CN115283682B - Preparation method of nickel-based alloy powder with high tungsten content - Google Patents
Preparation method of nickel-based alloy powder with high tungsten content Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 144
- 239000000956 alloy Substances 0.000 title claims abstract description 144
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 79
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 74
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000010937 tungsten Substances 0.000 title claims abstract description 72
- 239000000843 powder Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000003723 Smelting Methods 0.000 claims abstract description 25
- 238000009689 gas atomisation Methods 0.000 claims abstract description 22
- 230000006698 induction Effects 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims description 42
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 239000011651 chromium Substances 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 229910000521 B alloy Inorganic materials 0.000 claims description 4
- QDWJUBJKEHXSMT-UHFFFAOYSA-N boranylidynenickel Chemical compound [Ni]#B QDWJUBJKEHXSMT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910000592 Ferroniobium Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000004663 powder metallurgy Methods 0.000 abstract description 6
- 238000005204 segregation Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000002844 melting Methods 0.000 description 20
- 230000008018 melting Effects 0.000 description 20
- 239000000155 melt Substances 0.000 description 11
- 239000002245 particle Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 238000000889 atomisation Methods 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 230000005674 electromagnetic induction Effects 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910000816 inconels 718 Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- MOWMLACGTDMJRV-UHFFFAOYSA-N nickel tungsten Chemical compound [Ni].[W] MOWMLACGTDMJRV-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 238000011090 industrial biotechnology method and process Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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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
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- 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
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
-
- 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
- B22F2009/0824—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 with a specific atomising fluid
-
- 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
- B22F2009/0848—Melting process before atomisation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to the technical field of powder metallurgy, in particular to a preparation method of nickel-based alloy powder with high tungsten content. The method adopts vacuum induction smelting technology and tight coupling gas atomization technology to prepare nickel-based alloy powder with high tungsten content. Compared with the prior art, the invention effectively solves the defects of refractory ingredients, component segregation and high bar cost in the preparation of the traditional high-tungsten nickel-based alloy powder, and the prepared high-tungsten nickel-based alloy powder has the comprehensive advantages of stable ingredients, high sphericity, low oxygen content, low impurity content, low production cost and the like.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a preparation method of nickel-based alloy powder with high tungsten content.
Background
Powder metallurgy is an industrial technique for producing metal powders or producing metal materials, composite materials, and various types of products from metal powders (or a mixture of metal powders and non-metal powders) as raw materials by forming and sintering. The powder metallurgy technology is widely applied to the fields of traffic, machinery, electronics, aerospace, weapons, biology, new energy, information, nuclear industry and the like, and becomes one of the branches with the most development activity in new material science. The powder metallurgy technology has a series of advantages of remarkable energy conservation, material saving, excellent performance, high product precision, good stability and the like, and is very suitable for mass production. In addition, materials and complex parts that cannot be produced in part by conventional casting and machining methods can also be produced by powder metallurgy techniques and are therefore of great importance to the industry.
Vacuum induction melting (Vacuum induction melting, abbreviated as VIM) is a metal process for melting metal under vacuum by using electromagnetic induction heating principle. Eddy currents are generated during electromagnetic induction to melt the metal. The process can be used to increase the purity of the alloy and reduce the oxygen content of the alloy.
The main method for preparing the alloy powder is an air atomization method. The basic principle of the gas atomization method is that liquid metal flow is broken into small liquid drops by high-speed air flow and is quickly solidified to form powder, and the powder prepared by the gas atomization method has the advantages of high purity, low oxygen content, controllable powder granularity, low production cost, high sphericity and the like, so that the powder has become the main development direction of the preparation technology of high-performance and special alloy powder.
Chinese patent CN101497953a discloses an intermediate layer alloy for transient liquid phase connection of nickel-base single crystal superalloy and a preparation method thereof, which is mainly used for transient liquid phase connection of nickel-base single crystal superalloy. The intermediate layer alloy contains Ni, cr, co, W, mo, ta, B and other elements, and master alloy is smelted in a vacuum induction furnace; the nickel-based alloy powder is prepared by adopting an ultrasonic gas atomization method. The boron element is added to the interlayer alloy as a melting point reducing element to achieve a suitable melting temperature for the alloy. In the patent, the tungsten content of the intermediate layer alloy is 5-7wt% and the tungsten content is lower, the intermediate layer alloy is prepared by firstly mixing and melting ingredients, casting into a spindle, and then using the spindle as a master alloy to carry out ultrasonic atomization, so that the preparation method of the traditional nickel-based alloy powder is not related to specific methods of feeding and smelting, and meanwhile, the problem of stability and uniformity of alloy components is not considered in the patent.
Chinese patent CN110640151a provides a nickel-based alloy comprising: 18.0 to 23.5 weight percent of cobalt; 10-15 wt% of chromium; 2.5 to 3.5 weight percent of aluminum; 2.0 to 4.0 weight percent of titanium; 0.1 to 2.0 weight percent of niobium; 1.0 to 3.0 weight percent of tantalum; 0 to 2.5wt% of tungsten; 4 to 5.5 weight percent of molybdenum; 0.03 to 0.1 weight percent of zirconium; 0 to 1.0wt% of hafnium; 0.01 to 0.1 weight percent of carbon; 0.01 to 0.1 weight percent of boron; the balance nickel. The patent relates to a preparation method of nickel-based alloy powder containing tungsten, which adopts the same gas atomization method, the same tungsten content in the patent is lower, the patent is a traditional preparation method of nickel-based alloy powder, the patent does not relate to a specific method of feeding and smelting, and meanwhile, the patent does not consider the stability and uniformity of alloy components.
Chinese patent CN106735273a discloses an Inconel718 nickel base alloy powder for selective laser melting forming and a preparation method thereof. The method comprises the steps of adopting a vacuum electrode induction melting gas atomization technology and combining a high-pressure atomizer to prepare metal powder, and then adopting an ultrasonic vibration screening and gas flow classification method to mix metal powder with different particle sizes according to a certain proportion to obtain the Inconel718 nickel-based alloy powder for selective laser melting, wherein the particle sizes of the Inconel718 nickel-based alloy powder are uniform. The alloy comprises the following components in percentage by weight: ni: more than or equal to 50 percent, cr: 17-21%, mo:2.8 to 3.3 percent of Al:0.2 to 0.8 percent, ti: 0.65-1.15%, nb:4.75 to 5.5 percent, C: less than or equal to 0.08 percent, mn: less than or equal to 0.35 percent, si: less than or equal to 0.35 percent, cu: less than or equal to 0.3 percent, co: less than or equal to 1.0 percent, B: less than or equal to 0.006 percent, P: less than or equal to 0.01 percent, S: less than or equal to 0.01 percent. The patent adopts a rotary electrode gas atomization powder preparation technology, the raw material is common In718 alloy, and tungsten element is not contained In nickel-based alloy powder; the powder preparation method does not need a crucible or a leakage ladle, but processes a single master alloy rod, then hangs in a vacuum chamber, heats and melts the bottom of a bar, and drops the melted liquid drop into a spray disc to be atomized into powder, thus being a traditional preparation process.
Disclosure of Invention
Since tungsten has a high melting point and low solubility in other metals, if the tungsten content is too high, problems of incomplete melting and problems of alloy components are likely to occur, and the object of the present invention is to provide a method for preparing nickel-based alloy powder with high tungsten content. The invention adopts vacuum induction melting gas atomization powder preparation, and the finally prepared nickel-based alloy powder with high tungsten content has the performance characteristics of uniform components, low impurity content, high sphericity, low oxygen content and the like, and can be well applied to the laser cladding technology.
The aim of the invention can be achieved by the following technical scheme:
the invention provides a preparation method of nickel-based alloy powder with high tungsten content, which comprises the following steps:
(1) Material preparation: preparing a nickel-based alloy raw material with high tungsten content, wherein the W content of the nickel-based alloy with high tungsten content is not less than 18wt%, mixing and pressing all tungsten powder and part of nickel powder in the nickel-based alloy raw material with high tungsten content to obtain a nickel-tungsten green compact, paving a layer of nickel plate at the bottom of a smelting furnace, feeding according to the reciprocating sequence of tungsten bars, nickel plates, tungsten bars and nickel plates until tungsten and nickel are all added into the furnace, and then sequentially adding other alloy raw materials with high tungsten content into the nickel-based alloy raw material with high tungsten content;
(2) Alloy smelting: vacuum induction smelting is carried out on the nickel-based alloy raw material with high tungsten content in the furnace to obtain alloy melt;
(3) Atomizing and pulverizing: pouring the alloy melt into a tundish, allowing the alloy melt to flow into a gas atomizing furnace through a drain hole at the bottom of the tundish, crushing the alloy melt into fine droplets under the impact of high-speed airflow, cooling and solidifying to obtain alloy powder, allowing the powder to fall at the bottom of an atomizing tower, and allowing the powder to be brought into a powder collecting device under a cyclone by gas.
In one embodiment of the present invention, in step (1), the high tungsten content nickel-based alloy feedstock is Ni, fe, cr, nb or Mo, S, W, C, B; wherein the W content is not less than 18wt%.
In the scheme provided by the invention, in the step (1), tungsten bars are put into the bottom of the smelting furnace in the feeding process, then nickel plates are added, and the rest raw materials are used as secondary feeding. In the nickel-base alloy with high tungsten content, partial elements have an inhibition effect on the melting of tungsten in nickel, so nickel and tungsten are melted first to form alloy melt, the melting time can be effectively shortened, and component deviation caused by the fact that tungsten cannot be completely melted in the alloy solution is avoided.
In one embodiment of the invention, in the step (2), the vacuum degree in the vacuum induction furnace in the vacuum induction smelting process is lower than 1 multiplied by 10 -2 Pa; the high vacuum is beneficial to reduce the oxygen content of the powder.
In the step (2), after the nickel and tungsten raw materials in the furnace are completely melted to obtain alloy melt, other residual raw materials are added through secondary feeding, and heating is continued after all the alloy raw materials are completely melted, so that the superheat degree of the alloy melt reaches 200-230 ℃.
In a preferred embodiment of the invention, in the step (2), after the melt reaches the temperature, the intermediate frequency power is continuously adjusted to enable the power to continuously reciprocate between 30kW and 90kW, the superheat degree of the alloy melt is controlled to be 250-280 ℃, and the total duration of the process is 1.5h. In the smelting heating process, electromagnetic induction can exert force on the melt in the furnace, and is particularly obvious under high power, so that the power is regulated to enable the melt to continuously reciprocate between 30kW and 90kW, the electromagnetic stirring of the induction furnace on the melt is facilitated while the temperature stability of the melt is ensured, W is uniformly distributed in the whole melt, and component segregation of alloy powder is avoided.
In a preferred embodiment of the invention, in step (3), the temperature in the tundish is controlled between 1150 and 1250 ℃. It should be noted that the temperature of the leakage package has a larger influence on the atomization process, when the temperature of the leakage package is too low, the heat dissipation speed of the alloy liquid is too high, the alloy liquid is easy to condense in the leakage package, and the leakage hole is easy to be blocked; the temperature of the tundish should be raised as much as possible, as allowed by the plant conditions. Meanwhile, the invention designs a leak hole heating system, which uses graphite to transfer heat to leak holes, and controls the temperature to 1200-1300 ℃, thereby further reducing the probability of leak hole blockage.
In a preferred embodiment of the present invention, in step (3), the gas in the gas atomization furnace is an inert gas.
In one embodiment of the present invention, the inert gas is preferably high purity argon or high purity nitrogen, and the atomization pressure in the gas atomization furnace is 3.0-4.5MPa.
Since tungsten has a high melting point and low solubility in other metals, if the tungsten content is too high, incomplete melting is likely to occur, resulting in problems with alloy composition. The technical scheme mainly aims at solving the problems that tungsten is easy to appear in the preparation of nickel-based alloy powder with high tungsten content (more than 18 wt%) and the alloy components are not completely melted and segregation occurs.
Compared with the prior art, the invention has the following advantages:
the nickel-base alloy powder with high tungsten content prepared by the invention has low impurity content, low oxygen content (less than or equal to 200 ppm), stable component (W content loss less than 0.5 wt%) and uniform particle size distribution, high sphericity of powder particles (average sphericity of powder below 180 mu m is more than or equal to 0.80), and good powder flowability (less than or equal to 19s/50 g).
Drawings
FIG. 1 is a schematic diagram of the feed sequence of the feedstock according to the present invention;
1: a secondary hopper; 2: a crucible; 3: a nickel plate; 4: tungsten bars; 5: the rest raw materials.
FIG. 2 is a graph showing the morphology of nickel-base alloy powder particles with high tungsten content obtained in example 1 of the present invention.
FIG. 3 is a graph showing the morphology of nickel-base alloy powder particles with high tungsten content obtained in example 2 of the present invention.
Detailed Description
The invention provides a preparation method of nickel-based alloy powder with high tungsten content, which comprises the following steps:
(1) Material preparation: preparing a nickel-based alloy raw material with high tungsten content, wherein the W content of the nickel-based alloy with high tungsten content is not less than 18wt%, mixing and pressing all tungsten powder and part of nickel powder in the nickel-based alloy raw material with high tungsten content to obtain a nickel-tungsten green compact, paving a layer of nickel plate at the bottom of a smelting furnace, feeding according to the reciprocating sequence of tungsten bars, nickel plates, tungsten bars and nickel plates until tungsten and nickel are all added into the furnace, and then sequentially adding other alloy raw materials with high tungsten content into the nickel-based alloy raw material with high tungsten content;
(2) Alloy smelting: vacuum induction smelting is carried out on the nickel-based alloy raw material with high tungsten content in the furnace to obtain alloy melt;
(3) Atomizing and pulverizing: pouring the alloy melt into a tundish, allowing the alloy melt to flow into a gas atomizing furnace through a drain hole at the bottom of the tundish, crushing the alloy melt into fine droplets under the impact of high-speed airflow, cooling and solidifying to obtain alloy powder, allowing the powder to fall at the bottom of an atomizing tower, and allowing the powder to be brought into a powder collecting device under a cyclone by gas.
In one embodiment of the present invention, in step (1), the high tungsten content nickel-based alloy feedstock is Ni, fe, cr, nb or Mo, S, W, C, B; wherein the W content is not less than 18wt%.
In a preferred embodiment of the invention, in the step (1), tungsten bars are placed at the bottom of the smelting furnace in the feeding process, then nickel plates are added, and the rest raw materials are used as secondary feeding.
In one embodiment of the present invention, in step (1), in the nickel-base alloy with high tungsten content, part of the elements have an inhibiting effect on the melting of tungsten in nickel, so that nickel and tungsten are melted first to form an alloy melt, the melting time can be effectively shortened, and the component deviation caused by the fact that tungsten cannot be completely melted in the alloy solution is avoided.
In one embodiment of the invention, in the step (2), the vacuum degree in the vacuum induction furnace in the vacuum induction smelting process is lower than 1 multiplied by 10 -2 Pa; the high vacuum is beneficial to reduce the oxygen content of the powder.
In the step (2), after the nickel and tungsten raw materials in the furnace are completely melted to obtain alloy melt, other residual raw materials are added through secondary feeding, and heating is continued after all the alloy raw materials are completely melted, so that the superheat degree of the alloy melt reaches 200-230 ℃.
In a preferred embodiment of the invention, in the step (2), after the melt reaches the temperature, the intermediate frequency power is continuously adjusted to enable the power to continuously reciprocate between 30kW and 90kW, the superheat degree of the alloy melt is controlled to be 250-280 ℃, and the total duration of the process is 1.5h. In the smelting heating process, electromagnetic induction can exert force on the melt in the furnace, and is particularly obvious under high power, so that the power is regulated to enable the melt to continuously reciprocate between 30kW and 90kW, the electromagnetic stirring of the induction furnace on the melt is facilitated while the temperature stability of the melt is ensured, W is uniformly distributed in the whole melt, and component segregation of alloy powder is avoided.
In a preferred embodiment of the invention, in step (3), the temperature in the tundish is controlled between 1150 and 1250 ℃. It should be noted that the temperature of the leakage package has a larger influence on the atomization process, when the temperature of the leakage package is too low, the heat dissipation speed of the alloy liquid is too high, the alloy liquid is easy to condense in the leakage package, and the leakage hole is easy to be blocked; the temperature of the tundish should be raised as much as possible, as allowed by the plant conditions.
In a preferred embodiment of the present invention, in step (3), graphite is used to transfer heat to the leak holes, and the graphite temperature is controlled to 1200-1300 ℃, so as to further reduce the probability of leak hole blockage.
In a preferred embodiment of the present invention, in step (3), the gas in the gas atomization furnace is an inert gas.
In one embodiment of the present invention, the inert gas is preferably high purity argon or high purity nitrogen, and the atomization pressure in the gas atomization furnace is 3.0-4.5MPa.
Fig. 1 shows a schematic raw material charging sequence when preparing nickel-base alloy powder with high tungsten content, wherein the rest raw materials 5 are filled in the secondary charging hopper 1, and tungsten bars 4 and nickel plates 3 are filled in the crucible 2, wherein the tungsten bars 4 and the nickel plates 3 are charged according to the arrangement mode of fig. 1.
The invention will now be described in detail with reference to the drawings and specific examples.
Example 1
The embodiment provides a preparation method of nickel-based alloy powder with high tungsten content.
(1) Material preparation: preparing a high-tungsten-content nickel-based alloy raw material, wherein the components of the high-tungsten-content nickel-based alloy raw material meet the following requirements in percentage by mass: ni:55.2%, fe:1.2%, cr:15%, nb:0.7%, si:4.3%, W:20%, C:0.7%, B:2.9%. As shown in figure 1, tungsten bars are placed at the bottom of the smelting furnace during charging, and then nickel plates are added. Then placing pure chromium, pure iron, nickel-boron alloy, ferrocolumbium, silicon and carbon blocks into a secondary charging hopper;
(2) Alloy smelting: vacuum induction melting is carried out on the alloy raw materials. Controlling the vacuum degree in the vacuum induction furnace to be 0.9x10 -2 Pa. After the nickel and tungsten raw materials in the furnace are completely melted to obtain alloy melt, a secondary charging hopper is opened, the rest raw materials are added, and the heating is continued, so that the temperature of the alloy melt reaches 1630 ℃. Continuously adjusting the intermediate frequency power to enable the power to continuously reciprocate between 30kW and 90kW, controlling the temperature of alloy melt to be 1670 ℃, and enabling the duration of the process to be 1.5 hours; the temperature in the middle leakage ladle is controlled at 1230 ℃; the temperature of the bottom leak hole of the middle leak ladle is controlled at 1250 ℃;
(3) Atomizing and pulverizing: pouring the alloy melt into a tundish, allowing the alloy melt to flow downwards into a gas atomizing furnace through a drain hole at the bottom of the tundish, wherein inert gas is high-purity argon, the atomizing pressure in the gas atomizing furnace is 4.0MPa, and the alloy melt is crushed into fine liquid drops, cooled and solidified to obtain alloy powder.
The morphology of the alloy powder particles prepared in this example is shown in FIG. 2, the average particle diameter below 180 μm is 44.62. Mu.m, the sphericity is 0.83, the fluidity is 19.5s/50g, the oxygen content is 147ppm, and the W content is 19.7wt%.
Example 2
The embodiment provides a preparation method of nickel-based alloy powder with high tungsten content.
(1) Material preparation: preparing a high-tungsten-content nickel-based alloy raw material, wherein the components of the high-tungsten-content nickel-based alloy raw material meet the following requirements in percentage by mass: ni:47.4%, fe:4.8%, cr:15%, mo:5%, si:2.8%, W:22%, C:0.5%, B:2.5%. As shown in figure 1, tungsten bars are placed at the bottom of the smelting furnace during charging, and then nickel plates are added. Then putting pure molybdenum, pure chromium, pure iron, nickel-boron alloy, silicon and carbon blocks into a secondary charging hopper;
(2) Alloy smelting: vacuum induction melting is carried out on the alloy raw materials. Controlling the vacuum degree in the vacuum induction furnace to be 0.8x10 -2 Pa. After the alloy raw materials in the furnace are completely melted to obtain alloy melt, opening two partsAnd adding the rest raw materials into a secondary charging hopper, and continuously heating to enable the temperature of the alloy liquid to reach 1650 ℃. Continuously adjusting the intermediate frequency power to enable the power to continuously reciprocate between 30kW and 90kW, controlling the temperature of alloy melt to 1680 ℃, and enabling the duration of the process to be 1.5 hours; the temperature in the middle leakage ladle is controlled at 1220 ℃; the temperature of the bottom leak hole of the middle leak ladle is controlled at 1240 ℃;
(3) Atomizing and pulverizing: pouring the alloy melt into a tundish, allowing the alloy melt to flow downwards into a gas atomizing furnace through a drain hole at the bottom of the tundish, wherein inert gas is high-purity argon, the atomizing pressure in the gas atomizing furnace is 4.3MPa, and the alloy melt is crushed into fine liquid drops, cooled and solidified to obtain alloy powder.
The morphology of the alloy powder particles prepared in this example is shown in FIG. 3, the average particle diameter of the alloy powder particles is below 180 μm, the sphericity is 0.84, the fluidity is 18.6s/50g, the oxygen content is 153ppm, and the W content is 21.8wt%.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (2)
1. The preparation method of the nickel-based alloy powder with high tungsten content is characterized by comprising the following steps of:
(1) Material preparation: preparing a high-tungsten-content nickel-based alloy raw material, wherein the components of the high-tungsten-content nickel-based alloy raw material meet the following requirements in percentage by mass: ni:55.2%, fe:1.2%, cr:15%, nb:0.7%, si:4.3%, W:20%, C:0.7%, B:2.9%; during charging, tungsten bars are placed at the bottom of a smelting furnace, then nickel plates are added, and then pure chromium, pure iron, nickel-boron alloy, ferrocolumbium, silicon and carbon blocks are placed in a secondary charging hopper;
(2) Alloy smelting: for alloy raw materialVacuum induction smelting the material, and controlling the vacuum degree in the vacuum induction furnace to be 0.9x10 - 2 Pa, after the nickel and tungsten raw materials in the furnace are completely melted to obtain alloy melt, opening a secondary charging hopper, adding the rest raw materials, and continuously heating to ensure that the temperature of the alloy melt reaches 1630 ℃; continuously adjusting the intermediate frequency power to enable the power to continuously reciprocate between 30kW and 90kW, controlling the temperature of alloy melt to be 1670 ℃, and enabling the duration of the process to be 1.5 hours; the temperature in the middle leakage ladle is controlled at 1230 ℃; the temperature of the bottom leak hole of the middle leak ladle is controlled at 1250 ℃;
(3) Atomizing and pulverizing: pouring the alloy melt into a tundish, allowing the alloy melt to flow downwards into a gas atomizing furnace through a drain hole at the bottom of the tundish, wherein inert gas is high-purity argon, the atomizing pressure in the gas atomizing furnace is 4.0MPa, and the alloy melt is crushed into fine liquid drops, cooled and solidified to obtain alloy powder.
2. The preparation method of the nickel-based alloy powder with high tungsten content is characterized by comprising the following steps of:
(1) Material preparation: preparing a high-tungsten-content nickel-based alloy raw material, wherein the components of the high-tungsten-content nickel-based alloy raw material meet the following requirements in percentage by mass: ni:47.4%, fe:4.8%, cr:15%, mo:5%, si:2.8%, W:22%, C:0.5%, B:2.5 percent, during charging, tungsten bars are put at the bottom of a smelting furnace, then nickel plates are added, and then pure molybdenum, pure chromium, pure iron, nickel boron alloy, silicon and carbon blocks are put into a secondary charging hopper;
(2) Alloy smelting: vacuum induction smelting is carried out on the alloy raw material, and the vacuum degree in the vacuum induction furnace is controlled to be 0.8x10 - 2 Pa, after the alloy raw materials in the furnace are completely melted to obtain an alloy melt, opening a secondary charging hopper, adding the rest raw materials, continuously heating to enable the temperature of the alloy liquid to reach 1650 ℃, continuously adjusting the medium-frequency power to enable the power to continuously reciprocate between 30kW and 90kW, controlling the temperature of the alloy melt to be 1680 ℃, and enabling the duration of the process to be 1.5 hours; the temperature in the middle leakage ladle is controlled at 1220 ℃; the temperature of the bottom leak hole of the middle leak ladle is controlled at 1240 ℃;
(3) Atomizing and pulverizing: pouring the alloy melt into a tundish, allowing the alloy melt to flow downwards into a gas atomizing furnace through a drain hole at the bottom of the tundish, wherein inert gas is high-purity argon, the atomizing pressure in the gas atomizing furnace is 4.3MPa, and the alloy melt is crushed into fine liquid drops, cooled and solidified to obtain alloy powder.
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