CN111593225B - Preparation method for improving strength of chromium-zirconium-copper bar - Google Patents
Preparation method for improving strength of chromium-zirconium-copper bar Download PDFInfo
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- CN111593225B CN111593225B CN202010544840.XA CN202010544840A CN111593225B CN 111593225 B CN111593225 B CN 111593225B CN 202010544840 A CN202010544840 A CN 202010544840A CN 111593225 B CN111593225 B CN 111593225B
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- QZLJNVMRJXHARQ-UHFFFAOYSA-N [Zr].[Cr].[Cu] Chemical compound [Zr].[Cr].[Cu] QZLJNVMRJXHARQ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000005266 casting Methods 0.000 claims abstract description 97
- 239000000463 material Substances 0.000 claims abstract description 54
- 229910052802 copper Inorganic materials 0.000 claims abstract description 47
- 239000010949 copper Substances 0.000 claims abstract description 47
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000956 alloy Substances 0.000 claims abstract description 42
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 41
- 238000005242 forging Methods 0.000 claims abstract description 36
- 238000003723 Smelting Methods 0.000 claims abstract description 34
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000011651 chromium Substances 0.000 claims abstract description 23
- 238000002844 melting Methods 0.000 claims abstract description 22
- 230000008018 melting Effects 0.000 claims abstract description 22
- 230000032683 aging Effects 0.000 claims abstract description 17
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 13
- 238000005070 sampling Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 74
- 238000010438 heat treatment Methods 0.000 claims description 49
- 229910052786 argon Inorganic materials 0.000 claims description 37
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 19
- 230000007547 defect Effects 0.000 claims description 13
- 238000007670 refining Methods 0.000 claims description 13
- 238000007599 discharging Methods 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 17
- 239000002184 metal Substances 0.000 abstract description 17
- 238000005728 strengthening Methods 0.000 abstract description 17
- 239000006104 solid solution Substances 0.000 abstract description 16
- 239000007788 liquid Substances 0.000 abstract description 9
- GXDVEXJTVGRLNW-UHFFFAOYSA-N [Cr].[Cu] Chemical compound [Cr].[Cu] GXDVEXJTVGRLNW-UHFFFAOYSA-N 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 229910000831 Steel Inorganic materials 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000010959 steel Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 13
- XTYUEDCPRIMJNG-UHFFFAOYSA-N copper zirconium Chemical compound [Cu].[Zr] XTYUEDCPRIMJNG-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000010273 cold forging Methods 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000000265 homogenisation Methods 0.000 description 5
- 229910000881 Cu alloy Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000788 chromium alloy Substances 0.000 description 1
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D37/00—Controlling or regulating the pouring of molten metal from a casting melt-holding vessel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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Abstract
The invention discloses a preparation method for improving the strength of a chromium-zirconium-copper bar, which comprises the following steps: smelting an intermediate alloy CuZr40, preparing an electrolytic copper plate and a Cr block for vacuum smelting, adding CuZr40 into molten copper-chromium metal liquid in a secondary feeding mode, fully mixing and smelting the molten copper-chromium metal liquid and casting a steel die, roughly turning and detecting material components, carrying out hot forging treatment, solid solution treatment, rotary forging treatment and aging treatment on an ingot, and finally sampling and detecting material performance. The method of the invention improves the content of strengthening phase elements Cr and Zr by vacuum melting, and then improves the performance of the chromium-zirconium-copper bar by solid solution and aging strengthening by the subsequent rotary forging process, the tensile strength can reach more than 500MPa, and the method does not melt CuCr intermediate alloy but adopts direct addition of Cr blocks for melting, which is beneficial to the accuracy of batching, reduces the error, leads the material performance to be more stable, has good consistency, can reduce the working procedures and reduce the cost.
Description
Technical Field
The invention relates to the technical field of tungsten-copper alloy material preparation, in particular to a preparation method for improving the strength of a chromium-zirconium-copper bar.
Background
At present, high-conductivity and high-strength copper alloy is widely applied in various industries, particularly in the power industry, and in conductive products, higher requirements are put forward on the strength of stressed parts, so that the improvement of material performance by adjusting material components and changing processes is urgent.
At present, the mechanical properties of large-size bars (more than 60 mm) are improved mainly by adopting a hot forging and cold forging process mode, the hot forging process mode is mature, the primary deformation in the cold forging process is difficult to control, cracking easily occurs in the cold forging under the condition that the contents of chromium and zirconium in the copper-chromium-zirconium material are high, and the cold forging process determines that the forging ratio cannot be too large, if the forging ratio is too large, the forging ratio exceeds the range of the process, and the cracking phenomenon occurs. The rotary swaging can greatly improve the forging ratio and is not easy to break. Currently, by increasing the content of strengthening elements: cr and Zr elements. The material performance is improved by the subsequent rotary swaging process.
The method for improving the performance of the chromium-zirconium-copper alloy is mainly as follows:
1. solid solution and aging strengthening method: through a solid solution and aging strengthening mode, after the chromium-zirconium-copper is subjected to solid solution treatment, alloy elements are precipitated from a solid solution in subsequent aging to form strengthening phases which are distributed in a dispersing way, the dispersing phases prevent the movement of grain boundaries and dislocation, so that a matrix is strengthened, but through a large amount of data, the tensile strength detection data is 320-350 MPa after the cast copper-chromium-zirconium material is subjected to solid solution aging,
2. a deformation strengthening method: after the cast chromium-zirconium-copper ingot is forged (hot forged), and then is subjected to solid solution and aging strengthening treatment, the tensile strength is as follows: 380-420 MPa, and cold forging after hot forging, wherein the tensile strength is detected to be 420-450 MPa under the condition of an ultimate forging ratio, and the tensile strength cannot reach more than 500MPa at all.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method for improving the strength of a chromium-zirconium-copper bar, which improves the content of strengthening phase elements Cr and Zr through a vacuum smelting scheme, and improves the performance of the chromium-zirconium-copper bar through solid solution and aging strengthening by a subsequent rotary swaging process.
The technical scheme of the invention is as follows:
a preparation method for improving the strength of a chromium-zirconium-copper bar comprises the following steps:
preparation of one, CuZr40 intermediate alloy
(1) Preparing materials: according to the weight percentage, the electrolytic copper plate: 58%, zirconium sponge: 42 percent, weighing the required raw materials in proportion;
(2) vacuum melting and casting: placing the prepared electrolytic copper plate into a crucible, placing sponge zirconium into a secondary feeding device, closing a furnace cover, starting a mechanical pump, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa; when the vacuum degree is pumped to the pH value of less than or equal to 10Pa, heating and smelting until the electrolytic copper plate in the crucible is completely melted; when the power is reduced to 45KW, slowly adding the sponge zirconium for about 0.5 minute, fully dissolving for 1min, then starting casting, wherein a graphite crucible is used for casting, and the casting time is less than or equal to 2 min; after the casting is finished, closing the heating, cooling for 10 minutes, discharging, and checking the casting quality condition;
secondly, vacuum ingot casting and smelting of CuCr1Zr
(1) Preparing materials: weighing the materials according to the following weight ratio: proportion Cr block: 1-1.2%, CuZr 40: 0.65-0.7%, and the balance: electrolyzing a copper plate;
description of the drawings: the invention needs to control the material components to meet the following requirements: cr: 1-1.2%, CuZr 40: 0.65-0.7%, Fe < 0.08%, Si < 0.1%, the sum of other impurities < 0.2%, Cu: and (4) the balance.
Because Cr and Zr belong to strengthening phases, the material performance can be improved by increasing the contents of the two elements, and the mechanical performance of the material can be improved to the maximum extent by improving the upper line of the strengthening elements within the standard range of the material.
(2) Vacuum melting and casting: charging, namely, charging the prepared electrolytic copper plate and the chromium block wrapped by the copper sheet into a crucible, putting the CuZr40 intermediate alloy wrapped by the copper sheet into a secondary charging device, adding the CuZr40 into the molten copper-chromium metal liquid in a secondary charging mode, closing a furnace cover, closing a gas release valve, and cleaning an observation window; vacuumizing, starting a mechanical pump to vacuumize, and starting the roots pump when the vacuum pressure P in the furnace is less than or equal to 0.08 MPa;
description of the drawings: the CuZr40 is added after the crucible metal liquid is completely melted by adopting a secondary feeding mode, the reaction time is shorter than that of direct addition, the burning loss of alloy elements can be reduced, the CuZr40 is directly added into the metal liquid to be fully dissolved, and the uniformity of material components can be ensured.
(3) Smelting: during smelting, when the vacuum degree is pumped to a pH value of less than or equal to 10Pa, heating and raising the temperature, raising the power to 50 +/-5 KW, keeping for 15min, raising the power to 130 +/-5 KW, keeping for 15min, raising the power to 170 +/-5 KW until the power is melted, and when the power is reduced to 40 +/-5 KW, closing a roots pump and a slide valve pump, opening an argon valve, slowly filling argon into a furnace body to 0.08MPa, and closing an argon valve; then the power is adjusted to 80kW +/-5 kW, CuZr40 intermediate alloy in the secondary feeding device is added into the crucible, and the crucible is rotated back and forth for 2 times to ensure the homogenization of the copper-zirconium intermediate alloy;
(4) casting: reducing the power to 65KW +/-5 KW, keeping for about 1 minute, starting casting, closing heating after casting is finished, cooling for 35 minutes, and discharging;
description of the drawings: the steel mould is selected for use when vacuum melting, casting chromium zirconium copper ingot casting, and steel mould heat conduction is very high, easily material rapid cooling solidifies, and the rapid solidification is difficult for appearing thick column crystal, can make the crystalline grain tiny, easily later stage forging and improve material performance.
(5) Sawing and rough turning: sawing off a riser and the bottom of the cast ingot, removing casting defects such as shrinkage cavity and the like, and turning the outer circle until the black skin and the casting defects are completely removed;
(6) hot forging: carrying out hot forging treatment on the cast ingot after rough turning, and forging into a process size;
description of the drawings: coarse columnar crystals generated in the casting process are crushed through hot forging treatment to form fine grains, the microstructure is optimized, and the material performance can be improved;
(7) solution treatment: charging into a furnace for solution treatment at 995 ℃, keeping the temperature for 1.5 hours, and cooling with water for 5 minutes.
Description of the drawings: the material is solid-solution strengthened by the solid solution treatment, wherein the solid solution strengthening means that the lattice distortion is increased and the capability of inhibiting the movement of dislocation is increased along with the increase of the solute concentration of the alloy elements Cr and Zr, so that the strength and hardness of the material are improved.
Further, in the above scheme, in the operation of the step (2) in the first step, the heating and temperature-increasing smelting operation is: heating and raising temperature, raising power to 20 +/-2 KW, keeping for 6min, raising power to 40 +/-2 KW, keeping for 8min, raising heating power to 50KW, keeping the temperature for 10min, raising heating power to 60KW, and keeping for 10 min.
Description of the drawings: the adoption of the gradient heating mode is beneficial to the protection of a power supply of equipment, the gradient rising of the heating power can enable a melting layer, a heating layer and a preheating layer to exist in the crucible, the metal melting is facilitated, the gradient rising of the heating power can continuously accelerate the molten metal in the crucible to move in the crucible, and the component uniformity is facilitated.
Further, in the scheme, in the operation of the step (2) in the first step, after the electrolytic copper plate in the crucible is completely melted, the power is reduced to 40KW, an argon valve is opened, high-purity argon is slowly filled into the furnace body, when the pressure in the furnace is increased to about 0.08MPa, the argon valve is closed, the power is increased to 50KW, and refining is carried out for 2 min.
Description of the drawings: through refining, the alloy elements in the molten metal can be fully mixed and uniformly distributed.
Further, in the scheme, in the operation of the step (3) in the second step, after the smelting is finished, the power is slowly increased to 170kW +/-5 kW, and the refining is carried out for 20 minutes, so that the alloy elements in the molten metal are fully mixed and uniformly distributed.
Further, in the scheme, in the operation of the step (4) in the step two, the casting speed is firstly slow, then appropriately accelerated and finally slowed down, the slowest speed is 4-6ml/s, the fastest speed is 16-20ml/s, and the whole casting time is 5-6 min.
Further, in the above scheme, after the operation of the second step (7) is completed, the swaging treatment, the aging treatment and the sampling for detecting the material properties are also included.
Further, the swaging process is specifically: and (3) carrying out rotary swaging treatment on the forged ingot subjected to the solution treatment at normal temperature, and respectively achieving the required size after the forged ingot is subjected to diameter deformation of 7-7-7-7-5-5 mm.
The rotary swaging is forging at normal temperature, belongs to cold deformation, and can harden the material, refine grains and improve the tensile strength and hardness of the material.
Compared with the existing preparation method, the invention has the beneficial effects that:
the preparation method for improving the strength of the chromium-zirconium-copper bar material provided by the invention is characterized in that the contents of strengthening phase elements Cr and Zr are improved through vacuum melting, and the performance of the chromium-zirconium-copper bar material is improved through solid solution and aging strengthening through a subsequent rotary forging process, wherein the tensile strength can reach more than 500 MPa.
Compared with the mode that CuCrZr alloy is manufactured in the prior art, CuZr intermediate alloy and CuCr intermediate alloy are firstly manufactured, and then copper-chromium alloy and copper-zirconium intermediate alloy are put into bulk pure copper for smelting, the mode that the Cr block is directly added for smelting instead of the CuCr intermediate alloy is adopted, which is beneficial to the accuracy of material preparation and the reduction of errors.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a 100-fold magnification of a metallographic photograph of a product prepared in example 3 of the invention.
Fig. 3 is a 500-fold magnification of a metallographic photograph of a product prepared in example 3 of the invention.
Detailed Description
The invention provides a preparation method for improving the strength of a chromium-zirconium-copper bar.
The invention is described in further detail below with reference to the figures and the examples, which should not be construed as limiting the scope of the invention, but rather as enabling the skilled engineer in the field to make several insubstantial modifications and adaptations of the invention based on the above disclosure.
Example 1
A preparation method for improving the strength of a chromium-zirconium-copper bar comprises the following steps:
preparation of one, CuZr40 intermediate alloy
(1) Preparing materials: according to the weight percentage, the electrolytic copper plate: 58%, zirconium sponge: 42 percent, weighing the required raw materials in proportion;
(2) vacuum melting and casting: placing the prepared electrolytic copper plate into a crucible, placing sponge zirconium into a secondary feeding device, closing a furnace cover, starting a mechanical pump, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa; when the vacuum degree is pumped to reach a pH value of less than or equal to 10Pa, heating and smelting, and specifically operating as follows: heating and raising the temperature, wherein the power is increased to 18KW and kept for 6min, the power is increased to 438KW and kept for 8min, the heating power is increased to 50KW, the temperature is kept for 10min, the heating power is increased to 60KW and kept for 10 min. Melting the electrolytic copper plate in the crucible; reducing the power to 40KW, opening an argon valve, slowly filling high-purity argon into the furnace body, closing the argon valve when the pressure in the furnace rises to about 0.08MPa, increasing the power to 50KW, and refining for 2 min. When the power is reduced to 45KW, slowly adding the sponge zirconium for about 0.5 minute, fully dissolving for 1min, then starting casting, wherein a graphite crucible is used for casting, and the casting time is less than or equal to 2 min; after the casting is finished, closing the heating, cooling for 10 minutes, discharging, and checking the casting quality condition;
secondly, vacuum ingot casting and smelting of CuCr1Zr
(1) Preparing materials: weighing the materials according to the following weight ratio: proportion Cr block: 1%, CuZr 40: 0.72%, balance: electrolyzing a copper plate;
(2) vacuum melting and casting: charging, namely, charging the prepared electrolytic copper plate and the chromium block wrapped by the copper sheet into a crucible, putting the CuZr40 intermediate alloy wrapped by the copper sheet into a secondary charging device, adding the CuZr40 into the molten copper-chromium metal liquid in a secondary charging mode, closing a furnace cover, closing a gas release valve, and cleaning an observation window; vacuumizing, starting a mechanical pump to vacuumize, and starting the roots pump when the vacuum pressure P in the furnace is less than or equal to 0.08 MPa;
(3) smelting: during smelting, when the vacuum degree is pumped to a pH value of less than or equal to 10Pa, heating and raising the temperature, raising the power to 45KW, keeping for 15min, raising the power to 125KW, keeping for 15min, raising the power to 165KW until the materials are molten, closing a roots pump and a slide valve pump when the power is reduced to 35KW, opening an argon valve, and closing an argon valve when the argon is slowly filled into a furnace body to 0.08 MPa; then slowly adding power to 165kW, refining for 20 minutes, and fully mixing and uniformly distributing alloy elements in the molten metal. Then, adjusting the power to 75kW, adding the CuZr40 intermediate alloy in the secondary feeding device into the crucible, and rotating the crucible back and forth for 2 times to ensure the homogenization of the copper-zirconium intermediate alloy;
(4) casting: and reducing the power to 60KW, keeping the casting time for about 1 minute, and starting casting, wherein the casting speed is firstly slow, then is properly accelerated, and finally is slowed, the slowest is 4ml/s, the fastest is 16ml/s, and the whole casting time is 5 min. After the casting is finished, closing the heating, cooling for 35 minutes, and discharging;
(5) sawing and rough turning: sawing off a riser and the bottom of the cast ingot, removing casting defects such as shrinkage cavity and the like, and turning the outer circle until the black skin and the casting defects are completely removed;
(6) hot forging: carrying out hot forging treatment on the cast ingot after rough turning, and forging into a process size;
(7) solution treatment: charging into a furnace for solution treatment at 995 ℃, keeping the temperature for 1.5 hours, and cooling with water for 5 minutes.
Example 2
A preparation method for improving the strength of a chromium-zirconium-copper bar comprises the following steps:
preparation of one, CuZr40 intermediate alloy
(1) Preparing materials: according to the weight percentage, the electrolytic copper plate: 58%, zirconium sponge: 42 percent, weighing the required raw materials in proportion;
(2) vacuum melting and casting: placing the prepared electrolytic copper plate into a crucible, placing sponge zirconium into a secondary feeding device, closing a furnace cover, starting a mechanical pump, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa; when the vacuum degree is pumped to reach a pH value of less than or equal to 10Pa, heating and smelting, and specifically operating as follows: heating and raising the temperature, wherein the power is increased to 20KW and kept for 6min, the power is increased to 40KW and kept for 8min, the heating power is increased to 50KW, the temperature is kept for 10min, the heating power is increased to 60KW and kept for 10 min. Melting the electrolytic copper plate in the crucible; reducing the power to 40KW, opening an argon valve, slowly filling high-purity argon into the furnace body, closing the argon valve when the pressure in the furnace rises to about 0.08MPa, increasing the power to 50KW, and refining for 2 min. When the power is reduced to 45KW, slowly adding the sponge zirconium for about 0.5 minute, fully dissolving for 1min, then starting casting, wherein a graphite crucible is used for casting, and the casting time is less than or equal to 2 min; after the casting is finished, closing the heating, cooling for 10 minutes, discharging, and checking the casting quality condition;
secondly, vacuum ingot casting and smelting of CuCr1Zr
(1) Preparing materials: weighing the materials according to the following weight ratio: proportion Cr block: 1.09%, CuZr 40: 0.7%, the balance: electrolyzing a copper plate;
(2) vacuum melting and casting: charging, namely, charging the prepared electrolytic copper plate and the chromium block wrapped by the copper sheet into a crucible, putting the CuZr40 intermediate alloy wrapped by the copper sheet into a secondary charging device, adding the CuZr40 into the molten copper-chromium metal liquid in a secondary charging mode, closing a furnace cover, closing a gas release valve, and cleaning an observation window; vacuumizing, starting a mechanical pump to vacuumize, and starting the roots pump when the vacuum pressure P in the furnace is less than or equal to 0.08 MPa;
(3) smelting: during smelting, when the vacuum degree is pumped to a pH value of less than or equal to 10Pa, heating and raising the temperature, raising the power to 50KW, keeping for 15min, raising the power to 130KW, keeping for 15min, raising the power to 170KW until the materials are molten, closing a roots pump and a slide valve pump when the power is reduced to 40KW, opening an argon valve, and closing an argon valve when the argon valve is opened to slowly fill argon into a furnace body to 0.08 MPa; then slowly adding power to 170kW, refining for 20 minutes, and fully mixing alloy elements in the molten metal and uniformly distributing. Then the power is adjusted to 80kW, CuZr40 intermediate alloy in the secondary feeding device is added into the crucible, and the crucible is rotated back and forth for 2 times, so that the homogenization of the copper-zirconium intermediate alloy is ensured;
(4) casting: and reducing the power to 65KW, keeping the casting time for about 1 minute, and starting casting, wherein the casting speed is firstly slow, then is properly accelerated, and finally is slowed, the slowest is 5ml/s, the fastest is 18ml/s, and the whole casting time is 5 min. After the casting is finished, closing the heating, cooling for 35 minutes, and discharging;
(5) sawing and rough turning: sawing off a riser and the bottom of the cast ingot, removing casting defects such as shrinkage cavity and the like, and turning the outer circle until the black skin and the casting defects are completely removed;
(6) hot forging: carrying out hot forging treatment on the cast ingot after rough turning, and forging into a process size;
(7) solution treatment: charging into a furnace for solution treatment at 995 ℃, keeping the temperature for 1.5 hours, and cooling with water for 5 minutes.
Example 3
A preparation method for improving the strength of a chromium-zirconium-copper bar comprises the following steps:
preparation of one, CuZr40 intermediate alloy
(1) Preparing materials: according to the weight percentage, the electrolytic copper plate: 58%, zirconium sponge: 42 percent, weighing the required raw materials in proportion;
(2) vacuum melting and casting: placing the prepared electrolytic copper plate into a crucible, placing sponge zirconium into a secondary feeding device, closing a furnace cover, starting a mechanical pump, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa; when the vacuum degree is pumped to reach a pH value of less than or equal to 10Pa, heating and smelting, and specifically operating as follows: heating and raising the temperature, wherein the power is increased to 22KW and kept for 6min, the power is increased to 42KW and kept for 8min, the heating power is increased to 50KW, the temperature is kept for 10min, the heating power is increased to 60KW and kept for 10 min. Melting the electrolytic copper plate in the crucible; reducing the power to 40KW, opening an argon valve, slowly filling high-purity argon into the furnace body, closing the argon valve when the pressure in the furnace rises to about 0.08MPa, increasing the power to 50KW, and refining for 2 min. When the power is reduced to 45KW, slowly adding the sponge zirconium for about 0.5 minute, fully dissolving for 1min, then starting casting, wherein a graphite crucible is used for casting, and the casting time is less than or equal to 2 min; after the casting is finished, closing the heating, cooling for 10 minutes, discharging, and checking the casting quality condition;
secondly, vacuum ingot casting and smelting of CuCr1Zr
(1) Preparing materials: weighing the materials according to the following weight ratio: proportion Cr block: 1.15%, CuZr 40: 0.7%, the balance: electrolyzing a copper plate;
(2) vacuum melting and casting: charging, namely, charging the prepared electrolytic copper plate and the chromium block wrapped by the copper sheet into a crucible, putting the CuZr40 intermediate alloy wrapped by the copper sheet into a secondary charging device, adding the CuZr40 into the molten copper-chromium metal liquid in a secondary charging mode, closing a furnace cover, closing a gas release valve, and cleaning an observation window; vacuumizing, starting a mechanical pump to vacuumize, and starting the roots pump when the vacuum pressure P in the furnace is less than or equal to 0.08 MPa;
(3) smelting: during smelting, when the vacuum degree is pumped to a pH value of less than or equal to 10Pa, heating and raising the temperature, raising the power to 55KW, keeping for 15min, raising the power to 135KW, keeping for 15min, raising the power to 175KW until the materials are molten, closing a roots pump and a slide valve pump when the power is reduced to 45KW, opening an argon valve, and closing an argon valve when the argon is slowly filled into a furnace body to 0.08 MPa; then slowly adding power to 175kW, refining for 20 minutes to fully mix alloy elements in the molten metal and uniformly distribute the alloy elements. Then adjusting the power to 85kW, adding the CuZr40 intermediate alloy in the secondary feeding device into the crucible, and rotating the crucible back and forth for 2 times to ensure the homogenization of the copper-zirconium intermediate alloy;
(4) casting: and reducing the power to 70KW, keeping the casting time for about 1 minute, and starting casting, wherein the casting speed is firstly slow, then is properly accelerated, and finally is slowed, the slowest is 6ml/s, the fastest is 20ml/s, and the whole casting time is 5 min. After the casting is finished, closing the heating, cooling for 35 minutes, and discharging;
(5) sawing and rough turning: sawing off a riser and the bottom of the cast ingot, removing casting defects such as shrinkage cavity and the like, and turning the outer circle until the black skin and the casting defects are completely removed;
(6) hot forging: carrying out hot forging treatment on the cast ingot after rough turning, and forging into a process size;
(7) solution treatment: charging into a furnace for solution treatment at 995 ℃, keeping the temperature for 1.5 hours, and cooling with water for 5 minutes.
Example 4
A preparation method for improving the strength of a chromium-zirconium-copper bar comprises the following steps:
preparation of one, CuZr40 intermediate alloy
(1) Preparing materials: according to the weight percentage, the electrolytic copper plate: 58%, zirconium sponge: 42 percent, weighing the required raw materials in proportion;
(2) vacuum melting and casting: placing the prepared electrolytic copper plate into a crucible, placing sponge zirconium into a secondary feeding device, closing a furnace cover, starting a mechanical pump, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa; when the vacuum degree is pumped to reach a pH value of less than or equal to 10Pa, heating and smelting, and specifically operating as follows: heating and raising the temperature, wherein the power is increased to 22KW and kept for 6min, the power is increased to 42KW and kept for 8min, the heating power is increased to 50KW, the temperature is kept for 10min, the heating power is increased to 60KW and kept for 10 min. Melting the electrolytic copper plate in the crucible; reducing the power to 40KW, opening an argon valve, slowly filling high-purity argon into the furnace body, closing the argon valve when the pressure in the furnace rises to about 0.08MPa, increasing the power to 50KW, and refining for 2 min. When the power is reduced to 45KW, slowly adding the sponge zirconium for about 0.5 minute, fully dissolving for 1min, then starting casting, wherein a graphite crucible is used for casting, and the casting time is less than or equal to 2 min; after the casting is finished, closing the heating, cooling for 10 minutes, discharging, and checking the casting quality condition;
secondly, vacuum ingot casting and smelting of CuCr1Zr
(1) Preparing materials: weighing the materials according to the following weight ratio: proportion Cr block: 1.2%, CuZr 40: 0.72%, balance: electrolyzing a copper plate;
(2) vacuum melting and casting: charging, namely, charging the prepared electrolytic copper plate and the chromium block wrapped by the copper sheet into a crucible, putting the CuZr40 intermediate alloy wrapped by the copper sheet into a secondary charging device, adding the CuZr40 into the molten copper-chromium metal liquid in a secondary charging mode, closing a furnace cover, closing a gas release valve, and cleaning an observation window; vacuumizing, starting a mechanical pump to vacuumize, and starting the roots pump when the vacuum pressure P in the furnace is less than or equal to 0.08 MPa;
(3) smelting: during smelting, when the vacuum degree is pumped to a pH value of less than or equal to 10Pa, heating and raising the temperature, raising the power to 55KW, keeping for 15min, raising the power to 135KW, keeping for 15min, raising the power to 175KW until the materials are molten, closing a roots pump and a slide valve pump when the power is reduced to 45KW, opening an argon valve, and closing an argon valve when the argon is slowly filled into a furnace body to 0.08 MPa; then slowly adding power to 175kW, refining for 20 minutes to fully mix alloy elements in the molten metal and uniformly distribute the alloy elements. Then adjusting the power to 85kW, adding the CuZr40 intermediate alloy in the secondary feeding device into the crucible, and rotating the crucible back and forth for 2 times to ensure the homogenization of the copper-zirconium intermediate alloy;
(4) casting: and reducing the power to 70KW, keeping the casting time for about 1 minute, and starting casting, wherein the casting speed is firstly slow, then is properly accelerated, and finally is slowed, the slowest is 6ml/s, the fastest is 20ml/s, and the whole casting time is 6 min. After the casting is finished, closing the heating, cooling for 35 minutes, and discharging;
(5) sawing and rough turning: sawing off a riser and the bottom of the cast ingot, removing casting defects such as shrinkage cavity and the like, and turning the outer circle until the black skin and the casting defects are completely removed;
(6) hot forging: carrying out hot forging treatment on the cast ingot after rough turning, and forging into a process size;
(7) solution treatment: charging into a furnace for solution treatment at 995 ℃, keeping the temperature for 1.5 hours, and cooling with water for 5 minutes.
Example 5
After the operation of step (7) is completed, the material properties are examined by swaging, aging and sampling in example 3.
The rotary swaging treatment specifically comprises the following steps: and (3) carrying out rotary swaging treatment on the forged ingot subjected to the solution treatment at normal temperature, and respectively achieving the required size after the forged ingot is subjected to diameter deformation of 7-7-7-7-5-5 mm.
Example 6
After the operation of step (7) is completed, the material properties are examined by swaging, aging and sampling in example 4.
The rotary swaging treatment specifically comprises the following steps: and (3) carrying out rotary swaging treatment on the forged ingot subjected to the solution treatment at normal temperature, and respectively achieving the required size after the forged ingot is subjected to diameter deformation of 7-7-7-7-5-5 mm.
The above numerical value (7-7-7-7-5-5 mm) means the forging strain per one time, for example, the diameter is originally 90mm, and the diameter is 83mm at the time of first forging and drawing. The rotary swaging is forging at normal temperature, belongs to cold deformation, and can harden the material, refine grains and improve the tensile strength and hardness of the material.
In the solid solution and aging treatment, the solid solution and the aging are ensured to be sufficient, because the solid solution and the aging strengthening can lead the strengthening elements Cr and Zr to be distributed in a better dispersion way only under the condition of sufficient heat treatment, and the performance of the material is higher only if the material is distributed in a better dispersion way.
Table 1: material composition tables for examples 1 to 4
Table 2: product performance test results obtained in examples 1 to 6
As can be seen from the data in tables 1 and 2, when the Cr content is 1.15% and the Zr content is 0.28%, the comprehensive evaluation of various performance parameters of the prepared product is better, and the product performance is further improved after the product is subjected to the rotary swaging treatment and the aging treatment. That is, the product prepared in example 5 was optimized in performance.
Claims (2)
1. The preparation method for improving the strength of the chromium-zirconium-copper bar is characterized by comprising the following steps:
preparation of one, CuZr40 intermediate alloy
(1) Preparing materials: according to the weight percentage, the electrolytic copper plate: 58%, zirconium sponge: 42 percent, weighing the required raw materials in proportion;
(2) vacuum melting and casting: placing the prepared electrolytic copper plate into a crucible, placing sponge zirconium into a secondary feeding device, closing a furnace cover, starting a mechanical pump, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa; when the vacuum degree is pumped to the pH value of less than or equal to 10Pa, heating and smelting until the electrolytic copper plate in the crucible is completely melted; when the power is reduced to 45KW, slowly adding the sponge zirconium for about 0.5 minute, fully dissolving for 1min, and then starting casting, wherein the casting time is less than or equal to 2 min; after the casting is finished, closing the heating, cooling for 10 minutes, discharging, and checking the casting quality condition;
secondly, vacuum ingot casting and smelting of CuCr1Zr
(1) Preparing materials: weighing the materials according to the following weight ratio: proportion Cr block: 1-1.2%, CuZr 40: 0.65-0.7%, and the balance: electrolyzing a copper plate;
(2) vacuum melting and casting: charging, namely, charging the prepared electrolytic copper plate and the chromium block wrapped by the copper sheet into a crucible, putting the CuZr40 intermediate alloy wrapped by the copper sheet into a secondary charging device, closing a furnace cover, closing a gas release valve, and cleaning an observation window; vacuumizing, starting a mechanical pump to vacuumize, and starting the roots pump when the vacuum pressure P in the furnace is less than or equal to 0.08 MPa;
(3) smelting: during smelting, when the vacuum degree is pumped to a pH value of less than or equal to 10Pa, heating and raising the temperature, raising the power to 50 +/-5 KW, keeping for 15min, raising the power to 130 +/-5 KW, keeping for 15min, raising the power to 170 +/-5 KW until the power is melted, and when the power is reduced to 40 +/-5 KW, closing a roots pump and a slide valve pump, opening an argon valve, slowly filling argon into a furnace body to 0.08MPa, and closing an argon valve; then the power is adjusted to 80kW +/-5 kW, CuZr40 intermediate alloy in the secondary feeding device is added into the crucible, and the crucible is rotated back and forth for 2 times;
(4) casting: reducing the power to 65KW +/-5 KW, keeping for about 1 minute, starting casting, closing heating after casting is finished, cooling for 35 minutes, and discharging;
(5) sawing and rough turning: sawing off a riser and the bottom of the cast ingot, removing shrinkage cavity casting defects, and turning the outer circle until black skin and casting defects are completely removed;
(6) hot forging: carrying out hot forging treatment on the cast ingot after rough turning, and forging into a process size;
(7) solution treatment: charging into a furnace for solution treatment, keeping the temperature at 995 ℃ for 1.5 hours, and cooling by water for 5 minutes;
in the operation of the step (2) in the first step, the heating and temperature-raising smelting operation is as follows: heating and raising the temperature, wherein the power is raised to 20 +/-2 KW and kept for 6min, the power is raised to 40 +/-2 KW and kept for 8min, the heating power is raised to 50KW, the temperature is kept for 10min, the heating power is raised to 60KW and kept for 10 min;
in the operation of the step (3), after the smelting is finished, slowly adding power to 170kW +/-5 kW, and refining for 20 minutes;
in the operation of the step (4) in the second step, the casting speed is firstly slow, then appropriately accelerated and finally slowed, the slowest speed is 4-6ml/s, the fastest speed is 16-20ml/s, and the whole casting time is 5-6 min;
after the operation of the second step (7) is completed, rotary swaging treatment, aging treatment and sampling detection of material performance are further carried out;
the rotary swaging treatment specifically comprises the following steps: and (3) carrying out rotary swaging treatment on the forged ingot subjected to the solution treatment at normal temperature, and respectively achieving the required size after the forged ingot is subjected to diameter deformation of 7-7-7-7-5-5 mm.
2. The preparation method for improving the strength of the chromium-zirconium-copper bar as claimed in claim 1, wherein in the operation of the step (2), after the electrolytic copper plate in the crucible is completely melted, the power is reduced to 40KW, the argon valve is opened, high-purity argon is slowly filled into the furnace body, when the pressure in the furnace is increased to about 0.08MPa, the argon valve is closed, the power is increased to 50KW, and refining is carried out for 2 min.
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