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    • 专利摘要:
    A water-atomized metal powder is produced by dividing a molten metal stream into a metal powder by making injection water having a liquid temperature of 10°C or less and an injection pressure of 5 MPa or more impinge on the molten metal stream and cooling the metal powder. Cooling with injection water having a liquid temperature of 10°C or less and an injection pressure of 5 MPa or more enables can be performed not in the film boiling region but in the transition boiling region from the beginning of cooling. This facilitates cooling the metal powder and enables rapid cooling required for changing the metal powder into an amorphous state to be readily performed. A gas-atomized metal powder may also be produced by dividing a molten metal stream into a metal powder by making an inert gas impinge on the molten metal stream and cooling the metal powder with injection water having a liquid temperature of 10°C or less and an injection pressure of 5 MPa or more. It is preferable to perform the cooling of the metal powder with the injection water after the temperature of the metal powder has reached the MHF point or less.
    公开号:SE1651221A1
    申请号:SE1651221
    申请日:2015-03-13
    公开日:2016-09-12
    发明作者:Nakaseko Makoto；Nakamura Naomichi；Ozaki Yukiko
    申请人:Jfe Steel Corp；
    IPC主号:
    专利说明:

    [3] [0003] In a water atomization process, a water-atomized metalpowder is produced by dividing a molten metal stream into apowdered metal (metal powder) with a water jet ejected through nozzles and cooling the powdered metal (metal powder) with the water jet. On the other hand, in a gasatomization process, an atomized metal powder is produced bydividing a molten metal stream into a powdered metal (metalpowder) with an inert gas ejected through nozzles and,generally, cooling the powdered metal (metal powder) bydropping the powdered metal into a tank containing water ora drum containing swirling water which is disposed below theatomizing device.
    [4] [0004] Recently, a reduction in the iron losses of motor coresfor electric vehicles, hybrid vehicles, and the like hasbeen anticipated from the viewpoint of energy conservation.While motor cores are produced using multilayers ofelectromagnetic steel sheets, attention is being focused onmotor cores formed of a metal powder (electromagnetic ironpowder), which allows a high degree of flexibility indesigning the shapes of the motor cores. For reducing theiron losses of such motor cores, it is necessary to reducethe iron loss of a metal powder constituting the motorcores. For reducing the iron loss of the metal powder, itis considered to be effective to change the metal powderinto an amorphous state. For producing an amorphous metalpowder by an atomization process, however, it is necessaryto cool the metal powder that is in a high-temperature condition including a molten state at a considerably high cooling rate in order to prevent crystallization of themetal powder.[0005] Accordingly, there have been proposed several methodsfor rapidly cooling a metal powder.[0006] For example, Patent Literature l describes a method forproducing a metal powder in which scattered molten metalparticles are cooled and solidified to form a metal powder.The rate at which the molten metal particles are cooleduntil they solidify is set to l05 K/s or more. In thetechnique described in Patent Literature l, the abovecooling rate is achieved by bringing the scattered moltenmetal particles into contact with a stream of a coolingliquid which is generated by passing the cooling liquidalong the inner wall of a cylindrical body in a spiral. Itis described that the flow rate of the stream of the coolingliquid, which is generated by passing the cooling liquid ina spiral, is preferably set to 5 to 100 m/s.
    [7] [0007] Patent Literature 2 describes a method for producing arapidly solidified metal powder. In the technique describedin Patent Literature 2, a cooling liquid is fed from theouter periphery of the top end of a cylindrical portion of a cooling container having a cylindrical inner periphery in the circumferential direction so as to flow downward alongthe inner periphery of the cylindrical portion in a spiral.The cooling liquid forms a laminar, spiral cooling-liquidlayer having a cavity at the center due to the centrifugalforce generated by the spiral stream of the cooling liquid.A molten metal is fed to the inner periphery of the spiralcooling-liquid layer and rapidly solidified. This enables ahigh-quality, rapidly solidified powder to be produced witha high cooling efficiency.
    [8] [0008] Patent Literature 3 describes an apparatus forproducing a metal powder by a gas atomization process, whichincludes a gas jet nozzle through which a gas jet is made toimpinge on a molten metal stream in order to divide themolten metal stream into molten metal droplets and a coolingcylinder including a layer of a cooling liquid that flowsdownward along the inner periphery of the cylinder in aspiral. In the technique described in Patent Literature 3,the molten metal is divided in two stages by using the gasjet nozzle and the spiral cooling-liquid layer. Thisenables a fine, rapidly solidified metal powder to beproduced.
    [9] [0009]Patent Literature 4 describes a method for producing amorphous metal fine particles. In this method, a molten metal is fed into a liquid coolant such that a steam filmthat covers the molten metal is formed in the coolant, andthe steam film is broken in order to bring the molten metalinto direct contact with the coolant. This induces boilingthat is caused due to natural nucleation. While the moltenmetal is divided into particles with the power of thepressure wave resulting from the boiling, the molten metalparticles are rapidly cooled and changed into an amorphousstate. Thus, amorphous metal fine particles are produced.It is described that the steam film that covers the moltenmetal can be broken by controlling the temperature of themolten metal fed into the coolant such that, when the moltenmetal is brought into direct contact with the coolant, thetemperature of the molten metal at the interface between themolten metal and the coolant is equal to or lower than theminimum film boiling temperature and equal to or higher thanthe spontaneous nucleation temperature or by usingultrasound.
    [10] [0010] Patent Literature 5 describes a method for producingfine particles. In this method, a molten material is fedinto a liquid coolant in the form of droplets or a jetstream while the temperature of the molten material is setsuch that the molten material has a temperature equal to or more than the spontaneous nucleation temperature of the liquid coolant and is in a molten state when being broughtinto contact with the liquid coolant. Furthermore, thedifference in relative Velocity between the molten materialand a stream of the liquid coolant at the time the moltenmaterial is fed into the stream of the liquid coolant iscontrolled to be lO m/s or more. This causes the steam filmformed around the molten material to be forcibly broken andboiling to occur due to spontaneous nucleation. Thus, themolten material is formed into fine particles, and the fineparticles are cooled and solidified. It is described thatthis method enables materials that have been considered tobe difficult to be formed into fine particles and changedinto an amorphous state to be formed into fine particles andchanged into an amorphous state.
    [11] [0011] Patent Literature 6 describes a method for producing afunctional member, the method including a step in which araw material prepared by adding a functional additive to abase material is molten and fed into a liquid coolant inorder to cause steam explosion, which enables the molten rawmaterial to be formed into fine particles, and the fineparticles are cooled and solidified at a controlled coolingrate in order to form homogeneous functional finepolycrystalline or amorphous particles free from segregation and a step in which the functional fine particles and fine particles of the base material, which are used as rawmaterials, are solidified to form a functional member.Citation List Patent Literature
    [12] [0012] PTL 1: Japanese Unexamined Patent ApplicationPublication No. 2010-150587 PTL 2: Japanese Examined Patent Application PublicationNo. 7-107167 PTL 3: Japanese Patent No. 3932573 PTL 4: Japanese Patent No. 3461344 PTL 5: Japanese Patent No. 4793872 PTL 6: Japanese Patent No. 4784990Summary of InventionTechnical Problem[0013] In general, it is difficult to bring the surface of amolten metal into perfect contact with cooling water whenthe hot molten metal is brought into contact with thecooling water in order to rapidly cool the molten metal.This is because the cooling water vaporizes upon coming intocontact with the surface (surface to be cooled) of the hotmolten metal and forms a steam film between the surface tobe cooled of the molten metal and the cooling water, that is, the cooling water is brought into the film boiling state. The presence of the steam film inhibits thefacilitation of cooling of the molten metal.
    [14] [0014] In the techniques described in Patent Literatures l to 3, attempt is made to remove a steam film formed aroundmetal particles by feeding a divided molten metal into alayer of a cooling liquid which is formed of a spiral streamof a cooling liquid. However, if the temperature of themetal particles is high, film boiling is likely to occur inthe cooling-liquid layer. In addition, since the metalparticles fed into the cooling-liquid layer move togetherwith the cooling-liquid layer, the difference in relativevelocity between the metal particles and the cooling-liquidlayer is small. This makes it difficult to prevent filmboiling state.
    [15] [0015] In the techniques described in Patent Literatures 4 to 6, a steam film that covers a molten metal is broken withthe power of steam explosion by which the film boiling stateis serially into the nucleate boiling state in order toproduce amorphous metal fine particles. Removing a steamfilm formed during film boiling with the power of steamexplosion is an effective approach. However, for causingsteam explosion by making the film boiling state into the nucleate boiling state, as is clear from the boiling curve illustrated in Fig. 4, it is necessary at least to reducethe surface temperature of the metal particles to the MHF(minimum heat flux) point or less at first. The graph shownin Fig. 4 is referred to as "boiling curve", whichschematically illustrates the relationship between thecooling capacity of a coolant that is water (cooling water)and the surface temperature of a material to be cooled. Asillustrated in Fig. 4, if the surface temperature of metalparticles is high, cooling of the metal particles to the MHFtemperature is performed in the film-boiling region. Theintensity of cooling of the metal particles performed in thefilm-boiling region is low because of the presence of steamfilms interposed between the surfaces to be cooled of themetal particles and the cooling water. Accordingly, if themetal particles are cooled from a temperature equal to ormore than the MHF temperature in order to produce anamorphous metal powder, there is a problem that the coolingrate for producing amorphous is insufficient.
    [16] [0016] An object of the present invention is to address theabove-described issues of the related art and to provide amethod for producing an atomized metal powder which enablesrapid cooling of the metal powder to be achieved and anamorphous metal powder to be produced.
    [17] [0017] In order to address the above-described issues, theinventors of the present invention conducted extensivestudies of various factors that may affect the MHF point inwater-injection cooling and, as a result, found that thetemperature and injection pressure of cooling water greatlyaffect the MHF point.
    [18] [0018] The results of a fundamental experiment conducted bythe inventors of the present invention are described below.[0019] As a material, a SUS304 stainless steel sheet (size: 20mm thick x 150 mm wide X 150 mm long) was used. Athermocouple was inserted into the material from the rearsurface such that the temperature of the material at aposition (at the center in the width and longitudinaldirections) 1 mm below the front surface can be measured.The material was charged into a heating furnace purged withan oxygen-free atmosphere and heated to 1200°C or more.Immediately after the heated material was removed from theheating furnace, cooling water was made to impinge on thematerial through cooling nozzles for atomization at variouswater temperatures and various injection pressures. Thechanges in the temperature of the material at a position 1 mm below the front surface were measured. The cooling capacities of the cooling water during cooling of thematerial were estimated by a calculation based on themeasured temperature data. A boiling curve was prepared onthe basis of the estimated cooling capacities. The MHFpoint was determined by considering the point at which thecooling capacity was sharply increased as a point at which atransition was made from the film boiling state to thetransition boiling state.
    [20] [0020] Fig. l summarizes the results.
    [21] [0021] As illustrated in Fig. l, in the case where coolingwater having a water temperature of 30°C, which has beencommonly used in an ordinary water atomization process, ismade to impinge on a material to be cooled at an injectionpressure of l MPa, the MHF point is about 700°C while thecooling water is made to impinge on the material to becooled. In the case where cooling water having a watertemperature of l0°C or less and 2°C or more is made toimpinge on a material to be cooled at an injection pressureof 5 MPa or more and 20 MPa or less, the MHF point is aboutl000°C or more while the cooling water is made to impinge onthe material to be cooled. Thus, it was found that reducingthe temperature (water temperature) of the cooling water to l0°C or less and increasing the injection pressure to 5 MPa or more increases the MHF point, that is, the temperature atwhich a transition is made from the film boiling state tothe transition boiling state.
    [22] [0022] In general, a metal powder has a surface temperature ofabout lOOO°C to l300°C immediately after the metal powder hasbeen produced by atomization of a molten metal. Thetemperature range in which cooling needs to be performed inorder to prevent crystallization from occurring is fromabout lOOO°C to the first crystallization temperature orless. If water-injection cooling is started such that thetemperature at which the metal powder starts being cooled ishigher than the MHF point, cooling is performed in the filmboiling region, in which the cooling capacity of the coolingwater is low, at the beginning of cooling. Therefore, whenwater-injection cooling is performed such that the MHF pointis equal to or higher than the temperature range in whichcooling needs to be performed, it become possible to startcooling the metal powder at least from the transitionboiling region, in which cooling of the metal powder isfacilitated compared with the film boiling region. As aresult, the rate at which the metal powder is cooled can bemarkedly increased. It was found if the metal power iscooled in the above-described manner with a high cooling capacity, a rapid cooling in the crystallization temperature range, which is essential for producing an amorphous metalpowder, can be readily achieved.[0023] The present invention was made on the basis of theforegoing findings and additional studies. The summary ofthe present invention is as follows. (l) A method for producing an atomized metal powder,the method including dividing a molten metal stream into ametal powder by making a fluid impinge on the molten metalstream; and cooling the metal powder, the fluid beinginjection water having a liquid temperature of lO°C or lessand an injection pressure of 5 MPa or more, the fluid beingused for dividing the molten metal stream and cooling themetal powder. (2) A method for producing an atomized metal powder,the method including dividing a molten metal stream into ametal powder by making a fluid impinge on the molten metalstream; and cooling the metal powder, the fluid being aninert gas, the fluid being used for dividing the moltenmetal stream, the cooling of the metal powder beingperformed with injection water having a liquid temperatureof lO°C or less and an injection pressure of 5 MPa or more. (3) The method for producing an atomized metal powderdescribed in (2), wherein the impinging of the injection water is performed after a temperature of the metal powder has reached l000°C or less. (4) The method for producing an atomized metal powderdescribed in any one of (l) to (3), wherein the molten metalstream includes a Fe-B alloy or a Fe-Si-B alloy, and theatomized metal powder is an amorphous metal powder.
    [27] [0027] It is not necessary to limit a method for melting themetal material. Common melting means such as an electricfurnace, a vacuum melting furnace, and a high-frequencymelting furnace may be used.
    [28] [0028]The molten metal is transferred from the melting furnace to a container such as a tundish and formed into an atomized metal powder inside an atomized metal powderproduction device. Fig. 2 illustrates a preferable exampleof a water-atomized metal powder production device used inthe present invention.
    [29] [0029] An example case of the present invention in which awater atomization process is employed is described belowwith reference to Fig. 2.
    [30] [0030] A molten metal l is passed downward from a containersuch as a tundish 3 into a chamber 9 through a molten-metal-guide nozzle 4 in the form of a molten metal stream 8. Theinside of the chamber 9 is purged with an inert gas (e.g., anitrogen gas or an argon gas) atmosphere by opening an inertgas valve ll.
    [31] [0031] A fluid 7 is made to impinge on the molten metal stream8 through nozzles 6 disposed on a nozzle header 5 so as todivide the molten metal stream 8 into a metal powder 8a. Inthe case where a water atomization process is used in thepresent invention, injection water (water jet) is used as afluid 7.
    [32] [0032]In the present invention, injection water (water jet) is used as a fluid 7. The injection water (water jet) used has a liquid temperature of l0°C or less and an injectionpressure of 5 MPa or more.[0033] If the liquid temperature (water temperature) of theinjection water is higher than l0°C, it becomes impossibleto perform water-injection cooling such that the desired MHFpoint of about l000°C or more is achieved and, as a result,the desired cooling rate may fail to be achieved.Accordingly, the liquid temperature (water temperature) ofthe injection water is limited to be l0°C or less and ispreferably set to 7°C or less. The term "desired coolingrate" used herein refers to the minimum cooling rate atwhich an amorphous metal powder can be produced, that is, acooling rate of about 105 to l06 K/s on average at which thetemperature is reduced from the temperature at whichsolidification has terminated to the first crystallizationtemperature (e.g., about 400°C to 600°C) on average.
    [34] [0034] If the injection pressure of the injection water (waterjet) is less than 5 MPa, it becomes impossible to performwater-injection cooling such that the MHF point is equal toor higher than the desired temperature even when the watertemperature of the cooling water is l0°C or less and, as aresult, the desired rapid cooling treatment (desired cooling rate) may fail to be achieved. Accordingly, the injection pressure of the injection water is limited to be 5 MPa ormore. The injection pressure of the injection water ispreferably set to 10 MPa or less because the MHF point stopsincreasing when the injection pressure is higher than 10MPa.
    [35] [0035] In the production of a metal powder according to thepresent invention in which water atomization is used,injection water having a water temperature and an injectionpressure that are controlled to be specific values asdescribed above is made to impinge on a molten metal streamin order to divide the molten metal stream into a metalpowder and cool and solidify the metal powder (including ametal powder in a molten state) at the same time.
    [36] [0036] The cooling water used as injection water is preferablystored in a cooling-water tank 15 (heat-insulated structure)disposed outside the water-atomized metal powder productiondevice 14 after it has been cooled to a low temperature witha heat exchanger such as a chiller 16 capable of cooling thecooling water to a low temperature. Means for feeding icefrom an ice-making machine into the tank may optionally beprovided because it is difficult to make cooling waterhaving a temperature of less than 3°C to 4°C with a common cooling-water-making machine due to freezing of the inside of the heat exchanger. It is preferable to make coolingwater having a temperature of more than O°C since coolingwater having a temperature of O°C or less is likely tofreeze. Needless to say that the cooling-water tank 15 isprovided with a high-pressure pump 17 that increases thepressure of the cooling water and feeds the cooling water tothe nozzle header 5 and a pipe 18 through which the coolingwater is fed from the high-pressure pump to the nozzleheader 5.
    [37] [0037] In the present invention, the division of the moltenmetal stream may be performed by a gas atomization process,in which an inert gas 22a is used as a fluid 7. In such acase, in the present invention, the resulting metal powderis further cooled with injection water. That is, in theproduction of a metal powder according to the presentinvention in which a gas atomization process is used, aninert gas is made to impinge on a molten metal stream inorder to divide the molten metal stream into a metal powder,and the metal powder (including a metal powder in a moltenstate) is cooled with injection water having an injectionpressure: 5 MPa or more and a water temperature of 10°C orless. Fig. 3 illustrates a preferable example of a gas-atomized metal powder production device used in the present invention.
    [38] [0038] An example case of the present invention in which a gasatomization process is used is described below withreference to Fig. 3.
    [39] [0039] A molten metal l is transferred from a melting furnace2 to a container such as a tundish 3 and passed downwardfrom the container into a chamber 9 through a molten-metal-guide nozzle 4 of a gas-atomized metal powder productiondevice l9 in the form of a molten metal stream 8. Theinside of the chamber 9 is purged with an inert gasatmosphere by opening an inert gas valve ll.
    [40] [0040] An inert gas 22a is made to impinge on the molten metalstream 8 through gas injection nozzles 22 disposed in a gasnozzle header 2l in order to divide the molten metal stream8 into a metal powder 8a. Injection water 25a is made toimpinge on the metal powder 8a at the position at which thetemperature of the metal powder 8a is about l000°C, at whichthe temperature range in which cooling needs to be performedis preferably achieved, in order to cool the metal powder8a. The injection water 25a has an injection pressure of 5MPa or more and a water temperature of l0°C or less.
    [41] [0041] Performing cooling with injection water having an injection pressure of 5 MPa or more and a water temperatureof lO°C or less increases the MHF point to about lOOO°C.Accordingly, in the present invention, a metal powder thatpreferably has a temperature of about lOOO°C or less iscooled with injection water having an injection pressure of5 MPa or more and a water temperature of lO°C or less. Thisenables cooling to be performed in the transition boilingregion from the beginning of cooling and facilitates coolingthe metal powder. As a result, the desired cooling rate maybe readily achieved. The temperature of the metal powdercan be controlled by changing the distance between the gasatomization point and the position at which the injectionwater is made to impinge on the metal powder.
    [42] [0042] In the case where the temperature of the metal powder8a is as high as more than lOOO°C at the beginning ofcooling with the injection water, cooling is performed inthe film boiling state even when the water temperature ofthe injection water is less than 5°C. In such a case, thecooling capacity of injection water is low compared withcooling performed in the transition boiling state, whichoccurs when cooling is started at lOOO°C or less, but highcompared with an ordinary cooling treatment performed in thefilm boiling state at an injection pressure of less than 5 MPa and a water temperature of lO°C or more. In addition, the amount of time during which cooling is performed in thefilm boiling state can be reduced. Furthermore, reducingthe water temperature of the injection water and increasingthe injection pressure of the injection water increases theMHF point and enhances the amorphous nature of the metalpowder to be produced. For example, setting the watertemperature of the injection water to 5°C or less and theinjection pressure of the injection water to l0 MPa or moreincreases the MHF point to about l030°C. This enables ametal powder having a large particle diameter to be changedinto an amorphous state.
    [43] [0043] As described above, in the present invention, a moltenmetal stream is divided by a gas atomization process andsubsequently cooled with injection water having an injectionpressure of 5 MPa or more and a water temperature of l0°C orless. Performing water-injection cooling under the above-described conditions when the temperature of the metalpowder is the MHF point or less further increases thecooling rate.
    [44] [0044] Similarly to the above-described case where a wateratomization process used, the cooling water used asinjection water is preferably stored in the cooling-water tank 15 (heat-insulated structure) disposed outside the gas- atomized metal powder production device 19 after it has beencooled to a low temperature with a heat exchanger such as achiller 16 capable of cooling the cooling water to a lowtemperature. Means for feeding ice from an ice-makingmachine into the tank may optionally be provided. Needlessto say that the gas nozzle header 21 is connected to a gasbomb 27 with a pipe 28 and that the cooling-water tank 15 isprovided with, similarly to the water-atomized metal powderproduction device, a high-pressure pump 17 that increasesthe pressure of the cooling water and feeds the coolingwater to cooling-water injection nozzles 25 and a pipe 18through which the cooling water is fed from the high-pressure pump to the cooling-water injection nozzles 25.[0045] For changing a metal powder into an amorphous powder,it is necessary to rapidly cool the metal powder in thecrystallization temperature range. The critical coolingrate required for producing an amorphous powder variesdepending on the type of the alloy systemd For example, thecritical cooling rate of Fe-B alloys (FeæByfl is 1.0 x 106K/s and the critical cooling rate of Fe-Si-B alloys(FeWSi1fiä¿) is 1.8 X 105 K/s (The Japan Society of MechanicalEngineers: Boiling Heat Transfer and Cooling, p. 208, 1989,Japan Industrial Publishing Co., Ltd.). The critical cooling rates required for producing an amorphous powder of typical amorphous alloys such as Fe-base alloys and Ni-basealloys are about 105 to 106 K/s. The method for producing ametal powder, in which performing cooling in the filmboiling region is prevented from the beginning of coolingand cooling is performed in the transition boiling region orthe nucleate boiling region as in the present invention,enables the above-described cooling rate to be achieved.EXAMPLES
    [46] [0046] (Example 1) A metal powder was producing using a water-atomizedmetal powder production device illustrated in Fig. 2.
    [47] [0047] A raw material having a composition containing (withthe balance being inevitable impurities), by at%, 79%Fe-10%Si-11%B (FewSi1fiä¿) was prepared. The raw material wasmelted in a melting furnace 2 at about 1550°C. Thus, about50 kgf of a molten metal was prepared. The molten metal wasslowly cooled to 1350°C in the melting furnace 2 andsubsequently charged into a tundish 3. The inside of achamber 9 was purged with a nitrogen gas atmosphere byopening an inert gas valve 11. Before the molten metal wascharged into the tundish 3, a high-pressure pump 17 wasbrought into operation and cooling water stored in a cooling-water tank 15 (volume: 10 m3) was fed to a nozzle header 5. Thus, injection water (fluid) 7 started beingejected through water injection nozzles 6. The position atwhich the molten metal stream 8 was brought into contactwith the injection water (fluid) 7 was set to be a position200 mm below the molten-metal-guide nozzle 4.
    [48] [0048] The molten metal l charged in the tundish 3 was passeddownward into the chamber 9 through the molten-metal-guidenozzle 4 in the form of a molten metal stream 8. The moltenmetal stream 8 was contacted with injection waters (fluids)7 having various water temperatures and injection pressuresas described in Table l, and was divided into a metal powderand was cooled by being mixed with the cooling water. Themetal powder was collected through a collection portincluding a metal powder collection valve 13.
    [49] [0049] After dusts other than the metal powder particles hadbeen removed from the metal powders, a sample was taken fromeach of the metal powders and subjected to an X-raydiffraction measurement. The crystallization ratio of eachsample was determined on the basis of the ratio between theintegrated intensities of diffracted X-rays. The amorphousratio (= l - crystallization ratio) of each sample wascalculated by subtracting the crystallization ratio from l.
    [50] [0050] [Table 1] Powder Atomization method Division and cooling Amorphous ratio Remarks No. Type of Fluid injection conditions O: 90% or more injection Injection Water x: Less than 90%fluid pressure temperature(MPH) (°C) A1 Water atomization Water 5 30 x 74% Comparativeexample A2 Water 5 8 O 92% lnventionexample A3 Water 1 8 x 82% Comparativeexample
    [51] [0051] The metal powder prepared in Invention Example had acrystallization ratio of less than 10%. This confirms thatthe most part of the metal powder was amorphous. On theother hand, the metal powders prepared in ComparativeExamples which did not fall within the range of the presentinvention each had a crystallization ratio of 10% or more.This confirms that the metal powders were not amorphous.Since it is considered that the critical cooling raterequired for changing a metal powder having the same alloycomposition (FeWSi1fiä¿) as that of the metal powder used in Example 1 into an amorphous metal powder is 1.8 X 105 K/s, it is considered that a cooling rate of 1.8 X 105 K/s or morewas achieved in Invention Example.(Example 2) A metal powder was prepared using a gas-atomized metalpowder production device illustrated in Fig. 3.
    [52] [0052] A raw material having a composition containing (withthe balance being inevitable impurities), by at%, 79%Fe-10%Si-11%B (FewSi1fiä¿) was prepared. The raw material wasmelted in a melting furnace 2 at about 1550°C. Thus, about10 kgf of a molten metal was prepared. The molten metal wasslowly cooled to 1400°C in the melting furnace andsubsequently charged into a tundish 3. The inside of achamber 9 was purged with a nitrogen gas atmosphere byopening an inert gas valve 11. Before the molten metal wascharged into the tundish 3, a high-pressure pump 17 wasbrought into operation and cooling water stored in acooling-water tank 15 (volume: 10 m3) was fed to waterinjection nozzles 25. Thus, injection water (fluid) 25astarted being ejected through the water injection nozzles25.
    [53] [0053] The molten metal 1 charged in the tundish 3 was passed downward into the chamber 9 through the molten-metal-guide nozzle 4 in the form of a molten metal stream 8, which was brought into contact with an argon gas (fluid) 22a ejectedthrough gas nozzles 22 at an injection pressure of 5 MPa soas to be divided into a metal powder 8a. The metal powderwas cooled and solidified due to thermal radiation and theaction of the atmosphere gas. The metal powder wassubsequently cooled with each of injection waters havingvarious injection pressures and water temperatures asdescribed in Table 2 at the time the metal powder had beencooled to about l000°C, that is, at the position 350 mm (or,250 mm) below the gas atomization point (the point at whichthe molten metal stream 8 was brought into contact with theargon gas 22a). The cooled metal powder was collectedthrough a collection port including a metal powdercollection valve 13.
    [54] [0054] After dusts other than the metal powder particles hadbeen removed from the metal powders, a sample was taken fromeach of the metal powders and subjected to an X-raydiffraction measurement. The crystallization ratio of eachsample was determined on the basis of the ratio between theintegrated intensities of diffracted X-rays. The amorphousratio (= l - crystallization ratio) of each sample wascalculated by subtracting the crystallization ratio from l.Table 2 summarizes the results. A sample having an amorphous ratio of 90% or more was evaluated as passed.
    [56] [0056] The metal powders prepared in Invention Examples had acrystallization ratio of less than 10%. This confirms thatthe most parts of the metal powders were amorphous. It isalso confirmed that the most part of the powder No. B4,which had been cooled with injection water that fell withinthe range of the present invention, was amorphous althoughthe average temperature of the powder at the beginning ofcooling was 1046%L This is because, that the MHF point wasincreased to about 1050°C by setting the injection pressureof the injection water to 20 MPa and the water temperatureof the injection water to 4°C.
    [57] [0057] On the other hand, the metal powders prepared inComparative Examples which did not fall within the range ofthe present invention each had a crystallization ratio of10% or more. This confirms that the metal powders were notamorphous. Since it is considered that the critical coolingrate required for changing a metal powder having the samealloy composition (FewSi1&ä¿) as that of the metal powderused in Example 2 into an amorphous metal powder is 1.8 x 105K/s, it is considered that a cooling rate of 1.8 X 105 K/s ormore was achieved in Invention Examples.
    [59] [0059] The molten metal l charged in the tundish 3 was passeddownward into the chamber 9 through the molten-metal-guidenozzle 4 in the form of a molten metal stream 8, which wasbrought into contact with an argon gas (fluid) 22a ejectedthrough gas nozzles 22 at an injection pressure of 5 MPa soas to be divided into a metal powder 8a. The metal powderwas cooled and solidified due to thermal radiation and the action of the atmosphere gas. The metal powder was _33_ subsequently cooled with injection water having a specificinjection pressure and a specific water temperaturedescribed in Table 3 at the time the metal powder had beencooled to about l000°C, that is, at the position 450 mm (or,250 mm) below the gas atomization point. The metal powderwas collected through a collection port l3. After dustsother than the metal powder particles had been removed fromthe metal powders, a sample was taken from each of the metalpowders and subjected to an X-ray diffraction measurement.The crystallization ratio of each sample was determined onthe basis of the ratio between the integrated intensities ofdiffracted X-rays. The amorphous ratio (= l -crystallization ratio) of each sample was calculated bysubtracting the crystallization ratio from l. Table 3summarizes the results. A sample having an amorphous ratioof 90% or more was evaluated as passed. Although some ofthe metal powders contained compounds as impurities, thecontents of the compounds contained as impurities in suchmetal powders were less than 1% by mass.
    [60] [0060] _34_ [Table 3] Powder Atomization method Division Cooling Amorphous ratio Remarks No. Type of Injection Type of Fluid injection conditions Average powder Water O: 90% or more injection condition injection fluid temperature at injection x: Less than 90%fluid injection injection Water the beginning of position*pressure pressure temperature cooling (°C) (mm)(MPa) (MPa) (°C) C1 Gas atomization Gas 5 Water 5 30 995 450 x 87% Comparativeexample C2 Water 5 8 994 450 O 93% lnventionexample C3 Water 1 8 995 450 x 78% Comparativeexample C4 Water 20 4 1047 250 O 95% lnventionexample *) Distance from the gas atomization point
    [61] [0061] The metal powders prepared in Invention Examples had acrystallization ratio of less than 10%. This confirms thatthe most parts of the metal powders were amorphous. It isconfirmed that the most part of the powder No. C4, which hadbeen cooled with injection water that fell within the rangeof the present invention, was amorphous although the averagetemperature of the powder at the beginning of cooling was1047°C. This is because, while the metal powder was cooled,the MHF point was increased to about 1050°C by setting theinjection pressure of the injection water to 20 MPa and thewater temperature of the injection water to 4°C.
    [62] [0062] On the other hand, the metal powders prepared inComparative Examples which did not fall within the range ofthe present invention each had a crystallization ratio of10% or more. This confirms that the metal powders were notamorphous. Since it is considered that the critical coolingrate required for changing a metal powder having the samealloy composition (FeæB[fl as that of the metal powder usedin Example 3 into an amorphous metal powder is 1.0 x 106 K/s,it is considered that a cooling rate of 1.0 X 106 K/s or morewas achieved in Invention Examples.
    [63] [0063] 8a91112131416DEVICE)171819212224 MOLTEN METALMELTING FURNACE TUNDISHMOLTEN-METAL-GUIDE NOZZLENOZZLE HEADERNOZZLES (WATER INJECTION NOZZLES)FLUID (INJECTION WATER)MOLTEN METAL STREAM METAL POWDERCHAMBER HOPPER INERT GAS VALVE OVERFLOW VALVE METAL POWDER COLLECTION VALVE WATER-ATOMIZED METAL POWDER PRODUCTION DEVICECOOLING-WATER TANK CHILLER (LOW-TEMPERATURE COOLING WATER PRODUCTIONHIGH-PRESSURE PUMPCOOLING-WATER PIPEGAS-ATOMIZED METAL POWDER PRODUCTION DEVICENOZZLE HEADER (GAS NOZZLE HEADER)GAS NOZZLES HEADER VALVE COOLING-WATER INJECTION NOZZLES 25a INJECTION WATER 26 COOLING-WATER VALVE 27 GAS BOMB FOR GAS ATOMIZATION 28 HIGH-PRESSURE GAS PIPE
    权利要求:
    Claims (4)
    [1] 1. l. A method for producing an atomized metal powder, themethod comprising dividing a molten metal stream into ametal powder by making a fluid impinge on the molten metalstream; and cooling the metal powder, the fluid beinginjection water having a liquid temperature of lO°C or lessand an injection pressure of 5 MPa or more, the fluid beingused for dividing the molten metal stream and cooling the metal powder.
    [2] 2. A method for producing an atomized metal powder, themethod comprising dividing a molten metal stream into ametal powder by making a fluid impinge on the molten metalstream; and cooling the metal powder, the fluid being aninert gas, the fluid being used for dividing the moltenmetal stream, the cooling of the metal powder beingperformed with injection water having a liquid temperature of lO°C or less and an injection pressure of 5 MPa or more.
    [3] 3. The method for producing an atomized metal powderaccording to Claim 2, wherein the impinging of the injectionwater is performed after a temperature of the metal powder has reached lOOO°C or less. _39_
    [4] 4. The method for producing an atomized metal powderaccording to any one of Claims l to 3, wherein the moltenmetal stream includes a Fe-B alloy or a Fe-Si-B alloy, and the atomized metal powder is an amorphous metal powder.
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP2014072786|2014-03-31|
    PCT/JP2015/001407|WO2015151420A1|2014-03-31|2015-03-13|Processes for producing atomized metal powder|
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