Processing device and processing method for three-dimensional atom probe sample

Abstract

The invention relates to the technical field of material analysis, for example, relates to a processing device and method for three-dimensional atom probe samples, and the processing device comprises a sample bearing module which is provided with sample stations, and each sample station is used for placing a three-dimensional atom probe sample; the vacuum sealing pipe is used for accommodating the sample bearing module; the cooling module is provided with a cavity used for containing cooling liquid, the cavity is provided with a sealing pipe station, and the sealing pipe station is used for containing a vacuum sealing pipe. Based on the treatment device, a full-flow vacuum and low-temperature protection mechanism can be provided for the treatment process of the three-dimensional atom probe sample, the accuracy of subsequent material phase change analysis and component characterization can be remarkably improved, and it is ensured that three-dimensional atom probe data can truly reflect the microstructure characteristics of the three-dimensional atom probe sample.

Description

TECHNICAL FIELD

[0001] The present disclosure relates to the technical field of material analysis, for example to a processing device and a processing method for a three-dimensional atom probe sample. BACKGROUND

[0002] Three-Dimensional Atom Probe (3DAP) is a high-resolution material characterization technology that can realize atomic-scale element distribution analysis. Its basic principle is to evaporate the surface atoms of a needle-shaped three-dimensional atom probe sample layer by layer in an ultra-high vacuum environment by applying a high-voltage pulse electric field, and to detect the atomic species and spatial position information by a time-of-flight mass spectrometer, thereby reconstructing the three-dimensional atomic structure inside the material. This technology is widely used in composition analysis and microstructure research in the fields of metal materials, semiconductor devices, nanostructures, etc.

[0003] In the preparation process of a three-dimensional atom probe sample, the material to be tested is usually rough polished into a needle-shaped structure, and then fine polished to obtain a nanoscale three-dimensional atom probe sample end. However, some environmentally sensitive alloy materials (such as age-hardening aluminum alloy, titanium alloy, nickel-based high-temperature alloy, etc.) exhibit room temperature storage effect in the conventional sample preparation process. Specifically, after heat treatment, the three-dimensional atom probe sample needs to be exposed to room temperature environment for transfer and secondary sample preparation (such as electrolytic polishing). This process inevitably causes heat exchange between the material and the environment, resulting in room temperature storage effect, which leads to phenomena such as composition segregation, phase transformation or local precipitation in the three-dimensional atom probe sample, and the three-dimensional atom probe data obtained finally cannot accurately reflect the microstructure characteristics of the material, which seriously restricts the accurate characterization of the microstructure of the material under extreme process conditions.

[0004] In order to alleviate or inhibit the storage effect, the sample residence time at room temperature needs to be shortened or avoided as much as possible, i.e. the time from the start of sample preparation to the time when the sample is put into the analysis chamber. In the process of handling / transferring the three-dimensional atom probe sample, the related technology causes the sample to be in contact with air, which in turn causes oxidation. For example, in the process of heat treatment and transfer of the three-dimensional atom probe sample after rough polishing to the fine polishing device, the sample will be in contact with air, which will cause oxidation, and the sample needs to be re-polished, thereby increasing the time of the sample preparation process. Although the related technology provides a vacuum heat treatment device or a low-temperature transfer device for the three-dimensional atom probe sample to improve the pollution control and thermal stability in the sample preparation process, there is still a lack of vacuum environment control in the whole process from heat treatment to low-temperature transfer, which cannot effectively overcome the problems caused by product oxidation and room temperature storage effect. SUMMARY

[0005] The following presents a simplified summary of some aspects of the disclosure in order to provide a basic understanding. This summary is not an extensive overview of the disclosure and is not intended to identify key / critical elements or to delineate the scope of the embodiments. Its sole purpose is to present some aspects of the disclosure in a simplified form as a prelude to the more detailed description that is presented later.

[0006] The embodiments of the present disclosure provide a processing device and a processing method for a three-dimensional atom probe sample, provide a full-process vacuum and low-temperature protection mechanism, and significantly improve the accuracy of subsequent material phase change analysis and composition characterization.

[0007] According to a first aspect of the present disclosure, a processing device for a three-dimensional atom probe sample is provided, comprising:

[0008] A sample carrying module is provided with a sample station, and each sample station is used to place one three-dimensional atom probe sample;

[0009] A vacuum sealed tube is used to accommodate the sample carrying module;

[0010] A cooling module is provided with a cavity for accommodating a cooling liquid, and the cavity is provided with a sealed tube station for placing the vacuum sealed tube.

[0011] In some embodiments, the sample carrying module comprises:

[0012] A sample carrying base is provided with a sample station;

[0013] A sample protection cover is detachably buckled to the sample carrying base to place the sample station inside.

[0014] In some embodiments, the sample protection cover is provided with a through hole.

[0015] In some embodiments, the sample carrying base is a columnar structure with threads on the outer periphery, and one end face of the sample carrying base is provided with a sample station;

[0016] The sample protection cover is a cylindrical structure with threads on the inner periphery, and is buckled to the sample carrying base by threaded connection.

[0017] In some embodiments, one end face of the sample carrying base is provided with a plurality of sample stations.

[0018] In some embodiments, the sample protection cover comprises:

[0019] A bottom plate;

[0020] A cylindrical body, the inner periphery of the cylindrical body is provided with threads, the bottom plate is arranged at one end of the cylindrical body, and the other end of the cylindrical body is open;

[0021] At least one of the bottom plate and the cylindrical body is provided with a through hole.

[0022] In some embodiments, the bottom plate is provided with a plurality of through holes.

[0023] In some embodiments, the cylinder is provided with a plurality of through holes, which are distributed along the circumferential direction and / or the axial direction of the cylinder.

[0024] In some embodiments, the cooling module comprises:

[0025] The shell is provided with a chamber for accommodating the cooling liquid and has an open mouth;

[0026] The cover is detachably arranged at the open mouth of the shell;

[0027] The seal tube carrier is located inside the chamber and is provided with a plurality of seal tube stations.

[0028] In some embodiments, the outer wall of the shell is a vacuum sandwich structure, and / or the outer wall of the shell is provided with a heat insulation material.

[0029] In some embodiments, the seal tube carrier is provided with a plurality of seal tube stations.

[0030] In some embodiments, the seal tube carrier is a cylindrical structure, one end face of the seal tube carrier is connected to the bottom of the shell, and the other end face of the seal tube carrier is provided with a plurality of seal tube stations.

[0031] According to a second aspect of the present disclosure, a processing method for a three-dimensional atom probe sample is provided, which is implemented based on the processing device for the three-dimensional atom probe sample provided in the first aspect, and comprises:

[0032] Placing the three-dimensional atom probe sample after rough polishing in the sample station of the sample carrying module;

[0033] Placing the sample carrying module in the vacuum seal tube, vacuumizing the vacuum seal tube, and then performing heat treatment on the three-dimensional atom probe sample;

[0034] Placing the vacuum seal tube after heat treatment in the seal tube station of the cooling module, and cooling the three-dimensional atom probe sample by using the cooling liquid;

[0035] After the cooling is completed, the three-dimensional atom probe sample is taken out from the sample carrying module.

[0036] In some embodiments, the parameter requirements of the heat treatment process of the three-dimensional atom probe sample include at least one of the following:

[0037] The temperature of the heat treatment is not lower than 300℃;

[0038] The duration of the heat treatment is not less than 10min;

[0039] The vacuum degree in the vacuum sealed tube is not higher than 1*10 -2 Pa.

[0040] In some embodiments, the parameter requirements of the cooling process of the three-dimensional atom probe sample include at least one of the following:

[0041] The cooling rate is not less than 10℃ / s;

[0042] The temperature of the three-dimensional atom probe sample after cooling is not higher than-50℃.

[0043] The processing device and processing method for the three-dimensional atom probe sample provided by the embodiments of the present disclosure can achieve the following technical effects:

[0044] The processing device for the three-dimensional atom probe sample provided by the embodiments of the present disclosure, when applied to the processing process of the three-dimensional atom probe sample, provides a full-process vacuum protection environment for the three-dimensional atom probe sample through the vacuum sealed tube. Specifically, after being roughly polished, the three-dimensional atom probe sample is placed in the vacuum sealed tube to avoid contact with air. Subsequently, the three-dimensional atom probe sample enters the heat treatment process, and precise temperature control is achieved through the external heating system. After the heat treatment is completed, the three-dimensional atom probe sample is transferred to the cooling module together with the vacuum sealed tube, and rapid cooling is performed by using the cooling liquid. Since the three-dimensional atom probe sample remains in the vacuum environment during the entire cooling process, contact with air is further prevented. During the heat treatment and cooling process, the three-dimensional atom probe sample is always in a vacuum sealed state, effectively isolating contact with external air and preventing the three-dimensional atom probe sample from undergoing oxidation reaction, thereby helping to shorten the time of the preparation process of the three-dimensional atom probe sample. During the cooling process, the cooling liquid in the cooling module can quickly cool and maintain low temperature for a long time, avoiding the composition segregation or phase change problem caused by the room temperature parking effect. Finally, after the cooling is completed, the three-dimensional atom probe sample is taken out from the vacuum sealed tube and subjected to fine polishing treatment, and then quickly transferred to the three-dimensional atom probe equipment for characterization. Through this full-process vacuum and low-temperature protection mechanism, the accuracy of subsequent material phase change analysis and composition characterization is significantly improved, and it is ensured that the three-dimensional atom probe data can truly reflect the microstructure characteristics of the three-dimensional atom probe sample.

[0045] The foregoing general description and the following description are merely exemplary and explanatory, and are not intended to limit the present disclosure. BRIEF DESCRIPTION OF DRAWINGS

[0046] One or more embodiments are exemplarily illustrated by corresponding drawings, which do not constitute a limitation on the embodiments, elements with the same reference numerals in the drawings are shown as similar elements, the drawings do not constitute a proportional limitation, and wherein:

[0047] Figure 1 is a schematic diagram of a processing device for a three-dimensional atom probe sample provided by an embodiment of the present disclosure from one perspective;

[0048] Figure 2 is a schematic diagram of a processing device for a three-dimensional atom probe sample provided by an embodiment of the present disclosure from one perspective;

[0049] Figure 3 is a schematic diagram of a processing device for a three-dimensional atom probe sample provided by an embodiment of the present disclosure after being cut open at A shown in the figure; Figure 2

[0050] Figure 4 is a schematic diagram of a processing device for a three-dimensional atom probe sample provided by an embodiment of the present disclosure after the cover is removed;

[0051] Figure 5 is a schematic diagram of a vacuum-sealed tube provided by an embodiment of the present disclosure;

[0052] Figure 6 is a schematic diagram of a sample-bearing module provided by an embodiment of the present disclosure;

[0053] Figure 7 is an exploded schematic diagram of a sample-bearing module provided by an embodiment of the present disclosure;

[0054] Figure 8 is a flowchart of a processing method for a three-dimensional atom probe sample provided by an embodiment of the present disclosure.

[0055] The following is a description of the reference numerals:

[0056] 100 a processing device for a three-dimensional atom probe sample;

[0057] 1 a sample-bearing module;

[0058] 101 a sample station, 11 a sample-bearing base, 12 a sample protection cover;

[0059] 120 a through hole, 121 a bottom plate, 122 a barrel;

[0060] 2 a vacuum-sealed tube;

[0061] 3 a cooling module;

[0062] 301 a chamber, 302 a sealed tube station;

[0063] 31 a cover, 32 a shell, 33 a sealed tube-bearing seat;

[0064] 200 a three-dimensional atom probe sample. DETAILED DESCRIPTION

[0065] ​In order to enable a more detailed understanding of the features and technical content of the embodiments of the present disclosure, the implementation of the embodiments of the present disclosure is described in detail below with reference to the accompanying drawings, which are only used for reference and do not limit the embodiments of the present disclosure. In the following technical description, in order to facilitate explanation, a plurality of details are provided to provide a full understanding of the disclosed embodiments. However, one or more embodiments can still be implemented without these details. In other cases, well-known structures and devices can be simplified to facilitate the drawings.

[0066] The terms "first", "second", and the like in the specification and claims of the embodiments of the present disclosure and the above drawings are used to distinguish similar objects, and do not necessarily have to describe a specific order or sequence. It should be understood that the data thus used can be interchanged under appropriate circumstances, so that the embodiments of the present disclosure described herein can be implemented. In addition, the terms "include" and "have" and any variations thereof are intended to cover non-exclusive inclusion.

[0067] Unless otherwise specified, the term "a plurality of" means two or more.

[0068] In the embodiments of the present disclosure, the character " / " represents an "or" relationship between the objects before and after it. For example, A / B means: A or B.

[0069] The term "and / or" is a description of the association between objects, which means that there can be three relationships. For example, A and / or B means: A or B, or, A and B, the three relationships.

[0070] The term "corresponding" can refer to an association or binding relationship. A and B correspond to each other means that there is an association or binding relationship between A and B.

[0071] In combination Figures 1 to 7 For example, the embodiments of the present disclosure provide a processing device 100 for a three-dimensional atom probe sample, the processing device 100 comprising a sample carrying module 1, a vacuum sealed tube 2 and a cooling module 3.

[0072] The sample carrying module 1 is provided with a sample station 101, and each sample station 101 is used to place a three-dimensional atom probe sample 200. The vacuum sealed tube 2 is used to accommodate the sample carrying module 1. The cooling module 3 is provided with a cavity 301 for accommodating a cooling liquid, and the cavity 301 is provided with a sealed tube station 302 for placing the vacuum sealed tube 2.

[0073] The processing device 100 can perform pre-analysis processing on the three-dimensional atom probe sample 200. Specifically, first, the rough-polished three-dimensional atom probe sample 200 is placed in the sample workstations 101 of the sample carrier module 1. Each sample workstation 101 is adapted to the fixed copper tube of the three-dimensional atom probe sample 200, ensuring that the three-dimensional atom probe sample 200 remains stable during subsequent processing.

[0074] After placing the three-dimensional atom probe sample 200 in the sample workstations 101 of the sample carrier module 1, the sample carrier module 1 is placed in the vacuum-sealed tube 2, the vacuum-sealed tube 2 is evacuated, and then the three-dimensional atom probe sample 200 is subjected to heat treatment. The vacuum-sealed tube 2 is made of a high-temperature-resistant material (such as quartz), and the vacuum-sealed tube 2 can provide a vacuum environment for the three-dimensional atom probe sample 200 in the sample carrier module 1. Further, the temperature of the vacuum environment is controllable through an external heating system. The establishment of the vacuum environment effectively isolates the three-dimensional atom probe sample 200 from the external air, effectively preventing the sample from oxidizing, and provides a clean and stable heat treatment condition for the three-dimensional atom probe sample 200.

[0075] After heat treatment, the heat-treated vacuum-sealed tube 2 is placed in the sealed tube workstation 302 of the cooling module 3, and the three-dimensional atom probe sample 200 is cooled by a cooling liquid. The cooling chamber 301 in the cooling module 3 can be filled with different types of cooling liquids, such as liquid nitrogen, liquid carbon dioxide, or low-temperature ethanol, to achieve different cooling rates and final temperature control. With the help of the cooling liquid, rapid cooling and long-term low-temperature maintenance can be achieved, avoiding the composition segregation or phase change problems caused by room temperature parking effects. During the cooling process, the three-dimensional atom probe sample 200 is always in a vacuum-sealed state, effectively preventing the sample from oxidizing. After cooling is completed, the three-dimensional atom probe sample 200 is removed from the sample carrier module 1, and the three-dimensional atom probe sample 200 can be polished and then transferred to the three-dimensional atom probe equipment for characterization.

[0076] The processing device 100 for three-dimensional atom probe samples provided by the embodiments of the present disclosure provides a full-process vacuum protection environment for the three-dimensional atom probe sample 200 in the application of the processing process of the three-dimensional atom probe sample 200. Specifically, after being coarsely polished, the three-dimensional atom probe sample 200 is placed in the vacuum sealed tube 2 to avoid contact with air. Subsequently, the three-dimensional atom probe sample 200 enters the heat treatment process, and precise temperature control is achieved through an external heating system. After the heat treatment is completed, the three-dimensional atom probe sample 200 is transferred to the cooling module 3 together with the vacuum sealed tube 2, and rapid cooling is performed by using a cooling liquid. Since the three-dimensional atom probe sample 200 still remains in the vacuum environment during the entire cooling process, contact with air is further prevented. In the heat treatment and cooling and cooling stages, the three-dimensional atom probe sample 200 is always in a vacuum sealed state, effectively isolating contact with external air, preventing the three-dimensional atom probe sample 200 from undergoing oxidation reaction, and thus helping to shorten the time of the preparation process of the three-dimensional atom probe sample 200. In the cooling and cooling stage, the cooling liquid in the cooling module 3 can rapidly cool and maintain low temperature for a long time, avoiding the composition segregation or phase change problem caused by the room temperature parking effect. Finally, after the cooling is completed, the three-dimensional atom probe sample 200 is taken out from the vacuum sealed tube 2 and subjected to fine polishing, and then is quickly transferred to the three-dimensional atom probe equipment for characterization. Through this full-process vacuum and low-temperature protection mechanism, the accuracy of subsequent material phase change analysis and composition characterization is significantly improved, and it is ensured that the three-dimensional atom probe data can truly reflect the microstructure characteristics of the three-dimensional atom probe sample 200.

[0077] In some embodiments, the sample carrying module 1 is provided with a sample station 101. By providing a plurality of sample stations 101, a plurality of three-dimensional atom probe samples 200 can be processed at the same time. This design improves the throughput and efficiency of the experiment, and is particularly suitable for cases where batch analysis or comparative study is required.

[0078] In some embodiments, the sample station 101 is a mounting hole matched with the fixed copper tube of the three-dimensional atom probe sample 200, and the fixed copper tube of the three-dimensional atom probe sample 200 can be inserted into the mounting hole to realize fixation.

[0079] In some embodiments, the chamber 301 is provided with a plurality of sealed tube stations 302. The plurality of sealed tube stations 302 allow simultaneous processing of a plurality of vacuum sealed tubes 2 (each sealed tube can contain one or more sample carrying modules 1), thereby significantly improving the processing capacity of the samples, which enables the experiment to complete more sample processing tasks in a shorter time.

[0080] In some embodiments, the sealed tube station 302 is a mounting hole matched with the vacuum sealed tube 2, and the vacuum sealed tube 2 can be inserted into the mounting hole to realize fixation.

[0081] In some embodiments, the sample carrying module 1 comprises a sample carrying base 11 and a sample protection cover 12. The sample carrying base 11 is provided with a sample station 101. The sample protection cover 12 is detachably coupled to the sample carrying base 11 to enclose the sample station 101 inside. The sample carrying base 11 and the sample protection cover 12 are designed to be detachably coupled to facilitate the coupling of the sample protection cover 12 to the sample carrying base 11 to form a relatively closed space after the three-dimensional atom probe sample 200 is placed in the sample station 101 of the sample carrying base 11, so as to avoid damage to the three-dimensional atom probe sample 200.

[0082] In some embodiments, the sample protection cover 12 is provided with a through hole 120. The through hole 120 of the sample protection cover 12 can be used for heat exchange between the space, which helps to regulate the heat exchange process of the three-dimensional atom probe sample 200 and helps to accurately complete the heat treatment process.

[0083] In some embodiments, the sample carrying base 11 and the sample protection cover 12 can be detachably coupled by clamping. Alternatively, the sample carrying base 11 and the sample protection cover 12 can be detachably coupled by screwing. Alternatively, the sample carrying base 11 is a cylindrical structure with threads on the outer periphery, and one end surface of the sample carrying base 11 is provided with a sample station 101. The sample protection cover 12 is a cylindrical structure with threads on the inner periphery, and is detachably coupled to the sample carrying base 11 by screwing. By screwing, a fastening connection that can be repeatedly disassembled is formed between the sample carrying base 11 and the sample protection cover 12. The user can complete the installation or separation of the sample carrying base 11 and the sample protection cover 12 by rotating, which facilitates the loading, unloading and equipment cleaning and maintenance of the three-dimensional atom probe sample 200.

[0084] In some embodiments, one end surface of the sample carrying base 11 is provided with a plurality of sample stations 101. By providing a plurality of sample stations 101 on the sample carrying base 11, a plurality of three-dimensional atom probe samples 200 can be processed at the same time. This design improves the throughput and efficiency of the experiment, and is particularly suitable for situations that require batch analysis or comparative study.

[0085] In some embodiments, the plurality of sample stations 101 are uniformly distributed. The uniform distribution of the sample stations 101 is conducive to the uniform conduction and distribution of heat on the carrying base.

[0086] In some embodiments, the sample protection cover 12 comprises a bottom plate 121 and a cylinder 122, at least one of which is provided with a through hole 120. The inner circumferential surface of the cylinder 122 is provided with threads, and the bottom plate 121 is arranged at one end of the cylinder 122, and the other end of the cylinder 122 is open. By arranging the through hole 120 on both the bottom plate 121 and the cylinder 122, the heat in-and-out path in the space formed by the sample protection cover 12 and the sample carrying base 11 can be optimized, which helps to more accurately control the heat exchange process of the three-dimensional atom probe sample 200, so as to accurately complete the heat treatment process.

[0087] In some embodiments, after the sample protection cover 12 and the sample carrying base 11 are connected, the distance between the bottom plate 121 of the sample protection cover 12 and the end face of the sample carrying base 11 where the sample station 101 is arranged is between 10 mm and 20 mm.

[0088] In some embodiments, the bottom plate 121 is provided with a plurality of through holes 120, which are uniformly distributed. For example, the bottom plate 121 is provided with three through holes 120, which are uniformly distributed around the center of the bottom plate 121. The diameter of the through hole 120 arranged on the bottom plate 121 is between 0.5 mm and 2 mm, and the distance between adjacent through holes 120 is between 3 mm and 8 mm.

[0089] In some embodiments, the cylinder 122 is provided with a plurality of through holes 120. Optionally, the plurality of through holes 120 are distributed along the circumferential direction of the cylinder 122. Optionally, the plurality of through holes 120 are distributed along the axial direction of the cylinder 122. The diameter of the through hole 120 arranged on the cylinder 122 is between 0.5 mm and 2 mm, and the distance between adjacent through holes 120 is between 3 mm and 8 mm.

[0090] In some embodiments, the plurality of through holes 120 of the cylinder 122 are uniformly distributed along the circumferential direction of the cylinder 122. Alternatively, the plurality of through holes 120 of the cylinder 122 are uniformly distributed along the axial direction of the cylinder 122.

[0091] In some embodiments, the cooling module 3 comprises a cover 31, a shell 32 and a sealed tube carrying seat 33. The shell 32 is provided with a chamber 301 for containing cooling liquid and has an open end. The cover 31 is detachably arranged at the open end of the shell 32. The sealed tube carrying seat 33 is located inside the chamber 301 and is provided with a sealed tube station 302. The shell 32 cooperates with the detachable cover 31 to form a relatively closed chamber 301. This not only facilitates the convenient taking and placing of the vacuum sealed tube 2 in the sealed tube station 302, but also avoids the waste caused by the volatilization of the cooling liquid, so that the low-temperature environment in the chamber 301 can be maintained for a long time.

[0092] In some embodiments, the outer wall of the shell 32 is a vacuum sandwich structure. The vacuum sandwich structure can reduce heat conduction and convection between the inside and outside of the shell 32 by means of vacuumization, thereby achieving a better heat insulation effect, which helps to maintain a low-temperature environment in the chamber 301 for a long time.

[0093] In some embodiments, the outer wall of the shell 32 is provided with a heat insulation material (not shown in the figure). For example, the heat insulation material can be a composite structure layer composed of polyurethane material and ceramic fiber, which has a heat insulation function. By providing the heat insulation material on the outer wall, heat conduction and convection between the inside and outside of the shell 32 can be reduced, thereby achieving a better heat insulation effect, which helps to maintain a low-temperature environment in the chamber 301 for a long time.

[0094] In some embodiments, the outer wall of the shell 32 is a vacuum sandwich structure, and the sandwich is filled with a heat insulation material. The vacuum sandwich can significantly eliminate heat conduction and convection by means of vacuumization to reduce gas molecules, and the heat insulation material further blocks the remaining trace heat conduction and radiation heat transfer. The combination of the double heat insulation mechanisms of the vacuum sandwich and the heat insulation material greatly reduces the heat conduction and convection between the inside and outside of the shell 32, thereby achieving a better heat insulation effect, which helps to maintain a low-temperature environment in the chamber 301 for a long time.

[0095] In some embodiments, the sealed tube carrier 33 is provided with a plurality of sealed tube stations 302. The plurality of sealed tube stations 302 allows simultaneous processing of a plurality of vacuum sealed tubes 2 (each sealed tube can hold one or more sample carrier modules 1), thereby significantly improving the processing capacity of the samples, which enables more sample processing tasks to be completed in a shorter time.

[0096] In some embodiments, the plurality of sealed tube stations 302 are uniformly distributed. The uniform distribution of the sealed tube stations 302 helps to form a more uniform temperature field in the entire chamber 301, so that all three-dimensional atom probe samples 200 experience similar cooling processes.

[0097] In some embodiments, the sealed tube carrier 33 is a cylindrical structure, one end of the sealed tube carrier 33 is connected to the bottom of the shell 32, and the other end of the sealed tube carrier 33 is provided with a plurality of sealed tube stations 302, which are uniformly distributed along the circumference of the sealed tube carrier 33. The cylindrical structure of the sealed tube carrier 33 is in contact with the cooling liquid on the inside and outside in the working state, so that the sealed tube stations 302 arranged thereon can receive cooling action from multiple directions. This structure is conducive to improving the heat exchange uniformity of the vacuum sealed tube 2 during the cooling process, thereby improving the temperature consistency of the three-dimensional atom probe sample 200 inside the vacuum sealed tube 2.

[0098] The inside of the vacuum sealed tube 2 is a near-vacuum environment, which inhibits heat conduction and heat convection in the gas medium, but also retains the heat exchange paths of heat radiation and through solid contact. Although the vacuum environment can relatively reduce the overall cooling rate of the three-dimensional atom probe sample 200, due to the lack of gas flow and the effect of rapid heat dissipation, it helps to avoid uneven cooling caused by temperature gradient differences, thereby improving the uniformity of the temperature distribution inside the three-dimensional atom probe sample 200. More importantly, the vacuum environment can effectively prevent the three-dimensional atom probe sample 200 from being oxidized and contaminated during heating or cooling.

[0099] In some embodiments, an air extraction valve (not shown in the figure) can be arranged on the cover 31 of the cooling module 3, which can be used to adjust the air pressure in the chamber 301, so as to optimize the flow state and heat exchange efficiency of the cooling liquid, and further improve the cooling rate and temperature control accuracy of the sample.

[0100] The embodiments of the present disclosure provide a processing method for a three-dimensional atom probe sample, which is combined with the processing device 100 for a three-dimensional atom probe sample provided in the above embodiments. Figure 8 It is shown that the processing method is implemented based on the processing device 100 for a three-dimensional atom probe sample provided in the above embodiments, and the processing method comprises the following steps:

[0101] S801, placing the three-dimensional atom probe sample 200 after rough polishing in the sample work station 101 of the sample carrying module 1.

[0102] In some embodiments, the three-dimensional atom probe sample 200 is first soaked in a rough polishing etching liquid for rough polishing, and after the rough polishing is completed, the three-dimensional atom probe sample 200 is placed in the sample work station 101 of the sample carrying module 1.

[0103] In some embodiments, the three-dimensional atom probe sample 200 after rough polishing is placed in the sample work station 101 of the sample carrying base 11, and then the sample protection cover 12 is buckled on the sample carrying base 11 to form a complete sample carrying module 1.

[0104] S802, placing the sample carrying module 1 in the vacuum sealed tube 2, vacuumizing the vacuum sealed tube 2, and then performing heat treatment on the three-dimensional atom probe sample 200.

[0105] In some embodiments, during the heat treatment of the three-dimensional atom probe sample 200, the temperature of the heat treatment is not less than 300°C, the time length of the heat treatment is not less than 10 min, and the vacuum degree in the vacuum sealed tube 2 is not higher than 1x10 -2 Pa. Optionally, the temperature of the heat treatment is 300°C to 1200°C, the time length of the heat treatment is 10 min to 24 h, and the vacuum degree in the vacuum sealed tube 2 is 1x10 -2 Pa to 1x10 -4 Pa.

[0106] S803, the vacuum sealed tube 2 after heat treatment is placed in the sealed tube station 302 of the cooling module 3, and the three-dimensional atom probe sample 200 is cooled by the cooling liquid.

[0107] In some embodiments, the temperature reached by the cooling module 3 is -196℃ to -50℃.

[0108] In some embodiments, the cooling rate of the cooling process of the three-dimensional atom probe sample 200 is not less than 10℃ / s, and the temperature of the three-dimensional atom probe sample 200 after cooling is not higher than -50℃. Alternatively, the cooling rate of the cooling process of the three-dimensional atom probe sample 200 is 10℃ / s to 100℃ / s.

[0109] S804, after the cooling is completed, the three-dimensional atom probe sample 200 is taken out of the sample carrying module 1.

[0110] In some embodiments, after the three-dimensional atom probe sample 200 is taken out, the three-dimensional atom probe sample 200 can be finely polished and then transferred to the three-dimensional atom probe device for characterization.

[0111] In some embodiments, when the temperature of the three-dimensional atom probe sample 200 is not higher than -50℃, the three-dimensional atom probe sample 200 is taken out of the sample carrying module 1 and soaked in a fine polishing etching liquid for fine polishing. After the fine polishing is completed, the three-dimensional atom probe sample 200 is transferred to the three-dimensional atom probe device for characterization.

[0112] In some embodiments, the fine polishing time of the three-dimensional atom probe sample 200 should be controlled within 300s. The time from the end of fine polishing of the three-dimensional atom probe sample 200 to the transfer to the three-dimensional atom probe device should be controlled within 60s.

[0113] In the embodiments of the present disclosure, the three-dimensional atom probe sample 200 is first coarsely polished, and then placed in the sample carrying module 1 and placed in the vacuum sealed tube 2. In the subsequent heat treatment stage and cooling stage, the three-dimensional atom probe sample 200 does not need to be taken out of the vacuum sealed tube 2, and the three-dimensional atom probe sample 200 is always in a vacuum sealed state, thereby effectively isolating the three-dimensional atom probe sample 200 from the outside air, effectively preventing the sample from oxidizing, and helping to shorten the sample preparation process time.

[0114] Taking the Al-Mg-Si alloy as an example, the three-dimensional atom probe sample 200 is immersed in a rough polishing etching liquid for rough polishing. After the rough polishing is completed, the three-dimensional atom probe sample 200 is placed on the sample station 101 of the sample carrying base 11, and then the sample protection cover 12 is buckled on the sample carrying base 11 to form a complete sample carrying module 1. Here, the rough polishing etching liquid is a solution formed by 10% perchloric acid and 90% glacial acetic acid, and the etching voltage of the rough polishing process is 8V.

[0115] Subsequently, the sample carrying module 1 is placed in the vacuum sealed tube 2, the vacuum sealed tube 2 is vacuumized, and then the three-dimensional atom probe sample 200 is heat treated. During the heat treatment of the three-dimensional atom probe sample 200, the heat treatment temperature is 525℃, the heat treatment time is 4h, and the vacuum degree in the vacuum sealed tube 2 is 5×10 -3 Pa.

[0116] Then, the vacuum sealed tube 2 after the heat treatment is placed in the sealed tube station 302 of the cooling module 3, and the three-dimensional atom probe sample 200 is cooled by using a cooling liquid. The temperature of the cooling liquid is -196℃, the cooling rate of the three-dimensional atom probe sample 200 is 80℃ / s, and the three-dimensional atom probe sample 200 is maintained at not higher than -50℃ for 30min.

[0117] After the cooling of the three-dimensional atom probe sample 200 is completed, the three-dimensional atom probe sample 200 is taken out from the sample carrying module 1, and the three-dimensional atom probe sample 200 is immersed in a fine polishing etching liquid for fine polishing. After the fine polishing is completed, the three-dimensional atom probe sample 200 is transferred to a three-dimensional atom probe device for characterization within 60s. Here, the fine polishing etching liquid is a solution formed by 4% perchloric acid and 96% ethylene glycol butyl ether, the etching voltage of the fine polishing process is 5V, and the fine polishing time is 250s.

[0118] The processing device 100 and the processing method provided by the embodiments of the present disclosure for the three-dimensional atom probe sample can also be applied to other samples that need to undergo heat treatment and cooling, such as semiconductor material samples, ceramic material samples, optical material samples, etc.

[0119] The apparatus embodiments described above are only exemplary, for example, the division of the units can be only a logical function division, and actual implementation can have another division mode, for example, multiple units or components can be combined or integrated into another system, or some features can be ignored or not executed. In addition, the coupling or direct coupling or communication connection between the units shown or discussed can be indirect coupling or communication connection through some interfaces, devices or units, and can be electrical, mechanical or other forms. The units described as separate components can or can not be physically separated, and the components shown as units can or can not be physical units, that is, they can be located in one place, or can be distributed on multiple network units. Part or all of the units can be selected to implement the embodiments according to actual needs. In addition, the function units in the embodiments of the present disclosure can be integrated in one processing unit, or each unit can be physically present separately, or two or more units can be integrated in one unit.

Claims

1. A processing apparatus for three-dimensional atomic probe samples, characterized in that, include: The sample carrier module is equipped with sample stations, each of which is used to place a three-dimensional atom probe sample. Vacuum-sealed tube for housing the sample carrier module; The cooling module is equipped with a chamber for containing coolant, and the chamber is equipped with a sealing tube station for placing a vacuum sealing tube.

2. The processing apparatus according to claim 1, characterized in that, The sample carrier module includes: The sample support base is equipped with a sample station. The sample protective cover is detachably attached to the sample carrier base to hold the sample inside.

3. The processing apparatus according to claim 1, characterized in that, The sample protective cover has through holes.

4. The processing apparatus according to claim 2, characterized in that, The sample support base is a cylindrical structure with threads on its outer circumference, and a sample station is provided on one end face of the sample support base; The sample protective cover is a cylindrical structure with threads on its inner circumference, which is fastened to the sample support base by means of threaded connection.

5. The processing apparatus according to claim 3, characterized in that, Multiple sample stations are set on one end face of the sample support base.

6. The processing apparatus according to claim 3, characterized in that, The sample protective cover includes: Base plate; The cylinder has threads on its inner circumferential surface, a bottom plate at one end, and an opening at the other end. At least one of the bottom plate and the cylinder is provided with a through hole.

7. The processing apparatus according to claim 5, characterized in that, The base plate has multiple through holes.

8. The processing apparatus according to claim 5, characterized in that, The cylinder is provided with multiple through holes, which are distributed along the circumference and / or axial direction of the cylinder.

9. The processing apparatus according to claim 8, characterized in that, Multiple through holes in the cylinder are distributed along the circumferential and / or axial direction of the cylinder.

10. The processing apparatus according to any one of claims 1 to 9, characterized in that, The cooling module includes: The housing has a chamber for containing coolant and has an opening; The cover is detachably attached to the opening of the housing; The sealing tube support is located inside the chamber and has a sealing tube station.

11. The processing apparatus according to claim 10, characterized in that, The outer wall of the shell is a vacuum sandwich structure, and / or the outer wall of the shell is provided with heat insulation material.

12. The processing apparatus according to claim 10, characterized in that, The sealing tube support is equipped with multiple sealing tube stations.

13. The processing apparatus according to claim 10, characterized in that, The sealing tube support is a cylindrical structure. One end face of the sealing tube support is connected to the bottom of the shell, and the other end face of the sealing tube support is provided with multiple sealing tube stations.

14. A method for processing three-dimensional atomic probe samples, characterized in that, Based on the processing apparatus for three-dimensional atomic probe samples as described in any one of claims 1 to 13, comprising: The rough polished 3D atomic probe sample is placed in the sample station of the sample carrier module; The sample carrier module is placed in a vacuum-sealed tube, the vacuum-sealed tube is evacuated, and then the three-dimensional atomic probe sample is heat-treated. The heat-treated vacuum-sealed tube is placed in the sealing tube station of the cooling module, and the three-dimensional atomic probe sample is cooled by the coolant. After cooling is complete, the three-dimensional atom probe sample is removed from the sample carrier module.

15. The processing method according to claim 14, characterized in that, The parameter requirements for the thermal treatment process of three-dimensional atom probe samples include at least one of the following: The heat treatment temperature shall not be lower than 300℃; The heat treatment time shall not be less than 10 minutes; The vacuum level in the vacuum-sealed tube is no higher than 1×10⁻⁶. -2 Pa.

16. The processing method according to claim 14, characterized in that, The parameter requirements for the cooling process of three-dimensional atom probe samples include at least one of the following: Cooling rate not less than 10℃ / s; The temperature of the three-dimensional atom probe sample after cooling should not exceed -50℃.

Images