CN113174512A - Non-cold-deformation high-elastic thermal effect Ti-Ni bulk material and preparation method thereof - Google Patents
Non-cold-deformation high-elastic thermal effect Ti-Ni bulk material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a non-cold-deformation high-elastic thermal effect Ti-Ni block material and a preparation method thereof, wherein the preparation method comprises the following steps: carrying out argon arc melting on metal raw materials of 48.8-49.3% of Ti and 50.7-51.2% of Ni; suction casting and molding the molten alloy and performing wire cut electrical discharge machining; solid solution homogenization treatment is carried out to homogenize the microcosmic components, aging treatment and electrochemical surface finishing are carried out to obtain coarse crystal bulk Ti-Ni alloy bulk materials. The Ti-Ni bulk material prepared by the invention does not need cold deformation processing, the thickness of the plate-shaped bulk material is in millimeter level, the similar elastic heat effect is realized under the non-cold deformation condition, the maximum adiabatic temperature change can reach 22.7K, and the elastic heat refrigeration application in a wider range can be realized. The method obviously improves the elastic heat effect of the material and has wide application prospect.
Description
Technical Field
The invention relates to a non-cold-deformation block Ti-Ni alloy material with high elastic heat performance and a preparation method thereof, in particular to a block Ti-Ni material which can exceed 19K of heat insulation temperature drop.
Background
Refrigeration technology in the world is widely applied nowadays, the refrigeration energy consumption is more than 20% of the global total power consumption, however, the traditional refrigeration technology represented by vapor compression brings a series of environmental problems at the same time. The pop-up refrigeration technology has the advantages of environmental friendliness and high refrigeration efficiency, is considered to be one of the most potential new refrigeration technologies for replacing old refrigeration mechanisms, and has attracted extensive attention in recent years.
The basic performance evaluation indexes of the elastic thermal material are adiabatic temperature change and isothermal entropy change under specific environment. The application of large-scale elastic heating materials requires that the materials have high heat insulation temperature change and a block material state at the same time. Most of the existing shape memory alloy materials with high elastic thermal property are wire materials or film materials, which limits the application of elastic thermal materials in large scale; in addition, the manufacturing of shape memory alloys such as wire and sheet depends on low-temperature cold deformation machining means such as drawing and extrusion, and the machining is difficult and time-consuming, and has strict requirements on material plasticity. Therefore, the optimization of the elastic-thermal performance of the block alloy and the improvement of the material processing conditions have important significance for promoting the application of the elastic-thermal material.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a non-cold-deformation high-elasticity thermal effect Ti-Ni bulk material and a preparation method thereof, wherein the elasticity thermal effect is enhanced by generating a nano-scale precipitate and regulating the content of the nano-scale precipitate, so that the mechanical processing processes such as cold deformation and the like in alloy manufacturing are avoided; the prepared block material has high elastic thermal property and material macro scale of millimeter level.
The invention is realized by the following technical scheme.
A non-cold-deformation high-elastic-heat Ti-Ni bulk material and a preparation method thereof comprise the following steps:
1) carrying out argon arc melting on raw materials of 48.8-49.3% of Ti and 50.7-51.2% of Ni according to the atomic ratio under the working current of a melting furnace, carrying out electromagnetic stirring, and carrying out ingot casting and turn-over melting for multiple times to obtain a Ti-Ni ingot casting block material;
2) heating the ingot block material backing material treated in the step 1) into a molten state through electric arcs, carrying out vacuum suction casting to obtain a formed ingot block material, and cutting the formed ingot block material into an alloy plate-shaped block material;
3) polishing the plate-shaped block material treated in the step 2) to remove a surface oxide layer, and carrying out solid solution homogenization treatment under a vacuum condition to homogenize microscopic components of the alloy;
4) sealing the plate-shaped block material treated in the step 3) in an Ar gas environment, carrying out aging treatment, and then carrying out water-cooling quenching treatment to room temperature to obtain an aged coarse-grained alloy plate-shaped block material;
5) and 4) carrying out surface finishing on the plate-shaped block material treated in the step 4) by an electrochemical polishing method to finally obtain the millimeter-sized thick non-cold-deformation coarse-crystal Ti-Ni alloy plate-shaped block material.
With respect to the above technical solutions, the present invention has a further preferable solution:
preferably, in the step 1), a Cr element with an atomic ratio of less than or equal to 0.5% is further doped into 50.7-51.2% of Ni as a raw material to further regulate and control the internal consumption behavior in the phase change process of the alloy.
Preferably, in the step 1), the ingot is smelted for 1min and turned over for 5 times at 300-450A working current; the melting electromagnetic stirring current is 15A.
Preferably, in the step 2), the casting mold is cooled by room-temperature circulating water, and the opening time is 60-90 s after suction casting.
Preferably, in the step 3), the degree of vacuum of the solution treatment is 10-4～10-3Pa, the temperature is 1100 ℃, and the treatment time is 0.5-2 h.
Preferably, in the step 4), the aging treatment is carried out at 300-375 ℃, and the treatment time is 0.5-25 h.
Preferably, in the step 5), the electrochemical polishing method includes: the polishing solution is a mixed solution of sulfuric acid and methanol in a volume ratio of 1:4, the temperature of the solution is-20 ℃, and the voltage is 25-30V.
The non-cold-deformation high-elasticity thermal effect block Ti-Ni material prepared by the method comprises the following chemical components:
the elements are 48.8-49.3% Ti and 50.7-51.2% Ni according to atomic ratio. Further, Cr with an atomic ratio of not more than 0.5% is doped into the Ni element.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1) the invention is based on the coarse-grain Ti-Ni shape memory alloy, the elastic-thermal effect is obviously influenced by the fine adjustment of the components, and the proper amount of nano-scale precipitates are ensured to be generated in the alloy by accurately adjusting and controlling the alloy components and combining proper homogenization and aging conditions, so that the high elastic-thermal refrigeration effect is realized in the non-cold-processed coarse-grain alloy, and the adiabatic temperature change exceeding 19K is directly measured.
2) The invention can further regulate and control the internal consumption behavior of the shape memory alloy in the phase change process by introducing the third element Cr.
3) The Ti-Ni bulk alloy in the plate-shaped form is prepared by methods such as suction casting, the elastothermal effect of the plate-shaped bulk alloy is enhanced only by accurately designing and combining the components and appropriate homogenization and aging treatment conditions, the elastothermal performance of the alloy is not required to be improved by a mechanism of improving the grain boundary and dislocation density, various machining operations such as cold deformation and the like are avoided in the integral preparation process of the alloy, the material processing difficulty and time cost are reduced, and the macroscopic scale of the alloy material is effectively improved.
4) The Ti-Ni alloy plate-shaped block material prepared by the method is a block material with the thickness of millimeter level, and can be applied to a large range.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention:
FIG. 1 is a block diagram of the process of the present invention.
Detailed Description
The present invention will now be described in detail with reference to the drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the present invention are provided to explain the present invention without limiting the invention thereto.
As shown in FIG. 1, the preparation method of the non-cold-deformation high-elasticity thermal effect Ti-Ni bulk material provided by the invention comprises the following steps:
(1) alloy melting
Proportioning raw materials of 48.8-49.3% of Ti and 50.7-51.2% of Ni according to the atomic ratio, carrying out argon arc melting on the raw materials under the working current of a melting furnace, carrying out electromagnetic stirring with the current of 15A in the melting process, and carrying out single 1-minute melting and 5-time turn-over on an ingot under the working current of 300-450A to obtain the Ti-Ni ingot block material base material with the solid solution strengthening effect. The raw material 50.7-51.2% of Ni can be further doped with Cr with the atomic ratio less than or equal to 0.5% so as to further enhance the phase change regulation effect of the precipitates.
(2) Suction casting molding
And (2) heating the ingot block material backing material processed in the step (1) into a molten state through electric arcs, stopping the electric arcs, carrying out vacuum suction casting, enabling the molten alloy to enter a 10mm x 10mm columnar mold for suction casting molding, cooling the casting mold through room-temperature circulating water, and obtaining a cuboid ingot block material after 60-90 s of suction casting. And cutting the rectangular ingot into an alloy plate-shaped block material with the thickness of 2.5mm by using an electric spark wire.
(3) Solid solution homogenization treatment
Polishing the plate-shaped block material sand paper treated in the step (2) to remove a surface oxide layer, and then carrying out solid solution homogenization treatment in a vacuum tube furnace, wherein the vacuum degree is set to 10-4～10-3Pa, the temperature is 1100 ℃, and the treatment time is 0.5-2 h, so that the microcosmic components of the alloy are homogenized.
(4) Aging treatment
And (4) sealing the tube of the plate-shaped block material treated in the step (3) in an Ar gas environment, and performing aging treatment in a muffle furnace. The aging temperature is 300-375 ℃, the treatment time is 0.5-25 h, and then the water-cooling quenching treatment is carried out to the room temperature, so that enough nano-scale precipitates are precipitated in the alloy, and the aging-state coarse-grain alloy plate-shaped block is obtained.
(5) Electrochemical surface modification
And (4) carrying out surface finishing on the plate-shaped bulk material treated in the step (4) by an electrochemical polishing method. The polishing solution used in the electrochemical polishing method comprises a mixed solution of sulfuric acid and methanol in a volume ratio of 1:4, wherein the solution temperature is-20 ℃, and the voltage is 25-30V. Finally obtaining the coarse-grain Ti-Ni alloy plate-shaped block material with the thickness of 2-3 mm and without cold deformation.
Specific examples are given below to further illustrate the present invention.
Example 1:
the metal raw material is prepared according to the chemical composition (atom percentage) of 49.3 percent of Ti and 50.7 percent of Ni.
The preparation method comprises the following steps:
(1) alloy smelting: according to the chemical components of the mixture ratio, all metal raw materials are subjected to argon arc melting under the working current of a melting furnace, electromagnetic stirring with the current of 15A is carried out in the melting process, and single 1-minute melting and 5-time turnover are carried out on the cast ingot under the working current of 300A.
(2) Suction casting molding: heating the ingot obtained by smelting to be in a molten state through electric arc, stopping the electric arc, then carrying out vacuum suction casting, enabling the molten alloy to enter a 10mm x 10mm columnar mold for suction casting molding, cooling the casting mold through room-temperature circulating water, and obtaining a cuboid ingot block 75s after suction casting. And cutting the rectangular ingot into an alloy plate-shaped block material with the thickness of 2.5mm by using an electric spark wire.
(3) Solid solution homogenization treatment: polishing the plate-shaped block material obtained by linear cutting with abrasive paper to remove a surface oxide layer, and then carrying out solid solution homogenization treatment in a vacuum tube furnace, wherein the vacuum degree is set to 10-4Pa, the temperature is 1100 ℃, and the treatment time is 0.5 h. The microcosmic components of the alloy are homogenized.
(4) Aging treatment: and sealing the homogenized plate-shaped block material in an Ar gas environment, and performing aging treatment in a muffle furnace. The aging temperature is 325 ℃, the treatment time is 0.5h, and then the water-cooling quenching treatment is carried out to the room temperature.
(5) Electrochemical surface finishing: and (3) carrying out surface finishing on the homogenized plate-shaped bulk material by an electrochemical polishing method. The polishing solution used in the electrochemical polishing method comprises a mixed solution of sulfuric acid and methanol in a volume ratio of 1:4, wherein the solution temperature is-20 ℃, and the voltage is 25V.
Finally obtaining the high-elasticity thermal effect non-cold deformation coarse-grain Ti-Ni alloy plate-shaped block material with the block thickness of 2.5mm, wherein the measured refrigeration heat insulation temperature change is 19.3K.
Example 2:
the metal raw material is prepared according to the chemical composition (atom percentage) of 49.2 percent of Ti and 50.8 percent of Ni.
The preparation method comprises the following steps:
(1) alloy smelting: according to the chemical components of the mixture ratio, all metal raw materials are subjected to argon arc melting under the working current of a melting furnace, electromagnetic stirring with the current of 15A is carried out in the melting process, and the ingot is subjected to single 1min of melting and 5 times of turnover under the working current of 350A.
(2) Suction casting molding: heating the ingot obtained by smelting to be in a molten state through electric arc, stopping the electric arc, then carrying out vacuum suction casting, enabling the molten alloy to enter a 10mm x 10mm columnar mold for suction casting molding, cooling the casting mold through room-temperature circulating water, and obtaining a cuboid ingot block after 60s of suction casting. And cutting the rectangular ingot into an alloy plate-shaped block material with the thickness of 2.5mm by using an electric spark wire.
(3) Solid solution homogenization treatment: polishing the plate-shaped block material obtained by wire cutting with abrasive paper to remove a surface oxide layer, and then carrying out solid solution homogenization treatment in a vacuum tube furnace, wherein the vacuum degree is set to 5 x 10-4Pa, the temperature is 1100 ℃, and the treatment time is 0.5 h. The microcosmic components of the alloy are homogenized.
(4) Aging treatment: and sealing the homogenized plate-shaped block material in an Ar gas environment, and performing aging treatment in a muffle furnace. The aging temperature is 350 ℃, the treatment time is 15h, and then the water-cooling quenching treatment is carried out to the room temperature.
(5) Electrochemical surface finishing: and (3) carrying out surface finishing on the homogenized plate-shaped bulk material by an electrochemical polishing method. The polishing solution used in the electrochemical polishing method comprises a mixed solution of sulfuric acid and methanol in a volume ratio of 1:4, wherein the solution temperature is-20 ℃, and the voltage is 30V.
Finally obtaining the high-elasticity thermal effect non-cold deformation coarse-grain Ti-Ni alloy plate-shaped block material with the block thickness of 2.5mm, and measuring the refrigeration heat insulation temperature change to be 22.7K.
Example 3:
the metal raw material is prepared according to the chemical composition (atom percentage) of 48.8 percent of Ti and 51.2 percent of Ni.
The preparation method comprises the following steps:
(1) alloy smelting: according to the chemical components of the mixture ratio, all metal raw materials are subjected to argon arc melting under the working current of a melting furnace, electromagnetic stirring with the current of 15A is carried out in the melting process, and the ingot is subjected to single 1min of melting and 5 times of turnover under the working current of 450A.
(2) Suction casting molding: heating the ingot obtained by smelting to be in a molten state through electric arc, stopping the electric arc, then carrying out vacuum suction casting, enabling the molten alloy to enter a 10mm x 10mm columnar mold for suction casting molding, cooling the casting mold through room-temperature circulating water, and obtaining a cuboid ingot block 90s after suction casting. And cutting the rectangular ingot into an alloy plate-shaped block material with the thickness of 2.5mm by using an electric spark wire.
(3) Solid solution homogenization treatment: polishing the plate-shaped block material obtained by linear cutting with abrasive paper to remove a surface oxide layer, and then carrying out solid solution homogenization treatment in a vacuum tube furnace, wherein the vacuum degree is set to 10-3Pa, the temperature is 1100 ℃, and the treatment time is 2 h. The microcosmic components of the alloy are homogenized.
(4) Aging treatment: and sealing the homogenized plate-shaped block material in an Ar gas environment, and performing aging treatment in a muffle furnace. The aging temperature is 350 ℃, the treatment time is 25h, and then the water-cooling quenching treatment is carried out to the room temperature.
(5) Electrochemical surface finishing: and (3) carrying out surface finishing on the homogenized plate-shaped bulk material by an electrochemical polishing method. The polishing solution used in the electrochemical polishing method comprises a mixed solution of sulfuric acid and methanol in a volume ratio of 1:4, wherein the solution temperature is-20 ℃, and the voltage is 27.5V.
Finally obtaining the high-elasticity thermal effect non-cold deformation coarse-grain Ti-Ni alloy plate-shaped block material with the block thickness of 2.5mm, and measuring the refrigeration heat insulation temperature change to be 20.3K.
Example 4:
the metal raw material is prepared according to the chemical composition (atom percentage) of 49.0 percent of Ti and 51.0 percent of Ni.
The preparation method comprises the following steps:
(1) alloy smelting: according to the chemical components of the mixture ratio, all metal raw materials are subjected to argon arc melting under the working current of a melting furnace, electromagnetic stirring with the current of 15A is carried out in the melting process, and the ingot is subjected to single 1-minute melting and 5-time turn-over under the working current of 400A.
(2) Suction casting molding: heating the ingot obtained by smelting to be in a molten state through electric arc, stopping the electric arc, then carrying out vacuum suction casting, enabling the molten alloy to enter a 10mm x 10mm columnar mold for suction casting molding, cooling the casting mold through room-temperature circulating water, and obtaining a cuboid ingot block 90s after suction casting. And cutting the rectangular ingot into an alloy plate-shaped block material with the thickness of 2.5mm by using an electric spark wire.
(3) Solid solution homogenization treatment: polishing the plate-shaped block material obtained by linear cutting with abrasive paper to remove a surface oxide layer, and then carrying out solid solution homogenization treatment in a vacuum tube furnace, wherein the vacuum degree is set to 10-3Pa, 1100 ℃ and 1h of treatment time. The microcosmic components of the alloy are homogenized.
(4) Aging treatment: and sealing the homogenized plate-shaped block material in an Ar gas environment, and performing aging treatment in a muffle furnace. The aging temperature is 375 ℃, the treatment time is 1h, and then the water-cooling quenching treatment is carried out to the room temperature.
(5) Electrochemical surface finishing: and (3) carrying out surface finishing on the homogenized plate-shaped bulk material by an electrochemical polishing method. The polishing solution used in the electrochemical polishing method comprises a mixed solution of sulfuric acid and methanol in a volume ratio of 1:4, wherein the solution temperature is-20 ℃, and the voltage is 27.5V.
Finally obtaining the high-elasticity thermal effect non-cold deformation coarse-grain Ti-Ni alloy plate-shaped block material with the block thickness of 2.5mm, and measuring the refrigeration heat insulation temperature change to be 22.5K.
Example 5:
the metal material is prepared according to the chemical composition (atom percentage) of 49.2 percent of Ti and 50.8 percent of Ni (containing 0.5 percent of Cr).
The preparation method comprises the following steps:
(1) alloy smelting: according to the chemical components of the mixture ratio, all metal raw materials are subjected to argon arc melting under the working current of a melting furnace, electromagnetic stirring with the current of 15A is carried out in the melting process, and the ingot is subjected to single 1-minute melting and 5-time turn-over under the working current of 400A.
(2) Suction casting molding: heating the ingot obtained by smelting to be in a molten state through electric arc, stopping the electric arc, then carrying out vacuum suction casting, enabling the molten alloy to enter a 10mm x 10mm columnar mold for suction casting molding, cooling the casting mold through room-temperature circulating water, and obtaining a cuboid ingot block 75s after suction casting. And cutting the rectangular ingot into an alloy plate-shaped block material with the thickness of 2.5mm by using an electric spark wire.
(3) Solid solution homogenization treatment: polishing the plate-shaped block material obtained by linear cutting with abrasive paper to remove a surface oxide layer, and then carrying out solid solution homogenization treatment in a vacuum tube furnace, wherein the vacuum degree is set to 10-4Pa, the temperature is 1100 ℃, and the treatment time is 0.5 h. The microcosmic components of the alloy are homogenized.
(4) Aging treatment: and sealing the homogenized plate-shaped block material in an Ar gas environment, and performing aging treatment in a muffle furnace. The aging temperature is 300 ℃, the treatment time is 5h, and then the water-cooling quenching treatment is carried out to the room temperature.
(5) Electrochemical surface finishing: and (3) carrying out surface finishing on the homogenized plate-shaped bulk material by an electrochemical polishing method. The polishing solution used in the electrochemical polishing method comprises a mixed solution of sulfuric acid and methanol in a volume ratio of 1:4, wherein the solution temperature is-20 ℃, and the voltage is 27.5V.
Finally obtaining the high-elasticity thermal effect non-cold deformation coarse-grain Ti-Ni alloy plate-shaped block material with the block thickness of 2.5mm, and measuring the refrigeration heat insulation temperature change to be 21.6K.
The following table 1 shows the comparison of the thermal and elastic properties of the Ti — Ni alloy prepared by the method of the present invention with those of the prior art.
TABLE 1 comparison of Properties
As can be seen from the comparison of the elastic thermal effect of the shape memory alloy, the refrigeration heat insulation temperature change of the Ti-Ni alloy prepared by the method is not lower than 19K and can exceed 22K under specific conditions. Compared with the existing cold-processed wire material or block material alloy, the alloy prepared by the method does not need to be subjected to cold deformation machining process with high processing difficulty and time consumption, and has similar elastic and thermal properties; compared with the existing non-cold-deformation block alloy, the elastic thermal property is improved by 106%, and the improvement on the elastic thermal property of the non-cold-deformation Ti-Ni alloy is significant. Therefore, the application prospect is wide.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (9)
1. A preparation method of a non-cold-deformation high-elasticity thermal effect Ti-Ni bulk material is characterized by comprising the following steps:
1) argon arc melting is carried out on the raw materials of 48.8-49.3% of Ti and 50.7-51.2% of Ni according to the atomic ratio under the working current of a melting furnace, electromagnetic stirring is carried out, and ingot casting is carried out turnover melting for multiple times to obtain a Ti-Ni ingot casting block material bottom material;
2) arc heating the Ti-Ni ingot casting block material backing material to a molten state, carrying out vacuum suction casting to obtain a formed ingot casting block material, and cutting the formed ingot casting block material into an alloy plate-shaped block material;
3) polishing a surface oxide layer of a plate-shaped block material, and carrying out solid solution homogenization treatment under a vacuum condition;
4) sealing the homogenized plate-shaped block material in an Ar gas environment, performing aging treatment, and performing water-cooling quenching treatment to room temperature to obtain an aged coarse-grained alloy plate-shaped block material;
5) and (3) carrying out electrochemical polishing on the coarse-grained plate-shaped block material to obtain the coarse-grained Ti-Ni alloy plate-shaped block material with millimeter-scale thickness and without cold deformation.
2. The method for preparing the non-cold-deformation high-elastic thermal effect Ti-Ni bulk material as claimed in claim 1, wherein in the step 1), the raw material 50.7-51.2% of Ni is further doped with Cr element with atomic ratio not more than 0.5%.
3. The preparation method of the non-cold-deformation high-elasticity thermal effect Ti-Ni bulk material as claimed in claim 1, wherein in the step 1), the ingot is subjected to single melting for 1min and 5 times of turnover at a working current of 300-450A; the melting electromagnetic stirring current is 15A.
4. The preparation method of the non-cold-deformation high-elasticity thermal effect Ti-Ni bulk material as claimed in claim 1, wherein in the step 2), the casting mold is cooled by room-temperature circulating water, and the casting mold is opened 60-90 s after vacuum suction casting.
5. The method for preparing the non-cold-deformation high-elastic thermal effect Ti-Ni bulk material as claimed in claim 1, wherein in the step 3), the vacuum degree of the solution homogenization treatment is 10-4～10-3Pa, the temperature is 1100 ℃, and the treatment time is 0.5-2 h.
6. The method for preparing the non-cold-deformation high-elastic thermal effect Ti-Ni bulk material as claimed in claim 1, wherein in the step 4), the aging treatment is performed at 300-375 ℃ for 0.5-25 h.
7. The method for preparing the non-cold-deformation high-elastic thermal effect Ti-Ni bulk material as claimed in claim 1, wherein in the step 5), the electrochemical polishing method comprises the following steps: the polishing method is characterized in that a polishing solution is a mixed solution of sulfuric acid and methanol with a volume ratio of 1:4, the temperature of the solution is-20 ℃, and the polishing is carried out under a voltage of 25-30V.
8. A non-cold-deformation high-elastic thermal effect Ti-Ni bulk material prepared by the method of any one of claims 1 to 7, which is characterized by comprising the following raw materials:
the elements are 48.8-49.3% Ti and 50.7-51.2% Ni according to atomic ratio.
9. The non-cold-deformation high-elastic thermal effect Ti-Ni bulk material as claimed in claim 8, wherein the Ni element is further doped with Cr with an atomic ratio of 0.5% or less.
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| CN116287933A (en) * | 2023-03-29 | 2023-06-23 | 哈尔滨理工大学 | Ni-Mn-Sn-Ti shape memory alloy with high elastic and thermal properties and preparation method thereof |
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