CN207396352U - One kind face the wall and meditate material 3D microcells fuel be detained nondestruction quantitative analysis equipment - Google Patents

Abstract

The utility model discloses one kind face the wall and meditate material 3D microcells fuel be detained nondestruction quantitative analysis equipment.By using this equipment, and combine corresponding software and algorithm, induced with laser desorption techniques combination thermal desorption mass-spectrometric technique can be achieved, opposite walls material fuel is detained high-space resolution (μm magnitude), high depth differentiates (nm to mm magnitudes), lossless quantitative analysis.Its detection limit is low, detectivity is high, sample is without pretreatment, quickly (s magnitudes) can analyze sample.In addition, by using partial pressure calibration method, this method can be used for other gas molecules of quantitative analysis and organic molecule.

Description

One kind face the wall and meditate material 3D microcells fuel be detained nondestruction quantitative analysis equipment

Technical field

The utility model is related to detection technique field more particularly to one kind face the wall and meditate material 3D microcells fuel be detained harmless quantitative Analytical equipment.

Background technology

In fusion facility tokamak operational process, since magnetic field is to the imperfection of Particle confinement, as neutral particle, Plasma and device can occur for charge-exchange, Plasma disruption between particle that the magnetic line of force transports, charged particle etc. Wall interacts (Plasma-Wall-Interaction, PWI).PWI is a multi-crossed disciplines, more physics and chemical process Coupling and the challenge of multiple dimensioned variation, it may be said that when can tokamak magnetic confinement nuclear fusion or can be finally real It is existing, it is largely dependent upon the research and control of PWI processes.A key issue is during PWI：It faces the wall and meditates material (PFMs) Under fusionplasma irradiation, back scattering, desorption, physical sputtering, chemical attack, structural damage, impurity deposition, combustion will occur The complicated phenomenons such as material delay.These will make PFMs surface-element ingredients change, and fuel recycling control be influenced, so as to influence Plasma restraint performance causes various plasma instabilitys, reduces fusionplasma quality, even results in plasma Body ruptures.To realize that long pulse, high constraint, one of the electric discharge stablized, key issue are to want in Tokamak nuclear fusion device It understands and waits fusion ions body (mainly deuterium, tritium and helium) and the mechanism of PFMs interactions, wherein the important point is exactly poly- Become plasma fuel retention mechanism.Especially understand that the impurity deposition in the gap between divertor tile and fuel are detained pole To be important, this is because the cleaning and detection to the gap between tile are more difficult compared to other positions PFMs.Filter partially The fuel delay of device position plays an important role to the safe steady-state operation of device, and the maximum tokamak device currently built is international In thermonuclear fusion experimental reactor (International Thermonuclear Experimental Reactor, ITER) vacuum chamber The safe dose of tritium is 700g.The steady state Safe Operation of following superconducting tokamak device is to fuel in tokamak PFMs walls Being detained requirement can be very stringent, the deep understanding to fuel retention mechanism be current international fusion circle research hotspot and difficult point it One.The analysis method being detained at present to divertor PFMs fuel is concentrated mainly on off-line analysis, i.e., takes turns and discharge in fusion facility one After, vacuum chamber is opened, PFMs materials is taken out, is then analyzed it using means such as various electron beams, ion beams.

Current main off-line analysis means include nuclear reaction analysis method (Nuclear Reaction Analysis, NRA), Secondary Ion Mass Spectrometry (Secondary Ion Mass Spectroscopy, SIMS), tritium imaging technique (Tritium Image Photo Technology, TIPT), Auger electron spectroscopy (Auger Electron Spectroscopy, AES), X Photoelectron spectroscopy (X-ray Photoelectron Spectroscopy, XPS), X-ray diffractometer (X-Ray Diffraction, XRD), scanning electron microscope-energy dispersive spectra (Scanning Electron Microscope- Energy Dispersed Spectroscopy, SEM-EDS), atomic force microscope (Atomic Force Microscope, AFM), Laser Scanning Confocal Microscope (Confocal Microscopy, CM), focused ion beam-scanning electron microscope (Focus Ions Beam- Scanning Electron Microscope, FIB-SEM), laser induced breakdown spectroscopy (Laser Induced Breakdown Spectroscopy, LIBS), glow discharge emission spectrum (Glow Discharge-Optical Emission Spectroscopy, GD-OES), thermal desorption mass spectrum (Thermal Desorption Spectroscopy, TDS) Deng the relevant information for obtaining hydrogen isotope delay.

NRA technologies are especially effective to light element analysis, and depth resolution is preferable, and interference is small, anti-by D (3He, P) 4He cores The depth profile of fuel D should be measured, but its analysis depth is generally in a μm magnitude.SIMS is usually sputtered with Cs+, Ar+, O+, detection There is no limit for depth, but cost is very costly and time consuming, usually analyzes the fuel stay information of sample surfaces few microns below.TIPT The β x ray exposure xs imaging generated with tritium decay obtains the EDS maps information of tritium, but only sensitive to the tritium of 1 μm of distribution below surface, It is appropriate for the distribution detection of large area.AES is a kind of surface analysis technique for utilizing high-power electron beam as excitaton source, is analyzed Region excited atom launches the auger electrons with elemental characteristic, according to the spectral peak for having elemental characteristic in electron spectrum, thus it is speculated that The composition information of analyzed area, but Auger process at least will be there are two energy level and three electronic parameters, it is impossible to analyze hydrogen isotope And helium atom, the fuel stay information in measured material can only be speculated by indirect means.XPS is inspired using x-ray photon The inner electron of material surface atom by analyzing electron energy to obtain a kind of power spectrum, can carry out quantitative analysis to sample, But XPS cannot analyze hydrogen and helium element, and the analysis depth of XPS is generally sub-nanometer magnitude in addition and quantitative accuracy is poor.XRD Collection of illustrative plates can be used for sample crystal structure, grain size, stress and the equal analysis of object, it is impossible to analyze sample surface into Divide information.SEM-EDS technologies can not only characterize the microscopic appearance of sample, and semi-quantitative analysis can be also carried out to sample, but Its generally μm magnitude that fathoms, and the magnetic sample of tool cannot be analyzed.AFM and CM can only be to sample surface morphology, table Surface roughness and irregularity degree are characterized, it is impossible to carry out quantitative elementary analysis to sample.FIB-SEM technologies use high-strength It spends focused ion beam and cuttings of the nm to μm magnitude is carried out to material, the depth information of fuel retention layer can be analyzed, but cannot Quantitative analysis is detained to fuel.LIBS be it is a kind of can with remote control, in real time, the micro- damage analysis that detects simultaneously of online, multielement Technology can carry out analyzed sample 3D microcell imagings, however the current technology facing challenges limit not low enough, matrix for detection Effect is serious, and quantitative analysis precision is poor.GD-OES is that sample is carried out using the plasma that glow discharge generates Etching realizes the quantitative analysis to sample ingredient by the emission spectrum for gathering etching sample, which has higher Depth resolution, but measurement of spatial resolution cannot be carried out to sample, and have stringent limitation to the size of sample. TDS thermal desorption mass spectrums are that in high vacuum conditions, laboratory sample is heated by certain heating rate, so that sample is inhaled Attached gas desorption comes out, and records the chemical molecular partial pressure variation with temperature relation desorbed, is obtained from the spectrum of record sharp The information such as living energy, lattice vibration frequency, the adsorption form of gas and absolute gas adsorbance.

TDS is that fusion is studied towards the most effective means of fuel delay and dispersal events in plasma facing materials, The absolute hold-up of the gas being illuminated in material can accurately be analyzed.However this method can only be to the gas that is adsorbed on entire sample Molecule carries out absolute quantification analysis, but space cannot be carried out to the gas adsorbed in sample and the absolute of depth resolution is determined Amount analysis.Additionally due in TDS the thermodynamic property of heating module material limitation, cause highest can heating temperature limited System, furthermore sample needs fixed and is by entire block thermally equivalent in TDS devices, therefore cannot add sample Thermotropic fusing, this results in another limitation of TDS：The gas that cannot be adsorbed completely in desorption PFMs materials.For fusion support The PFMs materials at Karma gram device divertor position, a large amount of ions and He ashes generated due to fusion are all discharged via divertor, The gradient abnormal distribution that fuel is trapped in this divertor region is precipitous, such as deposits dominates district, etching dominates district, divertor watt seam The fuel in the regions such as area and the divertor back side is detained.Urgent need, which will be developed, a kind of can carry out spatial depth distribution measuring, Gao Ling The lossless PFMs fuel of sensitivity is detained analysis method.

Utility model content

The purpose of this utility model is：In order to realize the imaging of 3D microcells, can realize high-space resolution μm magnitude, gradient type Depth resolution (nm to mm magnitudes), high detection sensitivity, quick, high accurancy and precision, active, material fuel element of facing the wall and meditating detection and Nondestruction quantitative analysis method of the sample without pretreatment, a kind of special equipment provided.

The utility model provide one kind face the wall and meditate material 3D microcells fuel be detained nondestruction quantitative analysis equipment：Sample heated mould Block heats sample by way of heat transfer；Computer connects FPGA tfi modules by PXI Express ports, passes through USB, serial ports and quadruple mass-spectrometer connection are connected by network interface with ICCD cameras；FPGA tfi modules are connected by bnc interface ICCD cameras and desorption laser；The laser sent pass through with the laser beam expanding instrument of laser propagation direction placement in 90 °, pass through again Cross the laser energy regulator control system with the placement in 90 ° of laser propagation direction；It is divided by the laser of laser energy regulator control system Two beams, beam of laser are reflected in the remaining laser absorption device in 90 ° with laser light incident direction, and another beam of laser is along original There is direction to continue to propagate forward, after the quartz plate angled with incident laser, the sub-fraction laser reflected shines It is mapped on Joulemeter, scatters illumination and be mapped on photodiode；The angle that quartz plate is placed is according to the location determination of Joulemeter；It cuts Ripple device is placed in the light path in 90 ° with incident laser；Via chopper outgoing laser by with laser light incident direction is at 45 ° puts The laser high reflection mirror reflection put；The laser reflected is focused on the parabolic mirror of laser light incident direction placement at 45 ° To being placed on the sample of parabolic mirror focal point；Resolved gas is detected by quadruple mass-spectrometer, via string Mouth and USB port are transferred data in computer；The angle that ICCD cameras are placed is parallel with sample normal direction；Pass through adjusting The region that the lens focus of ICCD cameras interacts to laser with sample is shot；ICCD cameras are passed data by network interface It is defeated to arrive computer.

Preferably, FPGA tfi modules connect oscillograph by bnc interface；Oscillograph connects the first light by BNC interfaces Electric diode, the second photodiode and Joulemeter.

Preferably, FPGA tfi modules add detector by bnc interface connection spectrometer；Spectrometer adds detector to pass through SMA905 interfaces are connected with detection optical fiber；The position that detection optical fiber is placed is arrived according to the focal length of emission spectrum collecting lens with lens The distance of Al-flim reflector determines jointly plus the distance of Al-flim reflector to sample；Detection optical fiber end face and emission spectrum Collecting lens plane is parallel；The angle that Al-flim reflector is placed is condenser lens normal and the 1/2 of sample normal angulation；Light Spectrometer adds detector to be connected with computer by USB interface.

Advantageous effect：By using this equipment, and corresponding software and algorithm are combined, it can be achieved that induced with laser desorption skill Art combination thermal desorption mass-spectrometric technique, opposite walls material fuel is detained high-space resolution (μm magnitude), high depth differentiates (nm to mm amounts Grade), lossless quantitative analysis.Its detection limit is low, detectivity is high, sample is without pretreatment, quickly (s magnitudes) can analyze quilt Sample.In addition, by using partial pressure calibration method, this method can be used for other gas molecules of quantitative analysis and organic point Son.

Description of the drawings

The mass spectrographic material 3D microcells fuel of facing the wall and meditating of Fig. 1 the utility model induced with laser desorption combination thermal desorptions is detained lossless Quantitative analytical device schematic diagram.

The mass spectrographic material 3D microcells fuel of facing the wall and meditating of Fig. 2 the utility model induced with laser desorption combination thermal desorptions is detained lossless Quantitative analytical device schematic device.

Fig. 3 high-space resolution induced with laser desorption combination thermal desorption mass-spectrometric technique opposite walls material fuels isotope is detained Analysis result A.

Fig. 4 high-space resolution induced with laser desorption combination thermal desorption mass-spectrometric technique opposite walls material fuels isotope is detained Analysis result B.

Attached drawing identifies：

B1. data collection and analysis module, B2. time-sequence control modules, B3. pulse-width tunables laser (fs-ms) module, B4. laser energy regulation and control are tested with detection module, B5. laser pulse widths regulation and control module, B6. samples state detection module, B7. Sample surface morphology real-time monitoring module, B8. sample surfaces reflectivity monitoring module, B9.ICCD temperature measurement modules, B10. transmitting light Compose monitoring modular, B11. thermal desorptions module, B12. heating modules, B13. detecting modules, B14. samples.

C1. computer, C2.FPGA sequential, C3. data acquisitions storage and analysis oscillograph, C4. desorptions laser, C5. Laser beam expanding instrument, C6. laser energies regulator control system, C7. remnants' laser absorption device, C8. quartz plates, C9. Joulemeters, C10. One photodiode, C11. choppers, C12. laser high reflection mirror, C13. parabolic mirrors, C14. samples, C15.The removable sample heating module of the four-dimension, C16. quadruple mass-spectrometers, the second photodiodes of C17., C18.ICCD cameras, C19. Al-flim reflector, C20. emission spectrum collecting lens, C21. detection optical fibers, C22. spectrometers add detector.

Specific embodiment

The technical issues of to solve the utility model, the technical solution used and the technique effect reached are clearer, The utility model is described in further detail with reference to the accompanying drawings and examples.It is it is understood that described herein Specific embodiment is used only for explaining the utility model rather than the restriction to the utility model.It also should be noted that it is Convenient for description, part relevant with the utility model rather than full content are illustrated only in attached drawing.

Fig. 1 is refer to, the equipment principle of the utility model with lower module by forming：Data collection and analysis module B1 (its work( There can be mass spectrometric data acquisition；Emission spectra data gathers；Energy real-time monitoring data gathers；Sample surface temperature gathers in real time； Surface topography data gathers in real time；Surface reflectivity real time data acquisition；The temperature control of TDS heating modules and data acquisition；To acquisition Data are analyzed；Control sequential synchronization module), time-sequence control module B2 (its function have control laser sequential；Temporal regulation Laser pulse width module under long pulse；Temporal regulation ICCD temperature measurement modules；Temporal regulation emission spectrum module；Timing control oscillograph Data acquisition), pulse-width tunable laser B3 (fs-ms) module (its function have change measurement Z resolution ratio；Desorption is measured Sample), laser energy regulation and control (its function has adjusting incident laser energy with detection module B4；Measure desorption laser energy), Laser pulse width regulation and control module B5 (its function is in long pulse condition down regulation laser pulse width), sample state detection module (its function has observation sample tested region by B6, sample surface topography real-time monitoring module B7；Calculate the attached space of laser desorption point Resolution；Observation sample surface morphology), sample surfaces reflectivity monitoring module B8 (its function have calculate sample surfaces reflectivity；It comments Whether valency laser causes to damage to sample), (its function has real-time detection sample surface temperature to ICCD temperature measurement modules B9；Meter Calculate the attached spatial resolution of laser desorption and sample surface topography real-time monitoring module B7 cross validations), emission spectrum monitors (its function has whether monitoring sample is damaged and generates laser plasma to module B10；Analyze the laser plasma generated), (its function has heating sample by thermal desorption module B11, heating module B12；Auxiliary heating sample), detecting module B13 (its function has the gaseous sample that detection desorption goes out), sample B14.

Embodiment

Fig. 2 is refer to, material 3D microcells fuel of facing the wall and meditating is detained nondestruction quantitative analysis equipment, and sample heating module C15 leads to The mode for crossing heat transfer heats sample C14；Computer C1 by PXI Express ports connect FPGA tfi modules C2, It is connected by USB, serial ports and quadruple mass-spectrometer C16 connections, by network interface with ICCD cameras C18；FPGA tfi modules C2 passes through Bnc interface connects ICCD cameras C18 and desorption laser C4；The laser sent passes through and the placement in 90 ° of laser propagation direction Laser beam expanding instrument C5, using the laser energy regulator control system C6 with the placement in 90 ° of laser propagation direction；Pass through laser energy The laser of regulator control system C6 is divided into two beams, and beam of laser is reflected to inhales with laser light incident direction remaining laser in 90 ° It receives in device C7, another beam of laser continues to propagate forward along original direction, by the quartz plate angled with incident laser After C8, the sub-fraction laser that is reflected, which is irradiated on Joulemeter C9, scatters illumination is mapped on photodiode C10；Quartz plate The angle that C8 is placed is according to the location determination of Joulemeter C9；Chopper C11 is placed in the light path in 90 ° with incident laser；Through It is reflected by the laser that chopper C11 is emitted with the laser high reflection mirror C12 of laser light incident direction placement at 45 °；It is reflected Laser is focused on by the parabolic mirror C13 with the placement at 45 ° of laser light incident direction and is placed on parabolic mirror C13 On the sample C14 of focal point；Resolved gas is detected by quadruple mass-spectrometer C16, passes data via serial ports and USB port In the defeated C1 to computer；The angle that ICCD cameras C18 is placed is parallel with sample normal direction；By adjusting ICCD cameras C18's The region that lens focus interacts to laser with sample is shot；ICCD cameras C18 transfers data to meter by network interface Calculation machine C1.

FPGA tfi modules C2 connects oscillograph C3 by bnc interface；Oscillograph C3 connects the first light by BNC interfaces Electric diode C10, the second photodiode C17 and Joulemeter C9.

FPGA tfi modules C2 connects spectrometer by bnc interface and adds detector C 22；Spectrometer adds detector C 22 to pass through SMA905 interfaces are connected with detection optical fiber C21；The position that detection optical fiber C21 is placed is according to the coke of emission spectrum collecting lens C20 It is determined jointly away from the distance that Al-flim reflector C19 to sample C14 is added with the distance of lens C20 to Al-flim reflector C19； Detection optical fiber C21 end faces are parallel with emission spectrum collecting lens C20 planes；The angle that Al-flim reflector C19 is placed is saturating to focus on Mirror normal and the 1/2 of sample normal angulation；Spectrometer adds detector C 22 to be connected with computer C1 by USB interface.

Specifically used method：Comprise the following steps：

First,The removable sample heating module C15 of the four-dimension heats sample C14, and temperature is arrived in 300K 1300K is controllable；Secondly, computer C1 controls desorption laser C4 to send desorption laser by FPGA sequential C2, passes through successively It is anti-to cross laser beam expanding instrument C5, laser energy regulator control system C6, quartz plate C8, chopper C11, laser high reflection mirror C12, parabola Mirror C13 is penetrated to be radiated on sample C14；The attached XY resolution ratio of ICCD cameras C18 acquisition microcell laser desorptions；Desorbed gases Information in Mass Spectra is gathered via quadruple mass-spectrometer C16 again by the 70eV high energy electrons ionization that iridium filament is launched, is sent into computer C1； Finally, the intensity of mass spectra peak and broadening information that computer C1 extractions need to quantify, and with using authoritative dosing machine in computer C1 The quantitative calibration curve comparison analysis that the admittance type glass leakage hole partial pressure method of structure calibration obtains, by data processing, obtains micro- The quantitative analysis results that area's fuel is detained.

Computer C1 controls the first photodiode C10 to obtain the laser intensity that quartz plate C8 reflects by FPGA sequential C2 And by its data acquisition to oscillograph C3；Computer C1 controls the second photodiode C17 to obtain and is tested by FPGA sequential C2 The laser intensity of sample C14 reflections and by its data acquisition to oscillograph C3；The reflectivity of sample is drawn by the ratio of the two, If reflectivity changes relative scale is more than the relative scale of Joulemeter C9 variations, judgement sample has damaged.

Computer C1 controls spectrometer that detector C 22 is added to pass through Al-flim reflector C19, transmitting light by FPGA sequential C2 The emission spectrum that collecting lens C20 and detection optical fiber C21 obtains desorbed region is composed, if spectrometer adds detector C 22 can To collect plasma emission spectroscopy, then illustrate that sample C14 surfaces are breakdown and damage.

Computer C1 controls ICCD cameras C18 to be monitored sample C14 surfaces by FPGA sequential C2, passes through prison It surveys laser and is irradiated to the spot size of sample to judge the size of desorption microcell, obtain space X Y-resolution.

Theory analysis：Corresponding optical device desorption is combined using suitable laser parameter (such as pulsewidth, radiant quantity) The fuel molecule being detained in sample.Laser vaporization materials process can generally be described using one-dimensional heat flow equation

Wherein T, ρ, c, k, A are respectively temperature, mass density, specific heat capacity, the absorptivity of thermal conductivity and target material surface, I₀It is The intensity of incident laser, z are the normal directions of material, and α is material absorption co-efficient.For ultra-short pulse laser such as fs, ps laser Heating material：Since laser pulse is short, continue the optics that the interior depth with material interaction depends on material in the burst length Property, depth of interaction α^-1, can be described by equation (1-2)：

Wherein k ' is the extinction coefficient of material.To pulsewidth, more than the laser of 1ps, its depth of interaction then depends on material Macroscopic property, depth of interaction L_th, can be described by equation (1-3)：

L_th≈(2Dτ_l)^1/2 (1-3)

Wherein τ_lFor incident laser pulse width, D is the thermal diffusion coefficient of material, and D can be described by equation (1-4)

D=k/ ρ c (1-4)

Wherein ρ, c, k are respectively the mass density of material, specific heat capacity, thermal conductivity.Experimentally by changing laser pulse just It can realize different depth resolution (Z resolution ratio).

The surface temperature of material after laser heating materials, for fs, for ps laser, since its action time is short, in electricity Son has not just terminated with laser in the material lattice balance relaxation time, so ignoring the heat transfer item in equation (1-1)Equation becomes

When laser pulse persistently finishes, the surface temperature of material is

Wherein F_lFor laser energy-flux density, numerical value F_l=I₀τ_l.For laser heating materials of the pulsewidth more than ps, It can be obtained by energy conservation equation, the temperature of material surface is after pulsewidth

Wherein, I_lFor laser power density, τ_lFor incident laser pulsewidth.So experimentally in given optical maser wavelength, pulsewidth Under the conditions of can pass through change laser output energy realize in penetration depth region all gas desorption.Using two Whether the surface topography of the analyzed sample area of photodiode measurement sample reflectivity technology evaluation changes, and is to evaluate with this It is no to have damaged sample.Microcell imaging technique using CCD camera or ICCD camera combination camera lenses is attached to laser desorption XY resolution ratio evaluated.It is evaluated using whether Emission Spectroscopy one can damage sample to laser, two can To realize in accidentally attacking material, to the function of the analysis of sample.Using with sequential and gate-width regulation and control Function simultaneously quickly measures sample surface temperature by the ICCD cameras of black matrix radiant correction, during the response of measurement Between resolution ratio determined by the ICCD minimum integration times.Using TDS heating modules heating is aided in realize to be detained sample fuel Complete desorption, the 70eV high energy electrons that the gas that desorption goes out is launched by iridium filament are ionized again via quadrupole mass spectrometer (Quadrupole Mass Spectrometry, QMS) makes choice interested mass number, then projects secondary electron times Increase and desorbed on device (Secondary Electron Multiplier, SEM) or Faraday cup (Faraday Cup, FC) The quantitative analysis of attached gas.With reference to two kinds of technologies with realize high-space resolution (μm magnitude), gradient type depth resolution (nm to mm measure Grade), high detection sensitivity (10¹⁰Atoms magnitudes), quick (s magnitudes), high accurancy and precision, active, material fuel element of facing the wall and meditating inspection Go out and sample without pretreatment nondestruction quantitative analysis method.

It summarizes：The utility model is a kind of using the pulse laser induced desorption of distinct pulse widths (Laser Induced Desorption, LID) combine a kind of thermal desorption level Four mass spectrum (Thermal Desorption Spectroscopy, TDS) Large-scale tokamak fusion facility is faced the wall and meditated, and the delay of material (Plasma Facing Materials, PFMs) fuel is lossless to be quantified Analysis method.Especially this method can realize high-space resolution μm magnitude, gradient type depth resolution (nm to mm magnitudes), high spy Survey sensitivity, quick, high accurancy and precision, harmless quantitative point active, the detection of the first wall fuel element and sample are without pretreatment Analysis.This method includes two major parts, and one is induced with laser desorption, and two be thermal desorption mass spectrum.Compared to traditional laser Induce desorption (LID) or laser desorption attached (Laser Desorption, LD), the utility model combination thermal desorption mass spectrum TDS auxiliary sample heating so that laser realizes more sufficient desorption to analyzed material, convenient for being compared with other technologies Correction is detained analysis quantitative accurate degree to improve fuel；Compared to traditional TDS technologies, the utility model can be to measured material Middle fuel, which is detained, carries out 3D quantitative analysis, can be to region different in PFMs materials, such as impurity deposition dominates district, fuel It is detained dominates district, plasma etching area etc. and carries out absolute quantification analysis.In addition, by changing laser energy or changing focused spot The point controllable tested region temperature of size is, it can be achieved that the complete desorption of fuel molecule to being detained in sample.

" the mass spectrographic material fuel of facing the wall and meditating of microcell 3D distribution induced with laser desorption combination thermal desorptions is detained nothing to the utility model Damage quantitative analysis method ", the first portion in this method, laser pulse width arrives millisecond for femtosecond (femtosecond laser, fs) (millisecond laser, ms), wavelength does not do any restriction, and for heating or reheating analyzed sample, desorption goes out The fuel molecule deuterium and tritium being detained in sample, by changing degree of focus of the laser focusing lens to laser, the achievable μ of minimum M magnitudes spatial discrimination (XY resolution ratio), by changing the pulsewidth (fs-ms) of heating laser, it can be achieved that sample nm to mm Grade depth resolution (Z resolution ratio).TDS devices in this method can also be independently operated, device and contain thermocouple heating module in itself Between sample 300K to 1300K can be heated, linear heating rate is controllable, and scope is 0.1K/min to 100K/min.Directly Connect using the TDS in the utility model can in analysis of material gas desorption kinetic process, determine the chemistry of resolved gas Form can also calculate desorption gas absolute magnitude and desorption activation energy.

Finally it should be noted that：Various embodiments above is only to illustrate the technical solution of the utility model rather than it is limited System；Although the utility model is described in detail with reference to foregoing embodiments, those of ordinary skill in the art should Understand：It is modified to the technical solution recorded in foregoing embodiments either to which part or all technical characteristic Equivalent substitution is carried out, the essence of appropriate technical solution is not made to depart from the scope of various embodiments of the utility model technical solution.

Claims (3)

1. one kind is faced the wall and meditated, material 3D microcells fuel is detained nondestruction quantitative analysis equipment, which is characterized in that sample heating module (C15) Sample (C14) is heated by way of heat transfer；Computer (C1) connects FPGA sequential moulds by PXIExpress ports Block (C2) is connected by USB, serial ports and quadruple mass-spectrometer (C16), is connected by network interface with ICCD cameras (C18)；FPGA sequential Module (C2) connects ICCD cameras (C18) and desorption laser (C4) by bnc interface；The laser sent passes through and laser It broadcasts the laser beam expanding instrument (C5) of direction placement in 90 °, regulate and control system using with the laser energy of laser propagation direction placement in 90 ° It unites (C6)；Two beams are divided by the laser of laser energy regulator control system (C6), beam of laser is reflected to and laser light incident Direction remaining laser absorption device (C7) in 90 ° is inner, another beam of laser along original direction continue propagate forward, by with incidence After the angled quartz plate of laser (C8), the sub-fraction laser reflected is irradiated on Joulemeter (C9), scatters illumination It is mapped on photodiode (C10)；The angle that quartz plate (C8) is placed is according to the location determination of Joulemeter (C9)；Chopper (C11) it is placed in the light path in 90 ° with incident laser；Via chopper (C11) outgoing laser by with laser light incident direction Laser high reflection mirror (C12) reflection of placement at 45 °；The laser reflected is by the parabolic with the placement at 45 ° of laser light incident direction Face speculum (C13), which focuses on, to be placed on the sample (C14) of parabolic mirror (C13) focal point；Resolved Gas is detected by quadruple mass-spectrometer (C16), is transferred data to via serial ports and USB port in computer (C1)；ICCD cameras (C18) angle placed is parallel with sample normal direction；By adjusting the lens focus of ICCD cameras (C18) to laser and sample The region of interaction is shot；ICCD cameras (C18) transfer data to computer (C1) by network interface.

2. one kind according to claim 1 is faced the wall and meditated, material 3D microcells fuel is detained nondestruction quantitative analysis equipment, and feature exists In FPGA tfi modules (C2) connect oscillograph (C3) by bnc interface；Oscillograph (C3) connects the first light by bnc interface Electric diode (C10), the second photodiode (C17) and Joulemeter (C9).

3. one kind according to claim 1 is faced the wall and meditated, material 3D microcells fuel is detained nondestruction quantitative analysis equipment, and feature exists In FPGA tfi modules (C2) connect spectrometer by bnc interface and add detector (C22)；Spectrometer adds detector (C22) to pass through SMA905 interfaces are connected with detection optical fiber (C21)；The position that detection optical fiber (C21) is placed is according to emission spectrum collecting lens (C20) distance of focal length and lens (C20) to Al-flim reflector (C19) arrives sample plus Al-flim reflector (C19) (C14) distance determines jointly；Detection optical fiber (C21) end face is parallel with emission spectrum collecting lens (C20) plane；Aluminium film reflects The angle that mirror (C19) is placed is condenser lens normal and the 1/2 of sample normal angulation；Spectrometer add detector (C22) with Computer (C1) is connected by USB interface.