CN-116377181-B - Heat treatment device and rapid quenching method

CN116377181BCN 116377181 BCN116377181 BCN 116377181BCN-116377181-B

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 conduction sample chamber, a heating mechanism and a gas conveying mechanism, wherein the heat conduction sample chamber is provided with a containing cavity in an open state and a closed state, the heating mechanism is arranged on the periphery of the heat conduction sample chamber in a surrounding mode, the gas conveying mechanism is arranged outside the heat conduction sample chamber and 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 communicated 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 conduction sample chamber, a plurality of gas outlet channels are formed in the side wall of the gas conveying end at intervals along the periphery of the gas conveying pipe, the structure is simple, the assembly and the disassembly are convenient, and the rapid quenching of micro-nano samples can be realized and the introduction of impurities is avoided.

Inventors

ZHANG BO
ZHAO YONG
Jia Yanghua
XU LIMING
WANG PENG
YAN YUQIANG
HU JINLIANG
KE HAIBO
WANG WEIHUA

Assignees

松山湖材料实验室

Dates

Publication Date: 20260512
Application Date: 20230511

Claims (10)

1. A heat treatment apparatus, comprising: the heat conduction sample chamber is provided with a containing cavity for containing the micro-nano level sample, and the containing cavity is provided with an open state and a closed state; A heating mechanism surrounding the periphery of the heat conduction sample chamber and used for heating the heat conduction sample chamber, and The gas conveying mechanism is located outside the heat conduction sample chamber and comprises a gas conveying pipe and a gas source, the gas source is used for providing low-temperature inert gas with the temperature not higher than 10 ℃, the gas inlet end of the gas conveying pipe is communicated with the gas source, the end face of the gas feeding end of the gas conveying pipe abuts against the outer wall of the heat conduction sample chamber, and a plurality of gas outlet channels are formed in the side wall of the gas feeding end at intervals along the circumferential direction of the gas feeding end.
2. The heat treatment apparatus according to claim 1, wherein the air outlet passage is a notch formed in an end face of the air supply end, and a total cross-sectional area of the notch is 12.73% -66.71% of a total cross-sectional area of the air supply end.
3. The heat treatment apparatus according to claim 2, wherein the diameter of the inner wall of the gas supply end is 4mm, and the depth of the notch in the gas supply direction of the gas supply end is 1 to 5mm.
4. The thermal processing apparatus of claim 1, wherein said gas source is configured to output a flow rate of low temperature inert gas of 10m/s to 20m/s.
5. The thermal processing apparatus of any of claims 1-4, wherein said thermally conductive sample chamber comprises: a heat conducting carrier with a carrying surface for carrying the micro-nano sample, and The heat conduction crucible is detachably and reversely buckled on the bearing surface, and the heat conduction crucible and the bearing surface jointly form the accommodating cavity.
6. The heat treatment device according to claim 5, wherein the heat conduction sample chamber comprises a heat conduction joint, a heat conduction bearing piece and a heat conduction crucible, wherein the heat conduction joint is axially provided with a containing groove, an air inlet channel and a limiting groove which are sequentially communicated, the diameters of the containing groove and the limiting groove are larger than those of the air inlet channel; The gas delivery pipe comprises a first gas delivery pipe and a second gas delivery pipe, the end face of the gas delivery end of the first gas delivery pipe is used for limiting the heat conduction crucible to move along the axial direction of the heat conduction joint, a first gas outlet gap is formed between the side wall of the first gas delivery pipe and the side wall of the containing groove, the end face of the gas delivery end of the second gas delivery pipe is propped against the limiting groove, and a second gas outlet gap is formed between the side wall of the second gas delivery pipe and the limiting groove.
7. The heat treatment apparatus according to claim 6, wherein the heat conductive sample chamber further comprises a ceramic pressing ring detachably embedded in the accommodating groove and pressed against the carrying surface, the heat conductive crucible is detachably reversely fastened in an inner annular surface of the ceramic pressing ring, and a height of the ceramic pressing ring in an axial direction of the heat conductive joint is lower than a depth of the accommodating groove; the end face part of the air supply end of the first air pipe is propped against the ceramic compression ring.
8. The heat treatment apparatus according to any one of claims 1 to 4, wherein the gas delivery mechanism includes a connection pipe through which the gas source communicates with the gas delivery pipe, and a gas flow meter provided on the connection pipe.
9. The heat treatment apparatus according to any one of claims 1 to 4, further comprising: A temperature measuring mechanism positioned in the gas pipe, a temperature measuring point of the temperature measuring mechanism contacting with the outer wall of the heat conducting sample chamber, and The controller is respectively and electrically connected with the heating mechanism and the temperature measuring mechanism, and is used for receiving temperature data fed back by the temperature measuring mechanism, and the controller can control the working state of the heating mechanism according to the temperature data.
10. A rapid quenching method using the heat treatment apparatus according to any one of claims 1 to 9, comprising the steps of: And loading the micro-nano sample on a carrier, then putting the micro-nano sample into the accommodating cavity together, sealing the accommodating cavity, placing the heat treatment device in a vacuum box, vacuumizing the vacuum box to a target vacuum degree, starting the heating mechanism to heat the heat conduction sample chamber to a target temperature, preserving heat for a preset time, stopping heating, and starting the gas conveying mechanism to convey the low-temperature inert gas to the outer wall of the heat conduction sample chamber so as to enable the micro-nano sample to be rapidly cooled.

Description

Heat treatment device and rapid quenching method Technical Field The application relates to the field of heat treatment, in particular to a heat treatment device and a rapid quenching method. Background The heat treatment process is a heat treatment process for obtaining expected tissues and performances by heating, preserving heat and cooling materials in a solid state, and generally comprises annealing, normalizing, quenching, tempering and the like, and the four processes can evolve different heat treatment processes through reasonable combination, so that the treated materials obtain different strength and toughness, thereby achieving the purposes of eliminating the tissue defects and improving the performances of the materials. Quenching refers to heating a material to a specified temperature, then preserving heat for a period of time, and then placing the material into a quenching medium to quickly cool the material. At present, the structure of a heat treatment device for realizing rapid quenching is complex, a rotating mechanism is generally required to be designed to enable a sample to be fully contacted with a quenching agent, and a recycling cavity is designed to recycle the quenching agent, so that the occupied space is large, and meanwhile, the consumption of energy sources such as electric power and the like is increased. In the prior art, a micro-nano sample is subjected to heat treatment, which is mostly placed in a copper crucible, is heated to a high temperature in a vacuum environment, and is naturally cooled slowly along with a furnace or is introduced with water/oil cooling medium to realize rapid cooling after a period of constant temperature, so that the time consumption of one experiment is long and the efficiency is low along with the furnace cooling mode, and if the water/oil cooling medium is introduced to realize rapid cooling, the sample and the cooling medium react, impurities are introduced to influence the performance of the sample, and the condition that the sample falls off from a carrier due to the impact of the cooling medium exists, and the maximum cooling rate of the water/oil cooling medium is low, the cooling rate is slow, and the cooling effect is poor. Disclosure of Invention An object of an embodiment of the present 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. In a first aspect, embodiments of the present application provide a thermal processing apparatus that includes a thermally conductive sample chamber, a heating mechanism, and a gas delivery mechanism. The heat conduction sample chamber is provided with a containing cavity for containing micro-nano level samples, the containing cavity is provided with an open state and a closed state, the heating mechanism is arranged on the periphery of the heat conduction sample chamber in a surrounding mode and used for heating the heat conduction sample chamber, the gas conveying mechanism is arranged outside the heat conduction sample chamber and comprises a gas conveying pipe and a gas source, the gas source is used for providing low-temperature inert gas with the temperature not higher than 10 ℃, the gas inlet end of the gas conveying pipe is communicated with the gas source, the end face of the gas inlet end of the gas conveying pipe abuts against the outer wall of the heat conduction sample chamber, and a plurality of gas outlet channels are formed in the side wall of the gas inlet end at intervals along the circumferential direction of the gas inlet end. In the implementation process, the micro-nano level sample is accommodated in the accommodating cavity, and the gas conveying mechanism is positioned outside the heat conducting sample chamber, so that the micro-nano level sample can be prevented from being impacted by air flow and being exchanged with low-temperature inert gas generating substances during cooling, and impurities are prevented from being introduced to ensure the quality of the micro-nano level sample. The low-temperature inert gas and the heat conduction sample chamber are utilized for heat exchange, the temperature can be rapidly reduced, the temperature reduction rate can reach 1000K/s, rapid quenching is realized, the quenching efficiency is improved, the quenched nano-micron sample has complete structure and good performance, the whole heat treatment device has simple structure, convenient loading and unloading and high practicability, and the experimental efficiency can be effectively improved. In one possible embodiment, the air outlet channel is a notch formed in 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. In one possible embodiment, the diameter of the inner wall of the gas delivery end is 4mm and the depth of the gap in the gas delivery direction of the gas d