CN107745197A - A kind of apparatus and method that electron microscopic sample in situ is prepared using convergence femtosecond laser - Google Patents
A kind of apparatus and method that electron microscopic sample in situ is prepared using convergence femtosecond laser Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/70—Auxiliary operations or equipment
- B23K26/702—Auxiliary equipment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
- B23K26/03—Observing, e.g. monitoring, the workpiece
- B23K26/032—Observing, e.g. monitoring, the workpiece using optical means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/70—Auxiliary operations or equipment
- B23K26/702—Auxiliary equipment
- B23K26/707—Auxiliary equipment for monitoring laser beam transmission optics
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Abstract
The present invention relates to laser microcell manufacture field and Electronic Speculum original position field of sample preparation, and in particular to a kind of apparatus and method for carrying out retrofit shaping to electron microscopic sample using the laser through convergence.The device includes femto-second laser and convergence scanning system, sample stage machinery numerical control mobile system, coaxial microexamination alignment system, the monitoring of computer intensive data and visualization system, shock mitigation system and guard system.Can be quickly and easily using femtosecond laser to various electron microscopic samples, such as using said apparatus：Sheet metal, aluminium oxide ceramics block, transparency silica glass etc., carry out the retrofits such as Numerical control cutting, punching.So as to, the electron microscopic sample in situ of given shape, breach can be prepared by the present invention, with reference to electron microscope home position observation technology, the home position observation that mechanics, electricity and corrosion behavior etc. can be carried out to some particular tissues and structure is studied, have the advantages that working (finishing) area is wide, precision is high, without heat affected area and pollution-free.
Description
Technical Field
The invention relates to the field of material laser micro-area processing and the field of in-situ electron microscope sample preparation, in particular to a device and a method for finely processing a prepared sample by using a micro-beam femtosecond laser, which can process various materials according to the programming of drawings, can adopt different processing modes aiming at different samples and can be selected by various sample stages.
Background
With the continuous development of laser technology, the performance of the laser is also continuously improved, the research on the interaction between laser and substances draws great attention, and the laser processing technology also makes great progress.
In the early 90 s of the 20 th century, with the emergence of broadband tunable laser crystals and self-locking die technology, the femtosecond laser technology was rapidly developedAnd (6) unfolding. The duration of output light pulse can be as short as 5fs, the central wavelength of laser is positioned in near infrared band (about 800 nm), specially, by means of chirp pulse amplification technology, the single pulse energy can be amplified from several nano-foci to several hundred-milli-foci, even joule magnitude, at this time the peak power of pulse can be up to GW or TW, and the power density after focusing is 1015～1018W/cm2And even higher. When the optical pulse with high peak power and extremely short duration interacts with a substance, all energy of the optical pulse can be injected into a small action area at an extremely high speed, the absorption and movement modes of electrons are changed by high-energy-density deposition in an instant, and the influence of laser linear absorption, energy transfer, diffusion and the like is avoided, so that the interaction mechanism of the laser and the substance is fundamentally changed, the femtosecond pulse laser processing becomes a non-hot melting cold processing process with ultrahigh precision, ultrahigh spatial resolution and ultrahigh universality, and the brand-new field of laser processing is created.
At present, in the field of in-situ electron microscope sample preparation, the following four main technical methods exist: mechanical cutting, wire cutting, conventional laser and focused ion beam. The traditional machining/linear cutting method is still adopted for preparing the in-situ electron microscope sample of the block material, the requirements on the plasticity and the machinability of the sample are high, the accurate positioning of the sample at a special position is difficult, a series of problems of secondary pollution, edge effect, low sample preparation success rate and the like exist, and the efficiency of in-situ electron microscope research work and the reliability of results are seriously restricted. However, the common continuous laser, nanosecond laser and even picosecond laser processing method can not be used as a proper in-situ electrode sample because of the photothermal effect, the behavior of remelting, recrystallization, oxidation reaction and the like in a large area appears at the processing edge of the material. Although the method for preparing the in-situ electron microscope sample by the focused ion beam can greatly eliminate the edge effect and achieve the nanometer-level processing precision, the method has extremely high equipment cost and extremely low processing efficiency and cannot be popularized and applied in a large range.
Disclosure of Invention
The invention aims to provide a device and a method for preparing an in-situ electron microscope sample by using converged femtosecond laser, which can be used for programming according to a drawing and cutting and processing samples in various shapes in a numerical control manner, and the processing precision can reach a submicron level.
In order to achieve the purpose, the technical scheme of the invention is as follows:
an apparatus for preparing an in-situ electron microscope sample by using a focused femtosecond laser, the apparatus comprising: the system comprises a femtosecond laser, a convergence scanning system, a sample stage mechanical numerical control moving system, a coaxial microscopic observation positioning system, a computer centralized data monitoring and visualization system, a damping system and a protection system, wherein the femtosecond laser of a laser light source is emitted from the laser, converged by a multi-stage laser combined lens, and connected to the coaxial microscopic observation positioning system in a coaxial light form through different interfaces with the common cold light of a common light source; the coaxial microscopic observation positioning system and the sample stage mechanical numerical control moving system are connected with a computer centralized data monitoring and visualization system through a USB (universal serial bus) line or a network cable, and the structure is as follows:
the laser light source and the ordinary light source are respectively connected to the laser convergence and microscopic observation system in a coaxial light mode through an interface through an optical cable, and are switched through the electric switch; the laser convergence and microscopic observation system is connected with the input end of the CCD camera, and the output end of the CCD camera and the input end of the motion controller are connected with a computer through a USB (universal serial bus) line or a network cable to carry out microscopic observation positioning and numerical control programming; the laser convergence and microscopic observation system is provided with the long-focus objective lenses with different multiples, and observation selection is carried out according to different samples and processing requirements; the laser gathering and microscopic observation system is arranged on the laser gathering module mechanical moving system, the output end of the motion controller is connected with the sample table mechanical numerical control moving system, the sample table mechanical numerical control moving system is arranged on the air floatation damping platform, and the air inlet end of the air floatation damping platform is connected with the air pump.
Adopt and assemble femto second laser preparation normal position electron microscope sample's device, femto second laser instrument and assemble scanning system, include: the femtosecond laser device is formed by matching a femtosecond laser oscillator, a pumping source and a femtosecond laser amplifier and emits ultrafast laser with the pulse width of less than 400fs and the single pulse energy of more than 50 mu J; and the combined lens is arranged at a light outlet of the laser and is used for carrying out first-stage reduction on the femtosecond laser facula.
The device for preparing the in-situ electron microscope sample by converging the femtosecond laser and the coaxial microscopic observation positioning system comprise a laser optical cable interface, a common optical cable interface, an electric coaxial optical source change-over switch, a laser CCD camera, a common microscope eyepiece, an objective lens and a group of ultra-long focal length objective lenses with different multiplying powers, and the coaxial microscopic observation positioning system is used for carrying out secondary convergence on the laser in the optical fiber.
The device for preparing the in-situ electron microscope sample by adopting the converged femtosecond laser and the mechanical numerical control moving system of the sample stage comprise: a set of combined sliding tables which can move freely in x, y and z three-dimensional space; a light-transmitting and sealing sample cavity communicated with protective gas; a detecting device for monitoring the converged laser energy in real time; a sample stage for holding a film sample, a fiber sample and a bulk sample; a liquid nitrogen cooling low temperature processing table; wherein,
the combined sliding tables move randomly in x, y and z three-dimensional spaces, each direction sliding table is controlled by a separate servo motor, the three-dimensional combined sliding tables of x, y and z are connected into the same controller and further connected into a computer, and a graphic program needing to be processed is input through a displacement control software window of the computer, so that the continuously adjustable movement with the repeated positioning precision of 0.5 mu m and the movement speed of 1-1000 mm/min is realized; meanwhile, a sliding table rotating in the plane is also arranged, and the sample is rotated by computer software under the control of a servo motor;
the sample cavity is provided with an air exhaust port, an inflation port and an exhaust port, a gas flowmeter is arranged at the front end of the inflation port, and the gas flowmeter is used for adjusting the reading of the flowmeter to realize the protective environment of positive pressure anti-oxidation of inert gas during laser processing or blow the ash residue left during cutting of the sample; meanwhile, a mechanical dry pump is arranged at the front end of the air extraction opening, and a vacuum environment of less than 5Pa is obtained in the closed cavity; a laser anti-reflection lens is arranged above the cavity and used for processing a sample in the cavity through femtosecond laser;
the liquid nitrogen cooling low-temperature processing table is provided with a liquid nitrogen cooling chamber and a heat insulation cavity; further, the liquid nitrogen cooling chamber comprises: a liquid nitrogen inlet, an exhaust port;
a detection device for monitoring the converged laser energy in real time, wherein a power probe is used for focusing the laser beam on the positive objective lens and detecting the laser power actually acting;
the structure of the sample stage is that one side of the sample stage is fixed, and the other side of the sample stage is a sliding table which moves horizontally and adopts extrusion type to the block sample; for thin slice and fiber samples, a coaxial rotating motor is respectively arranged at the upper sides of a sliding block and a fixed block, the samples are fixed in the center of a motor bearing in a tabletting mode and are controlled by a computer, and the samples rotate in one dimension; for the film samples, the fixation was performed using a top pressed sheet.
Adopt and assemble femto second laser preparation normal position electron microscope sample's device, data monitoring and visual system are concentrated to the computer includes: a set of software for carrying out numerical control and real-time monitoring on mechanical displacement realizes the switching between laser and common light and the processing of images by inputting a CAD vector diagram and editing a program; one set of laser CCD camera image of imaging, conveniently carry out and implement observation, measurement and accurate positioning, also possess simultaneously and shoot, record a video and add the scale function.
The device for preparing the in-situ electron microscope sample by adopting the converged femtosecond laser and the damping system comprise an air floating optical platform and an air pump, are used for installing a sample stage mechanical numerical control moving system and a coaxial microscopic observation positioning system, and prevent the sample from vibrating and light spots from deviating in the processing process by adopting a mechanical fixing mode; the protection system includes: the protective cover covers the mechanical numerical control moving system and the coaxial microscopic observation positioning system of the sample stage, so that the damage of laser light leakage to operators is prevented; a filter glasses for protecting the eyes of the operator while working.
A method for preparing an in-situ electron microscope sample by using a converged femtosecond laser by using the device comprises the following steps:
(1) a microscopic positioning step, namely determining a processing area;
(2) programming a processing graph, and editing processing parameters;
(3) selecting laser parameters, namely selecting the laser parameters meeting the processing requirements;
(4) starting a mechanical moving system and a laser;
(5) and a detection step, namely monitoring the processing process in real time.
A method for preparing an in-situ electron microscope sample by using a converged femtosecond laser by using the device comprises the following steps:
(1) putting a sample in a sample cavity, pumping a vacuum with a pressure less than 5Pa by using a mechanical pump, introducing protective gas to atmospheric pressure, pumping again, and then pumping again for three times; finally, opening an exhaust valve to enable protective gas to flow in the cavity, and keeping the pressure of the cavity higher than one atmosphere to enable the pressure in the cavity to reach 0.105-0.11 MPa;
(2) a microscopic positioning step, namely determining a processing area;
(3) programming a processing graph, and editing processing parameters;
(4) selecting laser parameters, namely selecting the laser parameters meeting the processing requirements;
(5) starting a mechanical moving system and a laser;
(6) and a detection step, namely monitoring the processing process in real time.
A method for preparing an in-situ electron microscope sample by using a converged femtosecond laser by using the device comprises the following steps:
(1) fixing the sample on the upper surface of the cooling cavity by using a pressing sheet, and adding liquid nitrogen to cool the cavity;
(2) a microscopic positioning step, namely determining a processing area;
(3) programming a processing graph, and editing processing parameters;
(4) selecting laser parameters, namely selecting the laser parameters meeting the processing requirements;
(5) starting a mechanical moving system and a laser;
(6) and a detection step, namely monitoring the processing process in real time.
The method for preparing the in-situ electron microscope sample by adopting the converged femtosecond laser further comprises the steps of selecting an objective lens for microscopic observation and converging the laser; the method further includes a storing step of storing the edited processing drawing; the method further comprises a step of importing, namely importing a processing drawing stored before or an existing CAD vector drawing; the method further comprises a laser spot adjusting step, wherein the size of the laser spot is adjusted to meet the processing requirement.
The design idea of the invention is as follows:
firstly, aiming at a series of problems of secondary pollution, edge effect, low sample preparation success rate and the like caused by the fact that methods of machining, linear cutting and long pulse laser processing are generally adopted in the field of preparation of in-situ electron microscope samples at present, the invention adopts a femtosecond laser light source with the pulse width of less than 400fs to enable the width of a single pulse to be smaller than the heat conduction relaxation time of material lattices, and effectively eliminates the problem of the splash of heat affected zones and cut materials. Secondly, in the process of processing materials, a numerical control mechanical moving system is required to be matched, so that the combined lens and the sample table are arranged on a manual and electric combined sample table which can translate and rotate in three dimensions and the like, and a corresponding driver, a controller and a computer are matched to realize the omnibearing movement of laser spots and samples. And thirdly, because the processing size is very small and observation and positioning measurement are carried out by matching with a microscope, the same group of micro lenses is designed to be simultaneously connected with two coaxial optical cables of laser and common light, the switching between the two coaxial optical cables can be realized, and meanwhile, a specially matched laser imaging CCD camera is utilized to image on a software operation window of a computer, so that the operations of real-time observation, positioning, measurement and the like are convenient to carry out.
Based on the three main design guiding ideas, the numerical control femtosecond laser cutting processing method successfully realizes the numerical control femtosecond laser cutting processing of various materials with micron-sized precision and considers the special processing modes of samples in different shapes. Meanwhile, the processing of the specific position inside the transparent material can be realized by selecting a laser source with proper wavelength and power.
The invention has the following advantages and beneficial effects:
1. the apparatus and laser methods used in the present invention can process a variety of materials with substantially no heat affected zone. The method can well avoid a series of problems of secondary pollution, edge effect, low sample preparation success rate and the like caused by the traditional in-situ electron microscope sample preparation method. The invention mainly adopts a high-power femtosecond laser, the pulse width is less than 400fs, the single-pulse energy is more than 50 muJ, the laser is adjustable, the peak power can reach 100MW, almost any material can be instantly converted into a plasma state, and the material beside a light spot is not influenced.
2. The device and the method used by the invention have high processing precision, and after laser is subjected to multistage convergence, light spots with small enough size and high energy concentration are obtained on a sample, so that local high temperature is caused, and a local area of the sample is gasified. Because the laser spot is small, patterning of several microns can be achieved.
3. The invention is provided with different sample stages aiming at different materials, a protective gas sample cavity designed aiming at toxic and easily oxidized samples, an extrusion type clamping sample stage aiming at block-shaped samples, and a suspended clamping sample stage aiming at film and fiber samples. Meanwhile, the clamping of materials with different shape characteristics such as blocks, films and fibers is taken into consideration by the same sample table, the position of the lower sliding table can be adjusted according to the length difference of the films or the fibers, and the fiber material rotating platform also has a one-dimensional rotating function and has the advantage of high integration level.
4. The invention adds a sample table accessory which is internally cooled by liquid nitrogen and processed at low temperature. The liquid nitrogen is used for low-temperature cutting, so that the overall temperature of the sample is reduced, the sample which is not irradiated by the laser cannot be heated up due to the absorption of waste heat, structural changes such as grain growth, defect reduction and the like are avoided, and a heat affected zone is further reduced.
5. The invention can monitor the energy of the laser spot converged by the lens in real time, and the laser is attenuated in the converging process, but the energy of the actually processed sample is not displayed by the laser, so that a laser power monitor is necessary.
6. The device and the method can be controlled by computer software in most operations, and the multidimensional combined sliding table and the light source conversion switch can be linked, so that the computer programming can be carried out to realize automatic cutting of more complex image samples.
7. The invention can be used for transparent materials, such as: the inside of the quartz glass or the like is processed.
8. The device and the method used by the invention use the customized interface, can simultaneously access two coaxial optical cables of laser and common light, and can realize the electric switching between the two, thereby ensuring that the laser spot and the common light spot are at the same position, and being convenient for positioning measurement and processing control.
9. The device and the method used by the invention can observe the processing process in real time by using the special laser micro-combination lens and the camera.
10. The device and the method adopted by the invention adopt the air floatation damping platform, and compared with the common cast iron damping platform, the air floatation damping platform has better damping effect. The laser gathering system, the microscopic observation system and the mechanical moving system are arranged on the air floatation damping platform and isolated from the vibration unit, so that the processing error caused by environmental vibration can be greatly reduced or eliminated.
Drawings
FIG. 1 is a schematic diagram of an experimental apparatus according to the present invention. In the figure, 1, a laser convergence and microscopic observation system; 2, a laser light source; 3 a normal light source; 4, an air pump; 5, an air floatation damping platform; 6, a mechanical numerical control moving system of the sample stage; 7. a CCD camera; 8, a laser convergence module mechanical moving system; 9 a motion controller; 10, a computer; 11 light source automatic change-over switch.
Fig. 2 is a block diagram of a protective atmosphere sample chamber. In the figure, 12 a mechanical vacuum pump; 13 an exhaust valve; 14 protective gas cylinder; 15 gas mass flow controllers; 16 an intake valve; 17 laser anti-reflection window; 18 sample chamber.
FIG. 3 is a block diagram of a sample holding table for block, membrane and fiber samples. In the figure, 19 horizontal sliding tables; 20 tabletting; 21 a speed adjustable motor; 22 a fiber chuck; 23 fixing the table.
FIG. 4 is a block diagram of a liquid nitrogen cooled cryogenic processing station. In the figure, 24 liquid nitrogen injection ports; 25 an exhaust port; 26 an insulating material; 27 stainless steel chamber; 28 tabletting.
Detailed Description
In the specific implementation process, the core of the invention is to provide a device for finely processing the material by using the highly focused femtosecond laser, the device uses the femtosecond laser pulse width to be smaller than the relaxation time of lattice heat transfer, and the energy of a single pulse can instantly convert a sample at a light spot from a solid state to a plasma state, thereby achieving the effect of removing the material at a specific position. And because the pulse width is extremely small, a single pulse can only remove materials with the thickness of a few nanometers basically, so that the micro three-dimensional configuration processing can be carried out.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Referring to fig. 1, a block diagram of an apparatus for fine processing and processing of materials by using a highly focused laser according to an embodiment of the present invention is shown, the apparatus mainly includes the following systems: the system comprises a femtosecond laser, a convergence scanning system, a sample stage mechanical numerical control moving system 6, a coaxial microscopic observation positioning system, a computer centralized data monitoring and visualization system, a damping system and a protection system, wherein the femtosecond laser of a laser source is emitted from the laser, converged by a multi-stage laser combined lens, and connected to the coaxial microscopic observation positioning system in a coaxial light form through different interfaces with the common cold light of a common light source; the coaxial microscopic observation positioning system and the sample stage mechanical numerical control moving system are connected with a computer centralized data monitoring and visualization system through a USB (universal serial bus) line or a network cable, and the structure is as follows:
the laser light source 2 and the ordinary light source 3 are respectively connected to the laser convergence and microscopic observation system 1 through an optical cable in a coaxial light mode through a customized interface, and the laser light source 2 and the ordinary light source 3 can be switched through the electric switch 11. The laser convergence and microscopic observation system 1 is connected with the input end of the CCD camera 7, and the output end of the CCD camera 7 and the input end of the motion controller 9 are connected with the computer 10 through a USB line or a network cable for microscopic observation positioning and numerical control programming. The laser convergence and microscopic observation system 1 is provided with the long-focus objective lenses with different multiples, so that observation and selection can be conveniently carried out according to different samples and processing requirements. The laser gathering and microscopic observation system 1 is arranged on a laser gathering module mechanical moving system 8, the output end of a motion controller 9 is connected with a sample stage mechanical numerical control moving system 6, the sample stage mechanical numerical control moving system 6 is arranged on an air flotation damping platform 5, and the air inlet end of the air flotation damping platform 5 is connected with an air pump 4. The motion controller 9 of the device is used for storing and converting program commands of the computer and sending the program commands to the motor driver; the motor driver of the device is used for transmitting pulse electric signals to the stepping motor of the electric sample stage.
The femtosecond laser and the convergence scanning system of the device comprise a femtosecond laser which is formed by matching a femtosecond laser oscillator, a pumping source and a femtosecond laser amplifier and can emit ultrafast laser with the pulse width of less than 400fs and the single pulse energy of more than 50 muJ; and the combined lens is arranged at a light outlet of the laser and is used for carrying out first-stage reduction on the femtosecond laser facula.
The laser convergence and microscopic observation system 1 of the device is provided with a coaxial microscopic observation positioning system, the coaxial microscopic observation positioning system comprises a laser optical cable interface, a common optical cable interface, an electric coaxial light source change-over switch (a light source automatic change-over switch 11), a laser CCD camera 7, a common microscope eyepiece, an objective lens and a group of ultralong focal length objective lenses with different multiplying powers, and laser in the optical fiber is converged for the second time so as to meet the requirements of processing and processing precision.
The laser convergence module mechanical moving system 8 drives the laser convergence and microscopic observation system 1 to move randomly in x, y and z three-dimensional spaces, and is used for focusing of a microscope and moving of light spots. The mechanical numerical control moving system 6 of the sample stage drives the sample stage to move randomly in x, y and z three-dimensional spaces, the repeated positioning precision can reach 0.1 mu m, the mechanical numerical control moving system 6 of the sample stage realizes the rotation and the tilting of the sample in the plane, and the numerical control and the real-time state monitoring of the sample are realized. The laser convergence and microscopic observation system 1 is provided with a microscopic imaging system with adjustable magnification and a coaxial light source, and is used for positioning laser spots and observing, processing and treating samples, the observation resolution can reach 0.5 mu m, the cutting resolution can reach 4 mu m, and the laser spots can reach 4 mu m. And the numerical control and real-time monitoring of the mechanical displacement are realized through computer control software, the repeated positioning precision is 0.5 mu m, and the moving speed is 1 mm/min-1000 mm/min and can be continuously adjusted.
Sample platform machinery numerical control mobile system 6 includes: a set of combined sliding tables capable of moving randomly in x, y and z three-dimensional spaces; one is a light-transmitting and sealing sample cavity (namely a protective atmosphere sample cavity) which can be filled with protective gas such as Ar gas; a detection device capable of monitoring the converged laser energy in real time; the sample table (namely the clamping sample table) can clamp film samples, fiber samples, block samples and other samples with different shapes; a liquid nitrogen cooling low-temperature processing table. Wherein:
the combined sliding tables can move randomly in x, y and z three-dimensional spaces, each sliding table in each direction is controlled by a separate servo motor, the three-dimensional combined sliding tables of x, y and z are connected into the same motion controller 9 and further connected into a computer, and a graphic program needing to be processed is input through a displacement control software window of the computer, so that the continuous and adjustable movement with the repeated positioning precision of 0.5 mu m and the movement speed of 1-1000 mm/min can be realized. Meanwhile, the sample is also provided with a sliding table rotating in the plane, and the sample is rotated by computer software under the control of a servo motor.
A light-transmitting sealing sample cavity capable of being filled with protective gas such as Ar gas is provided with an air suction port, an air charging port and an air exhaust port, a gas flowmeter is arranged at the front end of the air charging port, and the positive pressure anti-oxidation protective environment of inert gas during laser processing or ash residue left during sample cutting can be swept by adjusting the reading of the flowmeter. Meanwhile, a mechanical dry pump is arranged at the front end of the pumping hole, so that a vacuum environment of less than 5Pa can be obtained in the closed cavity. And an anti-reflection lens of laser with a specific wavelength is arranged above the cavity and used for processing a sample in the cavity by penetrating the femtosecond laser.
As shown in fig. 2, the protective atmosphere sample chamber comprises: the device comprises a mechanical vacuum pump 12, an exhaust valve 13, a protective gas cylinder 14, a gas mass flow controller 15, an air inlet valve 16, a laser anti-reflection window 17 and a sample cavity 18, and has the following specific structure: an exhaust valve 13 is arranged at the upper part of one side of the sample cavity 18, and the lower part of one side of the sample cavity 18 is communicated with the mechanical vacuum pump 12 through a pipeline; the other side of the sample cavity 18 is connected with a protective gas cylinder 14 through a pipeline, and a gas mass flow controller 15 and a gas inlet valve 16 are arranged on the pipeline. The light beam of the laser light source 2 or the ordinary light source 3 enters the sample cavity 18 through the laser convergence and microscopic observation system 1 via the laser anti-reflection window 17, and the sample in the sample cavity 18 is finely processed by using the microbeam femtosecond laser.
A detection device capable of monitoring the converged laser energy in real time detects the laser power actually acting on the laser beam focused by the positive objective lens by the power probe.
The structure of the sample table is that one side of the sample table is fixed, and the other side of the sample table is a sliding table which can move horizontally and adopts extrusion type to the block sample; for a fiber sample, a coaxial rotating motor is respectively arranged on the upper sides of a sliding block and a fixed block, the sample is fixed in the center of a motor bearing in a chuck mode and is controlled by a computer, and the sample rotates in one dimension; for the film samples, the fixation was performed using a top pressed sheet.
As shown in fig. 3, the holding sample stage includes: horizontal slip table 19, preforming 20, adjustable speed motor 21, fibre chuck 22, fixed station 23, the concrete structure is as follows: the horizontal sliding table 19 and the fixed table 23 are arranged oppositely, the pressing sheet 20, the speed-adjustable motor 21 and the fiber chuck 22 are respectively arranged on the horizontal sliding table 19 and the fixed table 23, and the horizontal sliding table 19 corresponds to the fiber chuck 22 on the fixed table 23.
A liquid nitrogen cooling low-temperature processing table is provided with a liquid nitrogen cooling chamber and a heat insulation cavity. Further, the liquid nitrogen cooling chamber comprises: a liquid nitrogen inlet and an exhaust.
As shown in fig. 4, the liquid nitrogen-cooled cryogenic processing station includes: the liquid nitrogen injection port 24, the exhaust port 25, the heat insulating material 26, the stainless steel cavity 27 and the pressing sheet 28 have the following specific structures: the stainless steel cavity 27 is arranged in the heat insulation material 26, the lower part of one side of the stainless steel cavity 27 is connected with the liquid nitrogen injection port 24 through a pipeline, the top of the stainless steel cavity 27 is provided with the exhaust port 25 and the pressing sheet 28, and the sample is arranged on the top of the stainless steel cavity 27 through the pressing sheet 20.
The computer centralized data monitoring and visualization system comprises: the software for numerical control and real-time monitoring of mechanical displacement can input vector diagrams such as CAD (computer-aided design), can edit programs to realize switching between laser and common light, realizes processing of some complex images and has a certain degree of automation characteristic; one set can form images with laser CCD camera image, conveniently carry out and implement observation, measurement and accurate positioning, also possess functions such as shooing, video recording and adding the scale simultaneously.
The damping system comprises an air-floating optical platform and an air pump which are matched for use, is mainly used for installing a sample platform mechanical numerical control moving system and a coaxial microscopic observation positioning system, and can prevent the vibration and light spot deviation of a sample in the processing process through a firm mechanical fixing mode so as to improve the precision and stability of processing and treatment.
The protection system includes: the protective cover covers the mechanical numerical control moving system and the coaxial microscopic observation positioning system of the sample stage, so that the damage of laser light leakage to operators is prevented; a filter glasses is mainly used for protecting eyes of operators from laser injury during working.
By utilizing the device, the femtosecond laser can be used for rapidly and conveniently processing various electron microscope samples, such as: metal sheets, alumina ceramic blocks, transparent quartz glass and the like are subjected to fine processing such as numerical control cutting, punching and the like. Therefore, the invention can prepare in-situ electron microscope samples with specific shapes and gaps, can carry out in-situ observation research on mechanical, electrical and corrosion behaviors and the like on certain special tissues and structures by combining the in-situ observation technology of the electron microscope, and has the advantages of wide processing area, high precision, no heat influence area, no pollution and the like. Particularly for in-situ observation of a sample, the influence on the structure of the sample is required to be reduced or avoided as much as possible in the processing process, and the femtosecond laser processing device and the femtosecond laser processing method adopted by the invention can excellently reduce or even eliminate a heat affected zone and meet the requirement of preparing an electron microscope in-situ sample.
As shown in fig. 1, the present invention provides a material processing method, which utilizes the above experimental apparatus to perform laser processing on a material through the steps of micro-positioning, laser parameter selection, laser focusing, numerical control programming, etc., and specifically includes the following steps:
(S1) analyzing the material to be processed, selecting a proper laser, looking up the data to find the ablation threshold value of the material, using the ablation threshold value as a reference, detecting the energy of the actually processed light spot by using a power detector, selecting parameters such as proper laser power, the multiple of the adopted microscope objective, the moving speed of the sample stage mechanical numerical control moving system 6 during processing and the like, and connecting the selected laser optical cable into the laser converging and microscopic observation system 1.
Parameters of the laser light wave wavelength, the laser power, the repetition frequency, the type of the laser generator and the like of the used laser can be selected according to actual processing requirements, material types and the like.
(S2) selecting a proper sample stage, and fixing the sample on the sample stage. The ordinary light source 3 is turned on, the height of a microscope in the laser convergence and microscopic observation system 1 is adjusted, focusing is carried out, imaging is carried out on a microscope imaging software window of the computer 10 through observing the CCD camera 7, the position needing to be processed is selected, and the laser and the ordinary light are coaxial light, so that the laser spot is positioned in the center of the imaging of the CCD camera 7.
For toxic materials, which are easily reactive with gases in the air, a protective atmosphere chamber may be used. The block material adopts a pressing type clamping method, and the film and fiber type adopts a tabletting type clamping method.
(S3) opening the displacement control software window of the computer 10, inputting the graph and the processing parameter to be processed therein or importing the saved graph processing file, and at this time, the trial operation can be carried out, so as to ensure that the laser processing process is not interrupted due to the reasons of the overrange of the sample platform and the like.
(S4) closing the laser protective cover to prevent the laser leakage from causing injury to the operator or others.
(S5) the normal light source 3 is turned off, and the laser parameters are set. And starting the programmed processing program to perform processing operation. At the moment, the machining process can be monitored in real time through a microscope imaging software window and a displacement control software window on a computer.
(S6) when the operation of the processing program is finished, the laser is closed, the protective cover is opened, and the processed sample can be taken out.
The invention is further explained or illustrated by the following examples.
Example 1 a scanning electron microscope single crystal Ni in situ tensile V-notch sample was processed.
As shown in fig. 1, the apparatus for processing is as described above.
The processing method comprises the following steps: clamping the single crystal Ni sheet on a sample table, selecting an infrared femtosecond laser with the wavelength of 1040nm, and setting the power of the laser. And (3) carrying out the detailed steps of the material processing method to obtain the required scanning in-situ tensile sample with the V-shaped notch.
The embodiment result shows that the device can quickly and conveniently utilize femtosecond laser to treat various materials, such as: metallic nickel plate, transparent quartz glass, etc., and is subjected to fine processing with a sample size of less than 10cm × 10 cm. Meanwhile, the in-situ electron microscope sample almost without a heat influence area can be obtained by adjusting the single pulse energy, the spot size, the moving speed of the mechanical platform and the like of the femtosecond laser. Therefore, the invention can carry out numerical control processing with large range, high precision and low loss on the material, and can not influence the original microstructure of the sample after cutting processing as far as possible. The method has the advantages of high positioning precision, high energy concentration, small processing loss, high visualization degree, high automation degree, no noise, no pollution, no heat influence area and the like. And the material can be processed in a micro-nano scale by combining with the digital imaging of a microscope, so that the method has a wide application prospect in the field of in-situ electron microscope sample preparation and is greatly helpful in scientific research of the materials.
The device and the method for preparing the in-situ electron microscope sample by using the converged femtosecond laser are described in detail above. The principles and embodiments of the present invention are described herein using specific examples, which are presented only to assist in understanding the method and core concepts of the present invention. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (10)
1. The utility model provides an adopt and assemble femto second laser preparation normal position electron microscope sample's device which characterized in that, the device includes: the system comprises a femtosecond laser, a convergence scanning system, a sample stage mechanical numerical control moving system, a coaxial microscopic observation positioning system, a computer centralized data monitoring and visualization system, a damping system and a protection system, wherein the femtosecond laser of a laser light source is emitted from the laser, converged by a multi-stage laser combined lens, and connected to the coaxial microscopic observation positioning system in a coaxial light form through different interfaces with the common cold light of a common light source; the coaxial microscopic observation positioning system and the sample stage mechanical numerical control moving system are connected with a computer centralized data monitoring and visualization system through a USB (universal serial bus) line or a network cable, and the structure is as follows:
the laser light source and the ordinary light source are respectively connected to the laser convergence and microscopic observation system in a coaxial light mode through an interface through an optical cable, and are switched through the electric switch; the laser convergence and microscopic observation system is connected with the input end of the CCD camera, and the output end of the CCD camera and the input end of the motion controller are connected with a computer through a USB (universal serial bus) line or a network cable to carry out microscopic observation positioning and numerical control programming; the laser convergence and microscopic observation system is provided with the long-focus objective lenses with different multiples, and observation selection is carried out according to different samples and processing requirements; the laser gathering and microscopic observation system is arranged on the laser gathering module mechanical moving system, the output end of the motion controller is connected with the sample table mechanical numerical control moving system, the sample table mechanical numerical control moving system is arranged on the air floatation damping platform, and the air inlet end of the air floatation damping platform is connected with the air pump.
2. The apparatus for preparing in-situ electron microscope samples by using condensed femtosecond lasers according to claim 1, wherein the femtosecond laser and the condensed scanning system comprise: the femtosecond laser device is formed by matching a femtosecond laser oscillator, a pumping source and a femtosecond laser amplifier and emits ultrafast laser with the pulse width of less than 400fs and the single pulse energy of more than 50 mu J; and the combined lens is arranged at a light outlet of the laser and is used for carrying out first-stage reduction on the femtosecond laser facula.
3. The apparatus of claim 1, wherein the coaxial micro-observation positioning system comprises a laser cable interface, a common optical cable interface, an electric coaxial light source switch, a laser CCD camera, a common microscope eyepiece, an objective lens, and a set of ultra-long focal length objective lenses with different magnifications, and the coaxial micro-observation positioning system is used for performing secondary convergence on the laser in the optical fiber.
4. The apparatus for preparing in-situ electron microscope samples by using condensed femtosecond lasers according to claim 1, wherein the sample stage mechanical numerical control moving system comprises: a set of combined sliding tables which can move freely in x, y and z three-dimensional space; a light-transmitting and sealing sample cavity communicated with protective gas; a detecting device for monitoring the converged laser energy in real time; a sample stage for holding a film sample, a fiber sample and a bulk sample; a liquid nitrogen cooling low temperature processing table; wherein,
the combined sliding tables move randomly in x, y and z three-dimensional spaces, each direction sliding table is controlled by a separate servo motor, the three-dimensional combined sliding tables of x, y and z are connected into the same controller and further connected into a computer, and a graphic program needing to be processed is input through a displacement control software window of the computer, so that the continuously adjustable movement with the repeated positioning precision of 0.5 mu m and the movement speed of 1-1000 mm/min is realized; meanwhile, a sliding table rotating in the plane is also arranged, and the sample is rotated by computer software under the control of a servo motor;
the sample cavity is provided with an air exhaust port, an inflation port and an exhaust port, a gas flowmeter is arranged at the front end of the inflation port, and the gas flowmeter is used for adjusting the reading of the flowmeter to realize the protective environment of positive pressure anti-oxidation of inert gas during laser processing or blow the ash residue left during cutting of the sample; meanwhile, a mechanical dry pump is arranged at the front end of the air extraction opening, and a vacuum environment of less than 5Pa is obtained in the closed cavity; a laser anti-reflection lens is arranged above the cavity and used for processing a sample in the cavity through femtosecond laser;
the liquid nitrogen cooling low-temperature processing table is provided with a liquid nitrogen cooling chamber and a heat insulation cavity; further, the liquid nitrogen cooling chamber comprises: a liquid nitrogen inlet, an exhaust port;
a detection device for monitoring the converged laser energy in real time, wherein a power probe is used for focusing the laser beam on the positive objective lens and detecting the laser power actually acting;
the structure of the sample stage is that one side of the sample stage is fixed, and the other side of the sample stage is a sliding table which moves horizontally and adopts extrusion type to the block sample; for thin slice and fiber samples, a coaxial rotating motor is respectively arranged at the upper sides of a sliding block and a fixed block, the samples are fixed in the center of a motor bearing in a tabletting mode and are controlled by a computer, and the samples rotate in one dimension; for the film samples, the fixation was performed using a top pressed sheet.
5. The apparatus for preparing in situ electron microscope samples using condensed femtosecond lasers according to claim 1, wherein the computer centralized data monitoring and visualization system comprises: a set of software for carrying out numerical control and real-time monitoring on mechanical displacement realizes the switching between laser and common light and the processing of images by inputting a CAD vector diagram and editing a program; one set of laser CCD camera image of imaging, conveniently carry out and implement observation, measurement and accurate positioning, also possess simultaneously and shoot, record a video and add the scale function.
6. The apparatus for preparing in-situ electron microscope samples by using condensed femtosecond lasers according to claim 1, wherein the shock absorption system comprises an air-floating optical platform and an air pump, is used for installing a sample stage mechanical numerical control moving system and a coaxial microscopic observation positioning system, and adopts a mechanical fixing mode to prevent the samples from vibrating and light spots from deviating during the processing process; the protection system includes: the protective cover covers the mechanical numerical control moving system and the coaxial microscopic observation positioning system of the sample stage, so that the damage of laser light leakage to operators is prevented; a filter glasses for protecting the eyes of the operator while working.
7. A method for preparing in situ electron microscope samples using a focused femtosecond laser using the device according to any one of claims 1 to 6, wherein the method comprises the following steps:
(1) a microscopic positioning step, namely determining a processing area;
(2) programming a processing graph, and editing processing parameters;
(3) selecting laser parameters, namely selecting the laser parameters meeting the processing requirements;
(4) starting a mechanical moving system and a laser;
(5) and a detection step, namely monitoring the processing process in real time.
8. A method for preparing in situ electron microscope samples using a focused femtosecond laser using the device according to any one of claims 1 to 6, wherein the method comprises the following steps:
(1) putting a sample in a sample cavity, pumping a vacuum with a pressure less than 5Pa by using a mechanical pump, introducing protective gas to atmospheric pressure, pumping again, and then pumping again for three times; finally, opening an exhaust valve to enable protective gas to flow in the cavity, and keeping the pressure of the cavity higher than one atmosphere to enable the pressure in the cavity to reach 0.105-0.11 MPa;
(2) a microscopic positioning step, namely determining a processing area;
(3) programming a processing graph, and editing processing parameters;
(4) selecting laser parameters, namely selecting the laser parameters meeting the processing requirements;
(5) starting a mechanical moving system and a laser;
(6) and a detection step, namely monitoring the processing process in real time.
9. A method for preparing in situ electron microscope samples using a focused femtosecond laser using the device according to any one of claims 1 to 6, wherein the method comprises the following steps:
(1) fixing the sample on the upper surface of the cooling cavity by using a pressing sheet, and adding liquid nitrogen to cool the cavity;
(2) a microscopic positioning step, namely determining a processing area;
(3) programming a processing graph, and editing processing parameters;
(4) selecting laser parameters, namely selecting the laser parameters meeting the processing requirements;
(5) starting a mechanical moving system and a laser;
(6) and a detection step, namely monitoring the processing process in real time.
10. The method for preparing in-situ electron microscope samples by using the condensed femtosecond laser according to claim 7, 8 or 9, wherein the method further comprises selecting an objective lens for microscopic observation and condensing the laser; the method further includes a storing step of storing the edited processing drawing; the method further comprises a step of importing, namely importing a processing drawing stored before or an existing CAD vector drawing; the method further comprises a laser spot adjusting step, wherein the size of the laser spot is adjusted to meet the processing requirement.
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