CN108383507B - Method for preparing high-emissivity complex phase ceramic and FeCrCoNi high-entropy alloy in one step - Google Patents
Method for preparing high-emissivity complex phase ceramic and FeCrCoNi high-entropy alloy in one step Download PDFInfo
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Abstract
A method for preparing high-emissivity complex phase ceramic and FeCrCoNi high-entropy alloy in one step relates to the technical field of preparation of high-entropy alloy and high-emissivity complex phase ceramic materials. The invention mainly aims to solve the problems that the existing high-entropy alloy has high requirements on the performance of preparation equipment, and high-emissivity ceramic materials are easy to peel off and have performance attenuation. Mixing Fe2O3、Cr2O3、Co2O3Drying NiO and Al raw material powder, uniformly mixing and compacting to obtain a thermite precast block with the relative density of 40-60%; putting the obtained thermite precast block into a crucible and placing the crucible into high-pressure combustion reaction equipment; vacuumizing the reaction equipment, filling protective gas, and igniting the aluminothermic precast blocks by utilizing an electrified tungsten spiral wire to initiate a combustion synthesis reaction; after the reaction is finished, the product is automatically layered, the lower layer is a high-entropy alloy layer, and the upper layer is a ceramic layer. The method has the advantages of high speed, high efficiency, no pollution in the preparation process, low energy consumption and full utilization of raw materials.
Description
The technical field is as follows:
the invention relates to the technical field of preparation of high-entropy alloy and high-emissivity complex phase ceramic materials. In particular to a method for preparing high-emissivity complex phase ceramics and FeCrCoNi high-entropy alloy in one step.
Technical background:
the Fe-Cr-Co-Ni series high-entropy alloy has excellent mechanical property and high-temperature phase stability, so that the Fe-Cr-Co-Ni series high-entropy alloy is considered as a potential structural material for aerospace industry. However, the development of the high-entropy alloy is limited by the preparation technology, and the main reason is that the common induction melting technology and electric arc melting technology have obvious limitations for preparing the high-entropy alloy: 1. the melting point of the high-entropy alloy composition elements is higher, the performance requirement on preparation equipment is high, and the energy consumption is higher; 2. the purity requirement of the raw materials is high, and the raw materials are expensive; 3. the melting point difference of alloying elements is large, so that element volatilization and alloy composition unevenness are easily caused, and the smelting technology is difficult; 4. repeated smelting is needed to ensure the uniformity of alloy components, and the preparation period is longer; 5. the high melting point alloy elements are relatively active at high temperature, and oxidation reaction easily occurs in the smelting process. Therefore, the high-entropy alloy is difficult to efficiently prepare in large batch by using the traditional smelting method.
The high-emissivity ceramic material has important prospect in the energy-saving application of high-temperature thermal equipment because the radiation heat transfer efficiency and the temperature field uniformity at high temperature can be obviously enhanced. At present, one of the most widely used refractory materials in high-temperature thermal equipment is an alumina refractory material. Conventional high emissivity ceramic materials, which contain silicate, borate, etc. components that react with alumina substrates, are coated on refractory substrates in the form of coatings, and are prone to spalling and performance degradation. The high-emissivity complex phase ceramic material based on the alumina can realize stable combination with the alumina refractory base material while enhancing the radiation heat transfer efficiency. In addition, the low-cost and low-energy-consumption preparation of the high-emissivity ceramic material is also a key problem to be solved in the preparation research field of the high-emissivity ceramic material.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing high-emissivity complex phase ceramic and FeCrCoNi high-entropy alloy in one step; the method quickly realizes melt self-purification and strong mass transfer by generating ultrahigh temperature through chemical heat released by a strongly exothermic aluminothermic combustion reaction, inhibits element volatilization and melt splashing by using high-pressure atmosphere, and realizes separation and solidification of ceramics and high-entropy alloy materials with different densities under the action of gravity and wettability difference. The high-entropy alloy is obtained after separation, and the generated ceramic is alumina and ferrochrome spinel complex-phase ceramic with high infrared emissivity.
In order to achieve the above purpose, the invention adopts the technical scheme that:
firstly, mixing Fe2O3、Cr2O3、Co2O3Drying NiO and Al raw material powder, uniformly mixing and compacting to obtain a thermite precast block with the relative density of 40-60%;
secondly, the obtained thermite prefabricated block is put into a crucible and is placed in high-pressure combustion reaction equipment;
vacuumizing the reaction equipment, filling protective gas, and igniting the aluminothermic precast blocks by utilizing an electrified tungsten spiral wire to initiate a combustion synthesis reaction;
fourthly, after the reaction is finished, the product is automatically layered, the lower layer is a high-entropy alloy layer, and the upper layer is a ceramic layer.
The molar mass ratio of each raw material in the thermite precast block is Fe2O3：Cr2O3：Co2O3: NiO: al = 1+2 x: 1+ x: 1: 2: 8, wherein x is more than or equal to 0.15 and less than or equal to 0.20.
Unless otherwise specified, any of the powders described in the present invention means a powder having a purity of 99.5% or more and a particle size of 325 mesh.
The protective gas is argon, and the initial pressure of the protective gas is 1-2 MPa.
In the invention, the thermite precast block does not need external energy after being ignited and can automatically maintain the combustion reaction.
And after the reaction is finished, an upper-lower layered material is obtained, the upper layer is a high-emissivity complex-phase ceramic layer made of alumina and ferrochrome spinel, and the lower layer is FeCrCoNi high-entropy alloy.
The preparation time of the FeCrCoNi high-entropy alloy and the high-emissivity complex phase ceramic is less than 30 min.
Any of the raw materials described in the present invention can be obtained by commercially available methods unless otherwise specified.
The invention has the following beneficial effects:
the method adopted by the patent realizes the ultrahigh temperature through the chemical heat released by the strong exothermic aluminothermic combustion reaction, quickly realizes the self-purification and strong mass transfer of the melt, utilizes the high-pressure atmosphere to inhibit the volatilization of elements and the splashing of the melt, and simultaneously realizes the separation and solidification of ceramics and high-entropy alloy materials with different densities under the action of gravity and wettability difference. The high-entropy alloy is obtained after separation, and the generated ceramic is alumina and ferrochrome spinel complex-phase ceramic with high infrared emissivity.
The raw materials adopted by the method are oxides and Al powder, the price of the oxides is lower, and the requirement on purity is lower; the formed products are high-entropy alloy and complex phase ceramic which are automatically separated.
The method for preparing the high-emissivity complex phase ceramic and the FeCrCoNi high-entropy alloy in one step is rapid and efficient, the preparation process is pollution-free, the energy consumption is low, the raw materials are fully utilized, the relative density of the prepared FeCrCoNi high-entropy alloy material is more than 95%, and the phase composition is a single FCC phase; the emissivity of the prepared ceramic complex phase in the wavelength range of 250 nm-2500 nm is more than 0.88.
Description of the drawings:
FIG. 1 shows the X-ray diffraction pattern of FeCrCoNi high-entropy alloy and ceramic complex phase prepared in example 1 of the present invention.
FIG. 2 shows an emissivity spectrum of the complex phase ceramic prepared in the embodiment 1 of the invention in a wavelength range of 250nm to 2500 nm.
The specific implementation mode is as follows:
the technical scheme adopted by the invention is as follows:
firstly, mixing Fe2O3、Cr2O3、Co2O3Drying NiO and Al raw material powder, uniformly mixing and compacting to obtain a thermite precast block with the relative density of 40-60%;
secondly, the obtained thermite prefabricated block is put into a crucible and is placed in high-pressure combustion reaction equipment;
vacuumizing the reaction equipment until the vacuum degree is less than 1000Pa, filling protective gas, and igniting the aluminothermic precast block by utilizing an electrified tungsten spiral wire to initiate a combustion synthesis reaction;
fourthly, after the reaction is finished, the product is automatically layered, the lower layer is a high-entropy alloy layer, and the upper layer is a ceramic layer.
The molar mass ratio of each raw material in the thermite precast block is Fe2O3：Cr2O3：Co2O3: NiO: al = 1+2 x: 1+ x: 1: 2: 8, wherein x is more than or equal to 0.15 and less than or equal to 0.20.
Unless otherwise specified, any of the powders described in the present invention means a powder having a purity of 99.5% or more and a particle size of 325 mesh.
The protective gas is argon, and the initial pressure of the protective gas is 1-2 MPa.
In the invention, the thermite precast block does not need external energy after being ignited and can automatically maintain the combustion reaction.
And after the reaction is finished, an upper-lower layered material is obtained, the upper layer is a high-emissivity complex-phase ceramic layer made of alumina and ferrochrome spinel, and the lower layer is FeCrCoNi high-entropy alloy.
The preparation time of the FeCrCoNi high-entropy alloy and the high-emissivity complex phase ceramic is less than 30 min.
Example 1;
mixing Fe2O3、Cr2O3、Co2O3And uniformly mixing NiO and Al powder, drying and compacting to obtain the thermite precast block with the relative density of 50%. The molar mass ratio of each raw material in the thermite precast block is Fe2O3：Cr2O3：Co2O3: NiO: al = 1.3: 1.15: 1: 2: 8 (x = 0.15). And (3) putting the obtained thermite precast block into a corundum crucible and placing the corundum crucible into a high-pressure reaction kettle. Vacuumizing to vacuum degree<1000Pa, then argon gas was introduced until the argon pressure was 1 MPa. The exothermic reaction of the thermite prefabricated block is induced by the heating of the electrified tungsten spiral wire. The aluminothermic reaction obtains a product which is layered up and down, the upper layer is ceramic powder, and the lower layer is an alloy block. Separating to obtain upper ferrochrome spinel powder and lower ferrochrome spinel powderAnd (3) gold blocks.
After the obtained high-entropy alloy sample is tested and analyzed, the relative compactness is 96.4%, the main phase is an FCC multi-component solid solution phase, no second-phase diffraction peak is observed, a small amount of slag inclusion and pores exist in the alloy, and the metal elements of each component are close to the design ratio of 1:1:1: 1; the surplus chromium and iron oxide enter into the alumina ceramic phase to form ferrochrome spinel, and the ferrochrome spinel form the multiphase ceramic.
Example 2;
mixing Fe2O3、Cr2O3、Co2O3And uniformly mixing the NiO powder and the Al powder, drying and compacting to obtain the thermite precast block with the relative density of 40%. The molar mass ratio of each raw material in the thermite precast block is Fe2O3：Cr2O3：Co2O3: NiO: al = 1.34: 1.17: 1: 2: 8 (x = 0.17). And (3) putting the obtained thermite precast block into a corundum crucible and placing the corundum crucible into a high-pressure reaction kettle. Vacuumizing to vacuum degree<1000Pa, then argon gas was introduced until the argon pressure was 1.5 MPa. The exothermic reaction of the thermite prefabricated block is induced by the heating of the electrified tungsten spiral wire. The aluminothermic reaction obtains a product which is layered up and down, the upper layer is ceramic powder, and the lower layer is an alloy block. Separating to obtain the upper-layer ferrochrome spinel powder and the lower-layer high-entropy alloy block.
After the obtained high-entropy alloy sample is tested and analyzed, the relative density is 95.7%, the main phase is an FCC multi-component solid solution phase, no second-phase diffraction peak is observed, a small amount of slag inclusion and pores exist in the alloy, and the metal elements of each component are close to the design ratio of 1:1:1: 1; the surplus chromium and iron oxide enter into the alumina ceramic phase to form ferrochrome spinel, and the ferrochrome spinel form the multiphase ceramic.
Example 3;
mixing Fe2O3、Cr2O3、Co2O3And uniformly mixing NiO and Al powder, drying and compacting to obtain the thermite precast block with the relative density of 60%. The molar mass ratio of each raw material in the thermite precast block is Fe2O3：Cr2O3：Co2O3: NiO: al = 1.4: 1.2: 1: 2: 8 (x = 0.2). And (3) putting the obtained thermite precast block into a corundum crucible and placing the corundum crucible into a high-pressure reaction kettle. Vacuumizing to vacuum degree<1000Pa, then argon is filled until the argon pressure is 2 MPa. The exothermic reaction of the thermite prefabricated block is induced by the heating of the electrified tungsten spiral wire. The aluminothermic reaction obtains a product which is layered up and down, the upper layer is ceramic powder, and the lower layer is an alloy block. Separating to obtain the upper-layer ferrochrome spinel powder and the lower-layer high-entropy alloy block.
After the obtained high-entropy alloy sample is tested and analyzed, the relative density is 95.3%, the main phase is an FCC multi-component solid solution phase, no second-phase diffraction peak is observed, a small amount of slag inclusion and pores exist in the alloy, and the metal elements of each component are close to the design ratio of 1:1:1: 1; the surplus chromium and iron oxide enter into the alumina ceramic phase to form ferrochrome spinel, and the ferrochrome spinel form the multiphase ceramic.
Claims (3)
1. The method for preparing the high-emissivity complex phase ceramic and the FeCrCoNi high-entropy alloy in one step is characterized by comprising the following steps of: mixing Fe2O3、Cr2O3、Co2O3The NiO and Al raw material powder are dried, uniformly mixed and pressed into a compact to obtain a thermite precast block with the relative density of 40-60%; putting the obtained thermite precast block into a crucible and placing the crucible into high-pressure combustion reaction equipment; vacuumizing the reaction equipment, filling protective gas, and igniting the aluminothermic precast blocks by utilizing an electrified tungsten spiral wire to initiate a combustion synthesis reaction; after the reaction is finished, the product is automatically layered, the upper layer is a high-emissivity complex-phase ceramic layer, and the lower layer is a high-entropy alloy layer; the molar ratio of each raw material in the thermite precast block is Fe2O3：Cr2O3：Co2O3: NiO: al ═ 1+2 x: 1+ x: 1: 2: 8, wherein x is more than or equal to 0.15 and less than or equal to 0.20.
2. The method for preparing the high-emissivity complex phase ceramic and the FeCrCoNi high-entropy alloy in one step according to claim 1, wherein the method comprises the following steps: the prepared upper-layer high-emissivity complex-phase ceramic comprises alumina and ferrochrome spinel, and the lower-layer high-entropy alloy layer comprises FeCrCoNi high-entropy alloy.
3. The method for preparing the high-emissivity complex phase ceramic and the FeCrCoNi high-entropy alloy in one step according to claim 1, wherein the method comprises the following steps: the protective gas is argon, and the initial pressure of the protective gas is 1-2 MPa.
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| CN111349838B (en) * | 2018-12-24 | 2021-07-27 | 中国科学院理化技术研究所 | Preparation method of high-entropy alloy composite material |
| CN111101045A (en) * | 2020-01-03 | 2020-05-05 | 余果润 | High-entropy alloy material and preparation method thereof |
| CN114411008A (en) * | 2020-10-28 | 2022-04-29 | 中国科学院理化技术研究所 | Preparation method of high-entropy alloy composite material |
| CN113511693B (en) * | 2021-07-19 | 2023-03-14 | 中国科学院兰州化学物理研究所 | Colored spinel type high-entropy oxide (NiFeCrM) 3 O 4 Synthesis method |
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