CN111378868A - Preparation method of high-tin-content high-density copper-tin alloy - Google Patents
Preparation method of high-tin-content high-density copper-tin alloy Download PDFInfo
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- CN111378868A CN111378868A CN202010326791.2A CN202010326791A CN111378868A CN 111378868 A CN111378868 A CN 111378868A CN 202010326791 A CN202010326791 A CN 202010326791A CN 111378868 A CN111378868 A CN 111378868A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
- C22C9/02—Alloys based on copper with tin as the next major constituent
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0425—Copper-based alloys
Abstract
The invention discloses a preparation method of a high-tin-content high-density copper-tin alloy, which comprises the following steps: step 1: weighing 83.2-84.3 wt.% of Cu powder, 15.4-16.5 wt.% of Sn powder and 0.3 wt.% of Ti powder according to mass percent, and uniformly mixing the components by using a ball mill to obtain mixed powder; step 2: cold pressing the mixed powder obtained in the step 1 to obtain a cold pressed blank, and putting the cold pressed blank into an atomization deposition furnace for atomization deposition to obtain pre-alloy powder; and step 3: and (3) screening the pre-alloyed powder in the step (2), carrying out secondary cold pressing to obtain a secondary cold pressed blank, then placing the secondary cold pressed blank into an atmosphere sintering furnace, introducing inert gas, heating and pressurizing the atmosphere sintering furnace, keeping the temperature for a period of time, and then cooling and depressurizing the atmosphere sintering furnace to obtain the copper-tin alloy. The invention improves the content of tin in the copper-tin alloy, and the tin is distributed more uniformly, thereby ensuring the density and hardness of the copper-tin alloy.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a preparation method of a high-tin-content high-density copper-tin alloy.
Background
At present, the preparation of the copper-tin alloy for superconduction is mostly realized by a casting method, but a serious anti-segregation phenomenon is easy to occur in the cooling process of an ingot, the solute tin in a liquid phase can flow back to the surface of a casting, and a silvery white tin simple substance appears after the complete solidification, so that the tin content in a copper-tin alloy matrix is greatly reduced and the tin content is not uniformly distributed, and the preparation of Nb by adopting a bronze method is further influenced3Critical current density of the Sn superconducting wire.
In order to solve the problem of insufficient tin content, the copper-tin alloy is prepared by using Cu powder, Sn powder and Ti powder in a certain proportion at the early stage through a powder metallurgy method. In the process of powder metallurgy, because the melting points of copper and tin are greatly different, tin powder is firstly converted into liquid to be diffused into copper, but the solubility of copper to tin is low, when the tin content is high, one part of liquid-phase tin which is not dissolved into copper can react with a copper simple substance to generate various intermetallic compounds uncontrollably, and the other part of liquid-phase tin can be recovered into simple substance tin along with the reduction of temperature and exists in the copper-tin alloy. The copper-tin alloy prepared by the method has various existence modes of tin, complex structure and serious segregation. More intermetallic compounds lead to poor formability of the copper-tin alloy, which is not conducive to drawing. The more complex structure will result in Nb being produced3Sn superconducting wires are not sufficiently uniform. The copper-tin alloy prepared by the traditional powder metallurgy method has low hardness and a large number of tiny holes in the copper-tin alloy, and if a niobium rod contacts with the holes during assembly, the reaction of the parts contacting with the holes is insufficient in the process of generating the superconducting wire, so that the produced superconducting wire has poor uniformity.
Disclosure of Invention
The invention aims to provide a preparation method of a high-tin-content high-density copper-tin alloy, which solves the problems that the preparation method in the existing preparation method of the copper-tin alloy needs to be further optimized and the prepared copper-tin alloy has lower hardness.
The technical scheme adopted by the invention is that,
a preparation method of a high-tin-content high-density copper-tin alloy specifically comprises the following steps:
step 1: weighing 83.2-84.3 wt.% of Cu powder, 15.4-16.5 wt.% of Sn powder and 0.3 wt.% of Ti powder according to mass percent, and uniformly mixing the components by using a ball mill to obtain mixed powder;
step 2: cold pressing the mixed powder obtained in the step 1 to obtain a cold pressed blank, and putting the cold pressed blank into an atomization deposition furnace for atomization deposition to obtain pre-alloy powder;
and step 3: and (3) screening the pre-alloyed powder in the step (2) to obtain powder, adding alcohol into the powder, stirring, performing secondary cold pressing to obtain a secondary cold pressed blank, putting the secondary cold pressed blank into an atmosphere sintering furnace, introducing inert gas, heating the atmosphere sintering furnace to 540-570 ℃, starting to pressurize the cold pressed blank, keeping the pressure and the temperature for 45-60 min when the temperature of the atmosphere sintering furnace is increased to 640-660 ℃ and the pressure of the cold pressed blank reaches 20-30 MPa, then cooling the atmosphere sintering furnace to 400-450 ℃, and depressurizing to obtain the copper-tin alloy.
The present invention is also characterized in that,
in step 1, the ball mill is mixed with the following control parameters: the rotating speed of the ball mill is controlled to be 100-200 r/min, the forward and reverse rotation time is controlled to be 5-15 min, and the powder mixing time is controlled to be 3-5 h.
In the step 2, the cold pressing specifically comprises the following steps: and pouring the mixed powder into a pressing mold, and pressing into a cold pressed blank by using a cold press.
In the step 2, the atomization deposition specifically comprises: and vacuumizing the atomization deposition furnace, introducing argon gas of 0.01-0.02 MPa, raising the temperature of the furnace to 1200-1280 ℃, and continuously introducing nitrogen gas for atomization deposition after the cold pressed blank is melted to obtain the pre-alloy powder.
In the step 3, the inert gas is nitrogen, and the ventilation time is controlled to be 45-60 min.
In the step 3, the heating speed is controlled to be 5 ℃/min, and the pressurizing speed is controlled to be 1.00-1.5 MPa/min.
And 3, finishing the pressurization of the cold pressed compact and the heating of the sintering furnace at the same time.
The preparation method of the high-tin-content high-density copper-tin alloy has the beneficial effects that the preparation of the copper-tin alloy is carried out by adopting a powder metallurgy method, and the problems of insufficient tin content and uneven distribution in the copper-tin alloy caused by a casting method are solved. The method for performing supersolidus phase line sintering by using the prealloy powder abandons the method of directly using mixed powder of Cu, Sn and Ti to perform liquid-solid sintering, avoids complex tissues in the copper-tin alloy, makes the tissues uniform, effectively reduces precipitated phases and makes the precipitated phases in a dispersion rule. Before the prealloyed powder is poured into a pressing die, a proper amount of alcohol is added for stirring, so that the powder is easier to form. Before sintering, nitrogen is used for exhausting other gases in the furnace body, and the nitrogen is continuously introduced into the furnace body for protection in the sintering process, so that the pre-alloyed powder is prevented from reacting with oxygen or other gases in the sintering process to generate impurities. And continuously and slowly pressurizing in the heating process, raising the pressure to a target value when the heating process is just finished, and continuously maintaining the pressure before cooling to 400-450 ℃, so that the density of the copper-tin alloy is ensured.
Drawings
FIG. 1 is a microstructure diagram of a copper-tin alloy in examples 1 to 4 of a method for producing a high-tin-content high-density copper-tin alloy according to the present invention;
FIG. 2 is a graph showing the density curves of the copper-tin alloys in examples 1 to 4 in the method for preparing a high-tin-content high-density copper-tin alloy according to the present invention;
FIG. 3 is a hardness curve diagram of the copper-tin alloy in examples 1-4 in the preparation method of the high tin content high density copper-tin alloy of the present invention.
Detailed Description
The following describes a method for preparing a high-tin-content high-density copper-tin alloy in detail with reference to the accompanying drawings and specific embodiments.
A preparation method of a high-tin-content high-density copper-tin alloy specifically comprises the following steps:
step 1: weighing 83.2-84.3 wt.% of Cu powder, 15.4-16.5 wt.% of Sn powder and 0.3 wt.% of Ti powder according to mass percent, and uniformly mixing the components by using a ball mill to obtain mixed powder;
step 2: cold pressing the mixed powder obtained in the step 1 to obtain a cold pressed blank, and putting the cold pressed blank into an atomization deposition furnace for atomization deposition to obtain pre-alloy powder;
and step 3: and (3) screening the pre-alloyed powder in the step (2) to obtain powder, adding alcohol into the powder, stirring, performing secondary cold pressing to obtain a secondary cold pressed blank, putting the secondary cold pressed blank into an atmosphere sintering furnace, introducing inert gas, heating the atmosphere sintering furnace to 540-570 ℃, starting to pressurize the cold pressed blank, maintaining the pressure and preserving the temperature for 45-60 min when the temperature of the atmosphere sintering furnace is increased to 640-660 ℃ and the pressure of the cold pressed blank is increased to 20-30 MPa, then cooling the atmosphere sintering furnace to 400-450 ℃, and depressurizing to obtain the copper-tin alloy.
Further, in step 1, the ball mill is mixed with the following control parameters: the rotating speed of the ball mill is controlled to be 100-200 r/min, the forward and reverse rotation time is controlled to be 5-15 min, and the powder mixing time is controlled to be 3-5 h.
Further, in step 2, the cold pressing specifically comprises: and pouring the mixed powder into a pressing mold, and pressing into a cold pressed blank by using a cold press.
Further, in step 2, the atomization deposition specifically comprises: and vacuumizing the atomization deposition furnace, introducing argon gas of 0.01-0.02 MPa, raising the temperature of the furnace to 1200-1280 ℃, and continuously introducing nitrogen gas for atomization deposition after the cold pressed blank is melted to obtain the pre-alloy powder.
Further, in the step 3, the inert gas is nitrogen, and the ventilation time is controlled to be 45-60 min.
Further, in the step 3, the heating speed is controlled to be 5 ℃/min, and the pressurizing speed is controlled to be 1.00-1.5 MPa/min.
Further, in step 3, the pressurization of the cold compact and the heating of the sintering furnace are simultaneously completed.
The preparation method of the high-tin-content high-density copper-tin alloy of the invention is further explained in detail by the following specific examples.
Example 1
Weighing 83.7% of Cu powder, 16% of Sn powder and 0.3% of Ti powder, uniformly mixing the Cu powder, the Sn powder and the Ti powder by using a planetary ball mill, wherein the rotating speed of the ball mill is 100r/min, the forward and reverse rotation time is 5min, the powder mixing time is 3h, and after the powder mixing is finished, pouring the powder into a pressing dieIn the method, a cold press is used for pressing the mixture into a cold pressed blank. Finally, the cold pressing blank is put into an atomization deposition furnace, and the furnace body is vacuumized to 10 degrees-3And (3) introducing argon gas of 0.01MPa after Pa, heating the furnace to 1200 ℃, opening a nitrogen valve when the cold-pressed blank is completely melted, adjusting the index to 4.5MPa, and continuously introducing nitrogen gas for atomization and deposition to obtain prealloy powder.
Sieving the obtained alloy powder, vibrating for 2min, selecting powder with particle size of 75 μm, adding appropriate amount of alcohol into the powder, stirring, pouring into a pressing mold, and pressing on a cold press to obtain cold pressed compact.
Laying two layers of graphite paper at the bottom of a graphite crucible, putting the graphite crucible into a cold pressed blank, then covering the graphite crucible with the two layers of graphite paper, and putting the graphite crucible into an atmosphere sintering furnace after covering the graphite crucible with a cover. And opening a nitrogen valve, and introducing nitrogen into the furnace body so as to completely exhaust other gases in the furnace body, wherein the introducing time is 45 min. And after other gases are exhausted, continuously introducing nitrogen, starting heating, wherein the heating speed is 5 ℃/min, pressurizing the cold-pressed blank when the temperature rises to 540 ℃, the pressurizing speed is 1.00MPa/min, the pressurizing process is just finished when the heating process is finished, and when the pressure reaches 20MPa, the temperature in the furnace rises to 640 ℃, the heat preservation and pressure maintaining are started, and the heat preservation time is 45 min. The pressure is always maintained at 20MPa in the heat preservation process. After the heat preservation time is over, the temperature is reduced, the pressure can be slowly removed until the temperature is reduced to 400 ℃, the copper-tin alloy is obtained, and the result detection shows that the hardness of the copper-tin alloy is 109HB, and the density of the copper-tin alloy is 8.88g/cm3。
Example 2
Weighing 83.5% of Cu powder, 16.2% of Sn powder and 0.3% of Ti powder, uniformly mixing the Cu powder, the Sn powder and the Ti powder by using a planetary ball mill, wherein the rotating speed of the ball mill is 200r/min, the forward and reverse rotation time is 15min, and the powder mixing time is 5h, pouring the powder into a compacting die after the powder mixing is finished, and compacting into a cold compact by using a cold press. Finally, the cold pressing blank is put into an atomization deposition furnace, and the furnace body is vacuumized to 10 degrees-4Introducing argon gas of 0.02MPa after Pa, heating the furnace to 1280 ℃, opening a nitrogen valve when the cold pressed blank is completely melted, adjusting the indication to 5.5MPa, and continuously introducing nitrogen gas for atomization and deposition to obtain the pre-sintered compactAnd (3) alloying powder.
Sieving the obtained alloy powder, vibrating for 2min, selecting powder with particle size of 90 μm, adding appropriate amount of alcohol into the powder, stirring, pouring into a pressing mold, and pressing on a cold press to obtain cold pressed compact.
Laying two layers of graphite paper at the bottom of a graphite crucible, putting the graphite crucible into a cold pressed blank, then covering the graphite crucible with the two layers of graphite paper, and putting the graphite crucible into an atmosphere sintering furnace after covering the graphite crucible with a cover. And opening a nitrogen valve, and introducing nitrogen into the furnace body so as to completely exhaust other gases in the furnace body, wherein the introducing time is 60 min. And after other gases are exhausted, continuously introducing nitrogen, starting heating at the temperature rising speed of 5 ℃/min, starting pressurizing the cold-pressed blank when the temperature rises to 570 ℃, wherein the pressurizing speed is 1.00MPa/min, the pressurizing process is just finished when the heating process is finished, and when the pressure reaches 30MPa, the temperature in the furnace rises to 660 ℃, the heat preservation and pressure maintaining are started, and the heat preservation time is 60 min. The pressure is always maintained at 30MPa in the heat preservation process. After the heat preservation time is over, the temperature is reduced, the pressure can be slowly removed until the temperature is reduced to 450 ℃, so that the copper-tin alloy is obtained, and the result detection shows that the hardness of the copper-tin alloy is 114HB, and the density of the copper-tin alloy is 8.92g/cm3。
Example 3
Weighing 84.3% of Cu powder, 15.8% of Sn powder and 0.3% of Ti powder, uniformly mixing the Cu powder, the Sn powder and the Ti powder by using a planetary ball mill, wherein the rotating speed of the ball mill is 200r/min, the forward and reverse rotation time is 10min, and the powder mixing time is 4h, pouring the powder into a compacting die after the powder mixing is finished, and compacting into a cold compact by using a cold press. Finally, the cold pressing blank is put into an atomization deposition furnace, and the furnace body is vacuumized to 10 degrees-4And (3) introducing argon gas of 0.015MPa after Pa, heating the furnace to 1240 ℃, opening a nitrogen valve when the cold-pressed blank is completely melted, adjusting the indication to 5.0MPa, and continuously introducing nitrogen gas for atomization and deposition to obtain the prealloy powder.
Sieving the obtained alloy powder, vibrating for 2min, selecting powder with particle size of 80 μm, adding appropriate amount of alcohol into the powder, stirring, pouring into a pressing mold, and pressing on a cold press to obtain cold pressed compact.
In a graphite crucibleTwo layers of graphite paper are laid at the bottom of the furnace, then a cold pressed blank is placed, then two layers of graphite paper are covered, and then the furnace is placed in an atmosphere sintering furnace after the cover is covered. And opening a nitrogen valve, and introducing nitrogen into the furnace body so as to completely exhaust other gases in the furnace body, wherein the introducing time is 50 min. And after other gases are exhausted, continuously introducing nitrogen, starting heating, wherein the heating speed is 5 ℃/min, pressurizing the cold-pressed blank when the temperature rises to 570 ℃, the pressurizing speed is 1.25MPa/min, the pressurizing process is just finished when the heating process is finished, and when the pressure reaches 25MPa, the temperature in the furnace rises to 650 ℃, the heat preservation and pressure maintaining are started, and the heat preservation time is 50 min. The pressure is always kept at 25MPa in the heat preservation process. After the heat preservation time is over, the temperature is reduced, the pressure can be slowly removed until the temperature is reduced to 430 ℃, the copper-tin alloy is obtained, and the result detection shows that the hardness of the copper-tin alloy is 115HB, and the density is 8.93g/cm3。
Example 4
Weighing 84.1% of Cu powder, 15.6% of Sn powder and 0.3% of Ti powder, uniformly mixing the Cu powder, the Sn powder and the Ti powder by using a planetary ball mill, wherein the rotating speed of the ball mill is 130r/min, the forward and reverse rotation time is 12min, and the powder mixing time is 5h, pouring the powder into a compacting die after the powder mixing is finished, and compacting into a cold compact by using a cold press. Finally, the cold pressing blank is put into an atomization deposition furnace, and the furnace body is vacuumized to 10 degrees-3And (3) introducing argon gas of 0.02MPa after Pa, heating the furnace to 1280 ℃, opening a nitrogen valve when the cold-pressed blank is completely melted, adjusting the indication to 5.5MPa, and continuously introducing nitrogen gas for atomization and deposition to obtain the prealloy powder.
Sieving the obtained alloy powder, vibrating for 2min, selecting powder with particle size of 80 μm, adding appropriate amount of alcohol into the powder, stirring, pouring into a pressing mold, and pressing on a cold press to obtain cold pressed compact.
Laying two layers of graphite paper at the bottom of a graphite crucible, putting the graphite crucible into a cold pressed blank, then covering the graphite crucible with the two layers of graphite paper, and putting the graphite crucible into an atmosphere sintering furnace after covering the graphite crucible with a cover. And opening a nitrogen valve, and introducing nitrogen into the furnace body so as to exhaust other gases in the furnace body completely, wherein the introducing time is 55 min. After other gases are exhausted, nitrogen is continuously introduced, heating is started, and the temperature rising speed is acceleratedThe temperature is 5 ℃/min, the cold pressing blank is pressurized when the temperature rises to 555 ℃, the pressurizing speed is 1.00MPa/min, the pressurizing process is just finished when the heating process is finished, the temperature in the furnace is raised to 660 ℃ when the pressure reaches 30MPa, the heat preservation and pressure maintaining are started, and the heat preservation time is 60 min. The pressure is always maintained at 30MPa in the heat preservation process. After the heat preservation time is over, the temperature is reduced, the pressure can be slowly removed until the temperature is reduced to 450 ℃, so that the copper-tin alloy is obtained, and the result detection shows that the hardness of the copper-tin alloy is 110HB, and the density of the copper-tin alloy is 8.89g/cm3。
The invention adopts a powder metallurgy method to prepare the copper-tin alloy, and as shown in figure 1, the copper-tin alloy prepared by the invention has simple and uniform structure, less precipitated phase and dispersion distribution.
As shown in fig. 2, by comparing the density curves, it can be seen that the alloy density of the copper-tin alloy prepared by the present invention is higher than that of the copper-tin alloy prepared by the conventional powder metallurgy method with the same tin content.
As shown in fig. 3, by comparing the hardness curves, it can be seen that the hardness of the copper-tin alloy prepared by the present invention is higher than that of the copper-tin alloy prepared by the conventional powder metallurgy method with the same tin content.
The preparation method of the high-tin-content high-density copper-tin alloy solves the problems of insufficient tin content and uneven distribution in the copper-tin alloy caused by a casting method. The density and the hardness of the copper-tin alloy are ensured.
Claims (7)
1. The preparation method of the high-tin-content high-density copper-tin alloy is characterized by comprising the following steps of:
step 1: weighing 83.2-84.3 wt.% of Cu powder, 15.4-16.5 wt.% of Sn powder and 0.3 wt.% of Ti powder according to mass percent, and uniformly mixing the components by using a ball mill to obtain mixed powder;
step 2: carrying out cold pressing on the mixed powder in the step 1 to obtain a cold pressed blank, and carrying out atomization deposition on the cold pressed blank in an atomization deposition furnace to obtain pre-alloy powder;
and step 3: and (3) screening the pre-alloyed powder in the step (2) to obtain powder, adding alcohol into the powder, stirring, performing secondary cold pressing to obtain a secondary cold pressed blank, putting the secondary cold pressed blank into an atmosphere sintering furnace, introducing inert gas, heating the atmosphere sintering furnace to 540-570 ℃, starting to pressurize the cold pressed blank, keeping the pressure and the temperature for 45-60 min when the temperature of the atmosphere sintering furnace is increased to 640-660 ℃ and the pressure of the cold pressed blank reaches 20-30 MPa, then cooling the atmosphere sintering furnace to 400-450 ℃, and depressurizing to obtain the copper-tin alloy.
2. The method for preparing the high-tin-content high-density copper-tin alloy according to claim 1, wherein in the step 1, the ball mill is mixed with the following control parameters: the rotating speed of the ball mill is controlled to be 100-200 r/min, the forward and reverse rotation time is controlled to be 5-15 min, and the powder mixing time is controlled to be 3-5 h.
3. The preparation method of the high-tin-content high-density copper-tin alloy according to claim 1, wherein in the step 2, the cold pressing specifically comprises the following steps: and pouring the mixed powder into a pressing mold, and pressing into a cold pressed blank by using a cold press.
4. The method for preparing the high-tin-content high-density copper-tin alloy according to claim 1, wherein in the step 2, the atomization deposition is specifically as follows: and vacuumizing the atomization deposition furnace, introducing argon gas of 0.01-0.02 MPa, raising the temperature of the furnace to 1200-1280 ℃, and continuously introducing nitrogen gas for atomization deposition after the cold pressed blank is melted to obtain the pre-alloy powder.
5. The method for preparing the high-tin-content high-density copper-tin alloy as claimed in claim 1, wherein in the step 3, the inert gas is nitrogen, and the aeration time is controlled to be 45-60 min.
6. The method for preparing the high-tin-content high-density copper-tin alloy as claimed in claim 1, wherein in the step 3, the heating speed is controlled to be 5 ℃/min, and the pressurizing speed is controlled to be 1.00-1.5 MPa/min.
7. The method for preparing a high tin content high density copper-tin alloy as claimed in claim 6, wherein in step 3, the pressurizing of the cold compact and the heating of the sintering furnace are simultaneously finished.
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| CN113278824A (en) * | 2021-04-29 | 2021-08-20 | 西安理工大学 | Preparation method of Cu-Sn-Ti alloy with high tin content and high plasticity |
| CN115233026A (en) * | 2022-05-30 | 2022-10-25 | 广东华诺勤耕材料科技有限公司 | Preparation method of copper-tin alloy |
| CN115449660A (en) * | 2022-08-31 | 2022-12-09 | 西安理工大学 | Preparation method of ultrahigh Sn content high-density low-segregation copper-tin alloy |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113134615A (en) * | 2021-03-17 | 2021-07-20 | 西安理工大学 | Method for preparing antifriction and wear-resistant BN/CuSn10 powder by atomizing and pulverizing plasma rotating electrode |
| CN113278824A (en) * | 2021-04-29 | 2021-08-20 | 西安理工大学 | Preparation method of Cu-Sn-Ti alloy with high tin content and high plasticity |
| CN113278824B (en) * | 2021-04-29 | 2021-12-17 | 西安理工大学 | Preparation method of Cu-Sn-Ti alloy with high tin content and high plasticity |
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| CN115449660A (en) * | 2022-08-31 | 2022-12-09 | 西安理工大学 | Preparation method of ultrahigh Sn content high-density low-segregation copper-tin alloy |
| CN115449660B (en) * | 2022-08-31 | 2023-04-07 | 西安理工大学 | Preparation method of ultrahigh Sn content high-density low-segregation copper-tin alloy |
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