CN103436259A - Preparation of infrared radiation storage material - Google Patents
Preparation of infrared radiation storage material Download PDFInfo
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- CN103436259A CN103436259A CN2013103725319A CN201310372531A CN103436259A CN 103436259 A CN103436259 A CN 103436259A CN 2013103725319 A CN2013103725319 A CN 2013103725319A CN 201310372531 A CN201310372531 A CN 201310372531A CN 103436259 A CN103436259 A CN 103436259A
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Abstract
The invention discloses the preparation of an infrared radiation storage material. The preparation is characterized in that the matrix material is at least one of germanium oxide and gallium oxide, wherein an activator which contains chrome oxide and zinc oxide is added into the matrix material and the material which contains at least one of contain lithium, alkaline earth oxide and rare earth oxide is added into the matrix material to serve as a cosolvent or a fluxing agent; the temperature is kept at 800 to 1300 DEG C for 2 to 5 hours by using a high-temperature sintering method; the material is crushed to prepare the material with an infrared radiation storage function. The material can emit the near-infrared light with the wavelength of 800 to 1500 nm under the excitation of X-rays, ultraviolet light and visible light. The material can be widely applied to the places of medical rehabilitation, biological markers, anti-counterfeit label, concealed lighting, target recognition, industrial inspection, safety check, infrared night vision imaging and the like.
Description
Technical field
The invention belongs to the luminescent material applied technical field.
Background technology
Existing common infrared up-conversion luminous material, the ultra-violet light-emitting material of being categorized as of embedded photoluminescent material.Up-conversion luminescent material is mainly that luminescent material is launched visible ray by invisible infrared source exciting irradiation luminescent material; The ultra-violet light-emitting material is mainly by ultraviolet ray, after the irradiation luminous material of blue-ray light, produces VISIBLE LIGHT EMISSION, and it mainly contains long afterglow luminous material, lamp with luminescent material etc.
The present invention is by a kind of ir radiation storage medium of preparation, it can be by UV-light, excited by visible light, produce the invisible near infrared light radiation of human vision, it has infrared steady persistence radiation characteristic simultaneously, use night vision imaging instrument, cell-phone camera, digital camera etc., can clearly observe ir radiation luminous.
The present invention can be widely used in medical rehabilitation, biomarker, antifalsification label, cove lighting, Target Recognition, industrial detection, safety inspection, infrared night vision imaging etc. and locate.
Summary of the invention
A kind of preparation of ir radiation storage medium, it is characterized in that: substrate material is at least one in germanium, gallium oxide, wherein add the activator that contains chromium, zinc oxide, add and contain at least one in lithium, alkaline-earth oxide, rare-earth oxidation compound material, do congruent melting agent or solubility promoter; Use high-temperature sintering process, at temperature 800-1300 degree, hold-time 2-5 hour; Pulverize again, prepare the material with ir radiation storage; This material, under X ray, UV-light, excited by visible light, is launched the near infrared light of 800-1500nm.
Substrate material in the present invention is used sulfuric acid or nitric acid dissolve, can certainly use hydrochloric acid, hydrofluoric acid etc., and in the every gram weight of high-purity substrate material, the optimum concn of adding activator is 0.1%-10%, and activator can impel material luminous.When activator concentration is greater than 10%, ir radiation efficiency obviously reduces.In the every gram weight of substrate material, the concentration of adding congruent melting agent is 1%-30%, and adding of cosolvent can significantly improve the light absorbing scope of luminescent material.In the every gram weight of substrate material, add solubility promoter, the concentration of fusing assistant is 1%-10%, fusing assistant can reduce sintering temperature, improves luminous intensity, changes the radioluminescence wave band of luminescent material.
Substrate material in the present invention, activator material, congruent melting agent, flux material, used sulfuric acid, nitric acid, hydrochloric acid, acetate dissolution, remix, precipitation, oven dry, sintering.The method can make material easily mix.
Use high-temperature sintering process in the present invention, during sintering under air, nitrogen, hydrogen, sulphur atmosphere protection sintering; The material 3-20 micron of preparing, or compressing tablet becomes the block shape, after its shooting conditions stops, still having long-time near infrared light radiation.
Use hydrothermal synthesis method in the present invention is synthetic, with the sealing autoclave, and reflection temperature 100-300 degree, time 1-30 hour, prepare the nano-particle material that granularity is the 20-100 nanometer, after its shooting conditions stops, still having short period of time near infrared light radiation.
While selecting exciting light sources to be X ray, UV-light, visible blue in the present invention, ir radiation is luminous stronger, selects other visible ray, ir radiation is luminous fainter when infrared ray excited.
Embodiment
A kind of preparation of ir radiation storage medium, it is characterized in that: substrate material is at least one or more than one in germanium, gallium oxide, their purity is preferably more than 99.99%, when both existing, its twilight sunset illumination effect is best, as weight ratio germanic in substrate material is 20-40%, containing the weight ratio 60-80% of gallium.Add the activator that contains chromium, zinc oxide in substrate material, activator be take chromium usually as main, and it accounts for the 60-80% of activator gross weight.Add congruent melting agent and the solubility promoter that contains lithium, alkaline-earth oxide, rare earth oxide in matrix; Use high-temperature sintering process, at temperature 800-1300 degree, hold-time 2-5 hour; Pulverize again, prepare the material with ir radiation storage; This material, under X ray, UV-light, excited by visible light, is launched the near infrared light of 800-1500nm.
The present invention can use conventional dry method material mixing, directly selects the oxide compound of various types of materials, through grinding for a long time, mixes direct sintering.As germanium oxide, gallium oxide, chromic oxide, zinc oxide, Lithium Oxide 98min etc.
Substrate material in the present invention also can be used sulfuric acid or nitric acid dissolve, form nitric acid germanium, gallium nitrate, can certainly use hydrochloric acid, hydrofluoric acid etc., in the every gram weight of high-purity substrate material, the optimum concn of adding activator is 0.1%-10%, and activator can impel material luminous.When activator concentration is greater than 10%, ir radiation efficiency obviously reduces.In the every gram weight of substrate material, the concentration of adding congruent melting agent is 1%-30%, and adding of cosolvent can significantly improve the light absorbing scope of luminescent material.In the every gram weight of substrate material, add solubility promoter, the concentration of fusing assistant is 1%-10%, fusing assistant can reduce sintering temperature, improves luminous intensity, changes the radioluminescence wave band of luminescent material.
Substrate material in the present invention, activator material, congruent melting agent, flux material, used sulfuric acid, nitric acid, hydrochloric acid, acetate dissolution, as: chromium nitrate, zinc sulfate etc., remix, precipitation, oven dry, sintering.The method can make material easily mix.
Use high-temperature sintering process in the present invention, during sintering under air, nitrogen, hydrogen, sulphur atmosphere protection sintering; The material 3-20 micron of preparing, or compressing tablet becomes the block shape, after its shooting conditions stops, still having long-time near infrared light radiation more than 10 hours.
Use hydrothermal synthesis method in the present invention is synthetic, with the sealing autoclave, and reflection temperature 100-300 degree, time 1-30 hour, prepare the nano-particle material that granularity is the 20-100 nanometer, after its shooting conditions stops, still thering is the near infrared light radiation of 1-5 minute short period of time.The larger luminous intensity of granularity is relatively high, the time is relatively long.
the invention has the advantages that
1) the present invention is by a kind of ir radiation storage medium of preparation, it can be by UV-light, excited by visible light, can produce the invisible near infrared light radiation of human vision, it has infrared steady persistence radiation characteristic this radiation simultaneously, use night vision imaging instrument, cell-phone camera, digital camera etc., can clearly observe ir radiation luminous.
2) the present invention can be widely used in medical rehabilitation, biomarker, antifalsification label, cove lighting, Target Recognition, industrial detection, safety inspection, infrared night vision imaging etc. and locates.
Embodiment
Select substrate material germanium oxide 30 grams, gallium oxide 70 grams.Activator chromic oxide 5 grams, zinc oxide 2 grams.Congruent melting agent Lithium Oxide 98min 10 grams and solubility promoter lithium chloride 2 grams.Fully mix, the ceramic crucible of packing into, in temperature 1100 degree, 5 hours hold-times; Pulverize again, prepare the material with ir radiation storage; This material, under ultraviolet excitation, is launched the near infrared light of 800-1500nm.
After for the present invention, embodiment has been done to illustrate preferably in the above, what should understand to one skilled in the art is, in the situation that 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 (5)
1. the preparation of an ir radiation storage medium, it is characterized in that:: substrate material is at least one or more than one in germanium, gallium oxide, wherein interpolation contains chromium, zinc oxide is done activator, add and contain at least one in lithium or alkaline-earth oxide or rare earth oxide material, do congruent melting agent or solubility promoter; The preparation of use high-temperature sintering process, at temperature 800-1300 degree, hold-time 2-5 hour; Pulverize again, prepare the material with ir radiation storage; This material, under X ray, UV-light, excited by visible light, is launched the near infrared light of 800-1500nm.
2. a kind of preparation of ir radiation storage medium as claimed in claim 1, substrate material is used sulfuric acid or nitric acid dissolve, and in the every gram weight of substrate material, the weight ratio concentration of adding activator is 0.1%-10%; In the every gram weight of substrate material, the weight ratio concentration of adding congruent melting agent is 1%-30%; In the every gram weight of substrate material, the weight ratio concentration of adding solubility promoter is 1%-10%.
3. a kind of preparation of ir radiation storage medium as claimed in claim 1, substrate material, activator material, congruent melting agent, flux material, used sulfuric acid, nitric acid, hydrochloric acid, acetate dissolution, remix, precipitation, oven dry, sintering.
4. a kind of preparation of ir radiation storage medium as claimed in claim 1, used high-temperature sintering process, during sintering under air, nitrogen, hydrogen, sulphur atmosphere protection sintering; The material 3-20 micron of preparing, or compressing tablet becomes the block shape, after its shooting conditions stops, still having long-time near infrared light radiation.
5. a kind of preparation of ir radiation storage medium as claimed in claim 1, used hydrothermal synthesis method synthetic, with the sealing autoclave, reflection temperature 100-300 degree, time 1-30 hour, prepare nano-particle material, after its shooting conditions stops, still thering is short period of time near infrared light radiation.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105839874A (en) * | 2016-05-25 | 2016-08-10 | 洲建集团有限公司 | Wall surface structure containing germanium energy |
CN111671395A (en) * | 2020-05-28 | 2020-09-18 | 重庆大学 | Device for auxiliary diagnosis of breast cancer |
CN115340864A (en) * | 2022-09-15 | 2022-11-15 | 厦门理工学院 | Red luminescent material and preparation method and application thereof |
Citations (3)
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US20120193578A1 (en) * | 2009-09-21 | 2012-08-02 | University Of Georgia Research Foundation, Inc. | Near infrared doped phosphors having a zinc, germanium, gallate matrix |
CN103194228A (en) * | 2013-03-28 | 2013-07-10 | 华南理工大学 | Long-lasting phosphorescent material with optical excitation characteristic for biological imaging and preparation method and application thereof |
CN103215041A (en) * | 2013-05-17 | 2013-07-24 | 南开大学 | Preparation method of near infrared super-long afterglow luminescence nanomaterial |
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2013
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Patent Citations (3)
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US20120193578A1 (en) * | 2009-09-21 | 2012-08-02 | University Of Georgia Research Foundation, Inc. | Near infrared doped phosphors having a zinc, germanium, gallate matrix |
CN103194228A (en) * | 2013-03-28 | 2013-07-10 | 华南理工大学 | Long-lasting phosphorescent material with optical excitation characteristic for biological imaging and preparation method and application thereof |
CN103215041A (en) * | 2013-05-17 | 2013-07-24 | 南开大学 | Preparation method of near infrared super-long afterglow luminescence nanomaterial |
Non-Patent Citations (1)
Title |
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JONG SU KIM等: "Optical and structural properties of nanosized ZnGa2O4:Cr3+ phosphor", 《SOLID STATE COMMUNICATIONS》, vol. 131, 31 December 2004 (2004-12-31), pages 735 - 738, XP004533329, DOI: doi:10.1016/j.ssc.2004.07.026 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105839874A (en) * | 2016-05-25 | 2016-08-10 | 洲建集团有限公司 | Wall surface structure containing germanium energy |
CN111671395A (en) * | 2020-05-28 | 2020-09-18 | 重庆大学 | Device for auxiliary diagnosis of breast cancer |
CN111671395B (en) * | 2020-05-28 | 2021-04-23 | 重庆大学 | Device for auxiliary diagnosis of breast cancer |
CN115340864A (en) * | 2022-09-15 | 2022-11-15 | 厦门理工学院 | Red luminescent material and preparation method and application thereof |
CN115340864B (en) * | 2022-09-15 | 2023-08-25 | 厦门理工学院 | Red luminescent material and preparation method and application thereof |
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Application publication date: 20131211 |