CN104062269A - Nanosecond time-resolved absorption and emission spectrum measuring device and measuring method - Google Patents
Nanosecond time-resolved absorption and emission spectrum measuring device and measuring method Download PDFInfo
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- CN104062269A CN104062269A CN201310085906.3A CN201310085906A CN104062269A CN 104062269 A CN104062269 A CN 104062269A CN 201310085906 A CN201310085906 A CN 201310085906A CN 104062269 A CN104062269 A CN 104062269A
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Abstract
The invention relates to a nanosecond time-resolved absorption and emission spectrum measuring device. An excitation light source is orderly connected with a first sequence pulse generator, a working frequency coordinator, a second sequence pulse generator, and a data collector; the second sequence pulse generator is respectively connected with a light path system and a detection light source; the data collector is respectively connected with the working frequency coordinator, a first light intensity detector, a second light intensity detector, a third light intensity detector, and a monochromator; the light path system and a sample cell are also disposed between the detection light source and the monochromator. The measuring method comprises: setting the temperature of a sample, irradiating the sample by light beams emitted by the excitation light source to reach an electron excitation state, obtaining zero point time of time-resolved spectrum data by part of the light beams; after pulsed white light emitted by the detection light source passes through the sample, feeding back detection light intensity signals to the data collector, and converting the signals into absorption and emission spectra. The measuring device of the invention is equipped with a temperature controllable sample cell, and obtains spectrum data with a high signal to noise ratio.
Description
Technical field
The present invention relates to a kind of time resolved spectroscopy measurement mechanism and method, especially a kind of under the regulatable condition of sample temperature, can measure respectively instrument and the method for nanosecond time resolution Absorption and emission spectra.
Background technology
The photosynthesis of plant, the light degradation of pollutant reaction provides food source and good living environment for the mankind, study light-triggered physical and chemical process and contribute to understand these spontaneous phenomenons, meanwhile, for further developing clear energy sources and green environmental protection technique, new technical thought is proposed.Under normal circumstances, light triggers chemical reaction path: the material in electronic ground state is during by the light beam irradiates of suitable wavelength, the electronics of this material is triggered to excited state, formation has the intermediate of stronger reactivity, generates final product (document 1: Fan Meigong, the Yao Jiannian of electronics in ground state under varying environment, Tong Zhenhe etc., molecular photochemistry and optical function material science, Beijing: Science Press, 2009).The characteristic of excited state material will greatly affect photochemically reactive path, especially there is long-life excited state material and possessed even more important researching value, this long-life excited state material has the sufficient time, make self active electronics bring into play that it is functional, the life-span of this excited state material is often in time scale interior (the document 2:H.X.Han of nanosecond to millisecond, M.N.Paddon-row and R.F.Howe, Charge separation in mesoporousaluminosilicates, Res.Chem.Intermed., 2008,34,551-564; J.W.Verhoeven, H.J.van Ramesdonk and M.M.Groeneveld, et al.Long-livedcharge-transfer states in compact donor-acceptor dyads,
chemPhysChem, 2005,6,2251-2260), the characteristic that detects excited state material becomes the difficult problem that people need to break through, and time-resolved spectrum test technology becomes the powerful measure of dealing with problems.
Ripe commercialization spectrum test device mainly concentrates on stable state and absorbs and emission spectrometer, most representative two companies that produce this type product are respectively PerkinElmer company of the U.S. (document 3:http: //www.perkinelmer.com/) and French Horiba Jobin Yvon company (document 4:http: //www.horiba.com/cn/), with the spectroscopy equipment of time resolution function, often function is comparatively single, particularly, absorption spectrum or time-resolved emission spectrum that existing a set of equipment can only Measuring Time be differentiated, the time scale of its measurement is the longest in microsecond magnitude, its sample temperature can only be approximately equal to room temperature, cannot regulate and control, //www.edinst.com/) and AppliedPhotophysics company of Britain (document 6:http: //www.photophysics.com/) most representative two companies that produce this type product are respectively Britain EdinburghInstruments Ltd(document 5:http:.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of experimental provision and method of measuring time-resolved Absorption and emission spectra of nanosecond, the technical scheme that the present invention adopted is for achieving the above object:
Nanosecond time-resolved Absorption and emission spectra measurement mechanism, excitation source and First ray pulse producer, frequency of operation telegon, the second train pulse generator, data acquisition unit are linked in sequence; The second train pulse generator is connected with light path system, probe source respectively; Data acquisition unit is connected with frequency of operation telegon, the first light intensity detector, the second light intensity detector, the 3rd light intensity detector, monochromator respectively; Between probe source and monochromator, be also equipped with light path system and sample cell.
Sample, position, monochromator entrance port in light outlets and the sample cell of described probe source are a straight line.
The light beam that described excitation source sends is vertical with the pulsed light beam of probe source transmitting.
Described sample cell comprises: the cavity bottom outside surface of built-in cuvette posts semiconductor cooler, temperature control derby successively, and temperature control derby inside is equipped with liquid-circulating path, and the liquid in low temperature thermostat bath drives liquid to circulation path through ebullator; Cavity inner wall is equipped with temperature sensor.
Nanosecond time-resolved Absorption and emission spectra measuring method, comprise the following steps:
(1) the detection wavelength of setting monochromator;
(2) First ray pulse producer (sends frequency signal I, the II that two-way is identical and triggers respectively excitation source and the work of frequency of operation telegon, frequency of operation telegon sends frequency signal III and triggers the second train pulse generator, and the second train pulse generator sends three road frequency signal IV, V, VI trigger respectively light path system, probe source, data acquisition unit;
(3) sample that excitation source sends in nanosecond pulse light beam irradiates sample cell arrives excited electronic state, its segment beam is reflected to the second light intensity detector through light path system, the second light intensity detector send pulse signal to data acquisition unit the moment at zero point as time resolved spectroscopy data; The pulse white light that probe source sends is through after sample, and after monochromator, by light intensity detector record, this detection light intensity signal feeds back to data acquisition unit;
(4) repeating step (two)～(four), average the detection light intensity signal of data acquisition unit multi collect;
(5) reset the detection wavelength of monochromator and repeat step (two)～(four), the detection light intensity signal mean value during by the different detection of data acquisition unit collection wavelength converts Absorption and emission spectra to.
Described frequency signal I has time delay with respect to frequency signal II.
Described frequency signal V has time delay with respect to frequency signal III.
Described frequency signal VI has time delay with respect to frequency signal III.
Described frequency signal IV is synchronizeed with frequency signal III.
The present invention has following beneficial effect and advantage:
1. the present invention is equipped with temperature adjustable sample cell and a set of equipment have two kinds of measurement patterns for transient absorption and emission spectrum simultaneously.
2. in device of the present invention and measuring method, contribute to obtain the spectroscopic data of high s/n ratio according to the function of requirements set measurement average time.
Brief description of the drawings
Fig. 1 is structural principle schematic diagram of the present invention;
Fig. 2 is the measured transient absorption of the embodiment of the present invention and utilizing emitted light spectrogram;
Fig. 3 is sample pool structure schematic diagram of the present invention;
Wherein: 1 excitation source, 2 probe sources, 3 monochromes or polychromator, 4-1 the first light intensity detector, 4-2 the second light intensity detector, 4-3 the 3rd light intensity detector, 5 data acquisition units, 5-1 data collecting card, 5-2 computing machine, 5-3 oscillograph, 6 sample cells, 7-1 shutter controller, 7-2 shutter, 7-3 catoptron, 7-4 focus lamp, 8-1 First ray pulse producer, 8-2 the second train pulse generator, 9 frequency of operation telegons, 10 cavitys, 11 semiconductor coolers, 12 temperature control derbies, 13 liquid-circulating paths, 14 low temperature thermostat baths, 15 ebullators, 16 temperature sensors, 17 temp controlled meters.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Sample cell in the present invention is controllably arranged on sample a certain temperature within the scope of-50 DEG C-50 DEG C, at wavelength 200nm-900nm, within the scope of time 50ns-2ms, measure the time resolution Absorption and emission spectra of sample excitation state, its minimum strength resolution approximately 0.0005, survey frequency is adjustable within the scope of 1Hz-5Hz, in order to obtain high s/n ratio, the present invention adopts the mode that repeatedly measurement is averaged to obtain final experimental result, and average time is adjustable.This device will and be sought environmental protection new departure for development clear energy sources regeneration techniques reliable technical support will be provided.
The present invention who completes according to the above-mentioned object that will reach, to complete as follows surveying work mode: first set sample temperature, excitation source excites the sample to certain excited electronic state, in the time that probe source is in running order, the pulse that it sends strengthens white light through excited state material, the white light seeing through is measured by light intensity detector, subsequent data acquisition system records light intensity be converted to transient absorption spectra data, when probe source is during in closed condition, the sample utilizing emitted light of excited electronic state is directly measured by light intensity detector, subsequent data acquisition system records light intensity be converted to Instantaneous emission spectrum data, the working time order of each part mentioned above has been coordinated jointly by train pulse generator and frequency of operation telegon.
As shown in Figure 3, the controlled sample cell of temperature in the present invention, test sample controllably can be set as to a certain temperature between-50 DEG C to 50 DEG C, its constituted mode is: utilize red copper or aluminium material to make the cavity 10 that can place cubic shape quartz colorimetric utensil, this cavity three has been worn circular hole 18 can printing opacity, bottom surface is level and smooth, the chill surface of semiconductor cooler 11 is closely sticked on to above-mentioned cavity 10 lower surfaces with heat-conducting glue, semiconductor cooler 11 another sides are closely connected with temperature control derby 12 use heat-conducting glues, this temperature control derby 12 is derby empty in, and with an entrance for influent and an outlet for trickle, this entrance and exit is connected with low temperature thermostat bath 14 by water pipe, form liquid-circulating path, liquid in low temperature thermostat bath 14 drives via ebullator 15, the controlled liquid of temperature is flowed in continuous liquid-circulating path in temperature control derby 12, controllable metal piece 12 temperature equal the fluid temperature in cryostat, 14, in the time supplying positive voltage to semiconductor cooler, sample temperature in quartz colorimetric utensil will decline, and in the time supplying negative voltage to semiconductor cooler, the sample temperature in quartz colorimetric utensil will raise, temperature sensor 16 is popped one's head in and is deeply placed on inside cavity, external temp controlled meter 17, when measuring temperature while reaching design temperature, sensor sends instruction and stops power supply, and in the time measuring temperature departure design temperature, temp controlled meter 17 sends instruction powers to reach the object of regulating and controlling temperature to semiconductor cooler.By the fluid temperature in voltage supplied size and low temperature thermostat bath is reasonably set, this sample cell 6 can be realized between-50 DEG C to 50 DEG C and controllably set sample temperature.
Frequency of operation telegon 9 in the present invention, its effect is probe source 2 collaborative works that make the excitation source of high repetition frequency work 1 and low-repetition-frequency work.Under normal circumstances, excitation source 1 need to just can obtain stable mode of operation under higher repetition frequency, and probe source 2 need to obtain stable mode of operation under lower repetition frequency, the high repetition frequency trigger pip of excitation source 1 is reduced to suitable low frequency signal by this frequency of operation telegon 9, and as the external trigger signal of probe source 2, so, excitation source 1 and probe source 2 just can synchronous coordination work.
Integrated electronic chip model and connected mode that frequency of operation telegon 9 uses are as follows: first the trigger pip of high repetition frequency passes through phase inverter I(chip model 7404), then pass through counter (chip model CD4040), pass through again Sheffer stroke gate (chip model CD4011), pass through again phase inverter II(chip model 7404), pass through again Sheffer stroke gate (chip model 7400), export the negative pulse with certain phase shifts and pulse width through 2 monostalbe triggers (chip model 74123) subsequently, finally by the tunable final external trigger signal of overpower amplifier (chip model 74128) output low-repetition-frequency width, the wherein delivery outlet of another input end connection data capture card 5-1 of Sheffer stroke gate mentioned above (chip model 7400), in the time that computing machine 5-2 sends high level instruction by this data collecting card 5-1, this Sheffer stroke gate is in opening state, in the time that computing machine 5-2 sends low level instruction by this data collecting card 5-1, this Sheffer stroke gate is in closed condition, so just can realize the computer gate-controlled switch function of this device, in addition, phase inverter II(chip model 7404 mentioned above) output connect the monostalbe trigger (chip model 74123) of two series connection simultaneously, its output signal is given the Protection Counter Functions pin of counter mentioned above (chip model CD4040).
Light path system 7, for controlling beam diameter size and the direction of propagation, can adopt optical reflection, concentrating element and mechanical shutter, and the present embodiment comprises a shutter controller 7-1, two shutter 7-2, a catoptron 7-3, a focus lamp 7-4.Wherein, shutter 7-2, a catoptron 7-3 and a focus lamp 7-4 order are positioned between excitation source and sample, and this shutter is for stopping unnecessary excitation light pulse; Another shutter 7-2 is placed between probe source and sample, for stopping unnecessary detection irradiation.
Data acquisition unit 5 comprises data collecting card 5-1, computing machine 5-2 and oscillograph 5-3.The data that data collecting card 5-1 sends for acquisition pulse signal generator 8, are connected with frequency of operation telegon 9, second train pulse generator 8, light intensity detector 4-1, computing machine 5-2; Computing machine 5-2 is used for gathering the light intensity data of oscillograph 5-3, and light intensity data is converted to transient absorption spectra data; Computing machine 5-2 is connected with monochromator 3, oscillograph 5-3; Oscillograph 5-3 is used for reading light intensity data, is connected with light intensity detector 4-2,4-3.
Fig. 1 has shown Technology Roadmap of the present invention.Laboratory sample is the benzil acetonitrile solution 3mL of 4mM, first the temperature of setting this liquid by the controlled sample cell 6 of temperature is 22 DEG C, it is 350nm that computing machine 5-2 specifies the measurement wavelength coverage of monochromator 3 by instruction, and setting excitation source 1 pulse characteristic of sending is 33mJ@355nm.As shown in Figure 1, first, by the DG535 of SRS company of the train pulse generator 8-1(U.S.) to send two-way repetition frequency be that the trigger pip of 10Hz is respectively I and II, wherein signal I postpones 9ms than II, II passes to frequency of operation telegon 9 as input signal, now the Computercontrolled data acquisition card 5-1 in data acquisition unit 5 has sent high level signal VII to open frequency of operation telegon 9, through reducing after frequency effect, frequency of operation telegon 9 sends the low-repetition-frequency 3Hz signal III of synchronizeing with II, this signal passes to second DG645 of SRS company of the train pulse generator 8-2(U.S. as external trigger signal), it sends the signal IV of three road 3Hz, V, VI, wherein IV is synchronizeed in time with III, two mechanical shutter 7-2 open duration 12ms in opening after receiving IV, V postpones 7.3ms than III, probe source 2 is after receiving V, sending pulse width is the enhancing white light pulse of 6ms, VI postpones 13ms than III, data collecting card 5-1 starts record data receiving after this signal VI.Excitation source 1 is after receiving I, it sends the nanosecond pulse light beam that wavelength is 355nm, irradiate sample and arrive excited electronic state, the pulse white light that now probe source 2 sends just passes to vertical exciting light direction excited electronic state sample, its transmitted light is after monochromator after 3, by light intensity detector 4-3 record, strength signal passes to the oscillograph 5-3 in data acquisition unit 5, the small part of excitation pulse light is reflected to the light intensity detector 4-2(nanosecond open-interval photodiode in left side in Fig. 1) time, it sends a pulse signal and sends the zero point moment of oscillograph 5-3 as time resolved spectroscopy data to, subsequent data capture card 5-1 is receiving after VI, by the data storage in oscillograph 5-3, complete one-shot measurement process, go out continuous coverage 100 times in the 350nm position of monochromator 3, using average result as final testing result, the detection wavelength that computer is set monochromator 3 is subsequently for being 355nm, again measure 100 times in this position, and store average result, so circulation, until the detection wavelength of monochromator 3 is 650nm, and complete 100 measurements and be averaged after result, whole experimentation finishes, experimental data is stored in computer.
Fig. 2 has shown the experimental result that above-mentioned experimentation obtains, this figure is that 4mM benzil acetonitrile solution is under 33mJ@355nm shooting conditions, the transient absorption and the utilizing emitted light spectrogram that obtain, because single wavelength result is on average to be obtained by 100 measurement results, so the signal to noise ratio (S/N ratio) of these data is higher, wherein contain abundant physical chemistry intension, had very large scientific research to be worth.Fig. 3 has shown the pictorial diagram of the controlled sample cell of temperature in apparatus of the present invention, and this sample cell is durable, with other element cooperating well in the present invention.
Claims (9)
- Nanosecond time-resolved Absorption and emission spectra measurement mechanism, it is characterized in that: excitation source (1) and First ray pulse producer (8-1), frequency of operation telegon (9), the second train pulse generator (8-2), data acquisition unit (5) are linked in sequence; The second train pulse generator (8-2) is connected with light path system (7), probe source (2) respectively; Data acquisition unit (5) is connected with frequency of operation telegon (9), the first light intensity detector (4-1), the second light intensity detector (4-2), the 3rd light intensity detector (4-3), monochromator (3) respectively; Between probe source (2) and monochromator (3), be also equipped with light path system (7) and sample cell (6).
- Nanosecond according to claim 1 time-resolved Absorption and emission spectra measurement mechanism, it is characterized in that: sample, monochromator (3) position, entrance port in the light outlets of described probe source (2) and sample cell (6) are a straight line.
- Nanosecond according to claim 1 time-resolved Absorption and emission spectra measurement mechanism, it is characterized in that: the pulsed light beam of the light beam that described excitation source (1) sends and probe source (2) transmitting is vertical.
- Nanosecond according to claim 1 time-resolved Absorption and emission spectra measurement mechanism, it is characterized in that: described sample cell (6) comprising: cavity (10) bottom outer surface of built-in cuvette posts semiconductor cooler (11), temperature control derby (12) successively, temperature control derby (12) inside is equipped with liquid-circulating path (13), and the liquid in low temperature thermostat bath (14) drives liquid in circulation path (13) through ebullator (15); Cavity (10) inwall is equipped with temperature sensor (16).
- Nanosecond time-resolved Absorption and emission spectra measuring method, it is characterized in that comprising the following steps:(1) the detection wavelength of setting monochromator (3);(2) First ray pulse producer (8-1) sends frequency signal I, the II that two-way is identical and triggers respectively excitation source (1) and frequency of operation telegon (9) work, frequency of operation telegon (9) sends frequency signal III and triggers the second train pulse generator (8-2), and the second train pulse generator (8-2) sends three road frequency signal IV, V, VI trigger respectively light path system (7), probe source (2), data acquisition unit (5);(3) sample that excitation source (1) sends in nanosecond pulse light beam irradiates sample cell (6) arrives excited electronic state, its segment beam is reflected to the second light intensity detector (4-2) through light path system (7), the second light intensity detector (4-2) send pulse signal to data acquisition unit (5) moment at zero point as time resolved spectroscopy data; The pulse white light that probe source (2) sends is through after sample, and after monochromator (3), by light intensity detector (4-3) record, this detection light intensity signal feeds back to data acquisition unit (5);(4) repeating step (two)～(four), average the detection light intensity signal of data acquisition unit (5) multi collect;(5) reset the detection wavelength of monochromator (3) and repeat step (two)～(four), detection light intensity signal mean value when data acquisition unit (5) is gathered to different detection wavelength converts Absorption and emission spectra to.
- Nanosecond according to claim 5 time-resolved Absorption and emission spectra measuring method, it is characterized in that: described frequency signal I has time delay with respect to frequency signal II.
- Nanosecond according to claim 5 time-resolved Absorption and emission spectra measuring method, it is characterized in that: described frequency signal V has time delay with respect to frequency signal III.
- Nanosecond according to claim 5 time-resolved Absorption and emission spectra measuring method, it is characterized in that: described frequency signal VI has time delay with respect to frequency signal III.
- Nanosecond according to claim 5 time-resolved Absorption and emission spectra measuring method, it is characterized in that: described frequency signal IV is synchronizeed with frequency signal III.
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| CN109557039A (en) * | 2017-09-25 | 2019-04-02 | 中国科学院大连化学物理研究所 | The super-narrow line width infrared absorption spectrum measurement apparatus and method that gsec is differentiated |
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| CN114113003A (en) * | 2020-08-28 | 2022-03-01 | 中国科学院大连化学物理研究所 | In-situ monitoring chemical reaction double-cascade buckle stray light emission spectrum measuring device |
| CN114113003B (en) * | 2020-08-28 | 2024-05-07 | 中国科学院大连化学物理研究所 | In-situ monitoring chemistry chemical reaction double cascade button stray light emission spectrum measuring device |
| CN112229804A (en) * | 2020-09-17 | 2021-01-15 | 中国科学院上海光学精密机械研究所 | Non-coaxial transmission type ultrafast transient absorption system with temperature field regulation and control function and measurement method |
| CN112229804B (en) * | 2020-09-17 | 2021-07-06 | 中国科学院上海光学精密机械研究所 | Non-coaxial transmission type ultrafast transient absorption system with temperature field regulation and control function and measurement method |
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