CN107655909B - Electronic diffractometer capable of realizing automatic defect regulation - Google Patents

Electronic diffractometer capable of realizing automatic defect regulation Download PDF

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Publication number
CN107655909B
CN107655909B CN201710596412.XA CN201710596412A CN107655909B CN 107655909 B CN107655909 B CN 107655909B CN 201710596412 A CN201710596412 A CN 201710596412A CN 107655909 B CN107655909 B CN 107655909B
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laser
electron
defect
light path
regulation
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CN107655909A (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

Abstract

The invention relates to an electron diffractometer, and provides an electron diffractometer capable of realizing automatic defect regulation, which comprises a vacuum sample chamber, a detection light path, a defect regulation light path and a processing unit, wherein triple frequency laser of the detection light path is transmitted into the vacuum sample chamber through a first incidence window, double frequency laser of the defect regulation light path is transmitted to a sample stage in the vacuum sample chamber through a second incidence window, an electron gun is further arranged in the vacuum sample chamber, a cathode of the electron gun is positioned on the detection light path, a laser pulse energy regulating device and a laser pulse scanning device are arranged on the defect regulation light path, and the processing unit comprises a receiving component and a control center. The electron diffractometer can perform in-situ real-time nondestructive measurement on a micro-nano manufacturing process, growth and detection are realized at the same time, the surface defect information of a sample is obtained by processing a diffraction image, and the femtosecond laser pulse energy and the scanning position are adjusted according to the information in a feedback manner to repair the defect, so that the purposes of detection and regulation are realized at the same time.

Description

Electronic diffractometer capable of realizing automatic defect regulation
Technical Field
The invention relates to an electron diffractometer, in particular to an electron diffractometer capable of realizing automatic defect regulation and control.
Background
The advanced micro-nano manufacturing technology is used as the original productivity to promote the social progress, and the film growth represents one of the main development directions of the advanced micro-nano manufacturing industry. Typical representatives of the film growth include chemical vapor deposition, molecular beam epitaxy, pulsed laser deposition, ultrafast laser micro-nano processing, electronic pulse exposure, focused ion beam, nano welding/connection and the like, and the manufacturing means comprises film crystal growth, surface micro-nano composite structure, two-dimensional material preparation and the like, and is a technical basis of key materials and core chips of emerging industries such as power electronics, display, semiconductor illumination, bionic materials, micromachines, micro-nano electronics, photoelectrons, electronic packaging, novel solar energy, low-dimensional materials and devices, biological manufacturing, ultra-high temperature sensors and the like.
Typical micro-nano fabrication processes involve the formation or breaking of chemical bonds on the picosecond to femtosecond scaleAnd electron ionization, atomic adsorption and desorption structural evolution, nanosolder, and electron density (plasma) evolution. Micro-nano fabrication involves difficulties in measuring mesoscopic defects at the micro-to nano-scale, even at the nano-to angstrom scale of atomic molecular structuresMicroscopic defects of scale. At present, the measurement of the micro-nano manufacturing process is only limited to the measurement of temperature, layer number, roughness and the like, and the micro process cannot be measured and tracked in real time across space-time scales, so that the effective analysis and feedback regulation and control of a micro mechanism for defect formation are lacked, the improvement of the manufacturing process basically depends on the traditional trial-and-error method, and the development of a new material technology is hindered.
In the process of heteroepitaxial growth of crystal materials, particularly the growth of layered thin films, in-situ real-time monitoring of ultrafast processes occurring in a very short time is often required, and processes such as microstructure and defect formation, crystal structure evolution and the like all occur in the order of picoseconds to femtoseconds. These ultrafast changes directly affect and determine the growth quality of the thin film crystal. At present, the advanced laboratory has only an in-situ low-speed real-time monitoring function on defects, and the defect regulation and control are not mentioned. Therefore, it is urgently needed to monitor the ultrafast change process within the time scale from picoseconds to femtosecond, which is not only beneficial to effectively analyzing the microscopic mechanism of defect formation, but also makes it possible to feedback-regulate and control the defects to obtain a high-quality film.
At present, the micro-nano manufacturing process such as the laminated film manufacturing and the like is measured only by a low-speed detection means (RHEED, electronic diffractometer) belonging to nanosecond to picosecond in time resolution, so the mechanism of the ultrafast process of the defect formation and evolution of the picosecond to femtosecond time scale is not clear, and the feedback regulation and control of the defects are not mentioned. In addition, a large amount of electron pulse flow emitted by a high-energy electron gun of the RHEED device in the measurement process can cause variable damage to the surface of the film.
Disclosure of Invention
The invention aims to provide an electron diffractometer capable of realizing automatic defect regulation and control, and aims to solve the problem that growth defects are difficult to regulate and control effectively in the existing film manufacturing technology.
The invention is realized by the following steps:
the embodiment of the invention provides an electronic diffractometer capable of realizing automatic defect regulation and control, which comprises a vacuum sample chamber, a laser emitter, a detection light path, a defect regulation and control light path and a processing unit for analyzing diffraction images, wherein a sample stage is arranged in the vacuum sample chamber, the vacuum sample chamber is provided with a first incidence window and a second incidence window, the laser emitter sends light into the detection light path and the defect regulation and control light path through a light splitting light path, the light splitting light path comprises a first beam splitter, a laser frequency doubling device, a second beam splitter and a laser frequency tripling device, after the light sent out by the laser emitter is split by the first beam splitter, one part of the light passes through the laser frequency doubling device, the second beam splitter and the laser frequency tripling device in sequence, and the other part of the light enters the laser frequency tripling device after being reflected, the light outlet of the laser frequency tripling device is connected with the detection light path; the laser device comprises a laser double frequency device, a first beam splitter, a second beam splitter, a defect regulation and control optical path, a laser pulse energy regulation device, a laser pulse scanning device, a processing unit and a control unit, wherein the laser transmitter emits light which is acted by the laser double frequency device to generate double frequency laser, the second beam splitter splits the light, one part of the double frequency laser enters the defect regulation and control optical path, the other part of double frequency laser enters the laser triple frequency device, the triple frequency laser of the detection optical path is transmitted into the vacuum sample chamber through the first incident window, the double frequency laser of the defect regulation and control optical path is transmitted to the sample stage in the vacuum sample chamber through the second incident window, the vacuum sample chamber is also internally provided with an electron gun for transmitting electron pulses to the sample stage, the cathode of the electron gun is positioned on the detection optical path, the defect regulation and control optical path is provided with the laser pulse energy regulation device and the laser pulse scanning device, the processing unit comprises a receiving component for receiving The device comprises a quantity adjusting device and a control center of the laser pulse scanning device, wherein an optical path time delay assembly is arranged on a defect adjusting and controlling optical path.
Further, the electron gun also comprises a deflection assembly for controlling deflection of the electron pulse so as to control an incident angle of the electron pulse, wherein the incident angle of the electron pulse is 1-3 degrees.
Further, the receiving assembly includes a phosphor screen for receiving the diffraction image, an image intensifier for intensifying an image signal of the phosphor screen, and a charge-coupled camera for recording an image signal after the image intensifier is intensified, the phosphor screen is at least partially located in the vacuum specimen chamber, the image intensifier is located between the phosphor screen and the charge-coupled camera, and the charge-coupled camera is electrically connected with the control center.
Further, the laser emitter is a titanium-doped sapphire femtosecond laser, the laser emitter emits femtosecond laser pulses with the pulse width of 80-500 femtoseconds and the central wavelength of 1030 nanometers, and the energy dispersion degree of the femtosecond electronic pulses generated by the action of the frequency tripling femtosecond laser pulses generated by the femtosecond laser pulses on the cathode of the electron gun is less than 1 electron volt.
Furthermore, a cathode and an anode of the electron gun are oppositely arranged in parallel, an accelerating electric field applying 10-30 kilo-electron volts is arranged between the cathode and the anode, a small hole with the diameter of 50-120 micrometers is formed in the center of the anode, and the small hole is covered with a metal grid.
And the vacuum pump and the vacuum sample chamber are controlled to be on and off through an electromagnetic valve.
Further, the sample stage is a five-axis console, the five-axis console comprises an X axis, a Y axis, a Z axis, a first rotating shaft and a second rotating shaft, and the first rotating shaft is perpendicular to the second rotating shaft.
The invention has the following beneficial effects:
in the electron diffractometer, the film is grown on a sample platform in a vacuum sample chamber, in the growing process, the detection circuit emits frequency-tripled laser to the vacuum sample chamber, the frequency-tripled laser pulse acts on a cathode of the electron gun, the electron gun generates femtosecond electronic pulse, the electron gun diffracts when the femtosecond electronic pulse is emitted to the surface of the film, the processing unit receives the generated diffraction pattern, the processing unit can analyze and process the diffraction pattern to obtain the defect position and repair energy information of the surface of the film, and the information is respectively transmitted to the laser pulse scanning device and the laser pulse energy adjusting device on the defect adjusting and controlling optical path, so that the position and pulse energy of the frequency-doubled laser pulse emitted to the surface of the film on the defect adjusting and controlling optical path can be adjusted, and the adjustment, the repair and control of the defects on the surface of the film can be realized. In the process, on the basis of ensuring the nanoscale high spatial resolution, the time resolution of the electron diffractometer is improved to the femtosecond order to form the ultrafast electron diffractometer; the method has the advantages that the number and energy of femtosecond electronic pulses are controllable while the signal-to-noise ratio of detection signals is guaranteed by adjusting femtosecond laser pulse parameters, the method is used for forming microstructures and defects and carrying out in-situ real-time nondestructive measurement of ultrafast evolution transient dynamic characteristics in the micro-nano manufacturing process of manufacturing layered films and the like, the simultaneous growth and detection are realized, the surface defect information of a sample is obtained by analyzing and processing diffraction images, the femtosecond laser pulse energy and the scanning position are adjusted according to the information feedback, the defect repair is carried out, and the purposes of simultaneous detection and simultaneous regulation are realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic view of a working structure of an electron diffractometer capable of automatically adjusting and controlling defects according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, an embodiment of the present invention provides an electron diffractometer capable of automatically adjusting and controlling defects, including a vacuum sample chamber 1, a sample stage 11 is disposed in the vacuum sample chamber 1, and a sample can be prepared on the sample stage 11, mainly aiming at heteroepitaxial growth of a crystal material, such as growth of a layered thin film, and for the vacuum sample chamber 1, mainly ensuring that a preparation environment of the sample is in a vacuum state, which is not lower than 3 × 10-10In an ultrahigh vacuum environment, a vacuum sample chamber 1 is connected with a vacuum pump 12, the vacuum sample chamber 1 and the vacuum pump are controlled to be switched on and off through an electromagnetic valve 121, when the vacuum degree of the vacuum sample chamber 1 is higher than the above conditions, the electromagnetic valve 121 is opened, the vacuum pump 12 starts to work to ensure the vacuum degree of the vacuum sample chamber 1, the vacuum sample chamber 1 is also provided with a first incident window 13 and a second incident window 14, both of which are used for transmitting laser pulses, the electron diffractometer further comprises a detection light path 2, a defect regulating light path 3 and a processing unit 4, the detection light path 2 can emit frequency tripling laser pulses, the defect regulating light path 3 can emit frequency doubling laser pulses, specifically, the detection light path 2 corresponds to the first incident window 13, the frequency tripling laser pulses emitted by the detection light path 2 are emitted into the vacuum sample chamber 1 through the first incident window 13, an electron gun 21 is arranged at the position of the vacuum sample chamber 1, the electron gun 21 has a cathode 211, an anode 212 and a magnetic lens 213, the cathode 211 is a photocathode 211, when a frequency tripling laser pulse is emitted into the vacuum sample chamber 1 and acts on the cathode 211, a femtosecond electronic pulse is generated, the femtosecond electronic pulse is accelerated by an accelerating voltage between the cathode 211 and the anode 212, the accelerated femtosecond electronic pulse can be emitted to the surface of the sample after being focused by the magnetic lens 213, the femtosecond electronic pulse generates diffraction on the surface of the sample, whether a defect is generated on the surface of the sample can be analyzed and judged by a diffraction image, a defect regulating optical path 3 corresponds to the second incident window 14, and the defect regulating optical path 3 emits a defect regulating optical pathThe double-frequency laser pulse is emitted to the sample of the sample stage 11 through the second incident window 14, when the detection light path 2 detects a defect on the surface of the sample, the defect control light path 3 can repair the defect, the processing unit 4 comprises a receiving component 41 and a control center 42, the receiving component 41 can receive a diffraction image generated by the femtosecond electronic pulse on the surface of the sample, the control center 42 can analyze and process the diffraction image received by the receiving component 41, and further can control the position and the energy intensity of the defect control light path 3 emitted to the vacuum sample chamber 1, specifically, a laser pulse energy adjusting device 31 and a laser pulse scanning device 32 are arranged on the defect control light path 3, wherein the laser pulse energy adjusting device 31 can adjust the energy of the double-frequency laser pulse emitted into the vacuum sample chamber 1, and the laser pulse scanning device 32 can adjust the position of the sample acted by the femtosecond electronic pulse, the laser pulse energy adjusting device 31 and the laser pulse scanning device 32 are both electrically connected with the control center 42, the control center 42 analyzes the position of the sample surface defect and the energy required to be repaired through a diffraction image, and then the laser pulse scanning device 32 and the laser pulse energy adjusting device 31 are respectively controlled to work. In this embodiment, in the sample preparation process, the detection light path 2 injects a frequency tripling laser into the vacuum sample chamber 1 through the first incident window 13, the frequency tripling laser and the cathode 211 of the electron gun 21 act to generate a femtosecond electronic pulse, the femtosecond electronic pulse is accelerated under the action of an accelerating voltage between the cathode 211 and the anode 212 and focused after penetrating through the magnetic lens 213, the focused femtosecond electronic pulse is emitted to the sample surface and generates a diffraction image, the receiving component 41 of the processing unit 4 receives the diffraction image and processes and analyzes the diffraction image through the control center 42, when there is no defect, the sample surface does not need to be repaired through the defect regulating and controlling light path 3, and when there is a defect, the control center 42 can analyze the position of the defect on the sample surface and the energy required for repair, and transmit the information to the laser pulse scanning device 32 and the laser pulse energy adjusting device 31 respectively, and further, the defect repair of the corresponding position of the sample can be realized. In the process, the time of the electron diffractometer is divided on the basis of ensuring the high spatial resolution of the nanometer levelThe resolution is improved to the femtosecond level to form an ultrafast electron diffractometer; the method has the advantages that the number and energy of femtosecond electronic pulses are controllable while the signal-to-noise ratio of detection signals is guaranteed by adjusting femtosecond laser pulse parameters, the method is used for forming microstructures and defects and carrying out in-situ real-time nondestructive measurement of ultrafast evolution transient dynamic characteristics in the micro-nano manufacturing process of manufacturing layered films and the like, the simultaneous growth and detection are realized, the surface defect information of a sample is obtained by analyzing and processing diffraction images, the femtosecond laser pulse energy and the scanning position are adjusted according to the information feedback, the defect repair is carried out, and the purposes of simultaneous detection and simultaneous regulation are realized.
The above embodiment is optimized, the structure of the electron gun 21 is refined, and the electron gun further comprises a deflection component 214 for controlling deflection of the electron pulse, and the control of the incident angle of the electron pulse incident on the surface of the sample can be realized through the adjustment action of the deflection component 214. In this embodiment, because the electron pulse is incident on the sample surface and needs to generate diffraction, and the diffraction image needs to be received by the processing unit 4, the incident angle of the electron pulse needs to be adjusted according to the actual situation to ensure that the diffraction image can be received by the processing unit 4, and of course, the angle adjustment should be within a reasonable range, and the incident angle of the electron pulse (the included angle between the electron pulse and the sample surface, which is different from the conventional incident angle concept) is generally 1 to 3 °. For the deflection assembly 214, two sets of deflection plates may be adopted, wherein two plates of one set of deflection plates are horizontally disposed relatively, and two plates of the other set of deflection plates are vertically disposed relatively, so that the electronic pulse firstly enters between the two horizontally disposed plates and then enters between the two vertically disposed plates, and the effective deflection of the electronic pulse can be realized by the deflection assembly 214 arranged in this way. In addition, the cathode 211 and the anode 212 of the electron gun 21 are disposed in parallel and opposite to each other, an accelerating electric field of 10-30 kev is disposed between the cathode 211 and the anode 212 to increase the moving speed of the electron pulse, a small hole is disposed at the center of the anode 212, the diameter of the small hole should also meet a certain requirement and should be controlled to be 50-120 μm, the small hole is covered with a metal grid, the metal grid is grounded, the accelerated electron pulse can pass through the small hole, usually, the magnetic lens 213 is disposed between the anode 212 and the deflection assembly 214, the electron pulse passing through the small hole can be focused by the magnetic lens 213, and the focused electron pulse is incident on the surface of the sample under the action of the deflection assembly 214.
Continuing to optimize the above embodiment, an optical path delay component 33 is disposed on the defect-controlling optical path 3. In this embodiment, since the defect adjusting and controlling optical path 3 is used to realize the defect repairing of the sample surface, and the acquired diffraction information needs to be processed before the defect repairing, for this, a certain time difference should be provided between the detection optical path 2 and the defect adjusting and controlling optical path 3, and the time difference can be adjusted by the optical path delay component 33, so that the defect adjusting and controlling optical path 3 and the detection optical path 2 can be matched. The optical path delay assembly 33 includes a linear translation stage 331 and four reflectors, the optical path of the laser can be increased by the four reflectors, and along the direction of the optical path, the included angles between the four reflectors and the optical path are all 45 degrees, the two reflectors located in the middle are both located on the linear translation stage 331, the two reflectors are mutually perpendicular, and the other two reflectors and the adjacent reflectors are both arranged in parallel; the four reflectors are respectively defined as a No. 1 reflector 332, a No. 2 reflector 333, a No. 3 reflector 334 and a No. 4 reflector 335, wherein the No. 2 reflector 333 and the No. 3 reflector 334 are all positioned on a linear translation stage 331, laser is firstly incident to the No. 1 reflector 332 at 45 degrees, then reflected to the No. 2 reflector 333 and reflected to the No. 3 reflector 334 again, a light path between the No. 2 reflector 333 and the No. 3 reflector 334 is parallel to the incident laser, after being reflected by the No. 3 reflector 334, the laser is reflected to the No. 4 reflector 335, a light path between the No. 1 reflector 332 and the No. 2 reflector 333 is parallel to a light path between the No. 3 reflector 334 and the No. 4 reflector 335, finally the laser reflected by the No. 4 reflector 335 is emitted along a direction parallel to the incident direction, and because the No. 2 reflector 333 and the No. 3 reflector 334 are both positioned on the linear translation stage 331, the No. 2 reflector 333 and the No. 3 reflector 334 can be adjusted relative to the No. 1 reflector 332 and the No. 4 reflector 332 335, and further can realize the adjustment of the laser optical path to achieve the purpose of time delay.
Further, a thinning receiving assembly 41, which comprises a fluorescent screen 411 for receiving diffraction images, an image intensifier 412 for intensifying the image signals of the fluorescent screen 411 and a charge coupled camera 413 for recording the image signals after the image intensifier 412 intensifies, wherein the fluorescent screen 411 is at least partially positioned in the vacuum sample chamber 1, specifically, the fluorescent screen 411 is integrally embedded on the shell of the vacuum sample chamber 1, wherein the fluorescent screen is positioned in the vacuum sample chamber 1, the side opposite to the fluorescent screen is positioned outside the vacuum sample chamber 1, the sealing between the fluorescent screen 411 and the shell of the vacuum sample chamber 1 should be complete, the fluorescent screen 411 and the electron gun 21 are respectively positioned on two sides of the sample stage 11, the diffraction images of the electron pulses irradiated on the samples can be reflected to the fluorescent screen 411, the image intensifier 412 is arranged on the side of the fluorescent screen 411 away from the fluorescent screen, the image intensifier 412 is positioned outside the vacuum sample chamber 1, the CCD camera 413 is opposite to the image intensifier 412, that is, the image intensifier 412 is positioned between the fluorescent screen 411 and the CCD camera 413, and can capture the image signal intensified in the image intensifier 412, the CCD camera 413 is electrically connected with the control center 42 and can transmit the signal to the control center 42, and the control center 42 can analyze and process the acquired diffraction image, so as to judge whether the detected position of the sample is defective, and if so, the defective position and the required energy can be determined.
Furthermore, the electron diffractometer also comprises a laser emitter 5, laser emitted by the laser emitter 5 is divided into two beams through a light splitting light path 6, and the two beams of laser respectively enter the detection light path 2 and the defect regulating and controlling light path 3. In this embodiment, the electron diffractometer has only one laser emitter 5, and can detect the sample and regulate and control the defective portion of the sample under the action of the light splitting path 6. For the laser emitter 5, a titanium-doped sapphire femtosecond laser can be selected, the femtosecond laser can generate femtosecond laser pulses with the pulse width of 80-500 femtoseconds and the central wavelength of 1030 nanometers, the volume of the laser emitter 5 is small, and then the volume of the electron diffractometer is reduced to the size of a table top.
Optimizing the light splitting optical path 6, which includes a first beam splitter 61, a laser frequency doubling device 62, a second beam splitter 63 and a laser frequency tripling device 64, after the light emitted from the laser emitter 5 is split by the first beam splitter 61, one part of the light passes through the laser frequency doubling device 62, the second beam splitter 63 and the laser frequency tripling device 64 in sequence, and the other part of the light directly enters the laser frequency tripling device 64 in a reflection manner, the light outlet of the laser frequency tripling device 64 is connected with the detection optical path 2, and in the above process, the central wavelength of the laser entering the first beam splitter 61 is 1030 nm, wherein the wavelength of the part entering the laser frequency tripling device 64 after reflection is 1030 nm, and the frequency is doubled after the other part enters the laser frequency doubling device 62, and the wavelength of the laser correspondingly derived by the laser frequency doubling device 62 is 515 nm, and at this time, after the laser of this wavelength passes through the second beam splitter 63, one part of the laser light enters the laser frequency tripling device 64, the laser light can enter the laser frequency tripling device 64 after being reflected, the wavelength of the laser light is 1030 nanometers, the laser light enters the detection light path 2, the wavelength of the laser light is 343 nanometers, the wavelength of the laser light enters the vacuum sample chamber 1 after being reflected by the cooperation of a plurality of reflectors, thereby showing that the electron pulse detection sample is generated by the action of the frequency tripling laser light with the wavelength of 343 nanometers and the electron gun 21, the energy dispersion degree of the femtosecond electron pulse generated by the cathode 211 of the electron gun 21 under the action of the frequency tripling femtosecond laser pulse is less than 1 electron volt, the time resolution of the electron diffractometer can be greatly improved, and the low-speed detection means from nanosecond to picosecond is improved to the high-speed detection means of femtosecond level, in the above process, the other part of the frequency-doubled laser with the wavelength of 515 nm split by the second beam splitter 63 directly enters the defect-adjusting optical path 3, i.e. the defect of the sample is adjusted by the frequency-doubled laser with the wavelength of 515 nm.
Further, the sample stage 11 adopts a five-axis console, which includes an X axis, a Y axis, a Z axis, a first rotation axis and a second rotation axis, and the first rotation axis is perpendicular to the second rotation axis. In this embodiment, sample platform 11 can realize through the X axle, Y axle and Z axle that arbitrary position in the reasonable region is adjusted in vacuum sample room 1, and can realize the upset to two directions of sample platform 11 through first rotation axis and second rotation axis, and then can play the effect of adjusting sample platform 11 angle, and then guarantee that the sample forms better cooperation relation with detecting light path 2 and defect regulation and control light path 3 between, of course, sample platform 11 self regulation action should be accomplished before detection and defect regulation and control, and should not adjust sample platform 11 position and angle when detecting.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (7)

1. The utility model provides a can realize electron diffractometer of automatic regulation and control of defect, includes the vacuum sample room, be provided with the sample platform in the vacuum sample room, just the vacuum sample room is provided with first incident window and second incident window, its characterized in that: the diffraction image analyzing device comprises a laser emitter, a detection light path, a defect regulating light path and a processing unit for analyzing diffraction images, wherein light emitted by the laser emitter enters the detection light path and the defect regulating light path respectively through a light splitting light path, the light splitting light path comprises a first beam splitter, a laser frequency doubling device, a second beam splitter and a laser frequency tripling device, after the light emitted by the laser emitter is split by the first beam splitter, one part of the light sequentially passes through the laser frequency doubling device, the second beam splitter and the laser frequency tripling device, the other part of the light enters the laser frequency tripling device after being reflected, and a light outlet of the laser frequency tripling device is connected with the detection light path; the laser device comprises a laser double frequency device, a first beam splitter, a second beam splitter, a defect regulation and control optical path, a laser pulse energy regulation device, a laser pulse scanning device, a processing unit and a control unit, wherein the laser transmitter emits light which is acted by the laser double frequency device to generate double frequency laser, the second beam splitter splits the light, one part of the double frequency laser enters the defect regulation and control optical path, the other part of double frequency laser enters the laser triple frequency device, the triple frequency laser of the detection optical path is transmitted into the vacuum sample chamber through the first incident window, the double frequency laser of the defect regulation and control optical path is transmitted to the sample stage in the vacuum sample chamber through the second incident window, the vacuum sample chamber is also internally provided with an electron gun for transmitting electron pulses to the sample stage, the cathode of the electron gun is positioned on the detection optical path, the defect regulation and control optical path is provided with the laser pulse energy regulation device and the laser pulse scanning device, the processing unit comprises a receiving component for receiving The device comprises a quantity adjusting device and a control center of the laser pulse scanning device, wherein an optical path time delay assembly is arranged on a defect adjusting and controlling optical path.
2. The electron diffractometer capable of realizing automatic defect regulation according to claim 1, wherein: the electron gun further comprises a deflection assembly used for controlling deflection of the electron pulse so as to control an incident angle of the electron pulse, and the incident angle of the electron pulse is 1-3 degrees.
3. The electron diffractometer capable of realizing automatic defect regulation according to claim 1, wherein: the receiving assembly comprises a fluorescent screen for receiving diffraction images, an image intensifier for intensifying image signals of the fluorescent screen and a charge coupled camera for recording image signals after the image intensifier is intensified, the fluorescent screen is at least partially positioned in the vacuum sample chamber, the image intensifier is positioned between the fluorescent screen and the charge coupled camera, and the charge coupled camera is electrically connected with the control center.
4. The electron diffractometer capable of realizing automatic defect regulation according to claim 1, wherein: the laser emitter is a titanium-doped sapphire femtosecond laser, the laser emitter emits femtosecond laser pulses with the pulse width of 80-500 femtoseconds and the central wavelength of 1030 nanometers, and the energy dispersion of the femtosecond electronic pulses generated by the cathode of the electron gun is less than 1 electron volt through the action of triple frequency femtosecond laser pulses generated by the femtosecond laser pulses.
5. The electron diffractometer capable of realizing automatic defect regulation according to claim 1, wherein: the cathode and the anode of the electron gun are oppositely arranged in parallel, an accelerating electric field applying 10-30 kilo electron volts is arranged between the cathode and the anode, a small hole with the diameter of 50-120 micrometers is formed in the center of the anode, and the small hole is covered with a metal grid.
6. The electron diffractometer capable of realizing automatic defect regulation according to claim 1, wherein: the vacuum pump is connected with the vacuum sample chamber through a solenoid valve.
7. The electron diffractometer capable of realizing automatic defect regulation according to claim 1, wherein: the sample stage is a five-axis control stage, the five-axis control stage comprises an X axis, a Y axis, a Z axis, a first rotating shaft and a second rotating shaft, and the first rotating shaft is perpendicular to the second rotating shaft.
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