A method and device for preparing nickel-phosphorus alloy

Abstract

The present invention discloses a method and device for preparing a nickel-phosphorus alloy, and relates to the technical field of intermediate alloy preparation. The device for preparing the nickel-phosphorus alloy comprises: a smelting system, a feeding system and a vacuum system, wherein the smelting system comprises a smelting crucible and a cooling mold, the feeding system comprises a phosphorus storage tank and a gas source, and the vacuum system comprises two parts, a vacuum system 1 and a vacuum system 2. The device mainly adopts a phosphorus blowing method to send red phosphorus powder into a nickel liquid in a vacuum environment for reaction, thereby preparing a nickel-phosphorus alloy. The preparation of the nickel-phosphorus alloy includes the processes of vacuuming the smelting system and the phosphorus storage tank, heating and melting nickel blocks, conveying phosphorus powder, segmented temperature control, and refining and pouring. The present invention greatly reduces the amount of phosphorus burnout during the smelting process of the nickel-phosphorus alloy through the phosphorus blowing method and the segmented temperature control smelting method, and can significantly improve the phosphorus yield in the alloy; and the preparation device of the present invention is simple in design, has low material requirements for the device, and is easy to promote on an industrial scale.

Description

Technical Field

[0001] The present invention relates to the technical field of intermediate alloy materials, and in particular to a method and device for preparing a nickel-phosphorus alloy. Background Art

[0002] Relevant research on alloys such as GH761, GH4169G, GH4169D, and IN600 has shown that if the phosphorus content can be controlled within a certain range, the rupture and creep properties of this type of high-temperature alloy can be significantly improved. In addition, a small amount of phosphorus has a certain promoting effect on the forging properties of nickel-based high-temperature alloys. Therefore, during the smelting process of nickel-based high-temperature alloys, an appropriate amount of phosphorus is often added as a microalloying element to improve the alloy properties. However, elemental phosphorus has a low ignition point (white phosphorus 40°C, red phosphorus 260°C). Adding it in the form of elemental phosphorus has the problems of high burnout and low phosphorus yield. Moreover, during the addition process, phosphorus is exposed to oxygen and high temperature environment at the same time, which easily generates highly toxic yellow phosphorus and P2O5 gas, which endangers the health of operators. Therefore, nickel-phosphorus alloys are often used in industry to introduce phosphorus into high-temperature alloys.

[0003] In the prior art, nickel-phosphorus alloy preparation methods mainly include: chemical plating, electrochemical deposition, vapor deposition, high-energy ball milling alloying, and direct smelting. For example, patent CN 202210541927.0 discloses a method for preparing nickel-phosphorus alloy by chemical plating. However, the chemical plating solution is complex in composition, and the wastewater poses an environmental pollution risk. Patents CN 85104887A and CN106048567B use electrochemical deposition technology to form a layer of corrosion-resistant nickel-phosphorus alloy on the surface of the plated part. Although the coating formed by this method is dense and easy to operate, both chemical plating and electrochemical deposition techniques can only produce alloy coatings, which seriously limits the application of nickel-phosphorus alloys. Patent CN 102586640A uses high-energy grinding ball impact to induce chemical reactions in raw materials to prepare nickel-phosphorus alloys, but the alloys prepared by this method need to be annealed before the product can be obtained, which has high equipment requirements and a relatively complicated preparation process; Patent CN 202110883837.5 discloses a method for injecting liquid white phosphorus into a molten solution of metallic nickel and nickel-phosphorus alloy to prepare a nickel-phosphorus alloy, but the apparatus required for this method is relatively special, and the equipment required for injecting white phosphorus has high requirements in terms of material and design; Patent CN 103667796A discloses a process for preparing nickel-phosphorus alloys by phosphorus pressing, in which a layer of red sand is covered on red phosphorus powder, a nickel block is placed on the red sand and heated to melt, and then the red sand layer is pierced to allow the nickel and phosphorus to fully react to produce a nickel-phosphorus alloy. However, this method causes severe splashing of the alloy liquid during the process of piercing the red sand layer, which can easily burn people, and the pierced red sand is not cleaned up later, and exists in the alloy to form inclusions, reducing the quality of the alloy.

[0004] Therefore, there is an urgent need to develop a method for preparing bulk nickel-phosphorus alloy with low phosphorus burn-off rate, simple operation and pollution-free process to meet the smelting needs of phosphorus-containing high-temperature alloys. Summary of the Invention

[0005] In view of this, the present invention provides a method and apparatus for preparing nickel-phosphorus alloy, which solves the technical problems in the prior art such as severe phosphorus burnout, incomplete removal of impurities during the process, expensive equipment and complicated operation.

[0006] In order to solve the above technical problems, the present invention specifically provides the following technical solutions:

[0007] A preparation device for a nickel-phosphorus alloy comprises a smelting system, a feeding system and a vacuum system, wherein the smelting system comprises a smelting crucible and a cooling mold, the feeding system comprises a phosphorus storage tank, a gas source and a bubble generator, the feeding system is connected to the bottom of the smelting crucible via a pipeline, and the vacuum system comprises two parts, a vacuum system 1 and a vacuum system 2, wherein the vacuum system 1 is connected to the furnace shell of the smelting system, and the vacuum system 2 is connected to the upper part of the phosphorus storage tank.

[0008] Optionally, the smelting crucible is preferably made of white corundum or magnesia; the cooling mold is made of pure copper with a purity of more than 99.7%, and the mold is provided with a water cooling tank inside.

[0009] Furthermore, in the feeding system, the phosphorus storage tank is used to store red phosphorus powder, and an electromagnetic vibrating feeder is placed between the phosphorus storage tank and the material conveying pipe to control the supply amount of the red phosphorus powder.

[0010] Furthermore, the vacuum system 1 is connected to the furnace shell of the smelting system to ensure the vacuum environment in the smelting system; the vacuum system 2 is connected to the upper part of the phosphorus storage tank to remove the air inside the phosphorus storage tank to ensure that the red phosphorus powder is in a pure vacuum environment, avoiding the phosphorus powder being mixed with air and then transported to the crucible, causing the red phosphorus to oxidize after contact with high temperature, affecting the phosphorus yield and even causing danger.

[0011] Optionally, the gas source is an inert gas source, preferably argon, and nitrogen cannot be used.

[0012] Furthermore, the gas source and the phosphorus storage tank are connected via a pipeline, and a gas flow controller is provided on the pipeline between the gas source and the phosphorus storage tank for adjusting the flow rate of the transported gas.

[0013] Optionally, the bubble generator is placed at the bottom of the crucible and connected to the red phosphorus powder conveying pipeline. The upper surface of the bubble generator is covered with uniform holes, and the hole size is in the range of 150-200 μm. The hole design size is the result of comprehensive consideration of the surface tension of the nickel liquid at the smelting temperature and the particle size of the red phosphorus powder. If the hole size is too large, the nickel liquid will flow into the hole, causing the hole to be blocked. If the hole size is too small, the red phosphorus powder will not be discharged smoothly.

[0014] The present invention also discloses a process for preparing a nickel-phosphorus alloy using the above-mentioned preparation device, which specifically comprises the following steps:

[0015] S1. Weigh the raw material electrolytic nickel block and red phosphorus powder according to the designed nickel-phosphorus alloy grade and weight;

[0016] S2. Place the electrolytic nickel block in a smelting crucible, start vacuum system 1, evacuate the smelting system, and reduce the vacuum degree to below 0.6 Pa (0.001-0.6 Pa); put red phosphorus powder into a phosphorus storage tank, cover the tank, and start vacuum system 2 to evacuate the system, controlling the vacuum degree to below 0.05 Pa (0.001-0.05 Pa);

[0017] S3. Start the power supply of the smelting furnace and gradually increase the temperature to 1550-1600℃ to melt the nickel block. Keep the temperature for 15-20 minutes until the nickel block is completely dissolved. Then, turn on the gas flow controller and electromagnetic feed controller in sequence. After setting the parameters, feed red phosphorus powder into the nickel liquid.

[0018] S4. After heating and holding treatment according to the heating curve, adjust the melting temperature to 1220-1280℃, continue to introduce argon gas for 3-5 minutes, pour the alloy liquid into a pure copper cooling mold, cool it for 1.5-2 hours and then take it out of the furnace to obtain a nickel-phosphorus alloy that meets the requirements.

[0019] It should be noted that the purity of the electrolytic nickel block in step S1 is ≥99.9%, the purity of the red phosphorus powder is ≥99%, and the particle size of the red phosphorus powder is 200-400 mesh.

[0020] Furthermore, in step S3, the inert gas flow rate is adjusted within the range of 1.5-3.0 L / min by a gas flow controller, and the electromagnetic feeding controller is set to make the feeding speed within the range of 10.0-20.0 g / s.

[0021] Furthermore, the heating curve in step S4 is as follows: red phosphorus powder is introduced at 1550-1600°C, and after 53-57% by weight of the red phosphorus powder is introduced, the temperature is lowered to 1150-1200°C and kept warm for 5-10 minutes, then the temperature is raised to 1250-1300°C, the remaining weight of the red phosphorus powder is introduced, and kept warm for 10-15 minutes, and then the temperature is controlled at 1220-1280°C for pouring.

[0022] It is worth noting that according to the Ni-P binary alloy phase diagram, when the phosphorus content is between 0-11%, the liquidus temperature of the NiP alloy gradually decreases as the phosphorus content increases. Therefore, when 0-11% red phosphorus powder is introduced at 1550-1600°C, the melt actually gradually overheats. This overheating is detrimental to the phosphorus yield in the alloy, and phosphorus burnout becomes increasingly severe. Therefore, after adding approximately 11% phosphorus, the melt needs to be cooled to 1150-1200°C. Cooling too low can easily cause the alloy to become viscous or even prematurely solidify, while over-temperature reserve can lead to significant phosphorus burnout. When the phosphorus content is between 11% and 20%, the liquidus of the NiP alloy shows an upward trend, and the liquidus temperature gradually increases. Therefore, the alloy needs to be heated before the remaining red phosphorus powder is introduced, and the temperature after heating should preferably be 100-150°C above the liquidus temperature. In addition, sufficient time must be reserved after each phosphorus-passing stage for the reaction between Ni and P to occur.

[0023] Furthermore, in step S4, the purpose of continuing to introduce argon for a period of time is to stir the melt through small bubbles of inert gas so that the elements in the alloy liquid are evenly distributed.

[0024] Furthermore, in step S4, the cooling water temperature of the pure copper cooling mold is 10-24° C., the flow rate is 7.0-10.0 L / min, and the pouring speed is 2.0-4.0 kg / s.

[0025] It should be noted that the benefits of using a metal copper ingot mold with external circulating water cooling in step S4 are: increasing the cooling intensity of the alloy liquid and reducing the element segregation caused by the large density difference between nickel and phosphorus. The purpose of using rapid casting is also to reduce segregation.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] (1) The present invention adopts vacuum melting, phosphorus blowing method and segmented temperature control mode, which reduces the burning loss of P element and greatly increases the P yield in the alloy.

[0028] (2) The present invention adds phosphorus element to nickel liquid by phosphorus blowing method, which not only reduces the burn-off of P element, but also has simple equipment design and low equipment material requirements, which is conducive to industrial promotion.

[0029] (3) The present invention refines the melt by using small bubbles of inert gas and adopts a rapid pouring and water-cooled copper ingot mold cooling method to reduce the degree of alloy segregation. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are merely embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying any creative work.

[0031] Figure 1 Schematic diagram of the preparation device of nickel-phosphorus alloy of the present invention.

[0032] Figure 1 middle,

[0033] 1- Melting crucible, 2- Cooling mold, 3- Furnace shell, 4- Phosphorus storage tank, 5- Gas source, 6- Bubble generator, 7- Feed controller, 8- Flow controller, 9- Vacuum system 1, 10- Vacuum system 2. DETAILED DESCRIPTION

[0034] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the embodiments of the present invention and the accompanying drawings. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0035] like Figure 1 The device for preparing a nickel-phosphorus alloy shown includes a smelting system, a feeding system, and a vacuum system. The smelting system consists of a smelting crucible 1, a cooling mold 2, and a furnace shell 3. The feeding system mainly includes a phosphorus storage tank 4, a gas source 5, and a bubble generator 6. The vacuum system includes two parts: a vacuum system 1 and a vacuum system 2.

[0036] Among them, the vacuum system 1 is connected to the furnace shell 3 of the smelting system and is used for vacuum treatment inside the smelting system. Because the intermediate alloy products for high-temperature alloys have strict requirements on oxygen and nitrogen content, Ni is easily oxidized under non-vacuum conditions, resulting in excessive oxygen content in the final alloy. Therefore, a vacuum environment is preferred for nickel-phosphorus alloy smelting.

[0037] The cooling mold 2 is used to cool the molten alloy after melting. It is made of pure copper with a purity of at least 99.7% and must have circulating water cooling. The copper cooling mold cavity is preferably 300-500mm thick. These cooling mold designs help reduce the segregation of Ni and P elements. The smelting crucible is preferably made of white corundum or magnesia.

[0038] The feeding system pipeline is connected to the bottom of the melting crucible. The end of the feeding system pipeline in the crucible is connected to a disc-shaped bubble generator 6. The size of the bubble generator is slightly smaller than the inner diameter of the crucible. It is made of high-temperature resistant ceramic material. The upper surface of the bubble generator is covered with uniform holes. The hole size is in the range of 150-200μm. This hole design size is the result of comprehensive consideration of the surface tension of the nickel liquid at the melting temperature and the particle size of the red phosphorus powder. If the hole size is too large, the nickel liquid will flow into the hole, causing the hole to be blocked. If the hole size is too small, the red phosphorus powder will not be discharged smoothly, which will lead to a large amount of red phosphorus powder accumulated inside the bubble generator.

[0039] Phosphorus storage tank 4 is used to store red phosphorus powder. An electromagnetic vibrating feed controller 7 is installed between the tank and the material delivery pipe to precisely control the supply of red phosphorus powder. The upper portion of tank 4 is connected to a vacuum system 2 to remove air from the tank. Because phosphorus has a low ignition point (white phosphorus 40°C, red phosphorus 260°C), when adding phosphorus to the high-temperature melt, it is crucial to ensure that it is not exposed to oxygen to prevent combustion and other hazards.

[0040] Gas source 5 should be an inert gas source, preferably argon. Nitrogen should never be used, as it is an impurity element in the master alloy used for high-temperature alloys and can degrade the performance of the end product. Gas source 5 is connected to phosphorus storage tank 4 via a pipeline. A gas flow controller 8 is installed in the pipeline between the gas source and the phosphorus storage tank to regulate the flow of the delivered gas.

[0041] The device is used as follows: weighed nickel blocks and red phosphorus powder are placed in a crucible and a phosphorus storage tank respectively, vacuum systems 1 and 2 are started, and the smelting system and the phosphorus storage tank are vacuumed respectively; when the vacuum degree in the smelting furnace meets the requirement, the power is started to start smelting; when all the nickel is dissolved in water, the gas flow controller and the electromagnetic feed controller are set, and then the gas source switch, the gas flow controller and the electromagnetic feed controller are sequentially turned on to start blowing red phosphorus powder into the nickel liquid; then, during the powder blowing process, the temperature is strictly controlled according to the temperature control curve of the present invention; after all the red phosphorus powder is blown in, the inert gas is continuously introduced for a certain time; the circulating water in the cooling mold is turned on; after the alloy melt is kept warm for a certain time, the crucible is directly tilted to pour the alloy liquid into the cooling mold; the alloy liquid is taken out of the furnace after cooling for a period of time, and the nickel-phosphorus alloy with the required composition is obtained.

[0042] For a better understanding of the present invention, the present invention is further specifically described below through the following examples, but it should not be understood as limiting the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the above invention content are also considered to fall within the scope of protection of the present invention.

[0043] The technical solution of the present invention will be further described below in conjunction with specific embodiments.

[0044] Example 1 (preparation of 50 kg of NiP20 alloy):

[0045] Weigh 40 kg of 99.9% pure electrolytic nickel blocks and place them in a crucible. Weigh 10 kg of 99.8% pure red phosphorus powder with a particle size of 240-300 mesh and place it in a phosphorus storage tank. Start vacuum systems 1 and 2 to make the vacuum degrees in the smelting furnace and the phosphorus storage tank reach 0.5 Pa and 0.04 Pa respectively. Start the power supply of the smelting furnace, slowly make the temperature in the crucible reach 1550°C and then keep it warm. After 5 minutes, it is observed that the surface nickel blocks begin to melt. After 16 minutes, all the nickel blocks are converted into nickel water. After setting the gas flow rate to 2.2L / min and the powder feeding rate to 14.0g / s, the corresponding controllers were adjusted in sequence. After 6.5min of powder feeding, the powder feeding was stopped and the smelting temperature was reduced to 1165℃. After keeping the temperature at this temperature for 5min, the temperature was raised to 1250℃. The flow controller and the feeding controller were turned on again. At this time, there was no need to change the flow and powder feeding parameters. The remaining red phosphorus powder was supplied to the molten pool, and argon was continued to be introduced at the current flow rate for 3min. At the same time, the circulating water system in the cooling mold was turned on, the water temperature was controlled at 18±3℃, and the cooling water flow was controlled at 7.0L / min. After turning off the argon, the melt was kept warm for 10min, then cooled to 1220℃ and poured at a rate of 4.0kg / s. The ingot was removed after cooling in the furnace for 1.5h to obtain the NiP20 intermediate alloy.

[0046] Example 2 (preparation of 50 kg of NiP17 alloy):

[0047] Weigh 41.5 kg of 99.9% pure electrolytic nickel blocks and place them in a crucible. Weigh 8.5 kg of 99.9% pure red phosphorus powder with a particle size of 270-400 mesh and place it in a phosphorus storage tank. Start vacuum systems 1 and 2 to make the vacuum degrees in the smelting furnace and the phosphorus storage tank reach 0.6 Pa and 0.04 Pa respectively. Start the power supply of the smelting furnace, slowly make the temperature in the crucible reach 1600°C and then keep it warm. After 3.5 minutes, it is observed that the surface nickel blocks begin to melt. After 15 minutes, all the nickel blocks are converted into nickel water. After setting the gas flow rate to 2.0L / min and the powder feeding rate to 10.0g / s, the corresponding controllers are started in sequence. After feeding the powder for 7.6 minutes, the powder feeding is stopped and the melting temperature is reduced to 1155℃. After keeping it at this temperature for 5 minutes, the temperature is raised to 1260℃. The flow controller and the feeding controller are turned on again. At this time, there is no need to change the flow and powder feeding parameters. The remaining red phosphorus powder is supplied to the molten pool, and argon gas is continued to be introduced at the current flow rate for 3 minutes. At the same time, the circulating water system in the cooling mold is turned on, the water temperature is controlled at 18±3℃, and the cooling water flow rate is controlled at 8.0L / min. After turning off the argon gas, the melt is kept warm for 10 minutes, then cooled to 1280℃ and poured at a rate of 4.0kg / s. The ingot is removed after cooling in the furnace for 2.0 hours to obtain the NiP17 intermediate alloy.

[0048] The differences between Examples 3-5 and Example 1 are as follows:

[0049] Table 1 Differences between Examples 3-5 and Example 1

[0050]

[0051] Three samples were taken from each of the upper, middle and lower layers of the nickel-phosphorus alloy ingots prepared in Examples 1-5 for chemical composition analysis. The analysis results of the three samples in each layer were averaged. The analysis results are shown in Table 2.

[0052] Table 2 Chemical composition analysis results of nickel-phosphorus alloys prepared in Examples 1-5

[0053]

[0054] It can be seen from the composition analysis results in the table that the nickel-phosphorus alloy prepared by the method and apparatus of the present invention has less phosphorus burn-off, high yield and uniform composition distribution in various parts of the ingot.

[0055] Comparative Example 1:

[0056] The difference between Comparative Example 1 and Example 1 is as follows: in Comparative Example 1, after the temperature was raised to 1550°C and kept warm for 16 minutes, the electrolytic nickel block was completely hydrated, and then all the red phosphorus powder was directly introduced at one time. After the powder was supplied, argon gas was continued to be introduced for 3 minutes. After the gas source was turned off, the temperature was kept at 1550°C for 10 minutes, and then the temperature was lowered to 1220°C for casting.

[0057] Comparative Example 2:

[0058] Weigh 10kg of red phosphorus powder and put it into a crucible. Select 60-mesh red sand, moisten it with water, and let it stand for one day. Then mix it with a sand mixer and evenly cover the upper 20mm of the red phosphorus powder in the crucible. Press it flat to make the red sand densely distributed. Cover the above red sand layer with charcoal ash, and then weigh 40kg of electrolytic nickel block on the upper layer of charcoal ash. Cover the crucible lid and start heating at 1800℃. After 19 minutes, all the nickel blocks are melted. Then the red sand layer is pierced to allow the nickel liquid to react with phosphorus. A large amount of white smoke is generated during the process, accompanied by splashing of nickel liquid. After 5 minutes, the surface of the alloy liquid tends to calm down, and then it is kept warm at 1500℃ for 10 minutes, heated for 15 minutes, and kept warm for another 10 minutes. After skimming off the scum, pour it directly into the mold, sprinkle an appropriate amount of wood ash evenly on the upper part of the alloy liquid, and then cool it at room temperature.

[0059] Three samples were taken from each of the upper, middle and lower layers of the nickel-phosphorus alloy ingots prepared in Comparative Examples 1 and 2 for chemical composition analysis. The analysis results of the three samples in each layer were averaged. The analysis results are shown in Table 3.

[0060] Table 3 Chemical composition analysis results of nickel-phosphorus alloys prepared in Comparative Example 1 and Comparative Example 2

[0061]

[0062] As can be seen from Table 3, Comparative Example 1 does not adopt the stage temperature control method of the present invention, and the P element yield is reduced by 1.33%. Comparative Example 2 is a nickel-phosphorus alloy prepared by the phosphorus pressing method. The P element segregation in the upper, middle and lower parts of the alloy ingot is more obvious, and the comprehensive P yield is only 83.82%, which is significantly different from the present invention.

[0063] In addition, during the preparation process of Comparative Document 2, a large amount of toxic P2O5 gas will be generated, accompanied by violent splashing, and the operation process is dangerous.

[0064] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A device for preparing nickel-phosphorus alloy, characterized in that: include: A smelting system, a feeding system, and a vacuum system; wherein the smelting system includes a smelting crucible and a cooling mold, the feeding system includes a phosphorus storage tank, an air source, and a bubble generator, and the vacuum system includes a vacuum system 1 and a vacuum system 2; wherein the feeding system is connected to the bottom of the smelting crucible of the smelting system through the bubble generator; The vacuum system 1 is connected to the furnace shell of the smelting system; The vacuum system 2 is connected to the top of the phosphorus storage tank of the feeding system; The bubble generator is placed at the bottom of the smelting crucible, and is connected to the phosphorus storage tank and the gas source through a pipeline; An electromagnetic vibrating feeder is provided on the material conveying pipe between the phosphorus storage tank and the bubble generator, and a gas flow controller is provided on the pipeline between the gas source and the phosphorus storage tank.

2. The device for preparing a nickel-phosphorus alloy according to claim 1, characterized in that: The upper surface of the bubble generator is evenly covered with holes, and the hole size is 150-200 μm.

3. The device for preparing nickel-phosphorus alloy according to claim 1, characterized in that: The gas source is an inert gas source and the use of nitrogen is prohibited.

4. The device for preparing nickel-phosphorus alloy according to claim 3, characterized in that: The gas source is argon.

5. A method for preparing a nickel-phosphorus alloy, characterized in that: The method utilizes the preparation device as claimed in claim 1, and specifically comprises the following steps: S1. Weigh the raw material electrolytic nickel block and red phosphorus powder according to the designed nickel-phosphorus alloy grade and weight; S2. Place the electrolytic nickel block in a smelting crucible, start vacuum system 1, and evacuate the smelting system until the vacuum degree drops below 0.6 Pa; put red phosphorus powder into a phosphorus storage tank, cover the tank, and start vacuum system 2 to evacuate the system until the vacuum degree drops below 0.05 Pa; S3. Start the power supply of the smelting furnace and gradually increase the temperature to 1550-1600℃ to melt the nickel block. Keep the temperature for 15-20 minutes until the nickel block is completely dissolved. Then, turn on the gas flow controller and electromagnetic feed controller in sequence. After setting the parameters, feed red phosphorus powder into the nickel liquid. S4. After heating and holding treatment according to the heating curve, adjust the melting temperature to 1220-1280°C, continue to introduce argon gas for 3-5 minutes, pour the alloy liquid into a pure copper cooling mold, cool it for 1.5-2 hours and then take it out of the furnace to obtain a nickel-phosphorus alloy that meets the requirements; The heating curve in step S4 is as follows: red phosphorus powder is introduced at 1550-1600° C., and after 53-57% by weight of the red phosphorus powder is introduced, the temperature is lowered to 1150-1200° C. and kept warm for 5-10 minutes. The temperature is then raised to 1250-300° C., the remaining weight of the red phosphorus powder is introduced, and kept warm for 10-15 minutes. After that, the temperature is controlled at 1220-1280° C. for pouring.

6. The method for preparing a nickel-phosphorus alloy according to claim 5, characterized in that: In step S1, the purity of the electrolytic nickel is ≥99.9%, the purity of the red phosphorus is ≥99%, and the particle size of the red phosphorus powder is 200-400 mesh.

7. The method for preparing a nickel-phosphorus alloy according to claim 5, characterized in that: In step S3, the inert gas flow rate is adjusted to 1.5-3.0 L / min by a gas flow controller, and the electromagnetic feeding controller is set to make the feeding speed 10.0-20.0 g / s.

8. The method for preparing a nickel-phosphorus alloy according to claim 5, characterized in that: In step S4, the cooling water temperature of the pure copper cooling mold is 10-24° C., the flow rate is 7.0-10.0 L / min, and the pouring speed is 2.0-4.0 kg / s.

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