CN107655909A - The electron diffraction instrument of defect auto-control can be achieved - Google Patents

The electron diffraction instrument of defect auto-control can be achieved Download PDF

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Publication number
CN107655909A
CN107655909A CN201710596412.XA CN201710596412A CN107655909A CN 107655909 A CN107655909 A CN 107655909A CN 201710596412 A CN201710596412 A CN 201710596412A CN 107655909 A CN107655909 A CN 107655909A
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laser
control
light path
defect
frequency
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CN107655909B (en
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刘胜
李辉
张国庆
申胜男
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Wuhan University WHU
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Wuhan University WHU
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20058Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/20025Sample holders or supports therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/05Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • G01N2223/056Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
    • G01N2223/0565Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction diffraction of electrons, e.g. LEED
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/30Accessories, mechanical or electrical features
    • G01N2223/307Accessories, mechanical or electrical features cuvettes-sample holders
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/60Specific applications or type of materials
    • G01N2223/646Specific applications or type of materials flaws, defects

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The present invention relates to electron diffraction instrument, a kind of electron diffraction instrument of achievable defect auto-control is provided, including vacuum specimen chamber, also include light path, defect regulates and controls light path and processing unit, the frequency tripled laser of light path is transmitted through in vacuum sample room by the first incidence window, two double-frequency lasers of defect regulation and control light path are transmitted through on the sample stage in vacuum sample room by the second incidence window, in being additionally provided with electron gun in vacuum sample room, the negative electrode of electron gun is located in light path, laser pulse energy quantity regulating device and laser pulse scanning means are provided with defect regulation and control light path, processing unit includes receiving unit and control centre.The electron diffraction instrument of the present invention can be measured minute manufacturing process original position real non-destructive, realize that side growth, frontier inspection are surveyed, and by obtaining sample surfaces defect information to diffraction image processing, and femto-second laser pulse energy and scan position are adjusted according to this feedback of the information, the reparation of defect is carried out, realizes the purpose that frontier inspection is surveyed, side regulates and controls.

Description

The electron diffraction instrument of defect auto-control can be achieved
Technical field
The present invention relates to electron diffraction instrument, more particularly to a kind of electron diffraction instrument of achievable defect auto-control.
Background technology
Advanced minute manufacturing technology promotes the progress of society as bare productivity, and film growth then represents advanced micro- Receive one of manufacturing the main direction of development.The Typical Representative of film growth has chemical vapor deposition, molecular beam epitaxy, pulse to swash Light deposition, ultrafast laser micro-nano technology, electronic impulse exposure, focused ion beam, nano-weld/connection etc., including film crystal Growth, surface micro-nano compound structure, two-dimensional material such as prepare at the manufacture means, are power electronics, display, semiconductor lighting, bionical Material, micromechanics, micro-nano electronics, photoelectron, Electronic Packaging, new type solar energy, low-dimensional materials and device, biology manufacture, superelevation The technical foundation such as the critical material and acp chip of the infant industries such as temperature sensor.
Typical minute manufacturing process is related to formation or fracture and electron ionization, the atom of chemical bond of the psec to femtosecond yardstick Absorption and the evolution of the attached structure evolution of desorption, nano-weld and electron density (plasma).Minute manufacturing further relates to be difficult to survey Amount is in micron to Jie's sight defect of nanoscale, in addition be in the nanometer of atom and molecule structure to angstromThe microcosmic of yardstick lacks Fall into.Measurement for minute manufacturing process at present is only limited to the measurement such as temperature, the number of plies, roughness, and microprocess can not be carried out The real-time measurement tracking of yardstick spanning space-time, effectively analysis and feedback regulation are carried out to the micromechanism that defect is formed so as to lack, Thus the improvement for manufacturing process relies on traditional trial and error method substantially, hinders the development of new material new technology.
In crystalline material heteroepitaxial growth especially laminar film growth course, it is often necessary to occurring when extremely short In ultrafast process carry out monitoring in real time in situ, such as the formation of microstructure and defect, crystal structure the process such as develop all Occur in psec to femtosecond magnitude.These ultrafast changes directly affect and determine the growth quality of film crystal.Formerly at present Enter laboratory and also there was only low speed real time monitoring function in situ to defect, defect regulation and control are not known where to begin more.Therefore, there is an urgent need to monitor Ultrafast change procedure in psec to femtosecond time scale, this not only contributes to effectively divide the micromechanism that defect is formed Analysis, and make it possible to carry out feedback regulation to defect to obtain the film of high-quality.
At present to minute manufacturing processes such as laminar film manufactures only with belonging to low speed of the nanosecond to psec in time resolution Detection means (RHEED, electron diffraction instrument) measures, and therefore, is formed and drilled the defects of for psec to femtosecond time scale The mechanism of the ultrafast process of change is also unintelligible, and carrying out feedback regulation to defect does not know where to begin more.In addition, RHEED in measurement process A large amount of electronic impulse streams that the high energy electron rifle of device emits are possible to cause film surface variable amount of damage.
The content of the invention
It is an object of the invention to provide a kind of electron diffraction instrument of achievable defect auto-control, it is intended to existing for solving The problem of being difficult to carry out Effective Regulation to growth defect in some film fabrication techniques.
What the present invention was realized in:
The embodiment of the present invention provides a kind of electron diffraction instrument of achievable defect auto-control, including vacuum specimen chamber, institute State and sample stage is provided with vacuum sample room, and the vacuum specimen chamber is provided with the first incidence window and the second entrance window Mouthful, in addition to for launching the light path of frequency tripled laser, regulating and controlling light path and use for the defects of two double-frequency laser of transmitting In the processing unit of analysis diffraction image, the frequency tripled laser of the light path is transmitted through described by first incidence window In vacuum sample room, two double-frequency lasers of the defect regulation and control light path are transmitted through the vacuum sample by second incidence window On the indoor sample stage, in being additionally provided with the vacuum sample room for launching electronics pulse on the sample stage Electron gun, the negative electrode of the electron gun are located in the light path, and laser pulse energy is provided with the defect regulation and control light path Quantity regulating device and laser pulse scanning means, the processing unit include be used for receive diffraction image receiving unit and Diffraction image is to control the control of the laser pulse energy quantity regulating device and the laser pulse scanning means after analysis receives Center processed.
Further, the electron gun also includes being used to control the electronic impulse deflection to control the electronic impulse to enter The yoke assembly of firing angle, the incidence angle of the electronic impulse is 1~3 °.
Further, light path delay component is provided with the defect regulation and control light path.
Further, the receiving unit includes the image letter for receiving the fluorescent screen of diffraction image, the enhancing fluorescent screen Number image intensifier and record described image booster enhancing after picture signal charge coupling camera, the fluorescent screen It is at least partially disposed in the vacuum sample room, described image booster is located at the fluorescent screen and the charge coupling camera Between, and the charge coupling camera electrically connects the control centre.
Further, in addition to generating laser, the light that sends of the generating laser are respectively enterd by light splitting optical path In the light path and defect regulation and control light path.
Further, the light splitting optical path includes the first beam splitter, the frequency doubling device of laser two, the second beam splitter and laser Frequency tripling device, the generating laser send light after first beam splitter light splitting, and a portion is successively through described The frequency doubling device of laser two, second beam splitter and the laser frequency tripling device, another part enter described after reflection Laser frequency tripling device, the light-emitting window of the laser frequency tripling device connect the light path;The hair of the generating laser Light extraction generates two double-frequency lasers after the frequency doubling device of laser two effect, and after second beam splitter light splitting, wherein one The double-frequency laser of part two enters defect regulation and control light path, and the double-frequency laser of another part two enters the laser frequency tripling device It is interior.
Further, the generating laser is titanium-doped sapphire femto-second laser, and the generating laser sends pulsewidth The femto-second laser pulse for being 1030 nanometers for 80~500 femtoseconds and centre wavelength, and by caused by the femto-second laser pulse The energy dispersion degree that frequency tripling femto-second laser pulse acts on ultrashort electron pulses caused by the negative electrode of the electron gun is less than 1 electronics Volt.
Further, the negative electrode of the electron gun is oppositely arranged in parallel with anode, is set between the negative electrode and the anode Be equipped with the accelerating field of the kilo electron volt of application 10~30, and in the center of the anode be provided with one it is a diameter of 50~120 micro- The aperture of rice, the aperture is covered with metal gate.
Further, in addition to vavuum pump, led between the vavuum pump and the vacuum specimen chamber by solenoid valve control It is disconnected.
Further, the sample stage is five axle consoles, and the five axles console includes X-axis, Y-axis, Z axis, the first rotation Rotating shaft and the second rotary shaft, and first rotary shaft is perpendicular to second rotary shaft.
The invention has the advantages that:
In the electron diffraction instrument of the present invention, film growth is carried out on the sample stage in vacuum sample room, and growing Cheng Zhong, light path launch frequency tripled laser into vacuum sample room, by the negative electrode of frequency tripled laser impulse action electron gun, Electron gun produces ultrashort electron pulses, and diffraction occurs when ultrashort electron pulses are incident upon film surface, and processing unit receives production Raw diffraction pattern, and processing unit can analyze and process diffraction pattern, and then position and repair the defects of obtain film surface Multiple energy information etc., and the information is transmitted separately to the laser pulse scanning means and laser pulse in defect regulation and control light path Energy conditioner, and then the two double-frequency laser pulses that can adjust defect regulation and control light path are incident upon position and the arteries and veins of film surface Energy is rushed, and then the regulation and control reparation to film surface defects can be realized.In said process, nano level high spatial ensure that On resolution base, the temporal resolution of electron diffraction instrument is promoted to femtosecond magnitude and forms ultrafast electronic diffraction instrument;Pass through tune Femto-second laser pulse parameter is saved, ensures to realize ultrashort electron pulses quantity and energy-controllable while detection signal signal to noise ratio, uses The formation of micro-structural and defect and the ultrafast original for developing Transient Dynamics characteristic during the minute manufacturings such as laminar film manufacture Position real non-destructive measurement, realize that side growth, frontier inspection are surveyed, and believed by obtaining sample surfaces defect to diffraction image analyzing and processing Breath, and adjust femto-second laser pulse energy and scan position according to this feedback of the information, carries out the reparation of defect, realize frontier inspection survey, The purpose of side regulation and control.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the work structuring signal of the electron diffraction instrument of achievable defect auto-control provided in an embodiment of the present invention Figure.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on Embodiment in the present invention, those of ordinary skill in the art are obtained all other under the premise of creative work is not made Embodiment, belong to the scope of protection of the invention.
Referring to Fig. 1, the embodiment of the present invention provides a kind of electron diffraction instrument of achievable defect auto-control, including vacuum sample Product room 1, sample stage 11 is provided with vacuum specimen chamber 1, the preparation of sample can be realized on sample stage 11, mainly for crystal Material heteroepitaxial growth, such as the growth of laminar film, then mainly ensure sample for vacuum specimen chamber 1 prepares environment For vacuum state, not less than 3 × 10-10The ultra-high vacuum environment of support, vacuum specimen chamber 1 are connected with a vavuum pump 12, and both it Between by magnetic valve 121 control break-make, when the vacuum of vacuum specimen chamber 1 is higher than above-mentioned condition, magnetic valve 121 is opened, very Empty pump 12 is started working to ensure the vacuum of vacuum specimen chamber 1, vacuum specimen chamber 1 be additionally provided with the first incidence window 13 and Second incidence window 14, both of which are used to transmit for laser pulse, and electron diffraction instrument also includes light path 2, defect regulation and control Light path 3 and processing unit 4, light path 2 can launch frequency tripled laser pulse, and defect regulation and control light path 3 can launch two times Frequency laser pulse, specifically, light path 2 are corresponding with the first incidence window 13, the frequency tripled laser pulse that light path 2 is launched Injected in vacuum specimen chamber 1 by the first incidence window 13, set in the position of corresponding first incidence window 13 of vacuum specimen chamber 1 There is electron gun 21, electron gun 21 has negative electrode 211, anode 212 and magnetic lenses 213, and the negative electrode 211 is photocathode 211, when When frequency tripled laser pulse is incident upon in vacuum specimen chamber 1 and acted on negative electrode 211, ultrashort electron pulses are produced, pass through negative electrode Accelerating potential between 211 and anode 212 causes ultrashort electron pulses to accelerate, and the ultrashort electron pulses after accelerating are in magnetic lenses Sample surfaces can be incident upon after 213 focusing, ultrashort electron pulses produce diffraction in sample surfaces, and can divide by diffraction image Analysis judges whether sample surfaces produce defect, and defect regulation and control light path 3 is corresponding with the second incidence window 14, defect regulation and control light path 3 Two double-frequency laser pulses of transmitting are incident upon on the sample of sample stage 11 through the second incidence window 14, when light path 2 detects sample When product surface is defective, defect regulation and control light path 3 can repair to it, and processing unit 4 includes receiving unit 41 and control Center 42, receiving unit 41 can receive ultrashort electron pulses in diffraction image caused by sample surfaces, and control centre 42 is then The diffraction image of the reception of receiving unit 41 can be analyzed and processed, and then defect regulation and control light path 3 can be controlled to be incident upon vacuum specimen chamber 1 Position and energy intensity, specifically, defect regulation and control light path 3 on be provided with laser pulse energy quantity regulating device 31 and swash Two frequencys multiplication that light pulse scans device 32, wherein laser pulse energy quantity regulating device 31 can adjust injection vacuum specimen chamber 1 swash The energy of light pulse, and laser pulse scanning means 32 can then adjust the position of scanning ultrashort electron pulses effect sample, it is right This laser pulse energy quantity regulating device 31 electrically connects with laser pulse scanning means 32 with control centre 42, and control centre 42 is logical Cross diffraction image and analyze the position of sample surfaces defect and the energy of required reparation, then control laser pulse scanning respectively Device 32 and laser pulse energy quantity regulating device 31 work.In the present embodiment, in Sample Preparation Procedure, light path 2 is logical Cross the first incidence window 13 and frequency tripled laser, and the negative electrode 211 of frequency tripled laser and electron gun 21 are injected into vacuum specimen chamber 1 Effect produces ultrashort electron pulses, and ultrashort electron pulses accelerate under the accelerating potential effect between negative electrode 211 and anode 212, And focused on after through magnetic lenses 213, the ultrashort electron pulses after focusing are incident upon sample surfaces and produce diffraction image, and processing is single The receiving unit 41 of member 4 receives the diffraction image, and carries out Treatment Analysis to the diffraction image by control centre 42, when not depositing In defect, sample surfaces are repaired without regulating and controlling light path 3 by defect, and when existing defects, then control centre 42 The position of sample surfaces defect can be analyzed and repair required energy, and the information is transmitted separately to laser pulse and swept Imaging apparatus 32 and laser pulse energy quantity regulating device 31, and then can realize and the defects of sample correspondence position is repaired.It is above-mentioned During, on the basis of it ensure that nano level high spatial resolution, the temporal resolution of electron diffraction instrument is promoted to femtosecond Magnitude forms ultrafast electronic diffraction instrument;By adjusting femto-second laser pulse parameter, ensure to realize while detection signal signal to noise ratio Ultrashort electron pulses quantity and energy-controllable, the formation for micro-structural and defect during the minute manufacturings such as laminar film manufacture And the ultrafast real non-destructive in situ measurement for developing Transient Dynamics characteristic, realize that side growth, frontier inspection are surveyed, and by diffraction image Analyzing and processing obtains sample surfaces defect information, and adjusts femto-second laser pulse energy and scanning position according to this feedback of the information Put, carry out the reparation of defect, realize the purpose that frontier inspection is surveyed, side regulates and controls.
Optimize above-described embodiment, refine the structure of electron gun 21, it also includes being used for the deflection for controlling electronic impulse to deflect Component 214, the incidence angle control that sample surfaces are incident to electronic impulse can be realized by the adjustment effect of the yoke assembly 214 System.In the present embodiment, need to produce diffraction because electronic impulse is incident on sample surfaces, and diffraction image needs processed list Member 4 receives, and this needs is adjusted with the incidence angle of electronic impulse according to actual conditions, to ensure that diffraction image can be processed Unit 4 receives, and certain angular adjustment should in the reasonable scope, incidence angle (electronic impulse and the sample table of usual electronic impulse Angle between face, it is different from traditional incidence angle concept) it is 1~3 °.For yoke assembly 214, two groups of deflections can be used The structure type of plate, two plates of one of which deflecting plates are relatively horizontally disposed, the equal opposed vertical of two plates of another group of deflecting plates Set, then electronic impulse is introduced between horizontally disposed two plate, subsequently between two plates being vertically arranged, passes through this cloth The yoke assembly 214 put can realize effective deflection of electronic impulse.In addition, the negative electrode 211 of electron gun 21 is parallel with anode 212 It is oppositely arranged, and the accelerating field that can apply 10~30 kilo electron volts is provided between negative electrode 211 and anode 212, improves The translational speed of electronic impulse, and an aperture is offered at the center of anode 212, the diameter of aperture should also meet must Ask, should control between 50~120 microns, aperture can be worn covered with metal gate, metal gate ground connection, the electronic impulse after acceleration The aperture is crossed, usual magnetic lenses 213, can be to through small by magnetic lenses 213 between anode 212 and yoke assembly 214 The electronic impulse in hole is focused, and the electronic impulse after focusing is incident to sample surfaces in the presence of yoke assembly 214.
Continue to optimize above-described embodiment, light path delay component 33 is provided with defect regulation and control light path 3.In the present embodiment, Because defect regulation and control light path 3 is to be used to realize sample surfaces defect repair, and then need to spread out to acquisition before defect repair Penetrate information to be handled, on the other hand, there should be a timing difference between light path 2 and defect regulation and control light path 3, and be delayed by light path Component 33 can adjust the time difference, and then defect regulation and control light path 3 is formed with light path 2 and matched.Light path delay group Part 33 includes linear translation platform 331 and four speculums, can increase the light path of laser by four speculums, and along light path Direction, four angles between speculum and light path are 45 degree, and two speculums positioned at centre are respectively positioned on linear translation platform On 331, two speculums are mutually perpendicular to, and are be arranged in parallel between two other speculum and adjacent speculum;It is fixed respectively Adopted four speculums are No. 1 speculum 334 of speculum 333,3 of speculum 332,2 and No. 4 speculums 335, wherein No. 2 Speculum 333 and No. 3 speculums 334 are respectively positioned on linear translation platform 331, and laser is first incident to No. 1 speculum 332 for 45 degree, so Back reflection reflexes to No. 3 speculums 334 to No. 2 speculums 333 again, wherein No. 2 speculums 333 and No. 3 speculums 334 it Between light path parallel to incidence laser, and after No. 3 speculums 334 reflect, laser reflection to No. 4 speculums 335, and No. 1 Light path between speculum 332 and No. 2 speculums 333 parallel to the light path between No. 3 speculums 334 and No. 4 speculums 335, Most projected afterwards through the laser that No. 4 speculums 335 reflect along parallel to incident direction, and because No. 2 speculums 333 and No. 3 reflect Mirror 334 is respectively positioned on linear translation platform 331, anti-so as to adjust No. 2 speculums 333 and No. 3 speculums 334 No. 1 relatively The distance between mirror 332 and No. 4 speculums 335 are penetrated, and then the regulation of laser light path can be realized, reaches the purpose of delay.
Further, receiving unit 41 is refined, it includes receiving the fluorescent screen 411 of diffraction image, strengthens fluorescent screen 411 The charge coupling camera of picture signal after the image intensifier 412 and record image intensifier 412 of picture signal strengthen 413, wherein fluorescent screen 411 is at least partially disposed in vacuum specimen chamber 1, and specifically, fluorescent screen 411 is overall to be embedded in vacuum sample On the housing of room 1, wherein face is located in vacuum specimen chamber 1, and the side relative with face is located at outside vacuum specimen chamber 1 Side, it should seal between the housing of certain fluorescent screen 411 and vacuum specimen chamber 1 completely, and fluorescent screen 411 distinguishes position with electron gun 21 In the both sides of sample stage 11, then the diffraction image that electronic impulse is incident upon on sample can be reflexed on fluorescent screen 411, and image is increased Strong device 412 installs the side for deviating from face in fluorescent screen 411, then image intensifier 412 is located at the outside of vacuum specimen chamber 1, and The face image intensifier 412 of charge coupling camera 413, i.e. image intensifier 412 are located at fluorescent screen 411 and charge coupled image Between machine 413, it can catch enhanced picture signal in image intensifier 412, charge coupling camera 413 with control The heart 42 electrically connects, and it can transmit the signal to control centre 42, and control centre 42 can then analyze and process the diffraction of acquisition Image, and then can interpolate that whether the test position of sample is defective, if it is defective, it may be determined that defective locations and required Energy.
Further, electron diffraction instrument also includes generating laser 5, and the laser that generating laser 5 is sent passes through light splitting Light path 6 is divided into two beams, and two beam laser are respectively enterd in light path 2 and defect regulation and control light path 3.In the present embodiment, electronics spreads out Penetrate instrument and there was only a generating laser 5, and the detection to sample can have both been realized in the presence of light splitting optical path 6, can also be real Now to the regulation and control at sample defects position.Titanium-doped sapphire femto-second laser can be selected for generating laser 5, it can be produced The femto-second laser pulse that pulsewidth is 80~500 femtoseconds and centre wavelength is 1030 nanometers, the volume of generating laser 5 is smaller, And then cause the volume-diminished of electron diffraction instrument to size of desktop.
Optimize above-mentioned light splitting optical path 6, it include the first beam splitter 61, the frequency doubling device 62 of laser two, the second beam splitter 63 with And laser frequency tripling device 64, generating laser 5 send light after the light splitting of the first beam splitter 61, a portion is successively through swashing The frequency doubling device 62 of light two, the second beam splitter 63 and laser frequency tripling device 64, and another part is direct by way of reflection Into laser frequency tripling device 64, the light-emitting window connecting detection light path 2 of laser frequency tripling device 64, and in above process, enter The centre wavelength for entering the laser of the first beam splitter 61 is 1030 nanometers, wherein entering the part of laser frequency tripling device 64 after reflection Wavelength is 1030 nanometers, and after another part enters the frequency doubling device 62 of laser two, frequency is double, then accordingly by the frequency multiplication of laser two The wavelength of laser derived from device 62 is 515 nanometers, and now the laser of the wavelength after the second beam splitter 63, enter by a portion Enter laser frequency tripling device 64, it can be 1030 nanometers in laser three with entering laser frequency tripling device 64 and wavelength after reflection Combined in frequency doubling device 64, form frequency tripled laser, then now the wavelength of laser as derived from laser frequency tripling device 64 is 343 Nanometer, i.e., it is 343 nanometers into the wavelength of the laser in light path 2, and the wavelength laser passes through the cooperation of some speculums It is reflected into vacuum specimen chamber 1, so as to show to use wavelength to be produced for 343 nanometers of frequency tripled laser with the effect of electron gun 21 Electronic impulse detects sample, ultrashort electron pulses caused by the negative electrode 211 of frequency tripling femto-second laser pulse effect electron gun 21 Energy dispersion degree is less than 1 electron-volt, and it can be greatly enhanced the temporal resolution of electron diffraction instrument, make nanosecond to psec amount The low-speed detection means of level are promoted to the high speed detection means of femtosecond magnitude, and in above process, the second beam splitter 63 separates Another part wavelength be that 515 nanometers of two double-frequency lasers are directly entered defect and regulate and control light path 3, that is, use wavelength as 515 nanometers Two double-frequency lasers regulation and control sample defects.
Further, sample stage 11 uses five axle consoles, and five axle consoles include X-axis, Y-axis, Z axis, the first rotary shaft And second rotary shaft, and the first rotary shaft is perpendicular to the second rotary shaft.In the present embodiment, sample stage 11 passes through X-axis, Y-axis And Z axis can realize that any position is adjusted in reasonable region in vacuum specimen chamber 1, and pass through the first rotary shaft and the second rotation Rotating shaft can realize the upset to the both direction of sample stage 11, and then can play a part of adjusting the angle of sample stage 11, and then Ensure to form preferable matching relationship between sample and light path 2 and defect regulation and control light path 3, certainly, sample stage 11 itself Regulation action should be completed before detection and defect regulation and control, and should not adjust the position and angle of sample stage 11 when detection Degree.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.

Claims (10)

1. a kind of electron diffraction instrument of achievable defect auto-control, including vacuum specimen chamber, set in the vacuum sample room There is sample stage, and the vacuum specimen chamber is provided with the first incidence window and the second incidence window, it is characterised in that:Also include For launching the light path of frequency tripled laser, regulating and controlling light path and for analyzing diffraction for the defects of two double-frequency laser of transmitting The processing unit of image, the frequency tripled laser of the light path are transmitted through the vacuum specimen chamber by first incidence window Interior, two double-frequency lasers of the defect regulation and control light path are as described in being transmitted through in the vacuum sample room second incidence window On sample stage, in being additionally provided with the vacuum sample room for the electron gun of launching electronics pulse on the sample stage, institute The negative electrode for stating electron gun is located in the light path, and laser pulse energy quantity regulating device is provided with the defect regulation and control light path And laser pulse scanning means, after the processing unit includes receiving unit and analysis reception for receiving diffraction image Diffraction image is to control the control centre of the laser pulse energy quantity regulating device and the laser pulse scanning means.
2. the electron diffraction instrument of achievable defect auto-control as claimed in claim 1, it is characterised in that:The electron gun is also Including for controlling electronic impulse deflection to control the yoke assembly of the electronic impulse incidence angle, the electronic impulse Incidence angle is 1~3 °.
3. the electron diffraction instrument of achievable defect auto-control as claimed in claim 1, it is characterised in that:The defect regulation and control Light path delay component is provided with light path.
4. the electron diffraction instrument of achievable defect auto-control as claimed in claim 1, it is characterised in that:The receiving unit Including fluorescent screen, the image intensifier for the picture signal for strengthening the fluorescent screen and the record described image for receiving diffraction image The charge coupling camera of picture signal, the fluorescent screen are at least partially disposed in the vacuum sample room after booster enhancing, Described image booster is between the fluorescent screen and the charge coupling camera, and the charge coupling camera is electrically connected Meet the control centre.
5. the electron diffraction instrument of achievable defect auto-control as claimed in claim 1, it is characterised in that:Also include laser to send out Emitter, the light that sends of the generating laser respectively enter the light path and defect regulation and control light by light splitting optical path In road.
6. the electron diffraction instrument of achievable defect auto-control as claimed in claim 5, it is characterised in that:The light splitting optical path Including the first beam splitter, the frequency doubling device of laser two, the second beam splitter and laser frequency tripling device, the hair of the generating laser Light extraction is after first beam splitter light splitting, and a portion is successively through the frequency doubling device of laser two, second beam splitter And the laser frequency tripling device, another part enter the laser frequency tripling device, the laser frequency tripling after reflection The light-emitting window of device connects the light path;The generating laser sends light after the frequency doubling device of laser two effect Two double-frequency lasers are generated, and after second beam splitter light splitting, the double-frequency laser of a portion two regulates and controls into the defect Light path, the double-frequency laser of another part two enter in the laser frequency tripling device.
7. the electron diffraction instrument of achievable defect auto-control as claimed in claim 5, it is characterised in that:The Laser emission Device is titanium-doped sapphire femto-second laser, and the generating laser sends that pulsewidth is 80~500 femtoseconds and centre wavelength is 1030 The femto-second laser pulse of nanometer, and the electronics is acted on by frequency tripling femto-second laser pulse caused by the femto-second laser pulse The energy dispersion degree of ultrashort electron pulses caused by the negative electrode of rifle is less than 1 electron-volt.
8. the electron diffraction instrument of achievable defect auto-control as claimed in claim 1, it is characterised in that:The electron gun Negative electrode is oppositely arranged in parallel with anode, and the acceleration of the kilo electron volt of application 10~30 is provided between the negative electrode and the anode Electric field, and a diameter of aperture of 50~120 microns is provided with the center of the anode, the aperture is covered with metal gate.
9. the electron diffraction instrument of achievable defect auto-control as claimed in claim 1, it is characterised in that:Also include vacuum Pump, pass through solenoid valve control break-make between the vavuum pump and the vacuum specimen chamber.
10. the electron diffraction instrument of achievable defect auto-control as claimed in claim 1, it is characterised in that:The sample stage For five axle consoles, the five axles console includes X-axis, Y-axis, Z axis, the first rotary shaft and the second rotary shaft, and described One rotary shaft is perpendicular to second rotary shaft.
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CN108663381A (en) * 2018-05-09 2018-10-16 中国科学院长春光学精密机械与物理研究所 One kind mixing iron laser crystal defect inspection method and device
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CN112747837A (en) * 2020-12-23 2021-05-04 华中科技大学 Femtosecond CARS system for measuring gas phase temperature in MOCVD reaction cavity in real time
CN112747837B (en) * 2020-12-23 2021-10-29 华中科技大学 Femtosecond CARS system for measuring gas phase temperature in MOCVD reaction cavity in real time

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