CN112877570A - Cobalt-chromium-nickel multi-element casting alloy and preparation method thereof - Google Patents
Cobalt-chromium-nickel multi-element casting alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a cobalt-chromium-nickel multi-element casting alloy and a preparation method thereof, wherein the cobalt-chromium-nickel multi-element casting alloy adopts a powder metallurgy method to prepare a mixture, and then adopts a secondary argon arc melting method, the primary melting current is 300A-400A, and the secondary melting current is 200A-300A. The cobalt-chromium-nickel casting alloy is prepared from Co-Cr-Ni-M-C original powder, wherein M is selected from one or more of Mo, Fe, Si and Mn. And (3) quantifying the mass fraction of Co, wherein the sum of the mass fractions of all the alloy elements is 100%. Under the action of alloy elements, the phase composition and distribution of the alloy are quantitatively controlled by adopting a Cr equivalent and Ni equivalent method, the phase composition of the alloy is regulated and controlled by adjusting the content of Cr and Ni equivalents in the components of the raw materials, and the compact alloy is obtained by adopting an arc melting method.
Description
Technical Field
The invention relates to the field of powder metallurgy, in particular to a cobalt-chromium-nickel multi-element casting alloy and a preparation method thereof.
Background
The cobalt-chromium-nickel alloy has excellent mechanical property, wear resistance and biocompatibility, and can be used for dentistry, artificial joint connectors and the like. In addition, the cobalt-chromium-nickel alloy has high-temperature strength, high adhesion resistance and high corrosion resistance, and is widely applied to chemical industry, petroleum and natural gas equipment, gas turbines, aviation and steel industry.
The cobalt-chromium alloys of the high cobalt series are generally subjected to a hot forging process by casting or after casting. The cast alloy usually has the defects of coarse columnar crystals, shrinkage cavities and the like, and the mechanical properties of the alloy are seriously influenced, particularly the plasticity and the fatigue strength are low. These defects in cast cobalt chromium nickel alloys are believed to be the primary cause of accidental fracture failure of cobalt chromium nickel alloys as implant devices. Research work is currently being conducted in the field of powder superalloys, such as high nickel-cobalt-chromium alloys, and countries in the united states, russia, uk, france, germany, canada, sweden, china, japan, italy, and india, but only the united states, russia, france, and uk can independently develop powder superalloys and establish corresponding alloy grades. In China, powder superalloy is developed in the last 80 years, although the performance of the developed powder superalloy meets the international standard requirement, the flaw wave of ultrasonic flaw detection inclusions (axial accumulation of inclusions) is higher than the American standard, and the powder superalloy is not examined and applied all the time. And at present, China does not have the extrusion cogging capability of the powder high-temperature alloy large-size bar and large-size isothermal forging equipment protected by inert gas (or vacuum), and the lack of key equipment becomes the bottleneck of the development and production of the powder high-temperature alloy in the extrusion and isothermal forging process route.
Disclosure of Invention
In order to solve the technical problems, the invention provides a cobalt-chromium-nickel multi-element casting alloy and a preparation method thereof.
The scheme of the invention is as follows:
a cobalt chromium nickel multi-element casting alloy material adopts Co quantitative mass fraction, and adjusts the alloy phase composition by adjusting the mass fraction of Cr equivalent and Ni equivalent to form a pseudo-binary alloy phase diagram of CoCrNi multi-element alloy; the phase composition of the cobalt-chromium-nickel cast two-phase alloy is face-centered cubicα-fccPhase and hexagonal close packed hard phaseε-hcpPhase in which the columnar crystal trunk region isα-fccPhase, at the dendrite grain boundary, ofε-hcpAnd (4) phase(s).
Preferably, the material is prepared from the following raw material powders: the cobalt-chromium-nickel multi-element alloy material is prepared from Co-Cr-Ni-M-C original powder, wherein the addition amount of each raw material powder is as follows by mass percent: 62 percent; cr: 0 to 31 percent; ni: 0 to 31 percent; mo: 2% -12%; fe: 2% -12%; si: 2% -12%; c: 0.05-0.2%; the sum of the mass fractions of all the alloy elements is 100 percent;
meanwhile, the following expressions (1) and (2) are satisfied:
ni equivalent = Ni +35 × C, range: 1.5 to 34.4 (1);
cr equivalent = Cr + Mo +1.5 × (Fe + Si), range: 7.5 to 38.4 (2).
The method for preparing the cobalt-chromium-nickel multi-element alloy material comprises the following steps:
1) weighing the original powder according to a proportion, preparing mixed powder, and performing wet ball milling on the mixed powder to obtain mixed slurry.
2) Drying the mixed slurry obtained in the step 1) in a drying oven to obtain a mixed material;
3) pressing and forming the material obtained in the step 2) to obtain a pressed blank, wherein the pressing pressure is 450-600 MPa;
4) smelting the pressed blank in the step 3) by adopting argon arc to obtain liquid alloy;
5) and 4) cooling the material to room temperature after sintering to obtain the cobalt-chromium-nickel alloy material.
Preferably, absolute ethyl alcohol is adopted as a dispersing agent in the step 1), steel balls of ϕ 5- ϕ 10 are adopted as grinding balls, and the ball-to-material ratio is (7-10): 1, rotating speed (211-260) r/min, and mixing time is 48-60 h.
Preferably, the step 2) is implemented by sieving and granulating, and a 60-80 mesh sieve is selected; the drying temperature is 75-85 ℃.
Further preferably, in the step 3), the pressing pressure is 450-600 MPa.
Further preferably, in the step 4), the specific operation steps of argon arc melting are as follows:
s1, driving air by adopting argon, igniting electric arc between the tungsten electrode and the water-cooled copper mold, and placing the smelted alloy in the water-cooled copper mold;
s2, the first smelting current value is 300-400A, and the smelting time is 10-30S;
s3, overturning the alloy, and smelting again, wherein the smelting current value is 200-300A, and the smelting time is 10-30S;
obtaining the liquid alloy. The invention has the beneficial effects that:
according to the influence rule of the alloy elements on the phase composition of the Co-based alloy, the invention classifies the effects of the alloy elements into Cr and Ni equivalent, regulates the phase composition and phase distribution of the alloy through the Cr and Ni equivalent, can accurately control the phase composition and phase component of the Co-based alloy, and particularly can control the brittleness and hardness formed at a dendritic crystal boundaryhcpPhase volume fraction, thereby controlling the mechanical properties of the cast alloy. By the alloy phase composition rule of different component combinations, a cobalt-chromium-nickel pseudo-binary alloy phase diagram is established and enriched, and reliable guidance is provided for the research and application of cobalt-chromium-nickel alloy. On the basis of obtaining high-activity mixture by adopting a powder metallurgy method, an electric arc melting method is adopted to prepare the cobalt-chromium-nickel alloy, and the dendritic crystal main trunk of the multi-element casting alloy isfccPhase, grain boundary ofhcpThe liquid alloy after electric arc melting is cooled and then solidified to form casting alloy, and the casting structure is fine; the method has short process flow and high preparation efficiency, can prepare the cobalt-chromium-nickel alloy plate in one step, and a molten pool formed in the smelting process can be protected by a skull formed by the metal, so that the smelted molten metal is not polluted by a crucible and the surrounding environment.
Drawings
FIG. 1 shows the metallographic structure of a cobalt-chromium-nickel alloy according to example 1 of the present invention;
FIG. 2 is an XRD physical phase diagram of a cobalt-chromium-nickel alloy of example 1 of the present invention;
FIG. 3 shows the metallographic structure of a cobalt-chromium-nickel alloy according to example 2 of the present invention;
FIG. 4 is an XRD physical phase diagram of a cobalt-chromium-nickel alloy of example 2 of the present invention;
FIG. 5 shows the metallographic structure of a cobalt-chromium-nickel alloy according to example 3 of the present invention;
FIG. 6 is an XRD physical phase diagram of a cobalt chromium alloy of example 3 of the present invention;
FIG. 7 is a phase diagram of a cobalt-chromium-nickel pseudo-binary alloy obtained by the present invention;
FIG. 8 shows the metallographic structure of a cobalt-chromium-nickel alloy according to comparative example 1 of the present invention.
Detailed Description
To illustrate the effectiveness and stability of the arc melting method, the structure evolution law of the multi-element cast alloy obtained by adjusting the equivalent weight of Cr and Ni and the powder metallurgy preparation process will be detailed. The invention is described in detail below by way of examples of specific operations.
Example 1
A preparation method of a cobalt-chromium-nickel multi-element casting alloy comprises the following steps: according to the mass percentage Co, 62%; 20% of Cr; ni, 10.9%; 6 percent of Mo; 1% of Fe; c, 0.1 percent. Cr equivalent mass percent: 27.5 percent, and the mass percent of Ni equivalent is as follows: 14.4 percent. The Cr equivalent and the Ni equivalent are calculated by the formulas (1) and (2), respectively.
Mixing the raw materials according to the mass percentage, adopting steel balls of ϕ 5 and ϕ 10 as grinding balls, wherein the number ratio of the steel balls of ϕ 5 and ϕ 10 is 3: 1, the ball-material ratio is 7: 1, adopting absolute ethyl alcohol as a ball milling medium, wherein the dosage of the absolute ethyl alcohol is 0.35: 1 (ml/g); mixing materials on a planetary ball mill at the rotating speed of 221r/min for 20min to rotate positively and negatively for 48 h. And drying the mixed slurry in a furnace at the temperature of 80 ℃ to obtain a mixed material. And granulating the mixture by a screen of 60-80 meshes, and pressing the mixture into a sample blank on a molding press under the pressure of 500 MPa. The casting alloy is obtained by adopting a twice smelting method. Firstly, argon is adopted to drive air, electric arc is ignited between a tungsten electrode and a water-cooled copper mold, and a smelted alloy pressed compact block is placed in the water-cooled copper mold. The first melting current value was 300A, and the melting time was 30 s. Then, the alloy was turned over and melted again, the melting current value was 200A, and the melting time was 30 s. And cooling to obtain the cobalt-chromium-nickel multi-element casting alloy.
Fig. 1 shows the metallographic structure of the obtained cobalt-chromium-nickel multicomponent cast alloy, and it can be seen that the alloy structure is characterized by cast alloy and cast dendrite. FIG. 2 shows the XRD phase diagram of the obtained alloy, which can determine the alloy to be two-phaseα-fcc，ε-hcpA Co alloy. Further confirmed by SEM and energy spectrum that the high Ni phase isα-fccPhase, high chromium phase isε-hcpAnd (4) phase(s). The main part of the dendrite is a soft phaseα-fccTexture, brittle and hard at grain boundariesε-hcpPhase (C)。The cobalt-based alloy is paramagnetic when solidified from a liquid state to a solid statefcc paraThe phase with high nickel content does not generate solid phase change in the state of continuous cooling, but can generate magnetic transformation to form ferromagnetismfcc ferroAnd (4) phase(s). The high-chromium component phase is converted into paramagnetic with cooling to temperaturehcp paraFurther magnetically transformed into ferromagnetic phasehcp ferroAnd (4) phase(s).
On dendrite boundaries by image analysisε-hcpThe volume fraction of the phase was 33%.
Example 2
A preparation method of a cobalt-chromium-nickel multi-element casting alloy comprises the following steps of (1) preparing a cobalt-chromium-nickel multi-element casting alloy according to the mass percentage of Co, 62%; 30.9 percent of Cr; 6 percent of Mo; 1% of Fe; and C, preparing a mixture by 0.1 percent. Cr equivalent mass percent: 38.4 percent, and the mass percent of Ni equivalent is as follows: 3.5 percent. The preparation and compression molding processes of the mixture are the same as those of the example 1, and the mixing process of the planetary ball mill adopts the rotating speed of 260 r/min. In the preparation process of the electric arc melting, the first melting current value is 400A, and the melting time is 10 s. Then, the alloy was turned over and melted again, the melting current value was 300A, and the melting time was 20 s. And cooling to obtain the cobalt-chromium-nickel multi-element casting alloy.
FIG. 3 shows the metallographic structure of the obtained cast alloy, which is characteristic of cast dendrite and analyzed by XRDα-fcc+ε-hcpA dual phase alloy. At grain boundariesε-hcpThe volume fraction of phases is: 59 percent.
Example 3
A preparation method of a cobalt-chromium-nickel multi-element casting alloy comprises the following steps of (1) preparing a cobalt-chromium-nickel multi-element casting alloy according to the mass percentage of Co, 62%; 30.9 percent of Ni; 6 percent of Mo; 1% of Fe; and C, preparing a mixture by 0.1 percent. Cr equivalent mass percent: 7.5 percent, and the mass percent of Ni equivalent is as follows: 34.4 percent. The preparation and press-forming processes of the mixed material were the same as in example 1. The material mixing process of the planetary ball mill adopts the rotating speed of 240r/min, the ball-material ratio adopts 10: 1. in the preparation process of the electric arc melting, the first melting current value is 200A, and the melting time is 20 s. Then, the alloy was turned over and melted again, the melting current value was 300A, and the melting time was 20 s. And cooling to obtain the cobalt-chromium-nickel multi-element casting alloy.
FIG. 4 shows the metallographic structure of the obtained cast alloy, which is a coarse equiaxed structure having no distinct cast dendrite characteristics. As compared with example 1, the decrease of Cr equivalent with the increase of Ni equivalent reduces and eliminates the Cr equivalent in the structureε-hcpAnd the phase and the Ni content are increased, the growth process of dendrite presents the non-directional growth characteristic, the casting structure presents a nearly equiaxial crystal state, but compared with a double-phase casting structure, the single-phase casting structure has coarser crystal grains. The alloy structure is analyzed by XRD phaseα-fccMonophasic tissue.
Examples 4 to 5
Tissue evolution of cobalt-chromium-nickel alloy materials with different component ratios
Preparing two groups of components, wherein the component 1 is 62 percent of Co by mass percent; 27% of Cr; 3.9 percent of Ni; 6 percent of Mo; 1% of Fe; and C, preparing a mixture by 0.1 percent. Cr equivalent mass percent: 34.5 percent, and the mass percent of Ni equivalent is as follows: 7.4 percent.
Component 2, 62 percent of Co by mass; 23.5 percent of Cr; 7.4 percent of Ni; 6 percent of Mo; 1% of Fe; and C, preparing a mixture by 0.1 percent. Cr equivalent mass percent: 31 percent, and the mass percent of the Ni equivalent is as follows: 10.9 percent. The preparation process and the melting process were the same as in example 1 except that the ball milling process parameters such as the rotation speed and the ball milling time were changed and the current value adopted in the arc melting process was changed to some extent.
The metallographic structures of the cast alloys of the component 1 and the component 2 are both casting dendritic crystal characteristics and are analyzed by XRD to beα-fcc+ ε-hcpA dual phase alloy. At dendritic boundaries of component 1ε-hcpThe phase volume fraction was 43%. At dendritic boundaries in the cast alloy obtained from component 2ε-hcpThe phase volume fraction was 34%. As is clear from comparative analysis compared with examples 1 to 3, the CoCrNi multicomponent cast alloy is formed by increasing the Ni equivalentα-fcc+ε-hcpConversion of biphasic structure to monophasicα-fccAnd (4) organizing. Hard phases at dendritic boundaries of CoCrNi multicomponent casting alloysε-hcpThe phase decreases as the Ni equivalent increases, from which it can be concluded that the plasticity of the alloy increases as the Ni equivalent increases.
The phase diagram of the pseudo-binary alloy of the cobalt-chromium-nickel multi-element alloy obtained by the above embodiment is shown in FIG. 7. Tc in the graph is the Curie temperature.
Comparative example 1
A preparation method of a cobalt-chromium-nickel multi-element casting alloy is the same as that of example 1 in terms of preparing a mixture according to the mass percent of the components in example 1, and mixing and pressing methods. Putting the blank sample into an electric arc melting furnace, and vacuumizing to 5 multiplied by 10-3Pa, then argon gas with the pressure of 0.05MPa is introduced. Firstly, arc striking is carried out by using 35-50A of current, after arc striking is successful, a cobalt-chromium-nickel alloy blank sample is preheated by using 50A of current, the current is gradually increased after preheating, the smelting current is 50A-300A, and each current is respectively smelted for 10-30 seconds. And then melting the alloy by using a current of 200A, increasing the current to 600A, continuously melting for 30s, opening an absorption casting valve to absorb the alloy into a casting mold, cooling, and then disassembling the casting mold to obtain the cobalt-chromium-nickel cast alloy plate.
FIG. 8 is a metallographic structure of a cobalt-chromium-nickel multicomponent cast alloy obtained in this comparative example, and it can be seen that the alloy structure is a dendritic feature of the cast alloy. Analyzed by XRD to obtainα-fcc+ε-hcpThe dendrite size of the two-phase alloy is smaller than that of the two-phase alloy in example 1. At grain boundariesε-hcpThe volume fraction of phase was 32%, which is close to the results of example 1. The above-described embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and the scope of the present invention is defined by the claims, and equivalents including technical features described in the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (7)
1. A cobalt-chromium-nickel multi-element casting alloy material is characterized in that: the material adopts the method of Co quantitative mass fraction and adjusting the mass fraction of Cr equivalent and Ni equivalent to adjust the alloy phase composition to form a pseudo-binary alloy phase diagram of the CoCrNi multi-element alloy; the phase composition of the cobalt-chromium-nickel cast two-phase alloy is face-centered cubicα-fccPhase and hexagonal close packed hard phaseε-hcpPhase in which the columnar crystal trunk region isα-fccPhase, at the dendrite grain boundary, ofε-hcpAnd (4) phase(s).
2. The cobalt chromium nickel multicomponent casting alloy material of claim 1, wherein: the material is prepared from the following raw material powder: the cobalt-chromium-nickel multi-element alloy material is prepared from Co-Cr-Ni-M-C original powder, wherein the addition amount of each raw material powder is as follows by mass percent: 62 percent; cr: 0 to 31 percent; ni: 0 to 31 percent; mo: 2% -12%; fe: 2% -12%; si: 2% -12%; c: 0.05-0.2%; the sum of the mass fractions of all the alloy elements is 100 percent;
meanwhile, the following expressions (1) and (2) are satisfied:
ni equivalent = Ni +35 × C, range: 1.5 to 34.4 (1);
cr equivalent = Cr + Mo +1.5 × (Fe + Si), range: 7.5 to 38.4 (2).
3. A method for preparing the cobalt-chromium-nickel multi-element alloy material as claimed in any one of claims 1-2, characterized in that the method comprises the following steps:
1) weighing the original powder according to a proportion to prepare mixed powder, and performing wet ball milling on the mixed powder to obtain mixed slurry;
2) drying the mixed slurry obtained in the step 1) in a drying oven to obtain a mixed material;
3) pressing and forming the material obtained in the step 2) to obtain a pressed blank, wherein the pressing pressure is 450-600 MPa;
4) smelting the pressed blank in the step 3) by adopting argon arc to obtain liquid alloy;
5) and 4) cooling the material to room temperature after sintering to obtain the cobalt-chromium-nickel alloy material.
4. The method of claim 3, wherein: in the step 1), absolute ethyl alcohol is used as a dispersing agent, ϕ 5- ϕ 10 steel balls are used as grinding balls, and the ball-to-material ratio is (7-10): 1, rotating speed (211-260) r/min, and mixing time is 48-60 h.
5. The method of claim 3, wherein: granulating through a screen in the step 2), and selecting a screen with 60-80 meshes; the drying temperature is 75-85 ℃.
6. The method of claim 3, wherein: in the step 3), the pressing pressure is 450-600 MPa.
7. The method of claim 3, wherein: in the step 4), the specific operation steps of argon arc melting are as follows:
s1, driving air by adopting argon, igniting electric arc between the tungsten electrode and the water-cooled copper mold, and placing the smelted alloy in the water-cooled copper mold;
s2, the first smelting current value is 300-400A, and the smelting time is 10-30S;
s3, overturning the alloy, and smelting again, wherein the smelting current value is 200-300A, and the smelting time is 10-30S;
obtaining the liquid alloy.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113897561A (en) * | 2021-09-16 | 2022-01-07 | 三峡大学 | In-situ TiB2Reinforced Ni-containing eutectic high-modulus steel material and preparation method thereof |
| CN114480981A (en) * | 2022-01-09 | 2022-05-13 | 三峡大学 | Nano precipitation phase reinforced iron-chromium-nickel-aluminum alloy and preparation method thereof |
| CN115323221A (en) * | 2022-08-19 | 2022-11-11 | 三峡大学 | Cobalt-chromium-nickel alloy, heat treatment process thereof and heat treatment reinforced cobalt-chromium-nickel alloy obtained by using same |
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