CN103805201A - Red electroluminescence material for detecting infrared laser and preparation method thereof - Google Patents
Red electroluminescence material for detecting infrared laser and preparation method thereof Download PDFInfo
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- CN103805201A CN103805201A CN201410044355.0A CN201410044355A CN103805201A CN 103805201 A CN103805201 A CN 103805201A CN 201410044355 A CN201410044355 A CN 201410044355A CN 103805201 A CN103805201 A CN 103805201A
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Abstract
The invention relates to a red electroluminescence material for detecting infrared laser and a preparation method thereof. The red electroluminescence material comprises a SeS base material, wherein activating agent containing Co, Ag, Ti acid compounds is added, sulfur is added, the materials are uniformly mixed to be sintered at a high temperature in a sulfur protective atmosphere to form a three-dimensional structural luminescence material, the material is washed by a mixed liquid of ammonium hydroxide and hydrogen peroxide and then is washed to be neutral by utilizing deionized water, and the material is dried by infrared; the transmitting spectrum of the infrared laser detection red luminescence material is 590nm to 630nm, the infrared laser intensity of an infrared electroluminescence detector is in inverse relation with the working current of the luminescence material, the prepared infrared electroluminescence detector can be used for qualitatively and quantitatively detecting, tracking, correcting and recognizing invisible near-infrared ray, and the red electroluminescence material can be widely applied to the fields such as near-infrared laser detection, medical diagnosis and the like.
Description
Technical field
The invention belongs to infrared laser detecting and luminescent material applied technical field.
Background technology
Infrared laser is conventional product in the field such as industrial, medical, military, cannot directly observe feature, so the detection of infrared light is highlighted to practical application meaning because infrared light has human visual system.It is mainly by up-conversion luminescence or infrared quencher technology that existing use luminescent material is surveyed infrared light technology, has realized the detection of near infrared light, and its shortcoming is to survey infrared light with photoluminescence, and it cannot directly quantize and measure the power of infrared light.
Known up-conversion luminescent material, electron capture luminous material is mainly the rare earth doped activator such as rare earth fluorine and strontium sulfide calcium, it absorbs after near-ir energy, produce luminous, Chinese patent 85100247, Chinese patent 01142151.7, Chinese patent 96122293.X, Chinese patent 01138927.3, Chinese patent 01138920.6, Chinese patent 200710023804.3, Chinese patent 200610103418.0, US5541012, US7648648 is to this existing announcement
.
With ZnS, SeS is that the luminescent material of matrix is the luminescent material of common widespread use, as: electroluminescent material, CRT luminescent material etc., conventionally near infrared light luminously has a serious quenching effect to it, in same ZnS substrate material, add and contain Pb, Cu activator, after high temperature sintering, prepare electron capture luminous material, under infrared rays 800-2000nm excitation, produce green or orange luminescence, above Chinese patent 2013100020759, 96121255.1, 96247084.8, 201010214340.6, 201010214358.6 existing explanation, they all can only qualitative identification infrared light, cannot realize quantitative identification.
A kind of red electroluminescent materials and preparation of surveying infrared laser of the present invention, it comprises SeS substrate material, wherein add the luminescent material of the activator that contains Co, Ag, Tl acidic cpd, it is prepared into after device, can be for invisible near infrared light being realized to detection, tracking, check and correction, the identification of qualitative, quantitative, can be widely used in the multidisciplinary technical fields such as near-infrared laser detection, medical diagnosis, laser facula demonstration, optical information storage.
Summary of the invention
A kind of red electroluminescent materials and preparation of surveying infrared laser, it comprises SeS substrate material, wherein add the activator that contains Co, Ag, Tl acidic cpd, add sulphur, and evenly mix, in the protective atmosphere of sulphur, high temperature sintering becomes cube phase structure luminescent material, uses the mixed solution of ammoniacal liquor and hydrogen peroxide to clean, re-use washed with de-ionized water to neutral, infrared drying; This infrared laser detecting red illuminating material emmission spectrum is at 590-630nm, the infrared electroluminescent detector being prepared into, infrared laser intensity and the luminescent material working current relation that is inversely proportional to.
Luminescent material take zinc sulphide as matrix, common activator is Cu, Ag etc., and its common quencher is Co, Fe, Ni, and especially in existing electroluminescent material, Co, Fe, Ni are the important factors of infringement luminescent properties, in the present invention, the appropriate Co content of controlling, uses Tl to compensate luminous loss.
In the every gram weight of substrate material in the present invention, the concentration of adding dominant activator Co is 5X10
-3-1X10
-2, the concentration of Ag is 1X10
-2-5X10
-2, the concentration of Tl is 7X10
-5-1X10
-3.The present invention should strictly control Co mates concentration with Tl, otherwise will be without infrared cancellation or electroluminescent.In substrate material, can add auxiliary activator, bright voltage is initially opened in its work that can effectively reduce luminescent material, and in the every gram weight of substrate material, the concentration of adding auxiliary activator In is 1X10
-5-1X10
-3, or the concentration of Ga is 1X10
-5-1X10
-3.
High temperature sintering temperature in the protective atmosphere of sulphur in the present invention is at 600-800 degree, sintering time 8-12 hour, and luminescent material granularity 3-7 micron, powder crystal structure is in Emission in Cubic.Take selenium sulfide as main luminescent material system, its powder crystal is main mainly with high temperature hexagonal phase, and in the present invention, the existence of a large amount of hexagonal phases can improve electroluminescent intensity, damages the sensitivity of infrared reaction.The phase point temperature of known conventional selenium sulfide is near 1000 degree, and therefore the long-time sintering of low temperature is conducive to the formation of Emission in Cubic.But temperature is unfavorable for luminescent material particle growth when too low.
Luminescent material after sintering, then the 5-10 hour that anneals under temperature 250-350 degree, can effectively improve infrared acquisition sensitivity range.
Activator acidic cpd in the present invention is: sulphate, nitrate compound, halogenide, acetic acid compound.Activator is that acidic cpd is conducive to and the association reaction of selenium sulfide.
The preparation of the infrared laser detecting red illuminating material in the present invention, 3 times repeatedly, the mixed liquid dipping luminescent material of the use ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration 1 hour, re-uses washed with de-ionized water to neutral.In mixed solution, add carbonic acid ammonia, ammonia chloride to be conducive to clean, by carbonic acid ammonia, the mixed solution that adds the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration after water dissolution for ammonia chloride.
In the present invention, in substrate material, add ZnS, the spectrum that can not affect luminescent material obviously changes, and in the every gram weight of substrate material, can add ZnS material 0.5-1 gram.
A kind of infrared laser detecting red illuminating material of the present invention, use the electroluminescent device technology of preparing after improving, prepare infrared eye, it is at AC110V-220V, under frequency 50-400 hertz, produce emitting red light, emmission spectrum is at 590-630nm, in the time of infrared band 0.7-4 micron rayed, electroluminescent is quenched, its current draw is changed, ir radiation is stronger, electroluminescent is more weak, current draw is fewer, infrared laser intensity and the luminescent material working current relation that is inversely proportional to, by the curent change of measuring element, derive the exposure intensity of infrared source.
Luminescent material prepared by the present invention has faint light photoluminescence under ultraviolet ray, and electroluminescent is also weaker than the electroluminescent material that sell existing market, but it has sensitive infrared acquisition.
Embodiment
A kind of red electroluminescent materials and preparation of surveying infrared laser, it comprises substrate material SeS, wherein add the activator that contains Co, Ag, Tl acidic cpd, add sulphur, and evenly mix, in the protective atmosphere of sulphur, high temperature sintering becomes cube phase structure luminescent material, uses the mixed solution of ammoniacal liquor and hydrogen peroxide to clean, re-use washed with de-ionized water to neutral, infrared drying; This infrared laser detecting red illuminating material emmission spectrum is at 590-630nm, the infrared electroluminescent detector being prepared into, infrared laser intensity and the luminescent material working current relation that is inversely proportional to.
In the every gram weight of substrate material in the present invention, the concentration of adding dominant activator Co is 5X10
-3-1X10
-2, the concentration of Ag is 1X10
-2-5X10
-2, the concentration of Tl is 7X10
-5-1X10
-3.In substrate material, add the activator of strict ratio simultaneously, and full and uniform mixing.Auxiliary activator can effectively reduce the work of luminescent material and initially open bright voltage 30%, and in the every gram weight of substrate material, the concentration of adding auxiliary activator In is 1X10
-5-1X10
-3, or the concentration of Ga is 1X10
-5-1X10
-3.
High temperature sintering temperature in the protective atmosphere of sulphur in the present invention is at 600-800 degree, sintering time 8-12 hour, and luminescent material granularity 3-7 micron, powder crystal structure is in Emission in Cubic.Sintering can use tubular type electric heater or the box circuit of sealing, wherein adds the sulphur of 10-30% to do protective atmosphere, does not make selenium sulfide oxidation.5-10 hour again anneals under temperature 250-350 degree.
Activator acidic cpd in the present invention is: sulphate, nitrate compound, halogenide, acetic acid compound, use sulfuric acid, nitric acid, hydrochloric acid, acetic acid etc., as be prepared into Silver Nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, thallium trinitrate (TTN), rose vitriol, thallic sulfate, gallium nitrate, indium nitrate, they add in selenium sulfide with solution form, can easily be uniformly dispersed, as: make water regulate zinc sulphide pasty state state, add again Silver Nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, thallium trinitrate (TTN), uniform stirring, 120 degree are dry, add SULPHUR POWDER to grind.In the present invention, do not add solubility promoter, solubility promoter can improve granularity, reduces infrared sensitivity.
The preparation of the infrared laser detecting red illuminating material in the present invention, 3 times repeatedly, the mixed liquid dipping luminescent material of the use ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration 1 hour, re-uses washed with de-ionized water to neutral.Ammoniacal liquor and hydrogen peroxide are processed luminescent material, can make unnecessary dissolved the cleaning up of activator in luminescent material surface, are conducive to the raising of electroluminescent efficiency.
In mixed solution, add carbonic acid ammonia, ammonia chloride to be conducive to clean, by carbonic acid ammonia, the mixed solution that adds the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration after water dissolution for ammonia chloride.Conventionally carbonic acid ammonia, ammonia chloride add-on are total solution weight 10%.Concentration can regulate by water.Can there is vigorous reaction in the silver on mixed solution and luminescent material surface, cobalt, thallium ion, form red-hot blue liquid, pouring liquids after question response completes, 3 times repeatedly.
Re-use deionized water luminescent material is washed to neutrality repeatedly, clean to the long lifetime work that neutrality is conducive to luminescent material, finally dry at 120 degree.
In the present invention, in substrate material, add a small amount of ZnS, the spectrum that can not affect luminescent material obviously changes, and in the every gram weight of substrate material, can add ZnS material 0.5-1 gram.
A kind of red electroluminescent materials of surveying infrared laser of the present invention, use the electroluminescent device technology of preparing after improving, prepare infrared eye, it produces emitting red light at AC110V-220V under frequency 50-400 hertz, and emmission spectrum is at 590-630nm, survey infrared band 0.7-4 micron, infrared laser intensity and the luminescent material working current relation that is inversely proportional to, by the curent change of measuring element, derives the exposure intensity of infrared source.
In the present invention luminescent device use driving mechanism for the common product of market sale as: DH10-220, DH100-12-TB etc., the current measurement table using in the present invention is conventional volt ohm-milliammeter.
the invention has the advantages that
1, a kind of red electroluminescent materials and preparation of surveying infrared laser of the present invention, it is prepared into device, can under infrared rays 700-4000nm excitation, produce alternately variation luminous and cancellation, can determine infrared light intensity by current measurement.It can directly change infrared signal into electrical signal simultaneously.
2, the luminescent material that prepared by the present invention has satisfactory stability, and serious moisture decomposing phenomenon can not occur, and be the more than 5 times of photoluminescence infrared detecting materials work-ing life.It is life-time service out of doors, automatically controls, and especially the irradiation of infrared laser is quick on the draw, as the infrared laser detecting to 1.06 microns.
3, SeS luminescent material is common electroluminescent material, long afterglow luminous material, CRT luminescent material, and near infrared light has serious quenching effect to it, and the present invention has changed above-mentioned disadvantageous effect, has expanded material application system scope.Its infrared acquisition scope near infrared, in infrared, the monitoring to infrared laser in adaptable industry, military affairs, medical science, scientific research field.
Luminescent material of the present invention can be for surveying, follow the tracks of, proofread, identify invisible near infrared light.Can be widely used in the multidisciplinary technical fields such as near-infrared laser detection, laser facula demonstration, opticfiber communication indication, optical information storage, image processing, infrared imaging, as: conventional infrared LED telepilot, YAG laser cutter, 1550nm opticfiber communication etc. in household electrical appliances.
embodiment 1
Get 1000 grams of SeS substrate materials, add Cobaltous diacetate, relatively in every gram of substrate material, add Co content 1X10
-3; Add Silver Nitrate, relatively in every gram of substrate material, add Ag content 2X10
-2; Add thallium trinitrate (TTN), relatively in every gram of substrate material, add Tl content 1X10
-4; Add water to regulate pasty state, add 20 grams of sulphur, 120 degree are dried.Above-mentioned powder adds 3% sulphur to grind evenly again.Dry material is packed in alumina crucible, seal; Sintering 10 hours in 750 degree electric furnaces, takes out cooling crush, then anneals 8 hours under temperature 300 degree.
In beaker, configure 10 liters of the mixed solutions of the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration, soak luminescent material 1 hour, remove the liquid that reacts, 3 times repeatedly, re-use washed with de-ionized water to neutral, and 120 degree are dry.
embodiment 2
Get 100 grams of SeS materials, get 50 grams of ZnS materials, two kinds of substrate material mixed grindings are even, add Cobaltous diacetate, relatively in every gram of substrate material, add Co content 1X10
-2; Add silver chloride, relatively in every gram of substrate material, add Ag content 5X10
-2; Add thallium trinitrate (TTN), relatively in every gram of substrate material, add Tl content 1X10
-3; Add water to regulate pasty state, add 4 grams of sulphur, 120 degree are dried.Above-mentioned powder adds 3% sulphur to grind evenly again.Dry material is packed in silica tube, seal; Sintering 8 hours in 800 degree electric furnaces, takes out cooling crush, then anneals 10 hours under temperature 300 degree.
1 liter of the mixed solution that configures the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration in beaker adds carbonic acid ammonia to add 50 grams simultaneously, and ammonia chloride adds 50 grams, micro-heating for dissolving.Soak luminescent material 1 hour, remove the liquid that reacts, 3 times repeatedly, re-use washed with de-ionized water to neutral, and 120 degree are dry.
embodiment 3
Get 500 grams of SeS substrate materials, add Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, relatively in every gram of substrate material, add Co content 2X10
-3; Add Silver monoacetate, relatively in every gram of substrate material, add Ag content 3X10
-2; Add thaliium acetate, relatively in every gram of substrate material, add Tl content 3X10
-4; Relatively in every gram of substrate material, add In content 1X10
-4, add water to regulate pasty state, add 40 grams of sulphur, 120 degree are dried.Above-mentioned powder adds 3% sulphur to grind evenly again.Dry material is packed in alumina crucible, seal; Sintering 10 hours in 750 degree electric furnaces, takes out cooling crush, then anneals 8 hours under temperature 300 degree.
In beaker, configure 5 liters of the mixed solutions of the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration, soak luminescent material 1 hour, remove the liquid that reacts, 3 times repeatedly, re-use washed with de-ionized water to neutral, and 120 degree are dry.
After having done to illustrate for the good embodiment of the present invention in the above, it should be understood that to one skilled in the art, without departing from the spirit and scope of the present invention in the situation that, any changes and improvements made for the present invention all within the scope of the invention.
Claims (9)
1. survey red electroluminescent materials and the preparation of infrared laser for one kind, it comprises SeS substrate material, wherein add the activator that contains Co, Ag, Tl acidic cpd, add sulphur, and evenly mix, in the protective atmosphere of sulphur, high temperature sintering becomes cube phase structure luminescent material, uses the mixed solution of ammoniacal liquor and hydrogen peroxide to clean, re-use washed with de-ionized water to neutral, infrared drying; This infrared laser detecting red illuminating material emmission spectrum is at 590-630nm, the infrared electroluminescent detector being prepared into, infrared laser intensity and the luminescent material working current relation that is inversely proportional to.
2. a kind of red electroluminescent materials and preparation of surveying infrared laser as claimed in claim 1, in the every gram weight of substrate material, the concentration of adding dominant activator Co is 5X10
-3-1X10
-2, the concentration of Ag is 1X10
-2-5X10
-2, the concentration of Tl is 7X10
-5-1X10
-3.
3. a kind of red electroluminescent materials and preparation of surveying infrared laser as claimed in claim 1; in the protective atmosphere of sulphur, high temperature sintering temperature is at 600-800 degree; sintering time 8-12 hour, luminescent material granularity 3-7 micron, powder crystal structure is in Emission in Cubic.
4. a kind of red electroluminescent materials and preparation of surveying infrared laser as claimed in claim 1, acidic cpd is: sulphate, nitrate compound, halogenide, acetic acid compound.
5. a kind of red electroluminescent materials and preparation of surveying infrared laser as claimed in claim 1, luminescent material after sintering, use the ammoniacal liquor of 15% concentration and the hydrogen peroxide mixed liquid dipping luminescent material of 20% concentration 1 hour, 3 times repeatedly, re-use washed with de-ionized water to neutral.
6. a kind of red electroluminescent materials and preparation of surveying infrared laser as claimed in claim 1, adds carbonic acid ammonia, ammonia chloride in mixed solution, after dissolving, cleans 3 times.
7. a kind of red electroluminescent materials and preparation of surveying infrared laser as claimed in claim 1, the luminescent material after sintering, then the 5-10 hour that anneals under temperature 250-350 degree.
8. a kind of red electroluminescent materials and preparation of surveying infrared laser as claimed in claim 1, in the every gram weight of substrate material, the concentration of adding auxiliary activator In is 1X10
-5-1X10
-3, or the concentration of Ga is 1X10
-5-1X10
-3.
9. a kind of red electroluminescent materials and preparation of surveying infrared laser as claimed in claim 1 adds ZnS in substrate material, in the every gram weight of substrate material, adds ZnS material 0.5-1 gram.
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| CN103805201B CN103805201B (en) | 2015-08-12 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57202373A (en) * | 1981-06-05 | 1982-12-11 | Hitachi Ltd | Sulfide fluorescent substance |
| JPS59202284A (en) * | 1983-05-02 | 1984-11-16 | Kasei Optonix Co Ltd | Fluophor having long afterglow |
| CN1324912A (en) * | 2000-05-19 | 2001-12-05 | 中国科学院长春光学精密机械与物理研究所 | Fluorescnet material to convert and combine blue light of LED into white light |
| CN101030626A (en) * | 2006-03-03 | 2007-09-05 | 株式会社半导体能源研究所 | Light-emitting element, light-emitting device, and electronic device |
-
2014
- 2014-02-05 CN CN201410044355.0A patent/CN103805201B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57202373A (en) * | 1981-06-05 | 1982-12-11 | Hitachi Ltd | Sulfide fluorescent substance |
| JPS59202284A (en) * | 1983-05-02 | 1984-11-16 | Kasei Optonix Co Ltd | Fluophor having long afterglow |
| CN1324912A (en) * | 2000-05-19 | 2001-12-05 | 中国科学院长春光学精密机械与物理研究所 | Fluorescnet material to convert and combine blue light of LED into white light |
| CN101030626A (en) * | 2006-03-03 | 2007-09-05 | 株式会社半导体能源研究所 | Light-emitting element, light-emitting device, and electronic device |
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Address after: 201619 Pudong New Area Road, Shanghai, Lane Lane No. 999 3-901 Applicant after: Shanghai Keyan Phosphor Technology Co., Ltd. Address before: 201619, No. 8, 8 boat Road, Jing Jing Town, Songjiang District, Shanghai Applicant before: Shanghai Keyan Phosphor Technology Co., Ltd. |
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