CN108240926B - Preparation method of copper alloy multi-element diffusion couple - Google Patents
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- CN108240926B CN108240926B CN201611224938.7A CN201611224938A CN108240926B CN 108240926 B CN108240926 B CN 108240926B CN 201611224938 A CN201611224938 A CN 201611224938A CN 108240926 B CN108240926 B CN 108240926B
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Abstract
The invention relates to a preparation method of a copper alloy multi-element diffusion couple, belonging to the field of material research methods and technologies. Firstly, smelting pure metal and/or intermediate alloy to be researched to obtain a metal ingot; then designing a diffusion couple structure; manufacturing a sheath and a sheath cover by machining pure copper, and machining a metal ingot to obtain a metal part; carrying out surface treatment on the metal part; assembling the metal part into the sheath according to the diffusion couple structure design; welding the sheath cover and the sheath into a whole through vacuum electron beam welding; machining the outer part of the sheath and/or the sheath cover to reduce the thickness of the sheath and/or the sheath cover; carrying out hot isostatic pressing; mechanically cutting into pieces and performing surface cleaning treatment. By adopting the preparation method, the copper alloy multi-element diffusion couple sample can be efficiently manufactured, and copper alloy screening and research can be conveniently carried out. The method improves the success rate and the diversity of metal interfaces in the preparation process of the copper alloy multi-element diffusion couple sample.
Description
Technical Field
The invention relates to a preparation method of a copper alloy multi-element diffusion couple, belonging to the field of material research methods and technologies.
Background
With the continuous development of material science, higher and higher requirements are put forward on a material research method. The traditional alloy material experimental method is based on a trial-and-error method, and in order to master the performance change rule of the alloy, a huge amount of discrete experiments need to be carried out, so that the completeness of data and the rigor of the experiments cannot be guaranteed, and a large amount of manpower and material resources are consumed. The development of high-throughput research methods is of great significance in promoting the development of material science and related industries.
The copper alloy is an indispensable important industrial material for national economic construction in China, and has wide application in the industrial fields of electronic communication, aerospace, household appliances and the like. Under different service environments, different requirements are made on various properties of the copper alloy. The main additive elements of the copper alloy comprise more than ten elements such as Ag, Al, Be and the like. Although researchers have conducted extensive and intensive research on copper alloys, due to the limitations of the conventional research methods, a complete and relevant data system has not yet been established, thereby providing guidance for the preparation of novel materials. By utilizing the novel copper alloy sample preparation method, experimental data such as phase composition, components and performance of each alloy system can be efficiently obtained, and the method plays an important role in research and development of novel copper alloy products and understanding of related mechanism problems.
Disclosure of Invention
The invention aims to provide a preparation method of a multi-element diffusion couple, which can improve the success rate of sample preparation on the premise of keeping high metal interface selectivity by the preparation improvement of a sheath compared with the common preparation method, thereby improving the efficiency of scientific research.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the copper alloy multi-element diffusion couple comprises the following steps: (1) smelting pure metal or intermediate alloy meeting scientific research requirements, (2) designing a diffusion couple structure, (3) machining a part 1, (4) treating the surface of the part, (5) assembling a sample (shown in figure 1), (6) welding a vacuum electron beam, (7) machining the part 2, (8) performing hot isostatic pressing, and (9) cutting into pieces and performing surface cleaning treatment.
A preparation method of a copper alloy multi-element diffusion couple comprises the following specific steps:
(1) smelting pure metal and/or intermediate alloy to be researched to obtain a metal ingot;
(2) designing a diffusion couple structure;
(3) manufacturing a sheath and a sheath cover by machining pure copper, and machining a metal ingot to obtain a metal part;
(4) carrying out surface treatment on the metal part;
(5) assembling the metal part into the sheath according to the diffusion couple structure design;
(6) welding the sheath cover and the sheath into a whole through vacuum electron beam welding;
(7) machining the outer part of the sheath and/or the sheath cover to reduce the thickness of the sheath and/or the sheath cover;
(8) carrying out hot isostatic pressing;
(9) mechanically cutting into pieces and performing surface cleaning treatment.
In the step (2), in the diffusion couple structure design step, the shapes of the inner and outer contours of the cross section of the diffusion couple sheath include but are not limited to square, round, polygon and the like, the metal parts in the sheath have clear interfaces, and the metal parts are provided with more multi-metal interfaces.
The same metal (including copper) component can be used multiple times in the same multiplex diffusion couple sample during the diffusion couple structure design step.
In the step (3), in the step (1) of mechanical processing, pure copper is used as sheath metal, and a sheath cover are manufactured through mechanical processing; the processing shape of the sheath is a cylinder with an inner through hole, or the processing shape of the sheath is a square cylinder with an inner through hole, the side length is 20-50 mm, the height is 30-80 mm, and the wall thickness of the sheath is not more than 15 mm. The inner through hole of the sheath is used for nesting other metal/alloy blocks, and the cross section of the inner through hole can be designed to be square, circular or polygonal according to research needs. As shown in fig. 1, the sheath is in the shape of a cylinder with a square inner through hole.
Wherein, in the step of machining 1, the shape and the peripheral dimension of a sheath cover (copper cover) are consistent with the outer edge of the cross section of the copper sheath, and the thickness is 50-200 mm; the sheath cover is provided with a boss, the peripheral shape and size of the boss are consistent with those of the through hole in the sheath, and the boss on the sheath is matched with the inner hole of the sheath in size; when the through hole in the sheath is circular, a disk-shaped boss is arranged on the sheath cover, and the outer diameter of the boss is the same as the aperture of the through hole in the sheath, as shown in figures 2-1 and 2-2; when the through hole in the sheath is square, the sheath is covered by a square boss, and the side length of the square boss is consistent with that of the through hole in the copper-clad sheath, so that the square boss and the coupling clamping groove of the sheath are fixed. Or, the sheath cover is provided with a groove, the sheath is provided with a boss matched with the groove of the sheath cover in size, and the outer diameter of the groove is 1-3 mm smaller than that of the sheath cover, as shown in figures 3-1 and 3-2. The thickness (the thickness a in figure 2-1 and the height a of the clamping groove in figure 3-1) of the lug boss or the groove is 2-5 mm.
According to the invention, the sizes of the sheath cover and the clamping groove are thickened, preferably, the thickness of the sheath cover is 100-200 mm; the thickness a of the clamping groove caused by the sheathing cover and the peripheral sheathing is 2-5 mm.
In the step of machining 1, the metal parts embedded into the sheath are machined into solid columnar blocks, and the machining size of the diffusion couple parts enables the joint interface distance between the metal parts to be not more than 0.2 mm. According to the shape of the inner hole of the sheath and the requirement of researching an alloy system, the shape can be prepared as shown in (but not limited to) figures 4-1 to 4-4, and the section shape of the inner embedded block body is shown in (but not limited to) figures 4-1 to 4-4 after the inner embedded block body is completely embedded in the sheath.
In the step (6), electron beam welding: before welding, firstly, demagnetizing the magnetic metal (such as Ni), and then carrying out electron beam welding on the assembled sample under the vacuum condition, wherein the interface between the copper cover and the outer surface of the copper sheath is annular. The vacuum degree of the welding environment should reach 1 x 10-2Pa or more (P welding is less than or equal to 1X 10)-2Pa), and in the welding process, the rotating speed of the sample is 2.5-5 circles/minute. After welding, the welding seam is ensured to have no leakage point, and the interior of the sample is in a vacuum state.
In the step (7), the machining step 2 is to perform machining along the outside of the copper clad (including the copper cover) and thin the clad (including the copper cover) so that the sample is more suitable for processing treatment such as hot isostatic pressing and the like. The size of the capsule and/or the capsule cover is reduced to 30-50% of the thickness of the capsule and/or the capsule cover.
In the step (8), hot isostatic pressing: and carrying out hot isostatic pressing on the electron beam welded multi-element diffusion couple sample at the processing temperature of 450-800 ℃, at the processing pressure of 100-300 MPa, and for 2-8 hours. In the hot isostatic pressing process, each part of the sample deforms to a certain degree, so that the interfaces between the metal parts are well jointed, and the metal interfaces diffuse to a certain degree, so that the metal parts are metallurgically bonded. After hot isostatic pressing, the appearance of the sample is complete without cracking and severe distortion.
(9) Mechanical cutting and surface treatment: and cutting the sample subjected to hot isostatic pressing into small pieces with the thickness of 2-10 mm by adopting a mechanical cutting method (such as linear cutting), and then placing the small pieces in ethanol/acetone with industrial purity for ultrasonic cleaning for 15-20 minutes. Using proper corrosive liquid to enter the surface of the test sample for chemical polishing, sequentially using coarse sand paper and fine sand paper to polish the section of the multi-element diffusion even-sheet test sample, and then sequentially washing with deionized water and ethanol or cleaning and then drying at low temperature for later use.
In the invention, the preparation principle of the size of the embedded block mainly comprises two points: firstly, good interface contact is kept among all metal blocks (including a sheath and a cover) after nesting; or the size (including length, section side length or radius) of the embedded block body can have an error of 0-0.2 mm, so that after the block body is embedded into the sheath, the joint distance between the metal parts is within 0.2 mm.
In the invention, the layout principle of the embedded block body mainly comprises three points: firstly, generating more multi-element metal bonding interfaces; secondly, the metal interface is clear and definite; and thirdly, in order to meet the research requirement, the same metal (including copper) can be used for many times in the same multi-element diffusion couple sample.
Compared with the prior art, the invention is a better preparation method of the multi-element diffusion couple, and has the following excellent characteristics:
(1) ease of vacuum electron beam welding: since the mechanical claw in the electron beam welding equipment is generally ferromagnetic in tool steel products, the position of the electron beam is easy to deviate, and the deviation of the welding seam from the joint can cause welding failure. According to the invention, the copper-clad sleeve cover plate is thickened and prepared, the thickness is 50-200 mm, and the influence of a mechanical steel claw on an electron beam is reduced. If each metal part in the sheath has stronger magnetism, after degaussing treatment, the effect is not obvious, and the thickness of the clamping groove is thickened, so that good welding effect can be ensured even if the electron beam slightly deviates.
(2) Ease of hot isostatic pressing: after the multi-element diffusion couple sample is subjected to sheath thinning treatment, the sheath thickness is uniform, and internal metal parts can be uniformly stressed during hot isostatic pressing, so that uniform metallurgical bonding can be easily achieved.
Drawings
FIG. 1-1 is a view showing an example of the assembly of a multi-element diffusion couple (A to D are metal members), and FIG. 1-2 is a cross-sectional view thereof.
FIG. 2-1 shows a neck design 1 of the jacket; fig. 2-2 is a cross-sectional view thereof (jacket on top and cover on bottom).
FIG. 3-1 shows a neck design 2 of the jacket; fig. 3-2 is a cross-sectional view thereof (jacket on top and cover on bottom).
FIGS. 4-1 to 4-4 show the sheath shape and the layout of the metal parts (A-I are metal parts).
FIG. 5 shows the sheath morphology and the layout design of the metal parts (A-I are metal parts) according to the embodiment.
Detailed Description
The invention is described in detail below with reference to the drawings and examples, and the process methods and parameters related to the invention include, but are not limited to, the following examples.
Smelting pure Cu, pure Ni, pure Ti, Cu-20 wt.% Sn and Cu-25 wt.% Al alloy. Machining a pure copper sheath, as shown in figures 3-1 and 3-2, wherein the sheath is 50mm high, 30mm in outer diameter, 2mm in wall thickness at the notch, and is square in inner hole section with side length of 14.14mm, and the inner hole is concentric with the sheath section. The processed copper covers are 2 in a wafer shape, the outer diameter of the copper covers is 30mm, the thickness of the copper covers is 120mm, the inner diameter of a groove in the copper cover is 26mm, and the height of the groove and the gap of the sheath is 3 mm.
The embedded metal block 9 is respectively pure Cu, pure Ni, pure Ti, Cu-25 wt.% Al alloy and Cu-20 wt.% Sn alloy, and is processed into a cuboid shape with the length of 48mm and the bottom side length of 4.8 mm. Placing the processed part in an ethanol solution for ultrasonic cleaning for 15 minutes, taking out, wiping and drying, performing chemical polishing on the pure copper part for 15 seconds by adopting 80 vol.% HCl solution, and performing ultrasonic cleaning on the pure titanium part by adopting hydrofluoric acid: concentrated nitric acid: chemical polishing of the 1:3:7 water solution for 10 seconds with 50 vol.% HNO for the other metal parts3And chemically polishing the solution for 10-30 seconds, then sequentially cleaning the solution by using deionized water and ethanol solution, and drying the solution at a low temperature to clean and brighten the surface of the metal part. The capsule and the metal parts are then assembled as shown in fig. 1, where the metal parts are mounted as shown in fig. 5, E is pure Cu,A. h is pure Ni, B, I is pure Ti, F, G is Cu-20 wt.% Sn alloy, C, D is Cu-25 wt.% Al alloy. The distance between the fit interfaces of the samples is not more than 0.2 mm.
After degaussing treatment, vacuum electron beam welding is carried out, and the vacuum degree is 1.8 multiplied by 10-3Pa, the rotating speed of the sample is 2.5 circles/minute, the current is 20A, and the welded seam of the sample is uniform and has no leak points. And then cutting and thinning the sheath copper cover to 5mm in thickness by wire cutting. And (3) putting the sample into a hot isostatic pressing machine for hot isostatic pressing, wherein the processing temperature is 750 ℃, the processing pressure is 250MPa, and the processing time is 8 hours. After hot isostatic pressing, the appearance of the sample is complete and no crack exists. After the sample is completely cooled, the sample is radially cut into 5 mm-thick wafers, the parts in the sheath can achieve good metallurgical bonding, and 5 wafers of the wafer diffusion multi-couple sample without the copper cover can be obtained.
The method prepares the copper alloy multi-element diffusion couple through structural design and size regulation, and particularly relates to the structural design of the diffusion couple, the layout design of a metal interface, the size design of a sheath and the like. The multielement diffusion couple prepared by the method can be used for screening design of novel copper alloy by matching with a high-resolution performance scanning test after heat treatment. By adopting the preparation method, the copper alloy multi-element diffusion couple sample can be efficiently manufactured, and copper alloy screening and research can be conveniently carried out. The method improves the success rate and the diversity of metal interfaces in the preparation process of the copper alloy multi-element diffusion couple sample.
Claims (6)
1. A preparation method of a copper alloy multi-element diffusion couple comprises the following specific steps:
(1) smelting pure metal and/or intermediate alloy to be researched to obtain a metal ingot;
(2) designing a diffusion couple structure;
(3) manufacturing a sheath and a sheath cover by machining pure copper, and machining a metal ingot to obtain a metal part; thickening the sheath cover, wherein the thickness of the sheath cover is 100-200 mm;
(4) carrying out surface treatment on the metal part;
(5) assembling the metal part into the sheath according to the diffusion couple structure design; the joint interface distance between the metal components in the sheath is not more than 0.2 mm;
(6) welding the sheath cover and the sheath into a whole through vacuum electron beam welding;
(7) machining the outer part of the sheath and/or the sheath cover to reduce the thickness of the sheath and/or the sheath cover, wherein the reduced size of the sheath and/or the sheath cover is 30% -50% of the thickness of the sheath and/or the sheath cover; (8) carrying out hot isostatic pressing;
(9) mechanically cutting into pieces and performing surface cleaning treatment.
2. The method for preparing the copper alloy multi-element diffusion couple according to claim 1, wherein: the sheath cover is provided with a boss, and the shape and the size of the periphery of the boss are consistent with those of the through hole in the sheath.
3. The method for preparing the copper alloy multi-element diffusion couple according to claim 1, wherein: the sheath cover is provided with a groove, and meanwhile, the sheath is provided with a boss matched with the groove of the sheath cover in size.
4. The method for preparing a copper alloy multi-element diffusion couple according to claim 2 or 3, wherein: the thickness of the boss or the groove is 2-5 mm.
5. The method for preparing the copper alloy multi-element diffusion couple according to claim 1, wherein: the shapes of the inner contour and the outer contour of the sheath section comprise a square shape, a circular shape and a polygonal shape, clear interfaces are arranged among metal components in the sheath, and the metal components are provided with multi-metal interfaces.
6. The method for preparing the copper alloy multi-element diffusion couple according to claim 1, wherein: the same metal part can be used multiple times in the same multi-element diffusion couple sample.
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| CN109773428A (en) * | 2019-02-26 | 2019-05-21 | 北京航空航天大学 | A method of the iron-base superalloy annular element with internal feature connects Kufil |
| CN111721791A (en) * | 2019-08-30 | 2020-09-29 | 中南大学 | High-throughput alloy preparation, characterization and component design method |
| CN113189127B (en) * | 2021-04-13 | 2023-01-24 | 昆明贵金属研究所 | Method for preparing high-melting-point metal ternary diffusion couple |
| CN113899603A (en) * | 2021-09-16 | 2022-01-07 | 贵研铂业股份有限公司 | Method for preparing diffusion couple by hole type rolling mill |
| CN116593259B (en) * | 2023-07-17 | 2023-09-26 | 东北大学 | Copper-titanium diffusion couple and preparation method thereof |
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| CN105787144B (en) * | 2014-12-26 | 2019-02-05 | 北京有色金属研究总院 | A kind of design of material method of elastic copper alloy |
| CN106181250B (en) * | 2016-08-05 | 2018-07-03 | 航天材料及工艺研究所 | Xenogenesis composite component hot isostatic pressing diffusion connection preparation method |
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