CN110592409B - Preparation method of nickel-calcium intermediate alloy - Google Patents
Preparation method of nickel-calcium intermediate alloy Download PDFInfo
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- CN110592409B CN110592409B CN201911044265.0A CN201911044265A CN110592409B CN 110592409 B CN110592409 B CN 110592409B CN 201911044265 A CN201911044265 A CN 201911044265A CN 110592409 B CN110592409 B CN 110592409B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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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- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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Abstract
The invention belongs to the technical field of metallurgy, and particularly relates to a preparation method of a nickel-calcium intermediate alloy. The invention comprises the following steps: preparing raw materials, preparing a crucible, washing a furnace, charging the furnace, vacuumizing, filling argon, smelting nickel, smelting calcium, pouring and crushing. The invention is based on that the melting point of the nickel-calcium alloy is lower than that of the metal nickel, so that the metal liquid can be completely melted below the melting point of the nickel, the metal nickel is melted, the metal calcium is gradually melted by the enthalpy of the metal liquid, the melting point of the alloy is gradually reduced along with the melting of the metal calcium, the nickel calcium is changed into the intermediate alloy, the product can be used in the vacuum metallurgy capacity process, the metering and weighing are convenient, the alloy has high density, and the alloy is added into the nickel-containing alloy liquid and directly sinks to the bottom of the metal liquid, so that the utilization rate of the calcium is greatly improved.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a preparation method of a nickel-calcium intermediate alloy.
Background
Calcium metal, as a very active metal, is a powerful reducing agent, and its main uses include: deoxidation, desulfurization and degassing are carried out during metal melting. The calcium has active chemical property, and can form a layer of oxide or nitride film on the surface in the air, thereby slowing down further corrosion. Can be combined with oxygen to produce calcium oxide and nitrogen to produce calcium nitride Ca3N2The halogen compound is combined with fluorine, chlorine, bromine, iodine and the like to generate corresponding halide, and is combined with hydrogen to generate calcium hydride under the action of a catalyst at 400 ℃. Reacting with water at normal temperature to generate calcium hydroxide and release hydrogen, reacting with dilute sulphuric acid hydrochloride to generate salt and hydrogen, and reacting with carbon at high temperature to generate calcium carbide CaC2. The metal calcium has low melting point (828 deg.C), low boiling point (1484 deg.C), low solubility in molten metal (0.03% at 1600 deg.C and calcium vapor pressure of 0.186 MPa), and low calcium density (1.55 g/cm)3) The metal liquid is added to the slag to be easy to float to the surface of the slag to react with oxygen in the air and oxides in the slag liquid to be burnt away. In the traditional steelmaking process, the CaFe cored wire is generally added to the deep part of molten metal as much as possible, and the calcium reacts with oxygen, sulfur and the like in steel before being changed into calcium bubbles by utilizing the static pressure of the molten metal, so that the calcium bubbles are prevented from floating and losing once being added. When alloy containing nickel is vacuum smelted, the method is difficult to quantitatively use because of the requirement of vacuum sealing. Therefore, a nickel-calcium intermediate alloy is needed to be developed, and the nickel-calcium intermediate alloy is convenient to melt and use in vacuum. While the melting point of nickel is 1453 ℃, the density is 8.902g/cm3The physical properties of the two materials are obviously different, and the volatilization point of calcium is basically reached when the melting point of nickel is reached, so a good smelting process must be found to be convenient for smelting the alloy.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a nickel-calcium intermediate alloy aiming at the defects of the prior art. The method solves the problem that the nickel-containing alloy smelted in the vacuum smelting state can not be quantitatively added with calcium for desulfurization and deoxidation operation. The temperature control is enhanced, the temperature is controlled within the range of 1430-1460 ℃, and the direct sublimation of the metal calcium can be caused due to overhigh temperature; the aeration control is enhanced, and the vapor pressure of calcium can be reduced and the volatilization of calcium can be prevented when the aeration of argon exceeds the standard atmospheric pressure; the smelting control is optimized, the characteristic that the melting point of the intermediate alloy is lower than that of pure metal is adopted, the high-melting-point alloy is smelted firstly, and then the low-melting-point alloy is added.
In order to solve the technical problems, the invention adopts the technical scheme that: the preparation method of the nickel-calcium intermediate alloy is characterized by comprising the following steps of:
a preparation method of a nickel-calcium intermediate alloy comprises the following steps:
(1) preparing raw materials: preparing a high-purity nickel plate with the purity of more than 99 percent and metallic calcium with the purity of more than 98 percent and the granularity of 2-5 mm, cutting the nickel plate into nickel blocks, drying the nickel blocks in a vacuum oven at the temperature of 110-120 ℃, wherein the vacuum degree is less than or equal to 1 multiplied by 10-1Pa；
(2) Preparing a crucible: baking the calcium oxide crucible in a vacuum oven for 1-4 hours at the temperature of 110 DEG CAt 120 deg.C and vacuum degree of 1 × 10 or less-1Pa, and adopting a dry method to make the pan;
(3) washing the furnace: before smelting, washing the smelting furnace with high-purity nickel, and then baking a crucible;
(4) charging: adding the nickel block obtained in the step (1) into a crucible with the temperature of 50-100 ℃, and fixing metal calcium coated by nickel foil at the bottom end of an upper material rod;
(5) vacuumizing: smelting alloy in a vacuum induction smelting furnace, and pumping vacuum to less than or equal to 1 × 10-3Pa, then filling argon to (0.8-1.0) x 105Pa, then vacuumized to less than or equal to 1 × 10-3Pa, repeating the steps for three times;
(6) filling argon gas: charging argon gas into the vacuum induction melting furnace to (1.03-1.05) × 105Pa, ensuring that the pressure in the furnace is greater than the external atmospheric pressure during smelting;
(7) smelting nickel: controlling the power of a vacuum induction smelting furnace to be 50-200 kW, fully melting nickel, reducing the power after complete melting, and keeping the power unchanged after the surface of molten metal is slightly crusted;
(8) smelting calcium: adopting nickel foil to wrap calcium, fixing the nickel foil at the bottom end of an upper material rod, directly pricking the upper material rod into molten metal, and increasing power to raise the temperature in the furnace to 1440-1450 ℃;
(9) pouring: reducing the heating power to keep the temperature of the molten metal at 1410-1420 ℃, and casting the molten metal in a mold;
(10) crushing: vacuumizing to less than or equal to 1 × 10-3Pa, then filling argon to (0.8-1.0) x 105And Pa, repeating the steps for 3 times, cooling for 1-4 hours, taking out the cast ingot, cooling to room temperature, and crushing in a crusher to control the particle size to be 10-50 mm.
The smelting furnace adopted in the step (3) is a vacuum smelting furnace.
And (5) the purity of the argon in the step (5) and the step (6) is 99.99 percent of high-purity argon.
And (8) measuring the temperature by adopting an infrared temperature measuring system.
In the step (9), the die is a square die, and the height of the die is 10-50 mm.
In the step (10), the crusher is a jaw crusher.
Compared with the prior art, the invention has the following advantages:
(1) the invention changes nickel calcium into intermediate alloy, and compared with CaFe core-spun yarn, the product can be used in vacuum metallurgy capacity process, and is convenient for metering.
(2) The alloy prepared by the method has high density, and is added into the nickel-containing alloy liquid to directly sink to the bottom of the molten metal, so that the utilization rate of calcium is greatly improved.
(3) The invention adopts the characteristic that the melting point of the intermediate alloy is lower than that of pure metal, and provides a good method for the intermediate alloy with the boiling point close to the melting point of another metal.
Drawings
FIG. 1 is a flow chart of the preparation method of the nickel-calcium intermediate alloy of the invention.
Detailed Description
Example 1
A preparation method of a nickel-calcium intermediate alloy comprises the following steps:
(1) preparing raw materials: preparing a high-purity nickel plate with the purity of more than 99 percent and metallic calcium with the purity of more than 98 percent and the granularity of 2-5 mm, wherein the weight of the metallic calcium containing nickel foil is 7 kilograms; cutting nickel plate into pieces of 20mm × 20mm, weighing 93kg, oven drying at 110 deg.C and vacuum degree of 1 × 10-1Pa；
(2) Preparing a crucible: drying in a vacuum oven at 110 deg.C and 1 × 10 vacuum degree using a calcium oxide crucible-1Pa, baking for 2 hours, and baking in a pan by adopting a dry method;
(3) washing the furnace: before smelting, a high-purity nickel smelting furnace is used, so that the furnace condition is convenient to check, a crucible is baked, and the crucible is prevented from being wet;
(4) charging: adding a nickel block into a crucible with the temperature of 50 ℃, and fixing metal calcium coated by nickel foil at the bottom end of an upper material rod;
(5) vacuumizing: the alloy is smelted by vacuum induction smelting, and the vacuum degree is firstly pumped to 1 multiplied by 10-3Pa, then filling argon to 0.8X 105Pa, then vacuumized to 110-3Pa, repeating the steps for 3 times;
(6) filling argon gas: filling argon into the furnace body to 1.03 multiplied by 105Pa；
(7) Smelting nickel: the processing rate is 80kW, so that the nickel is fully melted, the power is reduced after the nickel is completely melted, the surface of the molten metal is slightly encrusted, and the power is kept unchanged;
(8) smelting calcium: wrapping calcium by nickel foil, fixing the nickel foil at the bottom end of an upper material rod, directly pricking the upper material rod into molten metal, and increasing power to enable the temperature to reach 1450 ℃;
(9) pouring: reducing the heating power, keeping the temperature of the metal liquid at 1419 ℃, and casting in a mould;
(10) crushing: vacuum-pumping to 1 × 10-3Pa then argon to 0.8X 105And Pa, repeating the steps for 3 times, cooling for 3 hours, taking out the cast ingot, cooling to room temperature, and crushing in a crusher with the average particle size of 10-50 mm.
The smelting furnace adopted in the step (3) is a vacuum smelting furnace.
And (5) the purity of the argon in the step (5) and the step (6) is 99.99 percent of high-purity argon.
And (8) measuring the temperature by adopting an infrared temperature measuring system.
In the step (9), the die is a square die, and the die is 1000mm long, 500mm wide and 30mm high.
In the step (10), the crusher is a jaw crusher.
Example 2
A preparation method of a nickel-calcium intermediate alloy comprises the following steps:
(1) preparing raw materials: preparing high-purity calcium metal with the purity of more than 98 percent and the granularity of 2-5 mm for a high-purity nickel plate with the purity of more than 99 percent, wherein the weight of the nickel foil containing the calcium metal is 8 kilograms; cutting nickel plate into 40mm × 40mm pieces with weight of 42kg, drying in vacuum oven at 110 deg.C and vacuum degree of 1 × 10-1Pa；
(2) Preparing a crucible: drying in a vacuum oven at 110 deg.C and 1 × 10 vacuum degree using a calcium oxide crucible-1Pa, baking time4 hours, adopting a dry method to make the pan;
(3) washing the furnace: before smelting, a high-purity nickel smelting furnace is used, so that the furnace condition is convenient to check, a crucible is baked, and the crucible is prevented from being wet;
(4) charging: adding a nickel block into a crucible with the temperature of 50 ℃, and fixing metal calcium coated by nickel foil at the bottom end of an upper material rod;
(5) vacuumizing: the alloy is smelted by vacuum induction smelting, and the vacuum degree is firstly pumped to 1 multiplied by 10-3Pa, then filling argon to 1.0X 105Pa, then vacuumized to 1X 10-3Pa, repeating the steps for 3 times;
(6) filling argon gas: filling argon into the furnace body to 1.05X 105Pa；
(7) Smelting nickel: the processing rate is 50kW, so that the nickel is fully melted, the power is reduced after the nickel is completely melted, the surface of the molten metal is slightly encrusted, and the power is kept unchanged;
(8) smelting calcium: wrapping calcium by nickel foil, fixing the nickel foil at the bottom end of an upper material rod, directly pricking the upper material rod into molten metal, and increasing power to ensure that the temperature is 1440 ℃;
(9) pouring: reducing the heating power to maintain the temperature of the metal liquid at 1410 ℃, and casting the metal liquid in a mould;
(10) crushing: vacuum-pumping to 1 × 10-3Pa then argon to 1.0X 105And Pa, repeating the steps for 3 times, cooling for 4 hours, taking out the cast ingot, cooling to room temperature, and crushing in a crusher with the average particle size of 10-50 mm.
The smelting furnace adopted in the step (3) is a vacuum smelting furnace.
And (5) the purity of the argon in the step (5) and the step (6) is 99.99 percent of high-purity argon.
And (8) measuring the temperature by adopting an infrared temperature measuring system.
In the step (9), the die is a square die, and the die is 1000mm long, 500mm wide and 30mm high.
In the step (10), the crusher is a jaw crusher.
The principle of the preparation method is based on that the melting point of the nickel-calcium alloy is lower than that of the metal nickel, so that the metal liquid can be completely melted below the melting point of the nickel, the metal calcium is gradually melted by the enthalpy of the metal liquid after the metal nickel is melted, and the melting point of the alloy is gradually reduced along with the melting of the metal calcium.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art will appreciate that various modifications and equivalent arrangements can be made within the spirit and scope of the present invention without departing from the spirit and scope of the present invention, which is defined by the appended claims.
Claims (6)
1. The preparation method of the nickel-calcium intermediate alloy is characterized by comprising the following steps of:
(1) preparing raw materials: preparing a high-purity nickel plate with the purity of more than 99 percent and metallic calcium with the purity of more than 98 percent and the granularity of 2-5 mm, cutting the nickel plate into nickel blocks, drying the nickel blocks in a vacuum oven at the temperature of 110-120 ℃, wherein the vacuum degree is less than or equal to 1 multiplied by 10-1Pa；
(2) Preparing a crucible: baking the calcium oxide crucible in a vacuum oven for 1-4 hours, wherein the temperature of the oven is 110-120 ℃, and the vacuum degree is less than or equal to 1 multiplied by 10-1Pa, and adopting a dry method to make the pan;
(3) washing the furnace: before smelting, washing the smelting furnace with high-purity nickel, and then baking a crucible;
(4) charging: adding the nickel block obtained in the step (1) into a crucible with the temperature of 50-100 ℃, and fixing metal calcium coated by nickel foil at the bottom end of an upper material rod;
(5) vacuumizing: smelting alloy in a vacuum induction smelting furnace, and pumping vacuum to less than or equal to 1 × 10-3Pa, then filling argon to (0.8-1.0) x 105Pa, then vacuumized to less than or equal to 1 × 10-3Pa, repeating the steps for three times;
(6) filling argon gas: charging argon gas into the vacuum induction melting furnace to (1.03-1.05) × 105Pa, ensuring that the pressure in the furnace is greater than the external atmospheric pressure during smelting;
(7) smelting nickel: controlling the power of a vacuum induction smelting furnace to be 50-200 kW, fully melting nickel, reducing the power after complete melting, and keeping the power unchanged after the surface of molten metal is slightly crusted;
(8) smelting calcium: adopting nickel foil to wrap calcium, fixing the nickel foil at the bottom end of an upper material rod, directly pricking the upper material rod into molten metal, and increasing power to raise the temperature in the furnace to 1440-1450 ℃;
(9) pouring: reducing the heating power to keep the temperature of the molten metal at 1410-1420 ℃, and casting the molten metal in a mold;
(10) crushing: vacuumizing to less than or equal to 1 × 10-3Pa, then filling argon to (0.8-1.0) x 105And Pa, repeating the steps for 3 times, cooling for 1-4 hours, taking out the cast ingot, cooling to room temperature, and crushing in a crusher to control the particle size to be 10-50 mm.
2. The method for preparing the nickel-calcium intermediate alloy according to claim 1, wherein the smelting furnace used in the step (3) is a vacuum smelting furnace.
3. The method for preparing a nickel-calcium master alloy according to claim 1, wherein the argon purity in the steps (5) and (6) is 99.99% high purity argon.
4. The method for preparing the nickel-calcium intermediate alloy as claimed in claim 1, wherein the temperature in the step (8) is measured by an infrared temperature measuring system.
5. The method for preparing the nickel-calcium intermediate alloy according to claim 1, wherein the die in the step (9) is a square die, and the height of the die is 10-50 mm.
6. The method for preparing a nickel-calcium master alloy according to claim 1, wherein the crusher in the step (10) is a jaw crusher.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3124137A1 (en) * | 2015-07-30 | 2017-02-01 | Belenos Clean Power Holding AG | Method for the production of msnx nanoparticles as anode materials for a rechargeable battery |
| CN107686901A (en) * | 2016-08-04 | 2018-02-13 | 中国科学院金属研究所 | A kind of high purity nickel or high temperature alloy smelting process using pure calcium line |
| CN108950307A (en) * | 2018-07-23 | 2018-12-07 | 江苏美特林科特殊合金股份有限公司 | A kind of nickel calcium intermediate alloy and the preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3124137A1 (en) * | 2015-07-30 | 2017-02-01 | Belenos Clean Power Holding AG | Method for the production of msnx nanoparticles as anode materials for a rechargeable battery |
| CN107686901A (en) * | 2016-08-04 | 2018-02-13 | 中国科学院金属研究所 | A kind of high purity nickel or high temperature alloy smelting process using pure calcium line |
| CN108950307A (en) * | 2018-07-23 | 2018-12-07 | 江苏美特林科特殊合金股份有限公司 | A kind of nickel calcium intermediate alloy and the preparation method and application thereof |
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