阅读说明：本技术 一种集冶金精炼与组织控制的材料无容器加工方法 (Material container-free processing method integrating metallurgical refining and structure control ) 是由 张桂芳 严鹏 漆鑫 姜琦 赵卫东 刘玳炜 易兵 刘宇 杨睿潇 施哲 于 2021-07-20 设计创作，主要内容包括：本发明涉及一种集冶金精炼与组织控制的材料无容器加工方法,属于材料电磁加工技术领域。首先将材料切割成颗粒状,然后将颗粒状材料用推杆并推入悬浮线圈中部；将悬浮腔关闭,抽真空；打开气氛保持系统阀门,使悬浮腔内保持设定惰性/还原/氧化气氛；打开线圈冷却水和电源,控制输入电流、频率以及功率,对颗粒状材料进行预热；经预热后颗粒状材料在电磁感应效应的作用下材料实现悬浮并熔化,然后迅速撤走推杆进行悬浮熔化；经悬浮熔化后,调低输入电流,待悬浮熔滴出现晃动,调节气氛保持系统开关,转换悬浮腔内冷却气体流量、冷却气氛种类,实现材料的组织控制与无容器凝固。本发明在一个系统中实现冶金精炼过程和无容器凝固两个过程。(The invention relates to a material container-free processing method integrating metallurgical refining and structure control, and belongs to the technical field of material electromagnetic processing. Firstly, cutting a material into particles, and then pushing the particle material into the middle part of a suspension coil by using a push rod; closing the suspension cavity and vacuumizing; opening a valve of an atmosphere maintaining system to maintain a set inert/reducing/oxidizing atmosphere in the suspension cavity; opening coil cooling water and a power supply, controlling input current, frequency and power, and preheating the granular materials; after preheating, the granular material is suspended and melted under the action of the electromagnetic induction effect, and then the push rod is quickly removed for suspension melting; after suspension melting, input current is reduced, when suspension molten drops shake, an atmosphere maintaining system switch is adjusted, the flow of cooling gas in a suspension cavity and the type of cooling atmosphere are converted, and the tissue control and container-free solidification of materials are realized. The invention realizes two processes of metallurgical refining and container-free solidification in one system.)

1. A material containerless processing method integrating metallurgical refining and structure control is characterized by comprising the following specific steps: .

(1) Firstly, cutting a material into granules by using a wire cutting machine, and then pushing the granular material into the middle part of a suspension coil by using a push rod;

(2) closing the suspension cavity, and then vacuumizing the suspension cavity; opening a valve of an atmosphere maintaining system to maintain a set inert/reducing/oxidizing atmosphere in the suspension cavity; opening coil cooling water and a power supply, controlling input current, frequency and power, and preheating the granular materials;

(3) after preheating, the granular material is suspended and melted under the action of the electromagnetic induction effect, and then the push rod is quickly removed for suspension melting;

(4) after suspension melting, input current is reduced, when suspension molten drops shake, an atmosphere maintaining system switch is adjusted, the flow of cooling gas in a suspension cavity and the type of cooling atmosphere are converted, and the tissue control and container-free solidification of materials are realized.

2. The vessel-less processing method of materials with integrated metallurgical refining and texture control as claimed in claim 1, wherein: the atmosphere gas in the inert/reducing/oxidizing atmosphere in the step (2) is x₁%Ar+y₁%H₂+z₁%H₂O，x₁+y₁+z₁And the gas flow is 0-1.5L/min by = 100.

3. The vessel-less processing method of materials with integrated metallurgical refining and texture control as claimed in claim 1, wherein: and (4) reducing the input current to 10-60A, and taking the shaking of the suspended molten drops as a limit.

4. The vessel-less processing method of materials with integrated metallurgical refining and texture control as claimed in claim 1, wherein: the cooling atmosphere in the solidification process of the step (4) is x₂%H₂+y₂%Ar+z₂%He，x₂+y₂+z₂=100, wherein x₂The flow rate of the gas is more than or equal to 50 and is 1-3L/min.

Technical Field

The invention relates to a material container-free processing method integrating metallurgical refining and structure control, and belongs to the technical field of material electromagnetic processing.

Background

With the increasing requirements of people on the material performance, the electromagnetic processing technology of the material melt is more and more valued by scientific researchers. At present, the electromagnetic technology is widely applied to metallurgical refining and the material processing and processing field; because the directions between the two flows are inconsistent and the realized targets are inconsistent, the realized technical paths are different from the realized methods, and the two processes of metallurgy and material forming are difficult to realize in one system. For example, impurity element removal is the key of the metallurgical process, and the control of the solidification structure is the key of the material forming process. The electromagnetic field is mainly used for strengthening the stirring effect of the melt through electromagnetic stirring in the metallurgical process, so that better metallurgical reaction kinetic conditions are created to strengthen the volatilization of impurity elements; the electromagnetic field is mainly used for promoting grain refinement and deep undercooling solidification to refine grains in the material forming process through strengthening convection in the solidification process. At present, the electromagnetic constraint forming technology is a container-free electromagnetic processing technology for materials which integrates electromagnetic induction heating and electromagnetic constraint forming; however, the refining effect in the metallurgical process cannot be realized in the whole process, so that the development of a short-flow and integrated material processing process integrating the control of the metallurgical refining process and the material container-free solidification process is the leading edge of the development of the new material field in the future from the viewpoints of saving energy and shortening the preparation process.

Disclosure of Invention

In view of the fact that the existing material metallurgy and material processing processes need to be realized in two systems, the invention provides a short-flow and integrated material processing method integrating metallurgy refining and solidification molding, and has the advantages that the electromagnetic suspension technology is matched with an atmosphere control system to design and provide a short-flow and integrated material electromagnetic processing device and technology integrating metallurgy refining and material solidification molding control.

In order to achieve the above object, the present invention is achieved by the following technical solutions.

A material containerless processing method integrating metallurgical refining and structure control comprises the following specific steps: .

(1) Firstly, cutting the material into granules by using a wire cutting machine, and then pushing the granular material into the middle part of a suspension coil by using a corundum push rod;

(2) closing the suspension cavity, and then opening a vacuum pump to vacuumize the suspension cavity; opening a valve of an atmosphere maintaining system to maintain a set inert/reducing/oxidizing atmosphere in the suspension cavity; opening coil cooling water and a power supply, controlling input current, frequency and power, and preheating the granular materials;

(3) after preheating, the granular material is suspended and melted under the action of the electromagnetic induction effect, and then the push rod is quickly removed for suspension melting;

(4) after suspension melting, input current is reduced, when suspension molten drops shake, an atmosphere maintaining system switch is adjusted, the flow of cooling gas in a suspension cavity and the type of cooling atmosphere are converted, and the tissue control and container-free solidification of materials are realized.

The atmosphere gas in the inert/reducing/oxidizing atmosphere in the step (2) is x₁%Ar+y₁%H₂+z₁%H₂O，x₁+y₁+z₁And the gas flow is 0-1.5L/min by = 100.

And (4) reducing the input current to 10-60A, and taking the shaking of the suspended molten drops as a limit.

The cooling atmosphere in the solidification process of the step (4) is x₂%H₂+y₂%Ar+z₂%He，x₂+y₂+z₂=100, wherein x₂The flow rate of the gas is more than or equal to 50 and is 1-3L/min.

The schematic structural diagram of the material container-free processing device integrating metallurgical refining and tissue control is shown in figure 1, and comprises a suspension device, an electromagnetic suspension coil and control system 4, a high-speed camera system 6, an IR (infrared) double-color temperature measurement system 7, a prism 8, a tail gas treatment system 9, a metallurgical process gas control system 10 and a solidification process gas control system 12, wherein the suspension device comprises a suspension cavity 2, the suspension cavity 2 is made of a glass tube 3, the electromagnetic suspension coil and control system 4 is arranged on the suspension cavity 2, the prism 8 is arranged at the top of the suspension cavity 2, the IR double-color temperature measurement system 7 is arranged at the light outlet of the prism 8, the high-speed camera system 6 is arranged in the middle of the suspension cavity 2, a gas inlet at the upper part of the suspension cavity 2 is respectively connected with the metallurgical process gas control system 10 and the solidification process gas control system 12 through a valve, the metallurgical process gas control system-10 comprises 3 gas cylinders I11, the solidification process gas control system 12 includes 3 gas cylinders ii 13.

The invention has the beneficial effects that:

compared with the prior electromagnetic processing technology, the invention realizes two processes of metallurgical refining and deep supercooling in one system, is particularly suitable for preparing high-purity materials and high-activity materials, and has the following beneficial effects: obviously shortens the metallurgical and preparation processes and procedures of the material, and the metallurgical and solidification processes are in a suspension state; therefore, the material purity in the whole process is high, and the grain size of the solidification structure can be obviously reduced, so that the performance of the prepared material is improved.

Drawings

FIG. 1 is a schematic structural view of a vessel-less processing apparatus for metallurgical refining and texture control of materials of the present invention;

FIG. 2 is a comparison of metallurgical grade silicon material before and after treatment according to example 1 of the present invention; wherein (a) is an object image of an untreated metallurgical grade silicon material, (b) is a scanning electron microscope image of the untreated metallurgical grade silicon material, (c) is an object image of a treated metallurgical grade silicon material, and (d) is a scanning electron microscope image of the treated metallurgical grade silicon material.

FIG. 3 is a comparison of the Si-Fe alloy material of example 2 of the present invention before and after treatment; wherein, (a) is an object picture of the silicon-iron alloy material before treatment, (b) is a scanning electron microscope picture of the silicon-iron alloy material before treatment, (c) is an object picture of the silicon-iron alloy material after treatment, and (d) is a scanning electron microscope picture of the silicon-iron alloy material after treatment.

In the figure: the device comprises a corundum sample feeding rod 1, a corundum sample feeding rod 2, a suspension cavity 3, a glass tube 4, an electromagnetic suspension coil and control system, a suspension material 5, a high-speed camera system 6, a 7-IR (infrared radiation) double-color temperature measurement system 8-a prism, a tail gas treatment system 9, a metallurgical process gas control system 10, a gas cylinder I11, a solidification process gas control system 12 and a gas cylinder II 13.

Detailed Description

The invention is further described with reference to the following drawings and detailed description.

Example 1

The container-free processing method of the material integrating metallurgical refining and structure control comprises the following specific steps: .

(1) Firstly, cutting 0.82g of metallurgical grade silicon material into granules by using a wire cutting machine (a hacksaw), and then pushing the granules into the middle part of a suspension coil by using a corundum push rod;

(2) closing the suspension cavity, and then opening a vacuum pump to vacuumize the suspension cavity to 0.5 Pa; opening a valve of an atmosphere maintaining system to maintain a set inert/reducing/oxidizing atmosphere in the suspension cavity, controlling the gas to be 100% Ar and the flow to be 1L/min; turning on coil cooling water and a power supply, controlling input current, frequency and power (current 58A, frequency 330kHz and input power 9.5 kw), and preheating the granular materials;

(3) after preheating for 15min, suspending and melting the granular material under the action of electromagnetic induction effect, then quickly removing the push rod, and controlling the temperature to 1550 ℃ under the conditions of current 40A and input power of 6.5kw for suspension melting (namely suspension refining) for 45 min;

(4) after the suspension refining is finished, the input current (current 12A) is reduced to be suspendedThe floating molten drops shake, the atmosphere maintaining system is switched on and off, and the flow of the cooling gas and the type of the cooling atmosphere (10% Ar +90% H) in the suspension cavity are converted_2，The gas flow is 3L/min), the structure control of the material and the container-free solidification (the molten drop falls after being completely solidified) are realized.

The impurity content and material hardness before and after the metallurgical grade silicon material treatment of this example are shown in table 1 below.

TABLE 1 comparison of the phosphorus removal effectiveness and solidification structure performance of metallurgical grade silicon materials before and after the inventive treatment

Metallurgical grade silicon material	Content of impurity phosphorus	Hardness of material
			Before treatment	90ppm	350Hv
After treatment	45ppm	456Hv

As can be seen from Table 1, by the method of the patent, impurity elements in the metallurgical silicon material are obviously removed, and the hardness performance of the material is also obviously improved.

A comparison of the metallurgical grade silicon material before and after treatment of the present example is shown in FIG. 2, from which it can be seen that the whole droplet exhibits substantially an ellipsoidal shape in FIG. 2 (c), demonstrating the containerless solidification effect of the present method; further, as is apparent from FIGS. 2 (b) and (d), the effect of refining the solidification structure based on the effect of the metallurgical refining by the method of the present invention is exhibited.

Example 2

The container-free processing method of the material integrating metallurgical refining and structure control comprises the following specific steps: .

(1) Firstly, cutting 0.67g of ferrosilicon alloy material into granules by using a wire cutting machine (hacksaw), and then pushing the granules into the middle part of the suspension coil by using a corundum push rod;

(2) closing the suspension cavity, and then opening a vacuum pump to vacuumize the suspension cavity to 0.5 Pa; opening a valve of an atmosphere maintaining system to maintain a set inert/reducing/oxidizing atmosphere in the suspension cavity, controlling the gas to be 100% Ar and the flow to be 1.5L/min; opening coil cooling water and a power supply, controlling input current, frequency and power (current 55A, frequency 330kHz and input power 9.0 kw), and preheating the granular materials;

(3) after preheating for 10min, suspending and melting the granular material under the action of electromagnetic induction effect, then quickly removing the push rod, and controlling the temperature to 1450 ℃ under the conditions of current 32A and input power of 4.5kw for suspension melting (namely suspension refining) for 45 min;

(4) after suspension refining is finished, input current (current 10A) is reduced, the atmosphere maintaining system is adjusted to switch when suspension molten drops shake, and the flow of cooling gas and the type of cooling atmosphere (100% H) in the suspension cavity are converted₂And the gas flow is 3L/min), the structure control of the material and the container-free solidification (the molten drop falls down after being completely solidified) are realized.

The impurity contents and material hardness before and after the treatment of the ferrosilicon alloy material of this example are shown in Table 2 below.

TABLE 2 comparison of phosphorus removal effect and solidification structure performance of Si-Fe alloy material before and after treatment according to the present invention

(Metallurgy)Graded silicon material	Content of impurity phosphorus	Hardness of material
			Before treatment	285ppm	713Hv
After treatment	29ppm	1274Hv

As can be seen from Table 2, after the ferrosilicon is treated by the method, on one hand, the content of impurity element phosphorus in the ferrosilicon is obviously reduced, and the ferrosilicon has good phosphorus removal effect; meanwhile, the hardness performance of the finally obtained material is also obviously improved, which indicates that the grain structure in the material is obviously refined. A comparison of the prior and post-treatment graphs of the Si-Fe alloy material of this example is shown in FIG. 3, which shows that the internal crystal grains of the alloy are slender coarse dendrite structures before treatment; the interior of the product is a fine isometric crystal structure after treatment.

While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.