Sample rod mechanism, transmission electron microscope and in-situ heating test method of transmission electron microscope

Abstract

The invention relates to a sample rod mechanism, a transmission electron microscope and an in-situ heating test method of the transmission electron microscope. The sample rod mechanism comprises a rod body, a chip, a conductive bearing part and a power supply assembly, the chip is borne on the rod body, the chip comprises a substrate, a first electrode and a second electrode, and the first electrode and the second electrode are borne on the substrate and arranged at an interval; the conductive bearing part is detachably mounted on the chip, two opposite ends of the conductive bearing part are electrically connected with the first electrode and the second electrode respectively, and the conductive bearing part is used for bearing a sample to be detected; the power supply assembly is electrically connected with the first electrode and the second electrode and used for loading voltage to the first electrode and the second electrode.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of transmission electron microscopy, in particular to a sample rod mechanism, a transmission electron microscope and an in-situ heating test method of the transmission electron microscope. BACKGROUND

[0002] A transmission electron microscope (TEM) is a high-resolution microscope that uses a high-energy electron beam to penetrate a sample and form an image through the interaction of electrons and the sample to observe the microstructure of the sample. The in-situ heating sample rod is a sample rod mechanism integrated with a heating element, which is a core accessory of the transmission electron microscope. It can heat the sample from room temperature to hundreds or even thousands of degrees Celsius, and the temperature can be accurately controlled. It can capture dynamic information such as structure, morphology and phase transition of the sample under temperature change in real time.

[0003] A common in-situ heating sample rod uses a chemical deposition method to deposit a thin film electrode on a chip. The size of such an electrode is nanoscale, and its preparation process is complex and costly. In addition, during transportation and installation, the chip with a deposited thin film electrode is easily damaged, such as being accidentally poked by tweezers or falling to the ground, which increases maintenance costs. Furthermore, the thin film electrode and the chip are designed in one piece, so when the thin film electrode is damaged, it cannot be repaired independently. That is, when the thin film electrode is damaged, the chip is also damaged, which greatly increases the consumable cost of the in-situ heating sample rod. SUMMARY

[0004] In view of this, the present application provides a sample rod mechanism, a transmission electron microscope and an in-situ heating test method of the transmission electron microscope, which has low consumable and maintenance costs and good use performance.

[0005] The present application provides a sample rod mechanism, which comprises a rod body, a chip, a conductive carrier and a power supply assembly. The chip is carried on the rod body. The chip comprises a substrate, a first electrode and a second electrode. The first electrode and the second electrode are carried on the substrate and are spaced apart. The conductive carrier is detachably installed on the chip. The opposite ends of the conductive carrier are electrically connected to the first electrode and the second electrode, respectively, for carrying a sample to be detected. The power supply assembly is electrically connected to the first electrode and the second electrode, respectively, for loading a voltage on the first electrode and the second electrode.

[0006] Further, the first electrode and the second electrode are exposed to the substrate, the power supply assembly comprises a power supply, a first voltage conducting head and a second voltage conducting head, the power supply is electrically connected to the first voltage conducting head and the second voltage conducting head respectively, the first voltage conducting head abuts against the first electrode, and the second voltage conducting head abuts against the second electrode.

[0007] Further, the power supply assembly further comprises a variable resistor connected in series with the first voltage conducting head, and the variable resistor is used to adjust the current flowing through the conducting carrier.

[0008] Further, the chip further comprises a third electrode and a fourth electrode, the third electrode and the fourth electrode are carried on the substrate and located between the first electrode and the second electrode, the first electrode, the third electrode, the fourth electrode and the second electrode are arranged in a predetermined direction, the third electrode and the fourth electrode are electrically connected to opposite ends of the conducting carrier respectively, and the third electrode and the fourth electrode are exposed to the substrate; the power supply assembly further comprises a third voltage conducting head, a fourth voltage conducting head and a voltage meter, the voltage meter is electrically connected to the third voltage conducting head and the fourth voltage conducting head respectively, the third voltage conducting head abuts against the third electrode, the fourth voltage conducting head abuts against the fourth electrode, and the voltage meter is used to detect the voltage at the opposite ends of the conducting carrier.

[0009] Further, the sample rod mechanism further comprises a pressing block assembly, the pressing block assembly comprises a pressing block and a locking member, the pressing block is arranged on the side of the chip away from the rod body, the conducting carrier is clamped between the pressing block and the chip, and the locking member is sequentially arranged in the pressing block and the rod body to fix the relative position of the conducting carrier and the chip.

[0010] Further, the rod body has a first window penetrating through two surfaces of the rod body in the thickness direction, the chip has a second window penetrating through two surfaces of the substrate in the thickness direction, the first window and the second window are communicated, at least part of the conducting carrier is arranged corresponding to the first window and the second window, the first electrode and the third electrode are located on the same side of the first window and the second window, and the second electrode and the fourth electrode are located on the other side of the first window and the second window.

[0011] Further, the pressing block comprises a body part, a first pressing part and a second pressing part, the first pressing part and the second pressing part are located at the same side of the body part and are arranged at intervals, along the preset direction, the first pressing part and the second pressing part are located at opposite sides of the first window respectively, the first pressing part and the second pressing part are used for pressing opposite ends of the conductive carrier respectively, the thickness of the first pressing part is less than the thickness of the body part, and the thickness of the second pressing part is less than the thickness of the body part.

[0012] Further, the conductive carrier is a tungsten wire, the conductive carrier is cylindrical, and the diameter of the conductive carrier is less than or equal to 50 μm.

[0013] The application provides a transmission electron microscope, which comprises a shell, a sample rod mechanism and a test assembly, the shell has a sample cavity, at least part of the rod body, the chip, the conductive carrier and at least part of the power supply assembly are located in the sample cavity, the test assembly comprises a tester and a receiver, the tester and the receiver are arranged in the sample cavity, along the height direction of the transmission electron microscope, the tester and the receiver are arranged at opposite sides of the rod body respectively, the tester is used for emitting an electron beam, and the receiver is used for receiving and storing detection information of a sample to be detected.

[0014] The application also provides an in-situ heating test method of a transmission electron microscope, which is applied to the transmission electron microscope provided by the application, and the test method comprises the following steps: providing a sample rod mechanism, the sample rod mechanism comprises a rod body, a chip, a conductive carrier and a power supply assembly, the chip is carried on the rod body, the chip comprises a substrate, a first electrode and a second electrode, the first electrode and the second electrode are carried on the substrate and are arranged at intervals; the conductive carrier is detachably installed on the chip, opposite ends of the conductive carrier are electrically connected to the first electrode and the second electrode respectively; the power supply assembly is electrically connected to the first electrode and the second electrode respectively and is used for loading a voltage on the first electrode and the second electrode; the power supply assembly comprises a variable resistor, and the variable resistor is connected in series with the conductive carrier; a sample to be detected is arranged on the conductive carrier; the transmission electron microscope is started to load a first preset voltage on the first electrode and the second electrode; the variable resistor is adjusted so that the voltage applied to the opposite ends of the conductive carrier is a second preset voltage, so as to adjust the temperature of the conductive carrier, wherein the second preset voltage is less than the first preset voltage; and the sample to be detected is detected by the test assembly.

[0015] Further, the loading of the first preset voltage on the first electrode and the second electrode comprises that the power supply assembly comprises a power supply, a first conductive voltage head and a second conductive voltage head, the power supply, the variable resistor, the first conductive voltage head, the first electrode, the conductive carrier, the second electrode and the second conductive voltage head form a first electric connection loop, the power supply is turned on to load the first preset voltage on the first electrode and the second electrode.

[0016] Further, the adjusting of the variable resistor to make the voltage applied on the opposite ends of the conductive carrier be a second preset voltage to adjust the temperature of the conductive carrier comprises that the power supply assembly comprises an ammeter, the ammeter is in series with the conductive carrier in the first electric connection loop and is used to detect the current flowing through the conductive carrier; the variable resistor is adjusted to change the current flowing through the conductive carrier and the voltage applied on the opposite ends of the conductive carrier; the power supply assembly comprises a third conductive voltage head, a fourth conductive voltage head and a voltage meter which are electrically connected in sequence, the third conductive voltage head, the voltage meter, the fourth conductive voltage head and the conductive carrier form a second electric connection loop, the voltage meter is used to detect the voltage applied on the opposite ends of the conductive carrier to make the voltage applied on the opposite ends of the conductive carrier be the second preset voltage; the resistance of the conductive carrier is obtained according to the current information detected by the ammeter and the voltage information detected by the voltage meter, and the temperature of the conductive carrier is obtained according to the preset relationship between the resistance and the temperature.

[0017] In the present application, the chip serves as a fixed carrier and an electrical adapter, the power supply component forms an electrical connection loop with the conductive carrier through the chip, so that the power supply component can supply power to the conductive carrier, and the conductive carrier generates heat to heat the sample to be detected carried on the conductive carrier. Specifically, the power supply component is electrically connected to the chip and supplies power to the chip, the conductive carrier is electrically connected to the chip and supplies power to the conductive carrier, the power supply component, the first electrode, the conductive carrier, the second electrode form a first electrical connection loop, when the power supply component is turned on and current passes through the conductive carrier, the conductive carrier generates heat and the temperature rises to heat the sample to be detected arranged on the conductive carrier. In addition, by adjusting the power supply component, the current flowing through the conductive carrier is adjusted, so as to change the temperature of the conductive carrier and change the test temperature of the sample to be detected. In other words, when the sample rod mechanism is arranged on the transmission electron microscope, the test temperature of the conductive carrier and the sample to be detected attached to the conductive carrier can be adjusted in real time by adjusting the current flowing through the conductive carrier in real time, so as to detect the dynamic information such as structure and phase transition of the sample to be detected at different temperatures, the sample rod mechanism can detect the sample to be detected in situ, and has good detection performance. Further, the conductive carrier can be detachably installed on the chip, after a period of use, if the conductive carrier is fatigued and aged, or damaged due to too high temperature, the conductive carrier can be directly replaced, and the chip can still be normally used. Compared with the scheme of depositing a thin film electrode on the chip, the conductive carrier and the chip are not integrated in the present application, the conductive carrier and the chip are easy to separate and electrically connect, when the conductive carrier is damaged, the chip with high precision design and high price can be repeatedly used, only the conductive carrier needs to be replaced and repaired, which greatly reduces the consumable cost and maintenance cost of the sample rod mechanism, and improves the use performance of the sample rod mechanism. Furthermore, compared with the scheme of depositing a thin film electrode on the chip, the size of the conductive carrier in the present application is micron level, and the conductive carrier is directly connected to the first electrode and the second electrode, which can reduce the precision micro-nano processing link, reduce the complexity of the sample rod mechanism, and enable the sample rod mechanism to be equipped with different specifications of conductive carriers, that is, the sample rod mechanism can be equipped with conductive carriers with different materials or diameters to meet the heating needs of the sample to be detected in different temperature ranges, and improve the use performance of the sample rod mechanism. BRIEF DESCRIPTION OF DRAWINGS

[0018] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments will be briefly introduced as follows. Obviously, the drawings described in the following embodiments are some of the drawings of the present application, and other drawings can also be obtained by those skilled in the art without any creative effort on the basis of these drawings.

[0019] Figure 1 A structural schematic diagram of a sample rod mechanism of an embodiment of the present application is shown in FIG. 1. Figure 2 A partial exploded structural schematic diagram of a sample rod mechanism of an embodiment of the present application is shown in FIG. 2. Figure 3 A top view structural schematic diagram of a sample rod mechanism of an embodiment of the present application is shown in FIG. 3. Figure 4 A structural schematic diagram of a transmission electron microscope of an embodiment of the present application is shown in FIG. 4. Figure 3 An enlarged view of the A dashed box in FIG. 4 is shown in FIG. 5. Figure 5 An electrical connection relationship schematic diagram of a sample rod mechanism of an embodiment of the present application is shown in FIG. 6. Figure 6 A structural schematic diagram of a transmission electron microscope of an embodiment of the present application is shown in FIG. 4. Figure 7 A partial structural schematic diagram of a sample rod mechanism of an embodiment of the present application is shown in FIG. 7. Figure 8 A structural schematic diagram of a pressing block of an embodiment of the present application is shown in FIG. 8. Figure 9 A flowchart of a test method of an embodiment of the present application is shown in FIG. 9. Figure 10 A flowchart of a test method of another embodiment of the present application is shown in FIG. 10.

[0020] Explanation of reference signs: 100 - sample rod mechanism, 110 - rod body, 111 - first window, 120 - chip, 121 - substrate, 122 - first electrode, 123 - second electrode, 124 - third electrode, 125 - fourth electrode, 126 - second window, 130 - conductive carrier, 131 - first conductive part, 132 - heating part, 133 - second conductive part, 140 - power supply assembly, 141 - power supply, 142 - first conductive pressure head, 143 - second conductive pressure head, 144 - variable resistor, 145 - third conductive pressure head, 146 - fourth conductive pressure head, 147 - voltmeter, 148 - connector, 149 - ammeter, 150 - pressing block assembly, 151 - pressing block, 1511 - body part, 1512 - first pressing part, 1513 - second pressing part, 152 - locking part, 200 - transmission electron microscope, 210 - shell, 211 - sample cavity, 220 - test assembly, 221 - tester, 222 - receiver, 230 - objective lens, 240 - collector. DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the scope of protection of the present application.

[0022] The terms "first", "second", and the like in the specification of the present application and the above-described drawings are used to distinguish different objects, rather than to describe a particular order. In addition, the terms "include" and "have" and any variations thereof are intended to cover non-exclusive inclusion. For example, a process, method, system, product, or device that includes a series of steps or units is not limited to the listed steps or units, but can optionally include steps or units not listed, or can optionally include other steps or units inherent to the process, method, product, or device.

[0023] Reference herein to "an embodiment" or "the embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment or embodiments can be included in at least one embodiment of the present application. The appearance of the phrase in various places in the specification does not necessarily all refer to the same embodiment, or necessarily alternatives to other embodiments. It will be explicitly understood by a person of ordinary skill in the art that the embodiments described herein can be combined with other embodiments.

[0024] A transmission electron microscope (TEM) is a high-resolution microscope that uses a high-energy electron beam to penetrate a sample and forms an image through the interaction of electrons and the sample to observe the microstructure of the sample. The basic principle is that when the electron beam penetrates the sample, different degrees of scattering will occur due to the difference in atomic density of different regions of the sample, and the transmitted electrons form a difference in strength, which is finally converted into a visible image on a fluorescent screen or a detector. The in-situ heating sample rod is a sample rod mechanism integrated with a heating element, which is the core accessory of the transmission electron microscope. It can heat the sample from room temperature to hundreds or even thousands of degrees Celsius, and the temperature can be accurately controlled, and can capture real-time dynamic information such as structure, morphology, and phase transition of the sample under temperature change.

[0025] The common in-situ heating sample rod deposits a thin film electrode on the chip by using a chemical deposition method, and the size of the electrode is nanoscale. The preparation process is complex, and the preparation cost is high. In addition, during transportation and installation, the chip with deposited thin film electrode is easy to be damaged, such as accidentally poked by tweezers, dropped on the ground, etc., and the maintenance cost is high. Furthermore, the thin film electrode is designed in one piece with the chip, and when the thin film electrode is damaged, the thin film electrode cannot be repaired independently, that is, when the thin film electrode is damaged, the chip is also damaged, which greatly increases the consumable cost of the in-situ heating sample rod.

[0026] Please see Figures 1 to 10 The application provides a sample rod mechanism 100, which comprises a rod body 110, a chip 120, a conductive carrier 130 and a power supply assembly 140. The chip 120 is carried on the rod body 110, and comprises a substrate 121, a first electrode 122 and a second electrode 123. The first electrode 122 and the second electrode 123 are carried on the substrate 121 and are arranged in a spaced manner. The conductive carrier 130 is detachably installed on the chip 120, and the opposite ends of the conductive carrier 130 are electrically connected to the first electrode 122 and the second electrode 123, respectively, for carrying a sample to be detected. The power supply assembly 140 is electrically connected to the first electrode 122 and the second electrode 123, respectively, for loading a voltage on the first electrode 122 and the second electrode 123.

[0027] Understandably, the sample rod mechanism 100 is applied to a transmission electron microscope 200, i.e. a transmission electron microscope. The transmission electron microscope 200 comprises a housing 210 having a sample cavity 211. The sample rod mechanism 100 is used for carrying a sample to be detected, and the sample rod mechanism 100 is at least partially arranged in the sample cavity 211, so as to realize detection of the sample to be detected in the sample cavity 211.

[0028] Understandably, the rod body 110, the chip 120 and the conductive carrier 130 are arranged in sequence.

[0029] Optionally, in some embodiments, the conductive carrier 130 is a metal wire.

[0030] Optionally, in some embodiments, the first electrode 122 is a positive electrode, and the second electrode 123 is a negative electrode. In other embodiments, the first electrode 122 is a negative electrode, and the second electrode 123 is a positive electrode.

[0031] It can be understood that the conductive carrier 130 is detachably installed on the chip 120, so that the conductive carrier 130 and the chip 120 can be repeatedly disassembled and assembled, or the conductive carrier 130 is replaceable, facilitating detachable connection of the chip 120 and the conductive carrier 130.

[0032] In the embodiment, the chip 120 serves as a fixed carrier and an electrical adapter, and the power supply assembly 140 forms an electrical connection loop with the conductive carrier 130 through the chip 120, so that the power supply assembly 140 can supply power to the conductive carrier 130, and the conductive carrier 130 generates heat to heat the sample to be detected carried on the conductive carrier 130. Specifically, the power supply assembly 140 is electrically connected to and supplies power to the chip 120, the conductive carrier 130 is electrically connected to and supplies power to the chip 120, the power supply assembly 140, the first electrode 122, the conductive carrier 130, the second electrode 123 form a first electrical connection loop, when the power supply assembly 140 is turned on and current flows through the conductive carrier 130, the conductive carrier 130 generates heat and the temperature rises to heat the sample to be detected arranged on the conductive carrier 130. In addition, by adjusting the power supply assembly 140, the current flowing through the conductive carrier 130 is adjusted, so that the temperature of the conductive carrier 130 is changed to change the test temperature of the sample to be detected. In other words, when the sample rod mechanism 100 is arranged on the transmission electron microscope 200, the current flowing through the conductive carrier 130 can be adjusted in real time to adjust the test temperature of the conductive carrier 130 and the sample to be detected attached to the conductive carrier 130 in real time, so that the structural and phase transition dynamic information of the sample to be detected at different temperatures is detected, the sample rod mechanism 100 can detect the sample to be detected in situ, and has good detection performance. Further, the conductive carrier 130 can be detachably installed on the chip 120, after a period of use, if the conductive carrier 130 is fatigued and aged, or damaged due to excessive temperature, the conductive carrier 130 can be directly replaced, and the chip 120 can still be normally used. Compared with the scheme of depositing a thin film electrode on the chip 120, the conductive carrier 130 and the chip 120 are not integrated, the conductive carrier 130 and the chip 120 are easy to separate and electrically connect, when the conductive carrier 130 is damaged, the chip 120 with high precision design and high price can be repeatedly used, only the conductive carrier 130 needs to be replaced and repaired, which greatly reduces the consumable cost and maintenance cost of the sample rod mechanism 100, and improves the use performance of the sample rod mechanism 100.Furthermore, compared with the scheme of depositing thin film electrodes on the chip 120, the size of the conductive carrier 130 of the present application is micron level, and the conductive carrier 130 is directly connected to the first electrode 122 and the second electrode 123, which can reduce the precise micro-nano processing link, reduce the complexity of the sample rod mechanism 100, and make the sample rod mechanism 100 can be equipped with different specifications of the conductive carrier 130, that is, the sample rod mechanism 100 can be equipped with conductive carriers 130 of different materials or diameters to meet the heating needs of different temperature ranges of the samples to be detected, and improve the use performance of the sample rod mechanism 100.

[0033] In some embodiments, the first electrode 122 and the second electrode 123 are both exposed to the substrate 121, the power supply assembly 140 includes a power supply 141, a first conductive pressure head 142 and a second conductive pressure head 143, the power supply 141 is electrically connected to the first conductive pressure head 142 and the second conductive pressure head 143 respectively, the first conductive pressure head 142 abuts the first electrode 122, and the second conductive pressure head 143 abuts the second electrode 123.

[0034] It can be understood that the power supply 141, the first conductive pressure head 142, the first electrode 122, the conductive carrier 130, the second electrode 123, and the second conductive pressure head 143 are sequentially electrically connected and form a first electrical connection loop.

[0035] In the embodiment, the chip 120 has the first electrode 122 and the second electrode 123 arranged at intervals, and the first electrode 122 and the second electrode 123 provide fixed positions for the connection of the conductive carrier 130 and the first conductive voltage head 142 and the second conductive voltage head 143, so that the power supply 141 can supply power to the conductive carrier 130 through the first conductive voltage head 142, the second conductive voltage head 143 and the chip 120. Specifically, one of the positive terminal or the negative terminal of the power supply 141, the first conductive voltage head 142, the first electrode 122 of the chip 120, the conductive carrier 130, the second electrode 123 of the chip 120, the second conductive voltage head 143 and the other of the positive terminal or the negative terminal of the power supply 141 are sequentially electrically connected and form a first electrical connection loop, when the current flows through the conductive carrier 130, the conductive carrier 130 generates heat and realizes heating of the sample to be detected. In the embodiment, the first conductive voltage head 142 is electrically connected to one of the positive terminal or the negative terminal of the power supply 141 and the first electrode 122 respectively, and the second conductive voltage head 143 is electrically connected to the other of the positive terminal or the negative terminal of the power supply 141 and the second electrode 123 respectively, which enhances the electrical connection stability of the first electrical connection loop, reduces the contact resistance, ensures the stability of the heating current in the conductive carrier 130, and further improves the stability of the control of the heating temperature of the sample to be detected, and further improves the use performance of the sample rod mechanism 100. In addition, the first electrode 122 and the second electrode 123 are exposed to the substrate 121, the first conductive voltage head 142 abuts against the first electrode 122, and the second conductive voltage head 143 abuts against the second electrode 123, and the power supply assembly 140 and the chip 120 are electrically connected in a simple and efficient manner, and the sample rod mechanism 100 has good assembly performance.

[0036] In some embodiments, the power supply assembly 140 further comprises a variable resistor 144 connected in series with the first conductive voltage head 142, and the variable resistor 144 is used to adjust the current flowing through the conductive carrier 130.

[0037] It can be understood that the variable resistor 144 is in the first electrical connection loop, and when the voltage of the power supply 141 is constant, the current of the first electrical connection loop can be adjusted by adjusting the variable resistor 144, so as to adjust the current flowing through the conductive carrier 130.

[0038] It can be understood that the variable resistor 144 is also connected in series with the second conductive voltage head 143 and the conductive carrier 130.

[0039] In the embodiment, the rheostat 144 is connected in series with the first conductive voltage head 142, and the rheostat 144 is in the first electric connection loop. When the rheostat 144 is adjusted, the current in the first electric connection loop can be adjusted, and thus the current of the conductive carrier 130 can be adjusted. According to Joule's law, the heat generated by the conductive carrier 130 is proportional to the square of the current. When the current flowing through the conductive carrier 130 increases, the heat generated by the conductive carrier 130 increases, the temperature of the conductive carrier 130 increases, and thus the sample carried by the conductive carrier 130 can be heated. Conversely, when the current flowing through the conductive carrier 130 decreases, the heat generated by the conductive carrier 130 decreases, the temperature of the conductive carrier 130 decreases, and thus the sample carried by the conductive carrier 130 can be cooled. In the embodiment, on the one hand, by arranging the rheostat 144 in the first electric connection loop, the heat generated by the conductive carrier 130 can be accurately controlled, the sample can be continuously and stably adjusted in a preset temperature range, the fine requirement of the sample for a “specific temperature point” or a “temperature gradient change” can be met, and the detection performance of the sample rod mechanism 100 can be improved. On the other hand, the rheostat 144 can flexibly expand the current adjustment range in the first electric connection loop, so that the sample rod mechanism 100 can be selected with different specifications of the conductive carrier 130, such as a metal wire with different materials and different diameters, and the universal performance of the sample rod mechanism 100 can be improved.

[0040] Optionally, in some embodiments, the power supply assembly 140 further comprises a current meter 149 connected in series with the conductive carrier 130, and the current meter 149 is configured to detect the current flowing through the conductive carrier 130.

[0041] It can be understood that the current meter 149 is in the first electric connection loop.

[0042] In the embodiment, the voltage of the power supply is constant, and the current flowing through the conductive carrier 130 can be adjusted by adjusting the rheostat 144. The current meter 149 can detect the current information of the conductive carrier 130 in real time, so as to facilitate the user to monitor the heating condition of the conductive carrier 130, and improve the use performance of the sample rod mechanism 100.

[0043] In some embodiments, the chip 120 further includes a third electrode 124 and a fourth electrode 125, both of which are supported on the substrate 121 and located between the first electrode 122 and the second electrode 123. The first electrode 122, the third electrode 124, the fourth electrode 125, and the second electrode 123 are aligned along a predetermined direction (e.g., ...). Figure 4 (As shown in the X direction) The third electrode 124 and the fourth electrode 125 are arranged at intervals and are electrically connected to the opposite ends of the conductive carrier 130, respectively. Both the third electrode 124 and the fourth electrode 125 are exposed on the substrate 121. The power supply assembly 140 also includes a third voltage conduction head 145, a fourth voltage conduction head 146 and a voltmeter 147. The voltmeter 147 is electrically connected to the third voltage conduction head 145 and the fourth voltage conduction head 146, respectively. The third voltage conduction head 145 abuts against the third electrode 124, and the fourth voltage conduction head 146 abuts against the fourth electrode 125. The voltmeter 147 is used to detect the voltage at the opposite ends of the conductive carrier 130.

[0044] Understandably, in some embodiments, the conductive carrier 130 extends along the preset direction.

[0045] Understandably, the portion of the conductive carrier 130 located between the third electrode 124 and the fourth electrode 125 is used to hold the sample to be tested.

[0046] Understandably, the third voltage connector 145, the voltmeter 147, the fourth voltage connector 146, and the conductive carrier 130 form a second electrical connection circuit.

[0047] Optionally, in some embodiments, the third electrode 124 is a positive electrode and the fourth electrode 125 is a negative electrode; in other embodiments, the third electrode 124 is a negative electrode and the fourth electrode 125 is a positive electrode.

[0048] In the embodiment, the first electrode 122, the third electrode 124, the fourth electrode 125 and the second electrode 123 are arranged at intervals along the preset direction, the first electrode 122 and the third electrode 124 are electrically connected to one end of the conductive carrier 130, the second electrode 123 and the fourth electrode 125 are electrically connected to the other end of the conductive carrier 130, and the part of the conductive carrier 130 between the third electrode 124 and the fourth electrode 125 is used for arranging the sample to be detected. The third conductive voltage head 145, the voltage meter 147, the fourth conductive voltage head 146 and the conductive carrier 130 form a second electrical connection loop, the voltage on the opposite ends of the conductive carrier 130 is detected by arranging the voltage meter 147, and the current flowing through the conductive carrier 130 is detected by arranging the ammeter 149 in the first electrical connection loop, so that the resistance of the conductive carrier 130 can be calculated in real time. Since the resistance changes with temperature, for example, the resistance of the metal wire has a positive temperature coefficient, the voltage information detected by the voltage meter 147 can indirectly reflect the actual temperature of the conductive carrier 130, which provides a quantitative basis for realizing accurate temperature control of the conductive carrier 130, avoids the error of inferring temperature only by current, and improves the detection accuracy of the sample rod mechanism 100 for the sample to be detected. In addition, the third electrode 124 and the fourth electrode 125 are located between the first electrode 122 and the second electrode 123, that is, the voltage information detected by the conductive carrier 130 can effectively eliminate the resistance error of the connection part, and more accurately reflect the voltage on the opposite ends of the conductive carrier 130. The sample rod mechanism 100 provided by the embodiment has higher test accuracy.

[0049] It can be understood that the two-electrode method for measuring the electrical properties of materials cannot avoid the error caused by polarization effect. The sample rod mechanism 100 of the embodiment adopts the four-electrode method, which can measure the voltage on the opposite ends of the conductive carrier 130 in real time while realizing power supply to the conductive carrier 130, and avoids polarization effect, thereby ensuring the accuracy of the obtained data.

[0050] Optionally, the conductive carrier 130 comprises a first conductive part 131, a heating part 132 and a second conductive part 133 connected along the preset direction, the heating part 132 is used for carrying the sample to be detected; the first conductive part 131 is electrically connected to the first electrode 122 and the third electrode 124 respectively, and the second conductive part 133 is electrically connected to the fourth electrode 125 and the second electrode 123 respectively.

[0051] It can be understood that the power supply 141, the first conductive voltage head 142, the first electrode 122, the first conductive part 131, the heating part 132, the second conductive part 133, the second electrode 123 and the second conductive voltage head 143 are sequentially electrically connected and form a first electric connection loop.

[0052] It can be understood that the first conductive part 131, the third conductive voltage head 145, the voltage meter 147, the fourth conductive voltage head 146, the second conductive part 133 and the heating part 132 form a second electric connection loop.

[0053] In some embodiments, the sample rod mechanism 100 further comprises a pressing block assembly 150, the pressing block assembly 150 comprising a pressing block 151 and a locking member 152, the pressing block 151 being arranged on a side of the chip 120 away from the rod body 110, the conductive carrier 130 being clamped between the pressing block 151 and the chip 120, and the locking member 152 being sequentially arranged through the pressing block 151 and the rod body 110 to fix the relative position of the conductive carrier 130 and the chip 120.

[0054] It can be understood that the rod body 110, the chip 120, the conductive carrier 130 and the pressing block 151 are sequentially arranged.

[0055] It can be understood that the first conductive part 131 is clamped between the pressing block 151 and the chip 120, and the second conductive part 133 is clamped between the pressing block 151 and the chip 120.

[0056] In the embodiment, the pressing block 151 is arranged on the side of the chip 120 away from the rod body 110, and the conductive carrier 130 is arranged between the pressing block 151 and the chip 120, so that one end of the conductive carrier 130 is always in contact with the first electrode 122 and the third electrode 124, and the other end of the conductive carrier 130 is always in contact with the second electrode 123 and the fourth electrode 125, thereby ensuring reliable electrical connection between the conductive carrier 130 and the chip 120, and finally enabling the power supply assembly 140 to provide stable power supply for the conductive carrier 130 through the chip 120. In addition, the locking member 152 is arranged in the pressing block 151 and the rod body 110 in sequence, and the relative positions of the conductive carrier 130 and the chip 120 are fixed, and the relative positions of the conductive carrier 130 and the rod body 110 are fixed, so that the conductive carrier 130 can be stably arranged on the rod body 110. When the conductive carrier 130 is used to carry the sample to be detected, the sample to be detected can be stably arranged on the rod body 110, so as to improve the stability of detecting the sample to be detected.

[0057] Optionally, the pressing block 151 is a ceramic block, so as to realize the insulation of the pressing block 151, the chip 120 and the conductive carrier 130.

[0058] Please refer to Figure 7 In some embodiments, the rod body 110 has a first window 111 penetrating through two opposite surfaces of the rod body 110 along the thickness direction thereof; the chip 120 has a second window 126 penetrating through two opposite surfaces of the substrate 121 along the thickness direction thereof, the first window 111 and the second window 126 are communicated; at least part of the conductive carrier 130 is arranged corresponding to the first window 111 and the second window 126, the first electrode 122 and the third electrode 124 are located on the same side of the first window 111 and the second window 126, and the second electrode 123 and the fourth electrode 125 are located on the other side of the first window 111 and the second window 126.

[0059] It can be understood that the second window 126 penetrates through two opposite surfaces of the substrate 121 along the thickness direction thereof; It can be understood that when the sample rod mechanism 100 is applied to the transmission electron microscope 200, the transmission electron microscope 200 further comprises a test assembly 220, the test assembly 220 comprises a tester 221 and a receiver 222, the tester 221 and the receiver 222 are both arranged in the sample cavity 211, and the tester 221 and the receiver 222 are arranged on opposite sides of the rod body 110 along the height direction of the transmission electron microscope 200, the tester 221 is used for emitting an electron beam, and the receiver 222 is used for receiving and storing detection information of a sample to be detected.

[0060] It can be understood that the tester 221 is in orthographic projection on the first window 111 and the second window 126 along the height direction of the transmission electron microscope 200, and the receiver 222 is in orthographic projection on the first window 111 and the second window 126.

[0061] It can be understood that the first conductive part 131 and the second conductive part 133 are respectively located on opposite sides of the first window 111 along a preset direction, and the orthographic projection of the heating part 132 falls within the range of the first window 111, that is, the heating part 132 is arranged corresponding to the first window 111; similarly, the first conductive part 131 and the second conductive part 133 are respectively located on opposite sides of the second window 126, and the orthographic projection of the heating part 132 falls within the range of the second window 126, that is, the heating part 132 is arranged corresponding to the second window 126.

[0062] In the embodiment, the first window 111 and the second window 126 are communicated to form a through channel, so that at least part of the conductive carrier 130 can be arranged corresponding to the first window 111 and the second window 126, to ensure that the electron beam emitted by the tester 221 can directly act on the sample to be detected carried on the conductive carrier 130, and then penetrate the first window 111 and the second window 126, so that the receiver 222 can receive and store the detection information of the sample to be detected, avoiding the entity structure of the chip 120 or the rod body 110 shielding the electron beam, meeting the core imaging requirement of the transmission electron microscope that the electron beam penetrates the sample to be detected, and ensuring the clarity of detecting the sample to be detected.

[0063] Please refer to Figure 8In some embodiments, the pressing block 151 comprises a body portion 1511, a first pressing portion 1512 and a second pressing portion 1513, the first pressing portion 1512 and the second pressing portion 1513 are located at the same side of the body portion 1511 and are spaced apart, the first pressing portion 1512 and the second pressing portion 1513 are respectively located at opposite sides of the first window 111 along the preset direction, the first pressing portion 1512 and the second pressing portion 1513 are respectively used for pressing opposite ends of the conductive carrier 130, the thickness of the first pressing portion 1512 is less than the thickness of the body portion 1511, and the thickness of the second pressing portion 1513 is less than the thickness of the body portion 1511.

[0064] Understandably, the first pressing portion 1512, the body portion 1511 and the second pressing portion 1513 are in a "U" shape structure.

[0065] Understandably, the first conductive portion 131 is clamped between the first pressing portion 1512 and the chip 120, and the second conductive portion 133 is clamped between the second pressing portion 1513 and the chip 120.

[0066] Understandably, the first pressing portion 1512 is offset from the first window 111 and the second window 126 on the bar body 110, and the second pressing portion 1513 is offset from the first window 111 and the second window 126 on the bar body 110.

[0067] Understandably, when the electron beam irradiates the sample to be detected carried on the conductive carrier 130, the sample to be detected will be excited to generate X-rays, and the transmission electron microscope 200 further comprises a collector 240, the collector 240 is arranged in the sample cavity 211, the collector 240 receives X-ray signals to obtain the element composition of the sample to be detected. Wherein, the X-ray is the carrier of the energy spectrum signal, which can reflect the element composition of the sample.

[0068] In the embodiment, when the sample rod mechanism 100 is applied to the transmission electron microscope 200, the first pressing part 1512 and the second pressing part 1513 are respectively used for pressing opposite ends of the conductive carrier 130, and the part of the conductive carrier 130 between the first pressing part 1512 and the second pressing part 1513 is used for carrying the sample to be detected. When the electron beam emitted by the tester 221 acts on the sample to be detected, the sample to be detected will generate X-rays emitted in all directions of 360°. The thickness of the first pressing part 1512 is less than the thickness of the body part 1511, and the thickness of the second pressing part 1513 is less than the thickness of the body part 1511, which can avoid the first pressing part 1512 and the second pressing part 1513 shielding the emission of the X-rays, so that the collector 240 can collect enough X-rays, and finally make the energy spectrum analysis structure more accurate and sensitive, and improve the detection performance of the sample rod mechanism 100 applied to the transmission electron microscope 200.

[0069] In some embodiments, the conductive carrier 130 is a tungsten wire, the conductive carrier 130 is cylindrical, and the diameter of the conductive carrier 130 is less than or equal to 50 μm.

[0070] Specifically, the diameter of the conductive carrier 130 can be, but is not limited to, 5 μm, 8 μm, 10 μm, 12 μm, 15 μm, 16 μm, 18 μm, 20 μm, 22 μm, 24 μm, 26 μm, 28 μm, 30 μm, 32 μm, 35 μm, 38 μm, 40 μm, 42 μm, 45 μm, 48 μm, 50 μm, etc.

[0071] In the embodiment, the conductive carrier 130 is tungsten wire, the heat production of the conductive carrier 130 is proportional to the square of the current flowing through the conductive carrier 130, and the resistance of the conductive carrier 130 has a positive temperature coefficient. By adjusting the current flowing through the conductive carrier 130, the temperature of the conductive carrier 130 can be changed, and the resistance of the conductive carrier 130 can be changed through the positive temperature coefficient characteristic, so as to adjust the conductive carrier 130 to different temperatures, so as to detect the sample to be detected at different temperatures. Further, the diameter of the conductive carrier 130 is less than or equal to 50 μm. When the diameter of the conductive carrier 130 is within a reasonable range, the temperature rising and falling speed of the conductive carrier 130 is within a reasonable range when the current flowing through the conductive carrier 130 changes, so as to facilitate the detection of the performance of the sample to be detected with temperature change, so as to realize in-situ heating detection of the sample to be detected. When the diameter of the conductive carrier 130 is too large, on the one hand, the temperature rising and falling speed of the conductive carrier 130 is too slow, which reduces the detection efficiency of the sample to be detected; on the other hand, as the diameter of the conductive carrier 130 increases, when the temperature of the conductive carrier 130 rises, the conductive carrier 130 expands due to thermal expansion and contraction, and the conductive carrier 130 is prone to thermal drift, so as to drive the sample to be detected carried on the conductive carrier 130 to move, causing the sample to be detected to shake during detection, and reducing the accuracy of detection of the sample to be detected. Furthermore, if the diameter of the conductive carrier 130 is too large, correspondingly, the volume is larger, the heat radiation generated after the temperature rises is too large, which may damage other components in the sample chamber 211 such as the tester 221, the receiver 222, the collector 240, etc., and shorten the service life of the transmission electron microscope 200.

[0072] Optionally, the power supply assembly 140 further comprises a connector 148 located at the end of the rod body 110 away from the chip 120 and a power wire (not shown in the figure) located in the rod body 110. The number of the power wire is four, and each power wire is electrically connected to the chip 120 and the connector 148 respectively. The connector 148 is used to be electrically connected to the power supply 141, the variable resistor 144, the voltmeter 147, etc.

[0073] It can be understood that the opposite ends of the first power supply wire are electrically connected to the first electrode 122 and the connector 148 respectively, the opposite ends of the second power supply wire are electrically connected to the second electrode 123 and the connector 148 respectively, the opposite ends of the third power supply wire are electrically connected to the third electrode 124 and the connector 148 respectively, and the opposite ends of the fourth power supply wire are electrically connected to the fourth electrode 125 and the connector 148 respectively.

[0074] Optionally, in some embodiments, the connector 148 is an aviation plug, facilitating electrical connection between the chip 120 and other parts.

[0075] Optionally, in some embodiments, the connector 148 is an aviation plug, facilitating electrical connection between the chip 120 and other parts. Figures 1 to 8 Optionally, in some embodiments, the connector 148 is an aviation plug, facilitating electrical connection between the chip 120 and other parts.

[0076] Optionally, in some embodiments, the connector 148 is an aviation plug, facilitating electrical connection between the chip 120 and other parts.

[0077] Optionally, in some embodiments, the connector 148 is an aviation plug, facilitating electrical connection between the chip 120 and other parts.

[0078] In the transmission electron microscope 200 provided in the embodiment, the tester 221, the sample rod mechanism 100 and the receiver 222 are sequentially arranged along the height direction of the transmission electron microscope 200, at least part of the rod body 110 is located in the sample cavity 211, and at least part of the rod body 110 is located outside the sample cavity 211, so as to facilitate the user to adjust the relative position of the rod body 110 and the shell 210. In the working process of the transmission electron microscope 200, the tester 221 emits an electron beam, the electron beam acts on the to-be-detected sample and penetrates the to-be-detected sample, and the receiver 222 receives and stores the detection information of the to-be-detected sample. The transmission electron microscope 200 comprises the sample rod mechanism 100 provided in the application, the power supply assembly 140 is electrically connected to the chip 120 and supplies power to the chip 120, the conductive carrier 130 is electrically connected to the chip 120 and supplies power to the conductive carrier 130, when the power supply assembly 140 is turned on and the current passes through the conductive carrier 130, the conductive carrier 130 generates heat and the temperature rises, so as to realize in-situ heating detection of the to-be-detected sample arranged on the conductive carrier 130. The conductive carrier 130 and the chip 120 provided in the embodiment of the application are detachably connected, after a period of use, if the conductive carrier 130 is fatigued and aged or damaged due to excessively high temperature, the conductive carrier 130 can be directly replaced, and the chip 120 can still be normally used, which greatly reduces the consumable cost and maintenance cost of the sample rod mechanism 100 and improves the use performance of the sample rod mechanism 100, so that the transmission electron microscope 200 has good use performance.

[0079] Optionally, the transmission electron microscope 200 further comprises an objective lens 230 located between the rod body 110 and the receiver 222, which is used for preliminary imaging, so as to facilitate the receiver 222 to further amplify and form a digital image.

[0080] Please refer to Figure 9 The application further provides an in-situ heating test method of a transmission electron microscope 200, which is applied to the transmission electron microscope 200 provided in the application, and the test method comprises the following steps: It can be understood that "in-situ heating" means "heating the to-be-detected sample during the test and observing the changes caused by heating in real time".

[0081] S101, provide a sample rod mechanism 100, the sample rod mechanism 100 includes a rod body 110, a chip 120, a conductive carrier 130 and a power supply assembly 140, the chip 120 is carried on the rod body 110, the chip 120 includes a substrate 121, a first electrode 122 and a second electrode 123, the first electrode 122 and the second electrode 123 are carried on the substrate 121 and are arranged at intervals;The conductive carrier 130 is detachably mounted on the chip 120, and the opposite ends of the conductive carrier 130 are electrically connected to the first electrode 122 and the second electrode 123 respectively;The power supply assembly 140 is electrically connected to the first electrode 122 and the second electrode 123 respectively, for loading voltage on the first electrode 122 and the second electrode 123;The power supply assembly 140 includes a rheostat 144, and the rheostat 144 is connected in series with the conductive carrier 130.

[0082] Understandably, the power supply assembly 140 realizes electrical connection with the conductive carrier 130 through the first electrode 122 and the second electrode 123, when the conductive carrier 130 is mounted on the chip 120 and the power supply assembly 140 is turned on, the power supply assembly 140 loads voltage on the first electrode 122 and the second electrode 123, so that current flows in the conductive carrier 130.

[0083] S102, a sample to be detected is arranged on the conductive carrier 130.

[0084] Understandably, the sample to be detected is a powdery sample.

[0085] S103, turn on the transmission electron microscope 200 to load a first preset voltage on the first electrode 122 and the second electrode 123.

[0086] Understandably, the power supply assembly 140 includes a power supply 141, which is electrically connected to the first electrode 122 and the second electrode 123 respectively, and the power supply 141 is turned on to load a first preset voltage on the first electrode 122 and the second electrode 123.

[0087] Understandably, when the power supply 141 is a constant voltage power supply, the first preset voltage is constant during in-situ heating detection of the transmission electron microscope 200.

[0088] S104, adjust the rheostat 144 to make the voltage applied to the opposite ends of the conductive carrier 130 a second preset voltage, so as to adjust the temperature of the conductive carrier 130, wherein the second preset voltage is less than the first preset voltage.

[0089] It can be understood that, in the process of adjusting the variable resistor 144, the voltage of the opposite ends of the conductive carrier 130 in the first electric connection loop is constantly changing, in other words, the second preset voltage is a variable value.

[0090] It can be understood that, by adjusting the variable resistor 144, the current flowing through the conductive carrier 130 and the voltage applied to the opposite ends of the conductive carrier 130 are changed, and the resistance of the conductive carrier 130 can be calculated. According to the relationship between the resistance and the temperature of the conductive carrier 130 itself, the actual temperature of the conductive carrier 130 can be calculated.

[0091] S105, detecting the sample to be detected by the test assembly 220.

[0092] In the in-situ heating test method of the transmission electron microscope 200 provided in the present application, the electric connection is realized by setting the power supply assembly 140, the chip 120 and the conductive carrier 130, so that the power supply assembly 140 can provide stable power supply for the conductive carrier 130 and make the conductive carrier 130 heat, thereby realizing the heating of the sample to be detected. Further, by setting the variable resistor 144 in the electric connection loop of the power supply assembly 140, the chip 120 and the conductive carrier 130, the current flowing through the conductive carrier 130 and the voltage applied to the opposite ends of the conductive carrier 130 are adjusted, thereby changing the resistance of the conductive carrier 130. Further, according to the preset relationship between the resistance and the temperature of the conductive carrier 130, the temperature of the conductive carrier 130 can be adjusted to a certain value to meet the temperature requirement of the sample to be detected during detection, thereby realizing the in-situ heating detection of the sample to be detected. In the test scheme provided in the embodiment of the present application, the electric connection relationship of the power supply assembly 140, the chip 120 and the conductive carrier 130 is simple, and high-precision micro-nano structure does not need to be set on the chip 120, which guarantees the stability of the electric connection, thereby guaranteeing the stability of the transmission electron microscope 200 in testing the sample to be detected. In addition, after a period of use, if the conductive carrier 130 needs to be replaced due to damage, the chip 120 with high-precision design and high price can be reused, and only the conductive carrier 130 needs to be replaced and repaired, which greatly reduces the consumable cost and maintenance cost of the sample rod mechanism 100, and the electric connection mode of the conductive carrier 130 and the chip 120 is simple, which is convenient for users to replace and improves the detection efficiency of detecting the sample to be detected.

[0093] In some embodiments, the loading of the first preset voltage on the first electrode 122 and the second electrode 123 includes that the power supply assembly 140 includes a power supply 141, a first conductive voltage head 142 and a second conductive voltage head 143, the power supply 141, the rheostat 144, the first conductive voltage head 142, the first electrode 122, the conductive carrier 130, the second electrode 123, the second conductive voltage head 143 form a first electric connection loop, and the power supply 141 is turned on to load the first preset voltage on the first electrode 122 and the second electrode 123.

[0094] In the present embodiment, the power supply 141 is electrically connected with the conductive carrier 130 through the first electrode 122 and the second electrode 123, and the turning on and off of the power supply 141 can control the on-off of the current flowing through the conductive carrier 130.

[0095] Please refer to Figure 10 In some embodiments, the adjusting of the rheostat 144 to make the voltage applied on the opposite ends of the conductive carrier 130 be the second preset voltage to adjust the temperature of the conductive carrier 130 includes: S1041, the power supply assembly 140 includes an ammeter 149, the ammeter 149 is in series with the conductive carrier 130 in the first electric connection loop, and the ammeter 149 is used to detect the current flowing through the conductive carrier 130.

[0096] S1042, the rheostat 144 is adjusted to change the current flowing through the conductive carrier 130 and the voltage on the opposite ends of the conductive carrier 130.

[0097] S1043, the power supply assembly 140 includes a third conductive voltage head 145, a fourth conductive voltage head 146 and a voltmeter 147 connected in sequence, the third conductive voltage head 145, the voltmeter 147, the fourth conductive voltage head 146 and the conductive carrier 130 form a second electric connection loop, and the voltmeter 147 is used to detect the voltage on the opposite ends of the conductive carrier 130 so that the voltage on the opposite ends of the conductive carrier 130 is the second preset voltage.

[0098] It can be understood that in the process of adjusting the rheostat 144, the voltage information detected by the voltmeter 147 and the current information detected by the ammeter 149 change in real time.

[0099] S1044, obtaining the resistance of the conductive carrier 130 according to the current information detected by the ammeter 149 and the voltage information detected by the voltmeter 147, and obtaining the temperature of the conductive carrier 130 according to the preset relationship between the resistance and the temperature.

[0100] It can be understood that the "preset relationship between the resistance and the temperature" is the corresponding relationship between the temperature of the conductive carrier 130 and the resistance. The calibration curve of the resistance and the temperature can be obtained and established by experimental measurement and data calibration. Specifically, before in-situ heating detection of the sample to be detected, the resistance of the conductive carrier 130 is calculated according to the current information detected by the ammeter 149 and the voltage information detected by the voltmeter 147 by adjusting the resistance of the rheostat 144 to adjust the voltage at the opposite ends of the conductive carrier 130 and the current flowing through the conductive carrier 130. The corresponding relationship between the resistance and the temperature is established, and the preset relationship is obtained through data calibration.

[0101] It can be understood that the resistance of the conductive carrier 130 is positively correlated with the temperature.

[0102] In the test method provided in the embodiment, the third conductive voltage head 145, the fourth conductive voltage head 146 and the voltmeter 147 are arranged to detect the voltage at the opposite ends of the conductive carrier 130 in real time, and the current information detected by the ammeter 149 is combined to obtain the real-time resistance of the conductive carrier 130. The user can obtain the temperature of the conductive carrier 130 and control the temperature of the conductive carrier 130, so as to accurately control the test temperature of the sample to be detected. The test method adopts a four-terminal connection method, two electrodes are used to provide the required current for measurement, and do not participate in voltage detection. The other two electrodes are directly connected to the opposite ends of the heating part 132. Since the input impedance is very high, almost no current flows through, which can avoid the voltage drop caused by the current on the electrode contact resistance to interfere with the measurement, and can accurately measure the voltage at the opposite ends of the conductive carrier 130. The test method has high test accuracy for the sample to be detected.

[0103] In this application, the terms "embodiment" and "implementation" mean that a specific feature, structure, or characteristic described in connection with an embodiment can be included in at least one embodiment of this application. The appearance of these phrases in various locations throughout the specification does not necessarily refer to the same embodiment, nor are they independent or alternative embodiments mutually exclusive with other embodiments. Those skilled in the art will understand, explicitly and implicitly, that the embodiments described in this application can be combined with other embodiments. Furthermore, it should be understood that the features, structures, or characteristics described in the various embodiments of this application can be arbitrarily combined to form another embodiment that does not depart from the spirit and scope of the technical solution of this application, provided there is no contradiction between them.

[0104] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application and are not intended to limit it. Although this application has been described in detail with reference to the above preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions to the technical solutions of this application should not depart from the spirit and scope of the technical solutions of this application.

Claims

1. A sample rod mechanism, characterized by, The sample rod mechanism comprises: a rod body; a chip carried on the rod body, the chip comprising a substrate, a first electrode and a second electrode, the first electrode and the second electrode being carried on the substrate and arranged in a spaced manner; a conductive carrier detachably mounted on the chip, opposite ends of the conductive carrier being electrically connected to the first electrode and the second electrode respectively, for carrying a sample to be detected; and a power supply assembly electrically connected to the first electrode and the second electrode respectively, for loading the first electrode and the second electrode with a voltage.

2. The sample bar mechanism of claim 1, wherein, The first electrode and the second electrode are both exposed to the substrate, the power supply assembly comprising a power supply, a first conductive voltage head and a second conductive voltage head, the power supply being electrically connected to the first conductive voltage head and the second conductive voltage head respectively, the first conductive voltage head abutting against the first electrode, and the second conductive voltage head abutting against the second electrode.

3. The sample bar mechanism of claim 2, wherein, The power supply assembly further comprises a variable resistor connected in series with the first conductive voltage head, the variable resistor being used for adjusting the current flowing through the conductive carrier.

4. The sample bar mechanism of claim 2, wherein, The chip further has a third electrode and a fourth electrode, the third electrode and the fourth electrode both being carried on the substrate and located between the first electrode and the second electrode, the first electrode, the third electrode, the fourth electrode and the second electrode being arranged in a spaced manner along a predetermined direction, the third electrode and the fourth electrode also being electrically connected to opposite ends of the conductive carrier respectively, the third electrode and the fourth electrode both being exposed to the substrate; The power supply assembly further comprises a third conductive voltage head, a fourth conductive voltage head and a voltmeter, the voltmeter being electrically connected to the third conductive voltage head and the fourth conductive voltage head respectively, the third conductive voltage head abutting against the third electrode, the fourth conductive voltage head abutting against the fourth electrode, and the voltmeter being used for detecting the voltage at opposite ends of the conductive carrier.

5. The sample bar mechanism of claim 4, wherein, The sample rod mechanism further comprises a pressing block assembly, the pressing block assembly comprising a pressing block and a locking member, the pressing block being arranged on a side of the chip away from the rod body, the conductive carrier being clamped between the pressing block and the chip, and the locking member being sequentially arranged on the pressing block and the rod body, so as to fix the relative positions of the conductive carrier and the chip.

6. The sample bar mechanism of claim 5, wherein, The rod body has a first window penetrating through two opposite surfaces of the rod body along the thickness direction thereof; the chip has a second window penetrating through two opposite surfaces of the substrate along the thickness direction thereof, the first window and the second window being in communication; At least part of the conductive carrier is arranged corresponding to the first window and the second window, the first electrode and the third electrode being located on the same side of the first window and the second window, and the second electrode and the fourth electrode being located on the other side of the first window and the second window.

7. The sample bar mechanism of claim 6, wherein, The pressing block comprises a body part, a first pressing part and a second pressing part, the first pressing part and the second pressing part are located at the same side of the body part and are arranged at intervals, along the preset direction, the first pressing part and the second pressing part are respectively located at opposite sides of the first window, the first pressing part and the second pressing part are respectively used for pressing opposite ends of the conductive carrier, the thickness of the first pressing part is less than the thickness of the body part, and the thickness of the second pressing part is less than the thickness of the body part.

8. The sample stick mechanism according to any one of claims 1 to 7, characterized in that The conductive carrier is a tungsten wire, the conductive carrier is cylindrical, and the diameter of the conductive carrier is less than or equal to 50 μm.

9. A transmission electron microscope, characterized by The transmission electron microscope comprises: a shell having a sample cavity; The sample rod mechanism of any one of claims 1 to 8, at least part of the rod body, the chip, the conductive carrier and at least part of the power supply assembly are located in the sample cavity; and A test assembly comprising a tester and a receiver, the tester and the receiver are arranged in the sample cavity, along the height direction of the transmission electron microscope, the tester and the receiver are respectively arranged at opposite sides of the rod body, the tester is used for emitting an electron beam, and the receiver is used for receiving and storing detection information of a sample to be detected.

10. An in-situ heating test method of a transmission electron microscope, characterized by, The test method applied to the transmission electron microscope of claim 9, the test method comprises: Providing a sample rod mechanism, the sample rod mechanism comprises a rod body, a chip, a conductive carrier and a power supply assembly, the chip is carried on the rod body, the chip comprises a substrate, a first electrode and a second electrode, the first electrode and the second electrode are carried on the substrate and arranged at intervals; the conductive carrier is detachably installed on the chip, opposite ends of the conductive carrier are respectively electrically connected to the first electrode and the second electrode; the power supply assembly is respectively electrically connected to the first electrode and the second electrode, and is used for loading voltage on the first electrode and the second electrode; the power supply assembly comprises a variable resistor, and the variable resistor is connected in series with the conductive carrier; A sample to be detected is arranged on the conductive carrier; The transmission electron microscope is started to load a first preset voltage on the first electrode and the second electrode; The variable resistor is adjusted to make the voltage applied to the opposite ends of the conductive carrier be a second preset voltage, so as to adjust the temperature of the conductive carrier, wherein the second preset voltage is less than the first preset voltage; and The sample to be detected is detected by the test assembly.

11. The in-situ heated test method of claim 10, wherein, The first preset voltage is loaded on the first electrode and the second electrode, which comprises: The power supply assembly comprises a power supply, a first conductive voltage head and a second conductive voltage head, the power supply, the variable resistor, the first conductive voltage head, the first electrode, the conductive carrier, the second electrode, the second conductive voltage head form a first electric connection loop, and the power supply is started to load a first preset voltage on the first electrode and the second electrode.

12. The in-situ heated test method of claim 11, wherein, The adjusting the rheostat to make the voltage applied on the opposite ends of the conductive carrier be a second preset voltage, so as to adjust the temperature of the conductive carrier comprises: The power supply assembly comprises an ammeter, the ammeter is in series with the conductive carrier in the first electric connection loop, and the ammeter is used to detect the current flowing through the conductive carrier; The rheostat is adjusted to change the current flowing through the conductive carrier and the voltage on the opposite ends of the conductive carrier; The power supply assembly comprises a third conductive voltage head, a fourth conductive voltage head and a voltage meter which are electrically connected in sequence, the third conductive voltage head, the voltage meter, the fourth conductive voltage head and the conductive carrier form a second electric connection loop, and the voltage meter is used to detect the voltage on the opposite ends of the conductive carrier so that the voltage on the opposite ends of the conductive carrier is a second preset voltage; According to the current information detected by the ammeter and the voltage information detected by the voltage meter, the resistance of the conductive carrier is obtained, and according to the preset relationship between the resistance and the temperature, the temperature of the conductive carrier is obtained.

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