High-temperature self-propagating reaction device and use method thereof

Abstract

The invention provides a high-temperature self-propagating reaction device. The high-temperature self-propagating reaction device comprises a waste residue tank, a graphite crucible, a collecting cover and an ignition assembly. Wherein the waste residue tank and the collecting cover can be connected into a stable integrated structure, so that the smooth proceeding of the reaction is ensured; the two cooling assemblies on the top wall and the side wall of the collecting cover are matched for use, so that a product generated by reaction can be timely and fully cooled, and the particle size of the product is controlled within a reasonable range; the air supply assembly can ensure that reactants are in full contact with airflow in the device, the yield is improved, and product aggregation is avoided; the inclined side walls and the corrugated plates arranged on the top and the third side wall can increase the collection area of products, and the collection rate of the products is improved. The invention further provides a using method of the device. The high-temperature self-propagating reaction device provided by the invention is simple in use method and convenient to operate, the prepared nanoparticles are high in yield, high in purity, controllable in particle size and uniform in distribution, and the high-temperature self-propagating reaction device has wide popularization and application prospects.

Description

Technical Field

[0001] The present invention belongs to the technical field of the preparation of nanoscale high-entropy oxides, and particularly relates to a high-temperature self-propagating reaction device and a method for using the same. Background Art

[0002] Self-propagating high-temperature synthesis (SHS), also known as combustion synthesis technology, is a technology for synthesizing materials by using the self-heating and self-conduction effects of the high chemical reaction heat between reactants. Once the reactants are ignited, they will automatically spread to the unreacted area until the reaction is complete, which is a new method for preparing high-temperature inorganic compound materials.

[0003] Conventional SHS technology is a technology that uses an instantaneous high-temperature pulse to locally ignite a compact of the reaction mixture, and then the combustion wave spreads to synthesize the target product. This technology is applicable to material systems with high heat release, such as TiC-TiB2, TiC-SiC, TiB2-Al2O3, Si3N4-SiC and other systems. Its characteristics are simple equipment, low energy consumption, fast process, and high reaction temperature. Thermal explosion SHS technology is a technology that rapidly heats the entire compact of the reaction mixture simultaneously, so that the synthesis reaction occurs simultaneously throughout the compact. The materials prepared by this technology mainly include various intermetallic compounds, metal-ceramic composite materials containing more metal phases, and ceramic composite materials with low heat release.

[0004] At present, the structure of the high-temperature self-propagating reaction device mainly includes a container for filling reaction substances, a collection device, and a waste residue tank. Some devices will also be equipped with additional structures such as a cooling device and a gas pump. This type of reaction device is mainly used to prepare powders with a specified particle size. The prepared powders usually have relatively uniform particles, less adhesion, and a size at the nanometer level. However, when the existing high-temperature self-propagating reaction device is used to prepare nanoscale high-entropy oxides, there are still some problems that need to be improved: First, the waste residue tank is separated from the reaction device. Under the condition of high pressure in the reaction system, the reaction device may be washed away by the high pressure, resulting in the failure of preparation; Second, most of the cooling devices only use a water tank, and the cooling effect is poor, resulting in the inability to meet the more precise requirements for the size of the generated nanoparticles; Third, the gas flow space in the device is limited, and oxygen cannot fully contact the reactants, resulting in a decrease in the yield. At the same time, small-sized nanoparticles are prone to aggregation; Fourth, the collection surface of the reaction product is mostly small in area and cannot effectively collect nanoparticles.

[0005] Based on this, it is an urgent technical problem to provide a high-temperature self-propagating reaction device with stable structure, good cooling effect, which can promote the full contact between reactants and gas flow to generate high-entropy oxides at the nanoscale, and can effectively collect the nanoparticle products. Summary of the Invention

[0006] One of the purposes of the present invention is to provide a high-temperature self-propagating reaction device with stable structure, good cooling effect, which can promote the full contact between reactants and gas flow to generate high-entropy oxides at the nanoscale, and can effectively collect the nanoparticle products.

[0007] Another purpose of the present invention is to provide a method for using a high-temperature self-propagating reaction device with stable structure, good cooling effect, which can promote the full contact between reactants and gas flow to generate high-entropy oxides at the nanoscale, and can effectively collect the nanoparticle products.

[0008] The technical solution adopted by the present invention to achieve the first purpose is: to provide a high-temperature self-propagating reaction device, including: a waste residue tank, a graphite crucible, a collection hood and an ignition assembly; The waste residue tank is provided with a waste residue accommodation cavity, the graphite crucible is placed above the waste residue accommodation cavity, and the bottom of the graphite crucible is provided with a slag discharge hole communicating with the waste residue accommodation cavity; The collection hood covers the outside of the graphite crucible and has a structure that is wider at the top and narrower at the bottom; the collection hood includes a top wall and a side wall, and the side wall of the collection hood is detachably connected to the waste residue tank; The top wall of the collection hood is provided with a first cooling assembly, and the side wall includes a pair of first side walls in the shape of inverted right trapezoids, a second side wall arranged vertically, and a third side wall arranged obliquely; The second side wall is provided with a air supply assembly facing the third side wall; the third side wall is provided with a second cooling assembly; the sides of the top wall and the third side wall facing the graphite crucible are respectively provided with corrugated plates for collecting products.

[0009] The general idea of the high-temperature self-propagating reaction device provided by the present invention is as follows: In view of the main problems existing in the existing high-temperature self-propagating reaction device when preparing high-entropy oxides at the nanoscale, the present invention provides a brand-new high-temperature self-propagating reaction device, and its structural improvement is mainly reflected in the following aspects: First of all, the product collection hood of the present invention is detachably connected to the waste residue tank at the bottom through the side wall, which enhances the integrity and firmness of the reaction device, and avoids the collection hood being washed away by the gas flow under the high heat and high pressure reaction conditions, thus affecting the smooth progress of the reaction.

[0010] Secondly, in order to prepare nanoparticle products with uniform size distribution, controllable particle size, and good dispersibility, the present invention improves the cooling structure and air supply structure: among them, the first cooling component is arranged on the top wall of the collection hood, and the second cooling component is arranged on the third side wall, increasing the cooling area and improving the cooling effect on the products; the air supply component on the second side wall is arranged near the path where the reactants are ejected to increase air flow, promoting the full contact between the reactants and the protective gas flow while reducing particle aggregation.

[0011] Finally, corrugated plates for collecting products are respectively arranged on the top wall provided with the cooling component and the inclined third side wall, increasing the collection area of the products, improving the collection rate, and effectively avoiding the aggregation of the products.

[0012] Based on the improvements in the above-mentioned multi-faceted structures, the high-temperature self-propagating reaction device provided by the present invention not only has a stable structure itself, ensuring the smooth progress of the reaction; the two cooling components are used in combination, with good cooling effect, capable of cooling the products generated by the reaction in a timely and sufficient manner, and controlling the particle size of the products within a reasonable range; at the same time, the setting of the air supply component can promote the full contact between the reactants and the gas flow, improve the yield, and avoid the aggregation of the products; the inclined third side wall and the corrugated plates arranged on the top and the third side wall can increase the collection area of the products, not only improving the collection rate of the products, but also ensuring the uniform dispersion of the products and avoiding aggregation that affects the particle size of the target products.

[0013] Furthermore, the waste residue tank is made of stainless steel with a surface roughness of Ra1.6, and refractory bricks made of silicate are laid at the bottom of the waste residue tank. The waste residue tank itself has a certain weight, improving the stability of the reaction device. Preferably, the waste residue accommodation cavity accounts for 3%-4% of the total volume of the waste residue tank.

[0014] Furthermore, mounting holes are provided at the four corners of the top surface of the waste residue tank, and the side wall bottom end of the collection hood is provided with a protruding mounting edge, and the edge is detachably connected to the waste residue tank through fastening screws.

[0015] Furthermore, the collection hood is made of stainless steel material with a thickness of 0.7-0.9 cm and a surface roughness of Ra1.6.

[0016] Furthermore, the collection hood is provided with holes for installing the ignition component.

[0017] Furthermore, the first cooling component is a water tank arranged above the top wall, and a water outlet is provided at the bottom of the water tank.

[0018] Furthermore, the second cooling component includes a cooling water pipeline arranged in a snake shape on the back of the third side wall, and flowing cooling water is provided in the cooling water pipeline.

[0019] Further, the inclination angle of the third side wall in the horizontal direction is 40 - 50°. If the angle is too small, it will cause particle aggregation, and if the angle is too large, it will cause particle slippage and affect the yield.

[0020] Further, the inlet of the cooling water pipeline is connected to the outlet at the bottom of the water tank. In the present invention, the first cooling component and the second cooling component are interconnected, and flowing cooling water is used to ensure sufficient cooling effect. The two cooling components cool the upper part and the side of the collection hood simultaneously, and the inclined third collection surface increases the contact area between the product and the corrugated plate.

[0021] Further, the air supply component includes a fan, a motor and an air pump. The air pump conveys a protective gas into the high-temperature self-propagating reaction device. The protective gas can be an inert gas such as nitrogen or argon, or a mixture composed of an inert gas and air or oxygen in a certain proportion. In the present invention, a motor and an air pump are configured at the fan of the air supply component. With the introduction of the protective gas, it can reduce particle aggregation, and appropriate air or oxygen can also be introduced into the protective gas according to the actual reaction requirements to adjust the oxygen content of the reaction system, so as to adjust the proportion of oxides in the product.

[0022] Preferably, the motor is a variable-speed DC motor to meet the preparation of powders with different particle size requirements.

[0023] Preferably, the fan blades are wide blades obtained by cutting stainless steel materials, which can not only increase the air supply flow rate, but also meet the requirements of long-term use under high-temperature conditions.

[0024] Further, the ignition component includes an electronic igniter, a capacitor and a power supply. In the present invention, the ignition component adopts a capacitive ignition device with a coil as the igniter. The coil generates a large amount of heat under the strong current generated by the instantaneous discharge of the capacitor to ignite the primer, eliminating the inconvenience of using ignition means such as magnesium strips. In addition, the coil has a low cost and is easy to manufacture, and capacitors, dry batteries, etc. are all common components, reducing the difficulty of assembling the ignition device and the difficulty of ignition operation. Preferably, the power supply is a dry battery.

[0025] Further, the corrugated plate is placed in a way that the corrugations are parallel to the ground; the corrugation spacing is 0.8 - 1.2 mm, and the mesh number of the corrugations is 350 - 500 meshes.

[0026] The technical solution adopted by the present invention to achieve the second object is: to provide a use method of the high-temperature self-propagating reaction device according to the first object of the present invention, including the following steps: S1. Place the waste residue tank on a heat-resistant plane and cover the waste residue accommodating cavity of the waste residue tank with cardboard; S2. Place the thermite and the substances to be reacted in the graphite crucible, and sprinkle the ignition agent; place the graphite crucible on the cardboard of the waste residue tank, and align the slag discharge hole at the bottom of the graphite crucible with the waste residue accommodating cavity; S3. Insert the electronic igniter of the ignition assembly through the hole of the collection hood into the ignition agent, and then connect the waste residue tank and the collection hood with the fastening screw; S4. Continuously add cooling water to the water tank of the first cooling assembly at the top of the collection hood. The cooling water enters the cooling water pipeline of the second cooling assembly located on the third side wall through the water tank outlet and is discharged from the end of the cooling water pipeline; S5. Turn on the air pump of the air supply assembly to introduce the protective gas into the reaction device, and turn on the fan to ensure the air flow in the reaction device; S6. Charge the capacitor of the ignition assembly. After charging is completed, disconnect the charging switch and close the ignition switch to ignite the ignition agent for reaction; S7. After the reaction is completed and the device cools down to room temperature, stop adding cooling water, stop introducing the protective gas, turn off the fan, remove the fastening screw and the ignition assembly, and then scrape and collect the product on the corrugated board.

[0027] Preferably, in step S4, the flow rate of the cooling water is 4 - 6 L / min, the inlet temperature of the cooling water is 15 - 25 °C, and the outlet temperature is 36 - 45 °C; in step S5, the flow rate of the introduced protective gas is 5 - 7 L / min.

[0028] Furthermore, the usage method further includes: S8. Clean the collection hood, graphite crucible, and waste residue tank; if necessary, dissolve and remove the attached waste with a specific cleaning agent for subsequent use.

[0029] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) For the high-temperature self-propagating reaction device provided by the present invention, the waste residue tank and the collection hood can be connected into a stable integrated structure to ensure the smooth progress of the reaction; the two cooling assemblies are used in combination, with good cooling effect, which can timely and fully cool the product generated by the reaction and control the particle size of the product within a reasonable range; the setting of the air supply assembly can ensure the full dispersion of the nano-powder and limit the growth of the nano-powder, improve the yield, and avoid the aggregation of the product; the inclined third side wall and the corrugated boards arranged on the top and the third side wall can increase the collection area of the product, not only improve the collection rate of the product, but also ensure the uniform dispersion of the product and avoid aggregation, which affects the particle size of the target product.

[0030] (2) The high-temperature self-propagating reaction device provided by the present invention has a simple usage method and convenient operation. The prepared nano-particles have a high yield, high purity, controllable particle size and uniform distribution, and have broad prospects for popularization and application. Brief Description of the Drawings

[0031] Figure 1 It is a schematic diagram of the overall structure of the high-temperature self-propagating reaction device provided by the embodiment of the present invention; Figure 2 It is a sectional view of the high-temperature self-propagating reaction device provided by the embodiment of the present invention; Figure 3 It is a schematic diagram of the structure of the waste residue tank in the high-temperature self-propagating reaction device provided by the embodiment of the present invention; Figure 4 It is a sectional view of the collection hood in the high-temperature self-propagating reaction device provided by the embodiment of the present invention; Figure 5 It is a schematic diagram of the structure of the collection hood in the high-temperature self-propagating reaction device provided by the embodiment of the present invention; Among them, 1 - waste residue tank; 11 - waste residue accommodating cavity; 12 - mounting hole; 2 - graphite crucible; 21 - slag discharge hole; 3 - collection hood; 31 - top wall; 32 - first cooling component; 33 - first side wall; 34 - second side wall; 35 - third side wall; 36 - air supply component; 37 - second cooling component; 38 - mounting edge; 4 - ignition component; 41 - electronic igniter; 42 - capacitor; 43 - power supply. Detailed Embodiments

[0032] Next, the technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0033] It should be noted that, without conflict, the embodiments in the present invention and the features in the embodiments can be combined with each other.

[0034] Please refer to Figures 1-5 , the present invention provides a high-temperature self-propagating reaction device, including: a waste residue tank 1, a graphite crucible 2, a collection hood 3 and an ignition component 4.

[0035] The waste residue tank 1 is provided with a waste residue accommodating cavity 11. The graphite crucible 2 is placed above the waste residue accommodating cavity 11. The bottom of the graphite crucible 2 is provided with a slag discharge hole 21 communicating with the waste residue accommodating cavity 11. The collecting hood 3 covers the outside of the graphite crucible 2 and has a structure that is wider at the top and narrower at the bottom. The collecting hood 3 includes a top wall 31 and side walls. The side walls of the collecting hood 3 are detachably connected to the waste residue tank 1. The top wall 31 of the collecting hood 3 is provided with a first cooling assembly 32. The side walls include a pair of first side walls 33 in the shape of an inverted right trapezoid, a second side wall 34 arranged vertically, and a third side wall 35 arranged obliquely. The second side wall 34 is provided with an air supply assembly 36 facing the third side wall 35. The third side wall 35 is provided with a second cooling assembly 37. The sides of the top wall 31 and the third side wall 35 facing the graphite crucible 2 are respectively provided with corrugated plates for collecting products. In an embodiment of the present invention, the corrugated plates are placed in parallel, and the extending direction of the corrugations is parallel to the ground. The length of the corrugated plate on the inclined surface is 35 cm, the corrugation pitch is 1 mm, and the number of corrugations is 350. The length of the top corrugated plate is 50 cm, the corrugation pitch is 1 mm, and the number of corrugations is 500.

[0036] Wherein, the bottom of the waste residue tank 1 is paved with silicate refractory bricks. Four corners of the top surface of the waste residue tank 1 are provided with installation holes 12. The bottom end of the side wall of the collecting hood 3 has a protruding installation edge 38, and the installation edge 38 is detachably connected to the installation holes 12 of the waste residue tank 1 through fastening screws. In the present invention, both the waste residue tank 1 and the collecting hood 3 are made of ordinary stainless steel, and the surface roughness is Ra1.6. The size of the bottom opening of the collecting hood 3 is 35 cm × 35 cm, and the size of the waste residue tank below it is 40 cm × 40 cm × 10 cm. The waste residue accommodating cavity accounts for 3% - 4% of the total volume of the waste residue tank. The top of the collecting hood 3 is 35 cm × 50 cm, and the included angle between the third side wall 35 and the horizontal direction is 45°.

[0037] The first cooling assembly 32 is a water tank arranged above the top wall 31, and the bottom of the water tank is provided with a water outlet. The second cooling assembly 37 includes a cooling water pipeline arranged in a snake shape on the third side wall 35, and flowing cooling water is provided in the cooling water pipeline. The inlet of the cooling water pipeline is communicated with the water outlet at the bottom of the water tank. In an embodiment of the present invention, the inside of the first cooling assembly 32 is 30 cm × 45 cm, with a depth of 4 cm, and the pipe diameter of the second cooling assembly 37 is 1 cm.

[0038] Furthermore, the air supply assembly 36 includes a fan, a motor, and an air pump. The motor is a variable speed DC motor. The blades of the fan are made of ordinary stainless steel, and the power of the fan is 10 W. The ignition assembly 4 includes an electronic igniter 41, a capacitor 42, and a power supply 43.

[0039] The present invention will be further described below in conjunction with specific embodiments, but it is not limited to the present invention.

[0040] Example 1 This example provides a method for preparing high-entropy oxide powder by using the Figures 1-5 high-temperature self-propagating reaction device shown, including the following steps: Step 1: Place the waste residue tank 1 on a heat-resistant plane and cover the waste residue accommodating cavity 11 of the waste residue tank 1 with cardboard; Step 2: Put silicate refractory bricks in the graphite crucible 2. By weight, put 10 parts of thermite Al powder, 30 parts of CuO powder, 57 parts of the substance to be reacted (the substance to be reacted is prepared by mixing powders of Al, Fe, Zn, Co, and Ni in a molar ratio of 42.5:17.5:10.5:18.5:11 and mechanically alloying for 3 h), and 3 parts of CaSO4 powder, and sprinkle with an ignition agent; Place the graphite crucible 2 on the cardboard of the waste residue tank 1, and align the slag discharge hole 21 at the bottom of the graphite crucible 2 with the waste residue accommodating cavity 11; Step 3: Insert the electronic lighter 41 of the ignition assembly 4 through the hole of the collection hood 3 into the ignition agent, and then connect the waste residue tank 1 and the collection hood 3 with fastening screws; Step 4: Continuously add cooling water to the water tank of the first cooling assembly 32 at the top of the collection hood 3. The cooling water enters the cooling water pipeline of the second cooling assembly 37 located on the third side wall 35 through the water tank outlet and is discharged from the end of the cooling water pipeline; Step 5: Turn on the air pump of the air supply assembly 36 to introduce argon into the reaction device (control the flow rate of argon to be 5 L / min), and turn on the fan to ensure the air flow in the reaction device; Step 6: Charge the capacitor 42 of the ignition assembly 4. After charging is completed, disconnect the charging switch and close the ignition switch to ignite the ignition agent for reaction; Step 7: After the reaction is completed and the device cools down to room temperature, stop adding cooling water, stop introducing argon, turn off the fan, remove the fastening screws and the ignition assembly 4, and then scrape and collect the product on the corrugated board to obtain high-entropy oxide powder.

[0041] Example 2 This example provides a method for preparing high-entropy oxide powder by using the Figures 1-5 high-temperature self-propagating reaction device shown, including the following steps: Step 1: Place the waste residue tank 1 on a heat-resistant plane and cover the waste residue accommodating cavity 11 of the waste residue tank 1 with cardboard; Step 2: Place the silicate refractory brick in the graphite crucible 2. By weight, add 12.5 parts of aluminum thermite Al powder, 37.5 parts of CuO powder, 46 parts of the reactant (the reactant is prepared by mixing powders of Al, Fe, Zn, Co, and Ni in a molar ratio of 45.5:20.5:14.5:19:0.5 and mechanically alloying for 3.5 h), and 4 parts of CaSO4 powder. Sprinkle the ignition agent; Place the graphite crucible 2 on the cardboard of the waste residue tank 1, and align the slag discharge hole 21 at the bottom of the graphite crucible 2 with the waste residue containing cavity 11; Step 3: Insert the electronic lighter head 41 of the ignition assembly 4 through the hole of the collection hood 3 into the ignition agent, and then connect the waste residue tank 1 and the collection hood 3 with fastening screws; Step 4: Continuously add cooling water to the water tank of the first cooling assembly 32 at the top of the collection hood 3. The cooling water enters the cooling water pipe of the second cooling assembly 37 located on the third side wall 35 through the water tank outlet and is discharged from the end of the cooling water pipe; Step 5: Turn on the air pump of the air supply assembly 36 to introduce argon into the reaction device (control the argon gas flow rate to be 6 L / min), and turn on the fan to ensure the air flow inside the reaction device; Step 6: Charge the capacitor 42 of the ignition assembly 4. After charging is completed, disconnect the charging switch and close the ignition switch to ignite the ignition agent for reaction; Step 7: After the reaction ends and the device cools down to room temperature, stop adding cooling water, stop introducing argon, turn off the fan, remove the fastening screws and the ignition assembly 4, and then scrape and collect the product on the corrugated board to obtain the high-entropy oxide powder.

[0042] Example 3 This example provides a method for preparing high-entropy oxide powder using the Figures 1-5 shown high-temperature self-propagating reaction device, including the following steps: Step 1: Place the waste residue tank 1 on a heat-resistant plane and cover the waste residue containing cavity 11 of the waste residue tank 1 with cardboard; Step 2: Place the silicate refractory brick in the graphite crucible 2. By weight, add 12 parts of aluminum thermite Al powder, 36 parts of CuO powder, 47 parts of the reactant (the reactant is prepared by mixing powders of Al, Fe, Zn, Co, and Ni in a molar ratio of 45:20:13:18.75:3.25 and mechanically alloying for 4 h), and 5 parts of CaSO4 powder. Sprinkle the ignition agent; Place the graphite crucible 2 on the cardboard of the waste residue tank 1, and align the slag discharge hole 21 at the bottom of the graphite crucible 2 with the waste residue containing cavity 11; Step 3: Insert the electronic lighter head 41 of the ignition assembly 4 through the hole of the collection hood 3 into the ignition agent, and then connect the waste residue tank 1 and the collection hood 3 with fastening screws; Step 4: Continuously add cooling water to the water tank of the first cooling component 32 at the top of the collection hood 3. The cooling water enters the cooling water pipeline of the second cooling component 37 located on the third side wall 35 through the water tank outlet and is discharged from the end of the cooling water pipeline. Step 5: Turn on the air pump of the air supply component 36 to introduce an argon gas flow into the reaction device (control the argon gas flow rate to be 7 L / min), and turn on the fan to ensure the air flow inside the reaction device. Step 6: Charge the capacitor 42 of the ignition component 4. After charging is completed, disconnect the charging switch and close the ignition switch to ignite the ignition agent for reaction. Step 7: After the reaction ends and the device cools down to room temperature, stop adding cooling water, stop introducing argon gas, turn off the fan, remove the fastening screws and the ignition component 4, and then scrape off and collect the product on the corrugated plate to obtain high-entropy oxide powder.

[0043] Comparative Example In this comparative example, a conventional self-propagating reaction device was used to prepare high-entropy oxide powder. The device used in the comparative example includes: a stainless steel waste residue tank, a graphite crucible, and a bowl-shaped collection device. The preparation method includes the following steps: Step 1: Place the stainless steel waste residue tank on the ground, place a silicate refractory brick in the waste residue tank, and cover the accommodation cavity of the waste residue tank with cardboard. Step 2: By weight, put 12 parts of aluminum thermal agent Al powder, 36 parts of CuO powder, 47 parts of the substance to be reacted (the substance to be reacted is prepared by mixing powders of Al, Fe, Zn, Co, and Ni in a molar ratio of 45:20:13:18.75:3.25 and mechanically alloying for 4 h), and 5 parts of CaSO4 powder in the graphite crucible. Sprinkle the ignition agent on it and insert a magnesium strip for ignition into the mixture. Place the graphite crucible on the cardboard of the waste residue tank, and align the slag discharge hole at the bottom of the graphite crucible with the accommodation cavity on the waste residue tank. Step 3: Invert a bowl-shaped stainless steel collection device above the crucible and the waste residue tank. Step 4: Ignite the magnesium strip to start the high-temperature self-propagating reaction. After the reaction ends and the bowl-shaped container cools down to room temperature, scrape off and collect the high-entropy oxide powder on the inner wall of the bowl-shaped container with a scraper.

[0044] Product Comparison The yield, purity, and particle size of the high-entropy oxide powder prepared in each example of the present invention and the comparative example were tested, and the results are shown in Table 1 below: Table 1

[0045] As can be seen from Table 1 above, The yields of the high-entropy oxide powders prepared by Examples 1-3 based on the high-temperature self-propagating reaction device provided by the present invention are 84%-90%, the purities are 86%-90%, and the particle size distributions are in the range of 220-350 nm. Compared with the comparative examples, they have the advantages of high yield, high product purity, and smaller product particle size.

[0046] The above are only the preferred embodiments of the present invention, and do not limit the implementation manners and protection scope of the present invention. Those skilled in the art should be able to realize that the solutions obtained by equivalent substitutions and obvious changes made by using the content of the specification of the present invention should all be included in the protection scope of the present invention.

Claims

1. A high-temperature self-propagating reaction device, characterized in that, Comprising: A waste residue tank (1), a graphite crucible (2), a collection hood (3) and an ignition assembly (4); The waste residue tank (1) is provided with a waste residue accommodating cavity (11), the graphite crucible (2) is placed above the waste residue accommodating cavity (11), and a slag discharge hole (21) communicating with the waste residue accommodating cavity (11) is opened at the bottom of the graphite crucible (2); The collection hood (3) covers the outside of the graphite crucible (2) and has a structure that is wider at the top and narrower at the bottom; the collection hood (3) includes a top wall (31) and side walls, and the side walls of the collection hood (3) are detachably connected to the waste residue tank (1); A first cooling assembly (32) is provided on the top wall (31) of the collection hood (3), and the side walls include a pair of first side walls (33) in the shape of an inverted right trapezoid, a second side wall (34) arranged vertically, and a third side wall (35) arranged obliquely; A blowing assembly (36) facing the third side wall (35) is provided on the second side wall (34); a second cooling assembly (37) is provided on the third side wall (35); corrugated plates for collecting products are respectively provided on one sides of the top wall (31) and the third side wall (35) facing the graphite crucible (2).

2. The high-temperature self-propagating reaction device according to claim 1, characterized in that, The waste residue tank (1) is made of stainless steel, and refractory bricks made of silicate are laid at the bottom of the waste residue tank.

3. The high-temperature self-propagating reaction device according to claim 1, characterized in that, Mounting holes (12) are opened at the four corners of the top surface of the waste residue tank (1), and the side wall bottom end of the collection hood (3) is provided with a protruding mounting edge (38), and the mounting edge (38) is detachably connected to the mounting holes (12) of the waste residue tank (1) by fastening screws.

4. The self-propagating high-temperature reaction device according to claim 1, characterized in that, The first cooling assembly (32) is a water tank arranged above the top wall (31), and a water outlet is opened at the bottom of the water tank.

5. The high-temperature self-propagating reaction device according to claim 4, characterized in that The second cooling assembly (37) includes a cooling water pipeline arranged in a serpentine shape on the third side wall (35), and flowing cooling water is provided in the cooling water pipeline.

6. The high-temperature self-propagating reaction device according to claim 5, characterized in that, The inlet of the cooling water pipeline is communicated with the water outlet at the bottom of the water tank.

7. The self-propagating high-temperature reaction device according to claim 1, characterized in that, The blowing assembly (36) includes a fan, a motor and an air pump.

8. The high-temperature self-propagating reaction device according to claim 7, characterized in that The motor is a variable speed DC motor.

9. The self-propagating high-temperature reaction device according to claim 1, wherein, The ignition assembly (4) includes an electronic lighter (41), a capacitor (42) and a power supply (43).

10. The method of using the high-temperature self-propagating reaction device according to any one of claims 1-9, characterized in that, Including the following steps: S1. Place the waste residue tank (1) on a heat-resistant plane, and cover the waste residue accommodating cavity (11) of the waste residue tank (1) with cardboard; S2. Put thermite and substances to be reacted into the graphite crucible (2), and sprinkle ignition agent; place the graphite crucible (2) on the cardboard of the waste residue tank (1), and align the slag discharge hole (21) at the bottom of the graphite crucible (2) with the waste residue accommodating cavity (11); S3. Insert the electronic lighter (41) of the ignition assembly (4) into the ignition agent through the hole of the collection hood (3), and then connect the waste residue tank (1) and the collection hood (3) with fastening screws; S4. Continuously add cooling water to the water tank of the first cooling assembly (32) at the top of the collection hood (3), the cooling water enters the cooling water pipeline of the second cooling assembly (37) located on the third side wall (35) through the water tank outlet, and is discharged from the end of the cooling water pipeline; S5. Turn on the air pump of the blowing assembly (36) to introduce protective gas into the reaction device, and at the same time turn on the fan to ensure the air flow in the reaction device; S6. Charge the capacitor (42) of the ignition assembly (4). After the charging is completed, disconnect the charging switch and close the ignition switch to ignite the igniter for reaction; S7. After the reaction ends and the device cools down to room temperature, stop adding cooling water, stop introducing the protective gas, turn off the fan, remove the fastening screws and the ignition assembly (4), and then scrape and collect the product on the corrugated plate.

Images