 3, the aluminum oxide film for preparing rare-earth europium doping：Using czochralski method, matrix material is immersed in rare-earth europium and is mixed
Lift after 15~40s in miscellaneous boehmite sol, room temperature is naturally cooled to after Overheating Treatment, that is, obtain described agricultural turning finish
Material.
In such scheme, step one prepares concretely comprising the following steps for boehmite sol：By aluminium isopropoxide grind into powder, according to
Aluminium isopropoxide is 1 with the mol ratio of deionized water：100~1:200 weigh sample, and aluminium isopropoxide is dividedly in some parts to 75 DEG C~95
In DEG C deionized water, it is fully hydrolyzed, the reaction time is 1.5h~2.5h, then evaporates unnecessary isopropanol in solution, cooling
Afterwards, according to acid and the mol ratio 1 of aluminium isopropoxide:10~3:10 add sour, precipitation, in 85 DEG C~95 DEG C refluxes, fully
12~16h of stirring, is clarified, homogeneous boehmite sol.
In such scheme, what step 3 was heat-treated concretely comprises the following steps：When substrate material surface solution evaporates, by matrix material
Material is put into air dry oven, is processed 8~15 minutes, is finally putting into Muffle furnace, is warming up to 450 DEG C~500 DEG C, processes 1.5h
~3.5h, naturally cools to room temperature.
In such scheme, the concentration of the europium nitrate aqueous solution is 0.001~0.010mol/L in step 2.
In such scheme, described matrix material is sheet glass or optical fiber.
In such scheme, pull rate is 4000~6000 μm/s in step 3.
In such scheme, 450~500 DEG C are warming up to the heating rate of 3~10 DEG C/min in step 3 Muffle furnace.
Compared with prior art, what the present invention was obtained has the technical effect that：The present invention use be aluminium isopropoxide as presoma,
Rear-earth-doped oxidation aluminium film is prepared with sol-gal process, preparation process is simple, heat treatment temperature is low, light conversion plastic film for agricultural use can
With the blood orange light required for the ultraviolet light of 200~400nm is converted into plant, have wide in terms of greenhouse corps production
Application prospect.
Brief description of the drawings
Fig. 1 is calcined to 450 DEG C of XRD spectra for dissolved glue film
Fig. 2 is the fluorescence spectra of the dissolved glue film after heat treatment
Fig. 3 is the pellumina stereoscan photograph after calcining.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples, and it is right that certain following embodiments should not be construed as
Limitation of the invention.
The present invention provides a kind of rare-earth europium doped aluminium film, aluminum oxide in the rare-earth europium doped aluminium film
Molar content is 99.99~99.90mol%, and the molar content of europium ion is 0.01%~0.10%.In excitation wave
During a length of 200~400nm, there is obvious characteristic radiation at 610~620nm in the rare-earth europium doped aluminium film.
The present invention also provides a kind of agricultural light conversion agent, and the agricultural light conversion agent includes matrix material and is arranged at matrix
The rare-earth europium doped aluminium film of material surface.Matrix material is sheet glass or optical fiber.
The present invention further provides the preparation method of the agricultural light conversion agent, specifically follow the steps below：
Step one, boehmite sol is prepared, by aluminium isopropoxide grind into powder, according to rubbing for aluminium isopropoxide and deionized water
You are than being 1：100~1:200 weigh sample, aluminium isopropoxide are dividedly in some parts in 75 DEG C~95 DEG C deionized waters, the reaction time
It is 1.5h~2.5h, then evaporates unnecessary isopropanol in solution, after cooling, according to the mol ratio 1 of acid and aluminium isopropoxide：10
~3：10 add acid, and precipitation in 85 DEG C~95 DEG C refluxes, is sufficiently stirred for 12~16h, are clarified, homogeneous Bo Mu
Stone colloidal sol；
Step 2, the boehmite sol for preparing rare-earth europium doping, the europium nitrate aqueous solution is added in boehmite sol, is mixed
Miscellaneous europium ion molar content in alumina sol is 0.01%~0.1%, in 85 DEG C~95 DEG C refluxes, is fully stirred
12~18h is mixed, the boehmite sol of rare-earth europium doping is obtained；
Step 3, the aluminum oxide film for preparing rare-earth europium doping, using czochralski method, matrix material are immersed in colloidal sol,
Lift out with 4000 μm/s~6000 μm/s pull rate, when substrate material surface solution evaporates, matrix material is put into
In air dry oven, 8~15min is processed, be finally putting into Muffle furnace, 450 DEG C~500 DEG C, place are warming up to 3~10 DEG C/min
Reason 1.5h~3.5h, naturally cools to room temperature.
Embodiment 1
The deionized water for taking 148.5mL is heated to 90 DEG C in flask, and aluminium isopropoxide then is ground to form into even thickness
Powder, weighs 15.318g aluminium isopropoxides, is slowly added into the flask for filling deionized water in batches, in reflux, allows it
After being fully hydrolyzed 2h, remove reflux, continue to heat 1h, evaporate unnecessary isopropanol in solution, treat that it is cooled to room temperature
Afterwards, it is the nitric acid 22.5mL precipitations of 1mol/L to add concentration, is clarified, homogeneous boehmite sol；Measuring concentration is
0.0025mol/L europium nitrate solutions 15mL is added in boehmite sol, in 95 DEG C of reflux, is sufficiently stirred for 16h, is obtained
To the boehmite sol of rare-earth europium doping；Fibre cladding in the range of the section that plated film is needed on optical fiber is peeled off, with 5000 μm/
The pull rate lifting of s, starts plated film, and the optical fiber layer that will finally plate dissolved glue film is warmed up to 450 in Muffle furnace with 5 DEG C/min
DEG C heat treatment.Fig. 1 is the XRD spectrum of dissolved glue film, there it can be seen that the main component in film is γ phase aluminas.
Embodiment 2
The deionized water for taking 148.5mL is heated to 90 DEG C in flask, and aluminium isopropoxide then is ground to form into even thickness
Powder, weighs 16.850g aluminium isopropoxides, is slowly added into the flask for filling deionized water in batches, in reflux, allows it
After being fully hydrolyzed 2h, remove reflux, continue to heat 1h, evaporate unnecessary isopropanol in solution, treat that it is cooled to room temperature
Afterwards, it is the nitric acid 16.5mL precipitations of 1mol/L to add concentration, is clarified, homogeneous boehmite sol；Measuring concentration is
0.001mol/L europium nitrate solutions 24.75mL is added in boehmite sol, in 95 DEG C of reflux, is sufficiently stirred for 16h,
Obtain the boehmite sol of rare-earth europium doping；Glass substrate is cleaned by ultrasonic in hydrochloric acid, acetone, alcohol successively, nitrogen is then used
Air-blowing is done, and is lifted with the pull rate of 4000 μm/s, starts plated film, will finally plate the glass substrate of film in Muffle furnace with 10
DEG C/min is warming up to 450 DEG C of heat treatments.
Embodiment 3
The deionized water for taking 148.5mL is heated to 90 DEG C in flask, and aluminium isopropoxide then is ground to form into even thickness
Powder, weighs 8.425g aluminium isopropoxides, is slowly added into the flask for filling deionized water in batches, in reflux, allows it
It is fully hydrolyzed, after about 2h, removes reflux, continue to heat 1h, evaporate unnecessary isopropanol in solution, treats that it is cooled to
After room temperature, it is the nitric acid 12.4mL precipitations of 1mol/L to add concentration, is clarified, homogeneous boehmite sol；Measuring concentration is
0.001mol/L europium nitrate solutions 10.3mL is added in boehmite sol, in 95 DEG C of reflux, is sufficiently stirred for 16h, is obtained
To the boehmite sol of rare-earth europium doping；Glass substrate is cleaned by ultrasonic in hydrochloric acid, acetone, alcohol successively, nitrogen is then used
Drying, is lifted with 6000 μm/s pull rate, starts plated film, will finally plate dissolved glue film glass substrate in Muffle furnace with 3 DEG C/
Min is warming up to 450 DEG C of heat treatments.From figure 2 it can be seen that when excitation wavelength is 394nm, prepared rare-earth europium doping oxygen
Change aluminium film and occur obvious characteristic radiation at 614nm.
Embodiment 4
The deionized water for taking 148.5mL is heated to 85~90 DEG C in flask, and it is equal that aluminium isopropoxide then is ground to form into thickness
Even powder, weighs 15.318g aluminium isopropoxides, is slowly added into the flask for filling deionized water in batches, in reflux,
After allowing it to be fully hydrolyzed 2h, remove reflux, continue to heat 1h, evaporate unnecessary isopropanol in solution, treat that it is cooled to
After room temperature, it is the nitric acid 7.5mL precipitations of 1mol/L to add concentration, is clarified, homogeneous boehmite sol；Taking concentration is
0.0025mol/L europium nitrate solutions 7.5mL is added in boehmite sol, in 95 DEG C of reflux, is sufficiently stirred for 16h,
Obtain the boehmite sol of rare-earth europium doping；Glass substrate is cleaned by ultrasonic in hydrochloric acid, acetone, alcohol successively, nitrogen is then used
Air-blowing is done, and is lifted with the pull rate of 5000 μm/s, starts plated film, will finally plate the glass substrate of dissolved glue film in Muffle furnace
500 DEG C of heat treatments are warming up to 5 DEG C/min.Fig. 3 is the SEM spectrum of dissolved glue film.It can be seen that prepared dissolved glue film
Surface topography is than more uniform.
It should be noted that it will be understood by those within the art that, technical scheme can be carried out
Modification or equivalent, without deviating from the objective and scope of technical solution of the present invention, it all should cover will in right of the invention
Ask in the middle of scope.
Claims (10)
1. a kind of rare-earth europium doped aluminium film, it is characterised in that aluminum oxide in the rare-earth europium doped aluminium film
Molar content is 99.99~99.90%, and the molar content of europium ion is 0.01%~0.10%.
2. rare-earth europium doped aluminium film as claimed in claim 1, it is characterised in that in excitation wavelength be 200~400nm
When, there is obvious characteristic radiation at 610~620nm in the rare-earth europium doped aluminium film.
3. a kind of agricultural light conversion agent, it is characterised in that the agricultural light conversion agent includes matrix material and is arranged at the base
The rare-earth europium doped aluminium film of body material surface, the rare-earth europium doped aluminium film is described in claim 1 or 2
Rare-earth europium doped aluminium film.
4. the preparation method of agricultural light conversion agent as claimed in claim 3, it is characterised in that comprise the following steps：
Step one, prepare boehmite sol：Aluminium isopropoxide is added to the water and is sufficiently stirred for, hydrolyzed, be subsequently adding nitric acid, obtain vigorous
Nurse stone colloidal sol；
Step 2, the boehmite sol for preparing rare-earth europium doping：The europium nitrate aqueous solution is added to boehmite sol, 85 DEG C~
In 95 DEG C of refluxes, 12~18h is sufficiently stirred for, obtains the boehmite sol of rare-earth europium doping；
Step 3, the aluminum oxide film for preparing rare-earth europium doping：Using czochralski method, matrix material is immersed in rare-earth europium doping
Lift after 15~40s in boehmite sol, room temperature is naturally cooled to after Overheating Treatment, that is, obtain the agricultural light conversion agent.
5. preparation method as claimed in claim 4, it is characterised in that step one prepares concretely comprising the following steps for boehmite sol：
It is 1 according to the mol ratio of aluminium isopropoxide and deionized water by aluminium isopropoxide grind into powder：100~1:200 weigh sample, will
Aluminium isopropoxide is dividedly in some parts in 75 DEG C~95 DEG C deionized waters, is fully hydrolyzed, and the reaction time is 1.5h~2.5h, is then evaporated
Fall unnecessary isopropanol in solution, after cooling, according to the mol ratio 1 of acid and aluminium isopropoxide:10~3:10 add sour, precipitation,
In 85 DEG C~95 DEG C refluxes, 12~16h is sufficiently stirred for, is clarified, homogeneous boehmite sol.
6. preparation method as claimed in claim 4, it is characterised in that step 3 heat treatment is concretely comprised the following steps：Treat matrix material
When material surface solution evaporates, matrix material is put into air dry oven, processed 8~15 minutes, be finally putting into Muffle furnace, risen
Temperature processes 1.5h~3.5h to 450 DEG C~500 DEG C, naturally cools to room temperature.
7. preparation method as claimed in claim 4, it is characterised in that the concentration of the europium nitrate aqueous solution is 0.001 in step 2
~0.010mol/L.
8. preparation method as claimed in claim 4, it is characterised in that described matrix material is sheet glass or optical fiber.
9. preparation method as described in claim 4, it is characterised in that in step 3 pull rate be 4000~6000 μm/
s。
10. preparation method as described in claim 4, it is characterised in that with the liter of 3~10 DEG C/min in step 3 Muffle furnace
Warm speed is warming up to 450~500 DEG C.
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| CN201710076850.3A CN106893584A (en) | 2017-02-13 | 2017-02-13 | Rare-earth europium doped aluminium film and agricultural light conversion agent and preparation method thereof |
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|---|---|---|---|
| CN201710076850.3A CN106893584A (en) | 2017-02-13 | 2017-02-13 | Rare-earth europium doped aluminium film and agricultural light conversion agent and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021009144A1 (en) | 2019-07-12 | 2021-01-21 | Physee Group B.V. | Luminescent greenhouse glazing structures |
| WO2024023112A1 (en) | 2022-07-28 | 2024-02-01 | Agc Glass Europe | High visible light transmittance glazing |
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| CN102391860A (en) * | 2011-09-28 | 2012-03-28 | 陕西科技大学 | Rare earth europium-doped alumina fiber luminous material and preparation method thereof |
| CN103113885A (en) * | 2013-02-21 | 2013-05-22 | 北京化工大学 | Rare earth europium-doped aluminium oxide nano fiber luminescent material and preparation method thereof |
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2017
- 2017-02-13 CN CN201710076850.3A patent/CN106893584A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102391860A (en) * | 2011-09-28 | 2012-03-28 | 陕西科技大学 | Rare earth europium-doped alumina fiber luminous material and preparation method thereof |
| CN103113885A (en) * | 2013-02-21 | 2013-05-22 | 北京化工大学 | Rare earth europium-doped aluminium oxide nano fiber luminescent material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021009144A1 (en) | 2019-07-12 | 2021-01-21 | Physee Group B.V. | Luminescent greenhouse glazing structures |
| NL2023498B1 (en) | 2019-07-12 | 2021-02-04 | Physee Group B V | Optical structures comprising luminescent materials for plant growth optimization |
| WO2024023112A1 (en) | 2022-07-28 | 2024-02-01 | Agc Glass Europe | High visible light transmittance glazing |
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