CN115229378A - High-entropy alloy brazing filler metal and preparation method and application thereof - Google Patents
High-entropy alloy brazing filler metal and preparation method and application thereof Download PDFInfo
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- CN115229378A CN115229378A CN202210958405.0A CN202210958405A CN115229378A CN 115229378 A CN115229378 A CN 115229378A CN 202210958405 A CN202210958405 A CN 202210958405A CN 115229378 A CN115229378 A CN 115229378A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Abstract
The invention relates to a high-entropy alloy brazing filler metal and a preparation method and application thereof, and belongs to the technical field of high-temperature brazing. In order to solve the problem of brittle phase in the brazing connection process of Ni-based alloy and stainless steel, the invention provides a high-entropy alloy brazing filler metal which comprises the following components in parts by weight: 3-8 parts of Co, 3-8 parts of Fe, 1-3 parts of Mn, 3-8 parts of Ni and 2-9 parts of Ti. The high-entropy alloy brazing filler metal forms a liquid phase at the brazing temperature by virtue of the pseudo-binary eutectic reaction of FeCoNi and MnTi, so that the fluidity of the brazing filler metal is improved, and the metallurgical bonding of an interface is effectively promoted. Active element Ti in the brazing filler metal can react with the base metal to promote interface bonding, and meanwhile, excessive reaction of Ni is inhibited, and the generation of a joint brittle phase is avoided. The high-entropy alloy solder is suitable for brazing Ni-based alloy and stainless steel, a welded joint meets the use requirement of 600 ℃, and the shear strength of the obtained joint can reach 470-550 MPa.
Description
Technical Field
The invention belongs to the technical field of high-temperature brazing, and particularly relates to a high-entropy alloy brazing filler metal and a preparation method and application thereof.
Background
The nickel-based alloy has excellent oxidation resistance and corrosion resistance, and is suitable for structural materials of steam generators in pressurized water reactor nuclear power stations. However, they are expensive and often require composite components with stainless steel to reduce material costs. Since the difference in thermal expansion coefficient between nickel and iron is large, a large residual stress is easily formed in the welded joint, resulting in welding defects such as cracks, pores, and the like. In addition, composition segregation and brittle phase formation at the weld are also another major technical challenge.
Although the diffusion bonding technology can bond dissimilar materials, the bonding temperature is high, and the strength dispersity of the obtained joint is high; the brazing connection temperature is low, the advantage of small deformation is achieved, cracks and air holes can be effectively inhibited, and intermetallic compounds (IMC) can be formed at the interface due to strong chemical affinity and small solid solubility between the base metal and the brazing filler metal on the two sides. Most of these IMCs are hard and brittle, which severely reduces the strength and toughness of the welded joint and deteriorates the mechanical properties. Therefore, how to inhibit the generation of brittle phases is an urgent problem to be solved in the field of high-strength brazing connection of nickel-based alloy and stainless steel.
Disclosure of Invention
The invention provides a high-entropy alloy brazing filler metal and a preparation method and application thereof, and aims to solve the problem that a brazed joint of Ni-based alloy and stainless steel has poor quality due to a brittle phase.
The technical scheme of the invention is as follows:
the high-entropy alloy brazing filler metal comprises the following components in parts by weight: 3 to 8 portions of Co, 3 to 8 portions of Fe, 1 to 3 portions of Mn, 3 to 8 portions of Ni and 2 to 9 portions of Ti.
The preparation method of the high-entropy alloy brazing filler metal comprises the steps of weighing 3-8 parts by weight of Co metal simple substance particles, 3-8 parts by weight of Fe metal simple substance particles, 1-3 parts by weight of Mn metal simple substance particles, 3-8 parts by weight of Ni metal simple substance particles and 2-9 parts by weight of Ti metal simple substance particles, uniformly mixing the weighed metal simple substance particles, smelting in a protective gas atmosphere to obtain a high-entropy alloy ingot, and preparing a sample to obtain the high-entropy alloy brazing filler metal.
Further, the smelting is repeated for 6 times to realize the uniformity of the components.
Further, the sample preparation is to cut the high-entropy alloy ingot into slices of 5mm multiplied by 5mm and 0.5mm in thickness, and then polish and polish the slices to 0.4mm in thickness.
An application of high-entropy alloy solder in brazing Ni-based alloy and stainless steel.
Further, the Ni-based alloy is GH3536, GH3230, GH3170 or GH4169, and the stainless steel is 304 stainless steel or 310 stainless steel.
Further, the specific brazing method comprises the following steps: and assembling the high-entropy alloy brazing filler metal between the surfaces to be welded, applying pressure for fixation, heating to 1100-1250 ℃ in a vacuum environment, preserving heat for 5-30 min, and cooling to 200 ℃ to finish brazing.
Further, the pressure is 1MPa, and the vacuum condition is that the vacuum degree is lower than 1 x 10 -3 Pa。
Further, the heating speed is 20 ℃/min, and the cooling speed is 5 ℃/min.
The invention has the beneficial effects that:
the high-entropy alloy solder provided by the invention forms a liquid phase at a soldering temperature by virtue of a pseudo-binary eutectic reaction of FeCoNi and MnTi to reduce the melting point of the solder, and the eutectic high-entropy alloy improves the fluidity of the solder and can effectively promote interface metallurgical bonding. Active element Ti in the brazing filler metal can react with the base metal to promote interface bonding, excessive reaction of Ni is inhibited, the generation of a brittle phase of a joint is avoided, and the strength of a welding seam and the high-temperature performance of the joint are improved.
The high-entropy alloy solder provided by the invention does not contain Au, pd and other precious metals, and is low in price. The high-entropy alloy brazing filler metal is prepared by a smelting method, so that the elements are uniformly mixed and reacted, and the formed brazing filler metal is flaky, and the dosage of the brazing filler metal is controlled during welding. The high-entropy alloy solder is suitable for brazing Ni-based alloy and stainless steel, and can effectively inhibit the formation of brittle IMC at an interface under the combined action of a high-entropy effect and a delayed diffusion effect, so that the quality of a welded joint is improved, the mechanical property of the welded joint is improved, the obtained welded joint meets the use requirement at 600 ℃, and the shear strength can reach 470-600 MPa and is far higher than that of brazed joints of other solders.
Drawings
FIG. 1 is an electron micrograph of the high entropy alloy filler metal prepared in example 1;
FIG. 2 is an electron micrograph of the high-entropy alloy solder prepared in example 1 used for welding a resulting soldered joint;
a picture is an electron microscope photograph of a welded joint magnified 5000 times;
b is an electron micrograph of the welded joint magnified 16000 times;
and c is an electron micrograph of the welded joint magnified 70000 times.
FIG. 3 is an electron micrograph of the microstructure of the Inconel 617/AISI 321 stainless steel brazed joint of comparative example 1.
Detailed Description
The technical solutions of the present invention are further described below with reference to the embodiments, but the present invention is not limited thereto, and any modifications or equivalent substitutions made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention should be covered in the protection scope of the present invention. The process equipment or apparatus not specifically mentioned in the following examples are conventional in the art, and if not specifically mentioned, the raw materials and the like used in the examples of the present invention are commercially available; unless otherwise specified, all technical means used in the examples of the present invention are conventional means well known to those skilled in the art.
Example 1
The embodiment provides a high-entropy alloy solder which is prepared by smelting 5.9g of Co elementary substance particles, 5.6g of Fe elementary substance particles, 1.2g of Mn elementary substance particles, 6.3g of Ni elementary substance particles and 3.8g of Ti elementary substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this example were 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 5.9g of Co simple substance particles, 5.6g of Fe simple substance particles, 1.2g of Mn simple substance particles, 6.3g of Ni simple substance particles and 3.8g of Ti simple substance particles; uniformly mixing all the metal simple substance particles, putting the mixture into a smelting furnace, and vacuumizing the furnace to 1 x 10 -3 And Pa, injecting argon gas, intermittently smelting for 6 times under the current of 150A to obtain a high-entropy alloy ingot, cutting the high-entropy alloy ingot into Cheng Qiecheng mm multiplied by 5mm slices with the thickness of 0.5mm by using an electric spark cutting machine, and polishing the thickness of the high-entropy alloy slices to 0.4mm by using a polishing machine to obtain the high-entropy alloy brazing filler metal.
Fig. 1 shows the micro-morphology of the high-entropy alloy solder prepared in this example, it can be found that the alloy has distinct eutectic phases, namely, an FCC phase soft phase and a Laves hard phase, and the combination of the two phases improves the strength and plasticity of the alloy itself.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 When Pa, the alloy is heated to 1180 ℃ at a heating rate of 20 ℃/min and is kept at the temperature for 10 minutes, and then the alloy is cooled to 200 ℃ at a cooling rate of 5 ℃/min, thus completing the GH3536 Ni-based alloyAnd 304 stainless steel.
The test shows that the shear strength of a soldering joint of GH3536 Ni-based alloy and 304 stainless steel obtained by soldering is 550MPa.
The GH3536 Ni-based alloy obtained in the present example and the 304 stainless steel brazed joint were observed by electron microscopy, and the results are shown in FIG. 2, and the chemical compositions and possible phases of A, B, C, D, E, F in FIG. 2 were analyzed, and the results are shown in Table 1.
TABLE 1 at%
As can be seen from FIG. 2 and Table 1, it can be seen from the photographs of the joint structure that the weld main body is FCC solid solution structure and IMC intermetallic compounds are dispersed and distributed in the joint. The active element Ti has higher activity and can generate interface reaction with GH3536 Ni-based alloy, thereby improving the interface bonding strength. Fe. The Co element forms a eutectic structure consisting of FCC and high-temperature resistant Laves phase in the center of the welding seam, so that the strength of the welding seam is improved, and the high-temperature performance of the joint is obviously improved. The weld seam matrix is composed of (Fe, co, ni) -FCC phase, the plasticity of the joint is improved, and the effect of relieving stress is achieved.
Example 2
The embodiment provides a high-entropy alloy solder which is prepared by smelting 5.9g of Co elementary substance particles, 5.6g of Fe elementary substance particles, 1.2g of Mn elementary substance particles, 6.3g of Ni elementary substance particles and 3.8g of Ti elementary substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this example were 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 5.9g of Co simple substance particles, 5.6g of Fe simple substance particles, 1.2g of Mn simple substance particles, 6.3g of Ni simple substance particles and 3.8g of Ti simple substance particles; uniformly mixing all the metal simple substance particles and then putting the mixture into a smelting furnaceThe furnace is vacuumized to 1 x 10 -3 And Pa, injecting argon gas, intermittently smelting for 6 times under the current of 150A to obtain a high-entropy alloy ingot, cutting the high-entropy alloy ingot into Cheng Qiecheng mm by 5mm slices with the thickness of 0.5mm by using an electric spark cutting machine, and polishing the high-entropy alloy slices to the thickness of 0.4mm by using a polishing machine to obtain the high-entropy alloy brazing filler metal.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 And when Pa is reached, heating to 1140 ℃ at the heating rate of 20 ℃/min, preserving heat for 10 minutes, and then cooling to 200 ℃ at the speed of 5 ℃/min, thus finishing the brazing of the GH3536 Ni-based alloy and the 304 stainless steel.
The test shows that the shear strength of a soldering joint of the GH3536 Ni-based alloy and 304 stainless steel obtained by brazing is 480MPa.
Example 3
The embodiment provides a high-entropy alloy solder which is prepared by smelting 5.9g of Co simple substance particles, 5.6g of Fe simple substance particles, 1.2g of Mn simple substance particles, 6.3g of Ni simple substance particles and 3.8g of Ti simple substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this embodiment are 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 5.9g of Co simple substance particles, 5.6g of Fe simple substance particles, 1.2g of Mn simple substance particles, 6.3g of Ni simple substance particles and 3.8g of Ti simple substance particles; uniformly mixing all the metal simple substance particles, putting the mixture into a smelting furnace, and vacuumizing the furnace to 1 x 10 -3 Pa, back flushing with argon at 150AIntermittently smelting for 6 times under the current to obtain a high-entropy alloy ingot, cutting the high-entropy alloy ingot into Cheng Qiecheng mm by 5mm slices with the thickness of 0.5mm by using an electric spark cutting machine, and grinding and polishing the thickness of the high-entropy alloy slices to 0.4mm by using a polishing machine to obtain the high-entropy alloy brazing filler metal.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 And when Pa is needed, heating to 1160 ℃ at the temperature rising speed of 20 ℃/min, preserving heat for 10 minutes, and then cooling to 200 ℃ at the speed of 5 ℃/min, thus finishing the brazing of the GH3536 Ni-based alloy and the 304 stainless steel.
The test shows that the shearing strength of a soldering joint of the GH3536 Ni-based alloy and 304 stainless steel obtained by brazing is 500MPa.
Example 4
The embodiment provides a high-entropy alloy solder which is prepared by smelting 5.9g of Co elementary substance particles, 5.6g of Fe elementary substance particles, 1.2g of Mn elementary substance particles, 6.3g of Ni elementary substance particles and 3.8g of Ti elementary substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this example were 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 5.9g of Co simple substance particles, 5.6g of Fe simple substance particles, 1.2g of Mn simple substance particles, 6.3g of Ni simple substance particles and 3.8g of Ti simple substance particles; uniformly mixing all the metal simple substance particles, putting the mixture into a smelting furnace, and vacuumizing the furnace to 1 x 10 -3 Pa, injecting argon, intermittently smelting for 6 times under the current of 150A to obtain a high-entropy alloy ingot, and obtaining the high-entropy alloy ingotCutting Cheng Qiecheng with a spark cutting machine into sheets which are 5363 mm multiplied by 5mm and 0.5mm in thickness, and grinding and polishing the high-entropy alloy sheets to 0.4mm in thickness through a polishing machine to obtain the high-entropy alloy brazing filler metal.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 And when Pa is needed, heating to 1200 ℃ at a heating rate of 20 ℃/min, preserving heat for 10 minutes, and then cooling to 200 ℃ at a speed of 5 ℃/min, thus finishing the brazing of the GH3536 Ni-based alloy and the 304 stainless steel.
The test shows that the shear strength of a soldering joint of the GH3536 Ni-based alloy and 304 stainless steel obtained by brazing is 470MPa.
Example 5
The embodiment provides a high-entropy alloy solder which is prepared by smelting 5.9g of Co elementary substance particles, 5.6g of Fe elementary substance particles, 1.2g of Mn elementary substance particles, 6.3g of Ni elementary substance particles and 3.8g of Ti elementary substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this example were 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 5.9g of Co simple substance particles, 5.6g of Fe simple substance particles, 1.2g of Mn simple substance particles, 6.3g of Ni simple substance particles and 3.8g of Ti simple substance particles; uniformly mixing all the metal simple substance particles, putting the mixture into a smelting furnace, and vacuumizing the furnace to 1 x 10 -3 Pa, injecting argon gas, intermittently smelting for 6 times under the current of 150A to obtain a high-entropy alloy ingot, cutting the high-entropy alloy ingot by using an electric spark cutting machine to obtain Cheng Qiecheng mm multiplied by 5mm and the thickness of 0And polishing the thickness of the high-entropy alloy sheet to 0.4mm by using a polishing machine to obtain the high-entropy alloy solder.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 And when Pa, heating to 1180 ℃ at a heating rate of 20 ℃/min, keeping the temperature for 5 minutes, and then cooling to 200 ℃ at a cooling rate of 5 ℃/min to complete the brazing of the GH3536 Ni-based alloy and the 304 stainless steel.
The test shows that the shear strength of a soldering joint of GH3536 Ni-based alloy and 304 stainless steel obtained by soldering is 502MPa.
Example 6
The embodiment provides a high-entropy alloy solder which is prepared by smelting 5.9g of Co elementary substance particles, 5.6g of Fe elementary substance particles, 1.2g of Mn elementary substance particles, 6.3g of Ni elementary substance particles and 3.8g of Ti elementary substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this example were 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 5.9g of Co simple substance particles, 5.6g of Fe simple substance particles, 1.2g of Mn simple substance particles, 6.3g of Ni simple substance particles and 3.8g of Ti simple substance particles; uniformly mixing all the metal simple substance particles, putting the mixture into a smelting furnace, vacuumizing the furnace to 1 x 10 -3 Pa, back-flushing argon, intermittently smelting for 6 times under the current of 150A to obtain a high-entropy alloy ingot, cutting the high-entropy alloy ingot into Cheng Qiecheng mm 5 multiplied by 5mm slices with the thickness of 0.5mm by using an electric spark cutting machine, and grinding and polishing the high-entropy alloy slices with the thickness of 0.5mm by using a polishing machine0.4mm, and obtaining the high-entropy alloy solder.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 And when Pa is reached, heating to 1180 ℃ at the temperature rising speed of 20 ℃/min, preserving heat for 15 minutes, and then cooling to 200 ℃ at the speed of 5 ℃/min, thus finishing the brazing of the GH3536 Ni-based alloy and 304 stainless steel.
The test shows that the shearing strength of the soldering joint of the GH3536 Ni-based alloy and the 304 stainless steel obtained by soldering is 525MPa.
Example 7
The embodiment provides a high-entropy alloy solder which is prepared by smelting 5.9g of Co elementary substance particles, 5.6g of Fe elementary substance particles, 1.2g of Mn elementary substance particles, 6.3g of Ni elementary substance particles and 3.8g of Ti elementary substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this example were 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 5.9g of Co simple substance particles, 5.6g of Fe simple substance particles, 1.2g of Mn simple substance particles, 6.3g of Ni simple substance particles and 3.8g of Ti simple substance particles; uniformly mixing all the metal simple substance particles, putting the mixture into a smelting furnace, and vacuumizing the furnace to 1 x 10 -3 And Pa, injecting argon gas, intermittently smelting for 6 times under the current of 150A to obtain a high-entropy alloy ingot, cutting the high-entropy alloy ingot into Cheng Qiecheng mm by 5mm slices with the thickness of 0.5mm by using an electric spark cutting machine, and polishing the high-entropy alloy slices to the thickness of 0.4mm by using a polishing machine to obtain the high-entropy alloy brazing filler metal.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 And when Pa is reached, heating to 1180 ℃ at the temperature rising speed of 20 ℃/min, preserving heat for 20 minutes, and then cooling to 200 ℃ at the speed of 5 ℃/min, thus finishing the brazing of the GH3536 Ni-based alloy and 304 stainless steel.
The test shows that the shear strength of a soldering joint of GH3536 Ni-based alloy and 304 stainless steel obtained by soldering is 500MPa.
In conclusion, the high-entropy brazing filler metal disclosed by the invention can well realize the brazing connection of the nickel-based alloy and the 304 stainless steel, the main body of a welding seam is an FCC solid solution tissue, and IMC intermetallic compounds are dispersed in a joint, so that the comprehensive performance of the joint is good, and the high-entropy brazing filler metal is simple in manufacturing process, convenient to operate and convenient to popularize.
Example 8
The embodiment provides a high-entropy alloy solder which is prepared by smelting 4.9g of Co elementary substance particles, 3.8g of Fe elementary substance particles, 1.5g of Mn elementary substance particles, 7.0g of Ni elementary substance particles and 4.2g of Ti elementary substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this embodiment are 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 4.9g of Co simple substance particles, 3.8g of Fe simple substance particles, 1.5g of Mn simple substance particles, 7.0g of Ni simple substance particles and 4.2g of Ti simple substance particles; uniformly mixing all the metal simple substance particles, putting the mixture into a smelting furnace, and vacuumizing the furnace to 1 x 10 -3 Pa, injecting argon gas, intermittently smelting for 6 times under the current of 150A,and cutting the high-entropy alloy ingot into Cheng Qiecheng mm multiplied by 5mm slices with the thickness of 0.5mm by using an electric spark cutting machine, and grinding and polishing the thickness of the high-entropy alloy slices to 0.4mm by using a polishing machine to obtain the high-entropy alloy brazing filler metal.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 And when Pa is reached, heating to 1180 ℃ at the temperature rising speed of 20 ℃/min, preserving heat for 10 minutes, and then cooling to 200 ℃ at the speed of 5 ℃/min, thus finishing the brazing of the GH3536 Ni-based alloy and 304 stainless steel.
The test shows that the shearing strength of a soldering joint of the GH3536 Ni-based alloy and 304 stainless steel obtained by brazing is 530MPa.
Example 9
The embodiment provides a high-entropy alloy solder which is prepared by smelting 5.0g of Co elementary substance particles, 6.1g of Fe elementary substance particles, 1.1g of Mn elementary substance particles, 6.5g of Ni elementary substance particles and 3.5g of Ti elementary substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this example were 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 5.0g of Co simple substance particles, 6.1g of Fe simple substance particles, 1.1g of Mn simple substance particles, 6.5g of Ni simple substance particles and 3.5g of Ti simple substance particles; uniformly mixing all the metal simple substance particles, putting the mixture into a smelting furnace, vacuumizing the furnace to 1 x 10 -3 Pa, back-flushing argon, intermittently smelting for 6 times under the current of 150A to obtain a high-entropy alloy ingot, and cutting the obtained high-entropy alloy ingot by using an electric spark cutting machineCutting Cheng Qiecheng mm 5mm multiplied by 5mm and 0.5mm thick slices, and grinding and polishing the thickness of the high-entropy alloy slices to 0.4mm by a polishing machine to obtain the high-entropy alloy solder.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 And Pa, heating to 1180 ℃ at a heating rate of 20 ℃/min, keeping the temperature for 10 minutes, and then cooling to 200 ℃ at a cooling rate of 5 ℃/min to complete the brazing of the GH3536 Ni-based alloy and the 304 stainless steel.
The test shows that the shearing strength of a soldering joint of the GH3536 Ni-based alloy and 304 stainless steel obtained by soldering is 541MPa.
Example 10
The embodiment provides a high-entropy alloy solder which is prepared by smelting 7.1g of Co elementary substance particles, 5.5g of Fe elementary substance particles, 1.8g of Mn elementary substance particles, 6.3g of Ni elementary substance particles and 4.2g of Ti elementary substance particles.
The purity of the Mn simple substance particles, the purity of the Ti simple substance particles, the purity of the Co simple substance particles, the purity of the Ni simple substance particles, and the purity of the Fe simple substance particles used in this example were 99.9%, and 99.9%, respectively.
The specific preparation method of the high-entropy alloy solder in the embodiment is as follows:
weighing 7.1g of Co simple substance particles, 5.5g of Fe simple substance particles, 1.8g of Mn simple substance particles, 6.3g of Ni simple substance particles and 4.2g of Ti simple substance particles; uniformly mixing all the metal simple substance particles, putting the mixture into a smelting furnace, and vacuumizing the furnace to 1 x 10 -3 Pa, injecting argon gas, intermittently smelting for 6 times under the current of 150A to obtain a high-entropy alloy ingot, cutting the high-entropy alloy ingot into Cheng Qiecheng mm multiplied by 5mm slices with the thickness of 0.5mm by using an electric spark cutting machine, and polishing the high-entropy alloy ingot by using a polishing millAnd (5) grinding and polishing the thickness of the alloy sheet to 0.4mm to obtain the high-entropy alloy solder.
The high-entropy alloy solder prepared in the embodiment is used for soldering GH3536 Ni-based alloy and 304 stainless steel, and the specific soldering method comprises the following steps:
polishing and cleaning the surfaces to be welded of GH3536 Ni-based alloy and 304 stainless steel, naturally drying the cleaned materials, assembling the materials in a form of 304 stainless steel-high entropy alloy brazing filler metal GH3536 Ni-based alloy from top to bottom, applying 1MPa pressure on the surface of the 304 stainless steel for fixing, and then putting the assembled workpiece into a vacuum heating furnace, wherein when the vacuum degree is lower than 1 multiplied by 10 -3 And when Pa is reached, heating to 1180 ℃ at the temperature rising speed of 20 ℃/min, preserving heat for 10 minutes, and then cooling to 200 ℃ at the speed of 5 ℃/min, thus finishing the brazing of the GH3536 Ni-based alloy and 304 stainless steel.
The test shows that the shear strength of a soldering joint of GH3536 Ni-based alloy and 304 stainless steel obtained by brazing is 539MPa.
Comparative example 1
This comparative example provides joint strength data and microstructure electron micrographs of joints obtained by brazing an Inconel 617 nickel-based alloy and AISI 321 stainless steel using AMS4772Ag brazing filler metal.
The components of AMS4772Ag solder are shown in table 2:
TABLE 2 (wt%)
As can be seen from the microstructure electron microscope photograph of the joint shown in fig. 3, fe enrichment occurs at the interface between the AISI 321 base material and AMS4772, and a brittle phase, which is an iron-rich boride, is easily formed, resulting in a large brittleness of the joint. Meanwhile, the base materials on the two sides are subjected to heat treatment in the brazing process, so that the crystal grains grow and coarsen, and the hardness value is reduced. In addition, because a large amount of soft and tough Ag-rich phases exist in the brazing seams, the hardness value is further reduced, and therefore, even under the condition that the brazing temperature is 750 ℃ and the holding time is 60min, the shearing strength of the joint only reaches 322.9MPa.
In conclusion, the comparison shows that the high-entropy alloy solder provided by the invention can obtain higher joint shear strength than other conventional solders when used for brazing nickel-based alloy and stainless steel. The high-entropy alloy solder disclosed by the invention forms a liquid phase at a soldering temperature by virtue of a pseudo-binary eutectic reaction of FeCoNi and MnTi to reduce the melting point of the solder, and the eutectic high-entropy alloy improves the fluidity of the solder and can effectively promote interface metallurgical bonding. Active element Ti in the brazing filler metal can react with the base metal to promote interface bonding, excessive reaction of Ni is inhibited, the generation of a brittle phase of a joint is avoided, and the strength of a welding seam and the high-temperature performance of the joint are improved. The high-entropy alloy solder is more suitable for brazing Ni-based alloy and stainless steel, and can effectively inhibit the formation of brittle IMC at an interface under the combined action of a high-entropy effect and a delayed diffusion effect, so that the quality of a welded joint is improved, the mechanical property of the welded joint is improved, the obtained welded joint meets the use requirement at 600 ℃, and the shear strength can reach 470-600 MPa and is far higher than that of brazed joints of other solders. Moreover, the high-entropy alloy solder provided by the invention does not contain precious metals such as Au, pd and the like, and is lower in price.
Claims (8)
1. The high-entropy alloy brazing filler metal is characterized by comprising the following components in parts by weight: 3-8 parts of Co, 3-8 parts of Fe, 1-3 parts of Mn, 3-8 parts of Ni and 2-9 parts of Ti.
2. A preparation method of the high-entropy alloy solder as claimed in claim 1, characterized in that 3-8 parts by weight of Co elemental metal particles, 3-8 parts by weight of Fe elemental metal particles, 1-3 parts by weight of Mn elemental metal particles, 3-8 parts by weight of Ni elemental metal particles and 2-9 parts by weight of Ti elemental metal particles are weighed, the weighed elemental metal particles are uniformly mixed and melted under a protective gas atmosphere to obtain a high-entropy alloy ingot, and the high-entropy alloy solder is obtained after sample preparation.
3. A preparation method of the high-entropy alloy solder according to claim 2, wherein the smelting is repeated 6 times.
4. A preparation method of a high-entropy alloy solder according to claim 2 or 3, characterized in that the sample preparation is to cut the high-entropy alloy ingot into slices of 5mm x 5mm and 0.5mm in thickness, and then polish the slices to 0.4mm in thickness.
5. Use of the high entropy alloy filler metal according to claim 1 for brazing Ni base alloy and stainless steel.
6. The application of the high-entropy alloy brazing filler metal in brazing Ni-based alloy and stainless steel according to claim 5, is characterized in that the specific brazing method comprises the following steps: and assembling the high-entropy alloy brazing filler metal between the surfaces to be brazed, applying pressure for fixing, heating to 1100-1250 ℃ in a vacuum environment, preserving heat for 5-30 min, and cooling to 200 ℃ to finish brazing.
7. Use of a high entropy alloy brazing filler metal according to claim 5 or 6 in brazing Ni base alloy and stainless steel, characterized in that the pressure is 1MPa, and the vacuum condition is a vacuum degree lower than 1 x 10 -3 Pa。
8. Use of a high entropy alloy brazing filler metal according to claim 7 in brazing Ni-based alloy and stainless steel, wherein the heating rate is 20 ℃/min and the cooling rate is 5 ℃/min.
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| CN116117379A (en) * | 2022-12-30 | 2023-05-16 | 大连理工大学 | Particle self-reinforced high-entropy amorphous alloy solder for soldering titanium, titanium alloy and stainless steel and preparation method thereof |
| CN116117379B (en) * | 2022-12-30 | 2024-05-03 | 大连理工大学 | Particle self-reinforced high-entropy amorphous alloy solder for soldering titanium, titanium alloy and stainless steel and preparation method thereof |
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