CN115921800A - Production method of nickel-titanium alloy ingot with low oxygen content and low porosity - Google Patents
Production method of nickel-titanium alloy ingot with low oxygen content and low porosity Download PDFInfo
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- CN115921800A CN115921800A CN202211717803.XA CN202211717803A CN115921800A CN 115921800 A CN115921800 A CN 115921800A CN 202211717803 A CN202211717803 A CN 202211717803A CN 115921800 A CN115921800 A CN 115921800A
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Abstract
The invention particularly relates to a production method of a nickel-titanium alloy ingot with low oxygen content and low porosity, which solves the problems of high porosity and high oxygen content in the existing smelting mode of nickel-titanium alloy ingots. A production method of a nickel-titanium alloy ingot with low oxygen content and low porosity is realized by adopting the following steps: step S1: weighing sponge titanium and electrolytic nickel according to the alloy component proportion; step S2: placing titanium sponge and electrolytic nickel into a water-cooled copper crucible, and starting a vacuum pump to vacuumize; and step S3: baking the metal in the water-cooled copper crucible; and step S4: increasing the induction heating power; step S5: refining the molten metal after the metal is completely melted; step S6: and then pouring the molten metal into a casting mold, and cooling and taking out to obtain the nickel-titanium alloy ingot. The invention realizes the production and manufacture of the nickel-titanium alloy cast ingot with low oxygen content and low porosity; the gas can be effectively discharged in the manufacturing process, and the generation of pores is reduced.
Description
Technical Field
The invention relates to the technical field of nickel-titanium alloy production, in particular to a production method of a nickel-titanium alloy ingot with low oxygen content and low porosity.
Background
The nickel-titanium shape memory alloy material has excellent shape memory effect and superelasticity, is wear-resistant and corrosion-resistant, has good biocompatibility, and is widely applied to the fields of electronics, aerospace, medical instruments and the like. The excellent nickel-titanium alloy cast ingot is the core basis for preparing nickel-titanium shape memory alloy products, the content of impurity elements in the nickel-titanium alloy cast ingot has important influence on the performance of the material, wherein carbon and oxygen are the two most main impurity elements, and the control of the content of the carbon and the content of the oxygen is beneficial to preparing the high-quality nickel-titanium alloy material.
Currently, nickel-titanium alloy cast ingots are smelted mainly in three ways: one is vacuum induction melting, which can obtain cast ingots with better component uniformity, but because of static mold casting, the molten metal solidification process has bad exhaust, higher porosity, coarse grains, and over-high porosity and coarse grains are easy to cause material cracking and fracture in the subsequent processing process; the second is vacuum arc consumable melting, because the density difference of nickel and titanium elements is large, cast ingots with uniform components are difficult to obtain in the vacuum arc consumable melting; the third method is a two-step smelting method combining vacuum induction smelting and vacuum arc consumable smelting, wherein nickel-titanium alloy ingots are obtained by adopting vacuum induction smelting, then the head and the tail of one ingot are cut off, the surface of the ingot is removed, a plurality of ingots are welded together and then smelted by adopting vacuum arc consumable smelting, and the nickel-titanium alloy ingots with larger weight can be obtained, but the problem of poor component uniformity still exists, the process is complex, the energy consumption is higher, and the material loss is larger.
The carbon content is usually avoided being effectively reduced by adopting a graphite crucible when the nickel-titanium alloy cast ingot is produced, but the conventional method for reducing the oxygen content is to add a certain amount of industrial pure calcium particles as an oxygen scavenger.
Therefore, there is a need to provide a method for producing a low oxygen content and low porosity nitinol ingot to solve the above problems.
Disclosure of Invention
The invention provides a production method of a nickel-titanium alloy ingot with low oxygen content and low porosity, aiming at solving the problems of high porosity and high oxygen content in the existing smelting mode of the nickel-titanium alloy ingot.
The invention is realized by adopting the following technical scheme:
a production method of a nickel-titanium alloy ingot with low oxygen content and low porosity is realized by adopting the following steps:
step S1: weighing sponge titanium and electrolytic nickel according to the alloy component proportion;
step S2: putting weighed titanium sponge and electrolytic nickel into a water-cooled copper crucible in a vacuum induction melting furnace, closing the furnace chamber, starting a vacuum pump to vacuumize to ensure that the vacuum degree in the furnace chamber reaches 8 multiplied by 10 -3 Pa; meanwhile, a heating and heat-insulating device is arranged on the outer side of the casting mold, and the heating and heat-insulating device is started to heat the casting mold to 300-600 ℃;
and step S3: starting an induction heater, setting the power of the induction heater to be 5-10kw, and then baking the metal in the water-cooled copper crucible for 15min-45min;
and step S4: increasing the power of the induction heater to 40kw to 60kw to completely melt the metal in the water-cooled copper crucible;
step S5: after the metal is completely melted, adjusting the power of the induction heater to be 20kw to 45kw, then refining the molten metal for 5min to 30min, and keeping the vacuum pump in a working state in the refining process;
step S6: argon with the purity of 99.999 percent is filled in the water-cooled copper crucible, so that the vacuum degree in the furnace cavity reaches 300Pa; meanwhile, connecting an ultrasonic vibration device on a supporting plate at the bottom of the casting mold, starting the ultrasonic vibration device and setting the ultrasonic vibration frequency to be 20kHz-40kHz; and then pouring the molten metal into a casting mold, and cooling and taking out to obtain the nickel-titanium alloy ingot.
The invention has reasonable and reliable structural design, and adopts the water-cooled copper crucible to effectively avoid the problem that the carbon and oxygen content of the material is additionally increased when the graphite crucible and the oxide crucible are smelted; the low-power baking can effectively remove gas adsorbed on the surface of the material, particularly the surface of the titanium sponge, and avoid the reaction of the titanium sponge and oxygen after the metal is melted to generate stable compounds which are difficult to eliminate; refining in a vacuum state can further promote the gas in the molten metal to be discharged, so that the gas content of the molten metal is reduced; the residual gas in the metal liquid can be discharged by filling high-purity argon under a certain pressure, so that the generation of pores is reduced; the heating and heat-insulating device arranged outside the casting mould can effectively control the solidification speed of the alloy melt, and provide certain floating discharge time for gas, meanwhile, the ultrasonic vibration device added to the casting mould can promote the discharge and loose closure of the gas, so that the porosity is further reduced, and the ultrasonic vibration device can also break coarse dendritic crystal grains to obtain a more compact ingot casting structure.
Drawings
FIG. 1 is a pore micrograph of a nickel titanium alloy ingot according to the present invention.
Detailed Description
Example 1
A production method of a nickel-titanium alloy ingot with low oxygen content and low porosity is realized by adopting the following steps:
step S1: according to the atomic ratio of 50: weighing sponge titanium and electrolytic nickel according to the alloy component ratio of 50;
step S2: placing weighed titanium sponge and electrolytic nickel into a water-cooled copper crucible in a vacuum induction melting furnace, closing the furnace chamber, starting a vacuum pump to vacuumize to enable the vacuum degree in the furnace chamber to reach 8 multiplied by 10 -3 Pa; meanwhile, a heating and heat-insulating device is arranged on the outer side of the casting mold, and the heating and heat-insulating device is started to heat the casting mold to 300 ℃;
and step S3: starting the induction heater, setting the power of the induction heater to be 5kw, and then baking the metal in the water-cooled copper crucible for 15min;
and step S4: increasing the power of the induction heater to 40kw so that the metal in the water-cooled copper crucible is completely melted;
step S5: after the metal is completely melted, adjusting the power of the induction heater to 20kw, then refining the molten metal for 5min, and keeping the vacuum pump in a working state in the refining process;
step S6: argon with the purity of 99.999 percent is filled in the water-cooled copper crucible, so that the vacuum degree in the furnace cavity reaches 300Pa; meanwhile, an ultrasonic vibration device is connected to a supporting plate at the bottom of the casting mold, the ultrasonic vibration device is started, and the ultrasonic vibration frequency is set to be 20Hz; and then pouring the molten metal into a casting mold, and cooling and taking out to obtain the nickel-titanium alloy ingot.
The casting mold in the step S2 is made of graphite with high strength, high purity and high density.
Example 2
A production method of a nickel-titanium alloy ingot with low oxygen content and low porosity is realized by adopting the following steps:
step S1: according to the atomic ratio of 50.2:49.8, weighing sponge titanium and electrolytic nickel according to the alloy component ratio;
step S2: placing weighed titanium sponge and electrolytic nickel into a water-cooled copper crucible in a vacuum induction melting furnace, closing the furnace chamber, starting a vacuum pump to vacuumize to enable the vacuum degree in the furnace chamber to reach 8 multiplied by 10 -3 Pa; meanwhile, a heating and heat-insulating device is arranged on the outer side of the casting mold, and the heating and heat-insulating device is started to heat the casting mold to 450 ℃;
and step S3: starting the induction heater, setting the power of the induction heater to be 8kw, and then baking the metal in the water-cooled copper crucible for 30min;
and step S4: increasing the power of the induction heater to 50kw so that the metal in the water-cooled copper crucible is completely melted;
step S5: after the metal is completely melted, adjusting the power of the induction heater to 30kw, then refining the molten metal for 15min, and keeping the vacuum pump in a working state in the refining process;
step S6: argon with the purity of 99.999 percent is filled in the water-cooled copper crucible, so that the vacuum degree in the furnace cavity reaches 300Pa; meanwhile, an ultrasonic vibration device is connected to a supporting plate at the bottom of the casting mold, the ultrasonic vibration device is started, and the ultrasonic vibration frequency is set to be 33KHz; and then pouring the molten metal into a casting mold, and cooling and taking out to obtain the nickel-titanium alloy ingot.
The casting mold in the step S2 is made of graphite with high strength, high purity and high density.
Example 3
A production method of a nickel-titanium alloy ingot with low oxygen content and low porosity is realized by adopting the following steps:
step S1: according to the atomic ratio of 50.5:49.5, weighing sponge titanium and electrolytic nickel according to the alloy component ratio;
step S2: placing weighed titanium sponge and electrolytic nickel into a water-cooled copper crucible in a vacuum induction melting furnace, closing the furnace chamber, starting a vacuum pump to vacuumize to enable the vacuum degree in the furnace chamber to reach 8 multiplied by 10 -3 Pa; meanwhile, a heating and heat-insulating device is arranged on the outer side of the casting mold, and the heating and heat-insulating device is started to heat the casting mold to 600 ℃;
and step S3: starting the induction heater, setting the power of the induction heater to 10kw, and then baking the metal in the water-cooled copper crucible for 45min;
and step S4: increasing the power of the induction heater to 60kw so that the metal in the water-cooled copper crucible is completely melted;
step S5: after the metal is completely melted, adjusting the power of the induction heater to 45kw, then refining the molten metal for 30min, and keeping the vacuum pump in a working state in the refining process;
step S6: argon with the purity of 99.999 percent is filled into the water-cooled copper crucible, so that the vacuum degree in the furnace cavity reaches 300Pa; meanwhile, an ultrasonic vibration device is connected to a bearing plate at the bottom of the casting mold, and the ultrasonic vibration device is started and the ultrasonic vibration frequency is set to be 40KHz; and then pouring the molten metal into a casting mold, and cooling and taking out to obtain the nickel-titanium alloy ingot.
The casting mold in the step S2 is made of graphite with high strength, high purity and high density.
The following table shows the nickel titanium alloy ingot test results of examples 1-3:
nickel-titanium alloy ingot | Carbon content (wt%) | Oxygen content (wt%) | Porosity (%) |
Example 1 | 0.0024 | 0.0154 | <0.2 |
Example 2 | 0.0028 | 0.0149 | <0.2 |
Example 3 | 0.0031 | 0.0162 | <0.2 |
Conventional methods | 0.02~0.06 | 0.04~0.08 | 0.4~0.6 |
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that these are by way of example only, and that the scope of the invention is defined by the appended claims. Various changes and modifications to these embodiments may be made by those skilled in the art without departing from the spirit and scope of the invention, and these changes and modifications are within the scope of the invention.
Claims (2)
1. A production method of a nickel-titanium alloy ingot with low oxygen content and low porosity is characterized by comprising the following steps: the method is realized by adopting the following steps:
step S1: weighing sponge titanium and electrolytic nickel according to the alloy component proportion;
step S2: placing weighed titanium sponge and electrolytic nickel into a water-cooled copper crucible in a vacuum induction melting furnace, closing the furnace chamber, starting a vacuum pump to vacuumize to enable the vacuum degree in the furnace chamber to reach 8 multiplied by 10 -3 Pa; meanwhile, a heating and heat-insulating device is arranged on the outer side of the casting mold, and the heating and heat-insulating device is started to heat the casting mold to 300-600 ℃;
and step S3: starting an induction heater, setting the power of the induction heater to be 5-10kw, and then baking the metal in the water-cooled copper crucible for 15min-45min;
and step S4: increasing the power of the induction heater to 40kw to 60kw so that the metal in the water-cooled copper crucible is completely melted;
step S5: after the metal is completely melted, adjusting the power of the induction heater to be 20kw to 45kw, then refining the molten metal for 5min to 30min, and keeping the vacuum pump in a working state in the refining process;
step S6: argon with the purity of 99.999 percent is filled in the water-cooled copper crucible, so that the vacuum degree in the furnace cavity reaches 300Pa; meanwhile, connecting an ultrasonic vibration device on a supporting plate at the bottom of the casting mold, starting the ultrasonic vibration device and setting the ultrasonic vibration frequency to be 20kHz-40kHz; and then pouring the molten metal into a casting mold, and taking out after cooling to obtain the nickel-titanium alloy ingot.
2. The method for producing the low-oxygen content and low-porosity nickel-titanium alloy ingot according to claim 1, wherein the method comprises the following steps: the casting mold in the step S2 is made of graphite.
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