CN103756672A - Green luminous material for detecting infrared laser and preparation - Google Patents
Green luminous material for detecting infrared laser and preparation Download PDFInfo
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- CN103756672A CN103756672A CN201410044353.1A CN201410044353A CN103756672A CN 103756672 A CN103756672 A CN 103756672A CN 201410044353 A CN201410044353 A CN 201410044353A CN 103756672 A CN103756672 A CN 103756672A
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- luminescent material
- infrared laser
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Abstract
The invention discloses a green luminous material for detecting infrared laser and preparation. The green luminous material comprises a ZnS substrate material, and is prepared through the following steps: adding an activator containing Co, Cu and Tl acid compounds, and adding sulfur for uniform mixing, performing high-temperature sintering in a sulfur protection atmosphere to form a luminous material with a cubic phase structure, washing the luminous material by using a mixed solution of ammonia water and hydrogen peroxide, washing by using de-ionized water until the mixed solution is neutral, and performing infrared drying, wherein the green luminous material for detecting the infrared laser has emission spectrums of 520 to 540 nm, and can be used for preparing an infrared electroluminescent detector. The green luminous material can be used for the qualitative and quantitative detection, tracking, correction and identification of invisible near infrared light, and can be widely applied to a plurality of technical fields of near infrared laser detection, laser spot display, optical information storage, 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 are 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 is to this existing announcement
.
The luminescent material that the ZnS of take is matrix is the luminescent material of common widespread use, as: electroluminescent material, long afterglow luminous 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 96121255.1, 96247084.8, 201010214340.6, 201010214358.6, 2013100020759 existing explanations, they all can only qualitative identification infrared light, cannot realize quantitative value identification.
A kind of green luminescent material and preparation of surveying infrared laser of the present invention, it comprises ZnS substrate material, wherein add the luminescent material of the activator that contains Co, Cu, Tl acidic cpd, it is prepared into after device, can, 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, laser facula demonstration, optical information storage.
Summary of the invention
A kind of preparation of infrared laser detecting green luminescent material, it comprises ZnS substrate material, wherein add the activator that contains Co, Cu, Tl acidic cpd, add sulphur, and evenly mix, in the protective atmosphere of sulphur, high temperature sintering becomes complete 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 green luminescent material emmission spectrum is at 520-540nm, the infrared electroluminescent detector being prepared into, infrared laser intensity and the luminescent material working current relation that is inversely proportional to.
The luminescent material that the zinc sulphide of take is 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, is used 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 Cu 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 zinc sulphide as main luminescent material system, and its powder crystal is main mainly with 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 zinc sulphide is near 1040 degree, so 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 the association reaction with zinc sulphide.
The green luminescent material of the detection infrared laser in the present invention, the mixed liquid dipping luminescent material of the use ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration 1 hour, 3 times repeatedly, 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.
A kind of infrared laser detecting green luminescent 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 green emitting, emmission spectrum is at 520-540nm, when 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 green luminescent material and preparation of surveying infrared laser, it comprises ZnS substrate material, wherein add the activator that contains Co, Cu, 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 green luminescent material emmission spectrum is at 520-540nm, 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 Cu 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 be used tubular type electric heater or the box circuit of sealing, wherein adds the sulphur of 10-30% to do protective atmosphere, does not make zinc sulphide 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 cupric nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, thallium trinitrate (TTN), copper sulfate, rose vitriol, thallic sulfate, gallium nitrate, indium nitrate, they add in zinc sulphide with solution form, can easily be uniformly dispersed, as: make water regulate zinc sulphide pasty state state, add again cupric 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 green luminescent material preparation of the detection infrared laser in the present invention, the mixed liquid dipping luminescent material of the use ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration 1 hour, 3 times repeatedly, 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 copper 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.
A kind of green luminescent material and preparation of surveying infrared laser of the present invention, use the electroluminescent device technology of preparing after improving, prepare infrared eye, it produces green emitting at AC110V-220V under frequency 50-400 hertz, and emmission spectrum is at 520-540nm, 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.
The driving mechanism that in the present invention, luminescent device is used 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 preparation for infrared laser detecting green luminescent material of the present invention, it is prepared into device, can under infrared rays 700-4000nm excitation, produce alternately variation luminous and cancellation, by current measurement, can determine infrared light intensity.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, ZnS 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.
Electron capture luminous 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 ZnS substrate materials, add Cobaltous diacetate, relatively in every gram of substrate material, add Co content 1X10
-3; Add copper sulfate, relatively in every gram of substrate material, add Cu 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; In 750 degree electric furnaces, sintering is 10 hours, 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 ZnS substrate materials, add Cobaltous diacetate, relatively in every gram of substrate material, add Co content 1X10
-2; Add cupric chloride, relatively in every gram of substrate material, add Cu 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 3 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; In 800 degree electric furnaces, sintering is 8 hours, 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 ZnS substrate materials, add Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, relatively in every gram of substrate material, add Co content 2X10
-3; Add neutralized verdigris, relatively in every gram of substrate material, add Cu content 3X10
-2; Add thaliium acetate, relatively in every gram of substrate material, add Tl content 3X10
-4; Add indium acetate, 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; In 750 degree electric furnaces, sintering is 10 hours, 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 (8)
1. green luminescent material and a preparation of surveying infrared laser, it comprises ZnS substrate material, wherein add the activator that contains Co, Cu, 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 green luminescent material emmission spectrum is at 520-540nm, 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 green luminescent material 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 Cu is 1X10
-2-5X10
-2, the concentration of Tl is 7X10
-5-1X10
-3.
3. a kind of green luminescent material and preparation of surveying infrared laser as claimed in claim 1, in the protective atmosphere of sulphur high temperature sintering temperature 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 green luminescent material 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 green luminescent material 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 green luminescent material 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 green luminescent material 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 green luminescent material 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.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458003A (en) * | 2014-11-24 | 2015-03-25 | 杭州电子科技大学 | Infrared radiation detection method |
| CN106634971A (en) * | 2016-10-09 | 2017-05-10 | 上海洞舟实业有限公司 | Preparation of high-sensitivity X-ray detection luminescent material |
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| CN101870867A (en) * | 2010-06-29 | 2010-10-27 | 上海科炎光电技术有限公司 | Sulphide electron capture luminous material |
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2014
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Patent Citations (4)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458003A (en) * | 2014-11-24 | 2015-03-25 | 杭州电子科技大学 | Infrared radiation detection method |
| CN104458003B (en) * | 2014-11-24 | 2017-10-27 | 杭州电子科技大学 | One kind detection infra-red radiation method |
| CN106634971A (en) * | 2016-10-09 | 2017-05-10 | 上海洞舟实业有限公司 | Preparation of high-sensitivity X-ray detection luminescent material |
| CN106634971B (en) * | 2016-10-09 | 2019-04-05 | 上海洞舟实业有限公司 | A kind of highly sensitive X-ray detection luminescent material preparation |
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