CN106053400B - For measuring the device of fluorescence lifetime - Google Patents
For measuring the device of fluorescence lifetime Download PDFInfo
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- CN106053400B CN106053400B CN201510520958.8A CN201510520958A CN106053400B CN 106053400 B CN106053400 B CN 106053400B CN 201510520958 A CN201510520958 A CN 201510520958A CN 106053400 B CN106053400 B CN 106053400B
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Abstract
Fluorescence lifetime measurement device provided herein can readily and accurately measure fluorescence lifetime without destroying object to be measured.Fluorescence lifetime measurement device includes multiple pump light electron guns, pump beam combiner, the first, second, and third multimode fibre, optoisolator, wavelength selective reflection optical filter, edge filter and photodiode.
Description
Technical field
Each embodiment of present disclosure is related to the device for measuring fluorescence lifetime.
Background technique
High-power output solid-state laser is using wherein adulterating a small amount of rare earth ion and manufactured with stick or disc-shape
Monocrystalline is as laser generation medium.Here, the doping concentration and fluorescence lifetime of the rare earth ion in laser generation medium are to determine
The core material characteristic of the medium of the oscillating characteristic of laser.
Determine as follows in general, fluorescence lifetime passes through: the decaying for measuring fluorescence intensity by time-resolved fluorescence spectrometry is dynamic
Mechanics.However, conventional fluorescence lifetime measurement is used to select certain wavelength of fluorescence using monochromator, therefore by measuring device collection
There is limitation at minimum aspect.
Method for analyzing doping concentration includes by using ICP-MS (inductive coupling etc. as chemical analysis method
Gas ions mass spectrograph) a small amount of atom of measurement quality method；It is measured with by using spectrophotometric analysis doping concentration
The method of the optical absorption of certain rare earth ion.
In ICP-MS, monocrystalline is dissolved in certain solvent to measure the mass ratio for the atom for forming monocrystalline, and therefore must
Given the test agent must be destroyed to measure, and obtain the average value of the concentration for the rare earth ion being present in inside the solvent.Therefore,
ICP-MS is unable to the doping concentration of the solid sample of measuring stick or disc-shape, and is not capable of measuring the spatial distribution of doping concentration.
Moreover, although optical absorption spectrometry can measure the concentration of disc-shape solid sample, in order to make to enter
The scattering and diffusing reflection (scattered reflection) of the light of sample minimize, two surfaces of disk must all be processed to have be equal to or
Concentration less than the surface of the optical quality of λ/5, and rod shape solid sample cannot be measured by optical absorption spectrometry.And
It is measurable and since only when optical density (OD) (OD) is equal to or less than 4, spectrophotometer just can be measured accurately
Disc thickness is restricted that (in general, using the disk with the thickness equal to or less than about 5mm, but it is according to rare earth ion
Type and doping concentration and change).Spectrophotometer equals or exceeds the light of 3mm using its beam sizes, and passes through light splitting light
The spatial resolution that degree counts measurable doping concentration in disk equals or exceeds 3mm.
Summary of the invention
The target of present disclosure is to solve the above problems, that is, offer can readily and accurately measure fluorescence lifetime
Device.
It includes following fluorescence lifetime measurement device that the embodiment of present disclosure, which provides: multiple pump beams (pump beam,
Pump beam) source, it is configured to the pump beam that output has different wave length；Pump beam combiner, being configured to will be from institute
The pump beam coupling of multiple pump light electron gun outputs is stated, and the pump beam of coupling is output to the first multimode fibre；First
Multimode fibre is configured to transmit the pump beam inputted from pump beam combiner；Optoisolator is configured to transmission from the
The pump beam of one multimode fibre transmission, and be isolated the light beam in the first multimode fibre is inputted；Wavelength selective reflection filters
Piece is configured to transmit the pump beam transmitted from optoisolator, and the fluorescent reflection that will be generated in object to be measured；The
Two multimode fibres, the pump beam for being configured to pass through wavelength selective reflection optical filter are transferred to the object, and will be
The fluorescence generated in the object is transferred to wavelength selective reflection optical filter；Third multimode fibre is configured to transmission in wave
The fluorescence reflected in long selective reflecting optical filter；Edge filter is configured to absorb or reflect to come since third multimode light
The pump beam wavelength of the fluorescence of fibre transmission, and the remaining fluorescence of transmission；And photodiode, being configured to will be from light cutoff filter
The fluorescence of piece transmission is converted into electric signal.
According to present disclosure, fluorescence lifetime can be precisely and easily measured, without destroying object to be measured.
Detailed description of the invention
Example embodiments are more fully described hereinafter with reference to attached drawing now；However, they can be different shape
Formula embodies and should not be construed as limited to embodiment described herein.On the contrary, thesing embodiments are provided so that the disclosure
Content will be thorough and complete, and the range for Example embodiments being fully communicated to those skilled in the art.
In the accompanying drawings, in order to illustrate it is clear, size can be amplified.It will be understood that when an element is referred to as " " two
Element " between " when, can sole component between described two elements, or one or more intermediary elements also may be present.
Identical appended drawing reference refers to identical element always.
Fig. 1 illustrates fluorescence lifetime measurement device according to the embodiment of the present disclosure；
Fig. 2 illustrates the absorption spectrum of the sample by conventional optical absorption spectrometry measurement；With
Fig. 3 illustrates the decaying of the sample measured by fluorescence lifetime measurement device according to the embodiment of the present disclosure
Dynamics.
Specific embodiment
Hereinafter, embodiment is more fully described with reference to the accompanying drawings.Herein with reference to (and intermediate as embodiment
Structure) the cross-sectional view of schematic diagram embodiment is described.After this manner, it will expect as such as manufacturing technology and/or tolerance
Result and diagram shape deviation.Therefore, embodiment should not be construed as limited to the tool in the region illustrated herein
Shape, but may include the deviation caused by for example manufacturing in shape.It in the accompanying drawings, for clarity, can amplification layer and area
The length and size in domain.Identical appended drawing reference in the accompanying drawings indicates identical element.
Term such as ' the first ' and ' the second ' can be used to describe each component, but they should not limit each component.That
A little terms are only used for the purpose for mutually distinguishing a component with other components.For example, without departing substantially from present disclosure spirit and
In the case where range, the first component is referred to alternatively as second component, and second component is referred to alternatively as first component etc..Moreover, ' and/
Or ' it may include either one or two of mentioned component or combination.
Moreover, singular may include plural form, as long as not referring to specifically in sentence.Moreover, in the description
The "comprises/comprising" used indicates that one or more components, step, operation and element exist or be added.
Moreover, unless otherwise defined, otherwise all terms used in this specification, including technical and scientific term, tool
There is the identical meaning that usually will be understood that with the technical staff in related fields.The term defined in common dictionary should be explained
For with meaning identical with what be will be explained in the context of related fields, and unless in addition definition in the present specification, no
The meaning of idealization or excessively form will be then interpreted as having.
It is also noted that in the present specification, " connection ()/combine () " is referred to: be not only directly with another component
In conjunction with a component, and to pass through an intermediate member component in conjunction with another component indirectly.On the other hand, " straight
Connect in succession ()/bind directly () " refer to a component in the case where no intermediate member directly with another component knot
It closes.
Fig. 1 illustrates fluorescence lifetime measurement device according to the embodiment of the present disclosure.
Fluorescence lifetime measurement device according to the embodiment of the present disclosure includes pump beam source unit 100, light beam
Transmitter 200, beam receiver 300 and fluorescence lifetime measurement unit 400.However, such division of component is only based on
The division that function carries out, and therefore actual component is modifiable.
Pump beam source unit 100 may include multiple pump light electron guns 111,113 ..., 11k, pump beam combiner
150 and first multimode fibre (MMF1) 170.Selectively, pump beam source unit 100 can further comprise pump light beam control
Unit 130 processed.
Multiple pump light electron guns 111,113 ..., 11k output have the pump beam of wavelength different from each other.According to this public affairs
The embodiment of content is opened, multiple pump light electron guns 111,113 ..., 11k is exportable to be had in a variety of rare earth ion (Nd3+、Er3 +、Yb3+Deng) excitation electronic state optical absorption peak wavelength light beam.In one embodiment, these multiple pump lights
Electron gun 111,113 ..., 11k may include one or more laser diodes.
Fluorescence lifetime measurement device according to the embodiment of the present disclosure may include that can control multiple pump beams
Source 111,113 ..., the pump beam control unit 130 of 11k.In one embodiment, pump beam control unit 130 can
Multiple pump light electron guns 111,113 ... are controlled, 11k is run in a pulsed mode and driven with square pulse and scheduled repetitive rate
It is dynamic.In one embodiment, pump beam control unit 130 can depend on the variable of the life span of fluorescence to be measured
Mode adjust multiple pump light electron guns 111,113 ..., the repetitive rate and pulse width of 11k.
Pump beam combiner 150 can will be pumped from multiple pump light electron guns 111,113 ..., a branch of or multi beam of 11k output
Pu light beam coupling, and the pump beam of coupling can be output to the first multimode fibre (MMF1).That is, pump beam combiner 150
It can provide for the pump beam with different wave length to be efficiently entered the means to the first multimode fibre 170.In a kind of reality
It applies in mode, pump beam combiner 150 may include the coupler based on waveguide or the combined free space coupling with lens
Clutch.
First multimode fibre 170 is used to transmit the pump beam inputted from pump beam combiner 150.According in the disclosure
The pump beam inputted from pump beam combiner 150 is output to optoisolator by the embodiment of appearance, the first multimode fibre 170
210.In one embodiment, the first multimode fibre 170 may include 171 He of lens in the input terminal of multimode fibre 170
Lens 172 in the output end of multimode fibre 170 are to improve the coupling efficiency of light.
In the prior art, in order to excite a variety of rare earth ions, it is necessary to use various light sources.However, according in the disclosure
Hold, it can be by using multiple pump light electron guns 111,113 ..., 11k and by the pump beam group of the output coupling of pump light electron gun
Clutch 150 configures an integrated pump beam source module.Therefore, it can produce the pump beam with multi-wavelength, thus swash
Send out rare earth ion a variety of.
Moreover, the present invention is advantageous, be: since it is using the first multimode fibre 170, there is no for additional
Optical alignment's (alignment, alignment) needs, and with the conventional time-resolved fluorescence spectrometry that is exposed to free space
Equipment is compared, and environment of the invention can be operated not only in experimental situation, but also can be operated in common (crystalline substance) ingot manufacturing site location.
Moreover, when using laser diodes, it is easy for making the miniaturization of pump light electron gun.
Beam Propagation device 200 may include optoisolator (OI) 210, wavelength selective reflection optical filter 230 and the second multimode
Optical fiber (MMF2) 250.
Optoisolator 210 transmits the pump beam transmitted from the first multimode fibre 170, but will input the first multimode fibre
Light beam isolation in 170.That is, optoisolator 210 is used to for the pump beam generated in pump beam source unit 100 being transferred to
Sample 500, but by the diffusion optical isolation in the fluorescence generated in sample 500 and the second multimode fibre (MMF2) 250 with not by
In input pumping light electron gun unit 100.Sample 500 is object to be measured.
Wavelength selective reflection optical filter 230 is transmitted through the pump beam of optoisolator 210, but reflects in sample 500
The fluorescence of middle generation.That is, when the pump beam that generate in pump beam source unit 100 passes through optoisolator 210 and defeated
When entering to wavelength selective reflection optical filter 230, wavelength selective reflection optical filter 230 will be defeated by the second multimode fibre 250
Enter beam Propagation to sample 500.And wavelength selective reflection optical filter 230 is received by the second multimode fibre 250 in sample 500
The fluorescence of middle generation and the received fluorescence of institute is transferred to beam receiver 300.
The pump beam that second multimode fibre (MMF2) 250 passes through wavelength selective reflection optical filter 230 is transferred to sample
Product 500, and the fluorescence generated in sample 500 is transferred to wavelength selective reflection optical filter 230.In a kind of embodiment
In, the second multimode fibre 250 may include lens 251 in the importation of the second multimode fibre 250 and in the second multimode light
Lens 252 in the output par, c of fibre 250, to improve coupling efficiency.In one embodiment, the second multimode fibre 250
It may include the lens 252 of the lens as convex shape, and by the lens 252 with convex shape, multimode fibre 250 can gather
Collection has 0.1mm or smaller pump beam with a tight waist and the pump beam of aggregation is output to sample 500.Pass through above-mentioned mistake
Journey, the electronic state of the rare earth ion of sample 500 can be excited to 0.1mm or smaller spatial resolution.Herein, by making sample
Product move in the x, y and z directions respectively and emit pump beam, can measure the spatial distribution of fluorescence, and by the process, can count
Calculate the spatial distribution of doping concentration.
State " is opened (ON) " in pumping pulse, fluorescence is continually transmitted by the rare earth ion that pump beam excites, and
Since that time pulse " disconnects (OFF) " state, the fluorescence-intensity decay of rare earth ion.What is had characteristics that is glimmering
Light is transferred to beam receiver 300 by beam Propagation device 200.Especially, in beam Propagation device 200, wavelength selectivity is anti-
It penetrates optical filter 230 and the second multimode fibre 250 is the region that wherein pump beam and signal light coexist, be used to pump beam is defeated
Enter to sample 500 and the fluorescence generated in sample 500 is transferred to beam receiver 300.
The prior art has the drawback that spatial resolution is low and needs optical alignment, thus leads to inconvenience, but according to this
Invention, due to provide the second multimode fibre 250, there is no the needs for additional optical alignment, and be exposed to free sky
Between conventional time resolved spectroscopy compare, operation of the invention can be carried out not only in experimental situation, but also can be usual
(crystalline substance) ingot manufacturing site location carry out.Moreover, can be by the fluorescence lifetime measurement of the sample of various shapes (ingot, stick, disk) to 0.1mm
Or smaller spatial resolution, without destroying sample.
Beam receiver 300 may include third multimode fibre (MMF3) 310, edge filter 330 and photodiode
350。
Third multimode fibre 310 transmits the fluorescence reflected from wavelength selective reflection optical filter 230.Reality according to the present invention
Apply mode, third multimode fibre 310 receive fluorescence reflect from wavelength selective reflection optical filter 230 and by received fluorescence
It is output to edge filter 330.Embodiment according to the present invention, third multimode fibre 310 may include in third multimode fibre
Lens 311 in 310 importation and the lens in the output par, c of third multimode fibre 310 312 are to improve optics coupling
Close efficiency.
Edge filter 330 absorbs or reflection carrys out the pump beam wavelength since the fluorescence of the transmission of third multimode fibre 310,
With the remaining fluorescence of transmission.That is, edge filter 330 absorb or reflect the pump beam wavelength and transmit the fluorescence so that
The optical power for being entered the pump beam in photodiode 350 minimizes.
The fluorescence that photodiode 350 is used to pass through edge filter is converted into electric signal.That is, photodiode 350
Fluorescence is converted into analyzable signal.
In the prior art, monochromator be used to select wavelength, and therefore, it is difficult to minimize fluorescence lifetime measurement device,
But according to the present invention, by the way that beam receiver is reduced to third multimode fibre (MMF3) 130, edge filter 330 and photoelectricity
Diode 350 can be such that fluorescence lifetime measurement device minimizes.Moreover, because provide third multimode fibre 310, there is no for
The needs of additional optical alignment, and compared with the conventional time resolved spectroscopy for being exposed to free space, exist following excellent
Point: operation can be carried out not only in experimental situation, but also can be carried out in common (crystalline substance) ingot manufacturing site location.
Fluorescence lifetime measurement unit 400 is used to analyze the electric signal converted by photodiode 350 to measure the fluorescence longevity
Life.In one embodiment, fluorescence lifetime measurement unit 400 may include amplifier 410, A/D converter 430 and signal point
Parser 450.
Amplifier 410 will be amplified to interpretable size from 350 received signal of photodiode.A/D converter 430 will
The analog signal of amplification is converted into digital signal.Signal analyzer 450 analyzes digital signal to measure fluorescence lifetime.Herein,
20MHZ or bigger broad band amplifier can be used in amplifier 410.In one embodiment, signal analyzer 450 can pass through meter
The average value of duplicate measurement result is calculated to measure fluorescence lifetime.
According to the present invention, pump beam source unit 100 and beam receiver 300 can be integrated and be simplified, fluorescence is thus reduced
The size of lifetime measurement device, and by the first, second, and third multimode fibre 150,250,310, optical path can be simplified,
Additional optical alignment is unnecessary, and operation can be carried out in common manufacturing site location.
In one embodiment, it can further comprise doping concentration computing unit, be configured to based in fluorescence lifetime
The fluorescence lifetime measured in measuring unit 400 calculates the doping concentration of sample by solution math equation (1).
[math equation (1)]
C=Q [(τo/τf)-1]1/2
C indicates doping concentration.Q indicates quenching parameter, τoIt indicates exciting when Nonradiative energy transfer process is not present
The service life of electronic state.τfIt indicates under the conditions of the scheduled doping concentration that wherein fluorescent quenching process occurs in excitation electronic state
Service life.
The concentration for being entrained in the rare earth ion (dopant) in the monocrystalline (main body) wait be used as solid-state laser can be by dividing
The service life for analysing the excitation electronic state of rare earth ion measures.More particularly, excite the service life of electronic state that can be based on decaying
The decaying kinetics of the fluorescence generated in journey are measured by time-resolved fluorescence spectrometry.That is, exciting the ion of electronic state
Nonradiative energy transfer process is proportionally activated with doping concentration, and Fluorescence-quenching occurs, and therefore doping concentration is got over
Greatly, fluorescence lifetime is shorter.Based on these characteristics, doping concentration can be calculated.The Q and τ of the rare earth ion of doping in single crystaloTo work as
The intrinsic constant that material and excitation electronic state determine when being determined, therefore, when measurement fluorescence life τfWhen, it may be determined that doping is dense
Degree.
Hereinafter, it will be obtained in the method and embodiment according to the present invention that obtain doping concentration by the prior art
It is compared between the method for doping concentration.
Fig. 2 illustrates the absorption spectrum of the sample measured by the prior art.
In Fig. 2, x-axis indicates wavelength, and y-axis indicates optical density (OD).
It hereinafter, will be dense with different doping to being obtained by conventional optical absorption spectrometry with math equation (2)
The Nd of the Nd:YAG crystal of degree3+The doping concentration of ion is illustrated.
[math equation (2)]
N=2.3* [OD/ (d* λ)]
OD indicates optical density (OD).The thickness of d expression sample.The absorption cross section of λ expression ion.
Sample with a thickness of 0.31cm, and Nd3+Absorption cross section of the ion at 808nm wavelength is 7.7 × 1020cm2.?
Here, N=1.38 × 1020cm-3Corresponding to 1 atom %Nd3+The doping concentration of ion.It is following to calculate sample A and sample based on this
The Nd of product B3+The doping concentration of ion.The Nd that the display of table 1 is calculated based on math equation (2)3+The doping concentration of ion.
[table 1]
| Sample A | Sample B | |
| Doping concentration | 1.16 atom % | 1.58 atom % |
Sample is excited by 808nm pump beam by using the fluorescence lifetime measurement device of embodiment according to the present invention
Product A and B, and measure the respective Nd of sample A and B3+The decaying kinetics of ion fluorescence (1064nm), as shown in Figure 3.
Fig. 3 illustrates the decaying of the sample measured by fluorescence lifetime measurement device according to the embodiment of the present disclosure
Dynamics.
In Fig. 3, x-axis indicates the time, and y-axis indicates fluorescence intensity.
The fluorescence lifetime that the display of table 2 obtains and the measurement data to Fig. 3 carries out linear fit.Table 2 shows Nd3+Ion
Fluorescence lifetime (τf)。
[table 2]
| Sample A | Sample B | |
| Fluorescence lifetime (μ s) | 124 | 111 |
Quench the constant that parameter Q is the type depending on material.Here, it is assumed that Q is 1.33 ± 0.01 × 1020cm-3, τo
For the life value when fluorescent quenching is not present.Herein, 260 μ s are used as τo.The doping calculated with above-mentioned factor
Concentration is as follows.Table 3 shows Nd3+The doping concentration of ion.
[table 3]
| Cabs[atom %] | τf[μs] | Q[1020cm-3] | |
| Sample A | 1.16 | 124 | 1.32 |
| Sample B | 1.58 | 111 | 1.34 |
Comparison sheet 1 and table 3, it can be seen that the doping concentration and embodiment through the invention calculated by the prior art
Fluorescence lifetime measurement device calculate doping concentration it is identical.
Example embodiments are disclosed herein, and although with specific nomenclature, but they are only summarizing and retouching
The purpose of limitation is used and explained and be not used in the sense that stating.In some cases, such as when the application submits
Those skilled in the art will be it is apparent, about the description of a specific embodiment feature, characteristic and/or want
Element can use individually or with the feature, characteristic, and/or factor combination described about other embodiment, unless clearly
It is otherwise indicated.Therefore, it will be understood by those skilled in the art that without departing substantially from of the invention as illustrated in the following claims
In the case where spirit and scope, a variety of variations in terms of form and details can be carried out.
Claims (9)
1. fluorescence lifetime measurement device, comprising:
Multiple pump light electron guns are configured to the pump beam of output different wave length；
Pump beam combiner is configured to couple the pump beam exported from the multiple pump light electron gun, and will coupling
Pump beam be output to the first multimode fibre；
First multimode fibre is configured to transmit the pump beam inputted from pump beam combiner；
Optoisolator is configured to transmit the pump beam transmitted from first multimode fibre, and will input more than described first
Light beam isolation in mode fiber；
Wavelength selective reflection optical filter is configured to transmit the pump beam transmitted from the optoisolator, and will be to be measured
The fluorescent reflection generated in the object of amount；
Second multimode fibre, the pump beam for being configured to pass through the wavelength selective reflection optical filter are transferred to the object
Body, and the fluorescence generated in the object is transferred to the wavelength selective reflection optical filter；
Third multimode fibre is configured to transmit the fluorescence reflected in the wavelength selective reflection optical filter；
Edge filter is configured to absorb or reflect the pump beam wave come since the fluorescence of third multimode fibre transmission
It is long, and the remaining fluorescence of transmission；With
Photodiode is configured to the fluorescence transmitted from the edge filter being converted into electric signal.
2. device according to claim 1 further comprises fluorescence lifetime measurement unit, it is configured to by analyzing via described
Photodiode conversion electric signal and measure fluorescence lifetime.
3. device according to claim 2 further comprises doping concentration computing unit, it is configured to based on by the fluorescence
The fluorescence lifetime of lifetime measurement unit measurement is based on the doping concentration that math equation (1) calculates the object:
[math equation (1)]
C=Q [(τo/τf)-1]1/2
C is doping concentration, and Q is quenching parameter, τoFor when be not present Nonradiative energy transfer process when the excitation electronic state service life,
And τfFor occur in wherein fluorescent quenching process scheduled doping concentration under the conditions of the excitation electronic state service life.
4. device according to claim 1, wherein at least one of the multiple pump light electron gun includes laser diode.
5. device according to claim 1 further comprises pump beam controller, it is configured to control the multiple pump light
Electron gun,
Wherein the pump beam controller controls the multiple pump light electron gun and runs in a pulsed mode, and with square pulse
It is driven with scheduled repetitive rate.
6. device according to claim 5, wherein fluorescence lifetime range tune of the pump beam controller based on the object
Save the pulse width and the scheduled repetitive rate of the multiple pump light electron gun.
7. device according to claim 1, wherein the pump beam combiner includes coupler based on waveguide or by saturating
Microscope group closes the free space coupling device provided.
8. device according to claim 1, wherein first multimode fibre, second multimode fibre and the third multimode
At least one of optical fiber includes lens in outputting and inputting part to improve optical coupling efficiency.
9. any one of -8 device according to claim 1, wherein second multimode fibre is in the defeated of second multimode fibre
It out include convex lens in part, second multimode fibre has 0.1mm or smaller with a tight waist by convex lens aggregation
Pump beam, and the pump beam of aggregation is output to the object.
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| CN109765206B (en) * | 2019-01-31 | 2020-11-24 | 清华大学 | Method for characterizing two-dimensional material defects and application thereof |
| CN110311293B (en) * | 2019-07-16 | 2020-10-13 | 安徽大学 | Method and system for measuring fluorescence lifetime of laser working substance |
| CN114608807B (en) * | 2022-02-25 | 2024-03-29 | 武汉睿芯特种光纤有限责任公司 | Multi-wavelength fluorescence lifetime measuring device for gain optical fiber |
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| KR102248372B1 (en) | 2021-05-07 |
| CN106053400A (en) | 2016-10-26 |
| KR20160120988A (en) | 2016-10-19 |
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