CN115565835A - Scanning electron microscope sample introduction protection device for air sensitive sample and use method thereof - Google Patents
Scanning electron microscope sample introduction protection device for air sensitive sample and use method thereof Download PDFInfo
- Publication number
- CN115565835A CN115565835A CN202211125138.5A CN202211125138A CN115565835A CN 115565835 A CN115565835 A CN 115565835A CN 202211125138 A CN202211125138 A CN 202211125138A CN 115565835 A CN115565835 A CN 115565835A
- Authority
- CN
- China
- Prior art keywords
- sample
- sleeve
- electron microscope
- sample chamber
- chamber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
-
- 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
- H01J37/18—Vacuum locks ; Means for obtaining or maintaining the desired pressure within the vessel
-
- 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 objects or the material; Means for adjusting diaphragms or lenses associated with the support
Abstract
The invention discloses a scanning electron microscope sample introduction protection device for an air sensitive sample and a using method thereof. The sample cabin is sealed in the sleeve by a resistance rubber plug capable of realizing good air tightness, and a sample chamber for loading a sample to be tested is arranged in the sample cabin; the fork-shaped baffle is used to ensure that the sample compartment is in a static sealed state during the preparation phase. Before testing, the parts of the sleeve are assembled in the glove box, and then the fixed base and the sleeve are fixed on an electron microscope sample table. The fork-shaped baffle is quickly drawn out before the electron microscope is vacuumized, the sample cabin is driven by the spring to slowly move towards the observation window on the sleeve, the sample cabin is kept in a closed state during the process, and when the electron microscope is in high vacuum, the sample cabin moves in place and is completely exposed in the electron microscope. The sample introduction method can ensure that the sample is not contacted with the air all the time, thereby simply, conveniently and effectively realizing the nondestructive sample introduction of the air sensitive sample.
Description
Technical Field
The invention relates to the technical field of scanning electron microscopes, in particular to a scanning electron microscope sample feeding protection device for an air sensitive sample and a using method thereof.
Background
The scanning electron microscope is a very common instrument analysis means for observing the microscopic morphology of a material and determining micro-area components, and the testing steps generally comprise three parts, namely sample preparation, sample transfer and electron microscope analysis. The sample transfer refers to a process of transferring a sample to be measured into a sample chamber of a scanning electron microscope, and in the case of a conventional sample, the process does not have any influence on the sample, but in the case of a sample sensitive to air, such as a simple metal like lithium, sodium and the like which are easily oxidized in the air, or a sample which is very easily deliquesced like calcium chloride and the like, the sample is inevitably exposed to the air in the step. Although the exposure time can be reduced to seconds, irreversible damage to the sample can occur, even resulting in ineffective test results.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a simple and convenient sample protection device with strong operability, so that the sample is ensured not to be contacted with air all the time in the process of transferring to a scanning electron microscope, and the possibility of sample deterioration is avoided; the sample protection device does not need external force drive, does not need to modify the electron microscope sample chamber, is simple, convenient and reliable in use process, can be widely applied to scanning electron microscopes of various manufacturers/models, and is high in applicability.
In order to achieve the purpose, the invention provides a scanning electron microscope sample injection protection device for an air sensitive sample, wherein a sleeve is a cylindrical hollow cylinder, the bottom end of the cylindrical hollow cylinder is sealed, and the top end of the cylindrical hollow cylinder is connected with a sleeve screw cap through threads; the sleeve screw cap is provided with a plurality of screw cap round holes which are communicated with each other and are used for keeping the spring chamber in the sleeve communicated with the external atmosphere and maintaining the air pressure balance at two sides of the sample chamber sealed in the sleeve during vacuumizing. A hollowed-out part with a rectangular projection is arranged on the side wall of the sleeve close to the bottom end and is an observation window; a sample chamber is hermetically arranged in the sleeve, resistance rubber plugs are respectively adhered to the circular cross sections at the two ends of the sample chamber, and a plurality of circles of rubber plug annular bulges are arranged on the outer edges of the resistance rubber plugs in a surrounding manner; a cuboid cavity is arranged in the sample chamber and is a sample chamber, the opening direction of the sample chamber is vertical to the long axis of the sleeve, and a sample table is fixedly arranged in the sample chamber; a plurality of baffle jacks are arranged at the contact positions of the observation window and the sample cabin, and fork-shaped baffles are clamped and placed on the baffle jacks; a spring chamber is arranged between the sample chamber and the sleeve screw cap, and a compression spring is arranged in the spring chamber; the upper surface of the fixed base is provided with two raised slide rail clamping grooves for sliding in and fixing two sheet-shaped supporting legs extending obliquely downwards and arranged below the outer side wall of the sleeve.
The outer diameter of the sleeve is 25-50mm, the length of the sleeve is 50-80mm, the thickness of the side wall of the sleeve is 2-3mm, the thickness of the bottom of the sleeve is 1-2mm, and the sleeve is made of one of aluminum and copper; the outer wall of the top opening of the sleeve is provided with sleeve external threads, and the thread width of the sleeve external threads is 2-4mm and is used for being connected with the sleeve screw cap in a screwing mode. The sleeve screw cap is a round metal cap made of one of aluminum and copper; the diameter of the inner edge of the annular convex part of the sleeve screw cap is consistent with the outer diameter of the sleeve, screw cap internal threads are arranged, the width of the threads is 2-4mm, and the threads can be screwed and sealed with sleeve external threads arranged on the outer wall of the sleeve; the thickness of the annular convex part of the sleeve screw cap is 2mm, the height of the protrusion is 3-5mm, and the thickness of the circular cap top is 1-2mm.
The main body of the sample cabin is a section of metal cylinder with the middle hollowed and the diameter consistent with the inner diameter of the sleeve, the length of the metal cylinder is 12-20mm, and the metal cylinder is made of one of aluminum or copper; the hollowed direction of the sample cabin is perpendicular to the longitudinal axis of the cylinder of the sleeve, the hollowed cavity part in the shape of a cuboid is a sample chamber, the width of the sample chamber is less than 90% of the diameter of the sample cabin, the length of the sample chamber is 10-18mm, the depth of the sample chamber is not more than 75% of the diameter of the sample cabin, and the residual thickness of two ends of the cabin body is 1-1.5mm; the size of the observation window is equivalent to the size of a sample chamber in the sample cabin.
The resistance rubber plug is a circular thin rubber sheet with the thickness of 2-4mm, the diameter of the rubber sheet is equal to the inner diameter of the sleeve and the diameter of the sample cabin, and the thickness of the rubber plug close to the observation window is larger than that of the rubber plug at the end contacted with the compression spring; the protruding height of the rubber plug annular bulge is 0.5mm, and the width is 1mm. The resistance rubber plug is used for realizing good air tightness between the sample cabin and the sleeve, increasing the friction coefficient of the sample cabin moving in the sleeve and providing enough long protection time for samples in the cabin.
A sample platform jack is arranged at the center of the bottom of the sample chamber, is a round hole with the depth of 2-4mm and the diameter of 2-3mm, and is used for inserting and fixing a sample platform; the sample table comprises a surface type sample table, a section type sample table and a mixed type sample table, the material is one of aluminum or copper, the base of the sample table is a cuboid, the length and the width of the sample table are completely consistent with the size of the sample chamber, the height of the sample table is different according to the sample, and the distance between the fixed sample on the sample table and the observation window is ensured to be 1-5 mm; the nail legs are arranged below the sample table base, and the diameter and the length of the nail legs are matched with the insertion holes of the sample table, so that the sample table can be completely and stably placed in the sample chamber.
The spring chamber is a cavity for accommodating the compression spring in the sleeve and is positioned between the sample chamber and the sleeve screw cap. The outer diameter of the compression spring is consistent with the inner diameter of the sleeve, the length of the compression spring is 20-60mm, and the diameter of the spring steel wire is less than 1.6mm; when the compression spring is in a compressed state, one end of the compression spring is propped against the resistance rubber plug of the sample chamber, and the other end of the compression spring is propped against the screwed sleeve screw cover.
The fork-shaped baffle is positioned between the observation window and the sample cabin, is a baffle with a plurality of strip-shaped extending ends, has the thickness of 2-3mm and the width not exceeding the diameter of the sleeve, and is made of one of titanium or aluminum; the extending direction of the long-strip-shaped extending end of the fork-shaped baffle is consistent with the inserting or pulling direction of the baffle, and the upper part of the fork-shaped baffle is fixed on a horizontal straight-strip-shaped cross bar; the fork-shaped baffle is inserted along the preset baffle jack position on the side wall of the sleeve, and after the fork-shaped baffle is completely inserted, the long-strip-shaped extending end of the fork-shaped baffle is just clamped into the jack at the bottom of the inner wall of the sleeve; the cross bar at the upper part of the fork-shaped baffle is provided with a circular sheet-shaped fork-shaped baffle handle, so that the fork-shaped baffle can be conveniently inserted and pulled out. The fork-shaped baffle is inserted from the direction perpendicular to the long axis of the sleeve and clings to one side of the sample chamber to prevent the sample chamber from moving under the action of the pressure of the spring and is pulled out manually before the electron microscope sample chamber is vacuumized.
The fixing base is a metal sheet with a cuboid main body and is made of one of aluminum or copper; the length of the sleeve is 40-70mm, the width of the sleeve is 30-60mm, the thickness of the sleeve is 2-3mm, and two slide rail clamping grooves extending upwards are arranged on the upper surface of the sleeve and are used for being clamped into two sheet-shaped supporting legs extending obliquely downwards at the bottom of the sleeve; the length of the slide rail clamping groove is 40-70mm, and the distance between the clamping grooves is 30-60mm; the sheet-shaped support legs are long sheets, the length of each sheet-shaped support leg is 30-60mm, the thickness of each support leg is 1-2mm, and the distance between every two support legs is 30-60mm; the width of the part of the flaky supporting leg clamped in the slide rail clamping groove is 2-3mm. The slide rail clamping groove is matched with the flaky supporting legs of the sleeve in shape, the sleeve is ensured to be stably fixed on the sample stage of the electron microscope, and the bottom of the fixed sleeve is tightly attached to the surface of the fixed base.
A method for using the device for protecting the sample introduction of the scanning electron microscope for the air-sensitive sample, which comprises the following steps:
a. assembling a sample injection protection device: fixing a sample to be detected on a sample table of the protection device under the protection of glove box atmosphere, inserting a nail leg below a base of the sample table into a sample table insertion hole at the bottom of a sample chamber, and stably placing the sample table in the sample chamber in a sample chamber; slowly pushing the sample chamber from one end of the sleeve opening to be close to the observation window; inserting the fork-shaped baffle into a baffle jack arranged on the sleeve to enable the sample cabin to be blocked outside the observation window; the compression spring is loaded from one side of the sleeve opening and the sleeve is screwed tightly, so that the compression spring is sealed in the spring chamber in a compressed state, and the assembly of the sample injection protection device is completed;
b. fixing the sleeve on an electron microscope sample table: b, taking the sample injection protection device assembled in the step a out of the glove box, preparing to be transferred into a scanning electron microscope, and sealing the device in a thick self-sealing bag filled with argon before transfer so as to further protect the sample; firmly fixing the fixed base on an electron microscope sample table by using a conductive adhesive tape, and pushing the sheet-shaped support legs at the bottom of the sleeve into the slide rail clamping grooves on the base to complete the fixation of the sleeve on the electron microscope sample table;
c. the sample chamber moves towards the observation window in the sleeve: rapidly pulling out the fork-shaped baffle, closing the cabin door of the electron microscope sample chamber and rapidly vacuumizing, wherein the sample chamber which is not blocked by the fork-shaped baffle slowly moves towards the observation window under the self-driving of the compression spring, and controlling the moving speed to ensure that the sample chamber is communicated with the atmosphere of the electron microscope sample chamber through the observation window by adjusting the relevant parameters of the resistance rubber plug and the compression spring, so that the inside of the electron microscope sample chamber reaches a high vacuum state;
d. and (3) observing by an electron microscope: and finally moving the sample cabin to one side of the seal of the sleeve, completely exposing the sample in the sample cabin below the observation window, and immediately carrying out normal electron microscope test.
The sample introduction protection device comprises a sleeve, a sleeve screw cap, a spring chamber, a compression spring, a sample chamber, a resistance rubber plug, a fork-shaped baffle, an observation window, a fixed base and the like. Wherein the sample chamber and the spring chamber are sealed in the sleeve, and the sample chamber with the sample chamber is arranged in front of the spring chamber. The sleeve is screwed to the opening end of the sleeve, namely one end of the spring chamber, so that the spring arranged in the spring chamber is in a compressed state, and one end of the compression spring is propped against one side of the sample chamber at the moment, and a driving force is provided for the movement of the sample chamber to the observation window in the sleeve. In the assembly stage of the sample introduction protection device, the sample cabin is sealed in the sleeve in the glove box, and good air tightness in the sample cabin is realized by means of the resistance rubber plug, so that the sample is ensured to be always under the protection of argon. A fork-shaped baffle is arranged at one end of the sample cabin close to the observation window, so that the sample cabin is prevented from moving towards the observation window before being transferred to the electron microscope.
After the whole device is placed into a scanning electron microscope sample chamber and fixed, the fork-shaped baffle is pulled out, and the cabin door of the electron microscope sample chamber is closed quickly to start vacuumizing. In the process, the sample chamber in the closed state slowly moves to the observation window under the self-driving of the spring; by adjusting the moving speed of the sample chamber, the sample chamber moves to the state that the observation window is communicated with the atmosphere of the electron microscope sample chamber, and the electron microscope sample chamber is in a high vacuum state, so that the electron microscope sample introduction without air contact in the whole process is realized. And when the sample cabin finally reaches the top end of the sleeve and is completely exposed below the observation window, normal electron microscope observation can be carried out. In order to ensure that the sleeve is stably fixed on the sample stage of the electron microscope in the whole process, the device is provided with a fixed base which can be fixed on the sample stage of the electron microscope, and the sleeve and the fixed base are connected and fixed through a sliding rail.
Compared with the prior art, the invention has the beneficial effects that: the sample cabin is driven to move in the sleeve independently through the compression spring, so that the scanning electron microscope lossless sample introduction of the air sensitive sample is realized effectively and controllably, and the sample is ensured not to be contacted with air all the time in the transferring and electron microscope sample room vacuumizing processes. The design of the resistance rubber plugs at two sides of the sample chamber not only ensures the air tightness of a sample chamber in the chamber, but also increases the moving resistance, prolongs the sample protection time, and can realize the regulation and control of the protection time by regulating the resistance of the rubber plugs and the parameters of the compression spring; the driving force of the compression spring is ingeniously utilized, external force is not needed, an electron microscope sample chamber is not transformed, the use is simple and convenient, the compression spring is suitable for electron microscopes of various brands and models, and the practicability is high.
Drawings
FIG. 1 is a perspective view of the internal structure of a sample protection device for a scanning electron microscope according to the present invention;
FIG. 2 is a cross-sectional view of the sample injection protection device for a scanning electron microscope of the present invention;
FIG. 3 is an external view of the sample injection protection device for scanning electron microscope of the present invention;
FIG. 4 is an external view of the sleeve;
FIG. 5 is a perspective view of the sleeve screw cap;
FIG. 6 is a side view of the sample compartment;
FIG. 7 is a cross-sectional view of the sample chamber;
FIG. 8 is a schematic view of a sample stage;
FIG. 9 is a cross-sectional view of a forked baffle;
FIG. 10 is a side view of the stationary base;
in the figure: 1-a sleeve; 2-screwing a sleeve; 3-observation window; 4-baffle jack; a 5-forked baffle; 501-a fork-shaped baffle handle; 6-external thread of the sleeve; 7-a sheet foot; 8-screwing the internal thread of the cover; 9-screwing a cover round hole; 10-a sample chamber; 11-a resistance plug; 12-annular bulge of the rubber plug; 13-a sample chamber; 14-sample stage jack; 15-sample stage; 1501-surface type sample stage; 1502-section sample stage; 1503-hybrid sample stage; 16-a spring chamber; 17-a compression spring; 18-a stationary base; 19-slide rail clamping groove.
Detailed Description
The invention is further illustrated but is not in any way limited by the following specific examples.
The invention provides a sample introduction protection device for a scanning electron microscope of an air sensitive sample, which is shown in the attached figures 1-10, wherein a sleeve 1 is a cylindrical hollow cylinder, the bottom end of the cylindrical hollow cylinder is sealed, the top end of the cylindrical hollow cylinder is connected with a sleeve screw cap 2 through threads, and a plurality of through screw cap round holes 9 are arranged on the sleeve screw cap 2; a hollowed-out part with a rectangular projection is formed in the side wall, close to the bottom end, of the sleeve 1, and is an observation window 3; a sample chamber 10 is hermetically arranged in the sleeve 1, two ends of the sample chamber 10 are respectively adhered with a resistance rubber plug 11, and the outer edge of the resistance rubber plug 11 is provided with a plurality of circles of rubber plug annular bulges 12 in a surrounding manner; a cuboid cavity serving as a sample chamber 13 is arranged in the sample chamber 10, the opening direction of the sample chamber 13 is vertical to the long axis of the sleeve 1, and a sample table 15 is fixedly arranged in the sample chamber; a plurality of baffle jacks 4 are arranged at the contact positions of the observation window 3 and the sample cabin 10, and fork baffles 5 are clamped on the baffle jacks 4; a spring chamber 16 is arranged between the sample chamber 10 and the sleeve screw cap 2, and a compression spring 17 is arranged in the spring chamber 16; the upper surface of the fixed base 18 is provided with two raised slide rail slots 19 for sliding in and fixing two sheet-shaped support legs 7 extending obliquely downwards and arranged below the outer side wall of the sleeve 1.
A method for using the device for protecting the sample introduction of the scanning electron microscope for the air-sensitive sample, which comprises the following steps:
a. assembling a sample injection protection device: fixing a sample to be detected on a sample table 15 of the protection device under the protection of glove box atmosphere, inserting a nail leg below a base of the sample table 15 into a sample table insertion hole 14 at the bottom of a sample chamber 13, and stably placing the sample table 15 in the sample chamber 13 in a sample cabin 10; slowly pushing the sample chamber 10 from the open end of the sleeve 1 to close to the observation window 3; inserting a fork-shaped baffle 5 into a baffle jack 4 arranged on the sleeve 1 to block the sample chamber 10 outside the observation window 3; the compression spring 17 is loaded from the side of the opening of the sleeve 1 and the sleeve screw cap 2 is screwed tightly, so that the compression spring 17 is sealed in the spring chamber 16 in a compressed state, and the assembly of the sample injection protection device is completed;
b. fixing the sleeve on an electron microscope sample table: b, taking the sample injection protection device assembled in the step a out of the glove box, preparing to be transferred into a scanning electron microscope, and sealing the device in a thick self-sealing bag filled with argon before transfer so as to further protect the sample; the fixed base 18 is firmly fixed on the electron microscope sample table by using a conductive adhesive tape, and the sheet-shaped support legs 7 at the bottom of the sleeve 1 are pushed into the slide rail clamping grooves 19 on the base to complete the fixation of the sleeve 1 on the electron microscope sample table;
c. the sample chamber moves towards the observation window in the sleeve: rapidly pulling out the fork-shaped baffle 5, closing the cabin door of the electron microscope sample chamber and rapidly vacuumizing, wherein the sample chamber 10 which is not blocked by the fork-shaped baffle 5 moves slowly towards the observation window 3 under the self-driving of the compression spring 17, and controlling the moving speed by adjusting the relevant parameters of the resistance rubber plug 11 and the compression spring 17 to ensure that the sample chamber 13 is communicated with the atmosphere of the electron microscope sample chamber through the observation window 3, and the electron microscope sample chamber is in a high vacuum state;
d. and (3) observing by using an electron microscope: the sample chamber 10 will finally move to the sealed side of the sleeve 1, and the sample therein will be exposed under the observation window 3 completely, and then the normal electron microscope test will be performed.
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings, however, the present invention is not limited to the specific details of the embodiments described below, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications all fall within the protection scope of the present invention.
Example 1
The outer diameter of the sleeve 1 is 30mm, the length is 50mm, the side wall thickness is 2mm, the material is copper, the bottom thickness of the bottom end sealing position is 2mm, the projection dimension of the observation window 3 is 20mm in length and 14mm in width; an upper group of baffle jacks 4 and a lower group of baffle jacks 4 are designed on the side wall of the sleeve 1 at the contact positions of the observation window 3 and the projection part thereof and the sample chamber 10, the jacks are square with the side length of 2mm, and the positions of the jacks are matched with the long-strip-shaped extending ends of the fork-shaped baffles 5. The length of the flaky support legs 7 at the outer side of the sleeve 1 is 40mm, the thickness is 1mm, the distance between the support legs is 36mm, the width of the part clamped in the slide rail clamping groove 19 on the base is 2mm, and the bottom of the sleeve 1 is tightly attached to the surface of the fixed base 18 after the sleeve is fixed on the base; the width of the external thread of the sleeve 1 is 3mm.
The sleeve screw cap 2 is made of metal copper, the diameter of the inner edge of the annular convex part of the sleeve screw cap is 30mm, threads are designed on one side of the inner edge, the width of the inner edge is 3mm, and the inner edge can be screwed and sealed with the opening end of the sleeve 1 with the external threads; the thickness of the annular convex part of the sleeve screw cap 2 is 2mm, the height of the convex part is 4mm, and the thickness of the circular cap top is 1mm; the sleeve screw cap 2 is provided with four screw cap round holes 9 on the surface of the cap top, and the aperture is 2mm.
The length of sample cabin 10 is 12mm, and the diameter is 26mm, and the material is metal aluminium, excavates out a shape along the vertical axis direction of perpendicular to sample cabin 10 and is the hollow part of cuboid, and the width is 10mm, and length is 20mm, and degree of depth 12mm, the remaining thickness in cabin body both ends is 1mm.
The diameter of the resistance rubber plug 11 is 26mm, wherein the thickness of the rubber plug on the side contacting with the compression spring 17 is 2mm, and the thickness of the other side is 3mm, and the resistance rubber plug is flatly adhered to the circular cross sections at the two ends of the sample chamber 10 by using super glue respectively. The design of the outer edge of the rubber plug with the thickness of 3mm is surrounded by two circles of annular bulges 12 of the rubber plug, the design of the outer edge of the rubber plug with the thickness of 2mm is surrounded by one circle of annular bulges, the height of each bulge is 0.5mm, and the width of each bulge is 1mm.
The sample chamber 13 is a hollow part of the sample chamber 10, and a round hole with a depth of 3mm and a diameter of 2mm is designed at the center of the bottom of the sample chamber and can be inserted into and fixed with the sample table 15. The sample table 15 has a surface type, a cross-section type and a mixed type, is made of metal aluminum, has a cuboid base with the length and the width of 20mm and 10mm and the height of 12mm, and is provided with nail legs below the base, the diameter of 2mm and the length of 3mm.
The spring chamber 16 is a cavity in the sleeve 1 accommodating a compression spring 17, and has a length of 14mm. The compression spring 17 is a section of spring with the outer diameter of 26mm, is made of 304 stainless steel, is 30mm long and is 1.2mm in diameter.
The fork-shaped baffle 5 is made of metal aluminum, the thickness of the fork-shaped baffle is 2mm, the length of the straight bar at the upper part of the fork-shaped baffle is 20mm, four equally-spaced strip-shaped extension ends are designed on the fork-shaped baffle, the cross section of each extension end is square, the side length of each extension end is 2mm, and the length of each extension end is 13mm; the fork-shaped baffle handle 501 on the straight bar-shaped cross bar of the baffle is semicircular and has the diameter of 10mm.
The fixed base 18 is made of copper, and has a length of 50mm, a width of 42mm and a thickness of 2mm. The length of the slide rail clamping groove 19 on the upper surface of the slide rail clamping groove is 40mm, the distance between the clamping grooves is 36mm, the groove thickness of the clamping groove is 1mm, and the groove width is 2mm.
Preparing a lithium ion battery composite electrode into a section sample in a glove box, and sticking the section sample on a special section type sample table 1502; the sample stage 1502 is securely fixed in the sample chamber 10, and the sample chamber 10 is slowly pushed into the vicinity of the observation window 3 from the open side of the sleeve 1. Inserting the fork-shaped baffle 5 into the baffle inserting hole 4 on the sleeve 1, and fixing the position of the sample chamber 10; the compression spring 17 is loaded from the open end of the sleeve 1, the sleeve screw cap 2 is pushed against the side of the spring extending out of the sleeve and slowly applies force until the sleeve screw cap 2 is completely screwed on the sleeve 1. The assembled sleeve 1 is sealed in a thick self-sealing bag and removed from the glove box.
Observing by using a Japanese electronic scanning electron microscope JSM-7900F, fixing a fixed base 18 on a sample pedestal of the electron microscope by using a conductive adhesive tape, and fixing a sleeve 1 on the base through a sliding rail clamping groove 19; breaking vacuum in a scanning electron microscope sample exchange chamber, loading the scanning electron microscope sample exchange chamber into an electron microscope sample pedestal fixed with a sleeve 1 and a fixed base 18, pulling out a fork-shaped baffle 5, rapidly closing a door of the exchange chamber and starting vacuum pumping, wherein the estimated vacuum pumping time is about 1min, and the movement time of a sample chamber is also set to be about 1min through early adjustment.
After the sample exchange chamber is vacuumized, the sample chamber in the sleeve is moved to the position below the observation window, the sample pedestal is pushed into the sample chamber of the electron microscope, and the elemental lithium on the cross-section sample is subjected to component surface distribution analysis by utilizing the carried Oxford Extreme windowless energy spectrum.
Example 2
The outer diameter of the sleeve 1 is 40mm, the length of the sleeve is 60mm, the thickness of the side wall of the sleeve is 2mm, the material of the sleeve is metal aluminum, the bottom thickness of the sealing position of the bottom end of the sleeve is 2mm, the length of the projection dimension of the observation window 3 is 20mm, and the width of the projection dimension of the observation window is 18mm; the side wall of the sleeve 1 is provided with an upper group of baffle jacks 4 and a lower group of baffle jacks 4 at the contact positions of the observation window 3 and the projection part thereof with the sample chamber, the projections of the jacks are rectangles with the length of 3mm and the width of 2mm, and the positions of the jacks are matched with the strip-shaped extending ends of the fork-shaped baffles 5. The length of the long flaky support legs 7 on the outer side of the sleeve 1 is 40mm, the thickness of the support legs is 2mm, the distance between the support legs is 48mm, the width of the part clamped in the slide rail clamping groove 19 on the base is 2mm, and the bottom of the sleeve 1 is tightly attached to the surface of the fixed base 18 after the sleeve is fixed on the base; the width of the external thread of the sleeve 1 is 3mm.
The sleeve screw cap 2 is made of metal aluminum, the diameter of the inner edge of the annular convex part of the sleeve screw cap is 40mm, threads are designed on one side of the inner edge, the width of the inner edge is 3mm, and the inner edge can be screwed and sealed with the opening end of the sleeve 1 with the external threads; the thickness of the annular convex part of the sleeve screw cap 2 is 2mm, the height of the convex part is 4mm, and the thickness of the circular cap top is 2mm; the sleeve screw cap 2 is provided with four screw cap round holes 9 on the top surface, and the aperture is 3mm.
The length of sample cabin 10 is 15mm, and the diameter is 36mm, and the material is metal aluminium, excavates out a shape along the direction of perpendicular to sample cabin 10 axis of ordinates and is the hollow part of cuboid, and width 13mm, length are 30mm, and degree of depth 15mm, the remaining thickness in cabin body both ends is 1mm.
The diameter of the resistance rubber plug 11 is 36mm, wherein the thickness of the rubber plug on one side contacted with the compression spring 17 is 2mm, the thickness of the rubber plug on the other side is 4mm, and the resistance rubber plug is smoothly adhered to the circular cross sections at the two ends of the sample cabin 10 by strong glue respectively. The outer edge design of the rubber plug with the thickness of 4mm is surrounded by three rings of annular bulges 12 of the rubber plug, the outer edge design of the rubber plug with the thickness of 2mm is surrounded by one ring of annular bulges, the height of each bulge is 0.5mm, and the width of each bulge is 1mm.
The sample chamber 13 is a hollowed part of the sample chamber 10, and a round hole with a depth of 4mm and a diameter of 3mm is designed at the center of the bottom of the sample chamber and can be inserted into and used for fixing the sample table 15. The sample table 15 has a surface type, a section type and a mixed type, is made of metal aluminum, has a cuboid base with the length and the width of 30mm and 13mm and the height of 15mm, and is provided with nail legs below the base, the diameter of 3mm and the length of 4mm.
The spring chamber 16 is a cavity in the sleeve 1 accommodating a compression spring 17, and has a length of 15mm. The compression spring 17 is a section of spring with the outer diameter of 36mm, is made of 304 stainless steel, is 32mm long and is 1.4mm in diameter of spring steel wires. In order to meet the requirement that the sample is not allowed to have magnetism by an electron microscope, the spring is demagnetized.
The fork-shaped baffle 5 is made of metal titanium, the thickness of the fork-shaped baffle is 2mm, the length of a straight bar at the upper part of the fork-shaped baffle is 30mm, five equally-spaced strip-shaped extension ends are designed on the fork-shaped baffle, the cross section of each extension end is a rectangle with the length of 3mm and the width of 2mm, and the length of each extension end is 28mm; the fork-shaped baffle handle 501 on the straight bar-shaped cross bar of the baffle is semicircular, and the diameter of the baffle handle is 15mm.
The fixed base 18 is made of metal aluminum, and has a length of 60mm, a width of 55mm and a thickness of 3mm. The length of the slide rail clamping groove 19 on the upper surface of the slide rail clamping groove is 40mm, the distance between the clamping grooves is 48mm, the groove thickness of the clamping groove is 2mm, and the groove width is 2mm.
Preparing a fresh surface of a magnesium-aluminum alloy sample in a glove box and adhering the fresh surface to a special mixed type sample table 1503; the sample stage 1503 is securely fixed in the sample chamber 10, and the sample chamber 10 is slowly pushed into the vicinity of the observation window 3 from the open side of the sleeve 1. Inserting the fork-shaped baffle 5 into the baffle inserting hole 4 on the sleeve 1, and fixing the position of the sample chamber 10; the compression spring 17 is loaded from the open end of the sleeve 1, the sleeve screw cap 2 is pushed against the side of the spring extending out of the sleeve and force is slowly applied until the sleeve screw cap 2 is completely screwed on the sleeve 1. The assembled sleeve 1 is sealed in a thick self-sealing bag and removed from the glove box.
Observing by using a Japanese electron scanning electron microscope JSM-7610F, fixing a fixed base 18 on a sample pedestal of the electron microscope by using a conductive adhesive tape, and fixing a sleeve 1 on the fixed base 18 through a slide rail clamping groove 19; breaking vacuum of a sample exchange chamber of a scanning electron microscope, loading the sample exchange chamber into a sample pedestal fixed with a sleeve 1 and a fixed base 18, pulling out a fork-shaped baffle 5, rapidly closing a door of the exchange chamber and starting vacuum pumping, wherein the estimated vacuum pumping time is about 1min, and the movement time of the sample chamber is also set to be about 1min through early adjustment.
After the sample exchange chamber is vacuumized, the sample chamber in the sleeve is moved to the position below the observation window, the sample pedestal is pushed into the sample chamber of the electron microscope, the electron beam is turned on for morphology analysis at high pressure, and the carried Oxford X-MAX energy spectrum is used for analyzing the oxygen content in the sample.
Example 3
The outer diameter of the sleeve 1 is 50mm, the length of the sleeve is 80mm, the thickness of the side wall of the sleeve is 3mm, the material of the sleeve is copper, the bottom thickness of the sealing position of the bottom end of the sleeve is 2mm, the projection dimension of the observation window 3 is 30mm in length, and the width of the observation window is 22.5mm; an upper group of baffle jacks 4 and a lower group of baffle jacks 4 are designed on the side wall of the sleeve 1 at the contact positions of the observation window 3 and the projection part thereof with the sample chamber, the projection of the baffle jacks 4 is a square with the side length of 3mm, and the position of the baffle jacks is matched with the position of the long strip-shaped extension end of the fork-shaped baffle 5. The length of the flaky support legs 7 at the outer side of the sleeve 1 is 60mm, the thickness is 2mm, the distance between the support legs is 60mm, the width of the inner part clamped in the slide rail clamping groove 19 on the fixed base 18 is 3mm, and the bottom of the sleeve 1 is tightly attached to the surface of the fixed base 18 after the sleeve is fixed on the fixed base 18; the width of the external thread of the sleeve 1 is 4mm.
The sleeve screw cap 2 is made of metal copper, the diameter of the inner edge of the annular convex part of the sleeve screw cap is 50mm, threads are designed on one side of the inner edge, the width of the inner edge is 4mm, and the inner edge can be screwed and sealed with the opening end of the sleeve 1 with the external threads; the thickness of the annular convex part of the sleeve screw cap 2 is 2mm, the height of the convex part is 5mm, and the thickness of the circular cap top is 2mm; the sleeve screw cap 2 is provided with four screw cap round holes 9 on the top surface, and the aperture is 3mm.
The length of sample cabin 10 is 20mm, and the diameter is 44mm, and the material is metal copper, excavates out a shape along the direction of perpendicular to sample cabin 10 axis of ordinates and is the hollow part of cuboid, and the width is 17mm, and length is 30mm, and the degree of depth is 20mm, and the remaining thickness in cabin body both ends is 1.5mm.
The diameter of the resistance rubber plug 11 is 44mm, wherein the thickness of the rubber plug on one side contacted with the compression spring 17 is 3mm, and the thickness of the rubber plug on the other side is 4mm, and the resistance rubber plug is smoothly adhered to the circular cross sections at the two ends of the sample cabin 10 by strong glue respectively. The outer edge design of the rubber plug with the thickness of 4mm is surrounded by three rings of rubber plug annular bulges 12, the outer edge design of the rubber plug with the thickness of 3mm is surrounded by two rings of annular bulges, the height of each bulge is 0.5mm, and the width of each bulge is 1mm.
The sample chamber 13 is a hollow part of the sample chamber 10, and a round hole with a depth of 4mm and a diameter of 3mm is designed at the center of the bottom of the sample chamber and can be inserted into and fixed with the sample table 15. The sample table 15 has a surface type, a section type and a mixed type, is made of metal copper, has a cuboid base with the length and the width of 30mm and 17mm and the height of 20mm, and is provided with nail legs below the base, the diameter of 3mm and the length of 4mm.
The spring chamber 16 is a cavity in the sleeve 1 that accommodates a compression spring and has a length of 23.5mm. The compression spring 17 is a section of spring with an outer diameter of 44mm, is made of 304 stainless steel, is 48mm long and has a spring steel wire diameter of 1.4mm.
The fork-shaped baffle 5 is made of metal titanium, the thickness of the fork-shaped baffle is 3mm, the length of the straight bar at the upper part of the fork-shaped baffle is 30mm, six equally-spaced strip-shaped extension ends are designed on the fork-shaped baffle, the cross section of each extension end is square, the side length of each extension end is 3mm, and the length of each extension end is 35mm; the fork-shaped baffle handle 501 on the straight bar-shaped cross bar of the baffle is semicircular, and the diameter of the baffle handle is 15mm.
The fixed base 18 is made of copper, and has a length of 70mm, a width of 70mm and a thickness of 3mm. The length of the slide rail clamping groove 19 on the upper surface of the slide rail clamping groove is 70mm, the distance between the clamping grooves is 60mm, the groove thickness of the clamping groove is 2mm, and the groove width is 3mm.
Preparing a sample compounded with calcium chloride particles which are easy to absorb moisture on a special surface sample table 1501 in a glove box; the sample stage 1501 is securely fixed in the sample chamber 10, and the sample chamber 10 is slowly pushed into the vicinity of the observation window 3 from the side of the opening of the sleeve 1. Inserting the fork-shaped baffle 5 into the baffle inserting hole 4 on the sleeve to fix the position of the sample chamber 10; the compression spring 17 is loaded from the open end of the sleeve 1, the sleeve screw cap 2 is pushed against the side of the spring extending out of the sleeve and force is slowly applied until the screw cap 2 is completely screwed on the sleeve 1. The assembled sleeve 1 is sealed in a thick self-sealing bag and removed from the glove box.
Observing by using a Hitachi scanning electron microscope SU5000, fixing a fixed base 18 on a sample pedestal of the electron microscope by using a conductive adhesive tape, and fixing a sleeve 1 on the base through a slide rail clamping groove 19; the fork-shaped baffle 5 is pulled out, the chamber door of the sample chamber is quickly closed and vacuumization is started, and the moving conditions of the sample introduction device and the sample chamber 10 are observed in real time through a camera in the sample chamber; the estimated vacuumizing time is about 3min, and the movement time of the sample cabin is also set to be about 3min through early adjustment.
After the sample chamber of the electron microscope is vacuumized, and the sample chamber in the sleeve moves to the position below the observation window, the electron beam is opened to carry out surface appearance analysis on the sample at high pressure, so that the original appearance of the sample can be displayed after the influence of moisture absorption is avoided.
It will be apparent to those skilled in the art that many changes and modifications can be made, or equivalents employed, to the presently disclosed embodiments without departing from the intended scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. The utility model provides a kind protection device is advanced to scanning electron microscope for sensitive sample of air, includes sleeve (1) and unable adjustment base (18), its characterized in that: the sleeve (1) is a cylindrical hollow cylinder, the bottom end of the sleeve is sealed, the top end of the sleeve is connected with a sleeve screw cap (2) through threads, and a plurality of through screw cap round holes (9) are formed in the sleeve screw cap (2); a hollow part with a rectangular projection is arranged on the side wall of the sleeve (1) close to the bottom end and is an observation window (3); a sample chamber (10) is hermetically arranged in the sleeve (1), resistance rubber plugs (11) are respectively adhered to the circular cross sections at the two ends of the sample chamber (10), and a plurality of circles of rubber plug annular bulges (12) are arranged on the outer edges of the resistance rubber plugs (11) in a surrounding manner; a cuboid cavity which is a sample chamber (13) is arranged in the sample chamber (10), the opening direction of the sample chamber (13) is vertical to the long axis of the sleeve (1), and a sample table (15) is fixedly arranged in the sample chamber; a plurality of baffle jacks (4) are arranged on the side wall of the sleeve (1) where the observation window (3) is in contact with the sample cabin (10), and fork-shaped baffles (5) are clamped on the baffle jacks (4); a spring chamber (16) is arranged between the sample cabin (10) and the sleeve screw cover (2), and a compression spring (17) is placed in the spring chamber (16); the upper surface of the fixed base (18) is provided with two raised slide rail clamping grooves (19) for sliding in and fixing two sheet-shaped support legs (7) which extend obliquely downwards and are arranged below the outer side wall of the sleeve (1).
2. The device for protecting the sample introduction of the scanning electron microscope for the air-sensitive sample according to claim 1, characterized in that: the outer diameter of the sleeve (1) is 25-50mm, the length is 50-80mm, the side wall thickness is 2-3mm, the bottom thickness is 1-2mm, and the material is aluminum or copper; the sleeve is characterized in that a sleeve external thread (6) is arranged on the outer wall of the top end opening of the sleeve (1), and the thread width of the sleeve external thread (6) is 2-4mm and is used for being screwed and connected with the sleeve screw cap (2).
3. A scanning electron microscope sampling protection device for air sensitive samples according to claim 2, characterized in that: the sleeve screw cap (2) is a circular metal cap made of one of aluminum and copper; the diameter of the inner edge of the annular convex part of the sleeve screw cap (2) is consistent with the outer diameter of the sleeve (1), a screw cap internal thread (8) is arranged, the width of the thread is 2-4mm, and the thread can be screwed and sealed with a sleeve external thread (6) arranged on the outer wall of the sleeve (1); the thickness of the annular convex part of the sleeve screw cap (2) is 2mm, the height of the bulge is 3-5mm, and the thickness of the circular cap top is 1-2mm.
4. The protective device for the sample injection of the scanning electron microscope as claimed in claim 3, characterized in that: the main body of the sample cabin (10) is a section of metal cylinder with the middle hollowed, the diameter of the metal cylinder is consistent with the inner diameter of the sleeve, the length of the metal cylinder is 12-20mm, and the metal cylinder is made of one of aluminum and copper; the hollowing direction of the sample chamber (10) is perpendicular to the longitudinal axis of the cylinder of the sleeve (1), the hollow part which is in the shape of a cuboid after hollowing is the sample chamber (13), the width of the sample chamber (13) is less than 90% of the diameter of the sample chamber (10), the length of the sample chamber is 10-18mm, the depth of the sample chamber is not more than 75% of the diameter of the sample chamber (10), and the residual thickness of two ends of the chamber body of the sample chamber (10) is 1-1.5mm; the size of the observation window (3) is equivalent to the size of a sample chamber (13) in the sample cabin (10).
5. The scanning electron microscope sample feeding protection device according to claim 4, characterized in that: the resistance rubber plug (11) is a round thin rubber sheet with the thickness of 2-4mm, the diameter of the rubber sheet is equal to the inner diameter of the sleeve (1) and the diameter of the sample cabin (10), and the thickness of the rubber plug close to the observation window (3) is larger than that of the rubber plug at one end contacted with the compression spring (17); the protruding height of plug annular bulge (12) is 0.5mm, and the width is 1mm.
6. The scanning electron microscope sample feeding protection device according to claim 5, characterized in that: a sample table jack (14) is arranged at the center of the bottom of the sample chamber (13), the sample table jack (14) is a round hole, the depth of the round hole is 2-4mm, the diameter of the round hole is 2-3mm, and the round hole is used for inserting and fixing the sample table (15); the sample table (15) comprises a surface type sample table (1501), a section type sample table (1502) and a mixed type sample table (1503), the material is one of aluminum and copper, the base of the sample table (15) is a cuboid, the length and the width of the cuboid are completely consistent with the size of the sample chamber (13), the height of the cuboid is different according to the sample, and the distance between the sample fixed on the cuboid and the observation window (3) is ensured to be 1-5 mm; the sample platform (15) base is provided with nail legs, and the diameter and the length of the nail legs are matched with the sample platform jack (14).
7. The scanning electron microscope sample feeding protection device according to claim 6, characterized in that: the outer diameter of the compression spring (17) is consistent with the inner diameter of the sleeve (1), the length is 20-60mm, and the diameter of the spring steel wire is less than 1.6mm.
8. The scanning electron microscope sample feeding protection device according to claim 7, characterized in that: the fork-shaped baffle (5) is positioned between the observation window (3) and the sample cabin (10), is a baffle with a plurality of strip-shaped extending ends, has the thickness of 2-3mm, the width of not more than the diameter of the sleeve (1), and is made of one of titanium or aluminum; the extending direction of the long strip of the fork-shaped baffle (5) is consistent with the inserting or pulling direction of the baffle, and the upper part of the fork-shaped baffle is fixed on a horizontal straight strip-shaped cross bar; the fork-shaped baffle (5) is inserted along the position of a baffle jack (4) preset on the side wall of the sleeve, and after the fork-shaped baffle is completely inserted, the strip-shaped extending end of the fork-shaped baffle is just clamped into the jack at the bottom of the inner wall of the sleeve (1); the size and the distribution of the baffle jacks (4) are matched with the long-strip-shaped extending ends of the fork-shaped baffles (5); a disc-shaped fork baffle handle (501) is designed on the cross bar at the upper part of the fork baffle (5).
9. A scanning electron microscope sampling protection device for air sensitive samples according to claim 8, characterized in that: the fixing base (18) is a metal sheet with a cuboid main body and is made of one of aluminum and copper; the length of the sliding rail is 40-70mm, the width of the sliding rail is 30-60mm, the thickness of the sliding rail is 2-3mm, and two sliding rail clamping grooves (19) extending upwards are designed on the upper surface of the sliding rail; the length of the slide rail clamping groove (19) is 40-70mm, and the distance between the clamping grooves is 30-60mm; the flaky support legs (7) are long flaky, the length is 30-60mm, the thickness of the support legs is 1-2mm, and the distance between the support legs is 30-60mm; the width of the part of the sheet-shaped supporting foot (7) clamped in the slide rail clamping groove (19) is 2-3mm.
10. Use of a scanning electron microscope sample introduction protection device for air sensitive samples according to any of claims 1 to 9, characterized in that the method comprises the following steps:
a. assembling a sample injection protection device: fixing a sample to be detected on a sample table (15) of the scanning electron microscope sample introduction protection device under the protection of glove box atmosphere, inserting a nail leg below a base of the sample table (15) into a sample table jack (14) at the bottom of a sample chamber (13), and stably placing the sample table (15) in the sample chamber (13) in a sample chamber (10); slowly pushing the sample chamber (10) from the open end of the sleeve (1) to close to the observation window (3); inserting a fork-shaped baffle (5) into a baffle jack (4) arranged on the sleeve (1) to enable the sample chamber (10) to be blocked outside the observation window (3); a compression spring (17) is loaded from one side of an opening of the sleeve (1) and a sleeve screw cap (2) is screwed, so that the compression spring (17) is sealed in a spring chamber (16) in a compressed state, and the assembly of the sample injection protection device is completed;
b. fixing the sleeve on an electron microscope sample table: b, taking the sample injection protection device assembled in the step a out of the glove box, preparing to be transferred into a scanning electron microscope, and sealing the device in a thick self-sealing bag filled with argon before transfer so as to further protect a sample; the fixed base (18) is firmly fixed on a scanning electron microscope sample table by using a conductive adhesive tape, and the sheet-shaped supporting legs (7) at the bottom of the sleeve (1) are pushed into slide rail clamping grooves (19) on the base to complete the fixation of the sleeve (1) on the scanning electron microscope sample table;
c. the sample chamber moves towards the observation window in the sleeve: rapidly pulling out the fork-shaped baffle (5), closing the cabin door of the scanning electron microscope sample chamber and rapidly vacuumizing, wherein the sample cabin (10) which is not blocked by the fork-shaped baffle (5) slowly moves towards the observation window (3) under the self-driving of the compression spring (17), and controlling the moving speed by adjusting the relevant parameters of the resistance rubber plug (11) and the compression spring (17) to ensure that the sample chamber (13) is communicated with the atmosphere of the electron microscope sample chamber through the observation window (3) and the electron microscope sample chamber is in a high vacuum state;
d. and (3) observing by an electron microscope: and finally moving the sample cabin (10) to the sealed side of the sleeve (1), completely exposing the sample to be tested in the sample cabin below the observation window (3), and immediately carrying out normal electron microscope test.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211125138.5A CN115565835A (en) | 2022-09-15 | 2022-09-15 | Scanning electron microscope sample introduction protection device for air sensitive sample and use method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211125138.5A CN115565835A (en) | 2022-09-15 | 2022-09-15 | Scanning electron microscope sample introduction protection device for air sensitive sample and use method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115565835A true CN115565835A (en) | 2023-01-03 |
Family
ID=84740640
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211125138.5A Pending CN115565835A (en) | 2022-09-15 | 2022-09-15 | Scanning electron microscope sample introduction protection device for air sensitive sample and use method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115565835A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117405719A (en) * | 2023-12-14 | 2024-01-16 | 崇义章源钨业股份有限公司 | Thin film material section scanning electron microscope sample preparation device |
-
2022
- 2022-09-15 CN CN202211125138.5A patent/CN115565835A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117405719A (en) * | 2023-12-14 | 2024-01-16 | 崇义章源钨业股份有限公司 | Thin film material section scanning electron microscope sample preparation device |
| CN117405719B (en) * | 2023-12-14 | 2024-03-05 | 崇义章源钨业股份有限公司 | Thin film material section scanning electron microscope sample preparation device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8087309B2 (en) | Hermetic sample holder and method for performing microanalysis under controlled atmosphere environment | |
| CN115565835A (en) | Scanning electron microscope sample introduction protection device for air sensitive sample and use method thereof | |
| EP1753051A2 (en) | Method and apparatus for providing a sealed container containing a detectable gas | |
| JPH10185776A (en) | Sample vial for gas analysis, vial closing device, method using them and apparatus for execution of the method | |
| KR20200096698A (en) | Apparatus for maintaining a controlled environment | |
| WO2022001107A1 (en) | System and method for self-driven vacuum transfer of sample | |
| CN113624565A (en) | Trace atmosphere sampling detection device and trace atmosphere sampling detection method | |
| CN218447802U (en) | A scanning electron microscope advances a kind protection device for air sensitive sample | |
| US4411575A (en) | Sample transfer vessel | |
| US5036205A (en) | Apparatus for the transfer and in-situ reactions under a controlled atmosphere, of specimens for transmissive electron microscopy | |
| US10773228B2 (en) | Self-sealing container for protecting air sensitive samples | |
| JPH11201920A (en) | Sample observing and analyzing method by vacuum system observing and analyzing device, and sample box for same device | |
| US3885320A (en) | Method for transfer of freeze-dried specimens | |
| JP2003121312A (en) | Fluid sampling container and fluid sampling method | |
| CN210192152U (en) | Device capable of accommodating medical sampling containers of different specifications | |
| JP3799317B2 (en) | Column positioning method and jig for ion source for mass spectrometer | |
| CN205718216U (en) | A kind of nitrogen reduced vacuum glass desicator | |
| CN210427411U (en) | A transfer device that is used for recoverable air sensitive sample of XPS | |
| JPH07270271A (en) | Method and equipment for measuring gas barrier properties of plating film | |
| JPH11213931A (en) | Sample introducing device | |
| JPH0741446U (en) | Lid for sample tube holding rack | |
| US20240014001A1 (en) | System of scanning electron microscope sample box and method of opening the same | |
| CN217576341U (en) | Sample applicator and reagent storage device thereof | |
| CN219407719U (en) | Transfer device for XPS (X-ray diffraction) air sensitive sample | |
| CN217688863U (en) | Triazophos analysis and determination reagent device with accuse temperature function |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |