CN107083501B - A kind of iron nickel-molybdenum alloy raw powder's production technology - Google Patents

A kind of iron nickel-molybdenum alloy raw powder's production technology Download PDF

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CN107083501B
CN107083501B CN201710359342.6A CN201710359342A CN107083501B CN 107083501 B CN107083501 B CN 107083501B CN 201710359342 A CN201710359342 A CN 201710359342A CN 107083501 B CN107083501 B CN 107083501B
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alloy
molybdenum
powder
iron
production technology
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CN107083501A (en
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刘志坚
陈远星
何坤宏
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South China Agricultural University
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GUANGDONG IRON STEEL RESEARCH INSTITUTE
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/03Alloys based on nickel or cobalt based on nickel
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/142Thermal or thermo-mechanical treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/023Alloys based on nickel
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

Abstract

The invention discloses a kind of iron nickel-molybdenum alloy raw powder's production technologies, comprising the following steps: melts the smelting ferroferrite that mass percent is 75%~85% nickel, 2%~8% molybdenum-iron intermediate alloy block, 0.05%~0.4% phosphorus, 0.1%~0.45% sulphur and residual mass percentage in induction smelting furnace;After alloy molten solution temperature is risen to 1530~1580 DEG C, it is poured to form alloy sheet using rapid hardening;The alloy sheet is crushed and passes through rod mill, thick alloy powder is made;Polygonal ball mill is added in the thick alloy powder and carries out ball milling under protective atmosphere, wears into fine powder material;The fine powder material is heat-treated under reducing atmosphere;Screening forms iron nickel-molybdenum alloy powder.This method can reduce scaling loss of precious metal molybdenum during alloy smelting, improve recovery rate;The alloy sheet brittleness of intermediate products is higher, easily crushes.Compared with the existing technology, this method is not necessarily to high temperature hot rolling, and production investment is few, and milling efficiency is high, and overall cost is low.

Description

A kind of iron nickel-molybdenum alloy raw powder's production technology
Technical field
The present invention relates to a kind of preparation methods of metal-powder, especially iron nickel-molybdenum alloy raw powder's production technology.
Background technique
As electronics industry continues to develop, the requirement to magnetic material is higher and higher, and metal magnetic powder core is using powder smelting The soft magnetic materials of gold manufacture, in the advantage that there are other materials to hardly match for many applications.In all metal magnetic powder cores, Iron nickel molybdenum powder core has minimum loss, highest Q value, when stability is good, frequency of use range is wide, different frequencies works The advantages that noiseless.But the difficulty of preparation technology of FeNiCo magnetic core material is big, and technique threshold is high.
Currently, the method that different manufacturers prepare FeNiCo magnetic core material both at home and abroad mainly includes mechanical alloying method, atomization Method, hot rolling crush method etc..It is simple that mechanical alloying method prepares iron nickel molybdenum soft-magnetic alloy powder body technology, but the period is long, energy consumption is high, holds Oxidizable, reduced performance.Atomization is divided into aerosolization and water atomization, and gas atomization produces spherical powder, purity is high, but mouldability Difference, hardly possible compacting, price;Water atomization produces irregular shape powder, and oxygen content is high, and impurity is more, and powder core loss is high, and performance is poor;Heat Rolling crush method after first passing through high temperature heavy reduction hot rolling ingot into band, then is crushed, powder processed using alloy smelting casting ingot-forming. Due to using air induced melting, precious metal molybdenum is directly added into smelting process, leading to the loss of metal molybdenum is about 8% left side The right side causes significant wastage.The process flow of such manufacturing process is long simultaneously, and material and energy loss are big, and alloy oxidation is serious. In addition technique requirement is not achieved in common equipment of hot rolling when high temperature heavy reduction hot rolling ingot, then the morphology microstructure produced through ball milling is not It is good;Although the powder good moldability of heavy reduction equipment of hot rolling preparation, performance is good, expensive, and hot rolling is caused to be crushed legal system The alloy powder overall cost height of work, long flow path, equipment investment are big.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention proposes a kind of iron nickel-molybdenum alloy raw powder's production technology, is improving While broken milling efficiency, the iron nickel-molybdenum alloy powder that pattern is good, magnetic property is good is prepared.
To achieve this purpose, the present invention adopts the following technical scheme:
A kind of iron nickel-molybdenum alloy raw powder's production technology provided by the invention is implemented as follows:
S10: by mass percent be 75%~85% nickel, 2%~8% molybdenum-iron intermediate alloy block, 0.05%~ The smelting ferroferrite of 0.4% phosphorus, 0.1%~0.45% sulphur and residual mass percentage melts in induction smelting furnace, Described in the sum of the mass percents of p and s be 0.2%~0.5%;
S20: after the alloy molten solution temperature in the induction smelting furnace is risen to 1530~1580 DEG C, shape is poured using rapid hardening At alloy sheet;
S30: the alloy sheet is crushed, and thick alloy powder is made by rod mill;
S40: polygonal ball mill is added in the thick alloy powder and carries out ball milling under protective atmosphere, wears into fine powder material;
S50: the fine powder material is heat-treated under reducing atmosphere, is heated to 750~850 DEG C, keeps the temperature 2~5 hours;
S60: the fine powder material through Overheating Treatment is sieved, and forms iron nickel-molybdenum alloy powder.
Preferably, the molybdenum-iron intermediate alloy block is the ratio of 1:1~1.2 in vacuum induction smelting by iron and molybdenum in mass ratio It is poured after fusing in furnace.
Preferably, in step slo, the sense is added in the molybdenum-iron intermediate alloy block again after other materials has melted Smelting furnace is answered to melt.
Preferably, in step slo, mass percent >=0.08% of the phosphorus, the mass percent of the sulphur >= 0.12%, and the sum of mass percent of the p and s is 0.2%~0.5%.
Preferably, further include step S25 between step S20 and S30: the alloy sheet being immersed cold in cooling water But it, and to alloy sheet after cooling is dried.
Preferably, in step s 25, the temperature of the cooling water is maintained at 10 DEG C or less.
Preferably, the gas that protective atmosphere described in step S40 uses is nitrogen or argon gas.
Preferably, further include step 35 between step S30 and step S40: the thick alloy powder is soaked in liquid nitrogen Bubble cooling.
Preferably, the hydrogen and nitrogen that the gas that reducing atmosphere described in step S50 uses cracks for pure hydrogen or liquefied ammonia Mixed gas.
The invention has the benefit that first by metal molybdenum and iron being made molybdenum-iron under vacuum using vacuum induction smelting furnace Intermediate alloy block, then the raw material such as nickel, smelting ferroferrite and molybdenum-iron intermediate alloy block smelting speed are added with antivacuum induction smelting furnace Solidifying tapping nickel-molybdenum alloy thin slice, can largely reduce scaling loss of precious metal molybdenum during alloy smelting;The smelting The iron nickel-molybdenum alloy thin slice brittleness that rapid hardening goes out is high, becomes more crisp after being quickly cooled down in cooling step, so that the iron nickel molybdenum Crushing effect of the alloy sheet in entire crushing process is more preferably.Compared with the existing technology, this method is not necessarily to high temperature hot rolling, production Investment overall cost is low, process is short, moreover it is possible to reduce alloy oxidation in preparation process, reduce oxygen content, enhance product performance.
Detailed description of the invention
Fig. 1 is that the part of main view when the chute for the alloy sheet casting device that embodiment one uses is moved to the rightmost side is cutd open Depending on schematic diagram;
Fig. 2 is that the part of main view when the chute for the alloy sheet casting device that embodiment one uses is moved to the leftmost side is cutd open Depending on schematic diagram;
Fig. 3 is the partial cutaway view schematic of alloy sheet casting device left view in Fig. 1.
Specific embodiment
Below by specific embodiment to further illustrate the technical scheme of the present invention.
Embodiment one
A kind of iron nickel-molybdenum alloy raw powder's production technology provided in this embodiment, uses alloy shown in Fig. 1~3 thin Piece casting device 100.The alloy sheet casting device 100, including cabinet 10, funnel brick 20, tundish 30, chute 40, drive Motivation structure 50, rapid hardening roller 60, cold plate 70 and cooling water tank 80.10 inner wall of cabinet is fixed with one without magnetic by screw Bracket 11 made of steel plate;The round funnel brick 20 of high 100mm made of being sintered as refractory material is set up on the bracket 11, The wide-mouth that its top is diameter 200mm, bottom are equipped with the funnel hole 21 that a diameter is 25mm.The height made by refractory material The tundish 30 of the prolate staving shape of 400mm, the tundish 30 is interior to be equipped with the oval upper opening 31 for being 650mm with long axis With the casting channel that diameter is 25mm circle under shed 32 and around the load coil 33 of casting channel setting.By The chute 40 of high 100mm, wide 500mm that refractory material makes, the chute 40 include the maximum width of the recessed formation in upper surface For the carrier 41 of 250mm, from the sprue gate that the width that carrier 41 extends to side is 20mm 42 and in being set to The resistance-type heating net 43 in portion.The driving mechanism 50 includes being equipped at the 21 underface 600mm of funnel hole in cabinet 10 The guide rail 51 of one long 1000mm and the hydraulic stem 52 positioned at 51 side of guide rail, hydraulic cylinder 53 and the control hydraulic stem 52 With the controller 54 of hydraulic cylinder 53.51 end positions of guide rail are equipped with the first limit switch 51A and the second limit switch 51B, The moving section of 900mm is formed, the midpoint of the moving section is located on the 21 central axes 21A of funnel hole.The tundish 30 are fixedly connected with the chute 40 by the fixed frame 34 that steel plate makes, and are set up in the moving section, described hydraulic 52 one end of bar connects the hydraulic cylinder 53, and the other end connects the outside of the chute 40.The rapid hardening roller 60 made of fine copper material It is set in the cabinet 10 at the 42 lower section 50mm of sprue gate, width 500mm, diameter 300mm, the rapid hardening roller 60 further include the electrodeless motor 61 being set to outside the cabinet 10 and the water-cooling system 62 for cooling down the rapid hardening roller 60, institute The position for stating sprue gate 42 is located at right above the central axes of rapid hardening roller 60;The water-cooling system 62 includes being located at the rapid hardening roller 60 The water pump 62A of outside, the waterway 62B inside the rapid hardening roller 60, entering for the water pump 62A and waterway 62B is connected Water pipe 62C and outlet pipe 62D.70 inner end of cold plate is arranged in below the rapid hardening roller 60 in the cabinet 10, outside It holds and extends outside the cabinet 10, and its upper surface is tilted down in ramped shaped and along extending direction, the cold plate 70 also wraps Include water inlet pipe 72 and outlet pipe 73 set on internal waterway 71, connection the water pump 62A and waterway 71.Stainless steel The cooling water tank 80 of matter is located at outside the cabinet 10, built with water temperature in 10 DEG C of cooling waters below, the cold plate 70 Outer end is located at the overthe openings of the cooling water tank 80, and the water-cooling system 62 further includes an outside cooling water tank (not shown), The water inlet of the water pump 62A, the outlet pipe 62D and the outlet pipe 73 are connect with the external cooling water tank, are followed Ring is cooling.
A kind of iron nickel-molybdenum alloy raw powder's production technology provided in this embodiment the following steps are included:
S01: being to pour among molybdenum-iron after 1:1.2 ratio melts in vacuum induction smelting furnace by iron and molybdenum in mass ratio Alloy block;
S10: 75% nickel, 0.1% phosphorus, 0.1% sulphur and 16.8% smelting ferroferrite are existed by mass percentage Incude fusing in smelting furnace;After above-mentioned raw material have melted, then by 8% by step S01 production molybdenum-iron intermediate alloy block The induction smelting furnace fusing is added, and begins to warm up tundish 30 and chute 40;
S20: the alloy molten solution temperature in the induction smelting furnace is risen to 1530 DEG C;In 80 water storage of cooling water tank to 2/3 Place is simultaneously put into ice cube, maintains cooling water temperature at 10 DEG C hereinafter, opening the Water-cooling circulating of water-cooling system 62 and cold plate 70;Starting The electrodeless motor 61 of rapid hardening roller 60 simultaneously adjusts revolving speed to 480 revs/min, at the same time, controls the liquid by the controller 54 Compression bar 52 is flexible to drive the tundish 30 and chute 40 in the first limit switch 51A and the second limit switch 51B It is moved in the moving section of formation;
S21: alloy molten solution is poured into the funnel brick 20 from the induction smelting furnace, with the tundish 30 Upper opening 31 receives the alloy molten solution flowed out from the funnel hole 21 of funnel brick 20;
S22: the institute for stablizing outflow from the under shed 32 of the tundish 30 is received using the carrier 41 of the chute 40 Alloy molten solution is stated, and slows down and stablize the flow velocity of the alloy molten solution using the biggish undertaking space of the carrier 41;
S23: the left side by the alloy molten solution with stable flow velocity from the sprue gate 42 of the chute 40 in Fig. 1 and Fig. 2 Right direction is back and forth cast on the rapid hardening roller 60 of high-speed rotation;
S24: when the alloy molten solution and the rapid hardening roller 60 contact, the property of 60 quick conductive of rapid hardening roller is made full use of It simultaneously is quickly thrown away to be formed with a thickness of 0.2-0.5mm alloy sheet 90 by the cooling alloy molten solution of matter;
S25: the alloy sheet 90, which is got rid of, to be fallen on the upper surface of the cold plate 70, and sliding outward under gravity Out, the cold plate 70 carries out secondary cooling to the alloy sheet 90 during skidding off;Cooling water tank 80 is received from institute The alloy sheet 90 for stating the landing of cold plate 70, is fully cooled the middle alloy sheet 90 using cooling water therein, and pass through Adding ice cube keeps the temperature of cooling water at 10 DEG C hereinafter, guaranteeing the cooling effect to the alloy sheet 90;To the alloy After the cooling completely of thin slice 90, it is drawn off and is dried moisture, is then placed in the baking oven that temperature is 150 DEG C, dries the alloy Moisture on thin slice 90;
S30: the alloy sheet 90 is crushed, and thick alloy powder is made by rod mill;
S35: the thick alloy powder is put into austenite stainless steel drum, and liquid nitrogen is then poured into bucket to described thick Alloy powder is cooled down, and is stopped being added after the thick alloy powder is completely covered in liquid nitrogen, is waited the liquid nitrogen spontaneous vaporization, Whole process about 5~10 minutes.
S40: the cooling thick alloy powder of low temperature of the liquid nitrogen is added in the crushing chamber of polygonal ball mill, in filling nitrogen Protective atmosphere under carry out ball milling, wear into fine powder material;
S50: the fine powder material is heat-treated under the reducing atmosphere of pure hydrogen, is heated to 750 DEG C, keeps the temperature 5 hours, The fine powder material is set desulfurization and to remove oxidation impurities while destressing;
S60: sieving the fine powder material through Overheating Treatment using the stainless steel mesh of 200 mesh, forms iron nickel-molybdenum alloy Powder.
In the present embodiment, molybdenum-iron intermediate alloy by metal molybdenum and iron is made under vacuum using vacuum induction smelting furnace Block, then the raw material such as nickel, smelting ferroferrite and molybdenum-iron intermediate alloy block smelting rapid hardening tapping nickel are added with antivacuum induction smelting furnace Molybdenum alloy thin slice, scaling loss ratio of precious metal molybdenum during entire alloy smelting is about 0.2%;It smelts and is added in raw material The brittleness of the iron nickel-molybdenum alloy thin slice, the alloy sheet and the thick alloy powder warp can be improved in the p and s of proper content Become more crisp after water cooling and liquid nitrogen are cooling, in broken and grinding, crush efficiency can be greatly improved.Move back and forth casting The cooling effect for each cooling step that thin slice can be made full use of to prepare, improves the production quality and efficiency of thin slice.
The alloy molten solution falls into the upper opening 31 of the tundish 30 from the funnel hole 21, through casting channel, under Opening 32 flows into the carrier 41 of the chute 40, and the flow velocity of the alloy molten solution through the funnel brick 20, tundish 30 and slips The three-stage casting channel that slot 40 is formed, which is slowed down, smoothly flows out from the sprue gate 42 afterwards and is cast in the rapid hardening roller 60 Surface.The load coil 33 and resistance-type heating net 43 of the tundish 30 and chute 40, can effectively guarantee the conjunction Golden melt keeps temperature when the tundish 30 and chute 40 flow;Certainly, to the heating of the tundish 30 and chute 40 Mode is not limited to the mode of induction heating or resistance heating, as long as being able to maintain the alloy molten solution is poured into the rapid hardening roller 60 Temperature before.As shown in Figure 1, when the left side of the chute 40 touches the first limit switch 51A, the leakage The signal that hole 21 is located at close to the position of 31 right end of upper opening, through the first limit switch 51A that struggles against is fed back, the control Device 54 controls the hydraulic stem 52 and shrinks, so that the tundish 30 and chute 40 be driven to move right.As shown in Fig. 2, working as institute When stating the right side of chute 40 and touching the second limit switch 51B, the funnel hole 21 is located at left close to the upper opening 31 The position at end, the signal feedback through the second limit switch 51B, the controller 54 control the hydraulic stem 52 and extend, from And the tundish 30 and chute 40 is driven to be moved to the left.In the reciprocating movement of above-mentioned tundish 30 and chute 40, institute The alloy molten solution for stating the casting of funnel hole 21 maintains to flow into the upper opening 31 of the tundish 30 always, not will cause alloy molten solution Waste, will not because spillage alloy molten solution caused by other component damage.The sprue gate 42 is also corresponded to described simultaneously It is moved back and forth above rapid hardening roller 60, to uniformly back and forth be poured in the width direction of the rapid hardening roller 60, makes full use of the speed The cooling surface of solidifying roller 60, can effectively extend the service life of the rapid hardening roller 60;The limitation of moving section further ensures The alloy molten solution that sprue gate 42 is flowed out is all fallen on the rapid hardening roller 60.Due to the reciprocating movement at sprue gate 42, so that the conjunction Golden thin slice 90 is uniformly scattered on the upper surface of the cold plate 70, carries out secondary cooling;Hereafter, due to the cold plate 70 Inclination angle design, what the alloy sheet 90 through secondary cooling can also be evenly distributed slowly slide into, and that the cooling water tank 80 carries out is last Water cooling.
Embodiment two
A kind of iron nickel-molybdenum alloy raw powder's production technology provided in this embodiment, wherein a kind of alloy sheet is used to be poured Device, the alloy sheet casting device is similar with the alloy sheet casting device in embodiment one, but is not provided with cold plate 70, Other sizes are slightly different, and this will not be repeated here.
Iron nickel-molybdenum alloy raw powder's production technology provided in this embodiment the following steps are included:
S01: being to pour among molybdenum-iron after 1:1.1 ratio melts in vacuum induction smelting furnace by iron and molybdenum in mass ratio Alloy block;
S10: by mass percentage by 80% nickel, 0.08% phosphorus, 0.22% sulphur and 14.7% smelting ferroferrite It is melted in induction smelting furnace;After above-mentioned material has melted, then by 5% by step S01 production molybdenum-iron intermediate alloy block The induction smelting furnace fusing is added, and begins to warm up tundish 30 and chute 40;In alternative embodiments, in this step The mass percents of p and s can replace with 0.18% and 0.12% respectively;
S20: the alloy molten solution temperature in the induction smelting furnace is risen to 1560 DEG C;In 80 water storage of cooling water tank to 2/3 Place is simultaneously put into ice cube, keeps cooling water temperature at 5 DEG C hereinafter, opening water-cooling system 62;Start the electrodeless motor 61 of rapid hardening roller 60 And revolving speed is adjusted to 550 revs/min, at the same time, it is flexible to drive institute that the hydraulic stem 52 is controlled by the controller 54 Tundish 30 and chute 40 is stated to move in the moving section that the first limit switch 51A and the second limit switch 51B is formed;
S21: it by alloy molten solution from being poured into the induction furnace in the funnel brick 20, is opened on the tundish 30 Mouth 31 receives the alloy molten solution flowed out from the funnel hole 21 of funnel brick 20;
S22: the institute for stablizing outflow from the under shed 32 of the tundish 30 is received using the carrier 41 of the chute 40 Alloy molten solution is stated, and slows down and stablize the flow velocity of the alloy molten solution using the biggish undertaking space of the carrier 41;
S23: the left side by the alloy molten solution with stable flow velocity from the sprue gate 42 of the chute 40 in Fig. 1 and Fig. 2 Right direction is back and forth cast on the rapid hardening roller 60 of high-speed rotation;
S24: when the alloy molten solution and the rapid hardening roller 60 contact, the property of 60 quick conductive of rapid hardening roller is made full use of It simultaneously is quickly thrown away to be formed with a thickness of 0.2-0.5mm alloy sheet 90 by the cooling alloy molten solution of matter;
S25: the cooling water tank 80 receives from the rapid hardening roller 60 and gets rid of the alloy sheet 90 fallen, utilizes cooling water therein The middle alloy sheet 90 is fully cooled, and keeps the temperature of cooling water at 5 DEG C hereinafter, guaranteeing to described by addition ice cube The cooling effect of alloy sheet 90;After the alloy sheet 90 is completely cooling, it is drawn off and is dried moisture, is then placed in temperature In the baking oven that degree is 200 DEG C, the moisture on the alloy sheet 90 is dried;
S30: the alloy sheet 90 is crushed, and thick alloy powder is made by rod mill;
S35: the thick alloy powder is put into austenite stainless steel drum, and liquid nitrogen is then poured into bucket to described thick Alloy powder is cooled down, and is stopped being added after the thick alloy powder is completely covered in liquid nitrogen, is waited the liquid nitrogen spontaneous vaporization, Whole process about 5~10 minutes;
S40: the cooling thick alloy powder of low temperature of the liquid nitrogen is added in the crushing chamber of polygonal ball mill, in filling nitrogen Protective atmosphere under carry out ball milling, wear into fine powder material;
S50: the fine powder material is heat-treated under the reducing atmosphere of liquefied ammonia cracking gas, is heated to 850 DEG C, heat preservation 2 Hour, so that the fine powder material desulfurization and is removed oxidation impurities while destressing;
S60: sieving the fine powder material through Overheating Treatment using the stainless steel mesh of 250 mesh, forms iron nickel-molybdenum alloy Powder.
In the present embodiment, the getting rid of of 90 Direct Uniform of alloy sheet dispersion fall into the cooling water tank 80 carry out it is cold But, structure is more simple with respect to embodiment one.
Embodiment three
A kind of iron nickel-molybdenum alloy raw powder's production technology provided in this embodiment, wherein a kind of alloy sheet is used to be poured Device, the alloy sheet casting device is similar with the alloy sheet casting device in embodiment two, and this will not be repeated here.
Iron nickel-molybdenum alloy raw powder's production technology provided in this embodiment the following steps are included:
S01: being to pour among molybdenum-iron to close after 1:1 ratio melts in vacuum induction smelting furnace by iron and molybdenum in mass ratio Gold bullion;
S10: by mass percentage by 85% nickel, 0.05% phosphorus, 0.45% sulphur and 12.5% smelting ferroferrite It is melted in induction smelting furnace;After above-mentioned material has melted, then by 2% by step S01 production molybdenum-iron intermediate alloy block The induction smelting furnace fusing is added, and begins to warm up tundish 30 and chute 40;In alternative embodiments, in this step The mass percents of p and s can be replaced 0.4% and 0.1%;
S20: the alloy molten solution temperature in the induction smelting furnace is risen to 1580 DEG C;In 80 water storage of cooling water tank to 2/3 Place is simultaneously put into ice cube, keeps cooling water temperature at 5 DEG C hereinafter, opening water-cooling system 62;Start the electrodeless motor 61 of rapid hardening roller 60 And revolving speed is adjusted to 520 revs/min;At the same time, the hydraulic stem 52 is controlled by the controller 54 to stretch to drive institute Tundish 30 and chute 40 is stated to move in the moving section that the first limit switch 51A and the second limit switch 51B is formed;
S21: it by alloy molten solution from being poured into the induction furnace in the funnel brick 20, is opened on the tundish 30 Mouth 31 receives the alloy molten solution flowed out from the funnel hole 21 of funnel brick 20;
S22: the institute for stablizing outflow from the under shed 32 of the tundish 30 is received using the carrier 41 of the chute 40 Alloy molten solution is stated, and slows down and stablize the flow velocity of the alloy molten solution using the biggish undertaking space of the carrier 41;
S23: the left side by the alloy molten solution with stable flow velocity from the sprue gate 42 of the chute 40 in Fig. 1 and Fig. 2 Right direction is back and forth cast on the rapid hardening roller 60 of high-speed rotation;
S24: when the alloy molten solution and the rapid hardening roller 60 contact, the property of 60 quick conductive of rapid hardening roller is made full use of It simultaneously is quickly thrown away to be formed with a thickness of 0.2-0.5mm alloy sheet 90 by the cooling alloy molten solution of matter;
S25: the cooling water tank 80 receives from the rapid hardening roller 60 and gets rid of the alloy sheet 90 fallen, utilizes cooling water therein The middle alloy sheet 90 is fully cooled, and keeps the temperature of cooling water at 5 DEG C hereinafter, guaranteeing to described by addition ice cube The cooling effect of alloy sheet 90;After the alloy sheet 90 is completely cooling, it is drawn off and is dried moisture, is then placed in temperature In the baking oven that degree is 200 DEG C, the moisture on the alloy sheet 90 is dried;
S30: the alloy sheet 90 is crushed, and thick alloy powder is made by rod mill;
S35: the thick alloy powder is put into austenite stainless steel drum, and liquid nitrogen is then poured into bucket to described thick Alloy powder is cooled down, and is stopped being added after the thick alloy powder is completely covered in liquid nitrogen, is waited the liquid nitrogen spontaneous vaporization, Whole process about 5~10 minutes.
S40: the cooling thick alloy powder of low temperature of the liquid nitrogen is added in the crushing chamber of polygonal ball mill, in filling argon gas Protective atmosphere under carry out ball milling, wear into fine powder material;
S50: the fine powder material is heat-treated under the reducing atmosphere of pure hydrogen, is heated to 800 DEG C, keeps the temperature 3 hours, The fine powder material is set desulfurization and to remove oxidation impurities while destressing;
S60: sieving the fine powder material through Overheating Treatment using the stainless steel mesh of 250 mesh, forms iron nickel-molybdenum alloy Powder.
In conclusion iron nickel-molybdenum alloy raw powder's production technology provided by the invention, using vacuum induction smelting furnace true Under sky by metal molybdenum and it is iron be made molybdenum-iron intermediate alloy block, then with antivacuum induction smelting furnace be added the raw material such as nickel, iron and Molybdenum-iron intermediate alloy block smelts rapid hardening tapping nickel-molybdenum alloy thin slice, and precious metal molybdenum can be greatly reduced during alloy smelting Scaling loss;The brittleness of the iron nickel-molybdenum alloy thin slice can be improved in the p and s for smelting addition proper content in raw material, so that institute State alloy sheet and thick alloy powder becomes more crisp after being quickly cooled down, and effectively improves the efficiency for preparing iron nickel-molybdenum alloy powder. By moving back and forth the cooling effect for each cooling step that casting can make full use of thin slice to prepare, the production quality of thin slice is improved And efficiency.And make alloy sheet have the advantages that ingredient uniformly, it is reduced in segregation, breakable;Alloy passes through in also Primordial Qi simultaneously It anneals under atmosphere, the sulphur added in alloy smelting raw material can be effectively removed, ensure that the magnetic property of iron nickel-molybdenum alloy powder.This hair Bright iron nickel-molybdenum alloy raw powder's production technology can prepare the iron nickel-molybdenum alloy powder that pattern is good, spherical and few impurity, effect Rate is high, consuming little energy, and whole input cost is low.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art The other embodiments being understood that.

Claims (8)

1. a kind of iron nickel-molybdenum alloy raw powder's production technology, comprising the following steps:
S10: being 75%~85% nickel, 2%~8% molybdenum-iron intermediate alloy block, 0.05%~0.4% by mass percent Phosphorus, 0.1%~0.45% sulphur and the smelting ferroferrite of residual mass percentage melt in induction smelting furnace, wherein the phosphorus It is 0.2%~0.5% with the sum of the mass percent of sulphur;
S20: it after the alloy molten solution temperature in the induction smelting furnace is risen to 1530~1580 DEG C, is poured to form conjunction using rapid hardening Golden thin slice;
S25: the alloy sheet is immersed into cooling in cooling water, and alloy sheet after cooling is dried;
S30: the alloy sheet is crushed, and thick alloy powder is made by rod mill;
S40: polygonal ball mill is added in the thick alloy powder and carries out ball milling under protective atmosphere, wears into fine powder material;
S50: the fine powder material is heat-treated under reducing atmosphere, is heated to 750~850 DEG C, keeps the temperature 2~5 hours;
S60: the fine powder material through Overheating Treatment is sieved, and forms iron nickel-molybdenum alloy powder.
2. iron nickel-molybdenum alloy raw powder's production technology according to claim 1, it is characterised in that: the molybdenum-iron intermediate alloy Block is to be poured after the ratio of 1:1~1.2 melts in vacuum induction smelting furnace by iron and molybdenum in mass ratio.
3. iron nickel-molybdenum alloy raw powder's production technology according to claim 1, it is characterised in that: in step slo, at it The molybdenum-iron intermediate alloy block is added the induction smelting furnace again after having melted and melted by his material.
4. iron nickel-molybdenum alloy raw powder's production technology according to claim 1, it is characterised in that: in step slo, described Mass percent >=0.08% of phosphorus, mass percent >=0.12% of the sulphur.
5. iron nickel-molybdenum alloy raw powder's production technology according to claim 1, it is characterised in that: in step s 25, described The temperature of cooling water is maintained at 10 DEG C or less.
6. iron nickel-molybdenum alloy raw powder's production technology according to claim 1, it is characterised in that: protected described in step S40 The gas that shield atmosphere uses is nitrogen or argon gas.
7. iron nickel-molybdenum alloy raw powder's production technology according to claim 1, it is characterised in that: in step S30 and step Further include step 35 between S40: the thick alloy powder is impregnated into cooling in liquid nitrogen.
8. iron nickel-molybdenum alloy raw powder's production technology according to claim 1, it is characterised in that: described in step S50 also The mixed gas of hydrogen and nitrogen that the gas that Primordial Qi atmosphere uses cracks for pure hydrogen or liquefied ammonia.
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