CN103756673B - Blue luminescent material for infrared laser detection and preparation method - Google Patents
Blue luminescent material for infrared laser detection and preparation method Download PDFInfo
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- CN103756673B CN103756673B CN201410044354.6A CN201410044354A CN103756673B CN 103756673 B CN103756673 B CN 103756673B CN 201410044354 A CN201410044354 A CN 201410044354A CN 103756673 B CN103756673 B CN 103756673B
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Abstract
The invention discloses a blue luminescent material for infrared laser detection and a preparation method. The blue luminescent material comprises a ZnS substrate material. The preparation method comprises the following steps: adding an activating agent containing Co, Ag and Tl acid compounds; adding sulfur; uniformly mixing; sintering into a luminescent material having a cubic phase structure at high temperature under a sulfur protective atmosphere; washing with mixed liquid of ammonium hydroxide and hydrogen peroxide; washing to neutrality with deionized water; and drying with infrared rays. The emission spectrum of the blue luminescent material for infrared laser detection is 430-470 nm; an infrared electroluminescent detector prepared through the blue luminescent material has the infrared laser intensity which is inversely proportional to the working current of the luminescent material. The blue luminescent material can be applied to qualitative and quantitative detection, tracking, calibration and identification for invisible near-infrared light and can be widely applied to the fields such as near-infrared laser detection, biological diagnosis and medical monitoring.
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, directly cannot observe feature, so highlight practical application meaning to the detection of infrared light because infrared light has human visual system.Existing use luminescent material detection infrared light technology, mainly by up-conversion luminescence or infrared quenching technique, has achieved the detection of near infrared light, and its shortcoming is that it directly cannot quantize and measure the power of infrared light with photoluminescence detection 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, after it absorbs 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
.
The luminescent material of the most common widespread use that to take ZnS as the luminescent material of matrix be, as: electroluminescent material, long afterglow luminous material, CRT luminescent material etc., usual near infrared light has serious quenching effect to its luminescence, in same ZnS substrate material, add containing Pb, Cu activator, electron capture luminous material is prepared after high temperature sintering, green or orange luminescence is produced under infrared rays 800-2000nm encourages, above Chinese patent 96121255.1, 96247084.8, 201010214340.6, 201010214358.6, 2013100020759 existing explanations, they all can only qualitative recognition infrared light, quantitative judge cannot be realized.
A kind of blue emitting material for infrared laser detecting of the present invention and preparation, it comprises ZnS substrate material, wherein add the luminescent material of the activator containing Co, Ag, Tl acidic cpd, after it is prepared into device, may be used for realizing the detection of qualitative, quantitative, tracking, check and correction, identification to invisible near infrared light, the multidisciplinary technical fields such as near-infrared laser detection, biological diagnosis, clinical disease detection, laser facula display, optical information storage can be widely used in.
Summary of the invention
A kind of blue emitting material for infrared laser detecting and preparation, it comprises ZnS substrate material, wherein add the activator containing Co, Ag, Tl acidic cpd, add sulphur, and Homogeneous phase mixing, 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 blue emitting material emmission spectrum is at 440-470nm, and the infrared electroluminescent detector be prepared into, infrared laser intensity and luminescent material working current are inversely.
Take zinc sulphide as the luminescent material of 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, appropriate control Co content in the present invention, 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 strictly should mate concentration by control Co and Tl, otherwise will without infrared cancellation or electroluminescent.Can add auxiliary activator in substrate material, bright voltage is initially opened in its work that effectively can 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, and sintering time 8-12 hour, luminescent material grains degree 3-7 micron, powder crystal structure is in Emission in Cubic.Luminescent material system based on zinc sulphide, its powder crystal is main mainly with hexagonal phase, and in the present invention, the existence of a large amount of hexagonal phase can improve electroluminescent intensity, damages the sensitivity of infrared reaction.The phase point temperature of known conventional zinc sulphide is near 1040 degree, and therefore low temperature sinters the formation being conducive to Emission in Cubic for a long time.But temperature is unfavorable for that luminescent material grains grows time 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 preparation of the infrared laser detecting blue emitting material in the present invention, uses the mixed liquid dipping luminescent material 1 hour of the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration, 3 times repeatedly, re-uses washed with de-ionized water to neutral.Add carbonic acid ammonia in mixed solution, ammonia chloride be conducive to cleaning, the mixed solution of the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration will be added after carbonic acid ammonia, ammonia chloride water dissolution.
A kind of blue emitting material for infrared laser detecting of the present invention and preparation, use the electroluminescent device technology of preparing after improving, prepare infrared eye, it is at AC110V-220V, blue-light-emitting is produced under frequency 50-400 hertz, emmission spectrum is at 440-470nm, 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 luminescent material working current are inversely, 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 light, and electroluminescent is also weaker than the electroluminescent material that existing market is sold, but it has sensitive infrared acquisition.
Embodiment
A kind of blue emitting material for infrared laser detecting and preparation, it comprises ZnS substrate material, wherein add the activator containing Co, Ag, Tl acidic cpd, add sulphur, and Homogeneous phase mixing, 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 blue emitting material emmission spectrum is at 440-470nm, and the infrared electroluminescent detector be prepared into, infrared laser intensity and luminescent material working current are inversely.
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.Add the activator of strict ratio in substrate material simultaneously, and full and uniform mixing.Bright voltage 30% is initially opened in the work that auxiliary activator effectively can 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, and sintering time 8-12 hour, luminescent material grains degree 3-7 micron, powder crystal structure is in Emission in Cubic.Sintering can use closed tubular type electric heater or box circuit, and the sulphur wherein adding 10-30% does protective atmosphere, does not make zinc sulphide be oxidized.Anneal 5-10 hour again 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 being 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 zinc sulphide in the form of a solution, can easily be uniformly dispersed, as: make water use regulation zinc sulphide paste state, add Silver Nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, thallium trinitrate (TTN) again, uniform stirring, 120 degree dry, adds SULPHUR POWDER grinding.Do not add solubility promoter in the present invention, solubility promoter can improve granularity, reduces infrared sensitivity.
The preparation of the infrared laser detecting blue emitting material in the present invention, 3 times repeatedly, uses the mixed liquid dipping luminescent material 1 hour of the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration, re-uses washed with de-ionized water to neutral.Ammoniacal liquor and hydrogen peroxide process luminescent material, can make the activator of luminescent material excess surface be cleaned up by dissolving, be conducive to the raising of electroluminescent efficiency.
Add carbonic acid ammonia in mixed solution, ammonia chloride be conducive to cleaning, the mixed solution of the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration will be added after carbonic acid ammonia, ammonia chloride water dissolution.Usual carbonic acid ammonia, ammonia chloride add-on are 10% of total solution weight.Concentration can water use regulation.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 and luminescent material is washed to neutrality repeatedly, clean to the long-lived operation that neutrality is conducive to luminescent material, finally dry at 120 degree.
A kind of infrared laser detecting blue emitting material of the present invention, use the electroluminescent device technology of preparing after improving, prepare infrared eye, it is at AC110V-220V, and produce blue-light-emitting under frequency 50-400 hertz, emmission spectrum is at 440-470nm, detection infrared band 0.7-4 micron, infrared laser intensity and luminescent material working current inversely, by the curent change of measuring element, derive the exposure intensity of infrared source.
The driving mechanism that in the present invention, luminescent device uses is for market sale usual products is as DH10-220, DH100-12-TB etc., and the current measurement table that uses in the present invention is conventional volt ohm-milliammeter.
the invention has the advantages that
1, a kind of blue emitting material for infrared laser detecting of the present invention and preparation, it is prepared into device, can produce luminous alternately changing with cancellation, can be determined the intensity of infrared light by current measurement under infrared rays 700-4000nm encourages.It directly can 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 work-ing life is more than 5 times of photoluminescence infrared detecting materials.It can life-time service out of doors, automatically controls, is especially quick on the draw to the irradiation of infrared laser, 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 changes above-mentioned disadvantageous effect, expands materials 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 may be used for invisible near infrared light detection, follows the tracks of, proofreads, identifies.The multidisciplinary technical fields such as near-infrared laser detection, laser facula display, opticfiber communication instruction, optical information storage, image procossing, infrared imaging can be widely used in, as: infrared LED telepilot, YAG laser cutter, 1550nm opticfiber communication etc. conventional in household electrical appliances.
embodiment 1
Get ZnS substrate material 1000 grams, add Cobaltous diacetate, relatively add Co content 1X10 in every gram of substrate material
-3; Add Sulfuric acid disilver salt, relatively add Ag content 2X10 in every gram of substrate material
-2; Add thallium trinitrate (TTN), relatively add Tl content 1X10 in every gram of substrate material
-4; Add water and regulate pasty state, add sulphur 20 grams, 120 degree of oven dry.Above-mentioned powder adds the sulphur grinding of 3% evenly again.The material of drying is loaded in alumina crucible, seals; In 750 degree of electric furnaces, sinter 10 hours, take out cooling crush, then anneal 8 hours at temperature 300 degree.
In beaker, configure the mixed solution 10 liters of the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration, soak luminescent material 1 hour, remove the liquid reacted, 3 times repeatedly, re-use washed with de-ionized water to neutral, and 120 degree dry.
embodiment 2
Get ZnS substrate material 100 grams, add Cobaltous diacetate, relatively add Co content 1X10 in every gram of substrate material
-2; Add silver chloride, relatively add Ag content 5X10 in every gram of substrate material
-2; Add thallium trinitrate (TTN), relatively add Tl content 1X10 in every gram of substrate material
-3; Add water and regulate pasty state, add sulphur 3 grams, 120 degree of oven dry.Above-mentioned powder adds the sulphur grinding of 3% evenly again.The material of drying is loaded in silica tube, seals; In 800 degree of electric furnaces, sinter 8 hours, take out cooling crush, then anneal 10 hours at temperature 300 degree.
In beaker, configure the mixed solution 1 liter of the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration, add carbonic acid ammonia simultaneously and add 50 grams, ammonia chloride adds 50 grams, micro-heating for dissolving.Soak luminescent material 1 hour, remove the liquid reacted, 3 times repeatedly, re-use washed with de-ionized water to neutral, and 120 degree dry.
embodiment 3
Get ZnS substrate material 500 grams, add Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, relatively add Co content 2X10 in every gram of substrate material
-3; Add Silver monoacetate, relatively add Ag content 3X10 in every gram of substrate material
-2; Add thaliium acetate, relatively add Tl content 3X10 in every gram of substrate material
-4; Add indium acetate, relatively add In content 1X10 in every gram of substrate material
-4, add water and regulate pasty state, add sulphur 40 grams, 120 degree of oven dry.Above-mentioned powder adds the sulphur grinding of 3% evenly again.The material of drying is loaded in alumina crucible, seals; In 750 degree of electric furnaces, sinter 10 hours, take out cooling crush, then anneal 8 hours at temperature 300 degree.
In beaker, configure the mixed solution 5 liters of the ammoniacal liquor of 15% concentration and the hydrogen peroxide of 20% concentration, soak luminescent material 1 hour, remove the liquid reacted, 3 times repeatedly, re-use washed with de-ionized water to neutral, and 120 degree dry.
After having done to illustrate for the good embodiment of the present invention above, it should be understood that to one skilled in the art, when without departing from the spirit and scope of the present invention, any changes and improvements made for the present invention all within the scope of the invention.
Claims (8)
1. the blue emitting material for infrared laser detecting, it comprises ZnS substrate material, wherein add the activator containing Co, Ag, Tl acidic cpd, add sulphur, and Homogeneous phase mixing, 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; In the every gram weight of substrate material, the concentration of adding dominant activator Co is 5 × 10
-3-1 × 10
-2, the concentration of Ag is 1 × 10
-2-5 × 10
-2, the concentration of Tl is 7 × 10
-5-1 × 10
-3this infrared laser detecting blue emitting material emmission spectrum is at 430-470nm, and the infrared electroluminescent detector be prepared into, infrared laser intensity and luminescent material working current are inversely.
2. a kind of blue emitting material for infrared laser detecting 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, and luminescent material grains degree 3-7 micron, powder crystal structure is in Emission in Cubic.
3. a kind of blue emitting material for infrared laser detecting as claimed in claim 1, acidic cpd is: sulphate, nitrate compound, halogenide, acetic acid compound.
4. a kind of blue emitting material for infrared laser detecting as claimed in claim 1, luminescent material after sintering, use the hydrogen peroxide mixed liquid dipping luminescent material 1 hour of the ammoniacal liquor of 15% concentration and 20% concentration, 3 times repeatedly, re-use washed with de-ionized water to neutral.
5. a kind of blue emitting material for infrared laser detecting as claimed in claim 1, adds carbonic acid ammonia, ammonia chloride, after dissolving, cleans 3 times in mixed solution.
6. a kind of blue emitting material for infrared laser detecting as claimed in claim 1, the luminescent material after sintering, then the 5-10 hour that anneals under temperature 250-350 degree.
7. a kind of blue emitting material for infrared laser detecting as claimed in claim 1, in the every gram weight of substrate material, the concentration of adding auxiliary activator In is 1 × 10
-5-1 × 10
-3, or the concentration of Ga is 1 × 10
-5-1 × 10
-3.
8. the preparation for the blue emitting material of infrared laser detecting, it comprises ZnS substrate material, wherein add the activator containing Co, Ag, Tl acidic cpd, add sulphur, and Homogeneous phase mixing, 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 blue emitting material emmission spectrum is at 430-470nm, and the infrared electroluminescent detector be prepared into, infrared laser intensity and luminescent material working current are inversely.
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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 |
| CN103013522A (en) * | 2013-01-06 | 2013-04-03 | 上海科润光电技术有限公司 | Preparation for luminescent material for probing and distinguishing middle and far infrared lasers |
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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 |
| CN103013522A (en) * | 2013-01-06 | 2013-04-03 | 上海科润光电技术有限公司 | Preparation for luminescent material for probing and distinguishing middle and far infrared lasers |
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