Heat treatment apparatus and rapid quenching method

Abstract

The application provides a heat treatment device and a rapid quenching method, and relates to the field of heat treatment. The heat treatment device comprises a heat-conducting sample chamber, a heating mechanism and a gas conveying mechanism. The heat-conducting sample chamber has a containing cavity in an open state and a closed state. The heating mechanism is arranged around the periphery of the heat-conducting sample chamber. The gas conveying mechanism is located outside the heat-conducting sample chamber. The gas conveying mechanism comprises a gas conveying pipe and a gas source. The gas source is used for providing low-temperature inert gas. The gas inlet end of the gas conveying pipe is in communication with the gas source. The end face of the gas conveying end of the gas conveying pipe abuts against the outer wall of the heat-conducting sample chamber. The side wall of the gas conveying end is provided with a plurality of gas outlet channels which are arranged at intervals in the circumferential direction. The structure is simple, convenient to assemble and disassemble, rapid quenching of micro-nano scale samples can be realized, and the introduction of impurities is avoided.

Description

Technical Field

[0001] This application relates to the field of heat treatment, and more specifically, to a heat treatment apparatus and a rapid quenching method. Background Technology

[0002] Heat treatment is a thermal processing technology that uses heating, holding, and cooling methods to obtain the desired structure and properties of materials in a solid state. It typically includes annealing, normalizing, quenching, and tempering. These four processes can be combined in a reasonable way to create different heat treatment processes, enabling the treated materials to obtain different strengths and toughnesses, thereby eliminating structural defects and improving material properties.

[0003] Quenching refers to heating a material to a specified temperature, holding it at that temperature for a period of time, and then immersing it in a quenching medium to rapidly cool it down.

[0004] Currently, heat treatment equipment for rapid quenching has a relatively complex structure. It typically requires a rotating mechanism to ensure full contact between the sample and the quenching agent, as well as a recycling chamber to recover the quenching agent. This results in a large space requirement and increased energy consumption. Existing technologies for heat treatment of micro / nano-scale samples often involve placing them in a copper crucible, heating them to a high temperature in a vacuum environment, maintaining that temperature for a period, and then allowing them to cool slowly naturally in the furnace or by introducing cooling media such as water / oil for rapid cooling. Furnace cooling leads to long experiment times and low efficiency. While using cooling media like water / oil for rapid cooling can cause reactions between the sample and the cooling medium, introducing impurities that affect sample performance, and can also cause the sample to detach from the carrier due to the impact of the cooling medium. Furthermore, water / oil cooling media have low maximum cooling rates, resulting in slow cooling and poor cooling effects. Summary of the Invention

[0005] The purpose of this application is to provide a heat treatment apparatus and a rapid quenching method, which can improve at least one of the above-mentioned technical problems.

[0006] In a first aspect, embodiments of this application provide a heat treatment apparatus, which includes a thermally conductive sample chamber, a heating mechanism, and a gas delivery mechanism.

[0007] The thermally conductive sample chamber has a accommodating cavity for containing micro-nano-scale samples, which has an open state and a closed state. The heating mechanism is located around the thermally conductive sample chamber and is used to heat the thermally conductive sample chamber. The gas delivery mechanism is located outside the thermally conductive sample chamber and includes a gas delivery pipe and a gas source. The gas source is used to provide low-temperature inert gas with a temperature not exceeding 10°C. The inlet end of the gas delivery pipe is connected to the gas source, and the end face of the gas delivery end of the gas delivery pipe abuts against the outer wall of the thermally conductive sample chamber. The side wall of the gas delivery end has multiple gas outlet channels arranged at intervals along its circumference.

[0008] In the above-described process, since the micro / nano-scale sample is housed within the containment cavity while the gas delivery mechanism is located outside the heat-conducting sample chamber, the impact of airflow on the micro / nano-scale sample and the exchange of matter with the low-temperature inert gas during cooling are avoided, preventing the introduction of impurities and ensuring the quality of the micro / nano-scale sample. Utilizing the low-temperature inert gas for heat exchange with the heat-conducting sample chamber allows for rapid cooling, with a cooling rate reaching 1000 K / s, achieving rapid quenching, improving quenching efficiency, and resulting in nano / micro-scale samples with intact structure and good performance after quenching. The entire heat treatment device has a simple structure, is easy to install and disassemble, and is highly practical, effectively improving experimental efficiency.

[0009] In one possible implementation, the air outlet channel is a notch formed on the end face of the air supply end, and the total cross-sectional area of ​​the notch accounts for 12.73%-66.71% of the total cross-sectional area of ​​the air supply end.

[0010] In one possible implementation, the inner wall diameter of the gas delivery end is 4 mm, and the depth of the notch in the gas delivery direction of the gas delivery end is 1-5 mm.

[0011] In one possible implementation, the gas source is configured to output a cryogenic inert gas flow rate of 10 m / s to 20 m / s.

[0012] In one possible implementation, the thermally conductive sample chamber includes: a thermally conductive support and a thermally conductive crucible, the thermally conductive support having a support surface for supporting micro-nano-scale samples; the thermally conductive crucible is detachably upside down on the support surface, and the thermally conductive crucible and the support surface together form a receiving cavity.

[0013] In one possible implementation, the thermally conductive sample chamber includes: a thermally conductive connector, which has a receiving groove, an air inlet channel, and a limiting groove connected sequentially along its axial direction, the diameters of the receiving groove and the limiting groove being larger than the diameter of the air inlet channel; a thermally conductive support member is detachably embedded in the receiving groove and closes one end of the air inlet channel near the receiving groove, the support surface being located on the side of the thermally conductive support member away from the limiting groove; a thermally conductive crucible is detachably inverted in the receiving groove and the open end of the thermally conductive crucible is closed by the support surface; and a gas supply pipe includes a first gas supply pipe and a second gas supply pipe, the end face of the gas delivery end of the first gas supply pipe is used to restrict the movement of the thermally conductive crucible along the axial direction of the thermally conductive connector, a first gas outlet gap is formed between the side wall of the first gas supply pipe and the side wall of the receiving groove, the end face of the gas delivery end of the second gas supply pipe abuts against the limiting groove, and a second gas outlet gap is formed between the side wall of the second gas supply pipe and the limiting groove.

[0014] In one possible implementation, the thermally conductive sample chamber further includes: a ceramic pressure ring, which is detachably embedded in the receiving groove and pressed against the bearing surface; a thermally conductive crucible is detachably upside down inside the inner ring surface of the ceramic pressure ring; in the axial direction of the thermally conductive joint, the height of the ceramic pressure ring is lower than the depth of the receiving groove; and the end face of the gas delivery end of the first gas delivery pipe abuts against the ceramic pressure ring.

[0015] In one possible implementation, the gas delivery mechanism includes a connecting pipe and a gas flow meter, wherein the gas source is connected to the gas delivery pipe via the connecting pipe, and the gas flow meter is mounted on the connecting pipe.

[0016] In one possible implementation, the heat treatment apparatus further includes: a temperature measuring mechanism and a controller. The temperature measuring mechanism is located inside the gas supply pipe, and the temperature measuring point of the temperature measuring mechanism is in contact with the outer wall of the heat-conducting sample chamber. The controller is electrically connected to both the heating mechanism and the temperature measuring mechanism. The controller is used to receive temperature data fed back by the temperature measuring mechanism and can control the working state of the heating mechanism according to the temperature data.

[0017] Secondly, embodiments of this application provide a rapid quenching method using the above-described heat treatment apparatus, comprising the following steps:

[0018] The micro-nano-scale sample is carried on a carrier and then placed together in the accommodating cavity and the accommodating cavity is sealed. The heat treatment device is placed in a vacuum chamber, and the vacuum chamber is evacuated to the target vacuum level. Then, the heating mechanism is started to heat the heat-conducting sample chamber to the target temperature and hold it at that temperature for a preset time. Then, the heating is stopped, and the gas delivery mechanism is started to deliver low-temperature inert gas to the outer wall of the heat-conducting sample chamber to rapidly cool down the micro-nano-scale sample. Attached Figure Description

[0019] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1 A schematic diagram of the heat treatment apparatus provided in this application;

[0021] Figure 2 A cross-sectional structural schematic diagram of the heat treatment apparatus provided in this application;

[0022] Figure 3 This is a schematic diagram of the assembly of the thermally conductive sample chamber with the first gas delivery pipe and the second gas delivery pipe;

[0023] Figure 4 A schematic diagram of the structure of the first gas transmission pipe provided in this application;

[0024] Figure 5 This is a schematic diagram of the structure of the second gas pipeline provided in this application;

[0025] Figure 6 A comparison chart of cooling rates for furnace cooling and the rapid quenching method provided in Example 1;

[0026] Figure 7 A schematic diagram showing the relationship between notch depth and cooling rate for the experimental example;

[0027] Figure 8 A schematic diagram showing the relationship between the ventilation cross-section ratio and the cooling rate for the experimental example;

[0028] Figure 9 A schematic diagram showing the relationship between the flow rate and cooling rate of the cryogenic inert gas provided for the experimental example.

[0029] Icons: 1000 - Heat treatment device; 10 - Thermally conductive sample chamber; 100 - Receptacle; 110 - Thermally conductive support component; 111 - Support surface; 120 - Thermally conductive crucible; 130 - Thermally conductive joint; 133 - Gas inlet channel; 140 - Ceramic pressure ring; 20 - Gas delivery mechanism; 200 - Gas source; 211 - Gas outlet channel; 220 - First gas delivery pipe; 230 - First three-way valve; 240 - Second gas delivery pipe; 250 - Second three-way valve Valve; 260-Connecting pipe; 270-Gas flow meter; 281-First gas outlet gap; 283-Second gas outlet gap; 30-Heating mechanism; 300-Heating furnace body; 310-Molybdenum heating belt; 320-Molybdenum conductive connector; 330-Ceramic block; 40-Temperature measuring mechanism; 50-Bracket; 500-Top plate; 510-Bottom plate; 520-Support screw; 530-Chassis; 540-Hollow support rod; 550-Fixing component. Detailed Implementation

[0030] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. The components of the embodiments of this application described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0031] Therefore, the following detailed description of the embodiments of this application provided in the accompanying drawings is not intended to limit the scope of the claimed application, but merely to illustrate selected embodiments of the application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0032] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0033] In the description of this application, it should be noted that the terms "upper," "lower," "inner," and "outer," etc., indicate the orientation or positional relationship based on the accompanying drawings, or the orientation or positional relationship commonly used when the product is in use. They are used only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on this application. In addition, the terms "first," "second," etc., are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0034] In the description of this application, it should also be noted that, unless otherwise expressly specified and limited, the terms "set up," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.

[0035] This application provides a heat treatment apparatus, which is particularly suitable for quenching micro-nano-scale samples.

[0036] Among them, micro-nano-level samples refer to samples with macroscopic dimensions of micrometers (e.g., ≤600μm) or nanometers used in the quenching heat treatment. Micro-nano-level samples include, but are not limited to, lunar soil tissue (referred to as lunar soil). It can be understood that lunar soil is usually placed on a carrier (e.g., a mesh platform), and then the two are placed as a whole in the heat treatment device 1000 for quenching treatment.

[0037] Please see Figures 1 to 3 The heat treatment device 1000 mainly includes a heat-conducting sample chamber 10, a heating mechanism 30, and a gas delivery mechanism 20.

[0038] The thermally conductive sample chamber 10 has a accommodating cavity 100 for accommodating micro-nano-level samples, and the accommodating cavity 100 has an open state and a closed state; the heating mechanism 30 is arranged around the outer periphery of the thermally conductive sample chamber 10 and is used to heat the thermally conductive sample chamber 10; the gas delivery mechanism 20 is located outside the thermally conductive sample chamber 10, and the gas delivery mechanism 20 includes a gas delivery pipe and a gas source 200. The gas source 200 is used to provide a low-temperature inert gas with a temperature not higher than 10°C. The gas inlet end of the gas delivery pipe is connected to the gas source 200, and the end face of the gas delivery end of the gas delivery pipe abuts against the outer wall of the thermally conductive sample chamber 10. The side wall of the gas delivery end is provided with a plurality of gas outlet channels 211 arranged at intervals along its circumference.

[0039] The accommodating cavity 100 has an open state and a closed state, meaning that the accommodating cavity 100 can be opened to facilitate the placement of micro-nano-level samples into or out of the accommodating cavity 100, and the accommodating cavity 100 can be closed to prevent low-temperature inert gas from entering the accommodating cavity 100 during cooling.

[0040] Low-temperature inert gas refers to an inert gas with a temperature not higher than 10°C and in a gaseous state, including but not limited to at least one of argon and nitrogen. In order to improve the cooling rate, the low-temperature inert gas can be a mixture of argon and liquid nitrogen. Using low-temperature inert gas as a cooling gas can extend the service life of the thermally conductive sample chamber 10.

[0041] It is understandable that the end face of the gas supply end of the gas supply pipe abuts against the outer wall of the heat-conducting sample chamber 10 to supply low-temperature inert gas to the heat-conducting sample chamber 10. The side wall of the gas supply end is provided with multiple gas outlet channels 211 arranged at intervals along its circumference. That is, the gas supply direction of the gas supply end and the gas outlet direction of the gas outlet channel 211 intersect, which is conducive to the low-temperature inert gas fully contacting the heat-conducting sample chamber 10 and improving the cooling rate. When the gas supply pipe is a straight pipe, the gas supply direction is parallel to the axial direction of the gas supply pipe.

[0042] Understandably, since the end face of the gas delivery pipe abuts against the outer wall of the thermally conductive sample chamber 10, the gas delivery pipe is a rigid gas delivery pipe, which is made of a material that is not easily deformed and has a certain degree of hardness. In order to prevent the end face of the gas delivery pipe from abutting against the outer wall of the thermally conductive sample chamber 10 without deformation and to generate a certain supporting force, the hardness of the gas delivery pipe material should be slightly higher than the hardness of the thermally conductive sample chamber 10. For example, if the material of the thermally conductive sample chamber 10 is copper, the hardness of the gas delivery pipe should be slightly higher than that of copper, for example, its Vickers hardness is 340 MPa.

[0043] The heat treatment apparatus 1000 provided in this application, because the micro / nano-scale sample is housed within the accommodating cavity 100 while the gas delivery mechanism 20 is located outside the thermally conductive sample chamber 10, avoids the micro / nano-scale sample being impacted by airflow and exchanging matter with the low-temperature inert gas during cooling, thus preventing the introduction of impurities and ensuring the quality of the micro / nano-scale sample. Utilizing the low-temperature inert gas for heat exchange with the thermally conductive sample chamber 10 allows for rapid cooling, with a quenching cooling rate reaching 1000 K / s, achieving rapid quenching, improving quenching efficiency, and ensuring that the quenched nano / micro-scale sample maintains its structural integrity and good performance. The entire heat treatment apparatus 1000 has a simple structure, is easy to install and disassemble, has high practicality, and can effectively improve experimental efficiency.

[0044] The number of gas supply pipes can be one or more, such as two or three.

[0045] The air outlet channel 211 can be a through hole, a notch on the end face of the air supply end, or both a through hole and a notch.

[0046] Please see Figure 4 as well as Figure 5 In some optional embodiments, the air outlet channel 211 is a notch formed on the end face of the air supply end, and the total cross-sectional area of ​​the notch accounts for 12.73%-66.71% of the total cross-sectional area of ​​the air supply end.

[0047] Cross section refers to the section perpendicular to the gas delivery direction.

[0048] Within the above range, the cooling rate is good. When the total cross-sectional area of ​​the notch is too small compared to the total cross-sectional area of ​​the gas delivery end, the cooling airflow is insufficient to pass through the notch completely. Some of the high-temperature gas after heat exchange remains in the internal cavity of the gas delivery end or generates backflow, reducing the cooling effect of the airflow. When the total cross-sectional area of ​​the notch is too large compared to the total cross-sectional area of ​​the gas delivery end, some of the cooling airflow flows out directly from the notch without effectively contacting the heat-conducting sample chamber 10, reducing the cooling effect of the airflow.

[0049] Optionally, the total cross-sectional area of ​​the notch accounts for 35%-66.71% of the total cross-sectional area of ​​the air supply end.

[0050] In some alternative embodiments, the inner wall diameter of the gas delivery end is 4 mm, and the depth of the notch in the gas delivery direction of the gas delivery end is 1-5 mm.

[0051] Within the above range, the cooling rate is excellent, reaching 900K / s or higher.

[0052] Optionally, the depth of the notch in the gas delivery direction at the gas delivery end is 2-5 mm, and can be 3 mm.

[0053] Within the aforementioned range, the cooling rate can reach 1000 K / s or higher. When the notch depth is around 3 mm, the cooling rate reaches its peak. This may be because when the notch is less than 3 mm, the cooling airflow cannot pass through the notch completely, resulting in backflow inside the air supply end and reducing the cooling effect of the airflow. When the notch is greater than 3 mm, some of the cooling airflow is lost into the environment without contacting the thermally conductive sample chamber 10, which reduces the airflow in contact with the thermally conductive sample chamber 10 and reduces the cooling effect.

[0054] Gas source 200 includes, but is not limited to, gas cylinders or gas tanks.

[0055] In some alternative embodiments, the gas source 200 is configured to output a cryogenic inert gas at a flow rate of 10 m / s to 20 m / s.

[0056] The faster the flow rate of the low-temperature inert gas, the greater the cooling rate. Taking a safety factor of 1.1 as an example, the slope of the cooling curve is the highest and the increase in cooling rate is the greatest in the range of 10m / s-20m / s, which effectively saves gas consumption while taking into account the experimental effect.

[0057] Optionally, the gas source 200 is configured to output a cryogenic inert gas flow rate of 16.8 m / s.

[0058] In some alternative embodiments, please refer to Figure 1 The gas delivery mechanism 20 includes a connecting pipe 260 and a gas flow meter 270. The gas source 200 is connected to the gas delivery pipe through the connecting pipe 260, and the gas flow meter 270 is installed on the connecting pipe 260.

[0059] In other words, the actual flow rate of the output low-temperature inert gas can be directly obtained using the gas flow meter 270, so as to adjust it to the required flow rate and thus adjust the cooling rate of the sample.

[0060] In some alternative embodiments, please refer to Figure 2 The heat treatment apparatus 1000 also includes a temperature measuring mechanism 40 and a controller (not shown).

[0061] The temperature measuring mechanism 40 is located inside the gas supply pipe, and the temperature measuring point of the temperature measuring mechanism 40 is in contact with the outer wall of the heat-conducting sample chamber 10. The controller is electrically connected to the heating mechanism 30 and the temperature measuring mechanism 40 respectively. The controller is used to receive the temperature data fed back by the temperature measuring mechanism 40, and the controller can control the working state of the heating mechanism 30 according to the temperature data.

[0062] By utilizing the temperature measuring mechanism 40 and the controller, temperature self-regulation can be achieved during heating, which is also beneficial for obtaining temperature changes during cooling.

[0063] For example, the temperature measuring mechanism 40 is a thermocouple.

[0064] The controller can be connected to an external computer to allow direct input of control parameters or intuitive display of temperature data.

[0065] In some alternative embodiments, please refer to Figure 2 as well as Figure 3 The thermally conductive sample chamber 10 includes a thermally conductive support 110 and a thermally conductive crucible 120. The thermally conductive support 110 has a support surface 111 for supporting micro-nano-scale samples. The thermally conductive crucible 120 is detachably upside down on the support surface 111, and the thermally conductive crucible 120 and the support surface 111 together form a receiving cavity 100.

[0066] The above-mentioned structure is simple and easy to open and close the accommodating cavity 100, enabling rapid loading and unloading of micro-nano level samples.

[0067] The heat-conducting bearing 110 is plate-shaped and can be a circular plate.

[0068] Both the thermally conductive support 110 and the thermally conductive crucible 120 are made of thermally conductive and high-temperature resistant metals, such as copper or molybdenum. Optionally, the thermally conductive support 110 and the thermally conductive crucible 120 are made of the same material.

[0069] In some alternative embodiments, please refer to Figure 3 The thermally conductive sample chamber 10 includes: a thermally conductive connector 130, which has a receiving groove, an air inlet channel 133 and a limiting groove connected sequentially along its axial direction. The diameters of the receiving groove and the limiting groove are both larger than the diameter of the air inlet channel 133. A thermally conductive support member 110 is detachably embedded in the receiving groove and closes one end of the air inlet channel 133 near the receiving groove. The support surface 111 is located on the side of the thermally conductive support member 110 away from the limiting groove. A thermally conductive crucible 120 is detachably inverted in the receiving groove and the open end of the thermally conductive crucible 120 is closed by the support surface 111.

[0070] The heating mechanism 30 is arranged around the outer periphery of the heat-conducting joint 130.

[0071] The gas supply pipe includes a first gas supply pipe 220 and a second gas supply pipe 240. The end face of the gas supply end of the first gas supply pipe 220 is used to restrict the movement of the heat-conducting crucible 120 along the axial direction of the heat-conducting joint 130. A first gas outlet gap 281 is formed between the side wall of the first gas supply pipe 220 and the side wall of the receiving groove. The end face of the gas supply end of the second gas supply pipe 240 abuts against the limiting groove. A second gas outlet gap 283 is formed between the side wall of the second gas supply pipe 240 and the limiting groove.

[0072] With the above configuration, the thermally conductive joint 130 can be used to limit the lateral (lateral refers to the direction perpendicular to the axial direction of the thermally conductive joint 130) displacement of the thermally conductive carrier 110 and the thermally conductive crucible 120. Since the heating mechanism 30 is arranged around the outer periphery of the thermally conductive joint 130, it is beneficial to use the heating mechanism 30 to uniformly heat the thermally conductive carrier 110 and the thermally conductive crucible 120 by heat exchange. Furthermore, the first gas supply pipe 220 and the second gas supply pipe 240 are used to limit the movement of the thermally conductive carrier 110 and the thermally conductive crucible 120 relative to the thermally conductive joint 130 along the axial direction of the thermally conductive joint 130, thereby ensuring the stability of the accommodating cavity 100 and preventing micro-nano-level samples from detaching from the carrier during actual use.

[0073] It is understandable that a first air outlet gap 281 is formed between the side wall of the first air supply pipe 220 and the side wall of the receiving groove, that is, the outer diameter of the first air supply pipe 220 is smaller than the diameter of the receiving groove; a second air outlet gap 283 is formed between the side wall of the second air supply pipe 240 and the limiting groove, that is, the outer diameter of the second air supply pipe 240 is smaller than the diameter of the limiting groove.

[0074] The materials of the heat-conducting joint 130, the heat-conducting carrier 110, and the heat-conducting crucible 120 include, but are not limited to, copper, and may also be molybdenum.

[0075] In some alternative embodiments, please refer to Figure 3 The thermally conductive sample chamber 10 includes: a ceramic pressure ring 140, which is detachably embedded in the receiving groove and pressed onto the bearing surface 111; a thermally conductive crucible 120 is detachably upside down inside the inner ring surface of the ceramic pressure ring 140; in the axial direction of the thermally conductive joint 130, the height of the ceramic pressure ring 140 is lower than the depth of the receiving groove; and the end face of the gas delivery end of the first gas delivery pipe 220 abuts against the ceramic pressure ring 140.

[0076] By introducing the ceramic pressure ring 140, the end face of the gas delivery end of the first gas pipe 220 is held against the ceramic pressure ring 140, which can simultaneously fix the heat-conducting bearing 110 and the heat-conducting crucible 120, preventing the heat-conducting crucible 120 from shifting, and also avoiding the problems of deformation and low cooling efficiency caused by directly pressing the entire heat-conducting crucible 120.

[0077] In some alternative embodiments, the height of the ceramic pressure ring 140 in the axial direction of the thermally conductive joint 130 may be the same as the height of the thermally conductive crucible 120.

[0078] In some alternative embodiments, the height of the ceramic pressure ring 140 is greater than the height of the heat-conducting crucible 120 in the axial direction of the heat-conducting joint 130, and the height difference between the two is less than or equal to 0.3 mm. This arrangement can alleviate the problem of deformation of the heat-conducting crucible 120 caused by the first gas supply pipe 220 being directly pressed against it.

[0079] Optionally, please refer to Figures 1 to 2 The heat treatment apparatus 1000 also includes a support 50, wherein the heat-conducting sample chamber 10, the heating mechanism 30 and the gas supply pipe are detachably mounted on the support 50.

[0080] The bracket 50 includes a top plate 500, a bottom plate 510, a support screw 520, a chassis 530, a hollow support rod 540, and a fastener 550.

[0081] The top plate 500 and the bottom plate 510 are provided with screw holes. The support screws 520 pass through the screw holes to be threadedly connected to the top plate 500 and the bottom plate 510. The top plate 500 and the bottom plate 510 can be rectangular plates. In this case, the top plate 500 and the bottom plate 510 are each provided with 4 screw holes. The 4 screw holes are located at the four corners of the bottom plate 510. The four support screws 520 are installed at the four corners of the top plate 500 and the bottom plate 510.

[0082] The chassis 530 is located between the top plate 500 and the bottom plate 510. The chassis 530 has a support groove for supporting the bottom wall of the heating mechanism 30. One end of the hollow support rod 540 passes through and is fixed to the bottom plate 510, and the other end passes through the chassis 530 but does not protrude from the bottom wall of the support groove. The hollow support rod 540 is used to support the chassis 530. The fixing member 550 is provided on the support screw 520 and is used to connect with the heating mechanism 30 so that the heating mechanism 30 is fixed to the bracket 50.

[0083] One end of the first gas supply pipe 220 abuts against the ceramic pressure ring 140, and the other end passes through the top plate 500 without moving axially and is provided with a first three-way valve 230. The second gas supply pipe 240 is coaxially inserted into the hollow support rod 540. One end of the second gas supply pipe 240 abuts against the limiting groove, and the other end passes through the bottom plate 510 without moving axially and is provided with a second three-way valve 250. The second gas supply pipe 240 suspends the heat-conducting sample chamber 10 above the chassis 530. With the cooperation of the first gas supply pipe 220 and the second gas supply pipe 240, the heat-conducting sample chamber 10 is stably installed on the bracket 50. At this time, one interface of the first three-way valve 230 and the second three-way valve 250, which is coaxial with the gas supply pipe, is used to insert the temperature measuring mechanism 40, and the other interface is used to connect to the gas source 200.

[0084] The heating mechanism 30 includes a heating furnace body 300, multiple molybdenum heating strips 310, a molybdenum conductive connector 320, and a ceramic block 330. The heating furnace body 300 is a hollow cylinder and is fitted around the heat-conducting joint 130. Ventilation holes are provided on the side walls at both ends of the heating furnace body 300. The molybdenum heating strips 310 are disposed inside the heating furnace body 300. Multiple molybdenum heating strips 310 are spaced apart along the circumference of the heating furnace body 300 on the side walls of the heating furnace body 300, and there is a gap between the molybdenum heating strips 310 and the heat-conducting joint 130. The molybdenum conductive connector 320 is fixed to the ceramic block 330 and is connected to the molybdenum heating strips 310 to control the working state of the molybdenum heating strips 310. The ceramic block 330 is connected to the fixing member 550.

[0085] Optionally, the heating furnace body 300 and the heat-conducting joint 130 are arranged coaxially, which is beneficial to ensure that the heat-conducting joint 130 is heated evenly.

[0086] In some optional embodiments, a rapid quenching method using the above-mentioned heat treatment device includes the following steps: carrying a micro-nano-scale sample on a carrier, then placing them together in a receiving cavity 100 and sealing the receiving cavity 100; placing the heat treatment device 1000 in a vacuum chamber; evacuating the vacuum chamber to a target vacuum level; then starting the heating mechanism 30 to heat the heat-conducting sample chamber 10 to a target temperature and holding it at that temperature for a preset time; then stopping the heating; and starting the gas delivery mechanism 20 to deliver a low-temperature inert gas to the outer wall of the heat-conducting sample chamber 10 to rapidly cool the micro-nano-scale sample.

[0087] Example 1

[0088] Please see Figures 1 to 3 The heat treatment device 1000 includes: a support 50, a thermally conductive sample chamber 10, a heating mechanism 30, a temperature measuring mechanism 40, and a controller (not shown).

[0089] The bracket 50 includes a top plate 500, a bottom plate 510, four supporting screws 520, a chassis 530, a hollow support rod 540, and a fastener 550.

[0090] The support screws 520 are threadedly connected to the top plate 500 and the bottom plate 510, respectively, and four support screws 520 are installed at the four corners of the top plate 500 and the bottom plate 510. The chassis 530 is located between the top plate 500 and the bottom plate 510. The chassis 530 is provided with a support groove. One end of the hollow support rod 540 passes through and is fixed to the bottom plate 510, and the other end passes through the chassis 530 with its end face flush with the bottom wall of the support groove. The hollow support rod 540 is used to support the chassis 530. The fastener 550 is provided on the support screws 520.

[0091] Please see Figure 2 as well as Figure 3The thermally conductive sample chamber 10 includes a thermally conductive connector 130, a thermally conductive support 110, a ceramic pressure ring 140, and a thermally conductive crucible 120.

[0092] A copper connector is used as the heat-conducting connector 130. The copper connector has a receiving groove, an air inlet channel 133, and a limiting groove connected sequentially along its axial direction. The diameters of the receiving groove and the limiting groove are both larger than the diameter of the air inlet channel 133. The outer wall diameter of the heat-conducting connector 130 is 10 mm, and its axial length is 10 mm. The side wall diameters of the receiving groove and the limiting groove are 8 mm, and the cross-sections of the receiving groove and the limiting groove are circular. A copper foil disc with a diameter of 8 mm and a thickness of 0.5 mm is used as the heat-conducting bearing 110. A ceramic pressure ring 140 has an outer ring diameter of 8 mm, an inner ring diameter of 5 mm, and a thickness of 2 mm. A thin-film copper crucible with an outer wall diameter of 5 mm, a wall thickness of 0.5 mm, and a height of 2 mm is used as the heat-conducting crucible 120.

[0093] Please see Figure 2 as well as Figure 3 The thermally conductive support 110 is detachably embedded in the receiving groove and closes the end of the air inlet channel 133 near the receiving groove. The thermally conductive support 110 has a support surface 111 for supporting micro-nano-level samples. The support surface 111 is located on the side of the thermally conductive support 110 away from the limiting groove. The ceramic pressure ring 140 is detachably embedded in the receiving groove and pressed on the support surface 111. In the axial direction of the thermally conductive joint 130, the height of the ceramic pressure ring 140 is lower than the depth of the receiving groove. The thermally conductive crucible 120 is detachably upside down in the inner ring surface of the ceramic pressure ring 140, and the open end of the thermally conductive crucible 120 is closed by the support surface 111. The thermally conductive crucible 120 and the support surface 111 together form the receiving cavity 100.

[0094] Please see Figure 1 as well as Figure 2 The heating mechanism 30 includes a heating furnace body 300, multiple molybdenum heating strips 310, a molybdenum conductive connector 320, and a ceramic block 330.

[0095] The heating furnace body 300 is a hollow cylinder. The heating furnace body 300 is coaxially sleeved around the heat-conducting joint 130 and supported in the support groove. The bottom wall of the heating furnace body 300 and the side walls at both ends of the heating furnace body 300 are provided with ventilation holes. The molybdenum heating belt 310 is set inside the heating furnace body 300. Multiple molybdenum heating belts 310 are arranged at intervals along the circumference of the heating furnace body 300 on the side walls of the heating furnace body 300, and there is a gap between the molybdenum heating belt 310 and the heat-conducting joint 130. The molybdenum conductive connector 320 is fixed to the ceramic block 330. The molybdenum conductive connector 320 is connected to the molybdenum heating belt 310 to control the working state of the molybdenum heating belt 310. The ceramic block 330 is connected to the fixing member 550.

[0096] Please see Figures 1 to 3The gas delivery mechanism 20 is located outside the thermally conductive sample chamber 10. The gas delivery mechanism 20 includes a gas source 200, a first gas delivery pipe 220, a second gas delivery pipe 240, a connecting pipe 260, and a gas flow meter 270.

[0097] Gas source 200 is a gas cylinder used to supply argon gas at a temperature of 0°C.

[0098] The first gas supply pipe 220 and the second gas supply pipe 240 are respectively connected to the gas source 200 via the connecting pipe 260. The hardness of the first gas supply pipe 220 and the second gas supply pipe 240 is greater than that of pure copper. The gas flow meter 270 is installed on the connecting pipe 260.

[0099] The first gas supply pipe 220 abuts against the ceramic pressure ring 140 at the gas delivery end, and the gas inlet end passes through the top plate 500 axially without moving and is provided with a first three-way valve 230, which is connected to the connecting pipe 260; the second gas supply pipe 240 is coaxially inserted into the hollow support rod 540, one end of the second gas supply pipe 240 abuts against the limiting groove and suspends the heat-conducting sample chamber 10 above the base plate 530, and the other end passes through the base plate 510 axially without moving and is provided with a second three-way valve 250, which is connected to the connecting pipe 260; a first gas outlet gap 281 is formed between the side wall of the first gas supply pipe 220 and the side wall of the receiving groove, and a second gas outlet gap 283 is formed between the side wall of the second gas supply pipe 240 and the limiting groove.

[0100] Please see Figure 3 as well as Figure 5 The outer wall diameter of the gas supply end of the first gas supply pipe 220 and the gas supply end of the second gas supply pipe 240 is 6mm, and the inner wall diameter is 4mm. Each gas supply end has four notches on its end face that serve as gas outlet channels 211. The four notches are arranged at equal intervals along the circumference of the corresponding gas supply end, and the total cross-sectional area of ​​the four notches accounts for 52.45% of the total cross-sectional area of ​​the gas supply end. The depth of the notches in the gas supply direction of the gas supply end is 3mm.

[0101] Please see Figure 1 as well as Figure 2 The temperature measuring mechanism 40 consists of two thermocouples. One thermocouple is inserted into the first gas supply pipe 220 through the first three-way valve 230 and its measuring point is in contact with the heat-conducting crucible 120. The other thermocouple is inserted into the second gas supply pipe 240 through the second three-way valve 250 and its measuring point is in contact with the heat-conducting carrier 110.

[0102] The controller is electrically connected to the molybdenum conductive connector 320 and the temperature measuring mechanism 40 respectively. The controller is used to receive temperature data fed back by the temperature measuring mechanism 40 and can control the working state of the heating mechanism 30 according to the temperature data.

[0103] Please see Figures 1 to 3 The assembly methods of the heat treatment device 1000 mainly include:

[0104] First, assemble the top plate 500, bottom plate 510, four support screws 520, and hollow support rod 540. Then, insert the base plate 530 into the hollow support rod 540. Next, place the heat-conducting connector 130 at the top of the hollow support rod 540, with the limiting groove facing the hollow support rod 540 and the receiving groove located at the top of the heat-conducting connector 130. Then, place the heat-conducting carrier 110 into the receiving groove of the heat-conducting connector 130 and place the ceramic pressure ring 140 on the heat-conducting carrier 110. Then, place the mesh platform and the lunar soil loaded on it together on the heat-conducting carrier 110. Then, invert the heat-conducting crucible 120 into the inner ring surface of the ceramic pressure ring 140 to cover the mesh platform and the lunar soil loaded on it, forming a closed receiving cavity 100. Next, the heating mechanism 30 is fitted around the heat-conducting joint 130 and its bottom wall is supported on the chassis 530, and it is fixed on the bracket 50 by connecting the ceramic block 330 to the fixing member 550.

[0105] Then, the second gas supply pipe 240 is coaxially inserted into the hollow support rod 540, with the gas delivery end of the second gas supply pipe 240 abutting against the limiting groove, thus suspending the thermally conductive sample chamber 10 above the base plate 530. Next, the first gas supply pipe 220 is axially fixed and inserted into the top plate 500, with the gas delivery end of the first gas supply pipe 220 abutting against the ceramic pressure ring 140. Then, a first three-way valve 230 is installed at the gas inlet end of the first gas supply pipe 220, connecting to a connecting pipe 260 through one inlet of the first three-way valve 230, and a thermocouple is inserted into the other inlet, ensuring that the thermocouple's measuring point is in contact with the thermally conductive crucible 120. A second three-way valve 250 is installed at the gas inlet end of the second gas supply pipe 240, connecting to a connecting pipe 260 through one inlet of the second three-way valve 250, and a thermocouple is inserted into the other inlet, ensuring that the thermocouple's measuring point is in contact with the thermally conductive carrier 110.

[0106] The rapid quenching method using the above-mentioned heat treatment apparatus mainly includes:

[0107] The mesh platform and the lunar soil loaded on it were placed together as a sample on the thermally conductive support 110. The rapid quenching device was assembled, placed in the vacuum chamber, and the control circuit was connected. Then, the vacuum pump was started to evacuate the vacuum chamber to a vacuum level of 10. -2 Pa, then restart the heating mechanism 30, heat the sample to 640℃, and then hold the temperature for 10 minutes. Then open the argon gas cylinder, adjust the flow meter pressure to 0.3MPa, the temperature of the low-temperature inert gas to 4℃, and the flow rate of the low-temperature inert gas to 16.8m / s. At the same time as stopping the heating, connect the gas supply line to achieve a rapid cooling process and quickly quench the sample.

[0108] Once the vacuum chamber has cooled to room temperature, remove the rapid quenching device, disassemble the gas delivery mechanism 20 and the thermally conductive sample chamber 10, and open the accommodating cavity 100 to remove the sample.

[0109] Please see Figure 6 Compared to the traditional furnace cooling method, the sample cooling rate is approximately 1-1.5 K / s. However, using the rapid quenching method provided in this embodiment, the sample can be cooled from 640℃ to 400℃ in 0.23s, which means the sample cooling rate is approximately 1043.5 K / s.

[0110] If a faster cooling rate is required for the sample, the gas cylinder pressure can be increased and liquid nitrogen can be added to the argon gas.

[0111] Test case

[0112] By adjusting only the depth of the notch in the heat treatment apparatus 1000 provided in Example 1, and designing notch depths of 1mm, 3mm, and 5mm, it was found that after introducing a cooling gas flow for 0.5s, the highest temperatures of the heat-conducting crucible were 462.93℃ (notch depth 1mm), 383.56℃ (notch depth 3mm), and 409.83℃ (notch depth 5mm), respectively. Figure 7 This is a schematic diagram showing the relationship between notch depth and cooling rate. Figure 7 It can be seen that the cooling rate reaches its peak when the notch depth is around 3mm. Theoretical analysis suggests that when the notch is less than 3mm, the cooling airflow cannot pass through the notch completely, resulting in backflow inside the gas pipe and reducing the cooling effect of the airflow; when the notch is greater than 3mm, some of the cooling airflow is lost into the environment without contacting the heat-conducting crucible, thus reducing the airflow in contact with the heat-conducting crucible and decreasing the cooling effect.

[0113] The influence of the ventilation cross-sectional ratio on the cooling rate was studied by adjusting only the ratio of the total cross-sectional area of ​​the four notches to the total cross-sectional area of ​​the air supply end provided in Example 1 (referred to as the ventilation cross-sectional ratio). Cases were designed where the total cross-sectional area of ​​the four notches accounted for 25.72%, 52.45%, and 66.71% of the total cross-sectional area of ​​the air supply end, respectively. The results showed that after 0.5s of cooling airflow, the highest temperatures of the heat-conducting crucible were 562.03℃ (ventilation cross-sectional ratio 12.73%), 562.21℃ (ventilation cross-sectional ratio 25.72%), 554.99℃ (ventilation cross-sectional ratio 52.45%), and 559.60℃ (ventilation cross-sectional ratio 66.71%). Figure 8The graph shows the relationship between the ventilation cross-sectional area ratio and the cooling rate. It can be seen that the cooling rate reaches its peak at 1116.32 K / s when the ventilation cross-sectional area ratio is 52.45%. Analysis suggests that when the cross-sectional area ratio is less than 52.45%, the cooling airflow is insufficient to pass entirely through the notch, resulting in some high-temperature gas remaining inside the gas pipe cavity or experiencing backflow, thus reducing the cooling effect. When the cross-sectional area ratio is greater than 52.45%, some cooling airflow flows directly out of the notch without contacting the crucible, further reducing the cooling effect.

[0114] Only the flow rate of the cryogenic inert gas provided in Example 1 was adjusted. To ensure the cooling rate of the experimental sample, a safety factor of 1.1 was selected, meaning the cooling rate during simulation reached 1100 K / s. The cooling gas flow was introduced at rates of 5 m / s, 10 m / s, 20 m / s, and 30 m / s, respectively. After 0.5 s, the highest temperatures of the thermally conductive crucible were 582.18℃ (5 m / s), 554.36℃ (10 m / s), 511.43℃ (20 m / s), and 483.45℃ (30 m / s), respectively. The relationship between the flow rate of the cryogenic inert gas and the cooling rate is as follows: Figure 9 As shown, the slope of the cooling curve is the highest and the increase in cooling rate is the greatest in the range of 10 m / s to 20 m / s. From the perspective of balancing experimental results and saving gas consumption, it is more appropriate to control the flow rate of low-temperature inert gas in this range.

[0115] In summary, the heat treatment device provided in this application has a simple structure and is easy to load and unload. It can be used to rapidly quench micro-nano-scale samples and avoid the introduction of impurities.

[0116] The above description is merely a preferred embodiment of this application and is not intended to limit this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.

Claims

1. A heat treatment apparatus, characterized in that, include: A thermally conductive sample chamber has a accommodating cavity for accommodating micro-nano-scale samples, the accommodating cavity having an open state and a closed state; A heating mechanism is disposed around the outer periphery of the thermally conductive sample chamber and is used to heat the thermally conductive sample chamber. as well as A gas delivery mechanism is located outside the thermally conductive sample chamber. The gas delivery mechanism includes a gas delivery pipe and a gas source. The gas source is used to provide a low-temperature inert gas with a temperature not exceeding 10°C. The gas inlet end of the gas delivery pipe is connected to the gas source. The end face of the gas delivery end of the gas delivery pipe abuts against the outer wall of the thermally conductive sample chamber. The side wall of the gas delivery end is provided with multiple gas outlet channels arranged at intervals along its circumference.

2. The heat treatment apparatus according to claim 1, characterized in that, The air outlet channel is a notch formed on the end face of the air delivery end, and the total cross-sectional area of ​​the notch accounts for 12.73%-66.71% of the total cross-sectional area of ​​the air delivery end.

3. The heat treatment apparatus according to claim 2, characterized in that, The inner wall diameter of the gas delivery end is 4mm, and the depth of the notch in the gas delivery direction of the gas delivery end is 1-5mm.

4. The heat treatment apparatus according to claim 1, characterized in that, The gas source is configured to output a low-temperature inert gas with a flow rate of 10 m / s to 20 m / s.

5. The heat treatment apparatus according to any one of claims 1-4, characterized in that, The thermally conductive sample chamber includes: A thermally conductive support having a support surface for supporting the micro / nano-scale sample; and A thermally conductive crucible is detachably inverted onto the supporting surface, and the thermally conductive crucible and the supporting surface together form the receiving cavity.

6. The heat treatment apparatus according to claim 5, characterized in that, The thermally conductive sample chamber includes: a thermally conductive connector, which has a receiving groove, an air inlet channel, and a limiting groove connected sequentially along its axial direction. The diameters of the receiving groove and the limiting groove are both larger than the diameter of the air inlet channel. The thermally conductive support is detachably embedded in the receiving groove and closes one end of the air inlet channel near the receiving groove. The support surface is located on the side of the thermally conductive support away from the limiting groove. The thermally conductive crucible is detachably inverted in the receiving groove and the open end of the thermally conductive crucible is closed by the support surface. The gas supply pipe includes a first gas supply pipe and a second gas supply pipe. The end face of the gas supply end of the first gas supply pipe is used to restrict the movement of the heat-conducting crucible along the axial direction of the heat-conducting joint. A first gas outlet gap is formed between the side wall of the first gas supply pipe and the side wall of the receiving groove. The end face of the gas supply end of the second gas supply pipe abuts against the limiting groove. A second gas outlet gap is formed between the side wall of the second gas supply pipe and the limiting groove.

7. The heat treatment apparatus according to claim 6, characterized in that, The thermally conductive sample chamber further includes: a ceramic pressure ring, which is detachably embedded in the receiving groove and pressed onto the bearing surface; the thermally conductive crucible is detachably inverted within the inner ring surface of the ceramic pressure ring; and in the axial direction of the thermally conductive joint, the height of the ceramic pressure ring is lower than the depth of the receiving groove. The end face of the first gas delivery pipe abuts against the ceramic pressure ring.

8. The heat treatment apparatus according to any one of claims 1-4, characterized in that, The gas delivery mechanism includes a connecting pipe and a gas flow meter. The gas source is connected to the gas delivery pipe via the connecting pipe, and the gas flow meter is installed on the connecting pipe.

9. The heat treatment apparatus according to any one of claims 1-4, characterized in that, The heat treatment apparatus further includes: A temperature measuring mechanism is located inside the gas supply pipe, and the temperature measuring point of the temperature measuring mechanism is in contact with the outer wall of the thermally conductive sample chamber; and The controller is electrically connected to both the heating mechanism and the temperature measuring mechanism. The controller receives temperature data fed back by the temperature measuring mechanism and can control the working state of the heating mechanism based on the temperature data.

10. A rapid quenching method using the heat treatment apparatus according to any one of claims 1-9, characterized in that, Includes the following steps: The micro-nano-scale sample is carried on a carrier and then placed together in the accommodating cavity and the accommodating cavity is sealed. The heat treatment device is placed in a vacuum chamber, and the vacuum chamber is evacuated to the target vacuum level. Then, the heating mechanism is started to heat the thermally conductive sample chamber to the target temperature and hold it at that temperature for a preset time. Then, the heating is stopped, and the gas delivery mechanism is started to deliver the low-temperature inert gas to the outer wall of the thermally conductive sample chamber to rapidly cool the micro-nano-scale sample.

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