CN101717641A - Preparation of high-sensitivity color-changeable up-conversion luminescent material - Google Patents
Preparation of high-sensitivity color-changeable up-conversion luminescent material Download PDFInfo
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- CN101717641A CN101717641A CN200910199778A CN200910199778A CN101717641A CN 101717641 A CN101717641 A CN 101717641A CN 200910199778 A CN200910199778 A CN 200910199778A CN 200910199778 A CN200910199778 A CN 200910199778A CN 101717641 A CN101717641 A CN 101717641A
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Abstract
The invention discloses the preparation of a color-changeable up-conversion luminescent material with high-sensitivity identification on a 980nm waveband of near infrared light. The material comprises the following raw materials in percentage by weight: 60 percent of YF3, 20 percent of YbF3, 3 percent of ErF3, 10 percent of NaF, 4 percent of MgF2, and 3 percent of BaF2. The preparation comprises the following steps of: fully mixing the raw materials, then sintering the mixture in oxygen at the temperature of 900 DEG C for more than 5 hours to form oxyfluoride co-crystals. The material can ensure that the luminescent color changes along with the enhancement of laser power, and change of laser emission spectrum and temperature can be correspondingly calculated; and the luminescent material can produce the fluorescence alteration from orange to red along with the change of the power, the spectrum and the temperature under the excitation of laser with a wavelength of 980nm.
Description
Technical field
The invention belongs to the solid luminescence technical field.
Background technology
Existing all kinds of laser apparatus all can produce higher temperature owing to be subjected to himself structural limitations when laser works.For infrared semiconductor laser, very little temperature variation during its work can make laser emission spectrum with temperature small drift take place, and its Laser emission power also can change simultaneously, this spectrum, power, variation of temperature have limited the precision of Laser Devices greatly.Because the semiconductor laser volume is less, number of applications is big, and people can't accurately measure temperature in actual the use, further causes realizing observation in time and control to emmission spectrum, the power of laser apparatus.People are to use error concept to give to avoid to the generation of this situation more, and noise spectra of semiconductor lasers just directly adopts passive method of cooling controlled temperature when reality is used, as: the liquid-cooling system of bigger metal fin, complexity.
Prior art such as needs identification infrared laser transmitted power and spectrum can only be by costing an arm and a leg, and the bigger fixedly photoelectric instrument interpretation of volume.People can't be directly by simple visual observation, and the corresponding relation of temperature, spectrum, power can only be measured the pusher opinion respectively and calculate; And to sensitivity less than below 0.1 centigradetemperature, laser power and spectrographic drift detection of dynamic then can't show.
Existing infrared up-conversion luminous material is mainly used in detection, identification, tracking, check and correction to infrared invisible laser, and its Application Areas has biomarker, laser processing industry, false proof etc., as Chinese patent 96122293.X.Its shortcoming of material of known technology preparation is only a certain large-scale exciting light to be shown and identification, and as to 808nm, 980nm, 1064nm, 1550nm, it is a manifestation mode with luminous power.Have up-conversion luminescence simple substance material or mixing material now and all can't discern the trickle emission band variation and the strong and weak variation of power of laser apparatus, as ± the 10nm variation.
Summary of the invention
A kind of changeable colour up-conversion luminescent material preparation to the highly sensitive identification of near infrared light 980nm wave band of the present invention, it contains weight ratio YF
360%, YbF
320%, ErF
33%, NaF 10%, MgF
24%, BaF
23%, sintering carries out in oxygen behind the thorough mixing, and temperature is 900 degree, and sintering should feed minor amounts of oxygen during sintering more than 5 hours, the mixing material of per kilogram, and oxygen feeding amount is 0.002-0.1 cubic meter per hour.It forms oxyfluoride cocrystallization body, this material can strengthen with laser power changes glow color, and can corresponding change of calculating laser emission spectrum and temperature, luminescent material is under 980nm laser excitation, along with power, spectrum, temperature variation, luminescent material can produce orange to red change in fluorescence.
The invention provides a kind of new material, technology of preparing and detection method, realized that cheap and simple detects the fluctuation and the laser power subtle change thereof of infrared laser spectroscopy.Luminescent material is an orange luminescence when laser power is big, and laser power is hour luminous to be red; When the laser works temperature is high, power reduction, the small spectrum and the temperature variation that produce in the time of can calculating laser works are thus judged the tiny mobile of 980nm semiconductor laser emmission spectrum, sensitivity is ± 5nm; Material of the present invention is made card, its low price, simple and easy to use, judge accurately.With the exception of this, but it is in also widespread uses of technical field such as biological markers detection, photo-electric tracing, the identifications of trickle temperature spectrum.The present invention can be widely used in laser communication, aerospace measurement, semiconducter device production testing, microcosmic temperature survey, power judgement etc.
Embodiment
A kind of changeable colour up-conversion luminescent material preparation to the highly sensitive identification of near infrared light 980nm wave band of the present invention, it contains weight ratio YF
360%, YbF
320%, ErF 33%, and NaF 10%, MgF
24%, BaF
23%, sintering carries out in oxygen behind the thorough mixing, temperature is 900 degree, sintering is more than 5 hours, and it forms oxyfluoride cocrystallization body, and this material can strengthen with laser power changes glow color, and can corresponding change of calculating laser emission spectrum and temperature, luminescent material is under 980nm laser excitation, and along with power, spectrum, temperature variation, luminescent material can produce orange to red change in fluorescence.
Substrate material used in the present invention is YF
3, its add-on is 60% of a gross weight; Activator is YbF
3, its add-on is 20% of a gross weight; Coactivator ErF
3, its add-on is 3% of a gross weight, fusing assistant is NaF, BaF
2, MgF
2, its add-on is respectively 10%, 4%, 3% of gross weight.Above-mentioned materials is thorough mixing and ball milling in proportion, and it uses quartz crucible to load sintering in vacuum oven, sintering temperature is 900 degree, and sintering time is more than 5 hours, should feed minor amounts of oxygen during sintering, the mixing material of per kilogram, oxygen feeding amount is 0.002-0.1 cubic meter per hour.
Synthetic material of the present invention forms oxyfluoride cocrystallization body, and this material sends fluorescent orange under 980-985nm excites, send red fluorescence under 976-978nm excites.The various composition part by weight of the material that relates among the present invention should strict control, and in suitable oxygen sintering, the variation characteristic of glow color is just arranged, otherwise has only green or emitting red light, more can't discern the trickle emission band error of laser apparatus.
The invention has the advantages that and realized that homogeneous material realizes surveying to 980nm laser apparatus emission invisible light, by the infrared color-changeable up-conversion luminescent material of highly sensitive, can tell ± the laser spectrum fluctuation of 5nm.The temperature that produces when the variation of Laser emission power, laser emission spectrum and laser works has corresponding relation, and is significant to production, application, the measurement of 980nm laser apparatus.
Embodiment:
Get YF
360 grams; Activator is YbF
320 grams; Coactivator ErF
33 grams, fusing assistant add NaF 10 grams, BaF respectively
24 grams, MgF
23 grams.Above-mentioned materials is thorough mixing and ball milling in proportion, and it uses quartz crucible to load, sintering in the vacuum oven, and sintering temperature is 900 degree, and sintering time is 5 hours, should feed minor amounts of oxygen during sintering, and oxygen feeding amount is per hour 0.01 cubic metre.
After embodiment had been done to illustrate preferably at the present invention in the above, what should understand to one skilled in the art was, under situation without departing from the spirit and scope of the present invention, to any change that the present invention did all within the scope of the invention.
Claims (2)
1. changeable colour up-conversion luminescent material preparation to the highly sensitive identification of near infrared light 980nm wave band, it contains weight ratio YF
360%, YbF
320%, ErF
33%, NaF 10%, MgF
24%, BaF
23%, sintering carries out in oxygen behind the thorough mixing, temperature is 900 degree, sintering is more than 5 hours, and it forms oxyfluoride cocrystallization body, and this material can strengthen with laser power changes glow color, and can corresponding change of calculating laser emission spectrum and temperature, luminescent material is under 980nm laser excitation, and along with power, spectrum, temperature variation, luminescent material can produce orange to red change in fluorescence.
2. according to claim 1, should feed minor amounts of oxygen during sintering, the mixing material of per kilogram, oxygen feeding amount is 0.002-0.1 cubic meter per hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910199778A CN101717641B (en) | 2009-12-01 | 2009-12-01 | Preparation of high-sensitivity color-changeable up-conversion luminescent material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910199778A CN101717641B (en) | 2009-12-01 | 2009-12-01 | Preparation of high-sensitivity color-changeable up-conversion luminescent material |
Publications (2)
| Publication Number | Publication Date |
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| CN101717641A true CN101717641A (en) | 2010-06-02 |
| CN101717641B CN101717641B (en) | 2012-09-26 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775990A (en) * | 2011-09-09 | 2012-11-14 | 太原理工大学 | Method for quickly preparing ultraviolet phosphors |
| CN103235347A (en) * | 2013-04-23 | 2013-08-07 | 上海洞舟实业有限公司 | Method for preparing multi-band infrared laser detection device |
| CN104962184A (en) * | 2015-04-30 | 2015-10-07 | 广东溢达纺织有限公司 | Visible infrared anti-counterfeiting coating and preparation method and application thereof |
| CN104962053A (en) * | 2015-04-30 | 2015-10-07 | 广东溢达纺织有限公司 | Visible infrared anti-counterfeiting button and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006089547A (en) * | 2004-09-22 | 2006-04-06 | National Institute For Materials Science | Phosphor, method for producing the same, and luminescent device |
-
2009
- 2009-12-01 CN CN200910199778A patent/CN101717641B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006089547A (en) * | 2004-09-22 | 2006-04-06 | National Institute For Materials Science | Phosphor, method for producing the same, and luminescent device |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775990A (en) * | 2011-09-09 | 2012-11-14 | 太原理工大学 | Method for quickly preparing ultraviolet phosphors |
| CN102775990B (en) * | 2011-09-09 | 2013-08-28 | 太原理工大学 | Method for quickly preparing ultraviolet phosphors |
| CN103235347A (en) * | 2013-04-23 | 2013-08-07 | 上海洞舟实业有限公司 | Method for preparing multi-band infrared laser detection device |
| CN103235347B (en) * | 2013-04-23 | 2016-07-13 | 上海洞舟实业有限公司 | A kind of preparation of multiband detection of infrared laser device |
| CN104962184A (en) * | 2015-04-30 | 2015-10-07 | 广东溢达纺织有限公司 | Visible infrared anti-counterfeiting coating and preparation method and application thereof |
| CN104962053A (en) * | 2015-04-30 | 2015-10-07 | 广东溢达纺织有限公司 | Visible infrared anti-counterfeiting button and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN101717641B (en) | 2012-09-26 |
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