CN117265321A - Copper-silver-zirconium alloy and preparation method and application thereof - Google Patents
Copper-silver-zirconium alloy and preparation method and application thereof Download PDFInfo
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- CN117265321A CN117265321A CN202311270918.3A CN202311270918A CN117265321A CN 117265321 A CN117265321 A CN 117265321A CN 202311270918 A CN202311270918 A CN 202311270918A CN 117265321 A CN117265321 A CN 117265321A
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- 229910001093 Zr alloy Inorganic materials 0.000 title claims abstract description 57
- UQRBYHQTQUAYQZ-UHFFFAOYSA-N copper silver zirconium Chemical compound [Cu][Ag][Zr] UQRBYHQTQUAYQZ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000956 alloy Substances 0.000 claims abstract description 86
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 84
- 238000010438 heat treatment Methods 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 41
- 238000005242 forging Methods 0.000 claims abstract description 37
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000000889 atomisation Methods 0.000 claims abstract description 32
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 32
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 28
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 27
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 22
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 21
- 230000008018 melting Effects 0.000 claims abstract description 21
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- 239000010949 copper Substances 0.000 claims abstract description 20
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 20
- 229910052709 silver Inorganic materials 0.000 claims abstract description 18
- 239000004332 silver Substances 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000011282 treatment Methods 0.000 claims abstract description 13
- 238000000280 densification Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 64
- 238000000034 method Methods 0.000 claims description 38
- 229910052786 argon Inorganic materials 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 17
- XTYUEDCPRIMJNG-UHFFFAOYSA-N copper zirconium Chemical compound [Cu].[Zr] XTYUEDCPRIMJNG-UHFFFAOYSA-N 0.000 claims description 10
- SKEYZPJKRDZMJG-UHFFFAOYSA-N cerium copper Chemical compound [Cu].[Ce] SKEYZPJKRDZMJG-UHFFFAOYSA-N 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000002485 combustion reaction Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 22
- 239000000155 melt Substances 0.000 description 19
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 16
- 238000003723 Smelting Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 230000006698 induction Effects 0.000 description 12
- 238000009864 tensile test Methods 0.000 description 12
- 238000005266 casting Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 238000007711 solidification Methods 0.000 description 7
- 230000008023 solidification Effects 0.000 description 7
- 238000011049 filling Methods 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000007769 metal material Substances 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 238000005204 segregation Methods 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000007873 sieving Methods 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 230000001360 synchronised effect Effects 0.000 description 5
- 230000002457 bidirectional effect Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007712 rapid solidification Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- 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
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
- F02K—JET-PROPULSION PLANTS
- F02K9/00—Rocket-engine plants, i.e. plants carrying both fuel and oxidant therefor; Control thereof
- F02K9/42—Rocket-engine plants, i.e. plants carrying both fuel and oxidant therefor; Control thereof using liquid or gaseous propellants
- F02K9/60—Constructional parts; Details not otherwise provided for
- F02K9/62—Combustion or thrust chambers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
- B22F2003/175—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging by hot forging, below sintering temperature
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
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Abstract
The invention discloses a copper-silver-zirconium alloy, a preparation method and application thereof, comprising the following steps: the copper-silver-zirconium alloy is prepared according to the composition of the copper-silver-zirconium alloy, wherein the copper-silver-zirconium alloy comprises the following components in percentage by mass: 2.1-3.8% of silver, 0.3-1.1% of zirconium, 0.1-0.3% of rare earth cerium and the balance of copper; carrying out vacuum melting and atomization on the alloy raw materials after the proportioning to obtain prealloyed powder; sintering and densification treatment are carried out on the prealloyed powder through hot isostatic pressing; forging, upsetting and deforming the hot isostatic pressing alloy; and carrying out heat treatment on the wrought alloy to obtain the copper-silver-zirconium alloy. The copper-silver-zirconium alloy cooperatively reinforced by the submicron-sized second phase with good thermal stability and the superfine crystal is obtained, and the high-temperature mechanical property of the alloy is effectively improved.
Description
Technical Field
The invention belongs to the technical field of alloys, and particularly relates to a copper-silver-zirconium alloy and a preparation method and application thereof.
Background
Liquid hydrogen liquid oxygen rocket engines need to work under high temperature and high pressure environment, and the inner wall of the combustion chamber of the liquid hydrogen liquid oxygen rocket engine needs to be made of materials with high heat conduction and certain high temperature strength. The copper silver zirconium (cu3ag0.5zr) alloy developed by NASA in the united states at the end of the 20 th century for the main engine combustion chamber of a space shuttle is the most typical inner wall material meeting the above requirements. The alloy has a thermal conductivity of up to 320W/(m.K), and the combustion chamber made of the alloy is designed with cooling channels, and the throat can bear up to 163 MW/m 2 Belongs to the inner wall material of the third generation combustion chamber. However, the preparation and structure control of the alloy have been a major problem. Because the Zr content in the copper-silver-zirconium alloy is up to 0.5 percent (mass fraction, the same applies below), and the maximum equilibrium solid solubility of Zr in copper is only about 0.14 percent, the alloy is extremely easy to cause second phase segregation in the conventional casting and solidification processes. The second phase size in the alloy is then from a few microns to tens of microns even through subsequent solid solution and plastic deformation treatments. The properties of copper silver zirconium alloys are largely dependent on the uniformity of the microstructure and the purity of the substrate. Therefore, how to improve the uniformity of the microstructure of the copper-silver-zirconium alloy, improve the appearance, the size and the distribution of the second phase precipitation, and purify the matrix is the research focus and the difficulty of the preparation process of the copper-silver-zirconium alloy.
Currently, the main production method of the alloy is vacuum smelting casting, forging and heat treatment (CN 104232978B). Because of the indissolvable property of zirconium, the copper-silver-zirconium alloy prepared by the process inevitably has micron-sized intermetallic compound segregation on the grain boundary. The NASA solution is to use laser or electron beam to carry out secondary treatment on the surface of the inner wall material, and the second phase with coarse surface layer is homogenized and refined, which is favorable for reducing the crack initiation tendency of the material in the service process and prolonging the service life (Journal of Materials Science, 1997, 32 (14): 3891-3903). However, the surface of the alloy prepared by the conventional casting method is subjected to laser or electron beam treatment, the depth of a refinement layer is generally only tens to hundreds of micrometers, the surface treatment cannot fundamentally solve the problem of the inside of the material, and the treatment process is complex and the cost is high. It can be seen that the performance of the copper-silver-zirconium alloy is also improved.
Disclosure of Invention
The invention aims to solve the technical problems, overcome the defects and the shortcomings in the background art, provide a copper-silver-zirconium alloy, a preparation method and application thereof, and improve the high-temperature mechanical properties of the alloy.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the preparation method of the copper-silver-zirconium alloy comprises the following steps:
s1, preparing materials according to the composition of copper-silver-zirconium alloy, wherein the copper-silver-zirconium alloy comprises the following components in percentage by mass: 2.1-3.8% of silver, 0.3-1.1% of zirconium, 0.1-0.3% of rare earth cerium and the balance of copper;
s2, carrying out vacuum melting and atomization on the alloy raw materials after the proportioning, controlling the temperature of an alloy melt in the vacuum melting at 1250-1450 ℃ and keeping the temperature for 30-60 min, and then adjusting the atomization pressure to 3-4 MPa for atomization to obtain prealloy powder;
s3, sintering and densification treatment are carried out on the prealloyed powder through hot isostatic pressing, the pressure is controlled to be 120-180 MPa, the temperature is controlled to be 800-950 ℃, and the pressure maintaining and heat preserving time is 2-24 hours;
s4, forging, upsetting and deforming the hot isostatic pressing alloy;
and S5, performing heat treatment on the wrought alloy to obtain the copper-silver-zirconium alloy.
As a further improvement, the content of zirconium in the copper-silver-zirconium alloy in S1 is 0.3-0.6%, and the content of rare earth cerium is 0.15-0.25%.
As a further improvement, the zirconium and the rare earth cerium in S1 are added in a mode of adopting copper-zirconium and copper-cerium intermediate alloy.
As a further improvement, in S2, vacuum melting is performed using argon as a shielding gas.
As a further improvement, in S3, adopting a cylindrical sheath for hot isostatic pressing sintering; s4, cutting the isostatic alloy into a cylinder, keeping a sheath on the cylindrical surface, removing the end surface sheath, and forging, upsetting and deforming.
As a further improvement, the forging upsetting deformation in the step S4 is carried out, and the initial forging temperature is 650-800 ℃.
As a further improvement, the heat treatment temperature in S5 is 350-400 ℃, and the heat treatment time is 2-10 h.
The invention provides a copper-silver-zirconium alloy, which is prepared by adopting the method, wherein the second phase is spherical, and the size is controlled to be 0.3-1.0 mu m.
The invention provides an application of a copper-silver-zirconium alloy prepared by the method in an inner wall material of a combustion chamber of an engine.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses vacuum smelting argon atomization to prepare prealloy powder, then adopts hot isostatic pressing to sinter and densify the powder, and finally regulates and controls alloy structure through plastic deformation and heat treatment to obtain copper-silver-zirconium alloy cooperatively reinforced by submicron-sized second phase and superfine crystals with good heat stability.
The invention adopts the powder metallurgy method and controls the process conditions, especially the conditions of vacuum melting and atomization, and the solidification speed of the molten alloy can reach 10 in the unbalanced solidification process from liquid phase solidification to solid phase solidification 4 ~10 6 K/s, far exceeds the solidification rate of conventional casting processes. Under rapid solidification conditions, the ultimate solid solubility of zirconium in copper expands from about 0.14% in the equilibrium state to about 1.33% in the non-equilibrium state. By controlling sintering conditions, supersaturated zirconium atoms dissolved in the powder can be dispersed and separated out in the form of submicron or even nanometer second phase at the sintering temperature lower than the melting point, thereby avoiding zirconium segregation in the conventional smelting process and improving the high-temperature mechanical property of the alloy.
In addition, the invention further improves the cleanliness of the melt by adding trace rare earth cerium to adsorb impurities and gas in the smelting process on the basis of the existing copper-silver-zirconium alloy components, further refines grains, spheroidizes a second phase and improves the thermal stability of the second phase, thereby further achieving the aim of improving the high-temperature mechanical properties of the alloy.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a photograph showing the microstructure of the Cu-Ag-Zr alloy in example 2.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
The copper-silver-zirconium alloy of some specific embodiments of the invention comprises the following components in percentage by mass: silver 2.1-3.8%, zirconium 0.3-1.1% (preferably 0.3-0.6%), rare earth cerium 0.1-0.3% (preferably 0.15-0.25%), and copper in balance.
The preparation method of the copper-silver-zirconium alloy comprises the following steps of:
s1: batching;
s2: vacuum smelting and atomizing to obtain prealloyed powder;
s3: sintering by hot isostatic pressing and densification;
s4: forging deformation of the belt sleeve;
s5: and (5) heat treatment.
In some embodiments, in the step S1, for the element zirconium and rare earth element cerium that are easy to burn out, the addition is performed by adopting a copper-zirconium and copper-cerium intermediate alloy mode, so that the burn out of the two elements in the smelting process can be effectively reduced.
In some embodiments, in the step S2, argon is used as a shielding gas for vacuum melting, the temperature of the alloy melt is controlled at 1250-1450 ℃, the temperature is kept for 30-60 min, and the atomization pressure of the argon is regulated to 3-4 MPa for atomization, so as to obtain prealloy powder. Compared with a powder product obtained by mechanical alloying, prealloyed powder is obtained by argon atomization, wherein metals with various components are smelted into an alloy in advance before sintering according to the designed component proportion, and then atomized and sprayed. Each powder contains various metal elements for forming the alloy, and the prealloyed powder has quite good component uniformity; the eutectic point is much lower than the melting point of the single element in the alloy, and sintering densification can be performed only when the sintering temperature exceeds the liquidus point of the prealloyed powder by a little during the sintering process. In addition, the possibility of introducing impurities during the mechanical alloying process is avoided.
The prealloy powder obtained by the invention is used as a raw material, so that the element segregation in the conventional smelting and casting process is fundamentally solved, and the uniformity of alloy components is ensured. The alloy material prepared from the prealloyed powder has high alloying degree, good uniformity and high purity.
In some embodiments, in the step S3, the prealloyed powder is first put into a sheath, and is pressurized and heated in a hot isostatic pressing furnace, the pressure is 120-180 MPa, the temperature is 800-950 ℃, and the pressure maintaining and heat preserving time is 2-24 hours. Sintering and densification treatment are carried out on the powder through hot isostatic pressing, so that the complete densification of the alloy material is ensured.
In some embodiments, in the step S4, the hot isostatic pressing alloy is cut into a cylindrical shape, the cylindrical surface is kept with a sheath, the end surface sheath is removed, forging upsetting deformation is performed, the initial forging temperature is 650-800 ℃, and upsetting is performed to 10-15 mm. The second phase and grains in the alloy are secondarily crushed by hot forging. Without sheath forging, the material is only subjected to unidirectional compressive stress and bidirectional tensile stress in the free forging process, the drum shape is easy to appear, difficult deformation areas exist on the upper surface and the lower surface, and the outer surface of the material can generate micro cracks and other defects under the action of the bidirectional tensile stress, so that the mechanical property is poor. Under the condition that the sheath exists, the material is in a three-way compressive stress state, so that the appearance of double drums of the forging can be avoided, and microcracks in the material can be effectively bridged.
In some embodiments, in the step S5, the heat treatment temperature is 350-400 ℃, the heat treatment time is 2-10 hours, and air cooling is adopted. The structure and the performance of the alloy are regulated and controlled through heat treatment, and the copper-silver-zirconium alloy with good high-temperature performance is obtained.
In some embodiments, the second phase is spherical, and the size is controlled to be between 0.3 and 1.0 μm, and the size is far lower than a few micrometers or even tens of micrometers in the prior art.
In some embodiments, the second phase contains copper, silver, zirconium and cerium, and the enrichment of cerium can spheroidize the second phase on one hand, reduce stress concentration in service state, improve the thermal stability of the second phase on the other hand, and improve high-temperature mechanical properties.
Compared with the prior art, the method for obtaining the copper-silver-zirconium alloy with fine dispersion of the second phase size and fine grain size through powder metallurgy rapid solidification is provided, and segregation of a zirconium-rich phase in a conventional vacuum smelting casting process can be effectively avoided, so that the tendency of initiation and expansion of microcracks from a coarse second phase in a high-temperature high-pressure service environment is reduced.
The invention also adds trace rare earth for adsorbing impurities in the melt, thus improving the purity of the material, and the addition of rare earth elements is helpful for further refining grains while not obviously reducing the plasticity of the alloy, spheroidizing the second phase, increasing the thermal stability of the second phase and the grain size and further effectively improving the high-temperature mechanical property of the alloy.
Example 1:
the copper-silver-zirconium alloy of the embodiment has the silver content of 3%, the zirconium content of 0.5%, the rare earth cerium of 0.1% and the balance copper. The preparation method comprises the following steps:
s1: and (5) batching. The raw materials used are electrolytic copper with the purity of 99.99 percent, pure silver with the purity of 99.99 percent, zirconium and rare earth elements are added in the form of intermediate alloy, wherein the zirconium content in the copper-zirconium intermediate alloy is 8 percent, and the cerium content in the copper-cerium intermediate alloy is 10 percent.
S2: vacuum smelting argon atomization. Firstly, placing the prepared pure metal and intermediate alloy into a vacuum melting crucible, vacuumizing a melting chamber and an atomizing chamber to 1.0X10 -2 Pa, maintaining for 10 min, then filling argon gas to the standard atmospheric pressure as protective gas, opening a high-frequency induction device for heating, adjusting the temperature of the melt to 1400 ℃ after the alloy in the crucible is completely melted, and preserving the temperature for 30 min to prepare for atomization. And adjusting the atomization pressure of the argon to 3.5 MPa, opening an argon valve, and lifting a ceramic blocking rod in the crucible to enable the melt to start atomization and crushing along the liquid guide tube. When the melt in the crucible flows out, the high-frequency induction device and the argon valve are closed, and the prealloyed powder in the collector is collected after being completely cooled. Sieving the powder with 200 mesh sieve for use.
S3: and (5) hot isostatic pressing sintering and densification treatment. The prealloyed powder is filled into a steel cylindrical sheath, the internal size of the sheath is phi 120 mm multiplied by 150 mm, the sheath filled with the powder is welded and sealed by a cover plate, and finally, the sealed sheath tank is placed into a hot isostatic pressing furnace for pressurized heating, the pressure is 150 MPa, the temperature is 900 ℃ and the pressure and heat preservation time is 5 h, and the pressurizing process and the heating process are kept synchronous.
S4: forging with a sheath. Cutting the hot isostatic pressing alloy into cylinders, wherein each block has the height of 100 mm, the cylindrical surface is reserved with a sheath, the end surface sheath is removed, forging upsetting deformation is carried out, and the initial forging temperature is 780 ℃ and the upsetting is 10 mm.
S5: and (5) heat treatment. And (3) performing heat treatment on the wrought alloy, wherein the heat treatment temperature is 350 ℃, and the heat treatment time is 2 h.
The copper-silver-zirconium alloy prepared in the embodiment is subjected to high-temperature tensile test at 400 ℃, 450 ℃ and 500 ℃ according to a standard GBT4338-2006 metal material high-temperature tensile test method, a tensile sample is taken along the radial direction, the tensile strength is 314 MPa, 290 MPa and 272 MPa, the yield strength is 298 MPa, 256 MPa and 169 MPa, and the elongation after break is 26%, 28% and 35%.
Example 2:
the copper-silver-zirconium alloy of the embodiment has the silver content of 3%, the zirconium content of 0.5%, the rare earth cerium of 0.2% and the balance copper. The preparation method comprises the following steps:
s1: and (5) batching. The raw materials used are electrolytic copper with the purity of 99.99 percent, pure silver with the purity of 99.99 percent, zirconium and rare earth elements are added in the form of intermediate alloy, wherein the zirconium content in the copper-zirconium intermediate alloy is 8 percent, and the cerium content in the copper-cerium intermediate alloy is 10 percent.
S2: vacuum smelting argon atomization. Firstly, placing the prepared pure metal and intermediate alloy into a vacuum melting crucible, vacuumizing a melting chamber and an atomizing chamber to 1.0X10 -2 Pa, maintaining for 10 min, then filling argon gas to the standard atmospheric pressure as protective gas, opening a high-frequency induction device for heating, adjusting the temperature of the melt to 1400 ℃ after the alloy in the crucible is completely melted, and preserving the temperature for 30 min to prepare for atomization. And adjusting the atomization pressure of the argon to 3.5 MPa, opening an argon valve, and lifting a ceramic blocking rod in the crucible to enable the melt to start atomization and crushing along the liquid guide tube. When the melt in the crucible flows out, the high-frequency induction device and the argon valve are closed, and the prealloyed powder in the collector is collected after being completely cooled. Sieving the powder with 200 mesh sieve for use.
S3: and (5) hot isostatic pressing sintering and densification treatment. The prealloyed powder is filled into a steel cylindrical sheath, the internal size of the sheath is phi 120 mm multiplied by 150 mm, the sheath filled with the powder is welded and sealed by a cover plate, and finally, the sealed sheath tank is placed into a hot isostatic pressing furnace for pressurized heating, the pressure is 150 MPa, the temperature is 900 ℃ and the pressure and heat preservation time is 5 h, and the pressurizing process and the heating process are kept synchronous.
S4: forging with a sheath. Cutting the hot isostatic pressing alloy into cylinders, wherein each block has the height of 100 mm, the cylindrical surface is reserved with a sheath, the end surface sheath is removed, forging upsetting deformation is carried out, and the initial forging temperature is 780 ℃ and the upsetting is 10 mm.
S5: and (5) heat treatment. And (3) performing heat treatment on the wrought alloy, wherein the heat treatment temperature is 350 ℃, and the heat treatment time is 2 h.
The microstructure photograph of the copper-silver-zirconium alloy of the present example is shown in fig. 1. It can be seen that the second phase is spherical and the size is controlled to be 0.3-1.0 μm.
The copper-silver-zirconium alloy prepared in this example was subjected to high temperature tensile test at 400 ℃, 450 ℃ and 500 ℃ according to the standard GBT4338-2006 metal material high temperature tensile test method, with tensile strengths of 334 MPa, 305 MPa and 289 MPa, respectively, yield strengths of 304 MPa, 256 MPa and 172 MPa, respectively, and elongation after break of 25%, 29% and 38%, respectively.
Example 3:
the copper-silver-zirconium alloy of the embodiment has the silver content of 3%, the zirconium content of 0.5%, the rare earth cerium of 0.3% and the balance copper. The preparation method comprises the following steps:
s1: and (5) batching. The raw materials used are electrolytic copper with the purity of 99.99 percent, pure silver with the purity of 99.99 percent, zirconium and rare earth elements are added in the form of intermediate alloy, wherein the zirconium content in the copper-zirconium intermediate alloy is 8 percent, and the cerium content in the copper-cerium intermediate alloy is 10 percent.
S2: vacuum smelting argon atomization. Firstly, placing the prepared pure metal and intermediate alloy into a vacuum melting crucible, vacuumizing a melting chamber and an atomizing chamber to 1.0X10 -2 Pa, maintaining for 10 min, then filling argon gas to the standard atmospheric pressure as protective gas, opening a high-frequency induction device for heating, adjusting the temperature of the melt to 1400 ℃ after the alloy in the crucible is completely melted, and preserving the temperature for 30 min to prepare for atomization. And adjusting the atomization pressure of the argon to 3.5 MPa, opening an argon valve, and lifting a ceramic blocking rod in the crucible to enable the melt to start atomization and crushing along the liquid guide tube. When the melt in the crucible flows out, the high-frequency induction device and the argon valve are closed, and the prealloyed powder in the collector is collected after being completely cooled. Sieving the powder with 200 mesh sieve for use.
S3: and (5) hot isostatic pressing sintering and densification treatment. The prealloyed powder is filled into a steel cylindrical sheath, the internal size of the sheath is phi 120 mm multiplied by 150 mm, the sheath filled with the powder is welded and sealed by a cover plate, and finally, the sealed sheath tank is placed into a hot isostatic pressing furnace for pressurized heating, the pressure is 150 MPa, the temperature is 900 ℃ and the pressure and heat preservation time is 5 h, and the pressurizing process and the heating process are kept synchronous.
S4: forging with a sheath. Cutting the hot isostatic pressing alloy into cylinders, wherein each block has the height of 100 mm, the cylindrical surface is reserved with a sheath, the end surface sheath is removed, forging upsetting deformation is carried out, and the initial forging temperature is 780 ℃ and the upsetting is 10 mm.
S5: and (5) heat treatment. And (3) performing heat treatment on the wrought alloy, wherein the heat treatment temperature is 350 ℃, and the heat treatment time is 2 h.
The copper-silver-zirconium alloy prepared in this example was subjected to high temperature tensile test at 400 ℃, 450 ℃ and 500 ℃ according to the standard GBT4338-2006 metal material high temperature tensile test method, with tensile strengths of 306 MPa, 281 MPa and 249 MPa, yield strengths of 293 MPa, 242 MPa and 159 MPa, respectively, and elongation after break of 22%, 25% and 34%, respectively.
Comparative example 1: the copper-silver-zirconium alloy of the comparative example has a silver content of 3%, a zirconium content of 0.5% and the balance copper. The preparation method comprises the following steps:
s1: and (5) batching. The raw materials used are electrolytic copper with the purity of 99.99 percent, pure silver with the purity of 99.99 percent and zirconium added in the form of intermediate alloy, wherein the zirconium content in the copper-zirconium intermediate alloy is 8 percent.
S2: vacuum smelting argon atomization. Firstly, placing the prepared pure metal and intermediate alloy into a vacuum melting crucible, vacuumizing a melting chamber and an atomizing chamber to 1.0X10 -2 Pa, maintaining for 10 min, then filling argon gas to the standard atmospheric pressure as protective gas, opening a high-frequency induction device for heating, adjusting the temperature of the melt to 1400 ℃ after the alloy in the crucible is completely melted, and preserving the temperature for 30 min to prepare for atomization. And adjusting the atomization pressure of the argon to 3.5 MPa, opening an argon valve, and lifting a ceramic blocking rod in the crucible to enable the melt to start atomization and crushing along the liquid guide tube. When the melt in the crucible flows out, the high-frequency induction device and the argon valve are closed, and the prealloyed powder in the collector is collected after being completely cooled. Sieving the powder with 200 mesh sieve for use.
S3: and (5) hot isostatic pressing sintering and densification treatment. The prealloyed powder is filled into a steel cylindrical sheath, the internal size of the sheath is phi 120 mm multiplied by 150 mm, the sheath filled with the powder is welded and sealed by a cover plate, and finally, the sealed sheath tank is placed into a hot isostatic pressing furnace for pressurized heating, the pressure is 150 MPa, the temperature is 900 ℃ and the pressure and heat preservation time is 5 h, and the pressurizing process and the heating process are kept synchronous.
S4: forging with a sheath. Cutting the hot isostatic pressing alloy into cylinders, wherein each block has the height of 100 mm, the cylindrical surface is reserved with a sheath, the end surface sheath is removed, forging upsetting deformation is carried out, and the initial forging temperature is 780 ℃ and the upsetting is 10 mm.
S5: and (5) heat treatment. And (3) performing heat treatment on the wrought alloy, wherein the heat treatment temperature is 350 ℃, and the heat treatment time is 2 h.
The copper-silver-zirconium alloy prepared in the comparative example is subjected to high-temperature tensile test at 400 ℃, 450 ℃ and 500 ℃ according to the standard GBT4338-2006 metal material high-temperature tensile test method, the tensile strength is 328 MPa, 292 MPa and 256 MPa, the yield strength is 278 MPa, 236 MPa and 198 MPa, and the elongation after break is 27%, 31% and 40%.
Comparative example 2: the copper-silver-zirconium alloy of the comparative example contains 3% of silver, 0.5% of zirconium, 0.3% of rare earth cerium and the balance copper. The preparation method comprises the following steps:
s1: and (5) batching. The raw materials used are electrolytic copper with the purity of 99.99 percent, pure silver with the purity of 99.99 percent, zirconium and rare earth elements are added in the form of intermediate alloy, wherein the zirconium content in the copper-zirconium intermediate alloy is 8 percent, and the cerium content in the copper-cerium intermediate alloy is 10 percent.
S2: vacuum smelting argon atomization. Firstly, placing the prepared pure metal and intermediate alloy into a vacuum melting crucible, vacuumizing a melting chamber and an atomizing chamber to 1.0X10 -2 Pa, maintaining for 10 min, then filling argon gas to the standard atmospheric pressure as protective gas, opening a high-frequency induction device for heating, adjusting the temperature of the melt to 1400 ℃ after the alloy in the crucible is completely melted, and preserving the temperature for 30 min to prepare for atomization. And adjusting the atomization pressure of the argon to 3.5 MPa, opening an argon valve, and lifting a ceramic blocking rod in the crucible to enable the melt to start atomization and crushing along the liquid guide tube. High frequency induction device and argon gas are turned off when the melt in the crucible is completely flowed outAnd a valve for collecting the powder after the prealloyed powder in the collector is completely cooled. Sieving the powder with 200 mesh sieve for use.
S3: and (5) hot isostatic pressing sintering and densification treatment. The prealloyed powder is filled into a steel cylindrical sheath, the internal size of the sheath is phi 120 mm multiplied by 150 mm, the sheath filled with the powder is welded and sealed by a cover plate, and finally, the sealed sheath tank is placed into a hot isostatic pressing furnace for pressurized heating, the pressure is 150 MPa, the temperature is 900 ℃ and the pressure and heat preservation time is 5 h, and the pressurizing process and the heating process are kept synchronous.
S4: removing the sheath and forging freely. Cutting the hot isostatic pressing alloy into cylinders, removing the sheath from each block with the height of 100 mm, forging, upsetting and deforming, wherein the initial forging temperature is 780 ℃ and the upsetting is 10 mm.
S5: and (5) heat treatment. And (3) performing heat treatment on the wrought alloy, wherein the heat treatment temperature is 350 ℃, and the heat treatment time is 2 h.
The copper-silver-zirconium alloy prepared in the comparative example is subjected to high-temperature tensile test at 400 ℃, 450 ℃ and 500 ℃ according to the standard GBT4338-2006 metal material high-temperature tensile test method, the tensile strength is 290 MPa, 265MPa and 236 MPa, the yield strength is 271 MPa, 209 MPa and 148 MPa, and the elongation after break is 19%, 21% and 31%.
Comparative example 3: the copper-silver-zirconium alloy of the comparative example contains 3% of silver, 0.5% of zirconium, 0.3% of rare earth cerium and the balance copper. The preparation method comprises the following steps:
s1: and (5) batching. The raw materials used are electrolytic copper with the purity of 99.99 percent, pure silver with the purity of 99.99 percent, zirconium and rare earth elements are added in the form of intermediate alloy, wherein the zirconium content in the copper-zirconium intermediate alloy is 8 percent, and the cerium content in the copper-cerium intermediate alloy is 10 percent.
S2: and (5) vacuum smelting and casting. Respectively placing electrolytic copper, pure silver, copper-zirconium alloy and copper-cerium intermediate alloy which are prepared according to the proportion into an induction furnace, vacuumizing, and keeping the vacuum degree below 10 -2 Maintaining for 10 min at Pa, then filling argon gas to standard atmospheric pressure as protective gas, opening a high-frequency induction device for heating, adjusting the temperature of the melt to 1400 ℃ after the alloy in the crucible is completely melted, preserving heat for 30 min,the melt was cast and subsequently cooled to room temperature.
S3: cutting the cast alloy into cylinders, forging, upsetting and deforming each block with the height of 100 mm, and upsetting to 10 mm at the initial forging temperature of 780 ℃.
S4: and (5) heat treatment. And (3) performing heat treatment on the wrought alloy, wherein the heat treatment temperature is 350 ℃, and the heat treatment time is 2 h.
The copper-silver-zirconium alloy prepared in the comparative example is subjected to high-temperature tensile test at 400 ℃, 450 ℃ and 500 ℃ according to a standard GBT4338-2006 metal material high-temperature tensile test method, wherein the tensile strength is 256 MPa, 209 MPa and 168 MPa, the yield strength is 206 MPa, 167 MPa and 121 MPa, and the elongation after break is 26%, 28% and 34%.
The performance data for the examples and comparative examples are now presented in table 1.
TABLE 1
From this, it can be seen that the example added 0.2% rare earth with the best performance. In example 3, when the rare earth addition amount was increased to 0.3%, the performance was rather in a decreasing trend. The addition of excessive rare earth can form excessive intermetallic compound with larger size on the grain boundary, reduce the strength and plasticity of the alloy and mask the adverse effect of the rare earth. Comparative example 1 shows inferior performance compared to the alloy added with 0.1% and 0.2% because strengthening is performed without adding rare earth. In comparative example 2, since the forging with the sheath is not performed, the material is only subjected to unidirectional compressive stress and bidirectional tensile stress in the free forging process, the drum shape is easy to appear, the upper surface and the lower surface have difficult deformation areas, and the outer surface of the material can generate defects such as microcracks under the action of the bidirectional tensile stress, so that the mechanical property performance is poor. Under the condition that the sheath exists, the material is in a three-way compressive stress state, so that the appearance of double drums of the forging can be avoided, and microcracks in the material can be effectively bridged. Comparative example 3, because no powder metallurgy method was used, caused segregation of the second phase grain boundaries during conventional casting and solidification, the subsequent plastic deformation also failed to break up the bulk second phase, resulting in a decrease in high temperature mechanical properties.
The foregoing is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Therefore, any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention shall fall within the scope of the technical solution of the present invention.
Claims (9)
1. The preparation method of the copper-silver-zirconium alloy is characterized by comprising the following steps of:
s1, preparing materials according to the composition of copper-silver-zirconium alloy, wherein the copper-silver-zirconium alloy comprises the following components in percentage by mass: 2.1-3.8% of silver, 0.3-1.1% of zirconium, 0.1-0.3% of rare earth cerium and the balance of copper;
s2, carrying out vacuum melting and atomization on the alloy raw materials after the proportioning, controlling the temperature of an alloy melt in the vacuum melting at 1250-1450 ℃ and keeping the temperature for 30-60 min, and then adjusting the atomization pressure to 3-4 MPa for atomization to obtain prealloy powder;
s3, sintering and densification treatment are carried out on the prealloyed powder through hot isostatic pressing, the pressure is controlled to be 120-180 MPa, the temperature is controlled to be 800-950 ℃, and the pressure maintaining and heat preserving time is 2-24 hours;
s4, forging, upsetting and deforming the hot isostatic pressing alloy;
and S5, performing heat treatment on the wrought alloy to obtain the copper-silver-zirconium alloy.
2. The method for preparing the copper-silver-zirconium alloy according to claim 1, wherein the zirconium content of the copper-silver-zirconium alloy in S1 is 0.3-0.6%, and the rare earth cerium content is 0.15-0.25%.
3. The method for preparing the copper-silver-zirconium alloy according to claim 1 or 2, wherein the zirconium and the rare earth cerium in the step S1 are added in a mode of copper-zirconium and copper-cerium intermediate alloy.
4. The method for producing a copper-silver-zirconium alloy according to claim 1 or 2, wherein the vacuum melting is performed using argon as a shielding gas in S2.
5. The method for preparing the copper-silver-zirconium alloy according to claim 1 or 2, wherein the step S3 is a hot isostatic pressing sintering by using a cylindrical sheath; s4, cutting the isostatic alloy into a cylinder, keeping a sheath on the cylindrical surface, removing the end surface sheath, and forging, upsetting and deforming.
6. The method for preparing the copper-silver-zirconium alloy according to claim 5, wherein the forging upsetting deformation in the step S4 is performed, and the initial forging temperature is 650-800 ℃.
7. The method for preparing the copper-silver-zirconium alloy according to claim 1 or 2, wherein the heat treatment temperature in S5 is 350-400 ℃, and the heat treatment time is 2-10 h.
8. A copper-silver-zirconium alloy, characterized in that it is prepared by the method of any one of claims 1 to 7, and the second phase is spherical, and the size is controlled to be 0.3 to 1.0 μm.
9. Use of the copper-silver-zirconium alloy prepared by the method of any one of claims 1-7 in an engine combustion chamber inner wall material.
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