CN101788485A - Measuring method of up-conversion intermediate energy level lifetime of erbium ions - Google Patents

Measuring method of up-conversion intermediate energy level lifetime of erbium ions Download PDF

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CN101788485A
CN101788485A CN201010300207A CN201010300207A CN101788485A CN 101788485 A CN101788485 A CN 101788485A CN 201010300207 A CN201010300207 A CN 201010300207A CN 201010300207 A CN201010300207 A CN 201010300207A CN 101788485 A CN101788485 A CN 101788485A
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李艾华
郑植仁
刘伟龙
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Harbin Institute of Technology
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Abstract

The invention discloses a measuring method of up-conversion intermediate energy level lifetime of erbium ions and relates to the measuring method of fluorescence lifetime, and the measuring method can solve the problems that the existing measuring method of the infrared fluorescence lifetime needs an expensive infrared detector, the testing process is complicated, double beams and the delay change between the double beams need to be introduced, and the testing difficulty is great. The method adopts a delay signal generator, a short pulse laser, a high voltage pulse generator, an enhanced charge-coupled device and a grating spectrometer for constituting a testing system, and fluorescence emitted by a tested material by pulse radiation enters into the spectrometer for testing the light intensity; and the corresponding visible light intensities under different excitation frequencies are measured under the condition of keeping the single pulse energy unchanged, an I-1/f relation map is drawn out, then fitting is carried out by utilizing the formula, and the fitted tau is the up-conversion intermediate energy level lifetime. The single beam is adopted and the visible light detector is used for measuring the infrared energy level fluorescence lifetime, the measuring process is simple, and the measuring method can be used for measuring the fluorescence lifetime of Er3+ doped materials.

Description

The measuring method in conversion intermediate level life-span on a kind of erbium ion
Technical field
The present invention relates to the measuring method of fluorescence lifetime.
Background technology
The optical communication amplifier generally is by Er 3+The ion doping material preparation, Er 3+An important referential data the when fluorescence lifetime of ion is design optical communication amplifier is so accurately measure Er in the material 3+The fluorescence lifetime of ion seems extremely important, measures Er at present 3+The ion fluorescence method of life mainly contains fast ion laser beam technology, postpones to meet switch technology and pump probe technology on single photon counting technology, pulse-sampling technique, the fluorescence, wherein fast ion laser beam technology, delay meets the single photon counting technology and pulse-sampling technique all requires the fluorescence that originates from energy level to be measured is monitored, if the fluorescence of energy level to be measured is at infrared region, then measure and need the very expensive infrared eye of price, and except the measurement of light intensity, also need demarcating apparatus expensive and test process complexity time delay; Though switch technology and pumping-detection technology have realized the measurement of infrared energy level in the visible region on the fluorescence, the delay that these two kinds of methods have all been introduced between twin-beam and the twin-beam changes, and this has just increased the difficulty that detects widely.
Summary of the invention
The present invention is that the delay that needs the infrared eye of costliness, test process complexity in order to solve existing measurement Infrared fluorescence method of life, needs to introduce between twin-beam and the twin-beam changes, the problem that detection difficulty is big, and the measuring method of changing the intermediate level life-span on a kind of erbium ion is provided.
The measuring method in conversion intermediate level life-span is carried out according to the following steps on a kind of erbium ion of the present invention: one, be connected with the output control terminal of short-pulse laser with the output channel of concentric cable with delayed signal generator, another output channel be connected with high-voltage pulse generator external trigger end again; Be connected with the external trigger port of enhancement mode electric charge coupling mechanism with the output terminal of concentric cable then high-voltage pulse generator; With the control port and the data acquisition card connection of enhancement mode electric charge coupling mechanism, data collecting card is inserted on the mainboard of computing machine; Enhancement mode electric charge coupling mechanism is inserted in the exit portal of grating spectrograph, and wherein the pulse wavelength of short-pulse laser output is 790nm~820nm or 960nm~1020nm, and the duration of pulse is 100fs~10ns; Two, the centre wavelength with grating spectrograph transfers to 550nm or 660nm, and the gate-width of enhancement mode electric charge coupling mechanism is made as 900 μ s; Three, with tested Er 3+The ion doping material sample is to be fixed on the specimen holder, starts short-pulse laser, and the pulse irradiation that is sent by short-pulse laser is at Er 3+On the ion doping material sample, the fluorescence that sample sends is collected laggard entrance slit of going into spectrometer through collecting lens, demonstrates light intensity on computers; Four, the frequency knob of control lag signal generator makes the frequency f of excitation pulse iBe increased to 1000Hz from 10Hz, and be recorded in different frequency f iPairing light intensity I on the following computing machine iFive, the array I to obtaining i-1/f i, be horizontal marking with 1/f, map for the vertical mark of doing with intensity I, use formula then
Figure G201010300207220100112D000021
Match obtains fluorescence lifetime τ.
Described Er 3+The ion doping material sample is Er 3+The powder, film, monocrystalline, polycrystalline, glass or the pottery that mix.
The principle of work of measuring method in conversion intermediate level life-span is on a kind of erbium ion of the present invention: (referring to accompanying drawing 1) under the effect of a laser pulse, Er 3+The ion ground state level ( 4I 15/2) on electronics be excited to pumping level (pumping level be under about 800nm laser excitation 4I 9/2, pumping level is under the laser excitation of about 980nm 4I 11/2), this process is that ground state absorbs (GSA).Pumping level instability, the electronics on it can be very fast relax towards the conversion intermediate level ( 4I 13/2) on, last conversion intermediate level is a metastable state, electronics stops several milliseconds at last conversion intermediate level, and ensuing pulse will cause changing portions of electronics on the intermediate level and further is energized into the up-conversion luminescence energy level (the up-conversion luminescence energy level is under about 800nm laser excitation 4S 3/2, the up-conversion luminescence energy level is under about 980nm laser excitation 4F 9/2), this process is excited state absorption (ESA).Last electronics is got back to ground state from the up-conversion luminescence energy level by radiation transistion, sends visible light.Whole process just is called the excited state absorption up-conversion luminescence.
The energy of single laser pulse remains unchanged, and keeps the transition probability of ground state absorption and excited state absorption constant exactly, and the transition probability of establishing the ground state absorption respectively is W GSA, the transition probability W of excited state absorption ESA, establishing the ground state electron number is N, the electron number that is excited on the pumping level of the energy of ground state Electron absorption laser pulse just is NW so GSAChange the time that intermediate level need about hundreds of microsecond owing to relax towards, if the duration of laser pulse is less than 10 nanoseconds, just can think that ground state absorbs and excited state absorption can not be excited by same laser pulse and causes, so excited state absorption is by second (t=t 1), the 3rd (t=2t 1) ... laser pulse excites and causes.Suppose that all can both be relaxed towards the conversion intermediate level by the GSA electrons excited, when interpulse interval greater than 1 millisecond, just can think zero constantly (t=0) to go up the electron number of changing on the intermediate level be NW GSAIf the life-span of going up the conversion intermediate level is τ, the electron number of going up when second laser pulse arrives on the conversion intermediate level is NW just so GSAExp (t 1/ τ), the electron number of going up when the 3rd laser pulse arrives on the conversion intermediate level is NW just GSAExp (2t 1/ τ) ..., the electron number that is excited to the up-conversion luminescence energy level when reaching stable state so just is The intensity I of up-conversion luminescence is proportional to the electron number on the up-conversion luminescence energy level, just
Figure G201010300207220100112D000023
Comprised the life-span τ information of last conversion intermediate level among the luminous intensity I of above conversion.By regulating the frequency f of laser pulse, the time interval t between just adjacent two laser pulses 1, t 1As independent variable, the up-conversion luminescence intensity I is a dependent variable, just can obtain the life-span τ of intermediate level by data fitting.
The present invention is keeping under the constant condition of single pulse energy, realize the control in recurrent interval by the adjusting of excitation pulse frequency, monitor that with the excited state absorption up-conversion luminescence population on the conversion intermediate level changes, derive the life-span of conversion intermediate level with the frequency change of excitation pulse according to up-conversion luminescence intensity, avoided fast ion laser beam technology, postpone to meet the single photon counting technology, these three kinds of technology of pulse-sampling technique will be used the region of ultra-red request detector, adopt single beam, avoided the twin-beam problem in the switch technology and pump probe technology two kinds of technology on the fluorescence, measuring process is simple, has realized the purpose of infrared energy level fluorescence lifetime with the detection of visible-light detector.
Description of drawings
Fig. 1 is the fundamental diagram of the measuring method in conversion intermediate level life-span on a kind of erbium ion of the present invention; Fig. 2 is the device block diagram of embodiment one; Fig. 3 is the relation and the matched curve of the light intensity and the pulsed frequency of embodiment nine.
Embodiment
Embodiment one: the measuring method in conversion intermediate level life-span is carried out according to the following steps on a kind of erbium ion of (referring to accompanying drawing 2) present embodiment: one, be connected with the output control terminal of short-pulse laser with the output channel of concentric cable with delayed signal generator, another output channel be connected with high-voltage pulse generator external trigger end again; Be connected with the external trigger port of enhancement mode electric charge coupling mechanism with the output terminal of concentric cable then high-voltage pulse generator; With the control port and the data acquisition card connection of enhancement mode electric charge coupling mechanism, data collecting card is inserted on the mainboard of computing machine; Enhancement mode electric charge coupling mechanism is inserted in the exit portal of grating spectrograph, and wherein the pulse wavelength of short-pulse laser output is 790nm~820nm or 960nm~1020nm, and the duration of pulse is 100fs~10ns; Two, the centre wavelength with grating spectrograph transfers to 550nm or 660nm, and the gate-width of enhancement mode electric charge coupling mechanism is made as 900 μ s; Three, with tested Er 3+The ion doping material sample is to be fixed on the specimen holder, starts short-pulse laser, and the pulse irradiation that is sent by short-pulse laser is at Er 3+On the ion doping material sample, the fluorescence that sample sends is collected laggard entrance slit of going into spectrometer through collecting lens, demonstrates light intensity on computers; Four, the frequency knob of control lag signal generator makes the frequency f of excitation pulse iBe increased to 1000Hz from 10Hz, and be recorded in different frequency f iPairing light intensity I on the following computing machine iFive, the array I to obtaining i-1/f i, be horizontal marking with 1/f, map for the vertical mark of doing with intensity I, use formula then Match obtains fluorescence lifetime τ.
The fitting formula of present embodiment In, I iFor stimulating frequency is f iThe time go up the conversion integrated intensity, τ is the life-span of last conversion intermediate level, is fitting parameter, A and I 0Be constant to be determined; The constant ground state that is meant that each excitation pulse causes of described single pulse energy absorbs and the excited state absorption probability is a fixed value.
Delayed signal generator in the present embodiment, short-pulse laser, high-voltage pulse generator, enhancement mode electric charge coupling mechanism and grating spectrograph are commercially available equipment.Dotted arrow among Fig. 2 is that concentric cable connects, and solid arrow is the round of light.
Present embodiment is keeping under the constant condition of single pulse energy, realize the control in recurrent interval by the adjusting of excitation pulse frequency, monitor that with the excited state absorption up-conversion luminescence population on the conversion intermediate level changes, derive the life-span of conversion intermediate level with the frequency change of excitation pulse according to up-conversion luminescence intensity, avoided fast ion laser beam technology, postpone to meet the single photon counting technology, these three kinds of technology of pulse-sampling technique will be used the region of ultra-red request detector, adopt single beam, avoided the twin-beam problem in the switch technology and pumping-detection technology two kinds of technology on the fluorescence, measuring process is simple, has realized the purpose of infrared energy level fluorescence lifetime with the detection of visible-light detector.
Embodiment two: what present embodiment and embodiment one were different is: the pulse wavelength of short-pulse laser output is 795nm~815nm in the step 1.Other is identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is: the pulse wavelength of short-pulse laser output is 800nm in the step 1.Other is identical with embodiment one or two.
Embodiment four: what present embodiment and embodiment one to three were different is: the pulse wavelength of short-pulse laser output is 970nm~1010nm in the step 1.Other is identical with embodiment one to three.
Embodiment five: what present embodiment and embodiment one to four were different is: the pulse wavelength of short-pulse laser output is 980nm in the step 1.Other is identical with embodiment one to four.
Embodiment six: what present embodiment and embodiment one to five were different is: the duration of the pulse of short-pulse laser output is 150fs~5ns in the step 1.Other is identical with embodiment one to five.
Embodiment seven: what present embodiment and embodiment one to six were different is: the duration of the pulse of short-pulse laser output is 500fs in the step 1.Other is identical with embodiment one to six.
Embodiment eight: no is for present embodiment and embodiment one to seven: described Er 3+The ion doping material sample is Er 3+The powder of ion doping, film, monocrystalline, polycrystalline, glass or pottery.Other is identical with embodiment one to seven.
Embodiment nine: the measuring method in conversion intermediate level life-span is carried out according to the following steps on a kind of erbium ion of (referring to accompanying drawing 3) present embodiment: one, be connected with the output control terminal of short-pulse laser with the output channel of concentric cable with delayed signal generator, another output channel be connected with high-voltage pulse generator external trigger end again; Be connected with the external trigger port of enhancement mode electric charge coupling mechanism with the output terminal of concentric cable then high-voltage pulse generator; With the control port and the data acquisition card connection of enhancement mode electric charge coupling mechanism, data collecting card is inserted on the mainboard of computing machine, and enhancement mode electric charge coupling mechanism is inserted in the exit portal of grating spectrograph; Wherein the pulse wavelength of short-pulse laser output is 800nm, and the duration of pulse is 130fs; Two, the centre wavelength with grating spectrograph transfers to 550nm, and the gate-width of enhancement mode electric charge coupling mechanism is made as 900 μ s; Three, with tested Er 3+Ion doping lithium niobate monocrystal sample is to be fixed on the specimen holder, starts short-pulse laser, and the pulse irradiation that is sent by short-pulse laser is at Er 3+On the ion doping lithium niobate monocrystal sample, the fluorescence that sample sends is collected laggard entrance slit of going into spectrometer through collecting lens, demonstrates light intensity on computers; Four, the frequency knob of control lag signal generator makes the frequency f of excitation pulse iBe respectively 1000Hz, 500Hz, 333Hz, 250Hz and 200Hz, calculate corresponding 1/f iBe respectively 1ms, 2ms, 3ms, 4ms and 5ms, and corresponding light intensity I on the logger computer iBe respectively 1.0cps, 0.47cps, 0.19cps, 0.16cps and 0.15cps; Five, the array I to obtaining i-1/f i, be horizontal marking with 1/f, map for the vertical mark of doing with intensity I, use formula then Match obtains fluorescence lifetime τ.
The model of the delayed signal generator in the present embodiment is: Spectra-Physics, SDGII; The model of short-pulse laser is: Spectra-Physics, Spitfire; The model of high-voltage pulse generator is: STANFORD RESEARCHSYSTEMS, DG535; The model of enhancement mode electric charge coupling mechanism is: ANDOR, iStar, DH720; The model of grating spectrograph is: BRUKER.Chromex 500IS/SM.
The I of present embodiment gained i-1/f iGraph of a relation as shown in Figure 3, the curve after match is y=Aexp (x/ τ)/[1-exp (x/ τ)]+y 0, A=0.63123 wherein, y 0=0.07323, definite coefficient of match is 0.9889, and the match variance is 0.0059.X=1/f in the following formula draws Er 3+The doped lithium columbate monocrystalline 4I 13/2The fluorescence lifetime τ of energy level=1.94170ms.The Er of Theoretical Calculation 3+The doped lithium columbate monocrystalline 4I 13/2Be 2.3ms the radiation lifetime of energy level, the fluorescence lifetime of actual measurement should be less than 2.3ms, the measured value range of report is 2.2ms~4.6ms at present, so compare with existing measuring technique, the fluorescence lifetime value of present embodiment more approaches its actual value, and measuring accuracy depends on the inhibition degree to radiation trapping, the inhibition degree is high more, the life-span of measuring, the measured value of present embodiment was with a high credibility more near actual value, had effectively suppressed the influence of radiation trapping.

Claims (5)

1. the measuring method in conversion intermediate level life-span on the erbium ion, the measuring method that it is characterized in that the conversion intermediate level life-span on a kind of erbium ion is carried out according to the following steps: one, be connected with the output control terminal of short-pulse laser with the output channel of concentric cable with delayed signal generator, another output channel be connected with high-voltage pulse generator external trigger end again; Be connected with the external trigger port of enhancement mode electric charge coupling mechanism with the output terminal of concentric cable then high-voltage pulse generator; With the control port and the data acquisition card connection of enhancement mode electric charge coupling mechanism, data collecting card is inserted on the mainboard of computing machine; Enhancement mode electric charge coupling mechanism is inserted in the exit portal of grating spectrograph, and wherein the pulse wavelength of short-pulse laser output is 790nm~820nm or 960nm~1020nm, and the duration of pulse is 100fs~10ns; Two, the centre wavelength with grating spectrograph transfers to 550nm or 660nm, and the gate-width of enhancement mode electric charge coupling mechanism is made as 900 μ s; Three, with tested Er 3+The ion doping material sample is fixed on the specimen holder, starts short-pulse laser, and the pulse irradiation that is sent by short-pulse laser is on sample, and the fluorescence that sample sends is collected laggard entrance slit of going into spectrometer through collecting lens, demonstrates light intensity on computers; Four, the frequency knob of control lag signal generator makes the frequency f i of excitation pulse be increased to 1000Hz from 10Hz, and is recorded under the different frequency f i pairing light intensity Ii on the computing machine; Five, the array Ii-1/fi to obtaining is horizontal marking with 1/f, marks mapping with intensity I for vertical the work, uses formula then
Figure F201010300207220100112C000011
Match obtains fluorescence lifetime τ.
2. the measuring method in conversion intermediate level life-span on a kind of erbium ion according to claim 1 is characterized in that the pulse wavelength of short-pulse laser output in the step 1 is 795nm~815nm.
3. the measuring method in conversion intermediate level life-span on a kind of erbium ion according to claim 1 and 2 is characterized in that the pulse wavelength of short-pulse laser output in the step 1 is 970nm~1010nm.
4. the measuring method in conversion intermediate level life-span on a kind of erbium ion according to claim 3 is characterized in that the duration of the pulse of short-pulse laser output in the step 1 is 150fs~5ns.
5. according to the measuring method in conversion intermediate level life-span on claim 1, the 2 or 4 described a kind of erbium ions, it is characterized in that the Er described in the step 3 3+The ion doping material sample is powder, film, monocrystalline, polycrystalline, glass or the pottery that Er3+ mixes.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106290277A (en) * 2016-08-08 2017-01-04 中国科学院苏州生物医学工程技术研究所 A kind of measure the device and method in conversion nano fluorescent particle life-span on single dispersing
CN110095258A (en) * 2019-05-26 2019-08-06 天津大学 Rare earth ion life time of the level measuring device and measuring method in a kind of Active Optical Fiber
CN113155795A (en) * 2021-04-15 2021-07-23 西北核技术研究所 Device and method for directly measuring upper energy level fluorescence lifetime of rare earth element doped optical fiber laser

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106290277A (en) * 2016-08-08 2017-01-04 中国科学院苏州生物医学工程技术研究所 A kind of measure the device and method in conversion nano fluorescent particle life-span on single dispersing
CN106290277B (en) * 2016-08-08 2019-05-14 中国科学院苏州生物医学工程技术研究所 The device and method in conversion nano fluorescent particle service life on a kind of measurement monodisperse
CN110095258A (en) * 2019-05-26 2019-08-06 天津大学 Rare earth ion life time of the level measuring device and measuring method in a kind of Active Optical Fiber
CN110095258B (en) * 2019-05-26 2021-04-27 天津大学 Device and method for measuring energy level life of rare earth ions in active optical fiber
CN113155795A (en) * 2021-04-15 2021-07-23 西北核技术研究所 Device and method for directly measuring upper energy level fluorescence lifetime of rare earth element doped optical fiber laser

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