CN110904355A - Smelting process of lead-free nickel-based solder containing Sn and Bi - Google Patents
Smelting process of lead-free nickel-based solder containing Sn and Bi Download PDFInfo
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- CN110904355A CN110904355A CN201911259413.0A CN201911259413A CN110904355A CN 110904355 A CN110904355 A CN 110904355A CN 201911259413 A CN201911259413 A CN 201911259413A CN 110904355 A CN110904355 A CN 110904355A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3033—Ni as the principal constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- Metallurgy (AREA)
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Abstract
The invention discloses a smelting process of a lead-free nickel-based solder containing Sn and Bi, belonging to the technical field of metal smelting and casting. The lead-free nickel-based solder contains Sn and Bi elements, and the smelting process comprises the following steps: (1) smelting alloy raw materials except Sn and Bi under a vacuum condition to obtain an alloy melt; (2) adding Sn and Bi elements into an alloy melt under an inert atmosphere, wherein the adding modes are two: the first mode is as follows: directly adding simple substance raw materials of Sn and Bi elements; the second way is: adding the Ni-Bi-Sn intermediate alloy; (3) and carrying out low-temperature smelting to obtain the Sn and Bi-containing lead-free nickel-based solder. The method is suitable for preparing the lead-free nickel-based solder rich in low-melting-point elements, can improve the component control accuracy of volatile elements, further improves the product quality, and has remarkable economic benefit.
Description
Technical Field
The invention relates to the technical field of metal smelting and casting, in particular to a smelting process of nickel-based solder rich in low-melting-point elements.
Background
The nickel-based high-temperature alloy is generally used for manufacturing main structural components of engines such as gas and turbines and the like, and needs to be in service under an ultrahigh-temperature environment. On one hand, because the nickel-based superalloy component usually has a complex structure, different castings (forgings) need to be welded into an integral structure in a welding mode, but because the melting point of the alloy is high, and because the nickel-based superalloy has a complex alloying system, the control of the components of the welding flux is strict, and the situation that the local mechanical property of the component is poor due to the fact that the difference between the welding area and the main component and the structure of the component is large is avoided. On the other hand, the nickel-based superalloy component often has fatigue cracks, abrasion and other damages during service, and in order to prolong the service life of the component, the surface damage of the component is usually repaired by adopting a brazing process and other processes. Therefore, in order to improve the operability of the soldering process, it is necessary to lower the melting point of the nickel-based alloy material for preparing the solder, and thus Pb, Si, Mn, and the like, which reduce the temperature-bearing capacity of the superalloy, are widely used for manufacturing the low-melting-point nickel-based alloy material. During soldering, Pb, Si, Mn and other elements can volatilize during the melting of the solder, so that the content of low-melting-point elements in a welding area is reduced, and therefore, the control of the content of the low-melting-point elements in the nickel-based alloy material for preparing the solder is particularly important.
With the increasing awareness of the modern society on environmental protection, lead-free solder is becoming a great trend, and therefore, the development of lead-free solder has important scientific and engineering significance. In recent years, it has been found that Sn and Bi can replace Pb to some extent, and they are one of the main component characteristics of lead-free solder. Since the melting points of Sn and Bi are low, 232 ℃ and 271 ℃, respectively, and the melting point of the nickel-based alloy can be greatly reduced, and the boiling point of Bi is only 1560 ℃, and the Bi has strong volatility, most Bi in the solder can be removed by high temperature generated during soldering when the solder containing Sn and Bi is used for soldering. When the content of Sn, Bi and other elements in the solder is low, the melting point of the solder is high, which is not beneficial to welding operation; when the content of elements such as Sn, Bi and the like in the solder is high, Bi and Sn elements remained in a welding area can cause poor high-temperature mechanical property of the brazing area, so that an alloy component is easy to generate high-temperature damage, and therefore, the content control of Bi and Sn in the solder is very critical.
When the solder containing Sn and Bi is prepared by the vacuum induction furnace, Bi and Sn not only can generate burning loss to a large extent, but also can cause pollution to the induction furnace to a certain extent, and the burning loss amount of Bi is difficult to control, so that the difficulty of component control is improved. Therefore, how to accurately control the addition of Bi and Sn elements and establish a smelting process are one of the main difficulties in preparing lead-free solder.
Disclosure of Invention
In order to improve the component accuracy of the lead-free nickel-based solder, the invention provides a smelting process of a lead-free nickel material containing Sn and Bi, which is characterized in that the lead-free nickel-based solder is prepared by directly adding elements such as Sn, Bi and the like into a melt for direct smelting or by preparing Ni-Bi-Sn intermediate alloy and adding elements such as Sn, Bi and the like into the melt in the form of intermediate alloy, so that the aim of accurately controlling the contents of Sn and Bi in the solder is achieved, and the smelting process has important scientific and economic significance for improving the preparation technology and the solder quality of the lead-free nickel-based solder.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a smelting process of a lead-free nickel-based solder containing Sn and Bi, wherein the lead-free nickel-based solder contains Sn and Bi elements, and the smelting process of the lead-free nickel-based solder comprises the following steps:
(1) smelting alloy raw materials except Sn and Bi under a vacuum condition to obtain an alloy melt;
(2) adding Sn and Bi elements into an alloy melt under an inert atmosphere (argon), wherein the adding modes are two: the first mode is as follows: directly adding simple substance raw materials of Sn and Bi elements; the second way is: adding the Ni-Bi-Sn intermediate alloy;
(3) and carrying out low-temperature smelting to obtain the Sn and Bi-containing lead-free nickel-based solder.
In the step (2), when the first simple substance raw material directly added with Sn and Bi elements is adopted for smelting, the Sn content added into the melt is 1.1-1.4 times of the Sn content in the designed solder component, and the Bi content added into the melt is 2.0-2.5 times of the Bi content in the designed solder component; the composition error of the finally prepared lead-free nickel-based solder is lower than 1.0 wt.% compared with the designed solder composition.
In the step (2), when the elemental raw materials of Sn and Bi elements are directly added into the alloy melt for smelting, Sn and Bi are added in a furnace under a negative pressure state of 0.02-0.04 MPa of argon pressure.
When the lead-free nickel-based solder contains Al, Si, Mn and other elements for reducing the melting point of the alloy and Sn and Bi are added in the step (2) in the first mode, the Al, Si, Mn and other elements are added into the alloy melt together with the Sn and Bi elements.
In the step (2), when smelting is carried out by adopting a second mode of adding Ni-Bi-Sn intermediate alloy, the intermediate alloy is added when the pressure of argon in the furnace is in a negative pressure state of 0.02-0.08 MPa; the composition of the finally prepared lead-free nickel-based solder has an error of less than 0.5 wt.% compared to the designed solder composition.
In the chemical components of the Ni-Bi-Sn intermediate alloy, the mass fraction of Bi + Sn is not less than 25%, wherein the ratio of Sn to Bi in the intermediate alloy is as follows:
wherein x isSn、xBiAre respectively the design component, X, in the master alloySn、XBiRespectively representing the contents of Sn and Bi in the lead-free nickel-based solder.
The preparation process of the Ni-Bi-Sn intermediate alloy is as follows:
designing the components of the intermediate alloy according to the content ratio of Bi to Sn in the solder to be smelted; firstly, adding a Ni simple substance into a crucible, carrying out vacuum induction heating, stopping vacuumizing after Ni is completely cleared, filling argon gas of 0.02-0.08 MPa into a furnace body, and sequentially adding Sn and Bi simple substance raw materials; after the surface of the melt is stable, raising the temperature of the melt to be 30-50 ℃ higher than the liquidus, preserving the heat for 5min, then raising the temperature to 10 ℃ and casting to obtain an intermediate alloy ingot; and after the intermediate alloy ingot is cooled, cutting off a dead head and polishing the surface for later use.
The invention has the following advantages and positive effects:
1. by adopting the solder smelting process, other main elements can be purified by vacuum smelting, the final purity of the product is ensured, the Sn and Bi simple substances or Ni-Bi-Sn intermediate alloy is added under the condition of argon of 0.02-0.08 MPa, the Bi and Sn contents in the product can be accurately controlled according to the requirement, a large amount of smoke dust caused by volatilization of Bi is not generated during smelting, the observation of the condition in the furnace by operators is facilitated, the pollution degree to smelting equipment is low, and the industrial operation and the product quality control are facilitated.
2. The accurate control can be achieved by smelting the Ni-Bi-Sn intermediate alloy, and when the intermediate alloy is added during smelting, the burning loss rate of elements such as Bi, Sn and the like can be greatly reduced due to the alloying action of the intermediate alloy, so that the control of the components of the product is facilitated, and the practicability is strong.
Detailed Description
For a further understanding of the present invention, the following description is given in conjunction with the examples which are set forth to illustrate, but are not to be construed to limit the present invention, features and advantages.
When the first scheme is adopted for smelting preparation, elements for reducing the melting point of the alloy, such as Sn, Bi, Al, Si, Mn and the like, are added after being cleaned and before low-temperature refining, and the furnace is in a negative pressure state of 0.02-0.04 MPa of argon when in addition; when the scheme II is adopted for smelting preparation, the adding time of the Ni-Bi-Sn intermediate alloy is the same as that of the scheme I, but the argon amount is 0.02-0.08 MPa.
The two smelting schemes provided by the invention comprise the following steps:
the first scheme is as follows:
(1) putting a Ni plate at the bottom of the crucible, putting elementary substances except Bi and Sn on the Ni plate, and carrying out cleaning and refining by a vacuum induction furnace;
(2) after refining is finished, when the temperature is reduced to the surface of the melt to generate a solidification trend, stopping the work of the vacuum pump, closing the gate valve, filling argon gas with the pressure of 0.02-0.04 MPa into the furnace body, and adding low-melting-point and volatile simple substances such as Bi and Sn, wherein the addition amount of Bi is 2.0-2.5 times of the design components, and the addition amount of Sn is 1.1-1.4 times of the design components;
(3) after the surface of the melt is stable, low-temperature refining and casting are carried out according to alloy components;
(4) and cutting off a riser after the alloy ingot is cooled to obtain the Ni-Bi-Sn lead-free nickel-based alloy solder.
Scheme II:
(1) designing and preparing Ni-Bi-Sn intermediate alloy according to the content ratio of Sn and Bi in the design components, wherein the design principle of Sn and Bi is 1x.S2n:2x.Bi0 ≈ XSn:XBi，xSn、xBiAre respectively the design component, X, in the master alloySn、XBiThe contents of Sn and Bi in the lead-free nickel-based solder are respectively;
(2) when the intermediate alloy is smelted, firstly adding a Ni simple substance into a crucible and carrying out vacuum induction heating, stopping the vacuum pump after the Ni is completely dissolved, closing a gate valve, filling argon gas of 0.02-0.08 MPa into a furnace body, and sequentially adding Sn and Bi simple substances, wherein when the latter simple substance is added, the surface of the alloy melt is in a stable state;
(3) after the surface of the melt is stable, increasing the temperature of the melt to be 30-50 ℃ higher than the liquidus, preserving the heat for 5min, heating to 10 ℃ and casting;
(4) cutting off a riser and polishing the surface for later use after the intermediate alloy ingot is cooled;
(5) calculating the quality of the nickel-based solder which can be prepared according to the content of Sn in the intermediate alloy, filling other main elements except Bi and Sn into a crucible according to the components of the alloy, carrying out vacuum induction heating and clearing, and then carrying out a high-temperature refining process;
(6) after the high-temperature refining is finished, when the melt is cooled to the surface and has a solidification trend, stopping the work of the vacuum pump, closing the gate valve, filling argon gas with the pressure of 0.02-0.04 MPa into the furnace body, and adding Al-Bi-Sn intermediate alloy;
(7) and after the intermediate alloy is completely melted, increasing the temperature of the melt to be 30-50 ℃ higher than the liquidus, preserving the heat for 5min, heating to 10 ℃ and casting to obtain the product Ni-Bi-Sn lead-free nickel-based alloy solder.
When the Ni-Bi-Sn intermediate alloy and the Ni-Bi-Sn nickel-based solder are smelted, high-temperature refining temperature and low-temperature refining temperature can be set according to a Ni-Bi and Al-Bi binary phase diagram, wherein the high-temperature refining temperature is higher than the liquidus line by 80-100 ℃, and the low-temperature refining and casting temperature is higher than the liquidus line by 10-30 ℃. According to experience, when the product alloy is prepared by adopting the first scheme, the actual addition amount of Bi is about 2.0-2.5 times of the designed components; when the product alloy is prepared by adopting the second scheme, the actual addition amount of Bi is about 1.5-2.0 times of the designed components. Before adding Bi or the intermediate alloy containing Bi, argon is introduced into the furnace to ensure that Bi does not generate a large amount of smoke dust during smelting and the smelting state observation is influenced.
The smelting process provided by the invention can ensure that the deviation of the actually measured content of Bi in the smelted product alloy and the designed components is lower than 0.5%, and no large amount of smoke dust influences observation during preparation, and is suitable for industrial production and new product research and development.
Example 1
The Ni-4.0Bi-4.0Sn lead-free nickel-based solder is prepared, and the smelting mass is 10 kg. Alloy design composition is as in table 1:
TABLE 1
The smelting process comprises the following steps:
(1) filling a burdening list according to the design components of the alloy, wherein Sn is 4.2 wt.%, Bi is 9.0 wt.%, Mo is 1.5 wt.%, Si is 1.1 wt.%, and the balance is Ni;
(2) putting Ni, Mo and Si into a crucible, and carrying out vacuum induction heating until the melt is completely cleared;
(3) high-temperature refining: at 1450 deg.C for 5 min;
(4) after the temperature of the melt is reduced to about 1420 ℃, the vacuum pump and the gate valve are closed, and argon gas with 0.02MPa is filled;
(5) sequentially adding simple substances such as Sn, Bi and the like, and standing for 1min after the liquid level is stable;
(6) low-temperature refining: multiplying at 1330 ℃ for 5 min;
(7) casting temperature: 1340 deg.c.
The alloy chemical compositions of the products are measured as shown in the table 2:
TABLE 2
Example 2:
the solder product alloy design composition is as in table 3:
TABLE 3
Preparing an intermediate alloy:
(1) filling a mixture list, wherein Bi accounts for 20 wt.%, Sn accounts for 16 wt.%, and the balance is Ni;
(2) putting Ni into a crucible, and carrying out vacuum induction heating until the Ni is completely cleaned;
(3) high-temperature refining: multiplying at 1500 ℃ for 5 min;
(4) stopping the vacuum pump, closing the gate valve and filling argon gas with pressure of about 0.04 MPa;
(5) slowly adding Sn when the temperature of the melt is reduced to about 1400 ℃;
(6) after the surface of the melt is stable, slowly adding Bi;
(7) low-temperature refining: multiplying by 5min at 700 ℃;
(8) pouring temperature: 710 ℃.
The master alloy composition (wt.%): ni-16Bi-17 Sn.
Preparing a product alloy:
ingredients are shown in table 4:
TABLE 4
The product alloy smelting process comprises the following steps:
(1) loading other raw materials except the intermediate alloy, Mn and Si into a crucible for preparing vacuum induction melting;
(2) high-temperature refining: at 1450 deg.C for 5 min;
(3) when the temperature of the melt is reduced to about 1400 ℃, stopping the vacuum pump, closing the gate valve, and filling argon gas with about 0.02 MPa;
(4) sequentially adding Mn, Si and intermediate alloy, and after completely melting, carrying out low-temperature refining: 1250 ℃ for 5 min;
(5) casting temperature: 1260 deg.C
The actual chemical composition of the product alloy was measured as shown in table 5:
TABLE 5
Claims (7)
1. A smelting process of lead-free nickel-based solder containing Sn and Bi is characterized by comprising the following steps: the lead-free nickel-based solder contains Sn and Bi elements, and the smelting process of the lead-free nickel-based solder comprises the following steps:
(1) smelting alloy raw materials except Sn and Bi under a vacuum condition to obtain an alloy melt;
(2) adding Sn and Bi elements into an alloy melt under an inert atmosphere, wherein the adding modes are two: the first mode is as follows: directly adding simple substance raw materials of Sn and Bi elements; the second way is: adding the Ni-Bi-Sn intermediate alloy;
(3) and carrying out low-temperature smelting to obtain the Sn and Bi-containing lead-free nickel-based solder.
2. The process of smelting the lead-free nickel-based solder containing Sn and Bi as claimed in claim 1, wherein: in the step (2), when the first simple substance raw material directly added with Sn and Bi elements is adopted for smelting, the Sn content added into the melt is 1.1-1.4 times of the Sn content in the designed solder component, and the Bi content added into the melt is 2.0-2.5 times of the Bi content in the designed solder component; the composition of the finally prepared lead-free nickel-based solder has an error of less than 1.0 wt.% compared to the designed solder composition.
3. The process for smelting the lead-free nickel-based solder containing Sn and Bi as claimed in claim 1 or 2, wherein: in the step (2), when elemental raw materials of Sn and Bi elements are directly added into the alloy melt for smelting, Sn and Bi are added in a furnace under the negative pressure state of 0.02-0.04 MPa of argon pressure.
4. The process of smelting the lead-free nickel-based solder containing Sn and Bi as claimed in claim 1, wherein: when the lead-free nickel-based solder contains other elements (such as Al, Si, Mn and the like) for lowering the melting point of the alloy, the simple substances of the elements can be added into the alloy melt together with the Sn and Bi elements by adopting the first mode.
5. The process of smelting the lead-free nickel-based solder containing Sn and Bi as claimed in claim 1, wherein: in the step (2), when smelting is carried out by adopting a second mode of adding Ni-Bi-Sn intermediate alloy, the intermediate alloy is added when the pressure of argon in the furnace is in a negative pressure state of 0.02-0.08 MPa; the composition of the finally prepared lead-free nickel-based solder has an error of less than 0.5 wt.% compared to the designed solder composition.
6. The process for smelting the lead-free nickel-based solder containing Sn and Bi according to claim 1 or 5, wherein: in the chemical components of the Ni-Bi-Sn intermediate alloy, the total mass fraction of Bi and Sn is not less than 25 percent, and the balance is Ni, wherein the ratio of Sn to Bi in the intermediate alloy is calculated according to a formula (1):
in the formula (1), xSn、xBiRespectively the weight percentage of Sn and Bi in the intermediate alloy, XSn、XBiThe weight percentages of Sn and Bi in the lead-free nickel-based solder are respectively.
7. The process of claim 6, wherein: the preparation process of the Ni-Bi-Sn intermediate alloy is as follows:
designing the components of the intermediate alloy according to the content proportion of Bi and Sn in the solder to be smelted, wherein the sum of the mass fractions of Bi and Sn in the intermediate alloy is not less than 25 percent; firstly, adding a Ni simple substance into a crucible, carrying out vacuum induction heating, stopping vacuumizing after Ni is completely cleared, filling argon gas of 0.02-0.08 MPa into a furnace body, and sequentially adding Sn and Bi simple substance raw materials; after the surface of the melt is stable, raising the temperature of the melt to be 30-50 ℃ higher than the liquidus, preserving the heat for 5min, then raising the temperature to 10 ℃ and casting to obtain an intermediate alloy ingot; and after the intermediate alloy ingot is cooled, cutting off a dead head and polishing the surface for later use.
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| CN112410617A (en) * | 2020-11-17 | 2021-02-26 | 丹阳润泽新材料科技有限公司 | Nickel alloy welding wire and preparation method thereof |
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