CN109632450B - Mechanism for cooling and transmitting sample in sealed cavity - Google Patents
Mechanism for cooling and transmitting sample in sealed cavity Download PDFInfo
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- CN109632450B CN109632450B CN201811375007.6A CN201811375007A CN109632450B CN 109632450 B CN109632450 B CN 109632450B CN 201811375007 A CN201811375007 A CN 201811375007A CN 109632450 B CN109632450 B CN 109632450B
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- 238000001816 cooling Methods 0.000 title claims abstract description 19
- 238000001073 sample cooling Methods 0.000 claims abstract description 11
- 238000005057 refrigeration Methods 0.000 claims abstract description 9
- 239000000523 sample Substances 0.000 claims description 158
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 19
- 230000033001 locomotion Effects 0.000 claims description 13
- 238000001514 detection method Methods 0.000 claims description 10
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 210000001503 joint Anatomy 0.000 claims description 3
- 238000010894 electron beam technology Methods 0.000 abstract description 13
- 238000010884 ion-beam technique Methods 0.000 abstract description 11
- 230000005540 biological transmission Effects 0.000 abstract description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 19
- 229910052802 copper Inorganic materials 0.000 description 19
- 239000010949 copper Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 11
- 239000002245 particle Substances 0.000 description 6
- 239000004677 Nylon Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229920001778 nylon Polymers 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65G—TRANSPORT OR STORAGE DEVICES, e.g. CONVEYORS FOR LOADING OR TIPPING, SHOP CONVEYOR SYSTEMS OR PNEUMATIC TUBE CONVEYORS
- B65G47/00—Article or material-handling devices associated with conveyors; Methods employing such devices
- B65G47/74—Feeding, transfer, or discharging devices of particular kinds or types
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a mechanism for cooling and transmitting a sample in a sealed cavity, which comprises: the low-temperature refrigeration unit is used for cooling the sealed cavity; the movable sample table is arranged in the sealed cavity; a transfer rod for transferring a sample between two or more sealed chambers. The sample cooling and transmitting device provided by the invention can be installed in micro-nano processing equipment comprising an electron beam source or an ion beam source, such as a scanning electron microscope, a transmission electron microscope, an electron beam exposure machine, a focused ion beam microscope and the like, so that the sample is cooled in vacuum, and the sample in a low-temperature state is characterized, detected or processed. And meanwhile, the sample stage is allowed to move with micron-scale precision, the sample is transmitted to other vacuum chambers, and the sample can be kept in a low-temperature state in the transmission process so as to carry out subsequent operation.
Description
Technical Field
The invention belongs to the technical field of micro-nano processing, and particularly relates to a mechanism for cooling and transmitting a sample in a sealed cavity.
Background
The cooling technology for the sample is widely applied to micro-nano processing and characterization technologies, such as terahertz low-temperature superconducting detection, a cryoelectron microscope technology, a low-temperature plasma etching technology, an ice mask electron beam exposure technology and the like. In these application scenarios, the sample is generally required to be cooled to the liquid nitrogen temperature (77K) or even the liquid helium temperature (4K) in the vacuum environment of the micro-nano processing equipment. In order to realize fixed-point sample characterization and processing, the position of the sample needs to be accurately moved, and the vibration of the sample is effectively isolated. Sometimes it is also necessary to transfer the sample between different vacuum chambers while maintaining the sample at a low temperature for the purpose of preceding or subsequent operations on the sample.
The conventional vacuum low-temperature sample table is usually fixed, a sample cannot be transferred among different vacuum chambers, and the moving stroke of the sample is very small even if some sample tables can move.
In summary, how to provide a sample cooling and transporting device capable of cooling a sample to a low temperature in micro-nano processing equipment, and allowing the sample to move with high precision and to be transferred between vacuum chambers is a technical problem that needs to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to provide a mechanism for cooling and conveying samples in a sealed cavity, which can be used for realizing cooling and high-precision and large-stroke movement of the samples in vacuum and conveying the samples between vacuum chambers.
The sealed cavity can be a detection cavity of micro-nano processing equipment, and the micro-nano processing equipment can be micro-nano processing equipment containing an electron beam source or an ion beam source, such as a scanning electron microscope, a transmission electron microscope, an electron beam exposure machine, a focused ion beam microscope and the like. The sealed cavity can be a sealed cavity obtained on the basis of the existing micro-nano processing equipment, and can also be a redesigned sealed cavity.
A mechanism for cooling and transporting a sample within a sealed chamber, comprising:
the low-temperature refrigeration unit is used for cooling the sealed cavity;
the movable sample table is arranged in the sealed cavity;
and the transfer rod is used for transferring or transmitting the sample between two or more sealed cavities.
In the invention, the low-temperature refrigeration unit can be a liquid nitrogen Dewar bottle structure, a liquid helium Dewar bottle structure, a pulse tube refrigerator, a JT refrigerator or a GM refrigerator and the like. The low-temperature refrigerating mechanism is used for providing cold energy and a low-temperature environment for the sealed cavity. Preferably, when the low-temperature refrigeration unit is of a liquid nitrogen dewar structure, the outer shell of the liquid nitrogen dewar is in sealed butt joint with the sealed cavity.
Preferably, the low-temperature cold source is a liquid nitrogen dewar (bottle) which comprises a shell, a liner bottle and a connecting pipe, the connecting pipe is led out from the top of the liner bottle and fixed on the shell through the connecting pipe, an interlayer space between the shell and the liner bottle is communicated with a vacuum cavity of a sealed cavity (such as a micro-nano processing device), and the bottom of the liner bottle is a refrigerating end. Preferably, the liquid nitrogen dewar has three connecting pipes, each connecting pipe has a length not less than 20 cm and a wall thickness not more than 1 mm. So as to reduce the heat leakage of the inner container bottle through the connecting pipe and prolong the preservation time of the liquid nitrogen in the inner container bottle. Preferably, the bottom material of the liquid nitrogen dewar is oxygen-free copper. To minimize heat loss during heat transfer.
When a pulse tube refrigerator, a JT refrigerator or a GM refrigerator and other low-temperature cold sources are adopted, the cold head is the refrigerating end.
Preferably, the refrigerator further comprises a low-temperature baffle, one end of the low-temperature baffle is connected with the refrigerating end of the low-temperature refrigerating unit, and the other end of the low-temperature baffle extends into the sealed cavity. Preferably, the low temperature baffle material is oxygen free copper. To minimize heat loss during heat transfer.
Preferably, the sealed cavity is a detection cavity of micro-nano processing equipment;
the low-temperature baffle goes deep into one end in the sealed cavity extends to the detection probe below, and the end is equipped with the hole of dodging that dodges detection probe transmission route simultaneously. For example, the low temperature baffle extends to the lower part of an electron beam source or an ion beam source of the micro-nano processing equipment, and an opening (avoiding hole) is formed in an emission path of the electron beam or the ion beam so as to pass through the electron beam or the ion beam.
Preferably, the sample stage includes:
a fixed sample holder which is fixed on the three-dimensional motion mechanism and can move in three dimensions;
and the movable sample rack is arranged in the fixed sample rack in a sliding mode and can move under the action of the transfer rod.
Preferably, the fixed sample rack is provided with a dovetail groove, and the movable sample rack is of a trapezoidal structure matched with the dovetail groove. With this configuration, even when the cooling and conveying mechanism of the present invention is used upside down, the movable sample rack is prevented from falling off from the fixed sample rack.
As an embodiment, the sample stage comprises a guide rail stage, a support column, a fixed sample holder and a movable sample holder. The guide rail table is fixed on the mobile table (or called three-dimensional motion mechanism) through a dovetail groove guide rail. The support column is fixed on the guide rail table and is vertical to the upper surface of the guide rail table; the support column is made of heat insulating materials. The fixed sample rack is arranged on the support column, and a groove is formed in the side face of the fixed sample rack. The movable sample rack is the same as the groove on the fixed sample rack, can slide into the groove and is attached to the fixed sample rack; a positioning piece used for realizing positioning with the transfer rod is arranged on the side surface of the movable sample rack; for example, the positioning element is a threaded hole formed in the side surface of the movable sample holder, and the threaded hole may be replaced by a positioning element of other structure, such as a screw structure, or a magnetic element, or a groove or hole structure for engagement, or a protrusion structure for engagement, so as to achieve relative fixation with the transfer rod; the cross section of the movable sample rack is in a shape of a rounded trapezoid.
Preferably, the support column material is nylon to prevent as much as possible heat transfer between the transfer screw and the moving sample stage.
Preferably, the fixed sample rack is arranged on the support column, and the side surface of the fixed sample rack is provided with a groove.
The movable sample rack is the same as the groove on the fixed sample rack, can slide into the groove and is attached to the fixed sample rack; the side surface of the movable sample rack is provided with a threaded hole.
Preferably, the groove is a dovetail groove; the movable sample rack is a trapezoidal block structure matched with the dovetail groove. The moving sample holder is trapezoidal in cross section (may further preferably be a rounded trapezoid). So that the movable sample rack will not fall off even if the fixed sample rack and the movable sample rack are installed in the vacuum equipment in an inverted manner, and can be in close contact with the fixed sample rack to maintain good heat conduction
Preferably, the material of the fixed sample holder and the movable sample holder is oxygen-free copper. To minimize heat loss during heat transfer.
Preferably, the front end of the transfer rod is provided with a second positioning piece for realizing mutual fixation with the movable sample rack. The second positioning element is generally configured to mate with a positioning element disposed on a side of the mobile sample holder. For example, the transfer rod may be a screw or a magnetic member provided at the tip end thereof, or may be a protrusion for engagement, or may be a groove or a hole for engagement. In one embodiment, the front end of the transfer rod is fixed with a transfer screw in a threaded manner, and the relative fixation with the moving sample rack is realized through the transfer screw. As a specific scheme, the front end of the transfer rod is provided with a screw hole for mounting a transfer screw rod; the material of the transfer screw is a heat insulating material.
Preferably, a flexible heat transfer element is arranged between the low-temperature baffle and the fixed sample rack.
Preferably, the flexible heat transfer member includes, but is not limited to, an oxygen-free copper woven belt, a red copper woven belt, a graphene strip, and the like. One end of the flexible heat transfer element is fixed at the refrigerating end of the low-temperature cold source, and the other end of the flexible heat transfer element is fixed on the fixed sample frame. The sample is cooled by the low-temperature cold source.
Preferably, the flexible heat conducting structure is externally wrapped with a heat reflective material to reduce heat loss due to heat radiation during heat transfer.
In addition, the temperature of the low-temperature baffle plate is higher than that of the flexible heat transfer element and the sample table, so that the low-temperature baffle plate has another important function, namely, the low-temperature baffle plate adsorbs residual particles and gas molecules in the vacuum cavity through the low-temperature adsorption function, and the residual particles and the gas molecules are prevented from being adsorbed on the sample to pollute the sample.
Preferably, the three-dimensional motion mechanism is a five-axis linkage mechanism. The five-axis linkage mechanism has a rotating shaft and a swinging shaft in addition to the X, Y, Z axis. The rotation axis can be an a axis (X axis) or a B (Y axis) or a C axis (Z axis), the rotation axis can rotate 360 degrees, the swing axis is one of the two remaining axes (e.g. B or C) except the rotation axis (e.g. a axis) defined, and the swing axis can generally swing within a certain angle (e.g. plus or minus 90 degrees). Preferably, the three-dimensional motion mechanism is controlled by an electromechanical device or piezoelectric ceramics to move, so that the moving platform can move in three directions of X, Y and Z (namely), the moving range is not less than 100 mm multiplied by 10 mm, and the moving precision is not less than 1 micron; can rotate 360 degrees, the inclination range is not less than minus 10 degrees to 30 degrees, and the inclination and rotation precision is not less than 0.1 degree.
In the invention, the transfer rod can be any magnetic transfer rod (or called magnetic rod), mechanical transfer rod, manipulator and other common vacuum system sample transfer tools, and the front end of the transfer rod is provided with a screw hole for mounting a transfer screw. The material of the transfer screw is a heat insulating material. In a further preferred embodiment of the present invention, the transfer bar may be an existing magnetic bar for transferring articles.
Preferably, the transfer screw material is polytetrafluoroethylene. To prevent as much as possible heat conduction between the transfer screw and the moving sample stage.
The sample cooling and conveying mechanism comprises a low-temperature cold source, a low-temperature baffle, a flexible heat transfer element, a three-dimensional movement mechanism, a sample table and a transfer rod. The low-temperature cold source is supported by the shell and connected with the wall of the micro-nano processing equipment cavity to form a closed vacuum cavity. The low-temperature baffle is fixed at the refrigerating end of the low-temperature cold source. The three-dimensional motion mechanism is positioned in a micro-nano processing equipment cavity, loads a sample table and drives the sample table to move in a three-dimensional space; the sample stage is connected with the low-temperature cold source through the flexible heat conduction structure, has the function of maintaining the low-temperature environment of the sample, and can realize the separation, installation and three-dimensional movement of the sample in the vacuum low-temperature environment; the transfer rod is used for transferring and transmitting the low-temperature sample in the vacuum environment. The sample cooling and conveying device can be integrated with micro-nano processing equipment, and keeps the low-temperature vacuum environment of a sample in the micro-nano processing process and the movement, rotation and transmission of the sample among a plurality of micro-nano processing procedures.
The sample cooling and transmitting device provided by the invention can be installed in micro-nano processing equipment comprising an electron beam source or an ion beam source, such as a scanning electron microscope, a transmission electron microscope, an electron beam exposure machine, a focused ion beam microscope and the like, so that the sample is cooled in vacuum, and the sample in a low-temperature state is characterized, detected or processed. And meanwhile, the sample stage is allowed to move with micron-scale precision, the sample is transmitted to other vacuum chambers, and the sample can be kept in a low-temperature state in the transmission process so as to carry out subsequent operation.
Drawings
Fig. 1 is a schematic structural diagram of a specific embodiment of a sample cooling and conveying device of micro-nano processing equipment provided by the invention.
Fig. 2 is an enlarged structural view of a portion a in fig. 1.
Fig. 3 is a diagram showing a state where the movable sample holder is separated from the fixed sample holder.
Detailed Description
The core of the invention is to provide a sample cooling and transmitting device of micro-nano processing equipment, which can be arranged in micro-nano processing equipment containing an electron beam source or an ion beam source, such as a scanning electron microscope, a transmission electron microscope, an electron beam exposure machine, a focused ion beam microscope and the like, and realizes the cooling, high-precision and large-stroke movement of a sample in vacuum and the transmission of the sample between vacuum chambers.
In order that those skilled in the art will better understand the disclosure, the invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Fig. 1 is a schematic structural diagram of a specific embodiment of a sample cooling and conveying device of micro-nano processing equipment provided by the invention.
Referring to fig. 2 and 3, the sample cooling and conveying device of the micro-nano processing equipment according to the embodiment of the present invention includes a low temperature refrigeration unit, a low temperature baffle 4, a flexible heat transfer element, a moving table 6, a sample table, and a transfer rod 7. The flexible heat transfer member adopts an oxygen-free copper woven belt 5.
The low temperature refrigeration unit can adopt a structure similar to an existing liquid nitrogen dewar bottle, but is an improved structure on the existing liquid nitrogen dewar bottle structure, and specifically comprises a shell 1, a liner bottle 2 and a connecting pipe 3, wherein the shell 1 is fixed on a vacuum cavity wall 9 of a micro-nano processing device (the micro-nano processing device is a scanning electron microscope in the embodiment), and can be processed into an integrated structure during processing, and also can be mutually fixed by welding, flange connection and other connection modes, so that the low temperature cavity of the low temperature refrigeration unit and the vacuum cavity of the micro-nano processing device form an integrated sealed cavity. A connecting pipe 3 is led out from the top of the inner container bottle 2, the inner container bottle 2 is fixed on the shell 1 through the connecting pipe 3, and the interlayer space between the shell 1 and the inner container bottle 2 is communicated with the vacuum cavity of the micro-nano processing equipment.
Specifically, the liquid nitrogen dewar has three connecting pipes 3, each connecting pipe is 25 cm in length, and the pipe wall thickness is 0.5 mm, so as to reduce heat conduction from the liner bottle 2 to the shell 1 and prolong the storage time of liquid nitrogen in the liner bottle. The bottom of the liquid nitrogen Dewar flask 2 is made of oxygen-free copper.
The low-temperature baffle 4 is fixed at the bottom of the inner container bottle 2 of the liquid nitrogen Dewar through an elastic gasket and a screw. Normally, the sample will adsorb the residual particles at low temperature after the temperature of the sample is reduced, but in the embodiment, the temperature of the low-temperature baffle is lower (the temperature is lower than the temperature of the flexible heat transfer member and the sample table), and the residual particles will be adsorbed on the low-temperature baffle firstly. The low-temperature baffle 4 adsorbs residual particles and gas molecules in the vacuum cavity through the low-temperature adsorption effect, so that the residual particles and the gas molecules are prevented from being adsorbed on a sample to pollute the sample.
Specifically, the cryo-baffle 4 extends to the lower portion of the electron gun 8 of the scanning electron microscope, leaving an opening (i.e., a relief hole or a relief hole) just below the muzzle of the electron gun 8 for the electron beam to pass through. The low-temperature baffle 4 is made of oxygen-free copper.
The moving stage 6 is a mechanical moving stage of the scanning electron microscope, and may adopt an existing three-dimensional moving mechanism or five-axis moving mechanism, for example, the moving stage of this embodiment may directly adopt a moving stage inherent to the scanning electron microscope, and may move in three directions of X, Y, and Z, with a moving precision of 1 micron and a moving range of 125 mm × 12 mm; can rotate 360 degrees (taking the central axis of the mobile station 6 as a rotating axis, namely a Z axis), can be inclined in a range of-10 degrees to 30 degrees (taking an X axis or a Y axis as an axis relative to a horizontal plane), and the inclination and the rotation precision are 0.1 degrees.
The sample stage comprises a guide rail stage 10, a support column 11, a fixed sample holder 12 and a movable sample holder 13.
Specifically, the rail stage 10 is fixed to the moving stage 6 via a dovetail groove rail. The support column 11 is fixed on the guide rail table 10 and is vertical to the plane of the guide rail table. The support column 11 is a nylon stud, and is connected with the guide rail table 10 and the fixed sample frame 12 through a nylon screw and a nylon nut, so that the fixed sample frame 12 is fixed relative to the guide rail table 10. The fixed sample frame 12 is erected on the support column 11, a round trapezoid groove (or a dovetail groove) is formed in the side face of the fixed sample frame, the opening width of the trapezoid groove is smaller than the width of the bottom of the trapezoid groove, and when the device needs to be inverted, the movable sample frame 13 is prevented from falling off from the fixed sample frame 12. The external structure of the movable sample holder 13 is the same as that of the trapezoidal groove on the fixed sample holder 12, and the two are mutually matched, so that the movable sample holder can slide into the groove, is tightly attached to the fixed sample holder 12 and cannot fall off. The side surface of the movable sample holder 13 is provided with a threaded hole.
Specifically, the material of the fixed sample holder 12 and the movable sample holder 13 is oxygen-free copper.
The sample platform is connected with the low temperature baffle 4 through an oxygen-free copper braided belt 5. Two ends of the oxygen-free copper braided belt 5 are welded copper sheet joints. 5 one end welding of oxygen-free copper braid over braid is at 4 lower surfaces of low temperature baffle, and the other end passes through screw and elastic washer and is fixing sample frame 12 side, and 4 temperatures of low temperature baffle this moment are less than 5 temperatures of oxygen-free copper braid over braid, and 5 temperatures of oxygen-free copper braid over braid are less than the temperature of fixing sample frame 12. The surface of the oxygen-free copper braided belt 5 is wrapped with a heat reflection material so as to reduce the external heat radiation of the oxygen-free copper braided belt 5.
The transfer rod 7 is a magnetic transfer rod, the existing commercially available magnetic rod can be selected, the front end of the transfer rod 7 is provided with a screw hole, a polytetrafluoroethylene material transfer screw 14 is installed, and the end part of the transfer screw 14 is provided with an external thread structure matched with the screw hole on the side surface of the movable sample rack 13. The transfer of the mobile sample holder 13 from one cryovacuum chamber to another is accomplished by means of the transfer rod 7.
Before cooling the sample, the sample is first fixed on the moving sample holder 13. The scanning electron microscope chamber is then evacuated. Then, liquid nitrogen is filled into the inner container bottle 2 through the connecting tube 3. The liquid nitrogen cools the bottle bottom of the inner container bottle 2, the low-temperature baffle 4 and the oxygen-free copper woven belt 5 which are connected with the bottle bottom, and then the fixed sample frame 12 and the movable sample frame 13 are cooled, and finally the sample is cooled. The top surface of the guide rail table 10 and the bottom surface of the fixed sample frame 12 are suspended to form a vacuum gap, and the fixed sample frame 12 is connected with the guide rail table 10 only through the nylon support columns 11 with low heat conductivity, so that the speed of conducting heat from the guide rail table 10 to the movable sample frame 13 is slow, and the fixed sample frame 12 and the movable sample frame 13 can be cooled to a lower temperature.
In the cooling process of sample and after the cooling is accomplished, the position of sample can be removed through mobile station 6, and oxygen-free copper braid over braid 5 can guarantee that low temperature baffle 4 and fixed sample frame 12 remain connected throughout, makes the sample maintain low temperature.
Referring to fig. 2, when the transfer sample leaves the sample stage, the transfer rod 7 is operated to extend into the cavity of the scanning electron microscope, and the positions of the sample stage 6 and the transfer rod 7 are adjusted, so that the screw hole on the movable sample holder 13 is aligned with the transfer screw 14. The transfer rod 7 is then rotated to screw the transfer screw 14 into the threaded hole in the mobile sample holder 13. Referring to fig. 3, the transfer rod 7 is then pulled to slide the movable sample holder 13 out of the groove of the fixed sample holder 14, so that the movable sample holder leaves the sample stage and can enter a subsequent detection or processing vacuum chamber for subsequent detection or processing. Since the transfer screw is made of polytetrafluoroethylene, the thermal conductivity is low, and the speed of transferring heat from the transfer rod 7 to the movable sample holder 13 is slow, so that the low temperature of the sample can be maintained in the short-time sample transferring process.
When a sample is transferred onto the sample table, the transfer rod 7 is operated to extend into the cavity of the scanning electron microscope, and the positions of the sample table 6 and the transfer rod 7 are adjusted, so that the movable sample frame 13 slides into the groove on the fixed sample frame 12. The transfer screw 14 is then screwed out of the threaded hole in the moving sample holder 13. The transfer bar 7 is then pulled away from the scanning electron scope chamber.
In this embodiment, the liquid nitrogen dewar structure may be replaced by a liquid helium dewar structure, a pulse tube refrigerator, a JT refrigerator, or a GM refrigerator.
Claims (4)
1. A mechanism for cooling and transporting a sample within a sealed chamber, comprising:
the low-temperature refrigeration unit is used for cooling the sealed cavity;
the movable sample table is arranged in the sealed cavity;
a transfer rod for transferring the sample between two or more sealed chambers;
the low-temperature baffle is connected with the refrigerating end of the low-temperature refrigerating unit at one end, and the other end of the low-temperature baffle extends into the sealed cavity;
the sealed cavity is a detection cavity of micro-nano processing equipment;
one end of the low-temperature baffle, which penetrates into the sealed cavity, extends to the position below the detection probe, and the end is simultaneously provided with an avoidance hole for avoiding the emission path of the detection probe;
the sample stage includes:
a fixed sample holder which is fixed on the three-dimensional motion mechanism and can move in three dimensions;
the movable sample rack is arranged in the fixed sample rack in a sliding mode and can move under the action of the transfer rod;
a flexible heat transfer element is arranged between the low-temperature baffle and the fixed sample rack;
when the low-temperature refrigeration unit is in a liquid nitrogen Dewar bottle structure or a liquid helium Dewar bottle structure, the shell of the liquid nitrogen Dewar bottle or the liquid helium Dewar bottle is in sealed butt joint with the sealed cavity.
2. The mechanism for sample cooling and transport within a sealed cavity of claim 1, wherein the stationary sample holder is provided with a dovetail slot and the moving sample holder is a trapezoidal structure that mates with the dovetail slot.
3. The mechanism for sample cooling and transport within a sealed cavity of claim 1, wherein the three dimensional motion mechanism is a five axis linkage.
4. The mechanism for cooling and transferring the sample in the sealed cavity according to claim 3, wherein the three-dimensional motion mechanism can drive the fixed sample frame to move in the X-axis, Y-axis and Z-axis directions with the precision of not less than 1 micron; the inclination and rotation precision is not lower than 0.1 deg.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811375007.6A CN109632450B (en) | 2018-11-19 | 2018-11-19 | Mechanism for cooling and transmitting sample in sealed cavity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811375007.6A CN109632450B (en) | 2018-11-19 | 2018-11-19 | Mechanism for cooling and transmitting sample in sealed cavity |
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| CN109632450A CN109632450A (en) | 2019-04-16 |
| CN109632450B true CN109632450B (en) | 2020-09-25 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110164744B (en) * | 2019-05-17 | 2024-04-16 | 中国科学院理化技术研究所 | Scanning electron microscope refrigerating system and method based on low-temperature solid cooling |
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| CN112505336B (en) * | 2019-09-16 | 2022-12-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Ultrahigh vacuum sample transfer equipment and method |
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