CN112080659A - Preparation method of CuMn25Ni10Sn alloy material - Google Patents
Preparation method of CuMn25Ni10Sn alloy material Download PDFInfo
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Abstract
The invention discloses a preparation method of a CuMn25Ni10Sn alloy material, which comprises the following steps: the raw materials are mixed according to the following weight percentage: mn: 23-27%, Ni: 8-12%, Sn: 0.1-0.5%, Cu: 60.5-68%, wherein Mn and Ni are added in the form of Mn72Ni28, Sn is added in the form of tin ingot, and Cu is added in the form of electrolytic copper plate; the prepared raw materials are put into a crucible of a vacuum induction melting furnace; starting a mechanical pump and a roots pump to vacuumize the smelting furnace; gradually heating the smelting furnace during smelting, increasing the heating power, opening an argon filling air valve when the raw materials in the crucible begin to melt and reduce the heating power, slowly filling high-purity argon into the furnace body of the vacuum induction smelting furnace, closing the argon filling valve when the pressure in the furnace rises to a preset value, and then increasing the heating power to refine the raw materials; reducing the heating power, and casting after keeping the heating power for a preset time; and after the casting is finished, closing the heating, cooling and discharging. The preparation method of the CuMn25Ni10Sn alloy material can prepare the CuMn25Ni10Sn alloy with low gas content, uniform structure and no segregation.
Description
Technical Field
The invention relates to the technical field of nonferrous metal alloy processing, in particular to a preparation method of a CuMn25Ni10Sn alloy material.
Background
CuMn25Ni10Sn is a resistance material, is a basic material for manufacturing resistance elements in electronic instruments, measuring instruments and other industrial devices, and is widely applied to various fields of motors, instruments, automobiles, aerospace, missile atomic energy and the like. It has very small resistance, low temperature coefficient, low copper electric heating potential, high resistance stability and high resistivity, and may be produced into powder, wire, foil, sheet, belt, rod, pipe, etc. and the surface may be coated with various kinds of insulating material. The method is mainly used for manufacturing standard resistors, separators, precise or common resistance elements, high-grade metering voltage, current, bridges, potential difference meters and precise resistance elements of other instruments, and is more suitable for manufacturing the resistance elements of the standard resistors for the reference. The low-temperature-coefficient and low-thermal electromotive force sensor has the characteristics of low temperature coefficient, low thermal electromotive force, good long-term stability, low inductance, high pulse load and the like.
The chip resistor is manufactured into a chip resistor product, and has a wide application range, such as automobile electronics, power electronics, driving technology, power detection, medical technology and the like.
The lap resistance is formed by welding copper and an alloy material by adopting high-energy electron beams, and can be almost punched and bent into any shape, thereby flexibly meeting the requirements of different applications and designs. Due to the excellent performance, the material is widely used in the fields of mobile phones, power grids, new energy automobiles and the like, and has a very wide prospect.
At present, high-end manganese-copper alloys in domestic markets are imported, and the preparation methods of the manganese-copper alloys in China mainly comprise the following steps:
1. powder metallurgy: mixing electrolytic manganese powder, electrolytic copper powder, nickel carbonyl and atomized iron powder, grinding, carrying out compression molding, and sintering at 900 ℃ in a protective atmosphere, wherein the method has the defects of high gas element content and poor compactness;
2. the non-vacuum casting-electroslag remelting method comprises the following steps: the method has the advantages that the metal copper, manganese and nickel are proportioned and subjected to non-vacuum melting and electroslag remelting, and the method has the defects of easy element burning loss, uniform components and poor consistency;
3. vacuum melting-metal mold casting: metal copper, manganese and nickel are mixed and subjected to vacuum melting and metal mold pouring, but the method has the defects of high requirement on a mold and poor realizability on special products;
4. horizontal continuous casting: smelting in atmosphere, and horizontally and continuously casting the bar and the plate, wherein the method has the defects of large material burning loss, poor material component uniformity and poor consistency of each furnace.
The chip resistor manufactured by the domestic production process has unqualified resistivity and resistance temperature coefficient.
Therefore, the present inventors have made extensive studies to design a method for producing a CuMn25Ni10Sn alloy material that can solve the above-described problems.
Disclosure of Invention
The invention aims to provide a preparation method of a CuMn25Ni10Sn alloy material, which can prepare a CuMn25Ni10Sn alloy material with low gas content, uniform structure and no segregation.
In order to achieve the above object, the present invention provides a method for preparing a CuMn25Ni10Sn alloy material, which comprises the following steps:
(1) preparing materials: the raw materials are mixed according to the following weight percentage: 23 to 27 percent of Mn element, 8 to 12 percent of Ni element, 0.1 to 0.5 percent of Sn element and 60.5 to 68 percent of Cu element, wherein the Mn element and the Ni element are added in a form of Mn72Ni28 intermediate alloy, the Sn element is added in a form of tin ingot, and the Cu element is added in a form of electrolytic copper plate;
(2) charging: loading the prepared raw materials into a crucible of a vacuum induction melting furnace, and covering a furnace cover;
(3) vacuumizing: starting a mechanical pump and a roots pump to vacuumize the smelting furnace;
(4) smelting: when smelting, gradually heating the smelting furnace to raise the temperature and gradually increasing the heating power, opening an argon filling air valve when the raw materials in the crucible begin to melt and reduce the heating power, slowly filling high-purity argon into the furnace body of the vacuum induction smelting furnace, closing the argon filling valve when the pressure in the smelting furnace rises to a preset value, and then increasing the heating power to refine the raw materials;
(5) casting: the heating power of the smelting furnace is reduced, casting is started after the preset time is kept, and the casting speed is firstly slow, then is gradually accelerated, and finally is slowed down;
(6) discharging: and after the casting is finished, closing the heating, cooling for 20-40 minutes, and discharging.
The invention discloses a preparation method of a CuMn25Ni10Sn alloy material, wherein the Mn72Ni28 intermediate alloy in the step (1) is processed and prepared by the following steps:
(a) preparing materials: the raw materials are mixed according to the following weight percentage: weighing 70-75% of Mn element and 25-30% of Ni element according to the proportion;
(b) charging: loading the prepared alloy raw materials into a crucible of a vacuum induction melting furnace, covering a furnace cover, closing an air release valve, and cleaning an observation window;
(c) vacuumizing: starting a mechanical pump, opening a low-vacuum baffle valve for vacuumizing, and starting a roots pump when the vacuum pressure p in the furnace is less than or equal to 0.08 MPa;
(d) smelting: when smelting, gradually heating the smelting furnace to raise the temperature and gradually increasing the heating power, opening an argon filling air valve when the raw materials in the crucible begin to melt and reduce the heating power, slowly filling high-purity argon into the furnace body of the vacuum induction smelting furnace, closing the argon filling valve when the pressure in the smelting furnace rises to a preset value, and then increasing the heating power to refine the raw materials;
(e) casting: the heating power of the smelting furnace is reduced, casting is started after the preset time is kept, and the casting speed is firstly slow, then is gradually accelerated, and finally is slowed down;
(f) discharging: and after the casting is finished, closing the heating, cooling for 20-40 minutes, and discharging.
According to the preparation method of the CuMn25Ni10Sn alloy material, after the furnace cover is covered in the step (b), the air release valve is closed, and the observation window is cleaned.
The preparation method of the CuMn25Ni10Sn alloy material comprises the steps of (c) opening a low-vacuum baffle valve after a mechanical pump is started, vacuumizing, and starting the roots pump when the vacuum pressure p in a furnace is less than or equal to 0.08 MPa.
The invention discloses a preparation method of CuMn25Ni10Sn alloy material, wherein during smelting in the step (d), when the vacuum degree in the smelting furnace is pumped to p less than or equal to 10Pa, the smelting furnace is heated, the heating power is increased to 30 +/-2 KW, the temperature is kept for 3-5min, the heating power is increased to 40 +/-2 KW, the temperature is kept for 3-5min, the heating power is increased to 50 +/-2 KW, the temperature is kept for 3-5min, the heating power is increased to 60 +/-2 KW, the temperature is kept for 3-5min, the heating power is increased to 65KW, raw materials in a crucible in the smelting furnace begin to melt, the heating power is reduced to 35 +/-2 KW and is kept, when furnace burden is completely melted, the heating power is reduced to below 20KW, an argon filling valve is opened, high-purity argon is slowly filled into the furnace body of a vacuum induction smelting furnace, the pressure in the smelting furnace is increased to-0.08 MPa, the argon filling valve is closed, the heating, refining for 2-4 min.
The preparation method of the CuMn25Ni10Sn alloy material comprises the steps of (e) reducing the heating power to 40KW +/-5 KW, keeping the temperature for 25-35s, and starting casting and copper mold casting, wherein the whole casting time is 20-30 s.
According to the preparation method of the CuMn25Ni10Sn alloy material, after the furnace cover is covered in the step (2), the air release valve is closed, and the observation window is cleaned.
The preparation method of the CuMn25Ni10Sn alloy material comprises the steps of (3) opening a low-vacuum baffle valve after a mechanical pump is started, vacuumizing, and starting the roots pump when the vacuum pressure p in a furnace is less than or equal to 0.08 MPa.
The invention discloses a preparation method of a CuMn25Ni10Sn alloy material, wherein in the step (4), when the vacuum degree in a smelting furnace is pumped to p less than or equal to 10Pa, the smelting furnace is heated and heated, the heating power is increased to 20 +/-1 KW, the temperature is kept for 2-4min, the heating power is increased to 30 +/-1 KW, the temperature is kept for 2-4min, the heating power is increased to 40 +/-1 KW, the temperature is kept for 2-4min, the heating power is increased to 50 +/-1 KW, the temperature is kept for 2-4min, the raw materials in a crucible in the smelting furnace begin to be melted, the heating power is reduced to be less than 20KW, an argon filling air valve is opened, high-purity argon is slowly filled into the furnace body of a vacuum induction smelting furnace, the internal pressure of the smelting furnace is increased to-0.08 MPa, the argon filling valve is closed, the heating power is increased to 55KW, and the smelting furnace is refined.
The method for preparing the CuMn25Ni10Sn alloy material comprises the step (5) of reducing the power of a smelting furnace to 35KW +/-5 KW, and keeping the time for casting to start for 20-30s, wherein the whole casting time is 50-60 s.
After the scheme is adopted, when the CuMn25Ni10Sn alloy material is prepared, the intermediate alloy Mn72Ni28 is added, and the Mn72Ni28 intermediate alloy is prepared by adopting a vacuum induction melting method, so that the raw material cost is reduced, the element burning loss is reduced, and the prepared CuMn25Ni10Sn alloy material has uniform components and tissues, compact tissues, less pores and impurities, and no defects of macroscopic and microscopic segregation such as Cu and Mn enrichment and the like.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a CuMn25Ni10Sn alloy material according to the invention;
FIG. 2 is a drawing of an ingot of CuMn25Ni10Sn alloy made by the present invention;
FIG. 3 is a 50X as-cast metallographic structure diagram of a CuMn25Ni10Sn alloy ingot prepared by the method;
FIG. 4 is a 100X as-cast metallographic structure diagram of a CuMn25Ni10Sn alloy ingot prepared by the method.
Detailed Description
An embodiment of the present invention is shown in the process flow diagram of fig. 1.
The first embodiment is as follows:
the invention discloses a preparation method of a CuMn25Ni10Sn alloy material, which comprises the following steps:
preparation of Mn72Ni28 intermediate alloy:
(a) preparing materials: the raw materials comprise the following elements in percentage by weight: mn: 70-75%, Ni: weighing 25-30% of required raw materials in proportion, and weighing an electrolytic manganese sheet and a nickel plate in proportion of Mn accounting for 72.2% and Ni accounting for 27.8% in the embodiment;
(b) charging: putting the alloy raw material prepared in the step (a) into a crucible (the crucible is a crucible without carbon) of a vacuum induction melting furnace, covering a furnace cover, closing an air release valve, and cleaning an observation window;
(c) vacuumizing: starting a mechanical pump, opening a low-vacuum baffle valve for vacuumizing until the vacuum pressure p in the furnace is less than or equal to 0.08MPa
When the pump is started, the roots pump is started;
(d) smelting: when smelting, when the vacuum degree in the furnace is pumped to p less than or equal to 10Pa, heating and raising the temperature, raising the heating power to 30KW, keeping the temperature for 4min, then raising the heating power to 40KW, keeping the temperature for 4min, then raising the heating power to 50KW, keeping the temperature for 4min, then raising the power to 60KW, keeping the temperature for 4min, then raising the heating power to 65KW, keeping the temperature, when the raw materials in the crucible in the furnace begin to melt, lowering the heating power to 35KW, when the furnace burden is completely melted, lowering the heating power to below 20KW, opening an argon filling valve, slowly filling high-purity argon into the furnace body of the vacuum induction smelting furnace, when the pressure in the furnace rises to-0.08 MPa, closing the argon filling valve, raising the heating power to 60KW, keeping;
(e) casting: reducing the heating power to 40KW, keeping the temperature for about 0.5 minute, and starting casting and copper mold casting, wherein the whole casting time is 25 s;
(f) discharging: and after the casting is finished, turning off the heating, cooling for 30 minutes, and discharging. The prepared intermediate alloy material is detected by chemical content as follows:
| Mn(％) | Ni(％) | 0(％) | N(％) | C(％) | S(％) | |
| Mn72Ni28 | 72.22 | 27.74 | 0.0014 | 0.0002 | 0.0028 | 0.0009 |
(II) preparing a CuMn25Ni10Sn alloy material:
(1) preparing materials: the raw materials comprise the following elements in percentage by weight: mn: 23-27%, Ni: 8-12%, Sn: 0.1-0.5%, Cu: 60.5-68%, Mn and Ni are added in the form of Mn72Ni28 master alloy prepared in the above way in the embodiment, Sn is added in the form of tin ingot, Cu is added in the form of electrolytic copper plate, the raw materials are weighed in the embodiment, Mn accounts for 25%, Ni accounts for 9.8%, Sn accounts for 0.2%, and Cu accounts for 65%;
(2) charging: putting the prepared raw materials in the step (1) into a crucible (the crucible is a crucible without carbon) of a vacuum induction smelting furnace, closing a furnace cover, closing a gas release valve, and cleaning an observation window;
(3) vacuumizing: starting a mechanical pump, opening a low-vacuum baffle valve for vacuumizing, and starting the roots pump when the vacuum pressure p in the furnace is less than or equal to 0.08 MPa;
(4) smelting: during smelting, when the vacuum degree in the smelting furnace is pumped to p less than or equal to 10Pa, the smelting furnace is heated and heated, the heating power is increased to 20KW, the temperature is kept for 3min, then the heating power is increased to 30KW, the temperature is kept for 3min, then the heating power is increased to 40KW, the temperature is kept for 3min, then the heating power is increased to 60KW for keeping, when the raw materials in a crucible in the smelting furnace begin to melt, the heating power is reduced to below 20KW, an argon filling valve is opened, high-purity argon is slowly filled into the furnace body of the vacuum induction smelting furnace, when the pressure in the smelting furnace is increased to-0.08 MPa, the argon filling valve is closed, the power is increased to 55KW, and the smelting is carried;
(5) casting: reducing the heating power of the smelting furnace to 35KW, keeping 25s to start copper mold casting, wherein the casting speed is firstly slow, then gradually accelerated, and finally slowed down, and the whole casting time is 55 s;
(6) ingot casting (tapping): and after the casting is finished, closing the heating, and cooling for 30 minutes to obtain the cast ingot and discharging.
As shown in fig. 2, a diagram of the prepared CuMn25Ni10Sn alloy ingot and 50X and 100X cast metallographic structures of the prepared CuMn25Ni10Sn alloy ingot are shown in fig. 3 and 4. The CuMn25Ni10Sn alloy material prepared by the method has uniform components and tissues, less inclusions, and no macroscopic and microscopic defects such as Cu and Mn enrichment.
The detection results of the ingredients and the chemical content of the CuMn25Ni10Sn alloy material prepared by the vacuum induction melting method are as follows:
1) ingredients
| Ingredients | Cu(％) | Mn72Ni28(％) | Sn(％) |
| CuMn25Ni10Sn① | 64.80 | 35 | 0.20 |
| CuMn25Ni10Sn② | 64.75 | 35 | 0.25 |
| CuMn25Ni10Sn③ | 64.75 | 35.1 | 0.25 |
2) Chemical composition detection
The embodiments of the present invention have been described in detail, but the description is only a preferred example of the present invention, and is not intended to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the design of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (10)
1. A preparation method of a CuMn25Ni10Sn alloy material is characterized by comprising the following steps:
(1) preparing materials: the raw materials are mixed according to the following weight percentage: 23 to 27 percent of Mn element, 8 to 12 percent of Ni element, 0.1 to 0.5 percent of Sn element and 60.5 to 68 percent of Cu element, wherein the Mn element and the Ni element are added in a form of Mn72Ni28 intermediate alloy, the Sn element is added in a form of tin ingot, and the Cu element is added in a form of electrolytic copper plate;
(2) charging: loading the prepared raw materials into a crucible of a vacuum induction melting furnace, and covering a furnace cover;
(3) vacuumizing: starting a mechanical pump and a roots pump to vacuumize the smelting furnace;
(4) smelting: when smelting, gradually heating the smelting furnace to raise the temperature and gradually increasing the heating power, opening an argon filling air valve when the raw materials in the crucible begin to melt and reduce the heating power, slowly filling high-purity argon into the furnace body of the vacuum induction smelting furnace, closing the argon filling valve when the pressure in the smelting furnace rises to a preset value, and then increasing the heating power to refine the raw materials;
(5) casting: the heating power of the smelting furnace is reduced, casting is started after the preset time is kept, and the casting speed is firstly slow, then is gradually accelerated, and finally is slowed down;
(6) discharging: and after the casting is finished, closing the heating, cooling for 20-40 minutes, and discharging.
2. The method for preparing the CuMn25Ni10Sn alloy material according to claim 1, wherein the Mn72Ni28 master alloy in the step (1) is processed by the following steps:
(a) preparing materials: the raw materials are mixed according to the following weight percentage: weighing 70-75% of Mn element and 25-30% of Ni element according to the proportion;
(b) charging: loading the prepared alloy raw materials into a crucible of a vacuum induction melting furnace, covering a furnace cover, closing an air release valve, and cleaning an observation window;
(c) vacuumizing: starting a mechanical pump, opening a low-vacuum baffle valve for vacuumizing, and starting a roots pump when the vacuum pressure p in the furnace is less than or equal to 0.08 MPa;
(d) smelting: when smelting, gradually heating the smelting furnace to raise the temperature and gradually increasing the heating power, opening an argon filling air valve when the raw materials in the crucible begin to melt and reduce the heating power, slowly filling high-purity argon into the furnace body of the vacuum induction smelting furnace, closing the argon filling valve when the pressure in the smelting furnace rises to a preset value, and then increasing the heating power to refine the raw materials;
(e) casting: the heating power of the smelting furnace is reduced, casting is started after the preset time is kept, and the casting speed is firstly slow, then is gradually accelerated, and finally is slowed down;
(f) discharging: and after the casting is finished, closing the heating, cooling for 20-40 minutes, and discharging.
3. The method for preparing the CuMn25Ni10Sn alloy material according to claim 2, wherein after the furnace cover is covered in the step (b), a vent valve is closed, and the observation window is cleaned.
4. The method for preparing the CuMn25Ni10Sn alloy material according to claim 2, wherein in the step (c), after the mechanical pump is started, a low vacuum baffle valve is opened to vacuumize, and when the vacuum pressure p in the furnace is less than or equal to 0.08MPa, the roots pump is started.
5. The method for preparing CuMn25Ni10Sn alloy material according to claim 2, wherein during smelting in step (d), when the vacuum degree in the smelting furnace is pumped to p is less than or equal to 10Pa, the smelting furnace is heated to raise the temperature, the heating power is raised to 30 +/-2 KW, the temperature is kept for 3-5min, the heating power is raised to 40 +/-2 KW, the temperature is kept for 3-5min, the heating power is raised to 50 +/-2 KW, the temperature is kept for 3-5min, the heating power is raised to 60 +/-2 KW, the temperature is kept for 3-5min, the heating power is raised to 65KW, when the raw materials in the crucible in the smelting furnace begin to melt, the heating power is lowered to 35 +/-2 KW and kept, when the furnace burden is completely melted, the heating power is lowered to below 20KW, the argon-filling air valve is opened, high-purity argon is slowly filled into the furnace body of the vacuum induction smelting furnace, and the pressure in the smelting furnace is raised to, closing the argon filling valve, increasing the heating power to 60KW, maintaining, and refining for 2-4 min.
6. The method for preparing the CuMn25Ni10Sn alloy material according to claim 2, wherein in the step (e), the heating power is reduced to 40KW +/-5 KW, the casting is started and the copper mold casting is carried out for 25-35s, and the whole casting time is 20-30 s.
7. The preparation method of a CuMn25Ni10Sn alloy material according to claim 1, wherein after the furnace cover is covered in the step (2), the air release valve is closed, and the observation window is cleaned.
8. The method for preparing the CuMn25Ni10Sn alloy material according to claim 1, wherein in the step (3), after a mechanical pump is started, a low vacuum baffle valve is opened to vacuumize, and when the vacuum pressure p in the furnace is less than or equal to 0.08MPa, the roots pump is started.
9. The method for preparing CuMn25Ni10Sn alloy material according to claim 1, it is characterized in that when the smelting is carried out in the step (4), when the vacuum degree in the smelting furnace is pumped to p less than or equal to 10Pa, the smelting furnace is heated to raise the temperature, the heating power is raised to 20 +/-1 KW, the temperature is kept for 2-4min, heating power is increased to 30 +/-1 KW, heat preservation is carried out for 2-4min, heating power is increased to 40 +/-1 KW, heat preservation is carried out for 2-4min, heating power is increased to 50 +/-1 KW, heat preservation is carried out for 2-4min, heating power is increased to 60KW for keeping, when raw materials in a crucible in the furnace begin to melt, heating power is reduced to be below 20KW, an argon filling air valve is opened, high-purity argon is slowly filled into the furnace body of the vacuum induction smelting furnace, and when the pressure in the smelting furnace is increased to-0.08 Mpa, closing the argon filling valve, increasing the heating power to 55KW, and refining for 2-4 min.
10. The method for preparing the CuMn25Ni10Sn alloy material according to claim 1, wherein in the step (5), the power of the smelting furnace is reduced to 35KW +/-5 KW, the casting is started for 20-30s, and the whole casting time is 50-60 s.
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| CN114959356A (en) * | 2022-06-23 | 2022-08-30 | 厦门火炬特种金属材料有限公司 | Novel high-resistivity low-temperature-drift copper-based precision resistance alloy and preparation method thereof |
| CN114959356B (en) * | 2022-06-23 | 2023-08-22 | 有研金属复材(忻州)有限公司 | Copper-based precise resistance alloy with high resistivity and low temperature drift and preparation method thereof |
| CN115255711A (en) * | 2022-07-15 | 2022-11-01 | 郑州轻工业大学 | Sn-based multielement low-temperature soft solder and preparation method thereof |
| CN115255711B (en) * | 2022-07-15 | 2024-04-26 | 郑州轻工业大学 | Sn-based multielement low-temperature soft solder and preparation method thereof |
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