Ultrahigh-temperature in-situ test heating chip for electron microscope and use method thereof

Abstract

The invention relates to an ultrahigh-temperature in-situ test heating chip for an electron microscope and a use method of the ultrahigh-temperature in-situ test heating chip. The heating chip is specially designed for testing ultrahigh-temperature performance of a material. The heating chip is used for electron microscope in-situ observation in an ultra-high temperature environment, and the highest temperature can reach 1800 DEG C. The heating chip comprises a high-temperature-resistant insulating substrate, a B-type platinum-rhodium thermocouple and an observation hole; the B-type platinum-rhodium thermocouple is embedded in a slot reserved in the high-temperature-resistant insulating substrate; the observation holes are distributed in the middle of the thermocouple. The in-situ electron microscope has the capability of rapidly heating and cooling, and is suitable for in-situ electron microscope experiments of samples under the temperature condition of 0-1800 DEG C.

Description

Technical Field

[0001] The present invention relates to the technical field of high-temperature in-situ testing of electron microscopes, and in particular to an ultra-high-temperature in-situ testing heating chip for electron microscopes and a method of using the same. Background Art

[0002] With the development of electron microscopy and nanofabrication, the in-situ analysis technology of scanning electron microscopy (SEM) and transmission electron microscopy (TEM) has made significant progress and has become a key technology for studying changes in the microstructure of materials. This technology can apply a variety of external field conditions in real time during the experiment, such as gas, liquid environment, force, heat, electricity and other factors, to explore the evolution of the microstructure of materials under these conditions and its relationship with physical and chemical properties. Especially in terms of the ability to observe the evolution of material structure in situ at the atomic level, TEM technology has shown its unique value.

[0003] However, existing SEM and TEM technologies still face challenges in achieving ultra-high temperature in-situ observation. For example, GiulianoGregori et al. proposed a SEM platform capable of in-situ observation at 1450°C; the transmission electron microscope heating sample rod developed by Gatan in the United States can be heated to 1000°C; and the transmission electron microscope sample rod of DensSolution in the Netherlands can reach 1300°C. However, how to achieve precise temperature control and rapid temperature adjustment at higher temperatures (>1500°C) is still a technical problem. Summary of the invention

[0004] The present invention relates to an ultra-high temperature in-situ test heating chip for electron microscope, and is particularly designed for electron microscope testing of material properties and microstructure observation under ultra-high temperature conditions. The present invention mainly solves the problem of limited heating temperature (less than 1500°C) of existing electron microscope heating chips, and provides an ultra-high temperature heating chip that can quickly and accurately control temperature, with a temperature range of 0-1800°C.

[0005] In order to solve the above technical problems, the present invention adopts the following technical solution: an ultra-high temperature in-situ test heating chip for an electron microscope, comprising a high temperature resistant insulating substrate, the upper surface of the high temperature resistant insulating substrate has a "J"-shaped groove, and the part of the high temperature resistant insulating substrate half-surrounded by the groove head has a plurality of observation holes.

[0006] It also includes a B-type platinum-rhodium thermocouple with the same shape as the groove, and the B-type platinum-rhodium thermocouple is tightly matched with the groove; the left and right tails of the B-type platinum-rhodium thermocouple are respectively used to set the terminal a and the terminal b.

[0007] Furthermore, the B-type platinum-rhodium thermocouple used for heating and temperature measurement functions is a type of thermocouple used for high-temperature measurement, which is made of a platinum-rhodium alloy, wherein the platinum-rhodium alloy is of two types, one is a platinum-rhodium alloy containing 70% platinum and 30% rhodium, or the other is a platinum-rhodium alloy containing 94% platinum and 6% rhodium.

[0008] Furthermore, the high temperature resistant insulating substrate is made of a high temperature resistant material with a melting point higher than 1800°C, and is punched and grooved using a processing technique for sample observation and embedding of a B-type thermocouple.

[0009] Furthermore, the terminal a and the terminal b are connected to the control system through the platinum-rhodium wire a and the platinum-rhodium wire b respectively, and one end of the platinum-rhodium wire a and the platinum-rhodium wire b connected to the control system is the thermocouple cold end, and the thermocouple cold end is controlled at 0°C, or the change of the cold end temperature is compensated by using cold end compensation.

[0010] The ultra-high temperature heating chip can achieve precise temperature control of 0-1800°C, wherein the temperature control accuracy is higher than 0.01°C.

[0011] A method for using an ultra-high temperature in-situ test heating chip for an electron microscope comprises the following steps:

[0012] Step 1: Place the test sample at the sample position of the heating chip, and fix the heating chip at the observation position of the electron microscope.

[0013] Step 2: Set the required temperature (0-1800°C) and heating curve of the experiment through the control system to heat the B-type platinum-rhodium thermocouple heating chip to the set temperature.

[0014] Step 3: Observe the set temperature curve and the actual temperature curve displayed by the control system to confirm the accuracy of the chip temperature.

[0015] Step 4: Use electron microscopy to perform high-resolution imaging, elemental composition analysis, crystal structure analysis, three-dimensional imaging, surface morphology measurement and quantitative analysis of the sample on the high-temperature chip.

[0016] Step 5: After the test is completed, remove the heating chip and proceed to the next round of testing or data analysis.

[0017] Compared with the prior art, the present invention has at least the following beneficial effects:

[0018] 1. Chip substrate design: The chip substrate is made of high temperature resistant materials to ensure the stability of the heating chip at high temperatures.

[0019] 2. Heating principle selection: The heating and temperature measuring elements of this chip are B-type platinum-rhodium thermocouples (Pt-Rh thermocouples), which have an operating temperature range of 0°C to 1800°C, making the maximum operating temperature of the chip up to 1800°C. The heating method uses the same thermocouple to achieve both heating and temperature measurement functions.

[0020] 3. Rapid heating capability: The heating chip design includes efficient heating elements (type B platinum-rhodium thermocouples) to achieve rapid heating (maximum heating rate greater than 10°C / s), meeting the requirements for temperature change rate under different experimental conditions.

[0021] 4. Stability and reliability at high temperatures: The structure and material selection of the heating chip are optimized to withstand temperatures up to 1800°C without affecting the structural stability and functionality of the chip.

[0022] 5. The heating chip of the present invention provides an ideal experimental platform for material performance testing and structural observation under ultra-high temperature, and is particularly suitable for electron microscope in-situ testing that needs to be performed under ultra-high temperature environment. This innovative heating chip technology is expected to promote research progress in the fields of materials science and nanotechnology. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 An ultra-high temperature in-situ testing heating chip system for an electron microscope is provided in an embodiment of the present invention.

[0024] Figure 2 It is a top view of an ultra-high temperature in-situ testing heating chip for an electron microscope provided by an embodiment of the present invention.

[0025] Figure 3 This is a three-dimensional exploded view of an ultra-high temperature in-situ testing heating chip for an electron microscope provided by an embodiment of the present invention.

[0026] Figure numerals: 1. Heating chip; 2. High temperature resistant insulating substrate; 3. Type B platinum-rhodium thermocouple; 4. Observation hole; 5. Terminal a; 6. Terminal b; 7. Platinum-rhodium wire a; 8. Platinum-rhodium wire b; 9. Heating wire; 10. Control system. DETAILED DESCRIPTION

[0027] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] The present invention proposes a super-high temperature in-situ test heating chip for an electron microscope, abbreviated as the heating chip. The heating chip 1 can not only achieve an ultimate heating temperature of up to 1800 °C, but also quickly adjust the temperature, significantly reducing thermal drift, thereby improving the resolution and accuracy of in-situ observation. The development of this innovative super-high temperature heating chip is expected to provide better experimental conditions for material property testing and structural observation under super-high temperature conditions.

[0029] Example 1: A super-high temperature in-situ test heating chip for an electron microscope includes a high-temperature resistant insulating substrate 2. The upper surface of the high-temperature resistant insulating substrate 2 has a "ji"-shaped groove. The part of the high-temperature resistant insulating substrate 2 that is semi-surrounded by the head of the groove has a number of observation holes 4; it also includes a type B platinum-rhodium thermocouple 3 with the same shape as the groove. The type B platinum-rhodium thermocouple 3 is closely fitted with the groove; the left and right tails of the type B platinum-rhodium thermocouple 3 are respectively used to set up a terminal a5 and a terminal b6.

[0030] Observation holes 4 are opened on the high-temperature resistant insulating substrate 2. The type B platinum-rhodium thermocouple 3 is semi-surrounded in the observation holes 4. The type B platinum-rhodium thermocouple 3 is also "ji"-shaped, and its left and right tails are respectively used to set up a terminal a5 and a terminal b6. The terminal a5 is connected to the control system through a platinum-rhodium wire a7, and the terminal b6 is connected to the control system through a platinum-rhodium wire b8. The terminal a5 and the terminal b6 are used to transmit temperature signals and achieve temperature control. The control system is located outside the high-temperature resistant insulating substrate 2 and can receive the temperature data of the type B platinum-rhodium thermocouple 3 through the platinum-rhodium wire a and the platinum-rhodium wire b and adjust the temperature of the heating chip to ensure precise temperature control. The heating chip can achieve a heating temperature of 0 - 1800 °C; the heating chip performs heating and cooling operations through the control system. The control system includes a temperature measurement module, a heating module, and a temperature adjustment module.

[0031] Specifically, the type B platinum-rhodium thermocouple 3 used for heating and temperature measurement is a type of thermocouple for high-temperature measurement, made of a platinum-rhodium alloy. There are two types of platinum-rhodium alloys. One is a platinum-rhodium alloy containing 70% platinum and 30% rhodium, and the other is a platinum-rhodium alloy containing 94% platinum and 6% rhodium. Specifically, the high-temperature resistant insulating substrate 2 is made of a high-temperature resistant material with a melting point higher than 1800 °C, and is punched and grooved using processing techniques for sample observation and embedding the type B thermocouple.

[0032] Specifically, one end of the platinum-rhodium wire a7 and the platinum-rhodium wire b8 connected to the control system 10 is controlled at 0 °C for the cold end of the thermocouple, or the change in the cold end temperature is compensated by using cold end compensation to ensure the temperature measurement accuracy of the super-high temperature heating chip. The super-high temperature heating chip can achieve precise temperature control of 0 - 1800 °C, and the temperature control accuracy is higher than 0.01 °C.

[0033] A method for preparing an ultra-high temperature in-situ test heating chip for an electron microscope comprises the following steps:

[0034] 1. Manufacturing of heating chip:

[0035] (1) Zirconium dioxide ceramic material with excellent high temperature resistance and mechanical strength is selected as the base material of the heating chip. The zirconium dioxide ceramic is laser cut to prepare a rectangular chip base with a size of 10 mm × 10 mm and a thickness of 3 mm. Laser cutting, with its non-contact processing method, can effectively reduce the mechanical and thermal stress on the material during the cutting process, thereby obtaining a chip base with smooth edges and high-precision dimensions.

[0036] (2) After obtaining the chip substrate of the required size, a groove for embedding the heating element is further processed on the surface of the chip substrate using laser processing technology. The design of the groove takes into account the size and position to ensure that the heating element can be stably embedded therein. Specifically, the processing depth is precisely controlled by laser, and a groove with a depth of 0.5 mm is cut.

[0037] (3) After the groove is processed, a B-type thermocouple wire is embedded into the groove as a heating and temperature measuring element. During the embedding process, ensure that the thermocouple wire fits tightly into the groove to ensure heating efficiency and temperature measurement accuracy.

[0038] (4) After the heating element is embedded, the entire heating chip is mechanically ground and polished. First, each surface of the chip is evenly ground using precision mechanical grinding equipment to remove any rough surfaces and tiny defects that may have occurred during the processing. Then, polishing is performed to further improve the smoothness of the chip surface.

[0039] 2. Heating chip connection:

[0040] (1) Platinum-rhodium materials corresponding to the chip heating elements are selected to connect to the control system for temperature measurement, wherein the platinum-rhodium wire a7 and the platinum-rhodium wire b8 are connected to the terminal a5 and the terminal b6 respectively.

[0041] (2) A pure silver wire is used as the heating wire 9 connected to the terminal a5 and the terminal b6 for heating.

[0042] Example 2: Experimental method and steps for ultra-high temperature in-situ testing of heating chip:

[0043] (1) Sample installation: Place the experimental sample at the sample position of the heating chip, that is, the position of the observation hole 4, and fix the heating chip at the electron microscope observation position.

[0044] (2) Temperature setting: The required heating temperature (0-1800°C) and heating curve are set through the control system. The setting range is 0-1800°C, and the fastest heating speed is greater than 10°C / s.

[0045] (3) Heating and testing: Start the heating system 10, monitor the sample stage temperature in real time, control the temperature of the heating chip, and simultaneously perform high-resolution imaging, elemental composition analysis, crystal structure analysis, three-dimensional imaging, surface morphology measurement, and quantitative analysis of the sample on the high-temperature chip.

Claims

1. An ultra-high temperature in-situ test heating chip for electron microscope, characterized in that: The invention comprises a high temperature resistant insulating base (2), wherein the upper surface of the high temperature resistant insulating base (2) has a "J"-shaped groove, and the portion of the high temperature resistant insulating base (2) half-surrounded by the groove head has a plurality of observation holes (4); and further comprises a B-type platinum-rhodium thermocouple (3) having the same shape as the groove, wherein the B-type platinum-rhodium thermocouple (3) is tightly matched with the groove; and the left and right tails of the B-type platinum-rhodium thermocouple (3) are respectively used to set a terminal a (5) and a terminal b (6).

2. The ultra-high temperature in-situ test heating chip for electron microscope according to claim 1, characterized in that: The B-type platinum-rhodium thermocouple (3) is a type of thermocouple used for high-temperature measurement and is made of a platinum-rhodium alloy, wherein the platinum-rhodium alloy contains 70% platinum and 30% rhodium, or 94% platinum and 6%.

3. The ultra-high temperature in-situ test heating chip for electron microscope according to claim 1, characterized in that: The high temperature resistant insulating base (2) is made of a high temperature resistant material having a melting point higher than 1800°C.

4. The ultra-high temperature in-situ test heating chip for electron microscope according to claim 1, characterized in that: The terminal a (5) and the terminal b (6) are connected to the control system via a platinum-rhodium wire a (7) and a platinum-rhodium wire b (8) respectively. One end of the platinum-rhodium wire a (7) and the platinum-rhodium wire b (8) connected to the control system (10) is the cold end of the thermocouple. The cold end of the thermocouple is controlled at 0°C, or the change of the cold end temperature is compensated by using cold end compensation.

5. A method for using an ultra-high temperature in-situ test heating chip for an electron microscope according to any one of claims 1 to 3, characterized in that: The steps include: Step 1: placing the test sample at the sample position of the heating chip, and fixing the heating chip at the observation position of the electron microscope; Step 2, setting the temperature and heating curve required for the experiment through the control system, so that the B-type platinum-rhodium thermocouple (3) heating chip is heated to the set temperature; Step 3: Observe the set temperature curve and the actual temperature curve displayed by the control system to confirm the accuracy of the chip temperature; Step 4: Perform high-resolution imaging, elemental composition analysis, crystal structure analysis, three-dimensional imaging, surface morphology measurement and quantitative analysis of the sample on the high-temperature chip through an electron microscope; Step 5: After the test is completed, remove the heating chip and proceed to the next round of testing or data analysis.

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