CN104451487B - Method for preparing copper alloy nanometer gradient material - Google Patents
Method for preparing copper alloy nanometer gradient material Download PDFInfo
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- CN104451487B CN104451487B CN201410656185.1A CN201410656185A CN104451487B CN 104451487 B CN104451487 B CN 104451487B CN 201410656185 A CN201410656185 A CN 201410656185A CN 104451487 B CN104451487 B CN 104451487B
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- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910017777 Cu—Al—Zn Inorganic materials 0.000 claims abstract description 26
- 238000000137 annealing Methods 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 6
- 239000010959 steel Substances 0.000 claims abstract description 6
- 238000005266 casting Methods 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 239000010949 copper Substances 0.000 abstract description 12
- 239000000956 alloy Substances 0.000 abstract description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052802 copper Inorganic materials 0.000 abstract description 8
- 239000007769 metal material Substances 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract 1
- 230000003116 impacting effect Effects 0.000 abstract 1
- 238000003754 machining Methods 0.000 abstract 1
- 238000007709 nanocrystallization Methods 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 239000002707 nanocrystalline material Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005480 shot peening Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/04—Alloys based on copper with zinc as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metal Rolling (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
Abstract
The invention discloses a method for preparing a copper alloy nanometer gradient material, and belongs to the technical field of metal material machining. The method comprises the following steps: carrying out vacuum homogenizing annealing on a Cu-Al-Zn ternary copper alloy ingot at the temperature of 800-840 DEG C for 2-3 hours, and rolling into a thin plate at room temperature; then carrying out destressing and homogenizing annealing at the temperature of 550-600 DEG C for 2-3 hours, and cooling with a furnace; impacting an annealed copper plate of the Cu-Al-Zn ternary copper alloy at a high speed by using a steel ball on a surface nanocrystallization testing machine with liquid nitrogen introduced to prepare the nanometer gradient copper alloy material, wherein the testing frequency of the testing machine is 20-50 HZ, and the time is 5-30 minutes. The method disclosed by the invention is simple in preparation process and can obtain the copper alloy gradient material which is obviously enhanced in strength and less reduced in property and has good toughness matching.
Description
Technical field
The present invention relates to the preparation method of an Albatra metal nanometer gradient material, belongs to metal material processing technical field.
Background technology
Materials microstructure structure directly affects the performance of material, in order to meet Service Environment to material property (such as
Intensity, hardness, fretting wear, corrosion and fatigue life-span and stress distribution etc.) specific demand, people propose various tables in succession
Face modification technology, such as shot-peening, plating, spraying, vapour deposition (PVD, CVD), ion implanting, surface laser process and surface
Chemical treatment etc..These technologies drastically increase the military service behavior of material by improving the organizational structure of material surface, because
This industrially achieves and is widely applied.With deepening continuously for nano material and nanotechnology research, by traditional table
Face modification technology is combined to be possible to provide one for the nanorize for realizing engineering metal material with nano fabrication technique and new is sent out
Exhibition direction.
At past more than 20 years, the research Showed Very Brisk of nano material and nanotechnology, this is primarily due to a nanometer material
Material with unique structure and excellent performance, not only further deepened people and solid material essence tied by research nano material
The understanding of structure feature, while also providing material and technical foundation for the design of high performance material of new generation, exploitation.It is so far
Only, people have developed various preparation method of nano material, such as evaporation of metal condensation-cold moudling method in situ, Amorphous Crystallization
Method, mechanical milling method and intense plastic strain method etc..But, due to complicated process of preparation, production cost height and material profile chi
The restriction of the factor such as very little limited, internal Presence of an interface pollution, hole class defect be more, existing technology of preparing are also failed in engineering gold
Practical application is obtained on category material.
Under arms under environment, the unstability of metal material, starting from surface, as long as therefore certain thickness is prepared on material more
Nanostructured surface laye, form functionally gradient material (FGM) with center portion gradual change, it is possible to by the complementary excellent of surface to core structure and performance
Change the overall performance and military service behavior for improving material.Making Nano surface technology and making Nano surface material have many unique distinctions：
First, making Nano surface is capable of achieving using Conventional surface treatment (or being improved to Conventional surface treatment),
There is no obvious technology barrier in industrially application；Secondly, do not exist substantially between the brilliant tissue of nano surface and matrix
Interface, delamination and separation will not occur；3rd, making Nano surface is not only suitable for the table that is overall, can be used for local again of material
Face is modified.As making Nano surface had not only been conceived to current scientific and technological level but also towards practical engineering application, it is therefore possible to
Performance and used life for Traditional project metal material is significantly improved using nanotechnology provides a practicable way
Footpath.
Copper has excellent characteristic, is industrially used widely, but the intensity of copper and hardness are all very low, and some are important
Occasion be difficult with, after adding other alloying element solution strengthening or second-phase strength, its intensity can be improved；By big plasticity
Preparing super fine crystal material, super fine crystal material due to effectively hindering the fortune of dislocation with substantial amounts of crystal boundary for the method for deformation
It is dynamic, intensity can be improved；But for the block body ultrafine grain or nanocrystalline material of the preparation of big plasticity, plasticity is relatively low, becomes which in work
The obstacle applied in industry.
In order to solve the shortcoming of above prior art, all good Cu alloy material of intensity and plasticity is obtained, the present invention is adopted
Specimen surface is clashed into using high speed small ball under the vacuum environment for leading to liquid nitrogen on making Nano surface of metal material testing machine, closing
Gold prepares Ultra-fine Grained nanometer gradient material, and top layer has high intensity, hardness, and center portion has higher toughness.Grain structure
With the change of stress gradient, make this material that there is excellent plasticity and intensity.
The content of the invention
The present invention is that the surface high energy that high strain rate is carried out to copper alloy plate hits under the vacuum low-temperature environment of logical liquid nitrogen
Process is hit, and one layer of stable Ultra-fine Grained nanometer gradient material is formed on copper alloy plate surface, so as to prepare the copper of high-strength tenacity
The method of alloy functionally gradient material (FGM), specifically includes following steps：
（1）By casting Cu-Al-Zn ternary copper-alloys ingot casting out, vacuum homogenization is moved back at a temperature of 800 ~ 840 DEG C
Fire 2 ~ 3 hours, is then rolled into thickness for 3mm ~ 4.5mm thin plates, then stress relief annealing 2 ~ 3 is little at a temperature of 550 ~ 600 DEG C
When；
（2）By step under the vacuum environment of logical liquid nitrogen（1）The middle thin plate for processing is used on making Nano surface testing machine
The steel ball of 160 ~ 200 a diameter of 6 ~ 8mm carries out high-speed impact 5 ~ 30min of deformation process and prepares copper alloy nanometer gradient material
Material.
Step of the present invention（2）Described in collision deformation processing procedure completed using making Nano surface testing machine, testing machine
Operating frequency is 20Hz ~ 50Hz.
The invention has the beneficial effects as follows：
（1）The present invention combines the copper of the method acquisition high-strength tenacity of traditional annealing process and surface fierceness plastic deformation and closes
Gold nano functionally gradient material (FGM), preparation method are simple；
（2）The copper alloy functionally gradient material (FGM) that the method for the invention is obtained with from surface to core structure and stress gradient
The characteristics of distribution, the high-ductility of the high intensity and center portion on top layer, realize the good fit of obdurability；
（3）Fund input low cost of the present invention, easily realizes industrialization production, and product quality is stable.
Description of the drawings
Fig. 1 is the stress strain curve of the Cu-Al-Zn ternary copper-alloys that embodiment 1 ~ 2 is prepared；
Fig. 2 is the stress strain curve of the Cu-Al-Zn ternary copper-alloys that embodiment 3 ~ 4 is prepared；
Fig. 3 is the microhardness curve of the Cu-Al-Zn ternary copper-alloys that embodiment 1 ~ 2 is prepared.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described, but protection scope of the present invention is simultaneously
It is not limited to the content.
Embodiment 1（Contrast test）
The concrete composition of Cu-Al-Zn described in the present embodiment is the mass percent of the mass percent for 81.20%, Al of Cu
Mass percent for 4.50%, Zn is 14.30%.
By the ingot casting of the casting a diameter of 30mm of Cu-Al-Zn ternary copper-alloys out, vacuum is uniform at a temperature of 840 DEG C
Annealing 2 hours, is then rolled into thin plate at room temperature, then stress relief annealing is prepared for 2 hours at a temperature of 600 DEG C
Cu-Al-Zn ternary copper-alloy materials.
The Cu-Al-Zn ternary copper-alloys material that this example is prepared does not carry out making Nano surface, tensile yield strength
For 106.6MPa, tensile strength is 378.4 MPa, and maximum strain is 67.7%.
Embodiment 2
The concrete composition of Cu-Al-Zn described in the present embodiment is the mass percent of the mass percent for 81.20%, Al of Cu
Mass percent for 4.50%, Zn is 14.30%.
（1）By the ingot casting of the casting a diameter of 30mm of Cu-Al-Zn ternary copper-alloys out at a temperature of 840 DEG C vacuum
Homogenizing annealing 2 hours, is then rolled into thin plate at room temperature, then stress relief annealing 2 hours at a temperature of 600 DEG C；
（2）On making Nano surface testing machine（Under the vacuum environment of logical liquid nitrogen）With 180 steel balls（6mm）Respectively to copper coin
Two surfaces carry out collision deformation and process the Cu-Al-Zn ternary copper-alloy materials for preparing, and test unit frequency is 20 ~ 50HZ,
Test period is 5 ~ 30min.
It is 247.6MPa for the tensile yield strength of the sample of 5min when the making Nano surface time, tensile strength is
391.3MPa, maximum strain are 62.6%；The making Nano surface time is 290.4MPa for the tensile yield strength of the sample of 15min,
Tensile strength is 411.2MPa, and maximum strain is 54.8%；Tensile yield strength of the making Nano surface time for the sample of 30min
For 290.4MPa, tensile yield strength is 266.2MPa, and tensile strength is 338.0MPa, and maximum strain is 52.8%.
Embodiment 3
The concrete composition of Cu-Al-Zn described in the present embodiment is the mass percent of the mass percent for 74.25%, Al of Cu
Mass percent for 1.86%, Zn is 23.89%.
（1）By the ingot casting of the casting a diameter of 30mm of Cu-Al-Zn ternary copper-alloys out at a temperature of 800 DEG C vacuum
Homogenizing annealing 3 hours, is then rolled into thin plate at room temperature, then stress relief annealing 3 hours at a temperature of 550 DEG C；
（2）On making Nano surface testing machine（Under the vacuum environment of logical liquid nitrogen）With 200 steel balls（8mm）Respectively to copper coin
Two surfaces carry out collision deformation and process the Cu-Al-Zn ternary copper-alloy materials for preparing, and test unit frequency is 50HZ, is tried
The time is tested for 30min.
The Cu-Al-Zn that the present embodiment for the Cu-Al-Zn ternary copper-alloy materials that the present embodiment is prepared is prepared
The tensile yield strength of ternary copper-alloy material is 266.2MPa, and tensile strength is 338.0MPa, and maximum strain is 52.8%.
Embodiment 4
The concrete composition of Cu-Al-Zn described in the present embodiment is the mass percent of the mass percent for 74.25%, Al of Cu
Mass percent for 1.86%, Zn is 23.89%.
（1）By the ingot casting of the casting a diameter of 30mm of Cu-Al-Zn ternary copper-alloys out at a temperature of 820 DEG C vacuum
Homogenizing annealing 1.5 hours, is then rolled into thin plate at room temperature, then stress relief annealing 2.5 hours at a temperature of 580 DEG C；
（2）On making Nano surface testing machine（Under the vacuum environment of logical liquid nitrogen）With 180 steel balls（7mm）Respectively to copper coin
Two surfaces carry out collision deformation and process the Cu-Al-Zn ternary copper-alloy materials for preparing, and test unit frequency is 30HZ, is tried
The time is tested for 5 ~ 30min.
The making Nano surface time is 226.7MPa for the tensile yield strength of the sample of 5min, and tensile strength is
357.5MPa, maximum strain are 57.6%；The making Nano surface time is 280.9MPa for the tensile yield strength of the sample of 15min,
Tensile strength is 364.6MPa, and maximum strain is 43.7%；Tensile yield strength of the making Nano surface time for the sample of 30min
For 319.5MPa, tensile strength is 385.8MPa, and maximum strain is 40.3%.
Fig. 1 is the Cu-Al- that the composition that embodiment 1 ~ 2 is prepared is 81.20%Cu-4.50%Al-14.30%Zn (wt.%)
The stress strain curve of Zn ternary copper-alloys；Preferably, intensity is worst, by nano surface for the plasticity of annealed state sample as seen from the figure
After change is processed, intensity is significantly improved, and plasticity is slightly reduced, and is increased with the making Nano surface time, and intensity continuous increase, and plasticity is held
It is continuous to reduce, but certain hour is arrived, the change of plasticity is with regard to little, the sample and making Nano surface 15min of making Nano surface 30min
Sample maximum strain value difference very little, intensity is also improved space.
Fig. 2 is the Cu-Al- that the composition that embodiment 3 ~ 4 is prepared is 74.25%Cu-1.86%Al-23.89%Zn (wt.%)
The stress strain curve of Zn ternary copper-alloys, is contrasted with Fig. 1 and also have identical rule.
Can be seen that this preparation method can significantly improve the intensity of Cu-Al-Zn ternary copper-alloys by Fig. 1 and Fig. 2, and
High plasticity is kept again.
Fig. 3 is the microhardness curve of the Cu-Al-Zn ternary copper-alloys that embodiment 1 ~ 2 is prepared, as seen from the figure
Annealing sample is from top layer to center portion microhardness difference less than the Cu-Al-Zn ternary copper-alloys crossed through Surface Nanocrystalline are tried
Sample surface layer microhardness highest, walks toward material center portion, and hardness is gradually lowered, and is minimum to center portion；Increase with the making Nano surface time
Plus, the degree of crystal grain refinement and depth increase, and hardness is improved；Annealing Cu-Al-Zn ternary copper-alloy microhardness values be
1.1GPa, the sample surface layer microhardness value after Surface Nanocrystalline 30min can reach 2.2GPa, double.
Claims (1)
1. the preparation method of an Albatra metal nanometer gradient material, it is characterised in that specifically include following steps：
（1）By casting copper alloy casting ingot out homogenizing annealing under vacuo, thin plate is then rolled into, then thin plate is carried out
Destressing, homogenizing annealing；
（2）By step（1）The middle thin plate for processing is on making Nano surface testing machine with the steel of 160 ~ 200 a diameter of 6 ~ 8mm
Ball carries out high-speed impact 5 ~ 30min of deformation process and prepares copper alloy nanometer gradient material；
Step（1）Described in gauge of sheet be 3mm ~ 4.5mm；
Step（1）Described in copper alloy be Cu-Al-Zn ternary copper-alloys；
Step（2）Described in high-speed impact deformation process carry out under the vacuum environment of logical liquid nitrogen；
Step（2）Described in making Nano surface testing machine test frequency be 20 ~ 50HZ；
Step（1）Described in ingot casting annealing annealing temperature be 800 ~ 840 DEG C, annealing time be 2 ~ 3h, the thin plate
The annealing temperature of annealing is 550 ~ 600 DEG C, and annealing time is 2 ~ 3h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410656185.1A CN104451487B (en) | 2014-11-18 | 2014-11-18 | Method for preparing copper alloy nanometer gradient material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410656185.1A CN104451487B (en) | 2014-11-18 | 2014-11-18 | Method for preparing copper alloy nanometer gradient material |
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| CN104451487A CN104451487A (en) | 2015-03-25 |
| CN104451487B true CN104451487B (en) | 2017-04-12 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104947013B (en) * | 2015-05-26 | 2016-12-07 | 昆明理工大学 | A kind of preparation method of double-deck gradient sphere grinding making Nano surface copper rod |
| CN105177645B (en) * | 2015-07-27 | 2017-05-31 | 昆明理工大学 | A kind of preparation method of MULTILAYER COMPOSITE gradient nano pure copper material |
| CN107299302B (en) * | 2016-04-15 | 2020-02-28 | 南京理工大学 | Method for improving metal gradient structure strength and plasticity matching degree |
| CN108517477B (en) * | 2018-04-16 | 2020-10-23 | 中国兵器工业第五九研究所 | Deep conical copper liner tissue superfine grain gradient control method |
| CN115627378A (en) * | 2022-10-19 | 2023-01-20 | 昆明理工大学 | Preparation method of Cu-Al-Zn alloy material |
| CN116213751A (en) * | 2022-12-13 | 2023-06-06 | 浙江大学 | 316L stainless steel surface treatment method |
| CN116516268A (en) * | 2023-04-14 | 2023-08-01 | 常熟市普华电工材料有限公司 | Alloy copper wire annealing process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392359A (en) * | 2008-11-07 | 2009-03-25 | 昆明理工大学 | Method for preparing high tension and high conductive pure copper material |
| CN101392358A (en) * | 2008-11-07 | 2009-03-25 | 昆明理工大学 | Method for preparing high tension pure copper by using high deformation speed |
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| JP2000256814A (en) * | 1999-03-03 | 2000-09-19 | Sumitomo Metal Mining Co Ltd | Manufacture of copper-based alloy bar for terminal |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392359A (en) * | 2008-11-07 | 2009-03-25 | 昆明理工大学 | Method for preparing high tension and high conductive pure copper material |
| CN101392358A (en) * | 2008-11-07 | 2009-03-25 | 昆明理工大学 | Method for preparing high tension pure copper by using high deformation speed |
Non-Patent Citations (1)
| Title |
|---|
| Friction and wear behaviors of nanocrystalline surface layer of pure copper;Y.S.Zhang, Z.Han, K.Wang, K.Lu;《Wear》;20050725;942-948 * |
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