CN106636702B - A kind of preparation method of the Ni-based foundry alloy of low oxygen content high-alloying and powder - Google Patents

A kind of preparation method of the Ni-based foundry alloy of low oxygen content high-alloying and powder Download PDF

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CN106636702B
CN106636702B CN201611100779.XA CN201611100779A CN106636702B CN 106636702 B CN106636702 B CN 106636702B CN 201611100779 A CN201611100779 A CN 201611100779A CN 106636702 B CN106636702 B CN 106636702B
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powder
alloy
melting
alloying
foundry alloy
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CN106636702A (en
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曲选辉
陈晓玮
章林
刘烨
李向前
单化杰
秦明礼
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University of Science and Technology Beijing USTB
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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
    • C22C1/02—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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • 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%

Abstract

The preparation method of a kind of Ni-based foundry alloy of low oxygen content high-alloying and powder, belongs to field of powder metallurgy, its technological process is：Pure mother alloy ingot is prepared using the duplex technique of vacuum melting+electroslag remelting first.During vacuum melting, using lime crucible, and by being pre-processed to raw material, refining period add carbon block and carry out deoxidation, supplement easy scaling loss element in melting latter stage, obtain designing the mother alloy ingot of composition.During electroslag melting, the parameter such as shape, depth, viscosity by adjusting slag bath create nonmetal inclusion floating condition, make the further sublimate of foundry alloy.It is broken to mother alloy ingot progress high-speed disc worn-off under protective atmosphere after the mother alloy ingot peeling after electroslag remelting, obtain ultra-fine master alloy powder.The K418 master alloy powders prepared using this method, particle diameter are respectively less than 20 μm, and oxygen content is less than 200ppm, sulfur content is less than 20ppm, after being mixed with carbonyl nickel powder, the production cost and process energy consumption of powder metallurgy superalloy in lower temperature sintering densification, can be substantially reduced.

Description

A kind of preparation method of the Ni-based foundry alloy of low oxygen content high-alloying and powder
Technical field
The invention belongs to field of powder metallurgy, there is provided the system of a kind of Ni-based foundry alloy of low oxygen content high-alloying and powder Preparation Method.
Background technology
Foundry alloy method is that the alloying element in material is prepared into the fine master alloy powder of high-alloying, then by foundry alloy Powder and matrix element powder are mixed in corresponding ratio, sinter the uniform alloy of composition into afterwards.This method is by increasing powder Last specific surface area and distortion of lattice, the chemical composition gradient between powder is improved to improve the driving of atomic migration in sintering process Gesture.The appearance temperature of liquid phase in sintering process and quantity are controlled by rationally designing foundry alloy composition, further reduces particle The resistance of rearrangement, sintering activity is improved, reduce sintering temperature.This provides new for low cost manufacture Ni-base P/M Superalloy By way of.
It is the premise for preparing high-performance Ni-base P/M Superalloy to obtain the Ni-based master alloy powder of low oxygen content high-alloying Condition.Active element Cr, Al, Ti and Zr content are closed far above common nickel-base high-temperature in high-alloying nickel-base alloy foundry alloy Gold.In sintering process, impurity oxygen can form more serious oxide folder to master alloy powder particle surface and crystal boundary migration It is miscellaneous, the comprehensive mechanical property of material is greatly lowered, therefore the oxygen content of master alloy powder has important shadow to properties of product Ring.The present invention prepares the female conjunction of high-alloying nickel-base alloy using the duplex technique of vacuum induction melting+inert atmosphere electroslag melting Gold.Vacuum induction melting can effectively control the chemical composition of alloy, it is therefore prevented that in high-alloying nickel-base alloy liquation and air The contact of hydrogen-oxygen nitrogen, but vacuum induction ingot casting is easily polluted by refractory crucible, introduces ceramic inclusions.Electroslag remelting mistake Cheng Zhong, the slag system for being adapted to Ni-based foundry alloy remelting is designed, the molten alloy droplets of fusing is passed through the molten slag layer of high temperature high activity dropwise, Provide extraordinary thermodynamics and kineticses condition for the floating of field trash, be remove alloy in non-metallic inclusion and efficiently One of maximally effective refinery practice of desulfurization, the content of sulphur can be effectively reduced, remove large scale foreing impuritys, be mingled with interior life Disperse refinement distribution, reduce active element Al, Ti etc. scaling loss.Changed under inert atmosphere protection by being continuously added to equivalent calcium oxide Kind desulfurization condition.During mother alloy ingot is broken, by controlling broken atmosphere and broken intensity to control powder Particle diameter reduce shattering process in oxygenation.By PHASE DIAGRAM CALCULATION, it is the alloy that temperature, which occurs, in the foundry alloy composition liquid phase of design System is minimum, and the temperature needed for sintering alloy powder is greatly reduced.
The content of the invention
It is an object of the invention to provide a kind of high-alloying high temperature alloy foundry alloy of low oxygen content and the preparation of powder Technique.Mother alloy ingot is prepared by vacuum induction melting+electroslag remelting process, reduces the oxygen content of mother alloy ingot, sulphur contains Amount and the amount of inclusions, ingot casting disintegrating apparatus is improved, reduce increased oxygen content in shattering process.
Concrete technology step has：
1st, pretreatment of raw material：Using conjunction among Ni-50wt.%Cr intermediate alloys, Ni-5wt.%B intermediate alloys, Ni-Mo Gold, Ni-Nb intermediate alloys, and aluminium block, titanium sponge, sponge zirconium, graphite block are all higher than as raw materials for metallurgy, its purity 99.9wt.%.Raw metal is pre-processed in 5vol.% aqueous hydrochloric acid solutions, removes oxide on surface, pretreatment time For 25-35min, rinsed afterwards in alcohol, and 30-90min is handled at 60 DEG C in baking oven, make raw material drying.
2nd, the vacuum induction melting of mother alloy ingot：Pretreated raw material is carried out according to the composition of high-alloying foundry alloy Dispensing, obtain mixed material.Mixed material carries out vacuum induction melting.The composition of high-alloying foundry alloy is Ni-9.15Al- (19.23Cr-6.62Mo-3.31Nb-1.15Ti-0.15Zr-0.02B-0.18C percentage by weight).Foundry alloy is in vacuum induction Melting is carried out in smelting furnace, lime crucible is used in fusion process, and power is increased after furnace charge is melting down, is made on bath temperature 1670 DEG C are risen to, adds 2wt.% carbon block, is incubated 25-35min, molten bath is stirred using magnetic stirrer during being somebody's turn to do Mix, oxygen is fully removed, be added followed by 1wt.% Al and Ti and 0.01wt.%B, be incubated 10min, cool afterwards, fill Enter argon gas, molten steel is poured and builds up mother alloy ingot.
3rd, the electroslag remelting of female alloying ingot：Inert atmosphere electroslag melting is carried out to the ingot casting of vacuum induction melting, slag charge is matched somebody with somebody Than for 15-20wt.%CaO, 3-5wt.%Ca, 8-10wt.%CeO, 10-15wt.%Al2O3, 3-5wt.%TiO2, surplus CaF2.After above-mentioned slag charge is heated into molten condition, pour into crystallizer, crystallizer is copper cold-crucible, by step 2 system Standby obtained foundry alloy consutrode rod is slowly drop down in the slag charge of melting, after the energization starting the arc, adjustment remelting voltage to 30- 50V, electric current 3000-5000A, consutrode is by the slow fusing of resistance heat, and the molten steel after fusing is with after slag charge reaction, purification, tying Brilliant device bottom crystal, obtain pure, uniform, any surface finish foundry alloy ESR ingot.
4th, mother alloy ingot is broken：Mother alloy ingot surface scale is removed, in one kind with cooling system with protecting The high-speed disc of shield atmosphere galls to be crushed in crushing device, and the ratio of grinding ring internal diameter and grinding block diameter is 5:1.Mill device is such as Shown in Fig. 2.Powder after broken is screened, obtains the master alloy powder of average grain diameter≤20 μm.
Foundry alloy is made in alloy with high activity element (such as Cr, Ti, Al, Nb, Zr, B and C) by the present invention in advance, then with mother The form of alloy, rather than the form of individual element are added in material, and by alloying element is oxidizable etc., condition is not limited, energy Enough oxidations for effectively avoiding active element, advantageously reduce oxygen content.Pretreatment to raw material can effectively reduce the purchasing of raw materials and Caused oxidation and impurity during storage, the high-purity of raw material when ensureing to smelt.Using in Ni-50Cr intermediate alloys, Ni-5B Between alloy, Ni-Mo intermediate alloys, Ni-Nb intermediate alloys as raw materials for metallurgy, can further reduce the temperature needed for alloying, So as to reduce scaling loss and oxidation, ensure the recovery rate of alloying element.Meanwhile utilize lime crucible during vacuum induction melting Good stability, desulfating and deoxidation reduce the oxygen content in fusion process, and further by the addition of melting later stage carbon block Deoxidation, and easy scaling loss element is supplemented before coming out of the stove, ensure the alloy content of foundry alloy in the range of requiring.Vacuum induction is melted The electroslag remelting that obtained ingot casting carries out inert gas shielding is refined, the further oxygen in reduction ingot casting, sulfur content, reduction is mingled with Thing, make ingot casting sublimate.Mother alloy ingot plasticity is low, is easily broken, readily available fine alloy powder.The high speed of designed, designed Mill device can effectively prevent the Powder Oxidation in shattering process, be easy to obtain the master alloy powder of low oxygen content, final to obtain Oxygen content is less than 200ppm, sulfur content is less than 20ppm master alloy powder, and its average grain diameter is below 20 μm.Closed using the mother Bronze end prepares K418 alloys, and sintering process can be made to be carried out under conditions of the appearance of a small amount of liquid phase, helps solve product burning Tie problem on deformation, it is possible to increase the dimensional accuracy of sample, moreover it is possible to significantly reduce material powder cost and process energy consumption.
In technical process, the change of foundry alloy impurity content is as shown in table 1.
The impurity content of foundry alloy under the Ni-based foundry alloy of the low oxygen content high-alloying of table 1 and each processing step of powder
Brief description of the drawings
Fig. 1 is process chart
Fig. 2 is that high-speed disc galls crushing device schematic diagram.
Embodiment
Embodiment 1：
By in Ni-50wt.%Cr intermediate alloys of the purity more than 99.9wt.%, Ni-5wt.%B intermediate alloys, Ni-Mo Between alloy, Ni-Nb intermediate alloys, and aluminium block, titanium sponge, sponge zirconium pre-processed in 5vol.% aqueous hydrochloric acid solutions, Oxide on surface, pretreatment time 30min are removed, 60min is dried in processing at 60 DEG C in an oven after alcohol is cleaned；Pre- place Raw material after reason carries out dispensing, target component Ni-9.15wt.%Al-19.23wt.%Cr- according to target component 6.62wt.%Mo-3.31wt.%Nb-1.15wt.%Ti-0.15wt.%Zr-0.02wt.%B-0. 18wt.%C.By raw material Melting is carried out in vacuum induction melting furnace, ceramic crucible is used in fusion process, and power is increased after furnace charge is melting down, makes to melt Pond temperature rises to 1670 DEG C, adds 2wt.% carbon block, is incubated 30min, using magnetic stirrer to molten bath during being somebody's turn to do It is stirred, oxygen is fully removed, be added followed by 1wt.% Al and Ti and 0.01wt.%B, is incubated 10min, drops afterwards Temperature, argon gas is filled with, molten steel is poured and builds up foundry alloy consutrode rod.The electroslag that consutrode rod is carried out to inert atmosphere protection melts Refining, slag charge proportioning is 18wt.%CaO, 4wt.%Ca, 9wt.%CeO, 12wt.%Al2O3, 4wt.%TiO2, surplus CaF2.Will After above-mentioned slag charge is heated to molten condition, pour into crystallizer.Consutrode rod is slowly drop down in the slag charge of melting, is powered After arc, adjustment remelting voltage to 50V, electric current 3000A, for consutrode by the slow fusing of resistance heat, the molten steel and slag charge after fusing are anti- After should, purifying, crystallized in crystalliser feet, obtain pure, uniform, any surface finish foundry alloy ESR ingot.Afterwards by ESR ingot Epidermis removes, and is crushed in crushing device is galled with the high-speed disc of cooling system and protective atmosphere.Powder after will be broken Screened, finally give master alloy powder.
Embodiment 2：
By in Ni-50wt.%Cr intermediate alloys of the purity more than 99.9wt.%, Ni-5wt.%B intermediate alloys, Ni-Mo Between alloy, Ni-Nb intermediate alloys, and aluminium block, titanium sponge, sponge zirconium are pre-processed in 5wt.% aqueous hydrochloric acid solutions, gone Except oxide on surface, pretreatment time 30min, 60min is dried in processing at 60 DEG C in an oven after alcohol is cleaned；Pretreatment Raw material afterwards carries out dispensing, target component Ni-9.15wt.%Al-19.23wt.%Cr-6.62wt.% according to target component Mo-3.31wt.%Nb-1.15wt.%Ti-0.15wt.%Zr-0.02wt.%B-0.18wt.%C.By raw material in vacuum induction Melting is carried out in smelting furnace, ceramic crucible is used in fusion process, and power is increased after furnace charge is melting down, bath temperature is increased To 1670 DEG C, 2wt.% carbon block is added, is incubated 30min, molten bath is stirred using magnetic stirrer during being somebody's turn to do, made Oxygen fully removes, and is added followed by 1wt.% Al and Ti and 0.01wt.%B, is incubated 10min, cools afterwards, is filled with argon Gas, molten steel is poured and builds up foundry alloy consutrode rod.Consutrode rod is carried out to the electroslag melting of inert atmosphere protection, slag charge is matched somebody with somebody Than for 16wt.%CaO, 3wt.%Ca, 10wt.%CeO, 12wt.%Al2O3, 5wt.%TiO2, surplus CaF2.By above-mentioned slag charge After being heated to molten condition, pour into crystallizer.Consutrode rod is slowly drop down in the slag charge of melting, after the energization starting the arc, is adjusted Bulk wight melts voltage to 30V, and electric current 5000A, consutrode is by the slow fusing of resistance heat, molten steel and slag charge reaction, purification after fusing Afterwards, crystallized in crystalliser feet, obtain pure, uniform, any surface finish foundry alloy ESR ingot.ESR ingot epidermis is gone afterwards Remove, crushed in crushing device is galled with the high-speed disc of cooling system and protective atmosphere.Powder after will be broken is sieved Choosing, finally gives master alloy powder.
Embodiment 3：
By in Ni-50wt.%Cr intermediate alloys of the purity more than 99.9wt.%, Ni-5wt.%B intermediate alloys, Ni-Mo Between alloy, Ni-Nb intermediate alloys, and aluminium block, titanium sponge, sponge zirconium are pre-processed in 5wt.% aqueous hydrochloric acid solutions, gone Except oxide on surface, pretreatment time 30min, 60min is dried in processing at 60 DEG C in an oven after alcohol is cleaned；Pretreatment Raw material afterwards carries out dispensing, target component Ni-9.15wt.%Al-19.23wt.%Cr-6.62wt.% according to target component Mo-3.31wt.%Nb-1.15wt.%Ti-0.15wt.%Zr-0.02wt.%B-0.18wt.%C.By raw material in vacuum induction Melting is carried out in smelting furnace, ceramic crucible is used in fusion process, and power is increased after furnace charge is melting down, bath temperature is increased To 1670 DEG C, 2wt.% carbon block is added, is incubated 30min, molten bath is stirred using magnetic stirrer during being somebody's turn to do, made Oxygen fully removes, and is added followed by 1wt.% Al and Ti and 0.01wt.%B, is incubated 10min, cools afterwards, is filled with argon Gas, molten steel is poured and builds up foundry alloy consutrode rod.Consutrode rod is carried out to the electroslag melting of inert atmosphere protection, slag charge is matched somebody with somebody Than for 15wt.%CaO, 5wt.%Ca, 8wt.%CeO, 11wt.%Al2O3, 4wt.%TiO2, surplus CaF2.By above-mentioned slag charge After being heated to molten condition, pour into crystallizer.Consutrode rod is slowly drop down in the slag charge of melting, after the energization starting the arc, is adjusted Bulk wight melts voltage to 45V, and electric current 3500A, consutrode is by the slow fusing of resistance heat, molten steel and slag charge reaction, purification after fusing Afterwards, crystallized in crystalliser feet, obtain pure, uniform, any surface finish foundry alloy ESR ingot.ESR ingot epidermis is gone afterwards Remove, crushed in crushing device is galled with the high-speed disc of cooling system and protective atmosphere.Powder after will be broken is sieved Choosing, finally gives master alloy powder.

Claims (1)

  1. A kind of 1. preparation method of the Ni-based master alloy powder of low oxygen content high-alloying, it is characterised in that：
    Step 1: to be closed among Ni-50wt.%Cr intermediate alloys, Ni-5wt.%B intermediate alloys, Ni-Mo intermediate alloys, Ni-Nb Gold, and aluminium block, titanium sponge, sponge zirconium, graphite block are all higher than 99.9% as raw material, the purity of various raw materials；Raw metal exists Pre-processed in 5vol.% aqueous hydrochloric acid solutions, remove oxide on surface, pretreatment time 25-35min, alcohol clean after 30-90min is dried in processing at 60 DEG C in baking oven；
    Step 2: pretreated raw material carries out dispensing according to the composition of high-alloying foundry alloy, mixed material is obtained；Mixing is former Material carries out vacuum induction melting, and the composition of described high-alloying foundry alloy is：Ni-9.15wt.%Al-19.23wt.%Cr- 6.62wt.%Mo-3.31wt.%Nb-1.15wt.%Ti-0.15wt.%Zr-0.02wt.%B-0.18wt.%C；Nickel-base alloy is female to be closed The liquid phase forming temperature of gold is 1135 DEG C；Ceramic crucible is used in fusion process, and power is increased after furnace charge is melting down, makes molten bath Temperature rises to 1670 DEG C, adds 2wt.% carbon blocks, is incubated 25-35min, and magnetic stirrer is used in fusion process to molten bath It is stirred, oxygen is fully removed, be added followed by 1wt.% Al and Ti and 0.01wt.%B, is incubated 8-12min, drops afterwards Temperature, argon gas is filled with, molten steel is poured and builds up foundry alloy consutrode rod；
    Step 3: after slag charge is heated into molten condition, pour into crystallizer, crystallizer is copper cold-crucible, by step 2 The foundry alloy consutrode rod being prepared is slowly drop down in the slag charge of melting, after the energization starting the arc, adjustment remelting voltage to 30- 50V, electric current 3000-5000A, consutrode is by the slow fusing of resistance heat, and the molten steel after fusing is with after slag charge reaction, purification, tying Brilliant device bottom crystal, obtain pure, uniform, any surface finish foundry alloy ESR ingot；After vacuum electroslag remelting, foundry alloy oxygen contains Amount is less than 150ppm, and sulfur content is less than 20ppm；
    Step 4: mother alloy ingot surface scale is removed, galled in the high-speed disc with cooling system and protective atmosphere broken Crushed in device；Powder after broken is screened, obtains master alloy powder；
    Wherein, the slag charge proportioning described in step 3 is 15-20wt.%CaO, 3-5wt.%Ca, 8-10wt.%CeO, 10-15wt.% Al2O3, 3-5wt.%TiO2, surplus CaF2；
    Mill breaker described in step 4 is cooled down using cooling water, is protected using high-purity argon gas, in grinding ring The ratio of footpath and grinding block diameter is 5:1；
    The final oxygen content of master alloy powder described in step 4 is less than 200ppm, and sulfur content is less than 20ppm, it is small to be mingled with amount of substance In 0.002wt.%, average grain diameter≤20 μm of powder particle.
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CN108546834B (en) * 2018-04-16 2020-02-07 北京科技大学 Purification smelting method for nickel-based high-temperature alloy master alloy
CN109295330B (en) * 2018-10-26 2020-06-19 北京科技大学 Method for refining nitride inclusions in nickel-based wrought superalloy
CN109161697B (en) * 2018-10-26 2020-05-08 北京科技大学 Method for controlling non-metallic inclusions in powder metallurgy high-temperature alloy master alloy
CN110760718B (en) * 2019-11-25 2021-01-15 北京科技大学 Preparation method of high-tungsten high-cobalt nickel alloy high-purity fine-grain bar
CN111118304A (en) * 2020-01-06 2020-05-08 江苏远航精密合金科技股份有限公司 Preparation method of high-purity nickel strip foil for electronic industry
CN111926198A (en) * 2020-06-04 2020-11-13 广东华鳌合金新材料有限公司 Method for controlling surface quality and secondary shrinkage cavity size of K418 master alloy vacuum induction melting electrode
CN112296343B (en) * 2020-09-04 2023-05-26 武汉科技大学 Method for preparing superfine metal powder by hollow electrode smelting
CN116287812B (en) * 2023-05-24 2023-07-21 江苏美特林科特殊合金股份有限公司 Smelting method of aluminum-free high-temperature alloy

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