CN108240926A - The preparation method of one Albatra metal multi-component diffusion idol - Google Patents
The preparation method of one Albatra metal multi-component diffusion idol Download PDFInfo
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- CN108240926A CN108240926A CN201611224938.7A CN201611224938A CN108240926A CN 108240926 A CN108240926 A CN 108240926A CN 201611224938 A CN201611224938 A CN 201611224938A CN 108240926 A CN108240926 A CN 108240926A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Abstract
The present invention relates to the preparation methods of an Albatra metal multi-component diffusion idol, belong to investigation of materials method and technical field.First, simple metal to be studied and/or intermediate alloy are subjected to melting and obtain ingot；Then diffusion couple structure is designed；Jacket and jacket lid are made, and ingot is machined to obtain metal parts by mechanical processing using fine copper；Metal parts is surface-treated；Metal parts is assembled to according to diffusion couple structure design in jacket；It is by vacuum electron beam welding, jacket lid and jacket is integrally welded；The outside of jacket and/or jacket lid is machined, the thickness of jacket and/or jacket lid is thinned；Carry out hot isostatic pressing processing；Machine cuts are in blocks and do surface cleaning processing.Using preparation method of the present invention, copper alloy multi-component diffusion idol sample can be efficiently made, easily carries out copper alloy screening and research.The method increase the success rates and the diversity of metal interface in copper alloy multi-component diffusion idol sample preparation.
Description
Technical field
The present invention relates to the preparation methods of an Albatra metal multi-component diffusion idol, belong to investigation of materials method and technical field.
Background technology
With the continuous development of material science, increasingly higher demands are proposed to investigation of materials method.Conventional alloys material
Expect that experimental method is based on " trial-and-error method ", in order to grasp the performance variation law of alloy, need to carry out the discreteness experiment of enormous amount,
Not only it cannot be guaranteed that data complete and the preciseness of experiment, but also expend a large amount of manpower and materials.Develop high pass quantifier elimination
Method has great significance for the development for pushing material science and related industry.
Copper alloy is that Chinese national economy builds indispensable essential industry material, in telecommunications, aerospace, family
The industrial circles such as electrical appliance have a wide range of applications.It is different to the properties of copper alloy under different Service Environments
Requirement.And the main adding elements of copper alloy cover more than ten kinds of Ag, Al, Be etc..Although researcher is to copper alloy
Extensive and deep exploration has been done, due to the limitation of tradition research method, has still not yet established complete related data system,
And then play the role of to the preparation of new material guiding.Using novel copper alloy preparation method of sample, effective acquisition is each
The experimental datas such as phase composition, ingredient and the performance of alloy system, research and development and Related Mechanism problem to Novel copper alloy product
Understanding play an important role.
Invention content
It is an object of the present invention to provide a kind of preparation methods of multi-component diffusion idol, are improved by the preparation of jacket, with common system
Preparation Method is compared, and the success rate of sample preparation can be improved under the premise of metal interface high selectivity is kept, so as to raising section
Learn the efficiency of research.
To achieve these goals, the present invention adopts the following technical scheme that：
The preparation method of copper alloy multi-component diffusion idol of the present invention, preparation include：(1) melting meets the proof gold of scientific research demand
Belong to or intermediate alloy, (2) diffusion couple structure design, (3) component mechanical processing 1, the processing of (4) parts surface, (5) sample assemble
(such as Fig. 1), (6) vacuum electron beam welding, (7) component mechanical processing 2, (8) carry out hot isostatic pressing processing, and (9) dicing is simultaneously
Do surface cleaning processing.
The preparation method of one Albatra metal multi-component diffusion idol, comprises the following specific steps that：
(1) simple metal to be studied and/or intermediate alloy are subjected to melting and obtain ingot；
(2) diffusion couple structure is designed；
(3) jacket and jacket lid are made, and ingot is machined to obtain gold by mechanical processing using fine copper
Belong to component；
(4) metal parts is surface-treated；
(5) metal parts is assembled to according to diffusion couple structure design in jacket；
(6) it is by vacuum electron beam welding, jacket lid and jacket is integrally welded；
(7) outside of jacket and/or jacket lid is machined, the thickness of jacket and/or jacket lid is thinned；
(8) hot isostatic pressing processing is carried out；
(9) machine cuts are in blocks and do surface cleaning processing.
In step (2), in diffusion couple structure design step, the inside and outside contour shape in diffusion couple jacket section includes but not office
It is limited to rectangular, round and polygon etc., jacket internal metal parts have clear interface, and metal parts is deployed with more polynary gold
Belong to interface.
In diffusion couple structure design step, same metal (including copper) component can make in same multi-component diffusion idol sample
With multiple.
In step (3), 1 step is being machined, using fine copper as jacket metal, jacket and packet are made by mechanical processing
Upper shield；Jacket machining shape is the cylinder with inner via hole or jacket machining shape is the square cylinder with inner via hole, the length of side 20
~50mm, 30~80mm of height, jacket wall thickness are not more than 15mm.The inner via hole of jacket is used for other nested metal/alloy blocks, interior
Through-hole cross sectional shape can need to be designed as rectangular, round or polygon according to research.As shown in Figure 1, jacket shape is with rectangular
The cylinder of inner via hole.
Wherein, 1 step is machined, shape and the Outside Dimensions and copper-clad of jacket lid (copper lid) processing cover section outer one
It causes, thickness is 50~200mm；Jacket covers setting boss, the peripheral shape and size of boss and the shape of jacket inner via hole and
Size is consistent, jacket convex platform and the cooperation of jacket hole size；When jacket inner via hole is round, it is convex that jacket covers setting disc-shaped
Platform, boss outer diameter is identical with the aperture of jacket inner via hole, as shown in Fig. 2-1 and Fig. 2-2；When jacket inner via hole is rectangular, jacket
Setting square boss is covered, the square boss length of side is consistent with the copper-clad set inner via hole length of side, plays and is fixed with the coupling card slot of jacket
Effect.Alternatively, jacket covers setting groove, while setting and the matched boss of jacket lid groove size on jacket, outside groove
Diameter is smaller 1~3mm than jacket lid outer diameter, as shown in Fig. 3-1 and Fig. 3-2.The thickness of boss or groove (thick a and Fig. 3 in Fig. 2-1-
High card slot in 1 a) is 2~5mm.
The present invention carries out thickening processing to jacket lid and card slot size, it is preferred that jacket lid thickness is 100~200mm；By
Card slot thickness a=2~5mm caused by jacket lid and peripheral jacket.
It is machined in 1 step, the metal parts of embedded jacket is machined into solid cylindrical block, and diffusion couple component adds
Chinese musical scale cun makes the fitting interface spacing between metal parts be not more than 0.2mm.According to jacket internal via shape and study alloy system
It needs, the shape as shown in (but being not limited to) Fig. 4-1 to Fig. 4-4 can be prepared into, after embedded block is had fully embedded into jacket,
Section morphology is as shown in (but being not limited to) Fig. 4-1 to Fig. 4-4.
In step (6), electron beam welding：Before welding, demagnetization processing is carried out to magnetic metal (such as Ni) first, it is then right
The sample assembled carries out electron beam welding, the outer surface interface ring of copper lid and copper-clad set under vacuum.Welding surroundings are true
Reciprocal of duty cycle should reach 1 × 10-2More than Pa (P welding≤1 × 10-2Pa), in welding process, 2.5~5 circles of sample rotation rate/minute.
After welding, weld seam is should ensure that without leak source, sample inside is in vacuum state.
In step (7), 2 steps are machined, are machined along copper-clad set (including copper lid) is external, to jacket (packet
Include copper lid) it is thinned, so that sample is more suitable for the working processes such as hot isostatic pressing.The size that jacket and/or jacket lid are thinned is it
Thickness 30%~50%.
In step (8), hot isostatic pressing processing：Multi-component diffusion idol sample after electron beam welding is carried out hot isostatic pressing to add
Work, 450~800 DEG C, 100~300MPa of tonnage of processing temperature, 2~8 hours process times.Hot isostatic pressing process
In, a degree of deformation occurs for each component of sample, makes metal parts boundary face good fit, and one occurs between metal interface
Determine the diffusion of degree, make to reach metallurgical binding between metal parts.After hot isostatic pressing processing, the appearance of a sample is completely without cracking, and nothing
Serious torsional deformation.
(9) machine cuts and surface treatment：Examination after hot isostatic pressing is processed using mechanical cutting method (such as wire cutting)
Sample is cut into the small pieces of 2~10mm thickness, is subsequently placed in ethanol/acetone more than technical pure and carries out ultrasonic cleaning 15~20 minutes.
Chemical polishing is carried out, and successively with coarse sandpaper and fine sandpaper to multi-component diffusion idol sheet into specimen surface using appropriate corrosive liquid
The section of sample is polished, and low temperature drying is spare after then being rinsed or cleaned with deionized water and ethyl alcohol successively.
In the present invention, the preparation principle of embedded block size mainly has at 2 points：1. after ensureing nesting, all metal blocks
Good interfacial contact is kept between (including jacket and lid)；Or 2. embed block size (including length, the section length of side or
Radius) can have the error of 0~-0.2mm, you can after making block insertion jacket, fitting spacing between metal parts 0.2mm with
It is interior.
In the present invention, the layout principles of embedded block mainly have at 3 points：1. make the multi-element metal combination interface that generation is more；
2. metal interface clear and definite；3. to meet research needs, same metal (including copper) is in same multi-component diffusion idol sample
It can be used multiple.
The present invention is compared with prior art a kind of more excellent multi-component diffusion idol preparation method, including the excellent spy of the following
Point：
(1) mobility of vacuum electron beam welding：Since gripper typically belongs to tool steel in electron-beam welding equipment
Product belong to ferromagnetism, are easy to cause electron-beam position deviation, and welding seam bias engaging portion can cause welding to fail.To copper in the present invention
Jacket cover board thicken and has been prepared, 50~200mm of thickness, reduces influence of the machined steel pawl to electron beam.It is if each in jacket
Metal parts has compared with ferromagnetism, and after carrying out demagnetization processing, effect unobvious, card slot thickness should also carry out thickening processing, in this way
Even if electron beam, which slightly deviates, has still ensured that good welding effect.
(2) mobility of hot isostatic pressing processing：For the multi-component diffusion idol sample of the present invention after jacket reduction processing, jacket is thick
Degree is uniform, and when hot isostatic pressing can make internal metal parts uniform force, easily reach uniform metallurgical binding.
Description of the drawings
Fig. 1-1 is multi-component diffusion occasionally assembling exemplary plot (A~D is metal parts), and Fig. 1-2 is its cross-sectional view.
Fig. 2-1 is the card slot designing scheme 1 of jacket；Fig. 2-2 is that its cross-sectional view (is above jacket, is jacket below
Lid).
Fig. 3-1 is the card slot designing scheme 2 of jacket；Fig. 3-2 is that its cross-sectional view (is above jacket, is jacket below
Lid).
Fig. 4-1 to Fig. 4-4 is jacket form and metal parts layout designs (A~I is metal parts).
Fig. 5 is embodiment jacket form and metal parts layout designs (A~I is metal parts).
Specific embodiment
It elaborates with reference to the accompanying drawings and examples to the present invention, process and parameter of the present invention include
But it is not limited to following embodiment.
The pure Cu of melting, pure Ni, pure Ti, Cu-20wt.%Sn, Cu-25wt.%Al alloy.Fine copper jacket is machined, such as
Shown in Fig. 3-1 and Fig. 3-2, jacket high 50mm, outer diameter 30mm, indentation, there wall thickness 2mm, inner hole section are rectangular, the length of side
14.14mm, endoporus and jacket section are concentric.Worked copper lid is disc-shaped, and 2, outer diameter 30mm, thick 120mm, copper covers groove
Internal diameter is a height of 3mm of 26mm, groove and jacket indentation, there.
9 pieces of embedded metal block, respectively pure Cu, pure Ni, pure Ti, Cu-25wt.%Al alloy and Cu-20wt.%Sn are closed
Gold is processed as rectangular shape, long 48mm, bottom surface length of side 4.8mm.It is clear that component after processing is placed in ultrasound in ethanol solution
After washing 15 minutes, wiping drying is taken out, chemical polishing 15 seconds is carried out using 80vol.%HCL solution to fine copper component, to pure titanium
Component uses hydrofluoric acid：Concentrated nitric acid：Water=1:3:7 solution carry out chemical polishing 10 seconds, other metal parts are used
50vol.%HNO3Solution carries out chemical polishing 10~30 seconds, is then cleaned successively with deionized water and ethanol solution, and low temperature dries
After dry, metal part surface cleaning is bright.Then jacket and metal parts mode as shown in Figure 1 are assembled, wherein metal
For parts mount position as shown in figure 5, E is pure Cu, A, H are pure Ni, and B, I are pure Ti, and F, G are Cu-20wt.%Sn alloys, and C, D are
Cu-25wt.%Al alloys.Fitting interface spacing between sample is not more than 0.2mm.
True electron beam welding, vacuum degree 1.8 × 10 are carried out after demagnetization processing-3Pa, sample rotation rate 2.5 enclose/minute, and electric current is
20A, sample even weld is without leak source after welding.Then by wire cutting, the cutting of jacket copper lid is thinned to thick 5mm.By sample
It is put into hot isostatic press and carries out hot isostatic pressing processing, 750 DEG C, tonnage 250MPa of processing temperature, 8 hours process times.Heat
After isostatic pressed processing, the appearance of a sample is completely without cracking.After sample completely cooling, sample is prolonged into the circle that radial cuts are 5mm thickness
Piece, jacket inner part reach good metallurgical binding, can obtain polynary even 5, the sample of disk diffusion of not cupric lid.
The method of the present invention prepares copper alloy multi-component diffusion idol by structure design and size regulation and control, and in particular to diffusion couple
Structure design, the layout designs of metal interface and the size design of jacket etc..Multi-component diffusion prepared by this method it is even through heat at
After reason, coordinate high-resolution performance sweep test, the screening design available for Novel copper alloy.It, can using preparation method of the present invention
Efficiently to make copper alloy multi-component diffusion idol sample, copper alloy screening and research are easily carried out.The method increase copper alloys
The diversity of success rate and metal interface in multi-component diffusion idol sample preparation.
Claims (9)
1. the preparation method of an Albatra metal multi-component diffusion idol, comprises the following specific steps that：
(1) simple metal to be studied and/or intermediate alloy are subjected to melting and obtain ingot；
(2) diffusion couple structure is designed；
(3) jacket and jacket lid are made, and ingot is machined to obtain metal portion by mechanical processing using fine copper
Part；
(4) metal parts is surface-treated；
(5) metal parts is assembled to according to diffusion couple structure design in jacket；
(6) it is by vacuum electron beam welding, jacket lid and jacket is integrally welded；
(7) outside of jacket and/or jacket lid is machined, the thickness of jacket and/or jacket lid is thinned；
(8) hot isostatic pressing processing is carried out；
(9) machine cuts are in blocks and do surface cleaning processing.
2. the preparation method of copper alloy multi-component diffusion idol according to claim 1, it is characterised in that：The jacket lid into
Row thickening is handled, and jacket lid thickness is 100~200mm.
3. the preparation method of copper alloy multi-component diffusion idol according to claim 2, it is characterised in that：The jacket covers
Boss is set, and the peripheral shape and size of boss are consistent with the shape and size of jacket inner via hole.
4. the preparation method of copper alloy multi-component diffusion idol according to claim 2, it is characterised in that：The jacket covers
Groove, while setting and the matched boss of jacket lid groove size on jacket are set.
5. the preparation method of copper alloy multi-component diffusion idol according to claim 3 or 4, it is characterised in that：The boss
Or the thickness of groove is 2~5mm.
6. the preparation method of copper alloy multi-component diffusion idol according to claim 1, it is characterised in that：The jacket section
Inside and outside contour shape includes rectangular, round and polygon, has clear interface, metal parts portion between the jacket inner metal component
There is multi-element metal interface in administration.
7. the preparation method of copper alloy multi-component diffusion idol according to claim 1, it is characterised in that：Same metal parts
It can be used in same multi-component diffusion idol sample multiple.
8. the preparation method of copper alloy multi-component diffusion idol according to claim 1, it is characterised in that：It is golden in the jacket
The fitting interface spacing belonged between component is not more than 0.2mm.
9. the preparation method of copper alloy multi-component diffusion idol according to claim 1, it is characterised in that：The jacket and/
Or the size that jacket lid is thinned is the 30%~50% of its thickness.
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| CN201611224938.7A CN108240926B (en) | 2016-12-27 | 2016-12-27 | Preparation method of copper alloy multi-element diffusion couple |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN113189127A (en) * | 2021-04-13 | 2021-07-30 | 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 |
| CN116593259A (en) * | 2023-07-17 | 2023-08-15 | 东北大学 | Copper-titanium diffusion couple and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113189127A (en) * | 2021-04-13 | 2021-07-30 | 昆明贵金属研究所 | Method for preparing high-melting-point metal ternary diffusion couple |
| 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 |
| CN116593259A (en) * | 2023-07-17 | 2023-08-15 | 东北大学 | Copper-titanium diffusion couple and preparation method thereof |
| CN116593259B (en) * | 2023-07-17 | 2023-09-26 | 东北大学 | Copper-titanium diffusion couple and preparation method thereof |
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