CN103013522B - Preparation for luminescent material for probing and distinguishing middle and far infrared lasers - Google Patents
Preparation for luminescent material for probing and distinguishing middle and far infrared lasers Download PDFInfo
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- CN103013522B CN103013522B CN201310002075.9A CN201310002075A CN103013522B CN 103013522 B CN103013522 B CN 103013522B CN 201310002075 A CN201310002075 A CN 201310002075A CN 103013522 B CN103013522 B CN 103013522B
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Abstract
The invention provides a preparation method for a luminescent material for probing and distinguishing middle and far infrared lasers. The preparation method adopts a ZnSe or CdSe base material. The preparation method is characterized by comprising the following steps in sequence: adding a Cu-containing dominant activator of an acid compound and at least one coactivator containing Pb, Au and Ag of the acid compound; uniformly mixing the dominant activator with the coactivator; drying; and sintering at a high temperature in protective atmosphere, wherein the material can emit visible light of 480 to 610nm after absorbing the ultraviolet ray, and the visible light is quenched under the irradiation of infrared rays of 2 to 10 microns, and black spots are generated at the same time, thus the luminescent material can be used for probing, tracking, calibrating and distinguishing the middle and far infrared lasers, and is applied to the fields such as the laser detecting field and the bio-labeling field.
Description
Technical field
The invention belongs to Submillineter Wave Technology detection and identify applied technical field.
Background technology
Infrared laser is conventional product in the field such as industrial, medical, military, and prior art has realized the detection of near infrared light by up-conversion luminescence or quencher, and it is mainly used in the infrared band of 0.7-1.6 micron.Along with the development of infrared technique, mid and far infrared laser uses all the more extensive, and present stage is surveyed the large volume infrared thermal imager device that mainly still relies on complex and expensive.
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, but it cannot realize the sensitive excitation luminescence to invisible Submillineter Wave Technology, 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
.commercially available prod trade mark HT582, HT612, HT111 also have abundant introduction.
Luminescent material taking ZnS as 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 existing explanation, they all can only survey near-infrared laser.
A kind of mid and far infrared laser acquisition identification luminescent material of the present invention, use ZnSe, CdSe, ZnS, CdS substrate material, add the activator that contains Cu, prepare the quencher luminescent material that can survey mid and far infrared, can be for invisible near infrared light be surveyed, follows the tracks of, proofreads, is identified.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
The preparation of a kind of mid and far infrared laser acquisition identification of the present invention luminescent material, it comprises ZnSe or CdSe substrate material, it is characterized in that: the dominant activator that wherein adds the acidic cpd that contains Cu, add the coactivator at least one acidic cpd that contains Pb, Au, Ag, dry after evenly mixing, high temperature sintering in protective atmosphere; After this absorbed ultraviolet ray, transmitting 480-610nm visible ray, produces cancellation simultaneously under the laser radiation of infrared 2-10 micron, produces blackspot.
The present invention is in the every gram weight of substrate material, and the concentration of adding dominant activator Cu is 1X10
-2-1X10
-4, in the every gram weight of substrate material, the concentration of adding coactivator is 1X10
-3-1X10
-4, when the concentration of dominant activator, coactivator exceeds this scope, easily produce flash of light or only near infrared produced to quencher.When taking CdSe as substrate material, can produce the green yellow or orange luminous of 540-610nm.The glow color that adds of silver moves to shortwave direction, and the glow color that adds of gold moves to long wave.
In the present invention, acidic cpd is: sulphate, nitrate compound, halogenide, phosphate cpd, acetic acid compound.Activator and coactivator adopt while containing acidic anionic compound can be effectively and substrate material hybrid reaction.
In the present invention, sintering temperature should be below 900 degree, and substrate material crystalline structure is in Emission in Cubic; Protective atmosphere is the one in sulphur, nitrogen, carbon reducing atmosphere, and protective atmosphere can prevent luminescent material oxidation, improves luminous efficiency.
In the present invention, can add fusing assistant when high temperature sintering, fusing assistant is the halogenide that contains Bi, Mg, Na, Ba, Li, K, and add-on is the 0.5-3% of substrate material weight, and it improves luminescence-utraviolet intensity, forms and quencher blackspot contrast contrast gradient.
The preparation of a kind of mid and far infrared laser acquisition identification of the present invention luminescent material, it comprises ZnSe or CdSe substrate material, it is characterized in that: wherein add the one in ZnS, CdS; Add the dominant activator of the acidic cpd that contains Cu simultaneously, add the coactivator at least one acidic cpd that contains Pb, Au, Ag, dry after evenly mixing, high temperature sintering in protective atmosphere, after this absorbed ultraviolet ray, transmitting 480-610nm visible ray, produces quencher simultaneously under the laser radiation of infrared 2-10 micron, produces blackspot; In the every gram weight of substrate material, the concentration of adding dominant activator Cu is 1X10
-2-1X10
-4, in the every gram weight of substrate material, the concentration of adding coactivator is 1X10
-3-1X10
-4.
In the present invention, wherein add ZnS, CdS add-on is the 10-50% of substrate material weight, it improves the quencher black degree of depth of infrared laser.Adding of CdS makes luminescence-utraviolet demonstration orange, and ZnS adds makes luminescence-utraviolet show green.
Middle-ultraviolet lamp radiation source of the present invention can be ultraviolet lamp 365nm, 253nm, can be also LED light source 400nm, 380nm, can also be royal purple laser 405nm, wherein selects soft ultraviolet lamp effect better.
The present invention also can make nano luminescent material by hydrothermal method, and hydro-thermal legal system can reduce synthesis temperature to 200 degree, after particle and surface treatment that it is less, and for biomarker and detection, as: in-vitro diagnosis, micro-imaging, drug disposition tracking etc.
Embodiment
The preparation of a kind of mid and far infrared laser acquisition identification of the present invention luminescent material, it comprises ZnSe or CdSe substrate material, it is characterized in that: the dominant activator that wherein adds the acidic cpd that contains Cu, add the coactivator at least one acidic cpd that contains Pb, Au, Ag, dry after evenly mixing, high temperature sintering in protective atmosphere; After this absorbed ultraviolet ray, transmitting 480-610nm visible ray, produces cancellation simultaneously under the laser radiation of infrared 2-10 micron, produces blackspot; In the every gram weight of substrate material, when the concentration of dominant activator, coactivator exceeds this scope, easily produce flash of light or only near infrared produced to quencher.
In the present invention, acidic cpd is: sulphate, nitrate compound, halogenide, phosphate cpd, acetic acid compound.As: copper sulfate, plumbic acetate, Silver Nitrate, gold trichloride etc.Above material adds rear use aqueous solution, and dries, and it can ensure activator and the coactivator homogeneity in substrate material.
In the present invention, sintering temperature should be below 900 degree, and substrate material crystalline structure is in Emission in Cubic; Protective atmosphere is the one in sulphur, nitrogen, carbon reducing atmosphere, and wherein the protective atmosphere of sulfur-bearing can produce good effect to agglomerated material, promotes the raising of luminous intensity.Sintering time should remain on 1-5 hour.When the invention process sintering, use high-temperature electric resistance furnace to carry out, the material preparing can pack in airtight silica tube or in alumina crucible.
In the present invention, can add fusing assistant when high temperature sintering, fusing assistant is the halogenide that contains Bi, Mg, Na, Ba, Li, K, and add-on is the 0.5-3% of substrate material weight.As: lithium fluoride, sodium-chlor, Potassium Bromide etc.Fusing assistant can improve crystalline perfection, strengthens luminosity.
The preparation of a kind of mid and far infrared laser acquisition identification of the present invention luminescent material, it comprises ZnSe or CdSe substrate material, it is characterized in that: wherein add the one in ZnS, CdS; Add the dominant activator of the acidic cpd that contains Cu simultaneously, add the coactivator at least one acidic cpd that contains Pb, Au, Ag, dry after evenly mixing, high temperature sintering in protective atmosphere, after this absorbed ultraviolet ray, transmitting 480-610nm visible ray, produces quencher simultaneously under the laser radiation of infrared 2-10 micron, produces blackspot; In the every gram weight of substrate material, the concentration of adding dominant activator Cu is 1X10
-2-1X10
-4, in the every gram weight of substrate material, the concentration of adding coactivator is 1X10
-3-1X10
-4.
In the present invention, wherein add ZnS, CdS add-on is the 10-50% of substrate material weight, it improves the quencher black degree of depth of infrared laser.
The present invention can add elemental sulfur in force in material, and add-on is the 1-10% of substrate material weight, its can be in the time of high temperature sintering protecting materials not oxidized.
Luminescent material prepared by the present invention and bonded adhesives mixing coating filmform, have better effects.Bonded adhesives material can use high temperature resistant good resin, rubber etc.Coating basis can be on surfaces such as plastics, metal, potteries, and wherein metal can have good heat radiation, can bear high power laser illumination.Bonded adhesives in the present invention also can use mineral-type materials, and as silicates, it is combined and can meets super high power laser radiation with pottery or glass.
the invention has the advantages that
A kind of mid and far infrared laser acquisition identification of the present invention luminescent material, it produces 480-610nm visible ray under UV-irradiation, then applies under the laser radiation of infrared 2-10 micron simultaneously and produce quencher blackspot, realizes the detection to infrared light.
Luminescent material of the present invention has satisfactory stability, and serious moisture decomposing phenomenon can not occur, and be the more than 5 times of sulfurated lime material work-ing life.
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, optical information storage.As: carbon dioxide laser detection etc.
embodiment 1
Get 100 grams of ZnSe substrate materials, add plumbic acetate, relatively in every gram of substrate material, add Pb content 1X10
-4; Add copper sulfate, relatively in every gram of substrate material, add Cu content 1x10
-3; Add 3 grams of fusing assistant lithium fluoride, add 3 grams of sulphur.Water is mixed, under 120 degree, dry.Dry material is packed in alumina crucible, seal; In 800 degree electric furnaces, sintering 3 hours, takes out cooling.
Material prepared by present method, produces gold-tinted at ultraviolet light irradiation, produces blackspot while using infrared 10 microns of LASER Light Source to irradiate.
embodiment 2
Get 1000 grams of CdSe substrate materials, add 300 grams of ZnS materials, add plumbic acetate, relatively in every gram of substrate material, add Ag content 5X10
-3; Add cupric nitrate, relatively in every gram of substrate material, add Cu content 7x10
-3; Add 20 grams, fusing assistant sodium-chlor, add 50 grams of sulphur.Water is mixed, under 120 degree, dry.Dry material is packed in alumina crucible, seal; In 800 degree electric furnaces, sintering 4 hours, takes out cooling.
Material prepared by present method, produces yellow green light at ultraviolet light irradiation, produces blackspot while using infrared 8 microns of LASER Light Source to irradiate.
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 (6)
1. the recognition methods of a mid and far infrared laser acquisition, it comprises ZnSe or CdSe substrate material, it is characterized in that: the dominant activator that wherein adds the acidic cpd that contains Cu, add the coactivator at least one acidic cpd that contains Pb, Au, Ag, dry after evenly mixing, high temperature sintering in protective atmosphere; Acidic cpd is: sulphate, nitrate compound, halogenide, phosphate cpd, acetic acid compound; After this absorbed ultraviolet ray, transmitting 480-610nm visible ray, produces cancellation simultaneously under the laser radiation of infrared 2-10 micron, produces blackspot.
2. a kind of recognition methods of mid and far infrared laser acquisition as claimed in claim 1, in the every gram weight of substrate material, the concentration of adding dominant activator Cu is 1 × 10
-2-1 × 10
-4; In the every gram weight of substrate material, the concentration of adding coactivator is 1 × 10
-3-1 × 10
-4.
3. a kind of recognition methods of mid and far infrared laser acquisition as claimed in claim 1, sintering temperature should be below 900 degree, and substrate material crystalline structure is in Emission in Cubic; Protective atmosphere is the one in sulphur, nitrogen, carbon reducing atmosphere.
4. a kind of recognition methods of mid and far infrared laser acquisition as claimed in claim 1, when high temperature sintering, can add fusing assistant, fusing assistant is the halogenide that contains Bi, Mg, Na, Ba, Li, K, and add-on is the 0.5-10% of substrate material weight, and it improves luminous intensity.
5. a recognition methods for mid and far infrared laser acquisition, it comprises ZnSe or CdSe substrate material, it is characterized in that: wherein add the one in ZnS, CdS; Add the dominant activator of the acidic cpd that contains Cu simultaneously, add the coactivator at least one acidic cpd that contains Pb, Au, Ag, dry after evenly mixing, high temperature sintering in protective atmosphere, after this absorbed ultraviolet ray, transmitting 480-610nm visible ray, produces cancellation simultaneously under the laser radiation of infrared 2-10 micron, produces blackspot; In the every gram weight of substrate material, the concentration of adding dominant activator Cu is 1 × 10
-2-1 × 10
-4, in the every gram weight of substrate material, the concentration of adding coactivator is 1 × 10
-3-1 × 10
-4; Acidic cpd is: sulphate, nitrate compound, halogenide, phosphate cpd, acetic acid compound.
6. a kind of recognition methods of mid and far infrared laser acquisition as claimed in claim 5, wherein adds ZnS, CdS add-on is the 10-50% of substrate material weight, and it improves the cancellation black degree of depth of infrared laser.
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|---|---|---|---|
| CN201310002075.9A CN103013522B (en) | 2013-01-06 | 2013-01-06 | Preparation for luminescent material for probing and distinguishing middle and far infrared lasers |
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| CN201310002075.9A CN103013522B (en) | 2013-01-06 | 2013-01-06 | Preparation for luminescent material for probing and distinguishing middle and far infrared lasers |
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| CN103013522B true CN103013522B (en) | 2014-10-22 |
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| CN103756672B (en) * | 2014-02-05 | 2016-03-16 | 上海科润光电技术有限公司 | A kind of green luminescent material and preparation detecting infrared laser |
| CN103756673B (en) * | 2014-02-05 | 2015-05-13 | 上海洞舟实业有限公司 | Blue luminescent material for infrared laser detection and preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1846291A (en) * | 2003-08-02 | 2006-10-11 | 磷光体技术公司 | Light emitting devices having sulfoselenide fluorescent phosphors |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0220590A (en) * | 1988-07-08 | 1990-01-24 | Nichia Chem Ind Ltd | Orange-emitting phosphor for cathode ray tube |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1846291A (en) * | 2003-08-02 | 2006-10-11 | 磷光体技术公司 | Light emitting devices having sulfoselenide fluorescent phosphors |
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| Title |
|---|
| JP平2-20590A 1990.01.24 |
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