A rapid solid-phase synthesis method of molybdenum antimonide-based material

Abstract

This invention relates to a method for rapidly preparing molybdenum antimonide-based materials using a combination of mechanical alloying, cold pressing, and ultrafast heat treatment. It is a method for rapidly preparing molybdenum antimonide-based materials using a pure solid-state reaction. The aim is to solve the problems of long preparation cycles, high energy consumption, and complex process control associated with existing traditional melt-annealing-hot pressing sintering methods for preparing molybdenum antimonide-based materials. The method includes: 1. Pre-treating the molybdenum antimonide-based raw materials using mechanical alloying, and then cold-pressing the resulting mechanically alloyed powder into a block; 2. Applying an ultrafast heat treatment method based on the Joule heating principle to the cold-pressed block to obtain the final molybdenum antimonide-based material; the molybdenum antimonide-based materials include, but are not limited to, Mo3Sb7 and Mo3Sb. 7‑x M x (M=Te,Se), Mo 3‑x Re x Sb7, Mo 3‑x Ru x Sb7, Mo 2.5 Ru 0.5 Sb 7–x Te x Ni x Mo 3‑y Ni y Sb7、A 0.05 Mo3Sb 5.4 Te 1.6 (A = Mn, Fe, Co, Ni). This invention utilizes a combination of mechanical alloying, cold pressing, and ultrafast heat treatment to simply and rapidly prepare molybdenum antimonide-based materials. This invention is applicable to the large-scale rapid preparation of molybdenum antimonide-based materials in the fields of thermoelectric materials, catalytic materials, nano-ion battery electrodes, and superconductivity.

Description

Technical Field

[0001] This invention relates to a rapid solid-phase synthesis method for molybdenum antimonide-based materials, which can be applied to the large-scale rapid preparation of molybdenum antimonide-based materials in fields such as thermoelectric materials, catalytic materials, nano-ion battery electrodes, and superconducting technology. Background Technology

[0002] Molybdenum antimonide (MoSb) materials, as novel materials with unique properties, have demonstrated their potential and application value in multiple fields in recent years. Currently, MoSb has been found to exhibit superconductivity at 2.08 K, and magnetization measurements indicate that Mo3Sb7 is a bulk π-type superconductor. In the field of thermoelectric materials, doping Mo3Sb7 with atoms having a high number of valence electrons can adjust the carrier concentration and mobility, thereby increasing the ZT value and optimizing its thermoelectric performance, providing a new approach for the development of high-efficiency thermoelectric materials. Furthermore, MoSb-based materials can replace platinum group metals as catalysts for the hydrogen evolution reaction, effectively reducing the cost of water electrolysis for hydrogen production. Simultaneously, MoSb-based materials possess high theoretical capacity, providing ultra-high sodium storage capacity for sodium-ion batteries. Their excellent electrochemical reversibility allows them to maintain stable performance during charging, contributing to improved battery cycle life and showing broad application prospects in the sodium-ion battery field.

[0003] Current methods for preparing molybdenum antimonide-based materials mainly involve first melting the raw materials into a liquid state, then cooling and subjecting them to prolonged annealing for hundreds of hours, sometimes with additional quenching steps. This method requires multiple prolonged heating processes, which can easily lead to complex reactions and the introduction of impurity phases. Furthermore, the large melting point differences among the elements in molybdenum antimonide-based materials cause elemental volatilization during heating, making it difficult to precisely control the phase composition of the product. Additionally, the preparation cycle is long and energy consumption is high. Alternatively, pure molybdenum antimonide single crystals can be obtained using a peritectic reaction between metallic molybdenum and liquid antimony; however, this method is complex and unsuitable for applications requiring semiconductor doping of molybdenum antimonide in thermoelectric materials and other fields. Therefore, there is an urgent need to develop a method for rapidly preparing pure-phase molybdenum antimonide-based materials through solid-state reactions. Currently, no methods have been reported for rapidly preparing molybdenum antimonide-based materials through a fully solid-state reaction via mechanical alloying pre-reaction followed by cold pressing and ultrafast heat treatment. Summary of the Invention

[0004] The purpose of this invention is to solve the problems of complex processes, long preparation cycles, high energy consumption, and easy inclusion of impurity phases in existing methods for preparing molybdenum antimonide-based materials. This invention proposes a rapid solid-state synthesis method for molybdenum antimonide-based materials that combines mechanical alloying, cold pressing, and ultrafast heat treatment.

[0005] The preparation method of this invention, which combines mechanical alloying, cold pressing, and ultrafast heat treatment, is carried out according to the following steps:

[0006] Step 1: Pretreatment of molybdenum antimonide-based raw materials using mechanical alloying. First, the raw materials are weighed according to the stoichiometric ratio. The raw materials, process control agent, and grinding balls are then placed into the mechanical alloying tank. Ball milling ensures uniform mixing of the raw materials at near room temperature and under a specific atmosphere, promoting atomic diffusion and alloying reactions between powder particles to generate high-surface-energy nanoparticles.

[0007] Step 2: The obtained mechanically alloyed powder is loaded into a cold-pressing mold and subjected to pressure for cold pressing. Cold pressing compresses the gaps between nanomaterials to obtain dense blocks of different shapes, so that the next solid-state reaction can proceed rapidly. The cold-pressed blocks are subjected to ultrafast heat treatment based on the Joule heating principle. During the ultrafast heating, ultrashort holding time and rapid cooling process, the cold-pressed blocks achieve complete phase transformation in the solid state in an extremely short heat treatment cycle. This avoids element volatilization caused by the large differences in melting and boiling points between the elements of the molybdenum antimonide-based material, and precisely controls the phase composition of the product to obtain the final pure phase of the molybdenum antimonide-based material.

[0008] The mechanical alloying method aims to pre-alloy and nano-size raw materials at near room temperature, including but not limited to ball milling methods;

[0009] The process control agents include, but are not limited to: ethanol, methanol, acetone, etc.

[0010] The atmospheric environment includes, but is not limited to, argon, helium, nitrogen, and air.

[0011] The dense blocks of different shapes include, but are not limited to: cylindrical, cuboid, triangular prism and other complex shapes;

[0012] The molybdenum antimonide-based materials include, but are not limited to, Mo3Sb7 and Mo3Sb. 7-x M x (M=Te,Se), Mo 3-x Re x Sb7, Mo 3- x Ru x Sb7, Mo 2.5 Ru 0.5 Sb 7–x Te x Ni x Mo 3-y Ni y Sb7、A 0.05 Mo3Sb 5.4 Te 1.6 (A=Mn, Fe, Co, Ni).

[0013] The principle and beneficial effects of this invention are as follows:

[0014] This invention utilizes mechanical alloying pre-reaction followed by cold pressing and ultrafast heat treatment to achieve rapid preparation of molybdenum antimonide-based materials through a fully solid-phase reaction. This effectively avoids the presence of impurity phases in the generated products. Furthermore, the process is simple to control, consumes little energy, and has low equipment requirements, enabling large-scale rapid preparation.

[0015] The reason why the solid-state reaction effectively avoids the presence of impurity phases in the generated products is that this invention uses, but is not limited to, high-energy ball milling to perform mechanical alloying pretreatment on molybdenum antimony-based raw materials under low-temperature conditions to obtain nanoscale products. The raw material, molybdenum antimony-based metal powder, undergoes a series of processes such as powder deformation, refinement, interatomic diffusion, and solid-state reaction under the continuous impact and friction of the grinding balls in a ball mill jar under a specific atmosphere. Mechanical alloying is mainly achieved through mechanical force to achieve solid-state alloying, rather than through chemical reactions of molten raw materials at high temperatures to generate new compounds, effectively avoiding impurity phases introduced by complex chemical reactions. Using an ultrafast heat treatment method based on the Joule heating principle for cold-pressed blocks can achieve ultrafast heating and cooling rates, significantly shortening side reactions during heating and cooling processes, while reducing grain growth within the material. This ensures that the material undergoes complete phase transformation in the solid state throughout the process, avoiding element volatilization caused by excessive differences in melting points between molybdenum antimony-based materials, precisely controlling the phase composition of the product, and obtaining the final pure phase of the molybdenum antimony-based material.

[0016] The reason for the simple process control and short preparation cycle is that this invention uses mechanical alloying to pre-alloy and nanostructure molybdenum antimony-based raw materials at near room temperature. The alloying process can be easily and precisely controlled by adjusting parameters such as ball mill speed and time, achieving atomic-level uniform mixing of raw materials without the need for prolonged high-temperature melting (tens of hours). The resulting nanostructured powder is then placed in a cold-pressing mold and subjected to pressure. Cold pressing compresses the gaps between the alloyed nanoparticles, increasing the contact area and promoting solid-phase reactions during ultrafast heat treatment. Simultaneously, cold pressing has low equipment requirements and can accommodate various shapes of molybdenum antimony-based materials. The ultrafast heat treatment method based on Joule heating for the cold-pressed block achieves millisecond-level rapid heating, cooling, and holding, eliminating the need for lengthy annealing (hundreds of hours) to obtain the final molybdenum antimony-based material. Therefore, molybdenum antimony-based materials can be prepared simply and rapidly.

[0017] This invention utilizes mechanical alloying and ultrafast heat treatment to achieve rapid preparation of molybdenum antimonide-based materials. The process is simple to control, requires low equipment and consumes little energy, making it suitable for mass production. Attached Figure Description

[0018] Figure 1 This is the X-ray diffraction pattern obtained in Example 1. Detailed Implementation

[0019] Specific Implementation Method 1: The rapid solid-state synthesis method of molybdenum antimonide-based materials combining mechanical alloying, cold pressing, and ultrafast heat treatment according to the present invention is carried out according to the following steps:

[0020] Step 1: Pre-treat the molybdenum antimonide-based raw materials using mechanical alloying. First, weigh the raw materials according to the stoichiometric ratio, then place the raw materials, process control agent, and grinding balls into the mechanical alloying tank. Ball milling ensures uniform mixing of the raw materials at near room temperature and in a specific atmosphere, promoting atomic diffusion and alloying reactions between powder particles to generate high-surface-energy nanoparticles.

[0021] Step 2: The obtained mechanically alloyed powder is loaded into a cold-pressing mold and subjected to pressure for cold pressing. Cold pressing compresses the gaps between nanomaterials to obtain dense blocks of different shapes, so that the next solid-state reaction can proceed rapidly. The cold-pressed blocks are subjected to ultrafast heat treatment based on the Joule heating principle. During the ultrafast heating, ultrashort holding time and rapid cooling process, the cold-pressed blocks achieve complete phase transformation in the solid state in an extremely short heat treatment cycle. This avoids element volatilization caused by the large differences in melting and boiling points between the elements of the molybdenum antimonide-based material, and precisely controls the phase composition of the product to obtain the final pure phase of the molybdenum antimonide-based material.

[0022] The mechanical alloying method aims to pre-alloy and nano-size raw materials at near room temperature, including but not limited to ball milling methods;

[0023] The process control agents include, but are not limited to: ethanol, methanol, acetone, etc.

[0024] The atmospheric environment includes, but is not limited to, argon, helium, nitrogen, and air.

[0025] The dense blocks of different shapes include, but are not limited to: cylindrical, cuboid, triangular prism and other complex shapes;

[0026] The molybdenum antimonide-based materials include, but are not limited to, Mo3Sb7 and Mo3Sb. 7-x M x (M=Te,Se), Mo 3-x Re x Sb7, Mo 3- x Ru x Sb7, Mo 2.5 Ru 0.5 Sb 7–x Te x Ni x Mo 3-y Ni y Sb7、A 0.05 Mo3Sb5.4 Te 1.6 (A=Mn, Fe, Co, Ni).

[0027] Specific Implementation Method Two: This implementation method differs from Specific Implementation Method One in that the mechanical alloying process described in step one is as follows: First, weigh the raw materials according to the stoichiometric ratio, then put the raw materials, process control agent and grinding balls into the ball mill jar in a glove box filled with argon gas, and then seal the ball mill jar and put it into the ball mill for mechanical alloying, setting parameters such as a ball milling speed of not less than 100 rpm and a ball milling time of not less than 1 min.

[0028] Specific Implementation Method 3: This implementation method differs from Specific Implementation Method 1 or 2 in that the cold pressing process described in step 2 is as follows: The obtained mechanical alloyed powder is loaded into a cold pressing mold and subjected to a pressure of not less than 50MPa for cold pressing to obtain dense blocks of different shapes.

[0029] Specific Implementation Method Four: This implementation method differs from Specific Implementation Methods One to Three in that the molybdenum antimonide-based material mentioned in step two includes, but is not limited to, Mo3Sb7 and Mo3Sb. 7-x M x (M=Te,Se), Mo 3-x Re x Sb7, Mo 3-x Ru x Sb7, Mo 2.5 Ru 0.5 Sb 7–x Te x Ni x Mo 3-y Ni y Sb7、A 0.05 Mo3Sb 5.4 Te 1.6 (A=Mn, Fe, Co, Ni).

[0030] Specific Implementation Method Five: This implementation method differs from Specific Implementation Methods One to Four in that the ultrafast heat treatment process described in step two is as follows: The ultrafast heat treatment is carried out in an ultrafast high-temperature furnace, and the atmosphere of the ultrafast high-temperature furnace is a vacuum or other protective atmosphere. When the ultrafast high-temperature furnace is in a vacuum state, the vacuum degree of the furnace cavity is not less than 1.0 × 10⁻⁶. -3 Pa, other protective atmospheres include but are not limited to argon, helium and nitrogen. First, heat to 600~800℃ at a rate of not less than 50℃ / s, hold at this temperature for not less than 5s, and then rapidly cool to room temperature at a rate of not less than 50℃ / s.

[0031] Example 1: This invention prepares Mo3Sb7 using a combination of mechanical alloying, cold pressing, and ultrafast heat treatment, following these steps:

[0032] Step 1: Pretreatment of molybdenum antimonide-based raw materials using mechanical alloying. First, weigh the raw materials Mo and Sb according to a stoichiometric ratio of 3:7. Then, place the raw materials, process control agent, and grinding balls into a mechanical alloying tank. Ball milling ensures uniform mixing of the raw materials at near room temperature and under a specific atmosphere, promoting atomic diffusion and alloying reactions between powder particles to generate high-surface-energy nanoparticles.

[0033] The mechanical alloying process described in step one is as follows: Mo and Sb are mixed in a stoichiometric ratio of 3:7 according to the chemical formula Mo3Sb7. Then, the raw materials, process control agent and grinding balls are placed into a ball mill jar in an argon-filled glove box. The ball mill jar is then sealed and placed into a ball mill for mechanical alloying. The ball milling program is set to 30min×30, for a total of 30 ball milling cycles. There is a 15min pause between each rotation cycle, and then the next cycle of ball milling is carried out, for a total ball milling time of 15 hours.

[0034] Step 2: The obtained mechanically alloyed powder is loaded into a cold-pressing mold and subjected to pressure for cold pressing. Cold pressing compresses the gaps between nanomaterials to obtain dense blocks of different shapes, so that the next solid-state reaction can proceed rapidly. The cold-pressed blocks are subjected to ultrafast heat treatment based on the Joule heating principle. During the ultrafast heating, ultrashort holding time and rapid cooling process, the cold-pressed blocks achieve complete phase transformation in the solid state in an extremely short heat treatment cycle. This avoids element volatilization caused by the large differences in melting and boiling points between the elements of the molybdenum antimonide-based material, and precisely controls the phase composition of the product to obtain the final pure phase of the molybdenum antimonide-based material.

[0035] The cold pressing process described in step two is as follows: mechanically alloyed powder is loaded into a cold pressing mold, and a pressure of 150MPa is applied by a cold press to compress the gaps between the nanomaterials to obtain dense blocks of different shapes.

[0036] The ultrafast heat treatment process described in step two is as follows: the ultrafast heat treatment is carried out in an ultrafast high-temperature furnace, the atmosphere of which is a vacuum or Ar protective atmosphere, and when the ultrafast high-temperature furnace is in a vacuum state, the vacuum degree of the furnace cavity is less than 2.2 × 10⁻⁶. -3 Pa, Ar gas pressure in the heating furnace under Ar protective atmosphere is -0.07 MPa; first, it is heated to 650℃ at a rate of 60℃ / s and held for 30s, then cooled to room temperature at a rate of 60℃ / s.

[0037] Figure 1 The X-ray diffraction pattern obtained in Example 1 is as follows: Figure 1 As shown, by comparing the standard XRD pattern, it can be seen that the obtained material is a single phase of molybdenum antimonide.

[0038] Example 2:

[0039] This invention utilizes a combination of mechanical alloying, cold pressing, and ultrafast heat treatment to prepare Mo3Sb. 5.4 Te 1.6 Follow these steps:

[0040] Step 1: Pretreatment of molybdenum antimonide-based raw materials using mechanical alloying. First, weigh the raw materials Mo, Sb, and Te according to a stoichiometric ratio of 3:5.4:1.6. Place the raw materials, process control agent, and grinding balls into the mechanical alloying tank. Ball milling ensures uniform mixing of the raw materials at near room temperature and under a specific atmosphere, promoting atomic diffusion and alloying reactions between powder particles to generate high-surface-energy nanoparticles.

[0041] The mechanical alloying process described in step one is as follows: Mo, Sb, and Te are alloyed according to the chemical formula Mo3Sb. 5.4 Te 1.6 The raw materials, process control agent, and grinding balls were mixed in a chemical stoichiometric ratio of 3:5.4:1.6. Then, in an argon-filled glove box, the raw materials, process control agent, and grinding balls were placed into a ball mill jar. The ball mill jar was then sealed and placed into a ball mill for mechanical alloying. The ball milling program was set to 60min × 15, for a total of 15 ball milling cycles. There was a 15min pause between each rotation cycle before starting the next cycle, for a total ball milling time of 15 hours.

[0042] Step 2: The obtained mechanically alloyed powder is loaded into a cold-pressing mold and subjected to pressure for cold pressing. Cold pressing compresses the gaps between nanomaterials to obtain dense blocks of different shapes, so that the next solid-state reaction can proceed rapidly. The cold-pressed blocks are subjected to ultrafast heat treatment based on the Joule heating principle. During the ultrafast heating, ultrashort holding time and rapid cooling process, the cold-pressed blocks achieve complete phase transformation in the solid state in an extremely short heat treatment cycle. This avoids element volatilization caused by the large differences in melting and boiling points between the elements of the molybdenum antimonide-based material, and precisely controls the phase composition of the product to obtain the final pure phase of the molybdenum antimonide-based material.

[0043] The cold pressing process described in step two is as follows: mechanically alloyed powder is loaded into a cold pressing mold, and a pressure of 200MPa is applied by a cold press to compress the gaps between the nanomaterials to obtain dense blocks of different shapes.

[0044] The ultrafast heat treatment process described in step two is as follows: the ultrafast heat treatment is carried out in an ultrafast high-temperature furnace, the atmosphere of which is a vacuum or Ar protective atmosphere, and when the ultrafast high-temperature furnace is in a vacuum state, the vacuum degree of the furnace cavity is less than 2.2 × 10⁻⁶. -3Pa, the Ar gas pressure in the heating furnace is -0.07 MPa when the protective atmosphere is Ar; first, it is heated to 750℃ at a rate of 80℃ / s and held for 60s, and then cooled to room temperature at a rate of 80℃ / s.

[0045] X-ray diffraction analysis revealed that the obtained Mo3Sb 5.4 Te 1.6 It is single-phase.

[0046] Example 3:

[0047] This invention utilizes a combination of mechanical alloying, cold pressing, and ultrafast heat treatment to prepare Mo. 2.2 Ru 0.8 Sb7, proceed with the following steps:

[0048] Step 1: Pretreatment of molybdenum antimonide-based raw materials using mechanical alloying. First, weigh the raw materials Mo, Sb, and Ru according to a stoichiometric ratio of 2.2:0.8:7. Place the raw materials, process control agent, and grinding balls into the mechanical alloying tank. Ball milling ensures uniform mixing of the raw materials at near room temperature and under a specific atmosphere, promoting atomic diffusion and alloying reactions between powder particles to generate high-surface-energy nanoparticles.

[0049] The mechanical alloying process described in step one is as follows: Mo, Sb, and Ru are alloyed according to the chemical formula Mo... 2.2 Ru 0.8 The raw materials, process control agent, and grinding balls were mixed in a stoichiometric ratio of 2.2:0.8:7 in Sb7. Then, the raw materials, process control agent, and grinding balls were placed into a ball mill jar in an argon-filled glove box. The ball mill jar was then sealed and placed into a ball mill for mechanical alloying. The ball milling program was set to 30 min × 30, for a total of 30 ball milling cycles. There was a 15-minute pause between each rotation cycle before starting the next cycle, for a total ball milling time of 15 hours.

[0050] Step 2: The obtained mechanically alloyed powder is loaded into a cold-pressing mold and subjected to pressure for cold pressing. Cold pressing compresses the gaps between nanomaterials to obtain dense blocks of different shapes, so that the next solid-state reaction can proceed rapidly. The cold-pressed blocks are subjected to ultrafast heat treatment based on the Joule heating principle. During the ultrafast heating, ultrashort holding time and rapid cooling process, the cold-pressed blocks achieve complete phase transformation in the solid state in an extremely short heat treatment cycle. This avoids element volatilization caused by the large differences in melting and boiling points between the elements of the molybdenum antimonide-based material, and precisely controls the phase composition of the product to obtain the final pure phase of the molybdenum antimonide-based material.

[0051] The cold pressing process described in step two is as follows: mechanically alloyed powder is loaded into a cold pressing mold, and a pressure of 350MPa is applied by a cold press to compress the gaps between the nanomaterials to obtain dense blocks of different shapes.

[0052] The ultrafast heat treatment process described in step two is as follows: the ultrafast heat treatment is carried out in an ultrafast high-temperature furnace, the atmosphere of which is a vacuum or Ar protective atmosphere, and when the ultrafast high-temperature furnace is in a vacuum state, the vacuum degree of the furnace cavity is less than 2.2 × 10⁻⁶. -3 Pa, the Ar gas pressure in the heating furnace is -0.07 MPa when the protective atmosphere is Ar; first, it is heated to 800℃ at a rate of 90℃ / s and held for 120s, and then cooled to room temperature at a rate of 90℃ / s.

[0053] The obtained Mo was detected by X-ray diffraction. 2.2 Ru 0.8 Sb7 is a single phase.

Claims

1. A rapid solid-state synthesis method for molybdenum antimonide-based materials, characterized in that: Mo was prepared by combining mechanical alloying, cold pressing and ultrafast heat treatment. 2.2 Ru 0.8 Sb7, proceed with the following steps; I. Pretreatment of molybdenum antimonide-based raw materials using mechanical alloying: First, Mo, Ru, and Sb are weighed according to a stoichiometric ratio of 2.2:0.8:

7. The raw materials, process control agent, and grinding balls are placed into a mechanical alloying tank. Ball milling is used to ensure uniform mixing of the raw materials at near room temperature and under a specific atmosphere, promoting atomic diffusion and alloying reactions between powder particles to generate nanoparticles with high surface energy. Then, the obtained mechanically alloyed powder is placed into a cold pressing mold and subjected to a pressure of 350 MPa for cold pressing. Cold pressing compresses the gaps between nanomaterials to obtain dense blocks of different shapes, so that the subsequent solid-phase reaction can proceed rapidly. The mechanical alloying process described in step one is as follows: Mo, Ru, and Sb are alloyed according to the chemical formula Mo... 2.2 Ru 0.8 The raw materials, process control agent and grinding balls were mixed in a stoichiometric ratio of 2.2:0.8:7 in Sb7. Then, the raw materials, process control agent and grinding balls were put into the ball mill jar in an argon-filled glove box. The ball mill jar was then sealed and put into a ball mill for mechanical alloying. The ball milling program was set to 30min×30, for a total of 30 ball milling cycles. There was a 15min pause between each rotation cycle before the next cycle was started, for a total ball milling time of 15 hours. The cold pressing process described in step one is as follows: mechanically alloyed powder is loaded into a cold pressing mold, and a pressure of 350MPa is applied by a cold press to press the powder into a block. Second, the cold-pressed block is subjected to ultra-fast heat treatment based on the Joule heating principle. During the ultra-fast heating, ultra-short holding time and rapid cooling process, the cold-pressed block can achieve a complete phase transformation in the solid state with an extremely short heat treatment cycle. This avoids the phenomenon of element volatilization caused by the large difference in melting point and boiling point between the elements of the molybdenum antimonide-based material. It also precisely controls the phase composition of the product and obtains the final pure phase of the molybdenum antimonide-based material. The ultrafast heat treatment process described in step two is as follows: the ultrafast heat treatment is carried out in an ultrafast high-temperature furnace, the atmosphere of which is a vacuum or Ar protective atmosphere, and when the ultrafast high-temperature furnace is in a vacuum state, the vacuum degree of the furnace cavity is less than 2.2 × 10⁻⁶. -3 Pa, the Ar gas pressure in the ultrafast high-temperature furnace under an Ar protective atmosphere is -0.07 MPa; firstly, it is heated to 800℃ at a rate of 90℃ / s and held for 120s, then cooled to room temperature at a rate of 90℃ / s; the obtained Mo is detected by X-ray diffraction. 2.2 Ru 0.8 Sb7 is a single phase.

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