CN115369272A - Preparation method of suspension smelting high-melting-point Cr2Nb intermetallic compound - Google Patents
Preparation method of suspension smelting high-melting-point Cr2Nb intermetallic compound Download PDFInfo
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Abstract
The invention discloses a preparation method of a Cr2Nb intermetallic compound with high melting point by suspension smelting, wherein the Cr element accounts for 52.0-56.0 percent and the Nb element accounts for 44.0-48.0 percent of the components of the Cr2Nb intermetallic compound by mass percent, and the preparation method comprises the following steps: s1, weighing Cr blocks and Nb blocks according to the mass percentage for later use; s2, placing the weighed Cr blocks into a crucible, then placing the crucible filled with the Cr blocks into a smelting furnace, and placing the weighed Nb blocks into an alloy box of the smelting furnace; s3, vacuumizing the smelting furnace; s4, filling protective gas nitrogen into the smelting furnace, and starting the smelting furnace to smelt the raw materials; s5, after the Cr and Nb raw materials in the smelting furnace in the step S4 are smelted, closing the smelting furnace to stop smelting; compared with the traditional mechanical grinding method, the preparation method of the Cr2Nb intermetallic compound shortens the preparation process and solves the problems that Nb is easy to oxidize, impurities are brought in, complete alloying cannot be realized and the like in the preparation process.
Description
Technical Field
The invention relates to the technical field of intermetallic compound preparation, in particular to a preparation method of a suspension smelting high-melting-point Cr2Nb intermetallic compound.
Background
In recent years, cuCrNb alloy has become a feasible substitute for high-conductivity materials such as Cu-Cr, cu-Ag-Zr and the like. A large amount of fine Cr2Nb precipitates are dispersed in the alloy matrix, so that the alloy can still maintain good mechanical properties after being exposed in a temperature range of up to 700 ℃ for a long time. These fine precipitates are very stable and pin the grain boundaries, preventing coarsening and grain boundary sliding during creep.
The high melting point intermetallic compound Cr2Nb is very stable and does not significantly coarsen upon prolonged exposure to temperatures in the range up to 700 c, thereby strengthening this type of copper-based alloy. However, since the alloying elements Cu (1083 ℃), cr (1863 ℃) and Nb (2469 ℃) have large differences in melting points, and Cu-Cr or Cu-Nb have no low-melting eutectic formation, the preparation of the main alloy is difficult. The problem of preparing the copper alloy of the type can be effectively solved by preparing the Cr2Nb intermediate alloy. The current mainstream preparation method is a mechanical grinding method, the main flow of the method is Cr powder + Nb powder-mixed powder-mechanical grinding-hot-pressing sintering-annealing, the preparation process is complicated, nb is easily oxidized to form NbO2 in the mechanical grinding process, and the Nb cannot be completely converted into Cr2Nb when the hot-pressing sintering temperature or pressure or the annealing temperature is insufficient.
The vacuum induction suspension smelting generates an alternating electromagnetic field through an electromagnetic coil, the alternating electromagnetic field induces current in metal in the coil, and the induced current heats and melts the metal; the smelting temperature is high and can exceed 3000 ℃; is suitable for preparing refractory metals and alloys with high melting points, such as Cr, nb, mo, ta and other refractory metals and alloys.
Disclosure of Invention
The invention aims to provide a preparation method of a high-melting-point Cr2Nb intermetallic compound by suspension smelting, which is used for preparing Cr2Nb by a vacuum induction suspension smelting method, avoids the oxidation of raw materials and the introduction of impurities, can obtain the Cr2Nb intermetallic compound with high alloying and uniform structure, and greatly shortens the preparation process.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a Cr2Nb intermetallic compound with high melting point by suspension smelting comprises the following steps of, by mass percent, 52.0% -56.0% of Cr element and 44.0% -48.0% of Nb element:
s1, preparing raw materials:
weighing Cr blocks and Nb blocks according to the mass percentage for later use;
s2, charging:
putting the weighed Cr blocks into a crucible, then putting the crucible filled with the Cr blocks into a smelting furnace, and putting the weighed Nb blocks into an alloy box of the smelting furnace;
s3, vacuumizing:
sequentially utilizing a mechanical pump and a roots pump to vacuumize the smelting furnace in the step S2, and when the vacuum degree in the smelting furnace is less than 10Pa, utilizing a diffusion pump to continuously vacuumize the smelting furnace;
s4, smelting:
filling protective gas nitrogen into a smelting furnace, starting the smelting furnace when the pressure in the smelting furnace reaches 0.02-0.03 MPa, gradually increasing the smelting power of the smelting furnace at the rate of 10-15 kW/min to smelt the raw material, and controlling the maximum smelting power of the smelting furnace at 270-330 kW;
s5, cooling:
after the Cr and Nb raw materials in the smelting furnace in the step S4 are smelted, closing the smelting furnace to stop smelting, and naturally cooling the smelted alloy in the crucible to room temperature;
preferably, the purity of the Cr blocks and the Nb blocks in the step S1 needs to be more than 99.95%, the sizes of the single Cr blocks and Nb blocks are controlled to be less than 20mm, and the surfaces of the Cr blocks and the Nb blocks are ensured to be clean and free of impurities during batching.
Description of the invention: the sizes of the Cr blocks and the Nb blocks are controlled to be smaller than 20mm, so that the Cr blocks and the Nb blocks can be smelted at a more proper smelting speed during smelting, and the quality of the finally obtained alloy is improved.
Preferably, during charging in the step S2, cr blocks are charged into a copper crucible having a water cooling function.
Preferably, in the step S3, when the vacuum pumping in the smelting furnace is continued by using the diffusion pump, the vacuum degree in the smelting furnace needs to reach 0.5 × 10 -3 Pa～1×10 -3 Pa。
Description of the drawings: the less impurities in the air in the smelting furnace, the less negative the negative impact on the smelted alloy.
Preferably, the smelting process in the step S4 is that a smelting furnace is started to smelt the Cr blocks in the crucible, the Cr blocks are refined for 3-5 min after being completely melted, then the Nb blocks in the alloy box are added into the crucible to be smelted together with Cr and stirred for 1-2 min, the smelting power is gradually increased at a rate of 10-15 kW/min during smelting, the maximum smelting power is controlled at 270-330 kW, and finally the Nb blocks are refined for 5-10 min after being completely melted.
Description of the invention: the smelting step can ensure that Cr and Nb are more fully and uniformly mixed.
Preferably, after the raw materials are completely alloyed in the step S4, the smelting furnace stops heating, the crucible filled with the alloy ingot is cooled in the smelting furnace for 30-60 min, the alloy ingot in the crucible is turned over, then the heating function of the smelting furnace is started again to continue smelting the alloy ingot in the crucible, and the step of cooling and then smelting is repeated for 3-4 times.
Description of the drawings: the step of cooling and then smelting is repeated for 3 to 4 times, so as to ensure that the alloy components are more uniform.
Preferably, the specific cooling mode in step S5 is that after the Cr block and the Nb block in the smelting furnace are smelted, the heating function of the smelting furnace is firstly turned off, so that the alloy obtained after smelting is naturally cooled in the smelting furnace for 60-90 min, then the smelting furnace is broken to be vacuum, and then the alloy ingot after smelting is taken out.
Compared with the prior art, the invention has the beneficial effects that: firstly, compared with the traditional mechanical grinding method, the preparation method of the Cr2Nb intermetallic compound shortens the preparation process and solves the problems that Nb is easy to oxidize, impurities are brought in, complete alloying cannot be realized and the like in the preparation process; and secondly, the preparation method of the Cr2Nb intermetallic compound has high preparation efficiency and success rate, and can effectively solve the preparation problem of CuCrNb and other Cr2Nb phase-containing alloys.
Drawings
FIG. 1 a Cr2Nb alloy ingot produced by the present invention;
FIG. 2 is a scan of Cr2Nb prepared in accordance with the present invention;
FIG. 3 is a XRD pattern of Cr2Nb prepared in accordance with the present invention;
FIG. 4 is a gold phase diagram of a CuCrNb alloy prepared by using Cr2Nb prepared by the invention.
Detailed Description
The present invention will be described in detail with reference to fig. 1 to 4.
Example 1:
a preparation method of a Cr2Nb intermetallic compound with high melting point by suspension smelting comprises the following steps of:
s1, preparing raw materials:
weighing Cr blocks and Nb blocks according to the mass percentage for later use;
s2, charging:
putting the weighed Cr blocks into a crucible, then putting the crucible filled with the Cr blocks into a smelting furnace, and putting the weighed Nb blocks into an alloy bin of the smelting furnace;
s3, vacuumizing:
sequentially utilizing a mechanical pump and a roots pump to vacuumize the smelting furnace in the step S2, and when the vacuum degree in the smelting furnace is less than 10Pa, utilizing a diffusion pump to continuously vacuumize the smelting furnace;
s4, smelting:
filling protective gas nitrogen into a smelting furnace, starting the smelting furnace when the pressure in the smelting furnace reaches 0.025MPa, gradually increasing the smelting power of the smelting furnace at a speed of 12.5kW/min to smelt the raw materials, and controlling the maximum smelting power of the smelting furnace at 300kW;
s5, cooling:
after the Cr and Nb raw materials in the smelting furnace in the step S4 are smelted, closing the smelting furnace to stop smelting, and naturally cooling the smelted alloy in the crucible to room temperature;
the purity of the Cr blocks and the Nb blocks in the step S1 is 99.96 percent, the sizes of the single Cr blocks and Nb blocks are controlled to be smaller than 20mm, and the surfaces of the Cr blocks and the Nb blocks are ensured to be clean and free of impurities during batching.
And when charging in the step S2, charging Cr blocks into a copper crucible with a water cooling function.
In the step S3, when the vacuum pumping in the smelting furnace is continuously performed by using diffusion pump, the vacuum degree in the smelting furnace needs to reach 1 × 10 -3 Pa。
And the smelting process in the step S4 comprises the steps of firstly starting a smelting furnace to smelt Cr blocks in a crucible, refining for 4min after the Cr blocks are completely smelted, then adding Nb blocks in an alloy material box into the crucible to be smelted together with Cr and stirred for 2min, gradually increasing smelting power at a speed of 12.5kW/min during smelting, controlling the maximum smelting power at 300kW, and finally refining for 10min after the Nb blocks are completely smelted.
And S4, after the raw materials are completely alloyed, stopping heating of the smelting furnace, cooling the crucible filled with the alloy ingot in the smelting furnace for 45min, turning over the alloy ingot in the crucible, starting the heating function of the smelting furnace again to continuously smelt the alloy ingot in the crucible, and repeating the step of smelting for 4 times after cooling.
And the specific cooling mode of the step S5 is that after the Cr blocks and the Nb blocks in the smelting furnace are smelted, the heating function of the smelting furnace is firstly closed, the alloy obtained after smelting is naturally cooled for 75min in the smelting furnace, then the smelting furnace is subjected to vacuum breaking, and then the smelted alloy ingot is taken out.
Detecting alloy components:
the alloy composition of 3 alloy ingot samples prepared by the method of the present example was measured, and the measurement results are shown in table 1.
TABLE 1 test results of example 1Cr2Nb alloy
| Sample block numbering | Cr(wt％) | Nb(wt％) |
| 1 | 52.68 | 47.32 |
| 2 | 52.23 | 47.77 |
| 3 | 52.78 | 47.22 |
Example 2:
a preparation method of a high-melting-point Cr2Nb intermetallic compound through suspension smelting comprises the following steps of:
s1, preparing raw materials:
weighing Cr blocks and Nb blocks according to the mass percentage for later use;
s2, charging:
putting the weighed Cr blocks into a crucible, then putting the crucible filled with the Cr blocks into a smelting furnace, and putting the weighed Nb blocks into an alloy bin of the smelting furnace;
s3, vacuumizing:
vacuumizing the smelting furnace in the step S2 by using a mechanical pump and a roots pump in sequence, and continuously vacuumizing the smelting furnace by using a diffusion pump when the vacuum degree in the smelting furnace is less than 10 Pa;
s4, smelting:
filling protective gas nitrogen into a smelting furnace, starting the smelting furnace when the pressure in the smelting furnace reaches 0.02MPa, gradually increasing the smelting power of the smelting furnace at the speed of 10kW/min to smelt the raw material, and controlling the maximum smelting power of the smelting furnace at 270kW;
s5, cooling:
after the Cr and Nb raw materials in the smelting furnace are smelted in the step S4, closing the smelting furnace to stop smelting, and naturally cooling the smelted alloy in the crucible to room temperature;
the purity of the Cr blocks and the Nb blocks in the step S1 is 99.98%, the sizes of the single Cr blocks and Nb blocks are controlled to be smaller than 20mm, and the surfaces of the Cr blocks and the Nb blocks are ensured to be clean and free of impurities during batching.
And when charging in the step S2, charging Cr blocks into a copper crucible with a water cooling function.
In the step S3, when the vacuum pumping in the smelting furnace is continuously performed by using diffusion pump, the vacuum degree in the smelting furnace needs to reach 1 × 10 -3 Pa。
And the smelting process in the step S4 is that the smelting furnace is started to smelt the Cr blocks in the crucible, the Cr blocks are refined for 3min after being completely smelted, then the Nb blocks in the alloy charging box are added into the crucible to be smelted together with Cr and stirred for 1min, the smelting power is gradually increased at the speed of 10kW/min during smelting, the maximum smelting power is controlled at 270kW, and finally the Nb blocks are refined for 8min after being completely smelted.
And S4, after the raw materials are completely alloyed, stopping heating of the smelting furnace, cooling the crucible filled with the alloy ingot in the smelting furnace for 30min, turning over the alloy ingot in the crucible, starting the heating function of the smelting furnace again to continuously smelt the alloy ingot in the crucible, and repeating the step of cooling and then smelting for 3 times.
And the specific cooling mode of the step S5 is that after the Cr blocks and the Nb blocks in the smelting furnace are smelted, the heating function of the smelting furnace is firstly closed, the alloy obtained after smelting is naturally cooled in the smelting furnace for 60min, then the smelting furnace is subjected to vacuum breaking, and finally the smelted alloy ingot is taken out.
Example 3:
a preparation method of a high-melting-point Cr2Nb intermetallic compound through suspension smelting comprises the following steps of, by mass, 56.0% of Cr and 44.0% of Nb, wherein the Cr2Nb intermetallic compound comprises the following components:
s1, preparing raw materials:
weighing Cr blocks and Nb blocks according to the mass percentage for later use;
s2, charging:
putting the weighed Cr blocks into a crucible, then putting the crucible filled with the Cr blocks into a smelting furnace, and putting the weighed Nb blocks into an alloy box of the smelting furnace;
s3, vacuumizing:
vacuumizing the smelting furnace in the step S2 by using a mechanical pump and a roots pump in sequence, and continuously vacuumizing the smelting furnace by using a diffusion pump when the vacuum degree in the smelting furnace is less than 10 Pa;
s4, smelting:
filling protective gas nitrogen into a smelting furnace, starting the smelting furnace when the pressure in the smelting furnace reaches 0.03MPa, gradually increasing the smelting power of the smelting furnace at the rate of 15kW/min to smelt the raw materials, and controlling the maximum smelting power of the smelting furnace at 330kW;
s5, cooling:
after the Cr and Nb raw materials in the smelting furnace are smelted in the step S4, closing the smelting furnace to stop smelting, and naturally cooling the smelted alloy in the crucible to room temperature;
the purity of the Cr blocks and the Nb blocks in the step S1 is 99.99%, the sizes of the single Cr blocks and Nb blocks are controlled to be smaller than 20mm, and the surfaces of the Cr blocks and the Nb blocks are ensured to be clean and free of impurities during batching.
And when charging in the step S2, charging Cr blocks into a copper crucible with a water cooling function.
In the step S3, when the vacuum pumping in the smelting furnace is continuously performed by using the diffusion pump, the vacuum degree in the smelting furnace needs to reach 0.5 multiplied by 10 -3 Pa。
And the smelting process in the step S4 is that the smelting furnace is started to smelt the Cr blocks in the crucible, the Cr blocks are refined for 5min after being completely smelted, then the Nb blocks in the alloy charging box are added into the crucible to be smelted together with Cr and stirred for 2min, the smelting power is gradually increased at the speed of 15kW/min during smelting, the maximum smelting power is controlled at 330kW, and finally the Nb blocks are refined for 10min after being completely smelted.
And S4, after the raw materials are completely alloyed, stopping heating of the smelting furnace, cooling the crucible filled with the alloy ingot in the smelting furnace for 60min, turning over the alloy ingot in the crucible, starting the heating function of the smelting furnace again to continuously smelt the alloy ingot in the crucible, and repeating the step of smelting for 4 times after cooling.
And the specific cooling mode of the step S5 is that after the Cr blocks and the Nb blocks in the smelting furnace are smelted, the heating function of the smelting furnace is firstly closed, the alloy obtained after smelting is naturally cooled for 90min in the smelting furnace, then the smelting furnace is subjected to vacuum breaking, and then the smelted alloy ingot is taken out.
Example 4:
in this example, the Cr2Nb alloy obtained in example 1 was used to prepare a GRCop-84 alloy, which comprises the following components in percentage by mass: cr2Nb 12 and the balance of copper.
Example 5:
in this example, the Cr2Nb alloy obtained in example 1 was used to prepare a GRCop-42 alloy, which had the following composition in mass percent: cr2Nb 6 and the balance of copper.
The alloy ingot samples prepared by the methods of examples 4 and 5 of the present invention were subjected to composition testing, and the results are shown in table 2.
Table 2 results of component detection of examples 4 and 5
Comparative example 1:
the comparative example is different from example 1 in that the Cr2Nb powder of the comparative example is prepared by low-temperature crushing and grinding. And the O and N contents of the alloy ingot sample block prepared in example 1 and the Cr2Nb powder prepared in the comparative example were measured, and the results are shown in Table 3.
Table 3 results of measuring contents of O and N in example 1 and comparative example 1
| Number of | O/wt％ | N/wt％ |
| Example 1 | 0.026 | 0.0039 |
| Comparative example 1 | 0.22 | 0.075 |
By the preparation method, the Cr2Nb alloy with qualified components can be prepared, compared with the traditional mechanical grinding process, the preparation process is greatly shortened, and the problem of raw material oxidation is effectively avoided. Furthermore, the Cr2Nb alloy prepared by the method can be used for preparing a CuCrNb alloy with qualified components, and the preparation problem of the alloy is successfully solved.
Claims (7)
1. A preparation method of a high-melting-point Cr2Nb intermetallic compound by suspension smelting is characterized in that the components of the Cr2Nb intermetallic compound are calculated according to the mass percent, the Cr element accounts for 52.0-56.0 percent, the Nb element accounts for 44.0-48.0 percent, and the preparation method comprises the following steps:
s1, preparing raw materials:
weighing Cr blocks and Nb blocks according to the mass percentage for later use;
s2, charging:
putting the weighed Cr blocks into a crucible, then putting the crucible filled with the Cr blocks into a smelting furnace, and putting the weighed Nb blocks into an alloy box of the smelting furnace;
s3, vacuumizing:
vacuumizing the smelting furnace in the step S2 by using a mechanical pump and a roots pump in sequence, and continuously vacuumizing the smelting furnace by using a diffusion pump when the vacuum degree in the smelting furnace is less than 10 Pa;
s4, smelting:
filling protective gas nitrogen into a smelting furnace, starting the smelting furnace when the pressure in the smelting furnace reaches 002 MPa-0.03 MPa, gradually increasing the smelting power of the smelting furnace at the rate of 10-15 kW/min to smelt the raw materials, and controlling the maximum smelting power of the smelting furnace at 270 kW-330 kW;
s5, cooling:
and (5) after the Cr and Nb raw materials in the smelting furnace are smelted in the step (S4), closing the smelting furnace to stop smelting, and naturally cooling the smelted alloy in the crucible to room temperature.
2. The method for preparing a suspension smelting high melting point Cr2Nb intermetallic compound according to claim 1, characterized in that: the purity of the Cr blocks and the Nb blocks in the step S1 needs to be more than 99.95 percent, the sizes of the single Cr blocks and Nb blocks are controlled to be less than 20mm, and the surfaces of the Cr blocks and the Nb blocks are ensured to be clean and free of impurities during batching.
3. The method for preparing a suspension smelting high melting point Cr2Nb intermetallic compound according to claim 1, characterized in that: and when charging in the step S2, charging Cr blocks into a copper crucible with a water cooling function.
4. The method for preparing a suspension smelting high melting point Cr2Nb intermetallic compound according to claim 1, characterized in that: in the step S3, when the vacuum pumping in the smelting furnace is continuously performed by using the diffusion pump, the vacuum degree in the smelting furnace needs to reach 0.5 multiplied by 10 -3 Pa～1×10 -3 Pa。
5. The method for preparing a suspension smelting high melting point Cr2Nb intermetallic compound according to claim 1, characterized in that: the smelting process in the step S4 comprises the steps of firstly starting a smelting furnace to smelt Cr blocks in a crucible, refining for 3-5 min after the Cr blocks are completely smelted, then adding Nb blocks in an alloy material box into the crucible to be smelted together with Cr and stirred for 1-2 min, gradually increasing smelting power at a speed of 10-15 kW/min during smelting, controlling the maximum smelting power at 270-330 kW, and finally refining for 5-10 min after the Nb blocks are completely smelted.
6. The method for preparing a suspension smelting high melting point Cr2Nb intermetallic compound according to claim 1, characterized in that: and S4, after the raw materials are completely alloyed, stopping heating the smelting furnace, cooling the crucible filled with the alloy ingot in the smelting furnace for 30-60 min, turning over the alloy ingot in the crucible, starting the heating function of the smelting furnace again to continuously smelt the alloy ingot in the crucible, and repeating the steps of cooling and smelting for 3-4 times.
7. The method for preparing a suspension smelting high melting point Cr2Nb intermetallic compound according to claim 1, characterized in that: and the specific cooling mode of the step S5 is that after the Cr blocks and the Nb blocks in the smelting furnace are smelted, the heating function of the smelting furnace is firstly closed, the alloy obtained after smelting is naturally cooled in the smelting furnace for 60-90 min, then the smelting furnace is subjected to vacuum breaking, and then the smelted alloy ingot is taken out.
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Application publication date: 20221122 Assignee: SIRUI ADVANCED COPPER ALLOY Co.,Ltd. Assignor: SHAANXI SIRUI ADVANCED MATERIALS Co.,Ltd. Contract record no.: X2023980040047 Denomination of invention: A preparation method for suspension melting of high melting point Cr2Nb intermetallic compounds Granted publication date: 20230509 License type: Common License Record date: 20230821 |