TW201730899A - Method of fabricating iron-based soft magnetic powder - Google Patents
Method of fabricating iron-based soft magnetic powder Download PDFInfo
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本發明係關於一種軟磁粉體的製造方法,特別是關於一種鐵基軟磁粉體的製造方法。 The present invention relates to a method for producing a soft magnetic powder, and more particularly to a method for producing an iron-based soft magnetic powder.
鐵矽鋁(FeSiAl)合金磁粉是一種具有軟磁性之金屬粉末,披覆一層導電絕緣物質如水玻璃、高嶺土、磷酸鹽、樹脂後,形成所謂之軟磁複合材(Soft magnetic composites;SMC)。軟磁複合材粉末可以用高壓成型機,通過模具直接壓製成各種形狀之軟磁性元件,經適當之溫度應力消除退火後直接使用,具有三維之均向磁性。軟磁複合材粉末可作為被動元件之電感,應用於3C產品、太陽能及電動車之大電流電源之扼流電感(Power choke),或是濾除電磁波干擾雜訊之共模濾波電感(Common mode choke)、功率因數修正電路(Power factor correction circuit、PFC)用電感。軟磁複合材粉末亦可發展應用於汽車之防鎖死剎車系統(Anti-lock Braking System;ABS)伺服馬達、方向盤液壓系統馬達、點火系統之脈衝變壓器(Pulse transformer)、傳感器、柴油引擎之燃料噴射(Injector)致動器等。 FeSiAl alloy magnetic powder is a kind of soft magnetic metal powder coated with a layer of conductive insulating materials such as water glass, kaolin, phosphate and resin to form so-called soft magnetic composites (SMC). The soft magnetic composite powder can be directly pressed into soft magnetic elements of various shapes by a high-pressure molding machine, and can be directly used after being subjected to appropriate temperature stress elimination annealing, and has three-dimensional uniform magnetic properties. Soft magnetic composite powder can be used as the inductance of passive components, applied to the choke inductor of 3C products, solar and electric vehicles, or common mode filter inductors that filter out electromagnetic interference noise (Common mode choke) ), inductance for power factor correction circuit (PFC). Soft magnetic composite powder can also be developed for anti-lock Braking System (ABS) servo motors, steering wheel hydraulic system motors, pulse transformers for ignition systems, sensors, fuel injection for diesel engines. (Injector) actuators, etc.
軟磁複合材之導磁率、磁損、耐偏壓磁性及價位各有所長,其中以Fe-9.5Si-5.5Al具有導磁率高、磁損低、成本低及性價比高之優點,所製之磁粉芯(Powder core)廣泛用於電源供應器之扼流電感。 The magnetic permeability, magnetic loss, bias-resistant magnetic properties and price of soft magnetic composite materials have their own advantages. Among them, Fe-9.5Si-5.5Al has the advantages of high magnetic permeability, low magnetic loss, low cost and high cost performance. The powder core is widely used in the choke inductor of power supplies.
鐵矽鋁合金磁粉之製備方法有鑄造粉碎法、氣噴霧法、及水噴霧法等。鑄造粉碎法製程包括熔融鑄錠、均質退火及 粉碎研磨等,製程長及成本高,且粉末顆粒有不規則之尖銳角,絕緣披覆效果差。氣噴法所製粉末為圓球形,視密度(Apparent density)高、氧含量低可小於100ppm,絕緣披覆於圓球形粉末均勻,但壓製磁粉芯之成型密度卻低,且具有孔隙多、反向磁場係數高、不易獲得高導磁率的缺點。為得到高成型密度,氣噴後粉末需再粉碎以改變圓球形貌。但即使如此,所壓製之磁粉芯強度仍差。以水噴霧法所製備之鐵矽鋁粉末,製程短、熔融湯液水噴後經篩選粒徑後即可使用,粉末形貌呈長條不規則形狀,粉末壓胚成型性高,低成形壓力下可得高磁芯密度、磁粉芯保形性、強度優於氣噴霧法所製之圓球形粉末,組成均勻性優於鑄造粉碎法,鑄造粉碎法所製粉末有組成偏析之問題。水噴霧法製得的鐵矽鋁粉末經絕緣披覆後,所製備之軟磁複合材磁芯導磁率和磁損等優於其它二種方法。軟磁複合材磁芯之磁損主要源自渦流損和磁滯損。渦流損與顆粒之絕緣披覆是否均勻、絕緣電阻是否夠大有關;絕緣披覆之均勻性則與顆粒形貌有關。顆粒銳角少、表面平滑則有助於提升絕緣披覆效果。磁滯損則與顆粒內晶粒大小有關,晶粒愈大則磁滯損愈小,通常粉末顆粒愈大、內部晶粒則愈大。不論使用何種方法生產,鐵矽鋁粉末粒徑大小與磁芯之導磁率和磁損關係密切,粒徑愈大則導磁率及磁損愈大。 The preparation method of the iron-iron aluminum alloy magnetic powder includes a casting pulverization method, a gas spray method, and a water spray method. The casting pulverization process includes molten ingots, homogenization annealing and Grinding and grinding, etc., the process length and cost are high, and the powder particles have irregular sharp angles, and the insulating coating effect is poor. The powder produced by the gas jet method is spherical, the apparent density is high, the oxygen content is less than 100ppm, the insulation is coated on the spherical powder, but the density of the pressed magnetic powder core is low, and the porosity is large and reversed. The magnetic field coefficient is high, and the disadvantage of high magnetic permeability is not easily obtained. In order to obtain a high molding density, the powder after the air jet needs to be pulverized to change the spherical shape. Even so, the strength of the pressed magnetic powder core is still poor. The iron strontium aluminum powder prepared by the water spray method has a short process and can be used after the sprayed water is sprayed, and the powder has a long and irregular shape, and the powder preform has high moldability and low forming pressure. The high magnetic core density, magnetic powder core shape retention and strength are superior to those of the spherical powder prepared by the gas spray method, and the composition uniformity is superior to the casting pulverization method, and the powder prepared by the casting pulverization method has the problem of composition segregation. After the iron enamel aluminum powder prepared by the water spray method is coated by insulation, the magnetic permeability and magnetic loss of the prepared soft magnetic composite core are superior to the other two methods. The magnetic loss of the soft magnetic composite core is mainly derived from eddy current loss and magnetic hysteresis loss. The eddy current loss is related to whether the insulation coating of the particles is uniform and whether the insulation resistance is large enough; the uniformity of the insulation coating is related to the particle morphology. The low sharp angle of the particles and the smooth surface help to improve the insulation coating effect. The magnetic hysteresis loss is related to the grain size in the particle. The larger the crystal grain, the smaller the magnetic hysteresis loss. Generally, the larger the powder particle, the larger the inner crystal grain. Regardless of the method used, the particle size of the iron-bismuth aluminum powder is closely related to the magnetic permeability and magnetic loss of the magnetic core. The larger the particle size, the larger the magnetic permeability and magnetic loss.
一般水噴霧金屬粉末之製程,可採用大氣下或充氮氣下以感應爐熔煉,高溫熔融之合金湯液經由分液槽之流出管垂直流入高壓水噴霧系統中,高溫熔融湯液與高壓水束撞擊細化為小液滴後進入水噴霧槽中冷卻,沉降過濾後,以溫度100~120℃於真空或大氣中烘乾。對於鐵系合金,如鐵矽鋁合金,由於在高溫熔煉過程及在熔湯出口流嘴處,矽和鋁易氧化形成氧化矽和氧化鋁,所以當熔湯細化冷卻成粉末顆粒後,粉末顆粒內部含有氧化介在物,且鐵矽鋁合金熔湯液滴與水蒸氣分解之氧發生氧化作用,故在液滴表面易形成氧化鋁。前述的氧化物、介在物及烘乾過程時鐵之鏽蝕會引入氧於鐵矽鋁合金中。其中,氧化物如以介 在物存在於鐵矽鋁合金粉中,則矯頑磁力(Hc)、磁滯損(Ph)增加且磁損增大。為減少水噴粉含氧量,一般皆以改良設備為出發點,包括;(1)熔湯不與大氣接觸;(2)噴霧時防止水蒸氣與熔湯液滴接觸;或(3)粉末凝固後在還原性環境中儲存等。或是,加入使熔湯不易氧化之元素,以降低水噴金屬粉末之含氧量。然而,這些方法會增加製造時間成本及硬體成本。 Generally, the process of spraying water metal powder can be smelted in an induction furnace under the atmosphere or under nitrogen, and the molten alloy molten solution flows vertically into the high-pressure water spray system through the outlet pipe of the liquid separation tank, and the high-temperature molten soup liquid and the high-pressure water beam After the impact is refined into small droplets, it enters the water spray tank for cooling, and after sedimentation and filtration, it is dried at a temperature of 100-120 ° C in a vacuum or in the atmosphere. For iron-based alloys, such as iron-bismuth aluminum alloys, tantalum and aluminum are easily oxidized to form cerium oxide and aluminum oxide during the high-temperature melting process and at the melt outlet nozzle, so when the melt is refined and cooled into powder particles, the powder The inside of the granule contains an oxidizing medium, and the molten iron of the smelting aluminum alloy melts with oxygen decomposed by water vapor, so that alumina is easily formed on the surface of the droplet. The rust of iron in the aforementioned oxide, intercalation and drying processes introduces oxygen into the iron-iron alloy. Among them, the oxide such as When the substance is present in the iron-bismuth aluminum alloy powder, the coercive force (Hc), the magnetic hysteresis loss (Ph) increase, and the magnetic loss increases. In order to reduce the oxygen content of the water spray powder, the improvement equipment is generally used as the starting point, including; (1) the molten soup is not in contact with the atmosphere; (2) the water vapor is prevented from contacting the molten liquid droplets during spraying; or (3) the powder is solidified. After storage in a reducing environment, etc. Alternatively, an element which makes the melt less oxidizable is added to reduce the oxygen content of the water spray metal powder. However, these methods increase manufacturing time and hardware costs.
故,有必要提供一種鐵基軟磁粉體的製造方法,以解決習用技術所存在的問題。 Therefore, it is necessary to provide a method for manufacturing an iron-based soft magnetic powder to solve the problems of the conventional technology.
本發明之主要目的在於提供一種鐵基軟磁粉體的製造方法,其係在大氣下使用水噴霧法,透過控制製程中的參數以得到一氧含量在1820ppm至3000ppm之間、一導磁率大於等於125,及一磁損值在0至1000kw/m3的鐵基軟磁粉體。 The main object of the present invention is to provide a method for producing an iron-based soft magnetic powder, which is subjected to a water spray method under the atmosphere, and controls a parameter in the process to obtain an oxygen content of between 1820 ppm and 3000 ppm and a magnetic permeability of greater than or equal to 125, and an iron-based soft magnetic powder having a magnetic loss value of 0 to 1000 kW/m 3 .
為達上述之目的,本發明提供一種鐵基軟磁粉體的製造方法,其包含步驟:進行一熔煉步驟,使具有一預定成分比例的多個材料熔煉形成一熔湯液,其中該熔湯液的溫度是在攝氏1519度至攝氏1588度之間;以及進行一水噴霧步驟,其中該熔湯液從口徑為6毫米至8毫米的一流嘴流出,並通過呈雙V型水幕的一水霧冷卻該熔湯液,以製得一鐵基軟磁粉體;其中該鐵基軟磁粉體具有一氧含量在1820ppm至3000ppm之間、一導磁率大於等於125,及一磁損值在0至1000kw/m3之間;其中該水霧與該熔湯液的一重量比值是在3.84至9.17之間。 In order to achieve the above object, the present invention provides a method for producing an iron-based soft magnetic powder, comprising the steps of: performing a melting step of smelting a plurality of materials having a predetermined composition ratio to form a molten broth, wherein the molten broth The temperature is between 1519 degrees Celsius and 1588 degrees Celsius; and a water spray step is performed, wherein the molten liquor flows out from a first-class mouth having a diameter of 6 mm to 8 mm, and passes through a water having a double V-shaped water curtain Cooling the molten liquid to obtain an iron-based soft magnetic powder; wherein the iron-based soft magnetic powder has an oxygen content of between 1820 ppm and 3000 ppm, a magnetic permeability of greater than or equal to 125, and a magnetic loss value of 0 to Between 1000kw/m 3 ; wherein the weight ratio of the water mist to the molten liquor is between 3.84 and 9.17.
在本發明之一實施例中,該水噴霧步驟包含:以一第一噴嘴組及一第二噴嘴組提供呈雙V型水幕的該水霧,其中該第一噴嘴組包含相對設置的二第一水噴嘴,且該水霧從該些第一水噴嘴中的每一個噴出至接觸該熔湯液的一第一噴距是在160毫米至254毫米之間;及該第二噴嘴組包含相對設置的二第二水噴嘴,且該水霧從該些第二水噴嘴中的每一個噴出至接觸該熔湯液的一第二噴距是在160毫米至254毫米之間。 In an embodiment of the present invention, the water spraying step includes: providing the water mist in a double V-shaped water curtain with a first nozzle group and a second nozzle group, wherein the first nozzle group comprises two opposite nozzles a first water nozzle, and the water mist is ejected from each of the first water nozzles to a first spray distance contacting the molten liquid between 160 mm and 254 mm; and the second nozzle group comprises Two second water nozzles are disposed opposite to each other, and the water mist is ejected from each of the second water nozzles to a second spray distance contacting the molten liquor between 160 mm and 254 mm.
在本發明之一實施例中,該雙V型水幕是通過將該第一噴嘴組及該第二噴嘴組交叉排列,且該些第一水噴嘴及該些第二水噴嘴係朝下進行一傾斜噴霧而形成。 In an embodiment of the present invention, the double V-shaped water curtain is arranged by crossing the first nozzle group and the second nozzle group, and the first water nozzles and the second water nozzles are downwardly arranged. Formed by a tilting spray.
在本發明之一實施例中,該流嘴的口徑為6毫米、及該水霧與該熔湯液的重量比值是在5.03至9.17之間,以製得該氧含量在1820ppm至2760ppm之間、該導磁率在125至130之間、及該磁損值在858kw/m3至983kw/m3之間的該鐵基軟磁粉體。 In an embodiment of the invention, the nozzle has a diameter of 6 mm, and the weight ratio of the water mist to the molten liquor is between 5.03 and 9.17 to obtain the oxygen content between 1820 ppm and 2760 ppm. The iron-based soft magnetic powder having a magnetic permeability of between 125 and 130 and a magnetic loss value of between 858 kw/m 3 and 983 kw/m 3 .
在本發明之一實施例中,該水霧之一水壓在300巴至350巴之間。 In one embodiment of the invention, one of the water mists has a water pressure between 300 and 350 bar.
在本發明之一實施例中,該流嘴的口徑為8毫米、該熔湯液的溫度是在攝氏1521度至攝氏1547度之間、及該水霧與該熔湯液的重量比值是在3.84至4.74之間,以製得該氧含量在2350ppm至2720ppm之間、該導磁率在134至147之間、及該磁損值在934kw/m3至993kw/m3的該鐵基軟磁粉體。 In an embodiment of the invention, the nozzle has a diameter of 8 mm, the temperature of the molten liquid is between 1521 degrees Celsius and 1547 degrees Celsius, and the weight ratio of the water mist to the molten liquor is Between 3.84 and 4.74, the iron-based soft magnetic powder having the oxygen content between 2350 ppm and 2720 ppm, the magnetic permeability between 134 and 147, and the magnetic loss value between 934 kw/m 3 and 993 kw/m 3 is obtained . body.
在本發明之一實施例中,該水霧之一水壓在350巴至380巴之間。 In one embodiment of the invention, one of the water mists has a water pressure between 350 and 380 bar.
在本發明之一實施例中,該鐵基軟磁粉體包含鐵矽鋁軟磁粉體、鐵矽軟磁粉體或鐵矽鉻軟磁粉體。 In an embodiment of the invention, the iron-based soft magnetic powder comprises iron-iron-aluminum soft magnetic powder, iron-iron soft magnetic powder or iron-iron chromium soft magnetic powder.
在本發明之一實施例中,該鐵基軟磁粉體的成分包含:9.6wt%至9.8wt%的矽;5.3wt%至6wt%的鋁;以及84.2wt%至85.0wt%的鐵。 In an embodiment of the invention, the composition of the iron-based soft magnetic powder comprises: 9.6 wt% to 9.8 wt% of rhodium; 5.3 wt% to 6 wt% of aluminum; and 84.2 wt% to 85.0 wt% of iron.
在本發明之一實施例中,該熔煉步驟係以一大氣熔煉法進行。 In one embodiment of the invention, the smelting step is carried out in an atmospheric melting process.
10‧‧‧方法 10‧‧‧ method
11‧‧‧步驟 11‧‧‧Steps
12‧‧‧步驟 12‧‧‧ steps
21‧‧‧第一噴嘴組 21‧‧‧First nozzle group
22‧‧‧第二噴嘴組 22‧‧‧second nozzle group
23‧‧‧水霧 23‧‧‧Water mist
24‧‧‧熔湯液 24‧‧‧ molten soup
211‧‧‧第一水噴嘴 211‧‧‧First water nozzle
221‧‧‧第二水噴嘴 221‧‧‧Second water nozzle
L1‧‧‧第一噴距 L1‧‧‧first spray distance
L2‧‧‧第二噴距 L2‧‧‧second spray distance
α‧‧‧角度 ‧‧‧‧ angle
第1圖:本發明實施例之鐵基軟磁粉體的製造方法的流程圖。 Fig. 1 is a flow chart showing a method of producing an iron-based soft magnetic powder according to an embodiment of the present invention.
第2A圖:本發明實施例之第一噴嘴組及第二噴嘴組的立體示意圖。 2A is a perspective view showing the first nozzle group and the second nozzle group in the embodiment of the present invention.
第2B圖:本發明實施例之第一噴嘴組及第二噴嘴組的側視 示意圖。 2B is a side view of the first nozzle group and the second nozzle group of the embodiment of the present invention schematic diagram.
為了讓本發明之上述及其他目的、特徵、優點能更明顯易懂,下文將特舉本發明較佳實施例,並配合所附圖式,作詳細說明如下。再者,本發明所提到的方向用語,例如上、下、頂、底、前、後、左、右、內、外、側面、周圍、中央、水平、橫向、垂直、縱向、軸向、徑向、最上層或最下層等,僅是參考附加圖式的方向。因此,使用的方向用語是用以說明及理解本發明,而非用以限制本發明。 The above and other objects, features and advantages of the present invention will become more <RTIgt; Furthermore, the directional terms mentioned in the present invention, such as upper, lower, top, bottom, front, rear, left, right, inner, outer, side, surrounding, central, horizontal, horizontal, vertical, longitudinal, axial, Radial, uppermost or lowermost, etc., only refer to the direction of the additional schema. Therefore, the directional terminology used is for the purpose of illustration and understanding of the invention.
請參照第1圖所示,第1圖是本發明實施例之鐵基軟磁粉體的製造方法10的流程圖。本發明實施例之鐵基軟磁粉體的製造方法10主要包含下列步驟:進行一熔煉步驟11,使具有一預定成分比例的多個材料熔煉形成一熔湯液,其中該熔湯液的溫度是在攝氏1519度至攝氏1588度之間;以及進行一水噴霧步驟12,其中該熔湯液從口徑為6毫米至8毫米的一流嘴流出,並通過呈雙V型水幕的一水霧冷卻該熔湯液,以製得一鐵基軟磁粉體;其中該鐵基軟磁粉體具有一氧含量在1820ppm至3000ppm之間、一導磁率大於等於125,及一磁損值在0至1000kw/m3之間;其中該水霧與該熔湯液的一重量比值是在3.84至9.17之間。 Referring to Fig. 1, Fig. 1 is a flow chart showing a method 10 for manufacturing an iron-based soft magnetic powder according to an embodiment of the present invention. The method 10 for manufacturing an iron-based soft magnetic powder according to an embodiment of the present invention mainly comprises the following steps: performing a melting step 11 to melt a plurality of materials having a predetermined composition ratio to form a molten liquid, wherein the temperature of the molten liquid is Between 1519 degrees Celsius and 1588 degrees Celsius; and a water spray step 12, wherein the molten liquor flows from a first-class mouth having a diameter of 6 mm to 8 mm, and is cooled by a water mist in a double V-shaped water curtain. The molten liquid is prepared to obtain an iron-based soft magnetic powder; wherein the iron-based soft magnetic powder has an oxygen content of between 1820 ppm and 3000 ppm, a magnetic permeability of greater than or equal to 125, and a magnetic loss value of from 0 to 1000 kw/ Between m 3 ; wherein the weight ratio of the water mist to the molten liquor is between 3.84 and 9.17.
請參照第1圖所示,本發明一實施例之鐵基軟磁粉體的製造方法10首先係:進行一熔煉步驟11,使具有一預定成分比例的多個材料熔煉形成一熔湯液,其中該熔湯液的溫度是在攝氏1519度至攝氏1588度之間。在本步驟中,該鐵基軟磁粉體可包含鐵矽鋁軟磁粉體、鐵矽軟磁粉體或鐵矽鉻軟磁粉體。例如,該鐵基軟磁粉體的成分包含:9.6wt%至9.8wt%的矽;5.3wt%至6wt%的鋁;84.2wt%至85.0wt%的鐵以及不可避免的雜質。在一實施例中,該熔煉步驟係以一大氣熔煉法進行,亦即該熔煉步驟是在大氣環境中進行,而非特定氣體(如氮氣)的氣氛中進行。 Referring to FIG. 1 , a method 10 for manufacturing an iron-based soft magnetic powder according to an embodiment of the present invention is first performed by performing a melting step 11 to smelt a plurality of materials having a predetermined composition ratio to form a molten liquid, wherein The temperature of the melt is between 1519 degrees Celsius and 1588 degrees Celsius. In this step, the iron-based soft magnetic powder may comprise iron-iron-aluminum soft magnetic powder, iron-iron soft magnetic powder or iron-iron chromium soft magnetic powder. For example, the composition of the iron-based soft magnetic powder includes: 9.6 wt% to 9.8 wt% of rhodium; 5.3 wt% to 6 wt% of aluminum; 84.2 wt% to 85.0 wt% of iron and unavoidable impurities. In one embodiment, the smelting step is carried out in an atmospheric smelting process, that is, the smelting step is carried out in an atmosphere of an atmosphere other than a specific gas such as nitrogen.
本發明實施例之鐵基軟磁粉體的製造方法10接著 係:進行一水噴霧步驟12,其中該熔湯液從口徑為6毫米至8毫米的一流嘴流出,並通過呈雙V型水幕的一水霧冷卻該熔湯液,以製得一鐵基軟磁粉體;其中該鐵基軟磁粉體具有一氧含量在1820ppm至3000ppm之間、一導磁率大於等於125,及一磁損值在0至1000kw/m3之間;其中該水霧與該熔湯液的一重量比值是在3.84至9.17之間。要提到的是,對於該重量比值而言,該水霧的重量會依據水霧噴出的水壓計算,以及該熔湯液的重量會依據該流嘴的口徑計算。 The method 10 for manufacturing an iron-based soft magnetic powder according to an embodiment of the present invention is followed by: performing a water spray step 12, wherein the molten liquid flows out from a first-class nozzle having a diameter of 6 mm to 8 mm, and passes through a double V-shaped water curtain. Cooling the molten liquor to obtain an iron-based soft magnetic powder; wherein the iron-based soft magnetic powder has an oxygen content of between 1820 ppm and 3000 ppm, a magnetic permeability of greater than or equal to 125, and a magnetic loss value Between 0 and 1000 kW/m 3 ; wherein the weight ratio of the water mist to the molten liquor is between 3.84 and 9.17. It should be mentioned that for the weight ratio, the weight of the water mist is calculated based on the water pressure sprayed by the water mist, and the weight of the molten liquid is calculated according to the diameter of the nozzle.
續言之,請一併參照第1、2A及2B圖,第2A圖是本發明實施例之第一噴嘴組21及第二噴嘴組22的立體示意圖。第2B圖是本發明實施例之第一噴嘴組21及第二噴嘴組22的側視示意圖。該水噴霧步驟12可包含:以一第一噴嘴組21及一第二噴嘴組22提供呈雙V型水幕的該水霧23,其中該第一噴嘴組21包含相對設置的二第一水噴嘴211,且該水霧23從該些第一水噴嘴211中的每一個噴出至接觸該熔湯液24的一第一噴距L1是在160毫米至254毫米之間;及該第二噴嘴組22包含相對設置的二第二水噴嘴221,且該水霧從該些第二水噴嘴221中的每一個噴出至接觸該熔湯液24的一第二噴距L2是在160毫米至254毫米之間。在一具體實施例中,該雙V型水幕是通過將該第一噴嘴組21及該第二噴嘴組22交叉排列,且該些第一水噴嘴211及該些第二水噴嘴221係朝下進行一傾斜噴霧而形成。在另一實施例中,該第一噴距L1及該第二噴距L2是通過把該些第一水噴嘴211及該些第二水噴嘴221向下傾斜來調整。以該些第一水噴嘴211各傾斜角度α為例(以第2B圖為例,位在左側的第一水噴嘴211朝右下傾斜角度α,位在右側的第一水噴嘴211朝左下傾斜角度α),當該些第一水噴嘴211的傾斜角度α是17.5度時,該第一噴距L1是183毫米;當該些第一水噴嘴211的傾斜角度α是17.5度時,該第一噴距L1是254毫米;當該些第一水噴嘴211的傾斜角度α是20度時,該第一噴距L1是160毫米;及當該些第一水噴嘴211 的傾斜角度α是15度時,該第一噴距L1是212毫米。同理,該些第二水噴嘴221也可以通過類似於該些第一水噴嘴211的調整方式來調整該第二噴距L2。在又一實施例中,該雙V型水幕是一方錐型水幕。 In other words, please refer to Figures 1, 2A and 2B together. Figure 2A is a perspective view of the first nozzle group 21 and the second nozzle group 22 in the embodiment of the present invention. Fig. 2B is a side elevational view showing the first nozzle group 21 and the second nozzle group 22 in the embodiment of the present invention. The water spray step 12 may include: providing the water mist 23 in a double V-shaped water curtain with a first nozzle group 21 and a second nozzle group 22, wherein the first nozzle group 21 includes two first waters disposed opposite to each other. a nozzle 211, and the water mist 23 is ejected from each of the first water nozzles 211 to a first spray distance L1 contacting the molten liquid 24 between 160 mm and 254 mm; and the second nozzle The group 22 includes two second water nozzles 221 disposed opposite to each other, and the water mist is ejected from each of the second water nozzles 221 to a second spray distance L2 contacting the molten liquid 24 at 160 mm to 254. Between millimeters. In a specific embodiment, the double V-shaped water curtain is arranged by crossing the first nozzle group 21 and the second nozzle group 22, and the first water nozzle 211 and the second water nozzles 221 are facing It is formed by performing a tilting spray. In another embodiment, the first spray distance L1 and the second spray distance L2 are adjusted by tilting the first water nozzles 211 and the second water nozzles 221 downward. Taking the inclination angle α of each of the first water nozzles 211 as an example (taking the second water diagram 211 as an example, the first water nozzle 211 positioned on the left side is inclined downward by an angle α, and the first water nozzle 211 positioned on the right side is inclined downward to the left. The angle α), when the inclination angle α of the first water nozzles 211 is 17.5 degrees, the first spray distance L1 is 183 mm; when the inclination angle α of the first water nozzles 211 is 17.5 degrees, the first A spray distance L1 is 254 mm; when the inclination angle α of the first water nozzles 211 is 20 degrees, the first spray distance L1 is 160 mm; and when the first water nozzles 211 When the inclination angle α is 15 degrees, the first spray distance L1 is 212 mm. Similarly, the second water nozzles 221 can also adjust the second spray distance L2 by adjusting the first water nozzles 211. In still another embodiment, the double V-shaped water curtain is a one-sided water curtain.
在一實施例中,該水噴霧步驟12中的該流嘴的口徑為6毫米、及該水霧與該熔湯液的重量比值是在5.03至9.17之間,以製得該氧含量在1820ppm至2760ppm之間、該導磁率在125至130之間、及該磁損值在858kw/m3至983kw/m3之間的該鐵基軟磁粉體。在另一實施例中,該水霧之一水壓在300巴至350巴之間。 In one embodiment, the nozzle of the water spray step 12 has a diameter of 6 mm, and the weight ratio of the water mist to the molten liquor is between 5.03 and 9.17 to obtain the oxygen content at 1820 ppm. The iron-based soft magnetic powder is between 2760 ppm, the magnetic permeability is between 125 and 130, and the magnetic loss value is between 858 kw/m 3 and 983 kw/m 3 . In another embodiment, one of the water mists has a water pressure between 300 and 350 bar.
在一實施例中,該水噴霧步驟12中的該流嘴的口徑為8毫米、該熔湯液的溫度是在攝氏1521度至攝氏1547度之間、及該水霧與該熔湯液的重量比值是在3.84至4.74之間,以製得該氧含量在2350ppm至2720ppm之間、該導磁率在134至147之間、及該磁損值在934kw/m3至993kw/m3的該鐵基軟磁粉體。在另一實施例中,該水霧之一水壓在350巴至380巴之間。 In one embodiment, the nozzle of the water spray step 12 has a diameter of 8 mm, the temperature of the molten solution is between 1521 degrees Celsius and 1547 degrees Celsius, and the water mist and the molten fluid The weight ratio is between 3.84 and 4.74 to produce the oxygen content between 2350 ppm and 2720 ppm, the magnetic permeability is between 134 and 147, and the magnetic loss value is between 934 kw/m 3 and 993 kw/m 3 . Iron-based soft magnetic powder. In another embodiment, one of the water mists has a water pressure between 350 and 380 bar.
為證明本發明實施例之鐵基軟磁粉體的製造方法,可在大氣下使用水噴霧法,透過控制製程中的參數以得到一氧含量在1820ppm至3000ppm之間、一導磁率大於等於125,及一磁損值在0至1000kw/m3的鐵基軟磁粉體。特舉出下列多個比較例及實施例。 In order to prove the method for manufacturing the iron-based soft magnetic powder of the embodiment of the present invention, the water spray method can be used under the atmosphere to obtain an oxygen content between 1820 ppm and 3000 ppm and a magnetic permeability of 125 or more by controlling the parameters in the process. And an iron-based soft magnetic powder having a magnetic loss value of 0 to 1000 kW/m 3 . The following comparative examples and examples are given.
實施例1 Example 1
首先配製9wt%至10wt%的矽原料、5wt%至6wt%的鋁原料及其餘是鐵之原料,使用頻率為2000赫茲之高週波感應爐熔煉將這些原料在大氣環境下進行熔煉步驟以形成一熔湯液。熔湯液的溫度(後稱熔湯溫度;Tm)在攝氏1547度時,進行水噴霧步驟,其中該熔湯液從流嘴口徑(MOD)為8毫米之流嘴(例如該熔湯液通過氧化鋁管的流嘴)流出,並在周圍充入氮氣保護。之後,流入雙V型水幕之中,以使呈雙V型水幕的一水霧冷卻該熔湯液,進而製得實施例1的鐵基軟磁粉體。雙V型水幕是通過交叉排列 的第一噴嘴組及第二噴嘴組朝下進行一傾斜噴霧,其中第一噴嘴組的第一噴距(L1)是183毫米及第二噴嘴組的第二噴距(L2)是254毫米。另外,該水霧的水壓(P)是350巴,及該水霧與該熔湯液的重量比值(Mw/Mm)是3.84。所得之實施例1的鐵基軟磁粉體的組成是:9.71wt%的矽、5.8wt%的鋁、氧含量([O])為2720ppm、雜質(包含錳、磷、鎳、鉻、銅、碳、硫及氮等)約為780ppm以及剩餘的成分是鐵。之後,對實施例1的鐵基軟磁粉體進行一篩選步驟,以分得中位粒徑(D50)為73.9微米的鐵基軟磁粉體,利用水玻璃絕緣披覆,並以硬酸脂酸鈣作潤滑劑,以15MT/cm2的壓力(X)壓製該鐵基軟磁粉體以得到一環型磁粉芯,該環型磁粉芯於氮氣中以攝氏760度進行退火30分,可得到導磁率(μe)為138、磁損Pcv為979kW/m3的該環型磁粉芯。 First, 9wt% to 10wt% of bismuth raw materials, 5wt% to 6% by weight of aluminum raw materials and the rest of the raw materials of iron are prepared, and the raw materials are smelted in a high-frequency induction furnace with a frequency of 2000 Hz to form a smelting step in an atmosphere to form a Melt solution. The temperature of the molten liquor (hereinafter referred to as the melt temperature; Tm) is subjected to a water spray step at a temperature of 1547 degrees Celsius, wherein the melt liquid is from a nozzle having a nozzle diameter (MOD) of 8 mm (for example, the melt liquid passes through) The nozzle of the alumina tube flows out and is filled with nitrogen gas protection. Thereafter, the mixture was poured into a double V-shaped water curtain to cool the molten liquid by a water mist having a double V-shaped water curtain, thereby producing the iron-based soft magnetic powder of Example 1. The double V-shaped water curtain performs a tilting spray downward through the first nozzle group and the second nozzle group which are arranged in a cross direction, wherein the first spray distance (L1) of the first nozzle group is 183 mm and the second nozzle group is second The spray distance (L2) is 254 mm. Further, the water pressure (P) of the water mist was 350 bar, and the weight ratio (Mw/Mm) of the water mist to the molten liquid was 3.84. The composition of the obtained iron-based soft magnetic powder of Example 1 was: 9.71 wt% of bismuth, 5.8 wt% of aluminum, an oxygen content ([O]) of 2720 ppm, impurities (including manganese, phosphorus, nickel, chromium, copper, Carbon, sulfur, nitrogen, etc.) is about 780 ppm and the remaining component is iron. Thereafter, the iron-based soft magnetic powder of Example 1 was subjected to a screening step to obtain an iron-based soft magnetic powder having a median diameter (D 50 ) of 73.9 μm, coated with water glass insulation, and hard acid ester. Calcium acid is used as a lubricant, and the iron-based soft magnetic powder is pressed at a pressure (X) of 15MT/cm 2 to obtain a ring-shaped magnetic powder core which is annealed at 760 degrees Celsius in nitrogen for 30 minutes. The ring-shaped magnetic powder core having a magnetic ratio (μ e ) of 138 and a magnetic loss P cv of 979 kW/m 3 was used.
實施例2~9及比較例1~8 Examples 2 to 9 and Comparative Examples 1 to 8
實施例2~9及比較例1~8的製造方式類似於實施例1,惟其不同點在於製程參數以及所得之鐵基軟磁粉體的組成、中位粒徑、及所得之環型磁粉芯之特性不同,請參照下表1及2所示。 The manufacturing methods of Examples 2 to 9 and Comparative Examples 1 to 8 were similar to those of Example 1, except that the process parameters and the composition of the obtained iron-based soft magnetic powder, the median diameter, and the obtained ring-shaped magnetic powder core were The characteristics are different, please refer to Tables 1 and 2 below.
關於環型磁粉芯之特性的評價方式,可以例如通過IWATSU公司生產的B-H磁性分析儀(型號為SY8232)來量測環型磁粉芯在頻率100千赫茲及磁場在0.1特斯拉下的磁損值(Pcv),並以安捷倫(Agilent)公司生產的阻抗測試儀(型號為LCRZ 42841A/4284A Meter)量測環型磁粉芯的電感,並由幾何尺寸和繞線圈數所對應之磁路計算等效導磁率(μe)。 Regarding the evaluation method of the characteristics of the toroidal magnetic powder core, the magnetic loss of the toroidal magnetic powder core at a frequency of 100 kHz and a magnetic field of 0.1 Tesla can be measured, for example, by a BH magnetic analyzer (model SY8232) manufactured by IWATSU. The value (P cv ), and the inductance of the toroidal powder core is measured by an Agilent impedance tester (model LCRZ 42841A/4284A Meter), and calculated by the geometrical path and the magnetic circuit corresponding to the number of coils. Equivalent permeability (μ e ).
關於比較例1,水霧/熔湯液的重量比值(Mw/Mm)較 小(僅為2.6),則使得雙V型水幕中,水蒸氣壓較小而無法液化冷凝為水。再加上熔湯溫度愈高,水蒸氣易分解為氧並與熔湯液滴起氧化反應,致使氧含量高達6590ppm,顆粒內氧化介在物如氧化鋁增多而導致磁滯損大,且氧化介在物會影響磁域移動,導致導磁率較低。 Regarding Comparative Example 1, the weight ratio (Mw/Mm) of the water mist/melting solution was compared. Small (only 2.6), the double V-shaped water curtain, the water vapor pressure is small and can not be liquefied and condensed into water. In addition, the higher the temperature of the molten soup, the water vapor is easily decomposed into oxygen and oxidized with the molten liquid droplets, resulting in an oxygen content of up to 6590 ppm. The oxidation of the particles in the particles, such as alumina, leads to a large magnetic hysteresis loss, and the oxidation is interposed. The object will affect the magnetic domain movement, resulting in a lower magnetic permeability.
關於比較例2,熔湯溫度不高僅1530℃,且Mw/Mm較大(達5.75),在方錐形水幕中之水蒸氣壓大分解為氧之量少,但因使用熔湯口徑較大,流嘴口徑MOD為10毫米,大面積之熔湯被高壓水霧刺穿,使得溶湯液滴的孔洞(Voids)增多,進而使得氧化作用面積增多,粉末顆粒含氧量增多。此外,孔洞內之水殘留時間較長,不易乾燥且易引發生鏽。關於比較例3,雖然磁損較低,但仍無法滿足磁損值低於1000kW/m3的要求。 Regarding Comparative Example 2, the melt temperature was not as high as 1530 ° C, and Mw / Mm was large (to 5.75), and the water vapor pressure in the square conical water curtain was greatly decomposed into a small amount of oxygen, but the use of the melt caliber Larger, the nozzle diameter MOD is 10 mm, and the large-area melt is pierced by the high-pressure water mist, which increases the number of voids (Voids) of the dissolved soup droplets, thereby increasing the oxidation area and increasing the oxygen content of the powder particles. In addition, the water in the hole has a long residual time, is not easy to dry and is prone to rust. Regarding Comparative Example 3, although the magnetic loss was low, the requirement that the magnetic loss value was less than 1000 kW/m 3 could not be satisfied.
比較例4之熔湯溫度高於比較例2和3,且Mw/Mm較小,但[O]相對較低,此與第一噴距L1、第二噴距L2分別為183、254毫米,相對於比較例2和3之160、212毫米長有關。另外,熔湯液先在充氮之環境中行進,故與水霧接觸前所花費的時間較久,且溫度降低幅度較大,故氧化溫度較低,這也是造成[O]相對較低的原因之一。再者,第一噴距L1、第二噴距L2較長,液滴動能減少,加上水壓較低,刺穿熔湯衝力小,故產生較少空洞,所以也造成[O]相對較低的原因之一。關於比較例5,雖然磁損較低,但仍無法滿足磁損值低於1000kW/m3的要求。 The melt temperature of Comparative Example 4 was higher than that of Comparative Examples 2 and 3, and Mw/Mm was small, but [O] was relatively low, which was 183, 254 mm with the first spray distance L1 and the second spray distance L2, respectively. It is related to 160, 212 mm long of Comparative Examples 2 and 3. In addition, the molten broth first travels in a nitrogen-filled environment, so it takes a long time before contact with the water mist, and the temperature decreases a lot, so the oxidation temperature is low, which also causes [O] to be relatively low. one of the reasons. Furthermore, the first spray distance L1 and the second spray distance L2 are longer, the kinetic energy of the droplet is reduced, and the water pressure is lower, and the impulse of the piercing melt is small, so that less voids are generated, so that [O] is relatively relatively One of the reasons for the low. Regarding Comparative Example 5, although the magnetic loss was low, the requirement that the magnetic loss value was less than 1000 kW/m 3 could not be satisfied.
比較例6~8使用的流嘴口徑(MOD)為8毫米。當熔湯溫度Tm為1543~1578℃、噴水對熔湯流量比Mw/Mm為3.5~5.08下,所得粉末含氧量[O]為3630~4210ppm,[O]仍高於3000ppm。比較例6和8之磁損皆高於1000kW/m3,比較例7之磁損為922kW/m3、雖小於1000kW/m3,但導磁率僅為110。比較例7使用較大之水壓(450巴),水霧刺穿熔湯液滴,使得磁粉空洞數量增多,導致內部反向磁場多,導磁率偏低。 The nozzle diameter (MOD) used in Comparative Examples 6 to 8 was 8 mm. When the melting temperature Tm is 1543~1578 °C, and the spray water to melt flow ratio Mw/Mm is 3.5~5.08, the oxygen content [O] of the obtained powder is 3630~4210ppm, and [O] is still higher than 3000ppm. The magnetic losses of Comparative Examples 6 and 8 were all higher than 1000 kW/m 3 , and the magnetic loss of Comparative Example 7 was 922 kW/m 3 , although it was less than 1000 kW/m 3 , but the magnetic permeability was only 110. In Comparative Example 7, a large water pressure (450 bar) was used, and the water mist pierced the molten liquid droplets, so that the number of magnetic powder voids increased, resulting in a large internal reverse magnetic field and a low magnetic permeability.
實施例1~3及比較例6~8皆使用MOD為8毫米之流 嘴,在熔湯溫度Tm為1521~1547℃,以及噴水對熔湯流量比Mw/Mm為3.84~4.74下,所得粉末含氧量[O]為2350~2720ppm,磁粉芯之導磁率為138~147、磁損為934~993kW/m3,皆小於1000kW/m3。實施例1及2使用較長之第一噴距L1及第二噴距L2,分別為183、254mm,所以和比較例8使用較短之噴距,在Mw/Mm皆約為4.74下,實施例1及2可得較低之含氧量。 In Examples 1 to 3 and Comparative Examples 6 to 8, a nozzle having a MOD of 8 mm was used, and the obtained powder was obtained at a melt temperature Tm of 1521 to 1547 ° C and a water spray to melt flow ratio Mw/Mm of 3.84 to 4.74. oxygen content [O] is 2350 ~ 2720ppm, magnetic permeability of the magnetic cores 138 to 147, the magnetic loss of 934 ~ 993kW / m 3, are all smaller than 1000kW / m 3. In the first and second embodiments, the first first spray distance L1 and the second spray distance L2 are 183 and 254 mm, respectively, so that a shorter spray distance is used with Comparative Example 8, and the Mw/Mm is about 4.74. Examples 1 and 2 gave lower oxygen content.
實施例4~9使用MOD為6毫米的流嘴,在熔湯溫度Tm為1519~1588℃,以及噴水對熔湯流量比Mw/Mm為5.03~9.17下,所得粉末含氧量[O]為1820~2760ppm,磁粉芯之導磁率為125~130、磁損為858~983kW/m3,導磁率可大於等於125、磁損皆小於等於1000kW/m3。使用MOD為6毫米之流出熔湯,因熔湯流出速度慢,Mw/Mm易大於等於5。由於水蒸氣壓大,在雙V形水幕中水蒸氣容易液化,故氧化較少。另一方面,熔湯面對水霧的液滴面積較少、穿孔機會較少、氧化作用面積較少、故粉末顆粒孔洞較少、殘留水較少、生鏽較少。值得一提的是,實施例4~9的熔湯液滴容易被細化,故水噴粉末相對較細。 In Examples 4 to 9, a nozzle having a MOD of 6 mm was used, and the oxygen content [O] of the obtained powder was at a melt temperature Tm of 1519 to 1588 ° C and a spray flow ratio of Mw/Mm of 5.03 to 9.17. 1820~2760ppm, the magnetic permeability of the magnetic powder core is 125~130, the magnetic loss is 858~983kW/m 3 , the magnetic permeability can be greater than or equal to 125, and the magnetic loss is less than or equal to 1000kW/m 3 . Use MOD is 6 mm outflow melt, because the melt outflow rate is slow, Mw/Mm is easy to be greater than or equal to 5. Since the water vapor pressure is large, water vapor is easily liquefied in the double V-shaped water curtain, so oxidation is less. On the other hand, the molten soup has a smaller droplet area facing the water mist, less perforation opportunities, and less oxidation area, so the powder particles have fewer pores, less residual water, and less rust. It is worth mentioning that the melt droplets of Examples 4 to 9 are easily refined, so that the water spray powder is relatively fine.
綜上所述,本發明實施例之鐵基軟磁粉體的製造方法,可在大氣下使用水噴霧法,透過控制製程中的參數以得到一氧含量在1820ppm至3000ppm之間、一導磁率大於等於125,及一磁損值在0至1000kw/m3的鐵基軟磁粉體。 In summary, the method for manufacturing the iron-based soft magnetic powder according to the embodiment of the present invention can use a water spray method under the atmosphere to obtain an oxygen content between 1820 ppm and 3000 ppm and a magnetic permeability greater than that by controlling the parameters in the process. Is equal to 125, and an iron-based soft magnetic powder having a magnetic loss value of 0 to 1000 kW/m 3 .
雖然本發明已以較佳實施例揭露,然其並非用以限制本發明,任何熟習此項技藝之人士,在不脫離本發明之精神和範圍內,當可作各種更動與修飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。 The present invention has been disclosed in its preferred embodiments, and is not intended to limit the invention, and the present invention may be modified and modified without departing from the spirit and scope of the invention. The scope of protection is subject to the definition of the scope of the patent application.
10‧‧‧方法 10‧‧‧ method
11‧‧‧步驟 11‧‧‧Steps
12‧‧‧步驟 12‧‧‧ steps
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