CN107488451A - A kind of light conversion agent and preparation method thereof and agricultural red conversion film and preparation method thereof - Google Patents

A kind of light conversion agent and preparation method thereof and agricultural red conversion film and preparation method thereof Download PDF

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Publication number
CN107488451A
CN107488451A CN201710496965.8A CN201710496965A CN107488451A CN 107488451 A CN107488451 A CN 107488451A CN 201710496965 A CN201710496965 A CN 201710496965A CN 107488451 A CN107488451 A CN 107488451A
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light conversion
film
preparation
conversion agent
agent
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楼坚
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Zhejiang Zhe Technology Co Ltd
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Zhejiang Zhe Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
    • C09K11/664—Halogenides
    • C09K11/665—Halogenides with alkali or alkaline earth metals
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protecting plants
    • A01G13/02—Protective coverings for plants; Coverings for the ground; Devices for laying-out or removing coverings
    • A01G13/0256—Ground coverings
    • A01G13/0262—Mulches, i.e. covering material not-pre-formed in mats or sheets
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G9/00—Cultivation in receptacles, forcing-frames or greenhouses; Edging for beds, lawn or the like
    • A01G9/14—Greenhouses
    • A01G9/1438—Covering materials therefor; Materials for protective coverings used for soil and plants, e.g. films, canopies, tunnels or cloches
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/16—Halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/16—Halogen-containing compounds
    • C08K2003/166—Magnesium halide, e.g. magnesium chloride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2262—Oxides; Hydroxides of metals of manganese
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/267—Magnesium carbonate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
    • Y02A40/25—Greenhouse technology, e.g. cooling systems therefor

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Polymers & Plastics (AREA)
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  • General Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
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  • Protection Of Plants (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
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Abstract

The invention belongs to light conversion agent and film to turn light technical field.A kind of light conversion agent, chemical composition are：Mg7Ge2‑xO10F2:xMn4+, wherein x span is 0.01≤x≤0.3.The beneficial effects of the invention are as follows light conversion agent chemical stability is good, light conversion efficiency is high, service life length, available for producing agricultural feux rouges film.

Description

A kind of light conversion agent and preparation method thereof and agricultural red conversion film and preparation method thereof
Technical field
The invention belongs to light conversion agent and film to turn light technical field, turns more particularly to a kind of light conversion agent and with agricultural red Light film.
Background technology
According to the research of plant growth physiology, the sunshine of different wave length plays a different role to plant growth, its In growth of the short ultraviolet to plant have inhibitory action, the ultraviolet light less than 400nm regions is harmful to crop；Visible ray is green Plant carries out the energy source of photosynthesis manufacture organic substance, green plants Chlorophyll absorption it is most be blood orange light, secondly It is blue violet light, and to the minimum of yellowish green light absorbs；Fuel factor occurs for far infrared, the heat of crop growth is supplied, red Under the irradiation of outside line, the maturation of fruit can be made to reach unanimity, and near infrared ray is little to the use of crop.
According to the demand of plant growth, there are various agricultural conversion films in the market, and particularly agricultural red conversion film is deep Paid close attention to by orchard worker.For red conversion film, its core technology is the development and utilization of red light conversion agent.From current conversion film Preparation and application research situation from the point of view of, the light conversion agent for agricultural film can be largely classified into three major types：Organic dyestuff class light conversion agent, Inorganic salts light conversion agent and complex light conversion agent.(1) organic light conversion agents belong to organic matter, and its maximum feature is and canopy film basic tree The compatibility of fat is preferable, with its manufacture conversion film have concentration controllable, be uniformly dispersed, it is easy to process the characteristics of, meanwhile, such Light conversion agent is used for the self-strength and other physicochemical properties for not influenceing film during plastic sheeting, and this causes organic light conversion agents in agricultural film There is good using effect in.The major defect of organic light conversion agents is that oxygen easily occurs under long-time illumination for organic dyestuff Change and decompose, service life is shorter.In addition, turn that luminous intensity is relatively low, cost is high and also all limit such the defects of the color of itself The application of light conversion agent.In addition to these chemical factors, there is phenyl ring or condensed ring, degraded after use because fluorescent dye is most During exist it is potentially hazardous.(2) compared to organic compound, inorganic salts are cheap, easily prepared and storage, and resistance to height Warm nature can be good, and the application of inorganic salts light conversion agent is relatively broad.Common inorganic light conversion agent be mostly rare earth ion or heavy metal from Alkaline earth aluminate, oxide, sulfide, tungstates and silicate of son doping etc..It is and thin but the crystallinity of inorganic matter is higher The compatibility of film resin is poor, is difficult to disperse, and causes uniformity of film and light transmittance to decline, processing characteristics is poor.(3) rare earth has Machine light conversion agent is the complex using organic ligand complex rare-earth element, and the luminous and inorganic salt of rare earth of such complex lights Situation is similar, is all to carry out turning light using rare earth ion.However, because rare earth ion has abundant d or f unoccupied orbitals, Ligancy is higher (6~12), and ion cluster is easily formed when tenor is high, and fluorescent quenching phenomenon often occurs, thus to make The rare earth high polymer functional material for obtaining high fluorescent is relatively difficult.
The conventional inorganic salts light conversion agent of document report mainly has CaS:Eu2+、Sr2Si5N8:Eu2+、Ca2Si5N8:Eu2+、 CaAlSiN3:Eu2+、CaAl12O19:Mn4+、3.5MgO·0.05MgF2·GeO2:Mn4+、Y2O3:Eu3+、Gd2Mo3O9:Eu3+、 YV04:Eu3+And Y2O2S:Eu3+Deng wherein the poor chemical stability of sulfide-based light conversion agent, divalence Eu2+Doped nitride is red The preparation cost of light conversion agent is too high, trivalent Eu3+The absorption spectrum of the emission spectrum and chlorophyll that adulterate light conversion agent mismatches, and Mn4+The light conversion agent emission peak of doping is usually located at 650nm or so, is highly suitable for agricultural red conversion film.
The content of the invention
In order to overcome the short service life of organic light conversion agents in above-mentioned existing red conversion film, inorganic salts light conversion agent and film The shortcomings such as the compatibility of resin is poor, the fluorescence intensity of rare earth organic light conversion agents is low, it is an object of the present invention to provide one Kind light conversion agent that chemical stability is good, light conversion efficiency is high and preparation method thereof；Another object of the present invention is to provide make Agricultural red conversion film with above-mentioned light conversion agent and preparation method thereof.
To solve above-mentioned the deficiencies in the prior art, the technical solution adopted in the present invention is as follows：A kind of light conversion agent, chemical group Turn into：Mg7Ge2-xO10F2:xMn4+, wherein x span is 0.01≤x≤0.3.
A kind of light conversion agent preparation method, comprises the following steps：(1) with MgCO3、MgF2、GeO2And MnO2For raw material, according to Chemical formula Mg7Ge2-xO10F2:xMn4+Stoichiometric proportion weigh each raw material, wherein x span is 0.01≤x≤0.3； (2) it is well mixed after the raw material that step (1) obtains is fully ground in agate mortar；(3) mixture for obtaining step (2) Be put into corundum crucible, then by corundum crucible and mixture be put into together batch-type furnace carry out calcination, calcination temperature be 1200~ 1400 DEG C, calcination time is 4~6 hours, and sintering atmosphere is air, and sample is cooled to room temperature with stove after the completion of calcination, and taking-up obtains Obtain sintered body；(4) sintered body for obtaining step (3) carries out ball mill grinding, produces the light conversion agent.
Agricultural red conversion film, including film matrix and light conversion agent, the chemical composition of light conversion agent are：Ca3B5O10Cl:Eu2+。
Preferably, the film matrix composition is polyethylene, polyvinyl chloride, ethylene-vinyl acetate copolymer, polypropylene In one or more combination.
The preparation method of agricultural red conversion film, comprises the following steps：(1) prepared by light conversion master batch, claims by weight percentage Take light conversion agent 10~30%, film matrix resin 60~80%, other modified additives 0~20%, then at 150~200 DEG C It is well mixed, is finally extruded using comminutor, air-cooled granulation is fabricated to light conversion master batch in plasticator；(2) prepared by conversion film, by weight Amount percentage weighs light conversion master batch 1~10%, film base material 90~99%, is uniformly mixed in batch mixer, then It is sent into extruder, by the melting, plasticizing and extrusion of extruder, obtains agricultural red conversion film.
Preferably, described other modified additives be salicylic acid to tert-butyl benzene vinegar, 2, it is 6 BHTs, poly- One or more in ethylene waxes and erucyl amide.
Compared with prior art, the beneficial effects of the invention are as follows：(1) light conversion agent chemical stability provided by the invention it is good, Light conversion efficiency is high, service life length, available for producing agricultural feux rouges film；(2) conversion film provided by the invention can by 300~ 420nm purple light and black light and 450~500nm of part blue green light are converted to 600~680nm feux rouges, and it is launched Peak is located at 650nm or so, is advantageous to the absorption of chlorophyll a and chlorophyll b, can effectively facilitate the photosynthesis of plant.
Brief description of the drawings
Fig. 1 is light conversion agent excitation spectrum provided in an embodiment of the present invention and emission spectrum.
Embodiment
The present invention is described in further detail with reference to Figure of description 1 and specific embodiment.
Embodiment
A kind of light conversion agent, chemical composition are：Mg7Ge2-xO10F2:xMn4+, wherein x span is 0.01≤x≤0.3.
Light conversion agent preparation method comprises the following steps：(1) with high-purity MgCO3、MgF2、GeO2And MnO2For raw material, according to Chemical formula Mg7Ge2-xO10F2:xMn4+Stoichiometric proportion weigh each raw material, wherein x is 0.1；(2) original for obtaining step (1) Material is well mixed after being fully ground in agate mortar；(3) mixture that step (2) obtains is put into corundum crucible, then Corundum crucible and mixture are put into high temperature box furnace together and carry out calcination, calcination temperature is 1200~1400 DEG C, calcination time For 4~6 hours, sintering atmosphere was air, and sample is cooled to room temperature with stove after the completion of calcination, finally takes out and obtains sintered body；(4) The sintered body that step (3) is obtained carries out ball mill grinding, produces the light conversion agent.
Agricultural red conversion film, including film matrix and light conversion agent.Preparation method comprises the following steps：(1) light conversion master batch Prepare, weigh light conversion agent 10% by weight percentage, film matrix resin 80%, salicylic acid is to tert-butyl benzene vinegar 5%, 2,6 two Butylated Hydroxytoluene 5%, then it is well mixed in 150 DEG C of plasticator, is finally extruded using comminutor, air-cooled be granulated makes Into light conversion master batch；(2) prepared by conversion film, weighs light conversion master batch 1%, film base material 99%, in batch mixing by weight percentage It is uniformly mixed, is then fed into extruder in machine, by the melting, plasticizing and extrusion of extruder, obtains agricultural red turn Light film.
Dotted line is the light conversion agent excitation spectrum that embodiment 1 provides in Fig. 1, and solid line is light conversion agent emission spectrum.
Turn without using the romaine lettuce A of film plantation, the romaine lettuce B planted using commercial membrane and the agricultural red prepared using embodiment The romaine lettuce C of light film plantation carries out Growth of Lettuce index Test.Growth of Lettuce index dynamic measure explanation：Randomly select 20 plants of samples The close romaine lettuce of parameter, is repeated 3 times, and measurement romaine lettuce plant height, strain width, leaf are long, leaf width.Portion above and below the ground is first weighed after sampling Fresh weight, its dry weight is surveyed after then being dried to constant weight in 60 DEG C of baking ovens；Chlorophylls and Carotenoids assay uses spectrophotometric Method；Crude protein content measure uses Coomassie brilliant G-250 decoration method；Vc assays use AAS；Soluble sugar Assay uses anthrone colorimetry；Nitrate content measure uses ultraviolet spectrophotometry.Experiment is single factor design Scheme, mean except film difference or whether there is film, other condition is basically identical, if so these indexs there were significant differences, All it is as caused by the difference of film, number of days is after planting 40 days, test data table 1 below.
Table 1：
Turn without using the cucumber A of film plantation, the cucumber B planted using commercial membrane and the agricultural red prepared using embodiment The cucumber C of light film plantation carries out cucumber growth index Test.Growth of Lettuce index dynamic measure explanation：Randomly select 20 plants of samples The close romaine lettuce of parameter, is repeated 3 times.12 days after nursery, test data table 2 below.
Table 2：
Cucumber A Cucumber B Cucumber C
Photosynthetic rate [μm ol/ (m2*s)] 2.53±0.11 3.18±0.13 3.42±0.1
Transpiration rate [mol/ (m2*s)] 2.73±0.14 3.2±0.14 3.58±0.21
Leaf area (cm2) 37.47±0.29 41.1±0.81 42.72±1.51
Root long (cm) 19.33±2.14 18.76±2.88 19.08±2.24
Plant height (cm) 11.27±0.54 7.81±0.09 6.98±0.15
It can be seen that in small seedling stage, cucumber C seedling photosynthesis is stronger, and transpiration is equally also stronger.Due to cucumber A Illumination is not used, and seedling has certain excessive growth.

Claims (6)

1. a kind of light conversion agent, it is characterised in that chemical composition is：Mg7Ge2-xO10F2:xMn4+, wherein x span is 0.01 ≤x≤0.3。
2. a kind of light conversion agent preparation method, it is characterised in that comprise the following steps：(1) with MgCO3、MgF2、GeO2And MnO2For original Material, according to chemical formula Mg7Ge2-xO10F2:xMn4+Stoichiometric proportion weigh each raw material, wherein x span is 0.01≤x ≤0.3；(2) it is well mixed after the raw material that step (1) obtains is fully ground in agate mortar；(3) step (2) is obtained Mixture is put into corundum crucible, and corundum crucible and mixture are then put into batch-type furnace together carries out calcination, and calcination temperature is 1200~1400 DEG C, calcination time is 4~6 hours, and sintering atmosphere is air, and sample is cooled to room temperature with stove after the completion of calcination, Take out and obtain sintered body；(4) sintered body for obtaining step (3) carries out ball mill grinding, produces the light conversion agent.
3. agricultural red conversion film, including film matrix and light conversion agent, it is characterised in that the chemical composition of light conversion agent is： Mg7Ge2O10F2:Mn4+。
4. the agricultural red conversion film of one kind according to claim 3, it is characterised in that the film matrix composition is poly- second One or more combination in alkene, polyvinyl chloride, ethylene-vinyl acetate copolymer, polypropylene.
5. the preparation method of agricultural red conversion film, it is characterised in that red conversion film is as claimed in claim 3, preparation method bag Include following steps：(1) prepared by light conversion master batch, weighs light conversion agent 10~30% by weight percentage, and film matrix resin 60~ 80%, other modified additives 0~20%, then it is well mixed in 150~200 DEG C of plasticator, is finally squeezed using comminutor Go out, air-cooled granulation is fabricated to light conversion master batch；(2) prepared by conversion film, weighs light conversion master batch 1~10%, film by weight percentage Matrix material 90~99%, is uniformly mixed in batch mixer, is then fed into extruder, by the melting of extruder, modeling Change and extrude, obtain agricultural red conversion film.
6. the preparation method of agricultural red conversion film according to claim 5, it is characterised in that described other modifications help Agent is salicylic acid to the one or more in tert-butyl benzene vinegar, 2,6 BHTs, Tissuemat E and erucyl amide.
CN201710496965.8A 2017-06-26 2017-06-26 A kind of light conversion agent and preparation method thereof and agricultural red conversion film and preparation method thereof Pending CN107488451A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110028724A (en) * 2019-04-29 2019-07-19 威海海穗农业科技有限公司 A kind of film for agricultural use and method
CN111302315A (en) * 2020-03-16 2020-06-19 昆明学院 Preparation method and application of nitrogen-carbon-based light conversion agent, light conversion plastic film and preparation method thereof

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JP2011006501A (en) * 2009-06-23 2011-01-13 Tokyo Kagaku Kenkyusho:Kk Deep red phosphor
CN101948132A (en) * 2010-09-16 2011-01-19 青岛正杰实业有限公司 Simple process for preparing magnesium fluorogermanate: manganese red fluorescent powder
CN102848683A (en) * 2012-09-25 2013-01-02 天津市天塑科技集团有限公司第二塑料制品厂 Coating-type light conversion film and preparation method thereof
CN104312583A (en) * 2014-09-28 2015-01-28 彩虹集团电子股份有限公司 Preparation method of near ultraviolet excited red fluorescent powder for LEDs (light emitting diodes)
CN105295188A (en) * 2015-11-17 2016-02-03 佛山安亿纳米材料有限公司 Nitride red light conversion film and preparation method thereof
CN105385014A (en) * 2015-12-11 2016-03-09 华南农业大学 Light conversion agricultural film, and making method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011006501A (en) * 2009-06-23 2011-01-13 Tokyo Kagaku Kenkyusho:Kk Deep red phosphor
CN101948132A (en) * 2010-09-16 2011-01-19 青岛正杰实业有限公司 Simple process for preparing magnesium fluorogermanate: manganese red fluorescent powder
CN102848683A (en) * 2012-09-25 2013-01-02 天津市天塑科技集团有限公司第二塑料制品厂 Coating-type light conversion film and preparation method thereof
CN104312583A (en) * 2014-09-28 2015-01-28 彩虹集团电子股份有限公司 Preparation method of near ultraviolet excited red fluorescent powder for LEDs (light emitting diodes)
CN105295188A (en) * 2015-11-17 2016-02-03 佛山安亿纳米材料有限公司 Nitride red light conversion film and preparation method thereof
CN105385014A (en) * 2015-12-11 2016-03-09 华南农业大学 Light conversion agricultural film, and making method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110028724A (en) * 2019-04-29 2019-07-19 威海海穗农业科技有限公司 A kind of film for agricultural use and method
CN111302315A (en) * 2020-03-16 2020-06-19 昆明学院 Preparation method and application of nitrogen-carbon-based light conversion agent, light conversion plastic film and preparation method thereof

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