CN113984484B - Multiple ion cutting device with nano etching precision - Google Patents
Multiple ion cutting device with nano etching precision Download PDFInfo
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- CN113984484B CN113984484B CN202111625998.0A CN202111625998A CN113984484B CN 113984484 B CN113984484 B CN 113984484B CN 202111625998 A CN202111625998 A CN 202111625998A CN 113984484 B CN113984484 B CN 113984484B
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Abstract
The invention belongs to the technical field of sample surface treatment, and aims to solve the problem that an ion cutting device in the prior art cannot perform quantitative repeated cutting and repeated positioning for multiple times, in particular to a nanometer etching precision repeated ion cutting device which comprises a master control center, a wide ion beam source, a constant temperature system, a sample transmission platform, a sample etching vacuum chamber, a wide ion beam source vacuum chamber, a vacuum pump and a vacuum gauge, wherein the vacuum pump is connected with the vacuum gauge and the wide ion beam source vacuum chamber; the top of the wide ion beam source vacuum chamber is provided with a vacuum chamber cover plate, and the vacuum chamber cover plate is provided with a transparent observation window which is positioned right above the ion beam convergence point; the wide ion beam source comprises one or more ion guns for generating a wide ion beam to slice the sample; the invention can realize repeated high-precision cutting and positioning of ion cutting.
Description
Technical Field
The invention belongs to the technical field of sample surface treatment, and particularly relates to a multiple-ion cutting device with nanometer etching precision.
Background
Ion polishing is a surface treatment method, is widely applied to sample surface treatment in the early stage of material, semiconductor device, rock and mineral surface analysis and test, provides a sample with a flat surface for surface analysis and test, and the flat sample surface is beneficial to observation and analysis, thereby improving the accuracy and efficiency of surface analysis and test; surface analysis tests include, but are not limited to, optical microscopy, scanning electron microscopy, and ion probe analysis tests, among others. Specifically, ion polishing is performed by ionizing gas by using an ion source to generate ions, accelerating the ions, and bombarding the surface of a sample by using the accelerated ions to perform etching and polishing, so that a damaged layer on the surface of the sample is removed, and the sample with a real structure and a smooth surface is obtained.
The ion polishing is divided into plane rotation polishing without an ion beam baffle plate and ion cutting with the ion beam baffle plate; the plane rotation polishing is easily influenced by the difference between the original roughness of the sample and the etching efficiency of different components, and the flatness of the sample is not high by ion cutting; and ion cutting, wherein the ion beam baffle plate is positioned in front of the bearing surface of the sample table and is in contact with the sample and used for covering the sample, so that the covered part of the sample is not cut by the argon ion beam. The part of the sample slightly higher than the ion beam baffle plate is the cut part of the sample, and the surface of the cut part of the sample, which is in contact with the argon ions, is an ion bombardment surface. The argon ion beam continuously bombards the ion bombarding surface of the sample, so that the sample positioned on the ion bombarding surface is continuously removed, and then the ion bombarding surface continuously sinks from the side surface of the sample until the top surface of the sample forms a flat sample cutting surface.
The existing argon ion polishing device structure only considers the situation of carrying out sample surface analysis and test after single polishing, a static ion cutting sample stage is usually fixedly connected with a vacuum chamber of a polishing machine, a sample is separated from an ion beam shielding plate after primary polishing to cause that the sample cannot be repositioned, and a dynamic ion cutting sample stage can realize the purpose of keeping the relative positions of the ion beam shielding plate and the sample to move simultaneously, but does not have the capability of accurately moving multiple samples relative to the ion beam shielding plate; however, in the current experimental tests, the requirement for multiple ion cutting of samples is more and more, for example, the three-dimensional spatial structure of a sample cannot be predicted only by a once cutting surface observation result of a plurality of samples with strong heterogeneous structures, such as micro-nano porous network structures of batteries, shale gas reservoirs and the like, and the spatial structure of the sample can be well determined only by performing secondary or tertiary ion cutting and observation imaging; and (4) re-polishing the damaged test sample, wherein secondary surface observation needs to be carried out after nano indentation and micro indentation are carried out on the polished section of the sample. Obviously, the existing ion cutting device can not meet the requirement of repeated quantitative polishing of different samples for multiple times.
Meanwhile, for a heat-sensitive sample, a refrigeration mechanism is generally required to be arranged on an argon ion polishing device, the existing argon ion polishing device is refrigerated through liquid nitrogen, but the liquid nitrogen refrigeration has many problems, the liquid nitrogen refrigeration efficiency is uncontrollable, the liquid nitrogen temperature is extremely low, and the sample which is not low-temperature resistant can be damaged. The semiconductor refrigerating chip is a device for producing cold by using the Peltier effect of a semiconductor, two different metals are connected by a conductor, and when direct current is switched on, the temperature of one contact point is reduced, and the temperature of the other contact point is increased. The semiconductor refrigeration is generally used for electronic equipment and wireless communication equipment to refrigerate electronic components, the cold end of a refrigeration piece is directly attached to the electronic components, and the hot end of the refrigeration piece is directly connected with a cooling fan to dissipate heat.
Disclosure of Invention
In order to solve the problems in the prior art, namely to solve the problem that the ion cutting device in the prior art cannot perform quantitative repeated cutting and repeated positioning for multiple times, the invention provides a multiple-time ion cutting device with nanometer etching precision.
The vacuum system is used for providing a vacuum environment; the vacuum system comprises a sample etching vacuum chamber, a wide ion beam source vacuum chamber, a vacuum pump and a vacuum gauge, wherein the vacuum pump is connected with the vacuum gauge and the wide ion beam source vacuum chamber, the wide ion beam source vacuum chamber is connected with the sample etching vacuum chamber through a sliding rail assembly, and the wide ion beam source vacuum chamber and the sample etching vacuum chamber form a closed chamber body; the top of the wide ion beam source vacuum cabin is provided with a vacuum cabin cover plate, the vacuum cabin cover plate is provided with a transparent observation window, and the transparent observation window is positioned right above the ion beam convergence point.
The wide ion beam source comprises one or more ion guns for generating a wide ion beam to slice the sample; when the number of the ion guns is multiple, the wide ion beams generated by the ion guns are converged at one point; the constant temperature system is used for keeping the temperature of the sample constant; the sample transfer station is used to load calibration samples and reposition the sample transfer process.
In some preferred embodiments, the constant temperature system includes a semiconductor chilling plate, a heat transfer mechanism, a heat dissipation fan, a thermally insulated base, and a temperature sensor.
The heat dissipation end of the semiconductor refrigeration piece is abutted against the side wall of the sample etching vacuum chamber, and the refrigeration end of the semiconductor refrigeration piece is contacted with the heat transfer mechanism.
The heat transfer mechanism is used for transferring the cold quantity of the semiconductor refrigerating sheet; the heat transfer mechanism comprises a heat conduction clamping plate, a heat insulation clamping plate, a heat conduction belt, a first heat conduction adapter plate, a second heat conduction adapter plate, a heat conduction adapter plate connecting shaft and a spring, wherein the heat conduction belt comprises a straight plate section and a C-shaped section, the C-shaped section is arranged at the top of the straight plate section and is used for being fixedly connected with the first heat conduction adapter plate, and the straight plate section is arranged between the heat conduction clamping plate and the heat insulation clamping plate; the outer side of the heat-conducting clamping plate is abutted against the refrigerating end of the semiconductor refrigerating sheet; the side wall of the heat insulation clamping plate is provided with a connecting bulge fixedly connected with the sample etching vacuum chamber; the spring penetrates through the heat conduction adapter plate connecting shaft, and the heat conduction adapter plate connecting shaft is arranged between the second heat conduction adapter plate and the first heat conduction adapter plate; the second heat conduction adapter plate is fixedly connected with the sample transmission table.
The heat dissipation fan is arranged on the outer side of the sample etching vacuum cabin and opposite to the semiconductor refrigerating sheet; the heat insulation base is fixedly arranged on the inner wall of the sample etching vacuum chamber, and the sample transmission platform is arranged at the top of the heat insulation base; the temperature sensor is used for detecting the temperature information of the sample transmission platform.
In some preferred embodiments, the sample transport stage comprises a sample position adjustment mechanism, a sample fixing mechanism, an ion beam shielding mechanism and a positioning mechanism; the sample position adjusting mechanism comprises a piezoelectric ceramic block, an angle adjusting device, a bottom plate and a translation adjusting device, wherein the piezoelectric ceramic block is used for generating deformation with nanometer precision by controlling applied electric fields with different strengths; the angle adjusting device is arranged at the bottom of the piezoelectric ceramic block so as to adjust the rotation angle of the horizontal plane of the piezoelectric ceramic block; the translation adjusting device is arranged between the angle adjusting device and the bottom plate so as to adjust the horizontal displacement of the piezoelectric ceramic block; the positioning mechanism is arranged at the top of the piezoelectric ceramic block and used for detecting the spatial position of the piezoelectric ceramic block in real time and transmitting the spatial position to the master control center; the sample fixing mechanism is arranged between the ion beam shielding mechanism and the side wall of the piezoelectric ceramic block so as to clamp a sample; the ion beam shielding mechanism is used for controlling the area of the sample to be etched.
In some preferred embodiments, the sample holding mechanism comprises a first clamping plate and a second clamping plate arranged in parallel, the first clamping plate being arranged away from the side wall of the piezo ceramic block, the second clamping plate being arranged away from the side of the wide ion beam source arrangement.
The height of the first clamping plate is lower than that of the second clamping plate.
The top of the first clamping plate is arranged to be a wedge-shaped structure matched with the ion beam shielding mechanism.
One side of the second clamping plate, which is far away from the first clamping plate, is connected with the piezoelectric ceramic block through a sample height coarse adjustment structure; the sample height coarse adjustment structure is used for adjusting the height of the sample.
In some preferred embodiments, the ion beam shielding mechanism comprises an ion beam shielding plate and a shielding plate bracket, one end of the shielding plate bracket is detachably connected with the bottom plate, and the other end of the shielding plate bracket is connected with the ion beam shielding plate; one side of the ion beam shielding plate, which is far away from the shielding plate bracket, is arranged in parallel with the wedge-shaped structure.
The top of the ion beam shielding plate is provided with an imaging calibration label for calibration during image acquisition; the imaging calibration label comprises a first label and a second label, a first groove for accommodating the first label and a second groove for accommodating the second label are formed in the ion beam shielding plate, and the top surface of the first label and the top surface of the ion beam baffle are arranged in parallel and level mode.
In some preferred embodiments, the positioning mechanism comprises a plurality of laser positioning sensors, and the plurality of laser positioning sensors are in signal connection with the master control center.
And the laser positioning sensors are uniformly arranged at the top of the piezoelectric ceramic block.
In some preferred embodiments, the slide assembly comprises a slide assembly disposed on a sidewall of the wide ion beam source vacuum chamber and a guide rail assembly disposed on a sidewall of the sample etching vacuum chamber, the slide assembly and the guide rail assembly being slidably disposed relative to each other.
The sliding rail assemblies are arranged in two groups, and the two groups of sliding rail assemblies are symmetrically arranged relative to the longitudinal axis of the device.
The slider assembly comprises one or more sliders; the guide rail assembly comprises a guide rail connecting part and a guide rail, the guide rail is fixedly connected with the sample etching vacuum chamber through the guide rail connecting part, and one or more sliding blocks are matched with the guide rail.
In some preferred embodiments, the first heat-conducting adapter plate, the second heat-conducting adapter plate and the heat-conducting adapter plate connecting shaft are made of red copper.
In some preferred embodiments, the area of the heat-conducting splint is smaller than the area of the heat-insulating splint; the heat conducting clamping plate is a red copper plate.
In some preferred embodiments, the material of the heat insulation base is heat insulation ceramic.
1) The invention discloses a multi-time ion cutting device with nanometer etching precision, which is a device with low cost and high resolution and capable of being used for multi-time ion cutting, not only provides a sample transmission platform capable of keeping constant temperature, but also can improve the vertical resolution of a continuous slice used by a wide ion beam-scanning electron microscope to be in a nanometer level, and reduce the alignment difficulty of the continuous slice during three-dimensional reconstruction; compared with a focused ion beam-scanning electron microscope, the high-resolution imaging area of the sample can be expanded to the level of square millimeter, the three-dimensional imaging volume with the same high resolution is improved by at least six orders of magnitude, and the cost of the three-dimensional imaging device is greatly reduced.
2) Compared with the liquid nitrogen refrigeration of the conventional ion beam etching device, the semiconductor refrigeration piece in the scheme disclosed by the invention can be continuously used for a long time without supplementing liquid nitrogen at a certain time interval, and the corresponding cold transmission mechanism has a simpler structure.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, made with reference to the accompanying drawings.
Fig. 1 is a schematic perspective view of an embodiment of the present invention.
Fig. 2 is a schematic view of the sample etching vacuum chamber, the constant temperature system, and the sample transfer station of fig. 1.
FIG. 3 is a schematic view of the sample etching vacuum chamber of FIG. 2 from another angle.
Fig. 4 is another perspective schematic view of the constant temperature system and sample transfer station of fig. 2.
FIG. 5 is a schematic view of the thermal pedestal of FIG. 4.
FIG. 6 is a schematic view of a sample etching vacuum chamber in the present invention.
Fig. 7 is a partial structural schematic view of the thermostat system in the present invention.
Fig. 8 is a schematic view of an ion beam blocking mechanism and a sample fixing structure in the present invention.
Fig. 9 is a schematic cross-sectional view of a sample transfer station in the present invention.
Fig. 10 is a schematic view of the heat insulating splint and the heat conductive splint according to the present invention.
Description of reference numerals: 110. etching a sample into a vacuum chamber 111 and radiating fins; 120. a wide ion beam source vacuum chamber; 130. a vacuum pump; 140. a vacuum gauge; 150. a slide rail assembly 151, a slide block assembly 152, a guide rail assembly; 200. a sample transfer station; 210. a sample position adjusting mechanism 211, a piezoelectric ceramic block 212, an angle adjusting device 213, a bottom plate 214, a translation adjusting device 215 and a dovetail hole; 220. the sample fixing mechanism 221, the first clamping plate 222, the second clamping plate 223 and the sample height coarse adjustment structure; 231. an ion beam shutter, 232, a shutter holder, 233, a first label, 234, a second label; 240. a positioning mechanism; 250. a sample; 310. the heat-conducting cooling device comprises a semiconductor refrigeration sheet, 320, a heat transfer mechanism, 321, a heat insulation clamping plate, 3211, a limiting protrusion, 322, a heat-conducting clamping plate, 323, a heat-conducting belt, 324, a first heat-conducting adapter plate, 325, a second heat-conducting adapter plate, 3251, a clamping part, 326, a heat-conducting adapter plate connecting shaft, 327 and a spring; 330. a heat insulating base 331, dovetail bosses 332, flanges; 400. a wide ion beam source, 410, ion gun; 420. a wide ion beam spot.
Detailed Description
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and are not intended to limit the scope of the present invention.
The invention is further illustrated by the following examples with reference to the accompanying drawings.
Referring to fig. 1 to 9, the present invention provides a multiple ion cutting device with nanometer etching precision, which comprises a master control center, a vacuum system, a wide ion beam source 400, a constant temperature system and a sample transmission platform 200, wherein the vacuum system, the wide ion beam source, the constant temperature system and the sample transmission platform are all in signal connection with the master control center; the vacuum system is used for providing a vacuum environment; the vacuum system comprises a sample etching vacuum chamber 110, a wide ion beam source vacuum chamber 120, a vacuum pump 130 and a vacuum gauge 140, wherein the vacuum pump and the vacuum gauge are connected with the wide ion beam source vacuum chamber, the wide ion beam source vacuum chamber and the sample etching vacuum chamber are connected through a sliding rail component 150, and the wide ion beam source vacuum chamber and the sample etching vacuum chamber form a uniform closed chamber body; the top of the wide ion beam source vacuum cabin is provided with a detachable vacuum cabin cover plate, the vacuum cabin cover plate is provided with a transparent observation window, and the transparent observation window is positioned right above the ion beam convergence point 420 and is convenient for observation; the wide ion beam source includes one or more ion guns 410 for generating a wide ion beam to slice the sample; when the number of the ion guns is multiple, a plurality of wide ion beams generated by the plurality of ion guns are converged at one point; the constant temperature system is used for keeping the temperature of the sample constant, and preventing the sample expansion caused by the bombardment heat of the ion beam from influencing the slicing precision and preventing the temperature from damaging the heat-sensitive sample; the sample transfer station is located inside the sample etching vacuum chamber for loading of the calibration sample and repositioning of the sample transfer process. The nanometer etching precision multi-time ion cutting device disclosed by the invention can realize high-precision nanometer-level shale sample etching slicing, and has great significance for three-dimensional imaging of shale samples.
The constant temperature system comprises a semiconductor refrigeration piece 310, a heat transfer mechanism 320, a cooling fan, a heat insulation base 330 and a temperature sensor; the heat dissipation end of the semiconductor refrigeration piece is abutted against the side wall of the sample etching vacuum chamber, and the refrigeration end of the semiconductor refrigeration piece is contacted with the heat transfer mechanism; the heat transfer mechanism is used for transferring the cold quantity of the semiconductor refrigerating sheet; the constant temperature system is connected with the sample transmission platform in a pluggable manner.
Furthermore, the sample transmission platform is parallel to the plane of the ion beam, and the center of the side edge of the front side of the top surface of the ion beam baffle plate is superposed with the ion beam convergence point.
Specifically, the heat transfer mechanism comprises a heat conduction clamping plate 322, a heat insulation clamping plate 321, a heat conduction band 323, a first heat conduction adapter plate 324, a second heat conduction adapter plate 325, a heat conduction adapter plate connecting shaft 326 and a spring 327, wherein the heat conduction band comprises a straight plate section and a C-shaped section, the C-shaped section is arranged at the top of the straight plate section and is used for being fixedly connected with the first heat conduction adapter plate, and the straight plate section is arranged between the heat conduction clamping plate and the heat insulation clamping plate; the outer side of the heat-conducting clamping plate is abutted against the refrigerating end of the semiconductor refrigerating sheet; the side wall of the heat insulation splint is provided with a connecting bulge fixedly connected with the sample etching vacuum chamber; the spring penetrates through the heat conduction adapter plate connecting shaft, and the heat conduction adapter plate connecting shaft is arranged between the second heat conduction adapter plate and the first heat conduction adapter plate; the second heat conduction adapter plate is fixedly connected with the sample transmission platform; the heat radiation fan is arranged at the outer side of the sample etching vacuum chamber and opposite to the semiconductor refrigerating sheet; the heat insulation base is fixedly arranged on the inner wall of the sample etching vacuum chamber, and the sample transmission platform is arranged at the top of the heat insulation base; the temperature sensor is used for detecting the temperature information of the sample transmission platform, and ideally, the temperature of the sample transmission platform is independent from other parts through the heat insulation effect of the heat insulation base.
Preferably, the straight plate section and the C-shaped section are fixedly connected or integrally formed.
The first heat conduction adapter plate and the second heat conduction adapter plate are both of an L-shaped structure, the horizontal section of the first heat conduction adapter plate is arranged inside the C-shaped section, the vertical section of the first heat conduction adapter plate is arranged opposite to the vertical section of the second heat conduction adapter plate, the spring is arranged between the first heat conduction adapter plate and the second heat conduction adapter plate, and the spring pressure ensures that the first heat conduction adapter plate and the second heat conduction adapter plate are in full contact with the sample transmission table; the horizontal section of the second heat conduction adapter plate is used for being fixedly connected with the top of the sample transmission table.
Referring further to fig. 7, the end of the second heat conducting adapter plate is provided with a clamping portion 3251 for fixedly connecting with the sample transmission stage, and the clamping portion is disposed obliquely.
Referring to fig. 9 together with fig. 4, the sample transmission platform is connected with a heat insulation base in a constant temperature system arranged at the bottom in a pluggable manner, and the upper part is connected with a heat transfer mechanism in a pluggable manner; the sample transmission stage comprises a sample position adjusting mechanism 210, a sample fixing mechanism 220, an ion beam shielding mechanism and a positioning mechanism 240; the sample position adjusting mechanism comprises a piezoelectric ceramic block 211, an angle adjusting device 212, a bottom plate 213 and a translation adjusting device 214, wherein the piezoelectric ceramic block is used for generating deformation with nanometer precision by controlling applied electric fields with different strengths; the angle adjusting device is arranged at the bottom of the piezoelectric ceramic block so as to adjust the rotation angle of the horizontal plane of the piezoelectric ceramic block; the translation adjusting device is arranged between the angle adjusting device and the bottom plate so as to adjust the horizontal displacement of the piezoelectric ceramic block; the positioning mechanism is arranged at the top of the piezoelectric ceramic block and used for detecting the spatial position of the piezoelectric ceramic block in real time and transmitting the spatial position to the master control center; the sample fixing mechanism is arranged between the ion beam shielding mechanism and the side wall of the piezoelectric ceramic block so as to clamp a sample; the ion beam shielding mechanism is used for controlling the area of the sample to be etched.
It should be noted that, in this embodiment, the piezoelectric ceramic block includes a piezoelectric ceramic block body and a cover plate disposed thereon, the cover plate is disposed to protect the piezoelectric ceramic block body and to conduct cold to the sample fixing device and the sample, and the angle adjusting device is disposed immediately below the nano-stage body.
The angle adjusting device comprises a position adjusting plate and a rotary convex shaft arranged on the position adjusting plate, and the bottom of the piezoelectric ceramic block is provided with a clamping groove matched with the rotary convex shaft; the translation adjusting device comprises a position adjusting reset spring assembly and a position adjusting knob, the position adjusting reset spring assembly is arranged at one end of the position adjusting plate, the position adjusting knob is arranged at the other end of the position adjusting plate, and the position adjusting plate moves under the adjusting effect of the position adjusting reset spring assembly and the position adjusting knob to adjust the distance between the sample and the ion beam shielding mechanism. The angle adjusting device and the translation adjusting device can be locked together through locking mechanisms such as screws after angle adjustment.
The sample fixing mechanism comprises a first clamping plate 221 and a second clamping plate 222 which are arranged in parallel, and the sample 250 is arranged between the first clamping plate and the second clamping plate; the first clamping plate is arranged far away from the side wall of the piezoelectric ceramic block, and the second clamping plate is arranged at one side far away from the wide ion beam source device; the height of the first clamping plate is lower than that of the second clamping plate; the top of the first clamping plate is provided with a wedge-shaped structure matched with the ion beam shielding mechanism; one side of the second clamping plate, which is far away from the first clamping plate, is connected with the piezoelectric ceramic block through a sample height coarse adjustment structure 223; the sample height coarse adjustment structure is used for adjusting the sample height.
Further, the sample height coarse adjustment structure is for adjusting the slide rail, is provided with the arch that corresponds with the slide rail on the second splint to carry out the coarse adjustment of sample height.
The ion beam shielding mechanism comprises an ion beam shielding plate 231 and a shielding plate bracket 232, one end of the shielding plate bracket is detachably connected with the bottom plate, and the other end of the shielding plate bracket is connected with the ion beam shielding plate; one side of the ion beam shielding plate, which is far away from the shielding plate bracket, is arranged in parallel with the wedge-shaped structure; the top of the ion beam shielding plate is provided with an imaging calibration label for calibration during image acquisition; the imaging calibration label comprises a first label 233 and a second label 234, a first groove for accommodating the first label and a second groove for accommodating the second label are formed in the ion beam shielding plate, and the top surfaces of the first label and the second label are flush with the top surface of the ion beam baffle.
Further, the ion beam shutter and the imaging calibration label are two compositionally different high hardness materials, such as tungsten steel and titanium.
Furthermore, the baffle plate bracket comprises a first section of baffle plate bracket and a second section of baffle plate bracket, one end of the first section of baffle plate bracket is fixedly connected with the bottom plate, the top end of the first section of baffle plate bracket is used for bearing the second section of baffle plate bracket, and the first section of baffle plate bracket is arranged vertically to the top surface of the bottom plate; the upward longitudinal axis of the second section of baffle plate bracket and the upward longitudinal axis of the first section of baffle plate bracket are obliquely arranged; the ion beam baffle plate is arranged at the top of the second section of baffle plate bracket.
The positioning mechanism comprises a plurality of laser positioning sensors which are in signal connection with the master control center; the laser positioning sensors are uniformly arrayed on the top of the piezoelectric ceramic block to form a positioning net covering a preset area, and complete repositioning can be realized.
In this embodiment, the sample transmission stage is used for positioning a sample in other imaging instruments, where the positioning mechanism may be a transmitter, and corresponding receivers are installed in other instruments for repeated positioning, and the instrument may not be limited to a detector commonly used in a scanning electron microscope, but may also be other two-dimensional imaging instruments, such as an optical microscope, an atomic force microscope, and the like, which can implement three-dimensional imaging.
With further reference to fig. 5 and 9, the top of the heat-insulating base is provided with dovetail projections 331 and a flange 332, and the bottom of the bottom plate is provided with dovetail holes 215 matching the dovetail projections to ensure the load-bearing of the heat-insulating base on the sample transmission stage, while the installation position of the sample transmission stage is ensured by the arrangement of the dovetail projections and the flange.
Referring to fig. 2 and 6, the outer wall of the sample etching vacuum chamber is provided with a heat sink 111; further, the sample etching vacuum chamber is processed by high heat conduction metal aluminum alloy or copper, the outer part of the sample etching vacuum chamber is cut into a heat dissipation sheet shape, and the sample etching vacuum chamber is connected with the wide ion beam source vacuum chamber in a sliding mode.
Further, the slide rail assembly comprises a slide block assembly 151 arranged on the side wall of the wide ion beam source vacuum chamber and a guide rail assembly 152 arranged on the side wall of the sample etching vacuum chamber, and the slide block assembly and the guide rail assembly can be arranged in a relatively sliding manner; the slide rail assemblies are arranged in two groups, and the two groups of slide rail assemblies are symmetrically arranged relative to the longitudinal axis of the device.
Preferably, the slider assembly comprises one or more sliders; the guide rail assembly comprises a guide rail connecting part and a guide rail, the guide rail is fixedly connected with the sample etching vacuum chamber through the guide rail connecting part, and one or more sliding blocks are arranged in a matching manner with the guide rail; the sliding stroke is larger than the distance from the contact surface of the wide ion beam source vacuum chamber and the sample etching vacuum chamber to the ion beam convergence point.
Preferably, the first heat conduction adapter plate, the second heat conduction adapter plate and the heat conduction adapter plate connecting shaft are all made of red copper.
Referring to fig. 10, the area of the heat conducting clamping plate is smaller than that of the heat insulating clamping plate, in this embodiment, the heat conducting clamping plate is arranged inside the heat insulating clamping plate, the heat conducting clamping plate and the heat insulating clamping plate are matched to ensure that copper strips are tightly matched, meanwhile, a bolt is arranged on the heat conducting clamping plate and the heat insulating clamping plate, and is used for being connected with a sample etching vacuum chamber and adjusting the contact pressure of the heat conducting clamping plate, a semiconductor refrigerating sheet and the semiconductor refrigerating sheet with the sample etching vacuum chamber wall, so that the heat resistance of each surface is fully contacted and reduced, meanwhile, the refrigerating sheet cannot be damaged due to over-high irradiation of pressure, and the bearing pressure of the refrigerating sheet is smaller.
Specifically, one side of the heat insulation clamping plate 321 is provided with opposite limiting protrusions 3211, and the transverse distance between the two limiting protrusions is greater than the width of the heat conduction clamping plate and the semiconductor refrigeration sheet; the limiting bulge is used for limiting the heat conduction belt and the heat conduction clamping plate; the side of the heat conducting clamping plate is provided with a limiting groove matched with the limiting protrusion.
Preferably, the heat conducting splint is a copper plate.
Preferably, the material of the heat insulation base is heat insulation ceramic.
Preferably, the heat conduction area comprises a plurality of thin flexible copper strips, the upper portion of the heat conduction area is fixedly connected with the first heat conduction adapter plate, and the lower portion of the heat conduction area is fixedly connected with the heat insulation clamping plate and the heat conduction clamping plate, so that the heat conduction effect is guaranteed, and meanwhile, the flexibility variability of the heat conduction area facilitates the disassembly and assembly of the heat transfer mechanism.
Thermal-insulated pottery is preferred to thermal-insulated base material, and thermal-insulated base fixed connection is in sample sculpture vacuum chamber, and thermal-insulated base top is provided with the forked tail corresponding with sample transmission platform bottom dovetail, and the forked tail end is provided with the flange and is used for fixing a position sample platform mounted position, but thermal-insulated base and sample transmission platform plug are connected.
It should be noted that, in the present embodiment, the sample is shale, but the protection of the disclosed scheme of the present invention is not limited to the shale sample, and therefore, the details are not repeated herein.
Although the high-resolution continuous-slice three-dimensional imaging device focusing ion beams-scanning electron microscope can realize the nanoscale resolution at the present stage, the imaging area is extremely small, and the imaging requirement of a heterogeneous sample is difficult to meet; the combination of the wide ion beam and the scanning electron microscope can carry out large-area etching, but the vertical resolution of continuous slices cannot reach below micrometers due to the fact that the beam diameter is large, the calorific value is large, and the slice thickness is difficult to control accurately, and meanwhile, the alignment of the continuous slices is difficult during three-dimensional reconstruction due to the fact that the imaging range of a sample is deviated due to the positioning error of repeated sample disassembly and assembly. The high-resolution continuous slice wide ion beam etching device provided by the invention can improve the vertical resolution of a continuous slice used by a wide ion beam-scanning electron microscope to be nano-scale, and reduce the alignment difficulty of the continuous slice during three-dimensional reconstruction; compared with a focused ion beam-scanning electron microscope, the high-resolution imaging area of the sample can be expanded to the level of square millimeter, the three-dimensional imaging volume with the same high resolution is improved by at least six orders of magnitude, and the cost of the three-dimensional imaging device is greatly reduced.
Although a focused ion beam-scanning electron microscope in the prior art has the characteristics of high-spatial-resolution slicing and high-resolution slicing imaging, the problem of limited three-dimensional reconstruction area exists all the time, which results in the micro-nano porous network structure and distribution of samples with three-dimensional space irregularity, such as batteries, shale gas reservoirs and the like, the three-dimensional reconstruction is not representative, and the research is difficult to form unified effective understanding; the wide ion beam etching is an advanced sample surface treatment technology, but because the diameter of the wide ion beam current is large, repeated etching for multiple times is difficult to accurately control the etching thickness, and the heat brought by the large current also increases the etching error, so that the vertical resolution of the scheme is difficult to reach below micrometers; meanwhile, the error of repeated positioning of the sample can be reflected as the deviation of the imaging range of the sample, which causes difficulty in the imaging alignment of the continuous slices. In addition, the focused ion beam-scanning electron microscope is used for etching a sample layer by utilizing the focused ion beam to obtain an imaging section, and an electron beam is combined with an imaging detector to acquire two-dimensional data of each slice. The resolution of the two-dimensional image of the field emission scanning electron microscope is up to 1nm, so that the three-dimensional imaging resolution is determined by the vertical resolution, namely the thinnest etching thickness of the focused ion beam. In order to achieve extremely high etching accuracy, the ion beam is focused to tens of nanometers to several nanometers, and although the etching accuracy and the ion etching thickness are improved, the small beam cannot complete etching in large volume. The limited three-dimensional reconstruction area is a problem of the technology, which results in the micro-nano porous network structure and distribution of samples with three-dimensional space irregularity, such as batteries, shale gas reservoirs and the like, and the three-dimensional reconstruction is not representative. The diameter of a wide ion beam is 1-2mm, the efficiency is extremely high when large-area etching is carried out, but when the wide ion beam is combined with a scanning electron microscope to carry out continuous slice three-dimensional imaging, the vertical resolution of continuous slices cannot reach below micrometers due to the fact that the beam diameter is large and the heating value is large, and the slice thickness is difficult to accurately control, and meanwhile, the alignment of the continuous slices during three-dimensional reconstruction is difficult due to the fact that the imaging range of a sample is deviated due to the positioning error of repeated sample disassembly and assembly; the multiple-time ion cutting device with nanometer etching precision can realize multiple-time repeated cutting and repeated positioning of ion cutting, and ensure the cutting quality and the cutting precision.
While the invention has been described with reference to a preferred embodiment, various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention, and particularly, features shown in the various embodiments may be combined in any suitable manner without departing from the scope of the invention. It is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
In the description of the present invention, the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like, which indicate directions or positional relationships, are based on the directions or positional relationships shown in the drawings, which are for convenience of description only, and do not indicate or imply that the devices or elements must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The terms "comprises," "comprising," or any other similar term are intended to cover a non-exclusive inclusion, such that a process, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, article, or apparatus.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
Claims (9)
1. A multi-time ion cutting device with nanometer etching precision is characterized by comprising a master control center, a vacuum system, a wide ion beam source, a constant temperature system and a sample transmission platform, wherein the vacuum system, the wide ion beam source, the constant temperature system and the sample transmission platform are in signal connection with the master control center;
the vacuum system is used for providing a vacuum environment; the vacuum system comprises a sample etching vacuum chamber, a wide ion beam source vacuum chamber, a vacuum pump and a vacuum gauge, wherein the vacuum pump is connected with the vacuum gauge and the wide ion beam source vacuum chamber, the wide ion beam source vacuum chamber is connected with the sample etching vacuum chamber through a sliding rail assembly, and the wide ion beam source vacuum chamber and the sample etching vacuum chamber form a closed chamber body; the top of the wide ion beam source vacuum cabin is provided with a vacuum cabin cover plate, the vacuum cabin cover plate is provided with a transparent observation window, and the transparent observation window is positioned right above an ion beam convergence point;
the wide ion beam source comprises one or more ion guns for generating a wide ion beam to slice the sample; when the number of the ion guns is multiple, the wide ion beams generated by the ion guns are converged at one point;
the constant temperature system is used for keeping the temperature of the sample constant;
the sample transfer station is used for loading a calibration sample and repositioning the sample transfer process; the sample transmission platform comprises a sample position adjusting mechanism, a sample fixing mechanism, an ion beam shielding mechanism and a positioning mechanism; the sample position adjusting mechanism comprises a piezoelectric ceramic block, an angle adjusting device, a bottom plate and a translation adjusting device, wherein the piezoelectric ceramic block is used for generating deformation with nanometer precision by controlling applied electric fields with different strengths; the angle adjusting device is arranged at the bottom of the piezoelectric ceramic block so as to adjust the rotation angle of the horizontal plane of the piezoelectric ceramic block; the translation adjusting device is arranged between the angle adjusting device and the bottom plate so as to adjust the horizontal displacement of the piezoelectric ceramic block; the positioning mechanism is arranged at the top of the piezoelectric ceramic block and used for detecting the spatial position of the piezoelectric ceramic block in real time and transmitting the spatial position to the master control center; the sample fixing mechanism is arranged between the ion beam shielding mechanism and the side wall of the piezoelectric ceramic block so as to clamp a sample; the ion beam shielding mechanism is used for controlling the area of the sample to be etched.
2. The multiple-ion cutting device with nanometer etching precision according to claim 1, wherein the constant temperature system comprises a semiconductor refrigeration piece, a heat transfer mechanism, a cooling fan, a heat insulation base and a temperature sensor;
the heat dissipation end of the semiconductor refrigeration piece is abutted against the side wall of the sample etching vacuum chamber, and the refrigeration end of the semiconductor refrigeration piece is contacted with the heat transfer mechanism;
the heat transfer mechanism is used for transferring the cold quantity of the semiconductor refrigerating sheet; the heat transfer mechanism comprises a heat conduction clamping plate, a heat insulation clamping plate, a heat conduction belt, a first heat conduction adapter plate, a second heat conduction adapter plate, a heat conduction adapter plate connecting shaft and a spring, wherein the heat conduction belt comprises a straight plate section and a C-shaped section, the C-shaped section is arranged at the top of the straight plate section and is used for being fixedly connected with the first heat conduction adapter plate, and the straight plate section is arranged between the heat conduction clamping plate and the heat insulation clamping plate; the outer side of the heat-conducting clamping plate is abutted against the refrigerating end of the semiconductor refrigerating sheet; the side wall of the heat insulation clamping plate is provided with a connecting bulge fixedly connected with the sample etching vacuum chamber; the spring penetrates through the heat conduction adapter plate connecting shaft, and the heat conduction adapter plate connecting shaft is arranged between the second heat conduction adapter plate and the first heat conduction adapter plate; the second heat-conducting adapter plate is fixedly connected with the sample transmission table;
the heat dissipation fan is arranged on the outer side of the sample etching vacuum cabin and opposite to the semiconductor refrigerating sheet; the heat insulation base is fixedly arranged on the inner wall of the sample etching vacuum chamber, and the sample transmission platform is arranged at the top of the heat insulation base; the temperature sensor is used for detecting the temperature information of the sample transmission platform.
3. The apparatus according to claim 2, wherein the sample holding mechanism comprises a first clamping plate and a second clamping plate arranged in parallel, the first clamping plate is arranged away from the side wall of the piezoelectric ceramic block, and the second clamping plate is arranged away from the wide ion beam source apparatus;
the height of the first clamping plate is lower than that of the second clamping plate;
the top of the first clamping plate is provided with a wedge-shaped structure matched with the ion beam shielding mechanism;
one side of the second clamping plate, which is far away from the first clamping plate, is connected with the piezoelectric ceramic block through a sample height coarse adjustment structure; the sample height coarse adjustment structure is used for adjusting the height of the sample.
4. The apparatus according to claim 3, wherein the ion beam shielding mechanism comprises an ion beam shielding plate and a shielding plate bracket, one end of the shielding plate bracket is detachably connected to the bottom plate, and the other end of the shielding plate bracket is connected to the ion beam shielding plate; one side of the ion beam shielding plate, which is far away from the shielding plate bracket, is arranged in parallel with the wedge-shaped structure;
the top of the ion beam shielding plate is provided with an imaging calibration label for calibration during image acquisition; the imaging calibration label comprises a first label and a second label, a first groove for accommodating the first label and a second groove for accommodating the second label are formed in the ion beam shielding plate, and the top surface of the first label and the top surface of the ion beam baffle are arranged in parallel and level mode.
5. The multiple-ion cutting device with nanometer etching precision according to claim 1, wherein the positioning mechanism comprises a plurality of laser positioning sensors, and the plurality of laser positioning sensors are in signal connection with the master control center;
and the laser positioning sensors are uniformly arranged at the top of the piezoelectric ceramic block.
6. The apparatus of claim 1, wherein the slide assembly comprises a slide assembly disposed on a sidewall of the wide ion beam source vacuum chamber and a guide assembly disposed on a sidewall of the sample etching vacuum chamber, the slide assembly and the guide assembly being slidably disposed relative to each other;
the two groups of sliding rail assemblies are symmetrically arranged relative to the longitudinal axis of the system;
the slider assembly comprises one or more sliders; the guide rail assembly comprises a guide rail connecting part and a guide rail, the guide rail is fixedly connected with the sample etching vacuum chamber through the guide rail connecting part, and one or more sliding blocks are matched with the guide rail.
7. The apparatus according to claim 2, wherein the first heat conducting adapter plate, the second heat conducting adapter plate, and the heat conducting adapter plate connecting shaft are made of red copper.
8. The apparatus according to claim 2, wherein the heat-conducting clamping plate has an area smaller than that of the heat-insulating clamping plate; the heat conducting clamping plate is a red copper plate.
9. The apparatus according to claim 2, wherein the thermal insulating base is made of a thermal insulating ceramic.
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| JP5732421B2 (en) * | 2012-03-26 | 2015-06-10 | 株式会社日立ハイテクノロジーズ | Ion milling equipment |
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