CN101717641B - Preparation of high-sensitivity color-changeable up-conversion luminescent material - Google Patents
Preparation of high-sensitivity color-changeable up-conversion luminescent material Download PDFInfo
- Publication number
- CN101717641B CN101717641B CN200910199778A CN200910199778A CN101717641B CN 101717641 B CN101717641 B CN 101717641B CN 200910199778 A CN200910199778 A CN 200910199778A CN 200910199778 A CN200910199778 A CN 200910199778A CN 101717641 B CN101717641 B CN 101717641B
- Authority
- CN
- China
- Prior art keywords
- laser
- luminescent material
- temperature
- percent
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Luminescent Compositions (AREA)
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 receive himself structural limitations when laser works.As far as 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, complicacy.
Prior art such as needs identification infrared laser transmitted power and spectrum can only be through costing an arm and a leg, and the bigger fixedly photoelectric instrument interpretation of volume.People can't be directly through 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 industrial, false proof etc., like 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, and 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 processed 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%, NaF 10%, MgF
24%, BaF
23%, sintering carries out in oxygen behind the thorough mixing, and 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, under 976-978nm excites, send red fluorescence.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, through 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.
In the above to the present invention after embodiment has been done to illustrate preferably, what should understand to one skilled in the art is, 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. preparation method to the changeable colour up-conversion luminescent material of the highly sensitive identification of near infrared light 980nm wave band, said material is YF by weight percent
360%, YbF
320%, ErF
33%, NaF 10%, MgF
24%, BaF
23% forms, and in oxygen, carries out sintering behind the thorough mixing, and temperature is 900 degree; Sintering is more than 5 hours, and it forms oxyfluoride cocrystallization body, and this material strengthens with laser power changes glow color; And the corresponding change of calculating laser emission spectrum and temperature of ability; Luminescent material is under 980nm laser excitation, and along with power, spectrum, temperature variation, luminescent material produces orange to red change in fluorescence.
2. the preparation method of a kind of changeable colour up-conversion luminescent material to the highly sensitive identification of near infrared light 980nm wave band as claimed in claim 1 should feed minor amounts of oxygen during sintering, the mixing material of per kilogram, and 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 |
---|---|
CN101717641A CN101717641A (en) | 2010-06-02 |
CN101717641B true CN101717641B (en) | 2012-09-26 |
Family
ID=42432284
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN200910199778A Expired - Fee Related CN101717641B (en) | 2009-12-01 | 2009-12-01 | Preparation of high-sensitivity color-changeable up-conversion luminescent material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN101717641B (en) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102775990B (en) * | 2011-09-09 | 2013-08-28 | 太原理工大学 | Method for quickly preparing ultraviolet phosphors |
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 |
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 |
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 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4674348B2 (en) * | 2004-09-22 | 2011-04-20 | 独立行政法人物質・材料研究機構 | Phosphor, method for producing the same, and light emitting device |
-
2009
- 2009-12-01 CN CN200910199778A patent/CN101717641B/en not_active Expired - Fee Related
Non-Patent Citations (1)
Title |
---|
JP特开2006-089547A 2006.04.06 |
Also Published As
Publication number | Publication date |
---|---|
CN101717641A (en) | 2010-06-02 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Zhang et al. | Upconversion luminescence of Ba9Y2Si6O24: Yb3+-Ln3+ (Ln= Er, Ho, and Tm) phosphors for temperature sensing | |
CN102798485B (en) | Temperature sensing method based on upconversion fluorescent powder | |
CN101717641B (en) | Preparation of high-sensitivity color-changeable up-conversion luminescent material | |
CN109341891B (en) | Method for high-sensitivity large-range temperature detection | |
Nayab Rasool et al. | Optical and luminescence properties of Eu3+-doped phosphate based glasses | |
CN105198225B (en) | One class bidifly work ion doping twin crystal phase glass ceramics fluorescence temperature probe material and preparation method thereof | |
Zhang et al. | Thermometry and up-conversion luminescence of Yb 3+–Er 3+ co-doped Na 2 Ln 2 Ti 3 O 10 (Ln= Gd, La) phosphors | |
Karki et al. | Physical, optical and luminescence properties of the Dy3+ doped barium borophosphate glasses | |
Ye et al. | White-light emission and chromaticity characterization of Dy3+ doped fluoride glass for standard white light source | |
Żur et al. | Absorption and luminescence properties of terbium ions in heavy metal glasses | |
Yu et al. | Determination of Judd-Ofelt parameters for Eu3+-doped alkali borate glasses | |
Żur | Structural and luminescence properties of Eu3+, Dy3+ and Tb3+ ions in lead germanate glasses obtained by conventional high-temperature melt-quenching technique | |
Pisarski et al. | Transition metal (Cr3+) and rare earth (Eu3+, Dy3+) ions used as a spectroscopic probe in compositional-dependent lead borate glasses | |
CN111073642B (en) | Novel self-calibration fluorescent temperature probe material and preparation method and application thereof | |
CN102829892B (en) | Temperature-sensing measurement method based on various mixed fluorescent materials | |
Farias et al. | Emission tunability and local environment in europium-doped OH−-free calcium aluminosilicate glasses for artificial lighting applications | |
Zhu et al. | Lanthanide-doped lead-free double perovskite La 2 MgTiO 6 as ultra-bright multicolour LEDs and novel self-calibrating partition optical thermometer | |
Wu et al. | Cross Relaxation Channel Tailored Temperature Response in Er3+‐rich Upconversion Nanophosphor | |
Zhang et al. | Optical temperature sensing of four modes by using CsPb (Cl/Br) 3 quantum dots and Tb3+ ions co-doping glass | |
CN107722985B (en) | Rare earth ion pair co-doped K3Y(PO4)2Up-conversion luminescent material and preparation method thereof | |
CN113429971A (en) | Optical temperature sensing type fluorescent powder and preparation method thereof | |
Pandey et al. | Rare earth doped materials for temperature sensors | |
Duan et al. | Luminescence and optical properties of sodium germanate glasses doped with Sm3+ ions | |
Borisov et al. | Red light-excitable dual lifetime referenced optical pH sensors with intrinsic temperature compensation | |
Torquato et al. | Influence of PbF2 content on optical thermometry of Er3+/Yb3+ co-doped tungsten sodium phosphate glasses |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120926 Termination date: 20151201 |
|
EXPY | Termination of patent right or utility model |