In-situ multi-position heating sample table for scanning electron microscope

Abstract

The utility model discloses an in-situ multi-position heating sample stage for a scanning electron microscope, and belongs to the technical field of electron microscopy application. The device structurally comprises a heat preservation cover (1), a first observation window (2), a second observation window (3), a third observation window (4), a first heat preservation cover supporting frame (5), a second heat preservation cover supporting frame (6), a water cooling base (7), a sample table (8), a heating table (9), a first sample clamping piece (10), a second sample clamping piece (11), a third sample clamping piece (12), a heating table supporting column (13), an anti-radiation piece (14), an anti-radiation piece supporting column (15), a heating table positive electrode power line (16) and a heating table negative electrode power line (17). A thermocouple (18), a water inlet conduit (19) and a water outlet conduit (20); according to the utility model, parallel heating and in-situ temperature change test of a plurality of samples can be completed in one heating process, and the in-situ heating test efficiency is effectively improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of the application of electron microscopy technology, and particularly relates to an in-situ multi-position heating sample stage for a scanning electron microscope. Background Art

[0002] As an important tool for microstructural morphology and composition analysis, scanning electron microscopes have been widely used in many fields such as materials, chemistry, biology, and microelectronics. Traditional electron microscope tests are non-in-situ static test characterizations of materials before and after experiments. By comparing and analyzing the changes in the microstructure and chemical composition of materials before and after experiments, the relationship between the structure and properties of materials is indirectly obtained, and thus the mechanism causing the changes is inferred. This indirect observation method will lose a lot of useful information during the change process because of the lack of intuitive microstructural evolution data. In response to this problem, the upsurge of in-situ electron microscope technology that has emerged in recent years has attracted extensive attention.

[0003] In-situ electron microscope technology makes use of the advantages of high spatial resolution of conventional electron microscopes and introduces external excitations such as heat, electricity, and magnetism inside the electron microscope, so as to realize real-time in-situ observation at the microscale and is more conducive to studying the structural and performance changes of materials and devices. Therefore, constructing an in-situ heating sample stage for a scanning electron microscope is of great significance in laboratory construction and testing. CN 211376583 U discloses an "in-situ physical and chemical reaction sample stage for a scanning electron microscope", and the sample stage can observe samples under different temperatures and different chemical atmospheres. CN 213184197 U discloses a "heating stage for a desktop scanning electron microscope", and the sample stage can observe samples at various temperatures or angles. These in-situ heating sample stages and some existing commercial sample stages can be used for the observation of microstructural morphology under different temperature conditions, but most of them have complex structures, high prices, and only one sample observation hole position, with low test efficiency and not suitable for the control experiment research of multiple samples. In summary, it is of practical significance to develop a multi-position scanning electron microscope sample stage with in-situ heating function. Summary of the Invention

[0004] The purpose of the utility model is to provide an in-situ multi-position heating sample stage for a scanning electron microscope. By setting a heating stage, the microstructural morphology of the sample can be observed in-situ under different temperature conditions; by setting a heat preservation cover on the sample stage, radiant heat loss can be avoided; by setting multi-position observation windows on the heat preservation cover and multi-position sample clamping pieces on the sample stage, the heating tests of multiple samples can be completed during one heating process, improving the in-situ heating test efficiency and facilitating the test research of parallel control experiments; by setting double-layer anti-radiation sheets and a water-cooled base, heat conduction between the heating stage and the five-axis motor sample stage of the scanning electron microscope can be effectively avoided.

[0005] To achieve the above purpose, the technical solution of the utility model is as follows:

[0006] An in-situ multi-position heating sample stage for a scanning electron microscope, the structure comprising a water-cooled base 7, a sample stage 8 and a heating stage 9; characterized in that the structure further comprises a heat preservation cover 1, a first observation window 2, a second observation window 3, a third observation window 4, a first heat preservation cover support frame 5, a second heat preservation cover support frame 6, a first sample clamping piece 10, a second sample clamping piece 11, a third sample clamping piece 12, a heating stage support column 13, a radiation protection sheet 14, a radiation protection sheet support column 15, a positive power supply wire 16 for the heating stage, a negative power supply wire 17 for the heating stage, a thermocouple 18, a water inlet conduit 19 and a water outlet conduit 20; the heat preservation cover 1 is fixed on the water-cooled base 7 through the first heat preservation cover support frame 5 and the second heat preservation cover support frame 6, and the first observation window 2, the second observation window 3 and the third observation window 4 are located at the top of the heat preservation cover 1; the heating stage 9 is located below the sample stage 8 for heating the sample stage; the sample clamping pieces 10, 11 and 12 are located on the surface of the sample stage for fixing the sample; the heating stage support column 13 connects the heating stage 9 and the radiation protection sheet 14; the radiation protection sheet support column 15 connects the radiation protection sheet 14 and the water-cooled base 7; the positive power supply wire 16 for the heating stage, the negative power supply wire 17 for the heating stage and the thermocouple 18 pass through the second heat preservation cover support frame 6 and are connected to the heating stage 9; the water inlet conduit 19 and the water outlet conduit 20 are connected to the hollow cavity of the water-cooled base 7.

[0007] Preferably, the temperature adjustment range of the heating stage 9 is from room temperature to 700 °C, and the temperature control accuracy is 0.1 °C.

[0008] The utility model fixes the sample through the first sample clamping piece 10, the second sample clamping piece 11 and the third sample clamping piece 12. After the sample is placed on the sample stage 8, the temperature of the heating stage 9 is adjusted through the positive power supply wire 16 for the heating stage, the negative power supply wire 17 for the heating stage and the thermocouple 18, so as to realize the in-situ heating of the sample stage of the scanning electron microscope; by setting the radiation protection sheet 14, the temperature of the water is adjusted to cool down the base through the connection of the water inlet conduit 19 and the water outlet conduit 20 with the hollow cavity of the water-cooled base 7, so as to avoid the heat conduction between the heating stage 9 and the five-axis motor sample stage of the scanning electron microscope; through the direct switching of the first observation window 2, the second observation window 3 and the third observation window 4, the heating test research of parallel comparison samples can be carried out.

[0009] Beneficial effects:

[0010] Compared with the prior art, the beneficial effects of the present utility model are as follows: When multiple samples are placed on the sample stage 8 and fixed respectively with the first sample clamping piece 10, the second sample clamping piece 11, and the third sample clamping piece 12, parallel heating tests of multiple samples can be completed during one heating process through the first observation window 2, the second observation window 3, and the third observation window 4, effectively improving the in-situ heating test efficiency; the radiation protection sheet 14 and the water-cooled base 7 can effectively avoid heat conduction between the heating stage 9 and the sample stage of the scanning electron microscope five-axis motor; the staggered arrangement of the heating stage support 13 and the radiation protection sheet support 15 can further reduce the heat conduction of the heating stage; the heat preservation cover 1 can effectively reduce the heat loss on the surface of the sample; the positive power supply wire 16 of the heating stage, the negative power supply wire 17 of the heating stage, and the thermocouple 18 are connected to the heating stage 9, and in-situ variable temperature tests of the sample can be achieved by adjusting the temperature of the heating stage 9. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 FIG. is a schematic diagram of the heat preservation cover 1 of an in-situ heating sample stage for a scanning electron microscope provided by an embodiment of the present utility model.

[0012] Figure 2 FIG. is a schematic diagram of the main structure of an in-situ heating sample stage for a scanning electron microscope provided by an embodiment of the present utility model. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0013] The technical solutions in the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model. Obviously, the described embodiments are only a part of the embodiments of the present utility model, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present utility model without creative efforts shall fall within the protection scope of the present utility model.

[0014] The purpose of the present utility model is to provide an in-situ multi-position heating sample stage for a scanning electron microscope, which realizes in-situ observation of the microscopic structure and morphology of samples under different temperature conditions by setting a heating stage; avoids radiant heat loss by setting a heat preservation cover on the sample stage; realizes heating tests of multiple samples during one heating process by setting multi-position observation windows on the heat preservation cover and multi-position sample clamping pieces on the sample stage, improves the in-situ heating test efficiency and is convenient for test research of parallel control experiments; effectively avoids heat conduction between the heating stage and the sample stage of the scanning electron microscope five-axis motor by setting a double-layer radiation protection sheet and a water-cooled base.

[0015] In order to make the above objects, features, and advantages of the present utility model more obvious and understandable, the present utility model will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0016] Embodiment 1 Specific Structure of the Present Utility Model

[0017] Figure 1 Schematic diagram of a heat preservation cover 1 of an in-situ heating sample stage for a scanning electron microscope provided by an embodiment of the present invention. A first observation window 2, a second observation window 3, and a third observation window 4 are opened at the top of the heat preservation cover 1; Figure 2 Schematic diagram of the main structure of an in-situ heating sample stage for a scanning electron microscope provided by an embodiment of the present invention, including a first heat preservation cover support frame 5, a second heat preservation cover support frame 6, a water-cooled base 7, a sample stage 8, a heating stage 9, a first sample clamping piece 10, a second sample clamping piece 11, a third sample clamping piece 12, a heating stage support pillar 13, a radiation protection sheet 14, a radiation protection sheet support pillar 15, a positive power supply wire 16 of the heating stage, a negative power supply wire 17 of the heating stage, a thermocouple 18, a water inlet conduit 19, and a water outlet conduit 20; the heat preservation cover 1 is fixed on the water-cooled base 7 through the first heat preservation cover support frame 5 and the second heat preservation cover support frame 6; the heating stage 9 is located below the sample stage 8 for heating the sample stage; the first sample clamping piece 10, the second sample clamping piece 11, and the third sample clamping piece 12 are located on the surface of the sample stage for fixing the sample; the heating stage support pillar 13 connects the heating stage 9 and the radiation protection sheet 14; the radiation protection sheet support pillar 15 connects the radiation protection sheet 14 and the water-cooled base 7; the positive power supply wire 16 of the heating stage, the negative power supply wire 17 of the heating stage, and the thermocouple 18 pass through the second heat preservation cover support frame 6 and are connected to the heating stage 9; the water inlet conduit 19 and the water outlet conduit 20 are connected to the hollow cavity of the water-cooled base 7.

[0018] The temperature adjustment range of the heating stage 9 is from room temperature to 700 °C, and the accuracy is 0.1 °C. <x

[0019] The first observation window 2, the second observation window 3, and the third observation window 4 can realize the observation and testing of multiple samples during a single heating process in the in-situ heating test.

[0020] The heat preservation cover 1 can effectively reduce the heat loss on the surface of the sample.

[0021] The radiation protection sheet 14 and the water-cooled base 7 can effectively avoid the heat conduction between the heating stage 9 and the five-axis motor sample stage of the scanning electron microscope.

[0022] Embodiment 2 Specific in-situ heating test process of the present invention

[0023] Place the sample on the sample stage 8 and fix the sample with the first sample clamping piece 10. The heat preservation cover 1 covers the sample stage 8, the heating stage 9, the first sample clamping piece 10, the second sample clamping piece 11, the third sample clamping piece 12, the heating stage support pillar 13, the radiation protection piece 14, and the radiation protection piece support pillar 15 through the first heat preservation cover support frame 5 and the second heat preservation cover support frame 6 to reduce the heat loss on the surface of the sample. Pass circulating water into the hollow cavity of the water-cooled base 7 through the water inlet conduit 19 and the water outlet conduit 20 to avoid heat conduction between the heating stage 9 and the sample stage of the scanning electron microscope five-axis motor. Subsequently, connect the positive power supply wire 16 and the negative power supply wire 17 of the heating stage, and control the temperature of the heating stage 9 through the thermocouple 18 to adjust the temperature of the sample stage 8 and the sample for in-situ heating test.

[0024] Multiple-sample parallel test function: After fixing three samples on the sample stage 8 with the first sample clamping piece 10, the second sample clamping piece 11, and the third sample clamping piece 12 respectively, cover the heat preservation cover 1 above the sample stage 8 and the heating stage 9 through the first heat preservation cover support frame 5 and the second heat preservation cover support frame 6. Pass circulating water into the hollow cavity of the water-cooled base 7 through the water inlet conduit 19 and the water outlet conduit 20. Connect the positive power supply wire 16 and the negative power supply wire 17 of the heating stage, and increase the temperature of the heating stage 9 through the thermocouple 18, thereby adjusting the temperature of the sample stage 8 and the sample. First, test the in-situ heating of the sample fixed on the first sample clamping piece 10 through the first observation window 1. Subsequently, move the sample stage and test the sample fixed on the second sample clamping piece 11 through the second observation window 2, and test the sample fixed on the third sample clamping piece 12 through the third observation window 3.

Claims

1. An in-situ multi-position heating sample stage for a scanning electron microscope, the structure comprising a water-cooled base (7), a sample stage (8) and a heating stage (9); characterized in that, The structure further includes a thermal insulation cover (1), a first observation window (2), a second observation window (3), a third observation window (4), a first thermal insulation cover support frame (5), a second thermal insulation cover support frame (6), a first sample clip (10), a second sample clip (11), a third sample clip (12), a heating stage support column (13), a radiation shield (14), a radiation shield support column (15), a positive power supply wire for the heating stage (16), a negative power supply wire for the heating stage (17), a thermocouple (18), a water inlet conduit (19) and a water outlet conduit (20); the thermal insulation cover (1) is fixed on the water-cooled base (7) through the first thermal insulation cover support frame (5) and the second thermal insulation cover support frame (6), and the first observation window (2), the second observation window (3) and the third observation window (4) are located at the top of the thermal insulation cover (1); the heating stage (9) is located below the sample stage (8) for heating the sample stage; the sample clips (10), (11) and (12) are located on the surface of the sample stage for fixing the sample; the heating stage support column (13) connects the heating stage (9) and the radiation shield (14); the radiation shield support column (15) connects the radiation shield (14) and the water-cooled base (7); the positive power supply wire for the heating stage (16), the negative power supply wire for the heating stage (17) and the thermocouple (18) pass through the second thermal insulation cover support frame (6) and are connected to the heating stage (9); the water inlet conduit (19) and the water outlet conduit (20) are connected to the hollow cavity of the water-cooled base (7).

2. The in-situ multi-position heating sample stage for a scanning electron microscope according to claim 1, characterized in that, The temperature adjustment range of the heating stage (9) is from room temperature to 700 °C, and the temperature control accuracy is 0.1 °C.

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