CN112680616A - Preparation method of vacuum induction melting Cu8Cr4Nb alloy - Google Patents
Preparation method of vacuum induction melting Cu8Cr4Nb alloy Download PDFInfo
- Publication number
- CN112680616A CN112680616A CN202011371858.0A CN202011371858A CN112680616A CN 112680616 A CN112680616 A CN 112680616A CN 202011371858 A CN202011371858 A CN 202011371858A CN 112680616 A CN112680616 A CN 112680616A
- Authority
- CN
- China
- Prior art keywords
- alloy
- cu8cr4nb
- cooling
- casting
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000956 alloy Substances 0.000 title claims abstract description 138
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 114
- 238000002844 melting Methods 0.000 title claims abstract description 23
- 230000008018 melting Effects 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 230000006698 induction Effects 0.000 title claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 70
- 238000005266 casting Methods 0.000 claims abstract description 39
- 229910052786 argon Inorganic materials 0.000 claims abstract description 35
- 239000010949 copper Substances 0.000 claims abstract description 24
- 229910052802 copper Inorganic materials 0.000 claims abstract description 21
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000003723 Smelting Methods 0.000 claims abstract description 13
- 238000011049 filling Methods 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 238000007599 discharging Methods 0.000 claims abstract description 11
- 238000007670 refining Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims description 59
- 239000000110 cooling liquid Substances 0.000 claims description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 5
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 5
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 8
- 229910052758 niobium Inorganic materials 0.000 abstract description 8
- 229910052804 chromium Inorganic materials 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000010955 niobium Substances 0.000 description 10
- 238000010010 raising Methods 0.000 description 10
- 239000011651 chromium Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000010790 dilution Methods 0.000 description 6
- 239000012895 dilution Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000004663 powder metallurgy Methods 0.000 description 5
- 238000005204 segregation Methods 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010308 vacuum induction melting process Methods 0.000 description 1
Images
Abstract
The invention discloses a preparation method of a vacuum induction melting Cu8Cr4Nb alloy, which comprises the following steps: s1, batching: prefabricating 8Cr4Nb intermediate alloy, and weighing an electrolytic copper plate and prefabricated 8Cr4Nb intermediate alloy according to percentage; s2 furnace charging: the prepared electrolytic copper plate and 8Cr4Nb intermediate alloy material are loaded into a crucible; s3, vacuumizing: starting the mechanical pump, and starting the roots pump when the vacuum pressure P in the furnace is less than or equal to 0.08 MPa; s4 smelting: when the pH value is less than or equal to 10Pa after the vacuum degree is pumped, heating the mixture in a gradient way to 65KW, reducing the power to 20KW after the metal in the crucible is completely melted, slowly filling high-purity argon into the furnace body, and closing an argon filling valve when the pressure in the furnace is increased to about 0.08 Mpa; s5 casting: increasing the power to 65KW, refining for 5min, reducing the power to 50KW, keeping for 1min, and starting casting, wherein the casting time is 1.5-2 min; s6 discharging: and (4) closing the heating after the casting is finished, and discharging the product after the product is cooled. The Cu8Cr4Nb alloy material prepared by the method has uniform components and structures, less inclusions, and no macroscopic and microscopic defects such as Cu, Cr and Nb enrichment.
Description
Technical Field
The invention relates to the technical field of alloy preparation, in particular to a preparation method of a Cu8Cr4Nb alloy by vacuum induction melting.
Background
In recent years, a copper alloy material with high strength, high conductivity and high temperature resistance is applied to the field of a non-destructive pulse strong magnetic field, the Cu8Cr4Nb material is verified for many times at present, all properties are superior to those of other materials, the material has the advantages of high-temperature strength, creep resistance, low cycle fatigue resistance, high thermal conductivity and the like, and can be used as a spraying material for rocket combustion chambers, the improvement of the performance of the lining wall surface material is a key of a long-life combustion chamber, the Cr2Nb particles in the alloy are mainly dispersed and strengthened, the high thermal conductivity of pure copper is kept, and the Cu8Cr4Nb alloy still keeps high mechanical properties under the high-temperature condition due to the fact that intermetallic compound particles have high melting points.
At present, the alloy material is imported at home, and the alloy material is manufactured by a powder metallurgy method at present in the domestic production process, so that the alloy material has the advantages of uneven composition structure, low density, low mechanical property and higher oxygen content; meanwhile, niobium belongs to high-melting-point metal, the melting point is 2468 ℃, the melting point of chromium is 1857 ℃, the melting point of copper is 1083 ℃, the difference of the melting points of the three metals is large, and the smelting difficulty is large.
Therefore, aiming at the defects in the prior art, the method for preparing the Cu8Cr4Nb alloy by vacuum induction melting is provided to solve the technical problems.
Disclosure of Invention
In order to solve the technical problem, the invention provides a preparation method of a vacuum induction melting Cu8Cr4Nb alloy.
The technical scheme of the invention is as follows: a preparation method of a vacuum induction melting Cu8Cr4Nb alloy comprises the following steps:
s1, batching: prefabricating 8Cr4Nb intermediate alloy, and weighing the electrolytic copper plate and the prefabricated 8Cr4Nb intermediate alloy according to percentage for later use;
s2 furnace charging: loading the prepared electrolytic copper plate and 8Cr4Nb intermediate alloy material into a crucible, closing a furnace cover, and closing a gas release valve;
s3, vacuumizing: starting a mechanical pump, opening a low-vacuum baffle valve for vacuumizing, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa;
s4 smelting: when the vacuum degree is pumped to reach a pH value of less than or equal to 10Pa, heating in a gradient manner to 65KW, keeping the temperature until the metal in the crucible is completely melted, reducing the power to 20KW, opening an argon filling valve, slowly filling high-purity argon into the furnace body, and closing the argon filling valve when the pressure in the furnace rises to about 0.08 Mpa;
s5 casting: increasing the power to 65KW, refining for 5min, reducing the power to 50KW, keeping for 1min, and starting casting, wherein the casting time is 1.5-2 min;
s6 discharging: and (4) after the casting is finished, closing the heating, cooling for 30min, and discharging.
Further, the Cu8Cr4Nb alloy consists of 5.5-7.5 wt% of Cr, 4.8-6.8 wt% of Nb and 85.7-89.7 wt% of Cu; however, considering that the loss of each metal element is inevitable in the preparation process of the Cu8Cr4Nb alloy, the percentage content of each metal ingredient in the Cu8Cr4Nb alloy is as follows: 6-8% of Cr, 5-7% of Nb and 86-90% of Cu. By providing different electrolytic copper plates and the content of 8Cr4Nb master alloy and the content of each element of 8Cr4Nb master alloy, the use of Cu8Cr4Nb for different purposes is met.
Further, in the step S1, baking and electric pulse composite treatment is performed after the 8Cr4Nb master alloy is prefabricated, specifically: the baking temperature is 180-240 ℃, the electric pulse treatment is carried out after baking is carried out for 20-30 min, the pulse current of the electric pulse treatment is 90-120A, the pulse frequency is 600-1100 Hz, then low-temperature high-purity argon is injected, the electric pulse treatment is removed when the temperature is reduced to 80-100 ℃, and then the temperature is continuously reduced to below 40 ℃ and the electric pulse treatment is taken out for standby application, wherein the low-temperature high-purity argon is specifically high-purity argon at the temperature of 10-15 ℃. The baking of the prefabricated 8Cr4Nb intermediate alloy is beneficial to accelerating the smelting speed and avoiding the splashing of alloy liquid, and meanwhile, the alloy forms amplitude-modulated-like structures through electric pulse treatment, so that the ordered segregation of the alloy is enhanced, and the electrical conductivity and other properties of the subsequently prepared Cu8Cr4Nb alloy are improved.
Further, the gradient heating and temperature rising in step S4 specifically includes: and (3) increasing the power to 30 +/-2 KW, keeping for 8min, increasing the power to 40 +/-2 KW, keeping for 10min, increasing the power to 50 +/-2 KW, keeping for 10min, and increasing the heating power to 65 KW. The gradient heating mode is adopted, so that the damage to equipment in the vacuum induction melting process can be reduced, and the release of lifting gas in raw materials is facilitated, so that the purity of the Cu8Cr4Nb alloy material is improved.
Further, in the step S5, a graphite crucible is used for casting, and the casting speed is specifically as follows: casting at the speed of 2.5 +/-1 t/min, accelerating to 4 +/-1 t/min, and decelerating to 2 +/-1 t/min. The casting speed is firstly slow, then properly accelerated and finally slowed down, thereby ensuring sufficient feeding and eliminating the metallurgical defects in the cast ingot.
As a technical solution of the present invention, the cooling method after casting in step S6 specifically includes: and discharging the steel plate from the furnace through a special water-cooling copper mold and water-cooling for 30 min. Since the Cu8Cr4Nb alloy material is cooled slowly, is easy to segregate and has deep shrinkage cavity, the problems can be effectively solved by cooling by adopting a water-cooling copper mold.
As another technical solution of the present invention, the cooling method in step S6 specifically includes: spray cooling with low-concentration cooling liquid with spray pressure of 8-12MPa in the early stage of cooling, air cooling with low-temperature high-purity argon gas with wind speed of 3-7m/s in the middle stage of cooling, soaking and cooling with high-concentration cooling liquid in the later stage of cooling, and washing with low-temperature pure water;
the low-concentration cooling liquid is cooling liquid (10-15X), and the high-concentration cooling liquid is cooling liquid (2-5X);
the early cooling period is 5-8min, the middle cooling period is 12-15min, the late cooling period is 7-13 min, the low-temperature high-purity argon is specifically high-purity argon at the temperature of 10-15 ℃, and the low-temperature pure water is specifically pure water at the temperature of 10-15 ℃.
Because the 8Cr4Nb alloy material is cooled slowly and is easy to segregate and has deep shrinkage holes, the alloy material is cooled and solidified by low-temperature high-purity argon through the staged cooling mode, then the solidified 8Cr4Nb alloy is subjected to spray cooling and immersion cooling by sequentially adopting high-multiple dilution cooling liquid and low-multiple dilution cooling liquid, and the problem that the Cu8Cr4Nb alloy is easy to segregate and has deep shrinkage holes through cooling in stages is effectively solved, so that the Cu8Cr4Nb alloy with compact and uniform structure and excellent performance is obtained.
Furthermore, the cooling liquid is prepared by mixing 10-15 parts by weight of sodium chloride, 5-8 parts by weight of polyvinyl alcohol, 2-3 parts by weight of disodium ethylene diamine tetraacetate, 1-2 parts by weight of sodium polyacrylate and 100-120 parts by weight of pure water. The low-concentration cooling liquid and the high-concentration cooling liquid which are formed by the cooling liquid in the proportion optimize the alloy structure and improve various mechanical properties of the Cu8Cr4Nb alloy while ensuring cooling.
The invention has the beneficial effects that:
(1) the preparation method of the invention adopts the 8Cr4Nb intermediate alloy, which can effectively reduce the secondary smelting temperature, enhances the uniformity of material components through secondary smelting, reduces element burning loss through smelting the intermediate alloy first, and effectively solves the problem of large smelting difficulty due to large difference of melting points of alloy elements of Nb, Cr and Cu.
(2) The Cu8Cr4Nb alloy material prepared by the preparation method has uniform components and tissues, few inclusions, and no macroscopic and microscopic defects such as Cu, Cr and Nb enrichment.
(3) The cooling method provided by the preparation method can accelerate the solidification of the molten metal, solve the problems of segregation defects and the like, and ensure that the produced Cu8Cr4Nb alloy ingot has compact structure, less pores and impurities and no metallurgical defects of enrichment, segregation and the like of alloy elements.
Drawings
FIG. 1 is a process flow diagram of the preparation method of the present invention.
FIG. 2 is a 50-fold metallographic photograph of the non-corrosive treatment of the 8Cr4Nb master alloy of the invention.
FIG. 3 is a 500-fold metallographic photograph of the corrosion-free intermediate alloy 8Cr4Nb of the present invention.
FIG. 4 is a 50-fold metallographic picture of a Cu8Cr4Nb alloy according to the invention after corrosion treatment.
FIG. 5 is a 500-fold metallographic photograph of the Cu8Cr4Nb alloy of the present invention after corrosion treatment.
Detailed Description
Example 1
A preparation method of a vacuum induction melting Cu8Cr4Nb alloy comprises the following steps:
preparation of 8Cr4Nb intermediate alloy
S11, batching: the raw materials comprise the following elements in percentage by weight: cr: 52.85%, Nb: 47.15 percent, and weighing the required raw materials in proportion;
s12 furnace charging: putting the prepared chromium block and niobium block into a crucible, closing a furnace cover, closing an air release valve, and cleaning an observation window;
s13, vacuumizing, starting a mechanical pump, opening a low-vacuum baffle valve for vacuumizing, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa;
s14 smelting: during smelting, when the pH value is less than or equal to 10Pa after vacuum pumping, heating and raising the temperature, raising the power to 18KW, keeping for 8min, raising the power to 40KW, keeping for 10min, raising the power to 52KW, keeping for 10min, raising the power to 65KW, keeping until metal in a crucible is completely melted, lowering the power to 20KW, opening an argon valve, slowly filling high-purity argon into a furnace body, and closing the argon filling valve when the pressure in the furnace is raised to about 0.08 MPa;
s15 casting: increasing power to 60KW, and refining for 5 min; enabling molten metal to be fully fused and uniform, then starting casting, using a graphite crucible for casting, and quickly casting, wherein the casting time is less than or equal to 30S;
s16 discharging: after the casting is finished, the heating is closed, the casting is carried out after the cooling is carried out for 20 minutes, and the casting quality condition is checked to obtain 8Cr4Nb intermediate alloy;
preparation of Cu8Cr4Nb alloy
S1, batching: weighing an electrolytic copper plate, a prefabricated 8Cr4Nb intermediate alloy, 89.35% of the electrolytic copper plate and 10.65% of the 8Cr4Nb intermediate alloy according to the percentage for later use;
s2 furnace charging: loading the prepared electrolytic copper plate and 8Cr4Nb intermediate alloy material into a crucible, closing a furnace cover, closing a gas release valve, and cleaning an observation window;
s3, vacuumizing: starting a mechanical pump, opening a low-vacuum baffle valve for vacuumizing, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa;
s4 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 30KW, keeping the power for 8min, raising the power to 40KW, keeping the power for 10min, raising the power to 50KW, keeping the power for 10min, raising the heating power to 65KW, keeping the power to 20KW after the metal in the crucible is completely melted, opening an argon filling gas valve, slowly filling high-purity argon into the furnace body, and closing the argon filling valve when the pressure in the furnace is raised to about 0.08 MPa;
s5 casting: increasing power to 65KW, refining for 5min, reducing power to 50KW, keeping for 1min, and starting casting, wherein a graphite crucible is used for casting, and the casting speed is specifically as follows: firstly, casting at the speed of 2.5t/min, then accelerating to 4t/min, finally decelerating to 2t/min, and using a special water-cooling copper mold for casting for 1.8 min;
s6 discharging: and (4) closing heating after the casting is finished, and discharging the casting from the furnace after water cooling for 30 min.
Example 2
The present embodiment is substantially the same as embodiment 1, except that the 8Cr4Nb master alloy is pre-fabricated and then subjected to baking + electric pulse composite treatment in step S1, specifically: the baking temperature is 210 ℃, the electric pulse treatment is carried out after the baking is carried out for 23min, the pulse current of the electric pulse treatment is 110A, the pulse frequency is 950Hz, then, low-temperature high-purity argon is injected, the electric pulse treatment is removed when the temperature is reduced to 95 ℃, then, the temperature is continuously reduced to below 40 ℃, and the argon is taken out for standby application, wherein the low-temperature high-purity argon is specifically high-purity argon at the temperature of 10 ℃. The baking of the prefabricated 8Cr4Nb intermediate alloy is beneficial to accelerating the smelting speed and avoiding the splashing of alloy liquid, and meanwhile, the alloy forms amplitude-modulated-like structures through electric pulse treatment, so that the ordered segregation of the alloy is enhanced, and the electrical conductivity and other properties of the subsequently prepared Cu8Cr4Nb alloy are improved.
Example 3
The present embodiment is substantially the same as embodiment 1, and the difference therebetween is that the cooling method in step S6 specifically includes: spray cooling is carried out by adopting low-concentration cooling liquid with the spray pressure of 9MPa in the early cooling stage, air cooling is carried out by adopting low-temperature high-purity argon with the wind speed of 6m/s in the middle cooling stage, soaking cooling is carried out by adopting high-concentration cooling liquid in the later cooling stage, and then washing is carried out by adopting low-temperature pure water;
the low-concentration cooling liquid is cooling liquid (12X), and the cooling liquid is diluted by 12 times by using pure water, and the high-concentration cooling liquid is cooling liquid (3X), and the cooling liquid is diluted by 3 times by using the pure water;
the early-stage cooling time is 7min, the middle-stage cooling time is 13min, the late-stage cooling time is 10min, the low-temperature high-purity argon is specifically high-purity argon at the temperature of 15 ℃, and the low-temperature pure water is specifically pure water at the temperature of 10 ℃.
Because the 8Cr4Nb alloy material is cooled slowly and is easy to segregate and has deep shrinkage holes, the alloy material is cooled and solidified by low-temperature high-purity argon through the staged cooling mode, then 8Cr4Nb alloy after solidification is subjected to spray cooling and immersion cooling by sequentially adopting high-multiple dilution cooling liquid and low-multiple dilution cooling liquid, and the problems that the 8Cr4Nb alloy is easy to segregate and has deep shrinkage holes through staged cooling are effectively solved, so that the Cu8Cr4Nb alloy with compact and uniform structure and excellent performance is obtained.
The cooling liquid is prepared by mixing 13 parts of sodium chloride, 7 parts of polyvinyl alcohol, 3 parts of disodium ethylene diamine tetraacetate, 2 parts of sodium polyacrylate and 110 parts of pure water in parts by weight. The low-concentration cooling liquid and the high-concentration cooling liquid which are formed by the cooling liquid in the proportion optimize the alloy structure and improve various mechanical properties of the Cu8Cr4Nb alloy while ensuring cooling.
Example 4
The present embodiment is substantially the same as embodiment 3, and the difference is that the ratio of the cooling liquid and the dilution ratio are different, specifically:
the low-concentration cooling liquid is cooling liquid (10X), and the high-concentration cooling liquid is cooling liquid (2X); the cooling liquid is prepared by mixing 10 parts of sodium chloride, 5 parts of polyvinyl alcohol, 2 parts of disodium ethylene diamine tetraacetate, 1 part of sodium polyacrylate and 100 parts of pure water in parts by weight. The low-concentration cooling liquid and the high-concentration cooling liquid which are formed by the cooling liquid in the proportion optimize the alloy structure and improve various mechanical properties of the Cu8Cr4Nb alloy while ensuring cooling.
Example 5
The present embodiment is substantially the same as embodiment 3, and the difference is that the ratio of the cooling liquid and the dilution ratio are different, specifically:
the low-concentration cooling liquid is cooling liquid (15X), and the high-concentration cooling liquid is cooling liquid (5X); the cooling liquid is prepared by mixing 15 parts of sodium chloride, 8 parts of polyvinyl alcohol, 3 parts of disodium ethylene diamine tetraacetate, 2 parts of sodium polyacrylate and 120 parts of pure water in parts by weight. The low-concentration cooling liquid and the high-concentration cooling liquid which are formed by the cooling liquid in the proportion optimize the alloy structure and improve various mechanical properties of the Cu8Cr4Nb alloy while ensuring cooling.
Cu8Cr4Nb alloy-related performance experiment
First, Cu8Cr4Nb alloy inspection
The Cu8Cr4Nb alloy was prepared three times by the method of example 1, and the alloy materials are numbered 1, 2 and 3, and the chemical content of the 8Cr4Nb master alloy material and the Cu8Cr4Nb alloy material are measured as shown in the following tables 1 and 2:
TABLE 18 CHEMICAL CONTENT DETECTION TABLE FOR CR4Nb MEDIUM ALLOY MATERIAL
| Numbering | Cr(％) | Nb(％) |
| 1 | 52.65 | 47.35 |
| 2 | 52.72 | 47.28 |
| 3 | 52.80 | 47.2 |
TABLE 2 Cu8Cr4Nb alloy material compounding and chemical content detection table
And the Cu8Cr4Nb alloy material prepared in the experimental example 1 is divided into two groups of samples to be respectively subjected to morphology observation,
the first group is Cu8Cr4Nb alloy which is not corroded, and the metallographic pictures of the Cu8Cr4Nb alloy material are shown in figures 2 and 3;
the second group is Cu8Cr4Nb alloy corrosion treatment, and the metallographic photos of the Cu8Cr4Nb alloy material are shown in FIGS. 4 and 5;
as can be seen from the tables 1 and 2, the alloy elements prepared by the preparation method disclosed by the invention are less in burning loss, and meanwhile, according to a metallographic photograph, the Cu8Cr4Nb alloy prepared by the preparation method disclosed by the invention is uniform in structure, less in inclusion and free of macroscopic and microscopic defects such as enrichment of Cu, Cr and Nb, and the metallurgical defects such as compact structure, less in pores and inclusion, enrichment and segregation of alloy elements and the like of a produced Cu8Cr4Nb alloy ingot due to large melting point difference of the alloy elements such as Nb, Cr and Cu are effectively overcome.
Comparative performance experiment of Cu8Cr4Nb alloy
Grouping experiments: the preparation method comprises the steps of selecting the existing powder metallurgy method, mixing electrolytic copper powder, chromium powder, niobium powder and atomization according to the alloy component proportion in example 1, mixing, grinding, pressing and forming, and sintering by adopting protective atmosphere to obtain a Cu8Cr4Nb alloy as a comparison example; the preparation methods of the embodiments 1 to 5 are selected to prepare Cu8Cr4Nb alloy which is respectively recorded as experiment example 1, experiment example 2, experiment example 3, experiment example 4 and experiment example 5;
detecting items: the tensile strength, yield strength and conductivity tests of the grouped Cu8Cr4Nb alloy are respectively carried out as follows:
1) tensile strength
Each group of Cu8Cr4Nb alloy samples are selected, and tensile test is carried out on a WDW-1 electronic universal testing machine according to GB228-2002 metal material room temperature tensile test method, and the test results are shown in the following table 3:
TABLE 3 tensile strength test chart for Cu8Cr4Nb alloy
2) Elongation percentage
Each group of Cu8Cr4Nb alloy samples were selected and subjected to elongation testing using a WDW-1 electronic universal tester, and the test results are shown in the following Table 4:
TABLE 4 yield strength test chart for Cu8Cr4Nb alloy
| Experimental example 1 | Experimental example 2 | Experimental example 3 | Experimental example 4 | Experimental example 5 | Comparative example | |
| Elongation/percent | 5.9 | 7.3 | 9.7 | 9.2 | 8.9 | 3.5 |
3) Electrical conductivity of
Each group of Cu8Cr4Nb alloy samples was taken and subjected to conductivity testing using a metal conductivity eddy current meter FD101, and the experimental results are shown in table 5 below:
TABLE 5 conductivity test chart for Cu8Cr4Nb alloy sample
| Experimental example 1 | Experimental example 2 | Experimental example 3 | Experimental example 4 | Experimental example 5 | Comparative example | |
| Electrical conductivity of | 87 | 92 | 89 | 87 | 88 | 80 |
And (4) experimental conclusion:
1) comparing experimental examples 1 to 5 with the comparative example,
as can be seen from the comparison of the data in FIG. 3, the tensile strength of the experimental examples 1-5 is superior to that of the Cu8Cr4Nb alloy prepared by the existing powder metallurgy method;
as can be seen from the comparison of the data in FIG. 4, the tensile ratios of the experimental examples 1-5 are superior to that of the Cu8Cr4Nb alloy prepared by the existing powder metallurgy method;
as can be seen from the comparison of the data in FIG. 5, the electrical conductivities of the experimental examples 1-5 are superior to those of the Cu8Cr4Nb alloy prepared by the existing powder metallurgy method.
2) In the comparative examples 1 and 2, the following,
according to the comparison of the data in FIG. 3, the tensile strength of the alloy in the experimental example 2 is improved to a certain extent compared with that in the experimental example 1, it can be seen that the tensile strength of the Cu8Cr4Nb alloy is influenced by the baking and electric pulse composite treatment of the prefabricated 8Cr4Nb intermediate alloy in the experimental example 2;
according to the comparison of the data in FIG. 4, the tensile rate of the experimental example 2 is improved to a certain extent compared with that of the experimental example 1, and it can be seen that the tensile strength of the Cu8Cr4Nb alloy is influenced to a certain extent by the baking and electric pulse composite treatment of the prefabricated 8Cr4Nb intermediate alloy in the experimental example 2;
as can be seen from the comparison of the data in FIG. 5, the conductivity of the alloy in Experimental example 2 is significantly improved compared to that in Experimental example 1, and it can be seen that the conductivity of the Cu8Cr4Nb alloy in Experimental example 2 is greatly influenced by the baking and electric pulse combined treatment of the prefabricated 8Cr4Nb intermediate alloy.
3) Comparative example 1 and examples 3 to 5,
according to the comparison of the data in FIG. 3, the tensile strength of the experimental examples 3-5 is obviously improved compared with that of the experimental example 1, and it can be seen that the experimental examples 3-5 have a great influence on the tensile strength of the Cu8Cr4Nb alloy by different cooling modes of the cast Cu8Cr4Nb alloy, wherein the tensile strength of the Cu8Cr4Nb alloy obtained under the parameters of the experimental example 4 is optimal;
as can be seen from the comparison of the data in FIG. 4, the elongation of the alloy in Experimental example 2 is significantly improved compared with that in Experimental example 1, and it can be seen that the elongation of the Cu8Cr4Nb alloy is significantly affected by different cooling modes of the cast Cu8Cr4Nb alloy in Experimental examples 3-5, wherein the elongation of the Cu8Cr4Nb alloy obtained under the parameters of Experimental example 4 is optimal;
as can be seen from the comparison of the data in FIG. 5, the conductivity of the alloy in Experimental example 2 has a certain effect on the conductivity of the Cu8Cr4Nb alloy in the experimental examples 3-5, which are different from the cooling method of the Cu8Cr4Nb alloy after casting.
Claims (8)
1. A preparation method of a vacuum induction melting Cu8Cr4Nb alloy is characterized by comprising the following steps:
s1, batching: prefabricating 8Cr4Nb intermediate alloy, and weighing the electrolytic copper plate and the prefabricated 8Cr4Nb intermediate alloy according to percentage for later use;
s2 furnace charging: loading the prepared electrolytic copper plate and 8Cr4Nb intermediate alloy material into a crucible, closing a furnace cover, and closing a gas release valve;
s3, vacuumizing: starting a mechanical pump, opening a low-vacuum baffle valve for vacuumizing, and starting a roots pump when the vacuum pressure in the furnace is less than or equal to 0.08 MPa;
s4 smelting: when the vacuum degree is pumped to reach a pH value of less than or equal to 10Pa, heating in a gradient manner to 65KW, keeping the temperature until the metal in the crucible is completely melted, reducing the power to 20KW, opening an argon filling valve, slowly filling high-purity argon into the furnace body, and closing the argon filling valve when the pressure in the furnace rises to about 0.08 Mpa;
s5 casting: increasing the power to 65KW, refining for 5min, reducing the power to 50KW, keeping for 1min, and starting casting, wherein the casting time is 1.5-2 min;
s6 discharging: and (4) after the casting is finished, closing the heating, cooling for 30min, and discharging.
2. The method for preparing the vacuum induction melting Cu8Cr4Nb alloy as claimed in claim 1, wherein the percentage content of each metal ingredient in the Cu8Cr4Nb alloy is respectively: 6-8% of Cr, 5-7% of Nb and 86-90% of Cu.
3. The method for preparing the vacuum induction melting Cu8Cr4Nb alloy according to claim 1, wherein the gradient heating temperature rise in the step S4 is specifically as follows: and (3) increasing the power to 30 +/-2 KW, keeping for 8min, increasing the power to 40 +/-2 KW, keeping for 10min, increasing the power to 50 +/-2 KW, keeping for 10min, and increasing the heating power to 65 KW.
4. The method for preparing the vacuum induction melting Cu8Cr4Nb alloy according to claim 1, wherein the step S5 of casting uses a graphite crucible, and the casting speed is as follows: casting at the speed of 2.5 +/-1 t/min, accelerating to 4 +/-1 t/min, and decelerating to 2 +/-1 t/min.
5. The method for preparing the vacuum induction melting Cu8Cr4Nb alloy according to claim 1, wherein the cooling method after casting in the step S6 is specifically as follows: and discharging the steel plate from the furnace through a special water-cooling copper mold and water-cooling for 30 min.
6. The method for preparing the vacuum induction melting Cu8Cr4Nb alloy according to claim 1, wherein the cooling method after casting in the step S6 is specifically as follows: in the early stage of cooling, low-temperature high-purity argon with the wind speed of 3-7m/s is adopted for air cooling, in the middle stage of cooling, low-concentration cooling liquid with the spraying pressure of 8-12MPa is adopted for spray cooling, in the later stage of cooling, high-concentration cooling liquid is adopted for soaking cooling, and then low-temperature pure water is adopted for flushing;
the low-concentration cooling liquid is cooling liquid (10-15X), and the high-concentration cooling liquid is cooling liquid (2-5X);
the early cooling period is 5-8min, the middle cooling period is 12-15min, the late cooling period is 7-13 min, the low-temperature high-purity argon is specifically high-purity argon at the temperature of 10-15 ℃, and the low-temperature pure water is specifically pure water at the temperature of 10-15 ℃.
7. The preparation method of the vacuum induction melting Cu8Cr4Nb alloy as claimed in claim 6, wherein the cooling liquid is prepared by mixing 10-15 parts by weight of sodium chloride, 5-8 parts by weight of polyvinyl alcohol, 2-3 parts by weight of disodium ethylene diamine tetraacetate, 1-2 parts by weight of sodium polyacrylate and 100-120 parts by weight of pure water.
8. The method for preparing the vacuum induction melting Cu8Cr4Nb alloy according to claim 1, wherein the 8Cr4Nb master alloy is pre-prepared and then is subjected to baking and electric pulse composite treatment in the step S1, which comprises the following steps: the baking temperature is 180-240 ℃, the electric pulse treatment is carried out after baking is carried out for 20-30 min, the pulse current of the electric pulse treatment is 90-120A, the pulse frequency is 600-1100 Hz, then low-temperature high-purity argon is injected, the electric pulse treatment is removed when the temperature is reduced to 80-100 ℃, and then the temperature is continuously reduced to below 40 ℃ and the electric pulse treatment is taken out for standby application, wherein the low-temperature high-purity argon is specifically high-purity argon at the temperature of 10-15 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011371858.0A CN112680616B (en) | 2020-11-30 | 2020-11-30 | Preparation method of vacuum induction melting Cu8Cr4Nb alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011371858.0A CN112680616B (en) | 2020-11-30 | 2020-11-30 | Preparation method of vacuum induction melting Cu8Cr4Nb alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112680616A true CN112680616A (en) | 2021-04-20 |
| CN112680616B CN112680616B (en) | 2022-01-11 |
Family
ID=75446941
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011371858.0A Active CN112680616B (en) | 2020-11-30 | 2020-11-30 | Preparation method of vacuum induction melting Cu8Cr4Nb alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112680616B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114293064A (en) * | 2022-03-09 | 2022-04-08 | 北京科技大学 | High-strength high-conductivity high-temperature-resistant Cu-Cr-Nb alloy and preparation method thereof |
| CN115156487A (en) * | 2022-06-29 | 2022-10-11 | 嘉兴微构电子科技有限公司 | Method for manufacturing homogenized copper alloy cast ingot |
| CN115369272A (en) * | 2022-07-23 | 2022-11-22 | 陕西斯瑞新材料股份有限公司 | Preparation method of suspension smelting high-melting-point Cr2Nb intermetallic compound |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013086157A (en) * | 2011-10-20 | 2013-05-13 | Sumitomo Chemical Co Ltd | Manufacturing method for cu-ga alloy slab |
| CN111036927A (en) * | 2019-12-25 | 2020-04-21 | 陕西斯瑞新材料股份有限公司 | Method for preparing GRCop-84 spherical powder based on VIGA process |
| CN111534708A (en) * | 2020-04-23 | 2020-08-14 | 陕西斯瑞新材料股份有限公司 | CuMn prepared by vacuum induction melting12Method for Ni alloy |
-
2020
- 2020-11-30 CN CN202011371858.0A patent/CN112680616B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013086157A (en) * | 2011-10-20 | 2013-05-13 | Sumitomo Chemical Co Ltd | Manufacturing method for cu-ga alloy slab |
| CN111036927A (en) * | 2019-12-25 | 2020-04-21 | 陕西斯瑞新材料股份有限公司 | Method for preparing GRCop-84 spherical powder based on VIGA process |
| CN111534708A (en) * | 2020-04-23 | 2020-08-14 | 陕西斯瑞新材料股份有限公司 | CuMn prepared by vacuum induction melting12Method for Ni alloy |
Non-Patent Citations (1)
| Title |
|---|
| 刘素芹等: ""电脉冲时效对Cu-Ni-Si合金组织和性能的影响"", 《河南科技大学学报（自然科学版）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114293064A (en) * | 2022-03-09 | 2022-04-08 | 北京科技大学 | High-strength high-conductivity high-temperature-resistant Cu-Cr-Nb alloy and preparation method thereof |
| CN115156487A (en) * | 2022-06-29 | 2022-10-11 | 嘉兴微构电子科技有限公司 | Method for manufacturing homogenized copper alloy cast ingot |
| CN115369272A (en) * | 2022-07-23 | 2022-11-22 | 陕西斯瑞新材料股份有限公司 | Preparation method of suspension smelting high-melting-point Cr2Nb intermetallic compound |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112680616B (en) | 2022-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112680616B (en) | Preparation method of vacuum induction melting Cu8Cr4Nb alloy | |
| CN109457167B (en) | Preparation method for CuFe alloy material with different Fe contents by vacuum induction melting | |
| CN109371271B (en) | Non-vacuum smelting and continuous casting process for copper-iron alloy | |
| CN109722553B (en) | Preparation method of copper-manganese intermediate alloy material | |
| CN111534708B (en) | CuMn prepared by vacuum induction melting12Method for Ni alloy | |
| CN110512104B (en) | CuMn prepared by vacuum induction melting25Ni10Method for alloying materials | |
| CN105506318B (en) | A kind of production technology of extra super duralumin alloy | |
| CN109913769B (en) | Fe-Mn-Cr-Ni series medium-entropy stainless steel and preparation method thereof | |
| CN111676404B (en) | Improved die casting forming method | |
| CN110714156A (en) | Light high-strength corrosion-resistant high-entropy alloy and preparation method thereof | |
| CN115044794B (en) | Cu- (Y) with excellent performance 2 O 3 -HfO 2 ) Alloy and preparation method thereof | |
| CN113736970B (en) | Preparation method of high-softening-resistance copper-chromium-zirconium alloy rod | |
| CN113564443B (en) | High-strength high-plasticity cast high-entropy alloy and preparation method thereof | |
| CN114381622A (en) | Preparation method of vacuum induction melting high-strength high-elasticity wear-resistant CuNiSn alloy material | |
| CN115558825B (en) | High-heat-conductivity high-strength and high-toughness die-casting aluminum alloy and preparation method thereof | |
| CN115404385B (en) | Refractory high-entropy alloy with excellent room-temperature tensile ductility and preparation method thereof | |
| CN110863124A (en) | High-strength high-plasticity medium-entropy alloy and preparation method thereof | |
| CN115612873A (en) | Equipment and method for preparing high-temperature alloy by combining high-temperature heat treatment and electric arc melting | |
| CN112080659B (en) | Preparation method of CuMn25Ni10Sn alloy material | |
| CN109913692B (en) | Preparation method of as-cast nickel-aluminum bronze alloy with high fatigue resistance | |
| CN111187968A (en) | Preparation method of 1.2367 hot-working extrusion die steel | |
| CN113151728B (en) | FeCrVTiCu high-entropy alloy and preparation method thereof | |
| CN115449582B (en) | Preparation method of high-purity iron | |
| CN113621849B (en) | Preparation method of high-strength high-conductivity Cu-Nb alloy material | |
| CN116970825A (en) | Preparation method of QSi3-1 alloy cast ingot by vacuum induction melting |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231110 Address after: 722200 room 888, No. 1, Wangyuan West Road, Xinxing Industrial Park, Fufeng County, Baoji City, Shaanxi Province Patentee after: Shaanxi Sirui Fufeng advanced copper alloy Co.,Ltd. Address before: 710071 No. 60 Wei Yi Road, Yanta Industrial Park, Yanta District, Xi'an, Shaanxi Patentee before: SIRUI ADVANCED COPPER ALLOY Co.,Ltd. |