Sample temperature regulation and control device

Abstract

The utility model provides a sample temperature regulation and control device. The sample temperature regulation and control device comprises a refrigerating / heating module, a liquid nitrogen tank module, a flange module and a temperature control module, a first temperature sensor, a second temperature sensor, a heating rod and a bolt connected with one end of a copper rod in a flange module through a copper wire rope are arranged on a sample table in a refrigerating / heating module, and the other end of the copper rod is inserted into a liquid nitrogen tank; in different modes, different connection modes of the first temperature sensor, the second temperature sensor and the heating rod with the temperature control module are selected, and the temperature of the sample table (namely the temperature of the sample to be tested) is set through the temperature control module. Therefore, the temperature-sensitive sample is effectively protected from being interfered by high-energy electron beams, the temperature-sensitive sample is analyzed by using the scanning electron microscope, and the influence of temperature change on the morphology and structure of a material is researched.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of scanning electron microscopy, in particular to a sample temperature regulating device. BACKGROUND

[0002] Scanning electron microscopy is an instrument analysis technology for observing and analyzing the micro-area morphology, structure and composition of a sample, and is widely used in the fields of material science, physics, chemistry, biology and geology.

[0003] In actual applications, when analyzing the influence of temperature on the morphology and structure of temperature-sensitive sample materials by using an electron microscope, the high-energy focused electron beam needs to be bombarded on the sample for scanning electron microscope testing. For temperature-sensitive samples that are not resistant to temperature, they will inevitably be damaged to different degrees under the bombardment of the electron beam, and even cannot obtain real and effective test results. CONTENT OF THE UTILITY MODEL

[0004] Therefore, the present application provides a sample temperature regulating device for regulating the temperature of a sample to be tested, effectively protecting temperature-sensitive samples from the interference of high-energy electron beams, and realizing the analysis of temperature-sensitive samples by using a scanning electron microscope and the study of the influence of temperature changes on the morphology and structure of materials.

[0005] The present application provides a sample temperature regulating device, which comprises:

[0006] a refrigeration / heating module, a liquid nitrogen tank module, a flange module and a temperature control module;

[0007] The refrigeration / heating module comprises at least a sample stage, a first temperature sensor, a second temperature sensor and a heating rod. The sample stage is provided with three deep holes and one threaded hole on the side. The top of the sample stage is provided with a nail stage placement position. The flange module comprises at least a flange plate and a copper rod. The flange plate is provided with at least three groups of aviation plugs and aviation sockets. The flange plate has a through hole. The liquid nitrogen tank module comprises at least a liquid nitrogen tank.

[0008] The sample stage is placed with the first temperature sensor, the second temperature sensor and the heating rod through the three deep holes respectively. The first temperature sensor, the second temperature sensor and the heating rod have lead wires respectively, and the other end of the lead wires has a first conversion head. The threaded hole of the sample stage is placed with a bolt.

[0009] 3 groups of wires are led out from 3 aviation sockets respectively; one end of each group of wires has an aviation plug, and the other end has a second conversion head; the first conversion head and the second conversion head are connected respectively; the aviation plug of the wire is inserted into the aviation socket on the flange plate; the aviation plug on the flange plate is connected with the temperature control module; the copper rod is inserted at the position of the through hole of the flange plate; one end of the copper rod is connected with the bolt on the sample table through the copper wire rope; the other end of the copper rod is inserted into the liquid nitrogen tank in the liquid nitrogen tank module.

[0010] Optionally, the refrigeration / heat module further comprises a block plate, a dovetail groove and an insulating plate.

[0011] Among them, the sample table, the insulating plate, the block plate and the dovetail groove are stacked in order from top to bottom, and are fixed together by fixed bolts; and the refrigeration / heat module is fixed on the sample base of the sample chamber of the electron microscope by the dovetail groove.

[0012] Optionally, the flange plate is provided with a sealing gasket position.

[0013] Optionally, the liquid nitrogen tank is provided with an opening at the top; the opening is provided with a plug; the plug is provided with a small hole; the side of the liquid nitrogen tank is provided with a through hole, and the copper rod in the flange module is inserted from the through hole on the side of the liquid nitrogen tank.

[0014] Optionally, the flange plate is provided with a through threaded hole; the liquid nitrogen tank has a flat side, and the flat side of the liquid nitrogen tank is at an angle of 90 degrees with the bottom of the tank; the bottom of the liquid nitrogen tank is provided with a threaded hole, and the liquid nitrogen tank module further comprises a support module; the support module comprises a hollow cylinder.

[0015] One end of the hollow cylinder is provided with a cross support, the cross support is at an angle of 90 degrees with the side wall of the hollow cylinder body, the cross support is provided with a through threaded hole, and the support module and the flange plate are fixed on the interface on the side of the electron microscope chamber by the through threaded hole on the cross support, the through threaded hole on the flange plate and the non-through threaded hole around the interface of the electron microscope.

[0016] The other end of the hollow cylinder is provided with an L-shaped support, the A face and the B face of the L-shaped support are at an angle of 90 degrees, the A face of the L-shaped support is connected with one end of the hollow cylinder and is at an angle of 90 degrees with the side wall of the hollow cylinder body, the A face is provided with a through threaded hole, and the through threaded hole on the A face is connected and fixed with the flat side of the liquid nitrogen tank by a bolt; the B face is parallel to the side wall of the hollow cylinder, the B face is provided with a through threaded hole, and the through threaded hole on the B face is connected and fixed with the bottom surface of the liquid nitrogen tank by a bolt; the copper rod is suspended and inserted from the through hole on the flat side of the liquid nitrogen tank through the hollow cylinder.

[0017] Optionally, the aviation socket on the flange plate is arranged in the electron microscope chamber, and the aviation plug on the flange plate is arranged outside the electron microscope chamber, wherein the aviation socket on the flange plate in the electron microscope chamber and the aviation plug on the flange plate outside the electron microscope chamber are in communication as a whole.

[0018] Optionally, the liquid nitrogen tank is a double-layered cylindrical shape.

[0019] Optionally, the first temperature sensor is a thermocouple temperature sensor.

[0020] Optionally, the second temperature sensor is a Pt1000 temperature sensor.

[0021] Optionally, the heat insulation plate is a heat insulation ceramic plate.

[0022] According to the above scheme, the application provides a sample temperature regulating device, which comprises a refrigeration / heating module, a liquid nitrogen tank module, a flange module and a temperature control module; a first temperature sensor, a second temperature sensor, a heating rod and a bolt connected with one end of a copper rod in the flange module through a copper wire rope are arranged on a sample stage in the refrigeration / heating module, the other end of the copper rod is inserted into the liquid nitrogen tank, different first temperature sensors, second temperature sensors and heating rods are selected in different modes to connect with the temperature control module, and the temperature of the sample stage (i.e. the temperature of the sample to be measured) is set by the temperature control module. Thus, the temperature-sensitive sample can be effectively protected from the interference of high-energy electron beams, the temperature-sensitive sample can be analyzed by using a scanning electron microscope, and the influence of temperature change on the morphology and structure of the material can be studied. BRIEF DESCRIPTION OF DRAWINGS

[0023] In order to more clearly illustrate the technical solutions of the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed in the embodiment or prior art description. Obviously, the drawings in the following description are only embodiments of the present application, and those skilled in the art can obtain other drawings according to the provided drawings without creative labor.

[0024] Figure 1 A schematic diagram of a sample temperature regulating device provided by an embodiment of the present application;

[0025] Figure 2 A schematic diagram of a sample temperature regulating device provided by another embodiment of the present application;

[0026] Figure 3 A schematic diagram of a refrigeration / heating module provided by another embodiment of the present application;

[0027] Figure 4A schematic diagram of a refrigeration / heating module according to another embodiment of the present application;

[0028] Figure 5 A schematic diagram of a flange module according to another embodiment of the present application;

[0029] Figure 6 A schematic diagram of a liquid nitrogen tank according to another embodiment of the present application;

[0030] Figure 7 A schematic diagram of a support module according to another embodiment of the present application. DETAILED DESCRIPTION

[0031] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only some of the embodiments of the present application, but not all of the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of protection of the present application.

[0032] The term "comprising" and variations thereof as used in the present application are open-ended, that is, "including but not limited to". The term "based on" is "at least partially based on". The term "one embodiment" means "at least one embodiment"; the term "another embodiment" means "at least one additional embodiment"; the term "some embodiments" means "at least some embodiments". Related definitions of other terms will be given in the following description.

[0033] It should be noted that the "first", "second", and the like concepts mentioned in the present application are only used to distinguish different devices, modules or units, and are not used to limit the order or interdependence of the functions performed by these devices, modules or units.

[0034] It should be noted that the modification of "one", "multiple" mentioned in the present application is illustrative but not restrictive, and those skilled in the art should understand that unless the context clearly indicates otherwise, it should be understood as "one or more".

[0035] The embodiments of the present application provide a sample temperature regulating device, as shown in Figure 1 as shown in the schematic diagram of the top view of the sample temperature regulating device, as shown in Figure 2 as shown in the schematic diagram of the front view of the sample temperature regulating device, comprising:

[0036] The refrigeration / heating module 100, the liquid nitrogen tank module 200, the flange module 300 and the temperature control module 400.

[0037] The refrigeration / heating module 100 at least includes a sample table 110, a first temperature sensor 120, a second temperature sensor 130 and a heating rod 140; the sample table 110 is provided with three deep holes 111 and one threaded hole 112 on the side; the sample table 110 is provided with a nail table placement position 113 on the top; the flange module 300 at least includes a flange plate 310 and a copper rod 320; the flange plate 310 is provided with at least three groups of aviation plugs 311 and aviation sockets 312; the flange plate 310 has a through hole 313; the liquid nitrogen tank module 200 at least includes a liquid nitrogen tank 210.

[0038] The sample table 110 is placed with the first temperature sensor 120, the second temperature sensor 130 and the heating rod 140 through the three deep holes 111 respectively; the first temperature sensor 120, the second temperature sensor 130 and the heating rod 140 have lead wires respectively, and the other end of the lead wires has a first conversion head 114; the threaded hole 112 of the sample table is placed with a bolt 115.

[0039] Three groups of lead wires are led out from the three aviation sockets 312 respectively; each group of lead wires has an aviation plug 314 at one end and a second conversion head 315 at the other end; the first conversion head 114 and the second conversion head 315 are connected respectively; the aviation plug 314 of the lead wire is inserted into the aviation socket 312 on the flange plate 310; the aviation plug 311 on the flange plate 310 is connected with the temperature control module 400; the copper rod 320 is inserted at the position of the through hole 313 of the flange plate; one end of the copper rod 320 is connected with the bolt 115 on the sample table 100 through the copper wire rope 500; the other end of the copper rod 320 is inserted into the liquid nitrogen tank 210 in the liquid nitrogen tank module 200.

[0040] The bolt on the sample table 100 is placed in the threaded hole 112 of the sample table, the copper wire rope 500 is wound on the bolt, and the bolt is tightened to fix the copper wire rope 500 on the sample table 100.

[0041] It should be noted that, Figure 1 The shape of the sample table 110 in the above is only an example of a square, and the nail table placement position 113 is only an example of a round hole, which can be other shapes in actual application, and is not limited here.

[0042] Figure 1 The three deep holes 111 and the threaded hole 112 provided on the sample table 110 in the above are only examples, and are not limited here.

[0043] In the implementation process of the present application, the first temperature sensor 120 can be, but is not limited to, a thermocouple temperature sensor, which is used to measure the temperature of the sample to be measured placed on the sample stage and the nail stage (medium-high temperature, 0-1000℃), the second temperature sensor 130 can be, but is not limited to, a thermocouple temperature sensor, a Pt1000 temperature sensor used to measure the temperature of the sample to be measured placed on the sample stage and the nail stage (low temperature, -200-100℃), and the heating rod 140 is used to heat the sample to be measured placed on the sample stage 110 and the nail stage.

[0044] In the implementation process of the present application, the copper wire can be wound on the bolt 115, and then the bolt 115 is tightened to fix the copper wire on the side of the sample stage 110.

[0045] In the implementation process of the present application, the nail stage can be designed into various types such as cross-section type, surface type and mixed type according to actual test needs.

[0046] Optionally, in another embodiment of the present application, an embodiment of the refrigeration / heat module 100 is shown in Figure 3 The refrigeration / heat module 100 further includes a block plate 150, a dovetail groove 160 and an insulating plate 170.

[0047] Among them, the sample stage 110, the insulating plate 170, the block plate 150 and the dovetail groove 160 are stacked in order from top to bottom and fixed together by the fixing bolt 180; and the refrigeration / heat module is fixed on the sample base of the sample chamber of the electron microscope by the dovetail groove 160.

[0048] It should be noted that the insulating plate 170 can be, but is not limited to, an insulating ceramic plate, which is not limited here.

[0049] In the implementation process of the present application, two non-through threaded holes can be provided below the sample stage 110, and two through threaded holes 190 are provided on the upper and lower surfaces of the insulating plate 170, the block plate 150 and the dovetail groove 160, so that the sample stage 110, the insulating plate 170, the block plate 150 and the dovetail groove 160 are fixed in order from top to bottom by the fixing bolt 180. The positions of the non-through threaded holes and the through threaded holes are not limited. As shown in Figure 4 It is an example diagram of the refrigeration / heat module 100 after the sample stage 110, the insulating plate 170, the block plate 150 and the dovetail groove 160 are fixed in order from top to bottom by the fixing bolt 180.

[0050] It should be noted that the refrigeration / heat module 100 provided by the present application Figure 3 and Figure 4 are only example diagrams of the refrigeration / heat module 100, Figure 3The shapes of the sample table 110, the heat insulation plate 170, the block plate 150 and the dovetail groove 160 in the embodiment can also be other shapes, which can be set or changed according to actual application scenarios, and are not limited herein.

[0051] As shown in FIG. 3, Figure 5 FIG. 3 is a schematic diagram of a flange module 300 provided by the embodiment of the application, Figure 5 FIG. 3 is a schematic diagram of a flange module 300 provided by the embodiment of the application,

[0052] It can be understood that, Figure 5 Only three groups of aviation plugs 311 and aviation sockets 312 are set on the flange plate 310 for example, and more aviation plugs 311 and aviation sockets 312 can be set in actual application, which are not limited herein. Figure 5 Only O-shaped sealing gaskets and placement positions are taken as examples, and other shapes can also be used in actual application scenarios.

[0053] In another embodiment of the application, the aviation sockets 312 on the flange plate 310 are arranged in the electron microscope chamber, and the aviation plugs 311 on the flange plate 310 are arranged outside the electron microscope chamber. The aviation sockets 312 on the flange plate 310 in the electron microscope chamber and the aviation plugs 311 on the flange plate 310 outside the electron microscope chamber are in communication as a whole. Three groups of wires are respectively led out from the three aviation sockets 312 on the flange plate 310 in the electron microscope chamber, each group of wires has an aviation plug 314 at one end and a conversion head 315 at the other end, the aviation plug 314 of each group of wires is inserted into the corresponding aviation socket 312 on the flange plate 314, and the conversion head 315 of each group of wires is connected to the conversion head 114 of the wire led out from the first temperature sensor 120, the second temperature sensor 130 and the heating rod 140. The aviation plugs 311 on the flange plate 310 outside the electron microscope chamber are respectively used for connecting three groups of wires led out from the temperature control module 400, and one end of the three groups of wires has an aviation socket for being inserted into the corresponding aviation plug 311 on the flange plate 310.

[0054] In the implementation process of the present application, the copper rod 320 is inserted through the flange plate 310 from the inside to the outside of the through hole 313, and is perpendicular to the flange plate 310. The copper rod 320 in the electron microscope chamber can be a short rod with a groove for tying the copper wire rope 500 to the groove. The other end of the copper wire rope 500 is fixed to the side of the sample table 110 by a bolt 115. The copper rod 320 outside the electron microscope chamber is a long rod used to extend into the liquid nitrogen tank 210. The low temperature of the liquid nitrogen in the liquid nitrogen tank 210 is conducted to the sample table 110 through the copper rod 320 and the copper wire rope 500, and then to the sample to be tested, realizing the refrigeration of the sample to be tested.

[0055] As shown in Figure 6 , it is a schematic diagram of the liquid nitrogen tank 210 provided by the present application. The top of the liquid nitrogen tank 210 is provided with an opening 211. The opening 211 is provided with a plug 212. The plug 212 is provided with a small hole 213.

[0056] It should be noted that in the implementation process of the present application, the liquid nitrogen tank 210 can be but not limited to a double-layer cylindrical shape. The double-layer structure is used for heat preservation, which is not limited here. The opening 211 is used for pouring liquid nitrogen. The plug 212 can be a T-shaped cylindrical plug used for heat preservation. The small hole 213 penetrates the top and bottom surfaces of the plug and is used for exhaust.

[0057] The liquid nitrogen tank is provided with a through hole 214 on the side. The copper rod 320 in the flange module 300 is inserted from the through hole 214 on the side of the liquid nitrogen tank. The liquid nitrogen tank 210 has a flat side 215 which is at an angle of 90 degrees with the bottom of the tank. The flat side 215 is provided with two non-penetrating threaded holes 216. The bottom of the liquid nitrogen tank 210 is provided with a threaded hole.

[0058] The liquid nitrogen tank module 200 further comprises a support module 600; as shown in Figure 7 , the support module 600 comprises a hollow cylinder 610. One end of the hollow cylinder 610 is provided with a cross support 611 which is at an angle of 90 degrees with the side wall of the cylinder body of the hollow cylinder 610. The cross support 611 has a through threaded hole 612. The support module 600 and the flange plate 310 are integrally fixed on the interface on the side of the electron microscope chamber by the through threaded hole 612 on the cross support, the through threaded hole 316 on the flange plate 310 and the non-penetrating threaded hole around the interface of the electron microscope. Among them, the threaded hole at the bottom of the liquid nitrogen tank 210 penetrates the outer layer of the double-layer structure at the bottom of the tank.

[0059] The other end of the hollow cylinder 610 is provided with an L-shaped support 613, the A face and the B face of the L-shaped support 613 are 90 degrees, wherein the A face of the L-shaped support 613 is connected with one end of the hollow cylinder 610 and is 90 degrees with the side wall of the hollow cylinder 610, the A face is provided with a through threaded hole 614, the through threaded hole 614 of the A face is connected and fixed with the non-through threaded hole 216 of the flat side 215 of the liquid nitrogen tank 210 through the bolt 616; the B face is parallel with the side wall of the hollow cylinder 610, the B face is provided with a through threaded hole 615, the through threaded hole 615 of the B face is connected and fixed with the threaded hole of the bottom of the liquid nitrogen tank 210 through the bolt 618; the copper bar 320 is suspended through the hollow cylinder 610 and is inserted from the through hole 214 of the flat side 215 of the liquid nitrogen tank 210.

[0060] In the practical application of the present application, the sample table can be refrigerated and heated.

[0061] Refrigeration operation: only the heating rod 140 and the second temperature sensor 130 (which can be a PT1000 temperature sensor) are connected on the temperature control module 400, and the connection between the first temperature sensor 120 (which can be a thermocouple temperature sensor) and the temperature control module 400 is disconnected. Open the large door of the scanning electron microscope, place the sample holder with the sample to be measured in the sample holder placement position 113 on the top surface of the sample table 110, close the electron microscope door, and vacuumize. After the vacuum degree of the electron microscope chamber reaches a certain value, fill the liquid nitrogen tank 210 with liquid nitrogen, and the low temperature (minus 196 degrees) of the liquid nitrogen is conducted to the sample table 110 (the low temperature of the sample table is the temperature of the sample to be measured) through the copper bar 320 and the copper wire rope 500. At this time, the temperature of the sample table 110 is displayed on the temperature control module 400. If the sample table 110 needs to reach a certain temperature, such as minus 120 degrees, minus 120 degrees can be set on the temperature control module 400. If the temperature of the sample table 110 is lower than the set minus 120 degrees after the command is issued, the heating rod 140 will heat the sample table 100, and when the sample table 110 reaches minus 120 degrees, the heating rod 140 will stop heating the sample table 110. In this way, the temperature of the sample table 110 is always maintained at the set minus 120 degrees.

[0062] Sample stage heating: only connect the heating rod 140 and the first temperature sensor 120 (which can be a thermocouple temperature sensor) on the temperature control module 400, disconnect the second temperature sensor 130 (which can be a PT1000 temperature sensor) from the temperature control module 400. Do not add liquid nitrogen to the liquid nitrogen tank 210, and the liquid nitrogen tank 210 is empty. Open the large door of the scanning electron microscope, place the sample stage 110 on the top surface of the sample stage 110, and close the electron microscope door. Vacuumize, and when the electron microscope chamber reaches a certain value, the sample stage 110 needs to reach a certain temperature, such as 600 degrees. Set 600 degrees on the temperature control module 400, and after the command is issued, the heating rod 140 in the sample stage 110 will heat the sample stage 110. When the temperature of the sample stage 110 reaches 600 degrees, the heating rod 140 will stop heating the sample stage 110. Subsequently, if the temperature of the sample stage 110 is lower than 600 degrees, the heating rod 140 will reheat the sample stage 110 until the temperature of the sample stage 110 reaches 600 degrees, and the heating rod 140 will stop heating the sample stage. This allows the temperature of the sample stage 110 to be maintained at a set temperature of 600 degrees.

[0063] It should be noted that the liquid nitrogen tank, the refrigeration / heating module, the support module, the flange module and other components can be made of common materials such as steel and copper, which are relatively low in cost. No special high-precision processing equipment is required, and the production is easy. No hardware and software upgrades are required for the scanning electron microscope except for the flange, and the use process is simple and convenient. It is widely applicable and can be matched with scanning electron microscopes of different manufacturers / models by only modifying the flange.

[0064] In the actual application process of the present application, the diameter of the liquid nitrogen tank can be 100-120mm or larger, and the height can be 160-200mm or larger. The diameter of the hollow cylinder of the support module can be 40-50mm or larger, and the length can be 60-80mm or larger. The diameter of the flange of the flange module can be 80-100mm or larger. When the sample stage is square, the side length of the square sample stage can be 20-50mm or larger, and the height can be 10-20mm or larger.

[0065] In the specific use of the present application, first, the cross support, flange plate (with aviation socket / plug, copper bar, O-shaped sealing washer) of the support module are fixed as a whole on the interface of the side of the electron microscope chamber with bolts, and the liquid nitrogen tank is fixed on the L-shaped support of the support module with bolts; then, 3 groups of wires with conversion heads at one end and aviation plugs at the other end are respectively inserted into the corresponding aviation sockets on the flange plate surface in the electron microscope chamber; 3 groups of wires with aviation sockets at one end are respectively inserted into the corresponding aviation plugs on the flange plate surface outside the electron microscope chamber, and the other end is connected to the corresponding joint of the temperature control module, after which the dovetail groove, square block plate, heat insulation ceramic plate and sample stage are fixed together, and the second temperature sensor (which can be a Pt1000 temperature sensor), the first temperature sensor (which can be a thermocouple temperature sensor) and the heating rod are respectively placed in and fixed in the 3 holes on one side of the sample stage, and the copper wire rope is fixed on the adjacent side of the side surface of the sample stage with bolts, thus completing the assembly of the refrigeration / heating module. Then open the large door of the electron microscope, fix the refrigeration / heating module on the sample base in the electron microscope chamber through the dovetail groove at the lower part of the refrigeration / heating module, then connect the conversion heads of the 3 groups of wires leading out from the Pt1000 temperature sensor, thermocouple temperature sensor and heating rod with the corresponding conversion heads of the 3 groups of wires leading out from the flange plate surface in the electron microscope chamber, fix the copper wire rope leading out from the adjacent side of the sample stage on the short copper bar on the flange plate surface in the electron microscope chamber, and then insert the nail table carrying the sample to be measured into the cylindrical hole on the top surface of the sample stage. Close the electron microscope chamber door and evacuate. Use the refrigeration mode of the refrigeration / heating module: only connect the heating rod and the Pt1000 temperature sensor on the temperature control module, and disconnect the thermocouple temperature sensor from the temperature control module. After the vacuum degree of the electron microscope chamber reaches a certain value, fill the liquid nitrogen tank with liquid nitrogen, and the low temperature of the liquid nitrogen is conducted to the sample stage, nail table and sample to be measured through the copper bar and copper wire rope. Set the temperature of the square sample stage (i.e. the temperature of the sample to be measured) on the temperature control module. Use the heating mode of the refrigeration / heating module: only connect the heating rod and the thermocouple temperature sensor on the temperature control module, and disconnect the Pt1000 temperature sensor from the temperature control module. Do not add liquid nitrogen to the liquid nitrogen tank, and the liquid nitrogen tank is empty. After the vacuum degree of the electron microscope chamber reaches a certain value, set the temperature of the square sample stage (i.e. the temperature of the sample to be measured) on the temperature control module.

[0066] From the above scheme, the application provides a sample temperature regulating device, which comprises a refrigeration / heating module, a liquid nitrogen tank module, a flange module and a temperature control module; a first temperature sensor, a second temperature sensor, a heating rod and a bolt connected with one end of a copper rod in the flange module through a copper wire rope are arranged on a sample stage in the refrigeration / heating module, the other end of the copper rod is inserted into the liquid nitrogen tank, different connection modes of the first temperature sensor, the second temperature sensor and the heating rod with the temperature control module are selected in different modes, and the temperature of the sample stage (i.e. the temperature of the sample to be measured) is set through the temperature control module. Thus, the temperature-sensitive sample can be effectively protected from the interference of high-energy electron beams, the temperature-sensitive sample can be analyzed by using a scanning electron microscope, and the influence of the change of temperature on the morphology and structure of the material can be studied.

[0067] Although the subject matter has been described in language specific to structural features and / or methodological acts, it is to be understood that the subject matter defined in the present application is not necessarily limited to the specific features or acts described above. Rather, the specific features and acts described above are merely exemplary forms of implementing the application.

[0068] Although several implementation details have been included in the above discussion, these should not be interpreted as limiting the scope of the application. Certain features described in the context of separate embodiments can also be implemented in combination with each other. Conversely, various features described in the context of a single embodiment can also be implemented separately or in any suitable sub-combination.

[0069] The above description is merely preferred embodiments of the application and a description of the principles of the technology used. Those skilled in the art should understand that the scope of the application involved in the application is not limited to the technical solutions formed by the specific combinations of the above technical features, and also covers other technical solutions formed by any combination of the above technical features or equivalent features without departing from the above application concept. For example, the above features are replaced with technical features with similar functions applied in the application (but not limited to) to form technical solutions.

Claims

1. A sample temperature control device, characterized in that, include: Cooling / heating module, liquid nitrogen tank module, flange module, and temperature control module; The cooling / heating module includes at least a sample stage, a first temperature sensor, a second temperature sensor, and a heating rod; the sample stage has three deep holes and one threaded hole on its side; the sample stage has a nail placement position on its top; the flange module includes at least a flange and a copper rod; the flange has at least three sets of aviation plugs and aviation sockets; the flange has a through hole; and the liquid nitrogen tank module includes at least a liquid nitrogen tank. The sample stage has a first temperature sensor, a second temperature sensor, and a heating rod respectively placed through three deep holes; the first temperature sensor, the second temperature sensor, and the heating rod are each led out with wires, and the other end of the wires has a first adapter; the threaded hole of the sample stage is used to place bolts; Three sets of wires are led out from three aviation sockets; each set of wires has an aviation plug at one end and a second adapter at the other end; the first adapter and the second adapter are connected respectively; the aviation plug of the wire is inserted into the aviation socket on the flange; the aviation plug on the flange is connected to the temperature control module; the copper rod is inserted into the through hole of the flange; one end of the copper rod is connected to the bolt on the sample stage by a copper wire rope; the other end of the copper rod extends into the liquid nitrogen tank in the liquid nitrogen tank module.

2. The sample temperature control device according to claim 1, characterized in that, The cooling / heating module also includes a block plate, a dovetail groove, and an insulation plate; The sample stage, insulation board, block plate, and dovetail groove are stacked in order from top to bottom and fixed together with fixing bolts; and the cooling / heating module is fixed to the sample base of the sample chamber of the electron microscope using the dovetail groove.

3. The sample temperature control device according to claim 1, characterized in that, The flange has a designated location for a sealing gasket.

4. The sample temperature control device according to claim 1, characterized in that, The liquid nitrogen tank has an opening at the top; the opening is fitted with a plug; the plug has a small hole; the liquid nitrogen tank has a through hole on the side, and the copper rod in the flange module is inserted through the through hole on the side of the liquid nitrogen tank.

5. The sample temperature control device according to claim 4, characterized in that, The flange is provided with a through threaded hole; the liquid nitrogen tank has a flat side surface, which is at a 90-degree angle to the bottom of the tank; the bottom of the liquid nitrogen tank is provided with a threaded hole; the liquid nitrogen tank module also includes a support module; the support module includes a hollow cylinder. One end of the hollow cylinder is provided with a cross bracket, which is at a 90-degree angle to the side wall of the hollow cylinder. The cross bracket has a through threaded hole. The support module and the flange are fixed to the interface on the side of the electron microscope chamber by bolts through the through threaded hole on the cross bracket, the through threaded hole on the flange, and the non-through threaded hole around the electron microscope interface. The other end of the hollow cylinder is provided with an L-shaped bracket, the A and B sides of the L-shaped bracket are at a 90-degree angle, wherein the A side of the L-shaped bracket is connected to one end of the hollow cylinder and is at a 90-degree angle to the side wall of the hollow cylinder, and the A side is provided with a through threaded hole, which is fixed to the flat side of the liquid nitrogen tank by bolts; the B side is parallel to the side wall of the hollow cylinder, and the B side is provided with a through threaded hole, which is fixed to the bottom of the liquid nitrogen tank by bolts; the copper rod is suspended through the hollow cylinder and inserted into the through hole on the flat side of the liquid nitrogen tank.

6. The sample temperature control device according to claim 1, characterized in that, The aviation socket on the flange is located inside the electron microscope chamber; the aviation plug on the flange is located outside the electron microscope chamber; wherein the aviation socket on the flange inside the electron microscope chamber and the aviation plug on the flange outside the electron microscope chamber are interconnected.

7. The sample temperature control device according to claim 1, characterized in that, The liquid nitrogen tank is a double-layered cylindrical shape.

8. The sample temperature control device according to claim 1, characterized in that, The first temperature sensor is a thermocouple temperature sensor.

9. The sample temperature control device according to claim 1, characterized in that, The second temperature sensor is a Pt1000 temperature sensor.

10. The sample temperature control device according to claim 2, characterized in that, The insulation board is an insulating ceramic board.

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