CN105624474A - Preparation method of superfine high-grade spherical EP741NP alloy powder - Google Patents
Preparation method of superfine high-grade spherical EP741NP alloy powder Download PDFInfo
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- CN105624474A CN105624474A CN201610219836.XA CN201610219836A CN105624474A CN 105624474 A CN105624474 A CN 105624474A CN 201610219836 A CN201610219836 A CN 201610219836A CN 105624474 A CN105624474 A CN 105624474A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
-
- 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
- B22F9/10—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 using centrifugal force
-
- 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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention relates to a preparation method of superfine high-grade spherical EP741NP alloy powder. The method comprises the following steps: 1) proportionally preparing materials according to the EP741NP alloy composition, and smelting to obtain an EP741NP alloy bar; 2) processing the smelted EP741NP alloy bar into an electrode bar; 3) installing the electrode bar into a reaction chamber, vacuumizing the reaction chamber, and proportionally charging inert gas into the reaction chamber; 4) heating the end of an electrode bar to uniformly melt the end, throwing atomized liquid drops from the end of the electrode bar so that the liquid drops are quickly cooled into spherical particles in an inert gas atmosphere and fall into a collector, wherein a plasma torch comprises a tungsten cathode and a copper anode, and the electrode bar is not used as an electrode; and 5) carrying out electrostatic separation on the prepared EP741NP alloy powder in an inert gas protective atmosphere, screening, sampling and packaging. The EP741NP alloy powder prepared by the method is superfine, and has the characteristics of high purity, high-grade sphericity and no hollow powder or satellite powder.
Description
Technical field
The invention belongs to the metallurgical preparing technical field of superalloy powder, it is specifically related to the preparation method of a kind of ultra-fine high-grade spherical EP741NP powdered alloy.
Background technology
EP741NP is a kind of nickel base superalloy, its composition has salient feature: higher Ti, Al, Nb content, �� ' phase content reaches more than 60%, ensure that the intensity of alloy, alloy has very low Ti/Al ratio simultaneously, add strong carbide simultaneously and form element Hf, Nb etc., reduce the formation trend on primary particle border, and with the addition of the refractory elements such as W, Mo in a large number. Traditional EP741NP alloy preparation technology is PREP powder process+directly hot isostatic pressing shaping+thermal treatment. Unique composition characteristic, ensure that alloy has good creep resistance, fatigue property, and since the 80's of last century, it is widely used in the crucial hot junction component of aerospace.
EP741NP alloy has good damage tolerance, but intensity is lower slightly, limits its application to a certain extent. This and alloy grain size are general thick relevant. Alloy grain size is thick, thus cannot meet requirement of strength. And for powder metallurgy, the grain-size of alloy depends on the granularity of powder to a great extent. Therefore, all the granularity using powder is optimized both at home and abroad. In the 80's, Russia adopts powder size to be 70��315 ��m, develops into 70 ~ 200 ��m afterwards gradually, 50��140 ��m; At present, being limited to capacity of equipment, domestic PREP powder main particle size is 50 ~ 150 ��m, and gas-atomised powders granularity can reach ~ 75 ��m, but the circularity of aerosolization powder is poor, easily there is the more defects such as adhesive powder, hollow powder, satellite powder. Therefore, prepare superfine spherical powder, it is the trend improving alloy property, be a technical problem being badly in need of solving.
Summary of the invention
For overcoming above-mentioned the deficiencies in the prior art, the one method of it is an object of the invention to provide, prepare in EP741NP alloy process that the grain-size occurred is excessive causes that performance is not enough, powder shape is not good causes the problems such as distortion ability to solve powder metallurgical technique, and the problem such as the obtained powdered alloy circularity of the milling method currently generally used is not good, granularity is excessive. The present invention provides the preparation method of a kind of circularity EP741NP powdered alloy ultra-fine, high, it is ensured that the EP741NP alloying constituent after shaping is even, fine microstructures, excellent performance, meets the application requirement of aerospace field.
For achieving the above object, the technical solution used in the present invention is:A kind of ultra-fine high-grade sphericalThe preparation method of EP741NP powdered alloy, comprises the following steps:
1) according to EP741NP base alloy composition for batching, Co:13 ~ 16%, Cr:8.0 ~ 10.0%, Al:4.8 ~ 5.3%, Ti:1.6 ~ 2.0%, W:5.2 ~ 5.9%, Mo:3.5 ~ 4.2%, C:0.02 ~ 0.06%, Hf:0.1 ~ 0.4%, Nb:2.4 ~ 2.8, Ni is matrix, adds the Mg of 0-1wt%, B, Zr, Ce element, adopts vacuum induction melting and electroslag remelting process melting to be smelted into EP741NP alloy bar;
2) the EP741NP alloy bar of melting being carried out essence Vehicle Processing, the diameter of the electrode bar after processing is 10-100mm, and length is 100-1000mm, and roundness deviation is less than 0.1mm, and linearity deviation is less than 0.1mm/m, and roughness is less than 1.6 ��m;
3) electrode bar is loaded to, in reaction chamber, reaction chamber being evacuated to 10-3-10-2Pa, is filled with helium, argon gas or helium to reaction chamber argon-mixed, makes cavity indoor pressure be 0.01-1MPa, in atmosphere, oxygen level is less than 0.1wt%;
4) the plasma gun power of PREP powder manufacturing apparatus is 100-300kW, plasmatorch comprises tungsten cathode and copper anode, electrode bar does not do electrode, electrode bar end is heated by plasma arc, and end is evenly melted, and electrode bar rotating speed is 10000-30000r/min, atomizing droplet is thrown out of from electrode bar end under centrifugal action, and forming drop, drop is cooled to spheroidal particle fast in inert gas environment, falls into reaction chamber bottom collector;
5) under protection of inert gas, to the screening of obtained EP741NP powdered alloy and packaging.
Described EP741NP powdered alloy mean particle size is 40 ��m-500 ��m.
Described EP741NP powdered alloy is the ultrafine powder that mean particle size is less than 50 ��m.
Described step 4) pulverizing process circularity is 90 ~ 95%.
The useful effect of the present invention is:
Use untransferable arc plasma rotating electrode processing, when ultrahigh rotating speed, it is possible to the EP741NP powdered alloy of obtained circularity ultra-fine, high, its profiled member can meet the application demand of aerospace parts.
The powder using present method obtained carries out hip moulding and thermal treatment, and its mechanical property can reach: yield strength is greater than 1100MPa, and tensile strength is greater than 1500MPa, and elongation after fracture is greater than 18%, and relative reduction in area is greater than 20%.
The present invention can obtain, by adjusting process parameter, the EP741NP powdered alloy that mean particle size is 40 ��m-500 ��m, especially the ultrafine powder that mean particle size is less than 50 ��m can be obtained, inclusion is less than 10/kg, and pulverizing process oxygenation amount is controlled within the scope of 100-1000ppm; And the circularity ensureing powder is greater than 90%. The hip moulding part mechanical property of this powder is: yield strength is greater than 1100MPa, and tensile strength is greater than 1500MPa, and elongation after fracture is greater than 18%, and relative reduction in area is greater than 20%.
Accompanying drawing explanation
Fig. 1 is EP741NP powdered alloy stereoscan photograph of the present invention.
Fig. 2 is EP741NP powdered alloy energy spectrum analysis of the present invention.
Fig. 3 is EP741NP powdered alloy circularity of the present invention measuring and calculating photo.
Fig. 4 is the single powder stereoscan photograph of EP741NP alloy of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1
A kind of ultra-fine high-grade sphericalThe preparation method of EP741NP powdered alloy, comprises the following steps:
1) according to EP741NP composition for batching, C:0.034%, Co:16.4%, Cr:9.15%, Al:5.08%, Ti:1.92%, W:5.31%, Mo:3.92%, Nb:2.70, Hf:0.25%, Ni surplus, adopts vacuum induction melting and electroslag remelting process to be smelted into EP741NP alloy bar;
2) the EP741NP alloy bar of melting being carried out essence Vehicle Processing, the electrode bar after processing is: diameter is 50mm, and length is 650mm, roundness deviation 0.02mm, linearity deviation 0.045mm/650mm, roughness 1.14 ��m;
3) electrode bar is loaded to, in reaction chamber, reaction chamber being evacuated to 2 �� 10-3Pa, is filled with helium to reaction chamber, makes cavity indoor pressure be 0.5MPa;
4) the plasma gun power of PREP powder manufacturing apparatus is 200kW, plasmatorch comprises tungsten cathode and copper anode, electrode bar does not do electrode, electrode bar end is heated by plasma body, electrode bar rotating speed is 22000r/min, and end is evenly melted, and atomizing droplet is thrown out of from electrode bar end under centrifugal action and forms drop, drop is cooled to spheroidal particle fast in inert gas environment, falls into reaction chamber bottom collector;
5) under protection of inert gas, to the screening of obtained EP741NP powdered alloy and packaging.
Described EP741NP powdered alloy mean particle size is 78 ��m.
Embodiment 2
A kind of ultra-fine high-grade sphericalThe preparation method of EP741NP powdered alloy, comprises the following steps:
1) according to EP741NP composition for batching, C:0.046%, Co:16.0%, Cr:8.92%, Al:4.90%, Ti:1.80%, W:5.51%, Mo:4.22%, Nb:2.42, Hf:0.29%, Ni surplus, is smelted into EP741NP alloy bar.
2) the EP741NP alloy bar of melting being carried out essence Vehicle Processing, the electrode bar after processing is: diameter is 20mm, and length is 300mm, roundness deviation 0.02mm, and whether linearity deviation 0.03mm/300mm[is correct], roughness 0.58 ��m;
3) electrode bar is loaded to, in reaction chamber, reaction chamber being evacuated to 7 �� 10-3Pa, is filled with helium to reaction chamber, makes cavity indoor pressure be 0.07MPa;
4) the plasma gun power of PREP powder manufacturing apparatus is 100kW, plasmatorch comprises tungsten cathode and copper anode, electrode bar does not do electrode, electrode bar end is heated by plasma body, electrode bar rotating speed is 15000r/min, and end is evenly melted, and atomizing droplet is thrown out of from electrode bar end under centrifugal action and forms drop, drop is cooled to spheroidal particle fast in inert gas environment, falls into reaction chamber bottom collector;
5) under protection of inert gas, to the screening of obtained EP741NP powdered alloy and packaging.
Described EP741NP powdered alloy mean particle size is 231 ��m.
Described step 4) powder circularity is 93.5%.
Embodiment 3
A kind of ultra-fine high-grade sphericalThe preparation method of EP741NP powdered alloy, comprises the following steps:
1) according to EP741NP composition for batching, C:0.038%, Co:15.8%, Cr:9.36%, Al:4.84%, Ti:1.95%, W:5.28%, Mo:4.14%, Nb:2.50, Hf:0.23%, Ni surplus, is smelted into EP741NP alloy bar;
2) the EP741NP alloy bar of melting being carried out essence Vehicle Processing, the electrode bar after processing is: diameter is 95mm, and length is 900mm, roundness deviation 0.07mm, linearity deviation 0.07mm/900mm, roughness 0.86 ��m;
3) electrode bar is loaded to, in reaction chamber, reaction chamber being evacuated to 3 �� 10-3Pa, is filled with helium to reaction chamber, makes cavity indoor pressure be 0.2MPa;
4) the plasma gun power of PREP powder manufacturing apparatus is 300kW, plasmatorch comprises tungsten cathode and copper anode, electrode bar does not do electrode, electrode bar end is heated by plasma body, electrode bar rotating speed is 28000r/min, and end is evenly melted, and atomizing droplet is thrown out of from electrode bar end under centrifugal action and forms drop, drop is cooled to spheroidal particle fast in inert gas environment, falls into reaction chamber bottom collector;
5) under protection of inert gas, to the screening of obtained EP741NP powdered alloy and packaging.
Described EP741NP powdered alloy mean particle size is 41 ��m.
Described step 4) powder circularity is 91.2%.
From microscopic appearance, the overall shape looks of described powder and power spectrum as shown in Figure 1, Figure 2 and Figure 4, can find out that EP741NP powdered alloy prepared by the method is very pure, circularity height, it does not have aspherical powder particle. Above-mentioned powder being carried out hip moulding, and heat-treats, its mechanical property is: yield strength 1136MPa, tensile strength 1522MPa, elongation after fracture 19%, relative reduction in area 20%, it is possible to meet the application demand of aerospace field.
Fig. 3 is the process calculating powder circularity. Adopt ImageJ software, powder is distinguished according to different contrast, thus calculates the circularity of powder.
Table 1 is EP741NP energy spectrogram.
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Claims (4)
1. the preparation method of a ultra-fine high-grade spherical EP741NP powdered alloy, it is characterised in that, comprise the following steps:
1) according to EP741NP base alloy composition for batching, Co:13 ~ 16%, Cr:8.0 ~ 10.0%, Al:4.8 ~ 5.3%, Ti:1.6 ~ 2.0%, W:5.2 ~ 5.9%, Mo:3.5 ~ 4.2%, C:0.02 ~ 0.06%, Hf:0.1 ~ 0.4%, Nb:2.4 ~ 2.8, Ni is matrix, adds the Mg of 0-1wt%, B, Zr, Ce element, adopts vacuum induction melting and electroslag remelting process melting EP741NP alloy bar;
2) the EP741NP alloy bar of melting being carried out essence Vehicle Processing, the diameter of the electrode bar after processing is 10-100mm, and length is 100-1000mm, and roundness deviation is less than 0.1mm, and linearity deviation is less than 0.1mm/m, and roughness is less than 1.6 ��m;
3) loading electrode bar to, in reaction chamber, reaction chamber being evacuated to 10-3-10-2Pa, be filled with helium, argon gas or helium to reaction chamber argon-mixed, make cavity indoor pressure be 0.01-1MPa, in atmosphere, oxygen level is less than 0.1wt%;
4) the plasma gun power of PREP powder manufacturing apparatus is 100-300kW, plasmatorch comprises tungsten cathode and copper anode, electrode bar does not do electrode, electrode bar end is heated by plasma body, and electrode bar end is evenly melted, and electrode bar rotating speed is 10000-30000r/min, atomizing droplet is thrown out of from electrode bar end under centrifugal action, forming drop, drop is cooled to spheroidal particle fast in inert gas environment, falls into reaction chamber bottom collector;
5) under protection of inert gas, to the screening of obtained EP741NP powdered alloy and packaging.
2. the preparation method of a kind of ultra-fine high-grade spherical EP741NP powdered alloy according to claim 1, it is characterised in that, described EP741NP powdered alloy mean particle size is 40 ��m-500 ��m.
3. the preparation method of a kind of ultra-fine high-grade spherical EP741NP powdered alloy according to claim 1, it is characterised in that, described EP741NP powdered alloy is the ultrafine powder that mean particle size is less than 50 ��m.
4. the preparation method of a kind of ultra-fine high-grade spherical EP741NP powdered alloy according to claim 1, it is characterised in that, in described step 4) pulverizing process, circularity is 90-95%.
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| CN106312083A (en) * | 2016-09-23 | 2017-01-11 | 中国科学院合肥物质科学研究院 | Preparation process suitable for low activation martensitic steel microsphere powder |
| CN106348308A (en) * | 2016-08-31 | 2017-01-25 | 赵放 | High-melting-point metal powder, solid propellant and process for preparing same by using boron powder |
| CN106670486A (en) * | 2016-12-19 | 2017-05-17 | 西安欧中材料科技有限公司 | Preparation method for aluminium alloy powder for near-net forming |
| CN106670482A (en) * | 2016-12-19 | 2017-05-17 | 西安欧中材料科技有限公司 | Preparing method for superfine high-grade spherical GH4133 alloy powder |
| CN106670487A (en) * | 2016-12-19 | 2017-05-17 | 西安欧中材料科技有限公司 | Rotating electrode preparing micro spherical metal powder and method of rotating electrode |
| CN106735276A (en) * | 2016-12-19 | 2017-05-31 | 西安欧中材料科技有限公司 | A kind of preparation method of high-quality globular powdered nickel |
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| CN107119211A (en) * | 2017-06-29 | 2017-09-01 | 西安欧中材料科技有限公司 | A kind of preparation method of 3D printing Ni3Al base alloy powders |
| CN107900368A (en) * | 2017-12-21 | 2018-04-13 | 西安欧中材料科技有限公司 | A kind of preparation method of MCrAlY alloy powder used for plasma spraying |
| JP2019044209A (en) * | 2017-08-30 | 2019-03-22 | 山陽特殊製鋼株式会社 | Ni-BASED SUPERALLOY POWDER FOR LAMINATE MOLDING |
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| CN110643857A (en) * | 2019-09-29 | 2020-01-03 | 西安欧中材料科技有限公司 | Nickel-based alloy powder without original grain boundary and preparation method thereof |
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