TWI526544B - Preparation of High Density Powder Metallurgy Metal Soft Magnetic Materials - Google Patents

Preparation of High Density Powder Metallurgy Metal Soft Magnetic Materials Download PDF

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TWI526544B
TWI526544B TW103118040A TW103118040A TWI526544B TW I526544 B TWI526544 B TW I526544B TW 103118040 A TW103118040 A TW 103118040A TW 103118040 A TW103118040 A TW 103118040A TW I526544 B TWI526544 B TW I526544B
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powder
soft magnetic
iron
magnetic material
metal soft
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TW201544606A (en
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Kuen Shyang Hwang
yang liang Fan
Wei Chen Tseng
Yung Chung Lu
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Taiwan Powder Technologies Co Ltd
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高密度粉末冶金金屬軟磁材料的製備方法Method for preparing high-density powder metallurgy metal soft magnetic material

本發明係有關一種金屬軟磁材料的製備方法,尤指一種利用乾壓、燒結成形技術之高密度粉末冶金金屬軟磁材料的製備方法。The invention relates to a preparation method of a metal soft magnetic material, in particular to a preparation method of a high-density powder metallurgy metal soft magnetic material using dry pressing and sintering forming technology.

由於金屬軟磁材料高感應磁束密度(Induced magnetism,簡稱BS )以及低矯頑磁力(Coercive force,簡稱HC )的特性,使其大量被應用於電子、電磁相關產業之中。其在工業中的應用最早始於19世紀末。隨著電力工業及電訊技術的興起,開始使用低碳鋼製造電機機械和變壓器,在電話線路中的電感線圈的磁芯中使用了細小的鐵粉、氧化鐵、細鐵絲等。到20世紀初,研製出了矽鋼片代替低碳鋼,提高了變壓器的效率,降低了損耗。直至現在矽鋼片在電力工業用金屬軟磁材料中仍居首位。 常見的金屬軟磁材料製備方法之一為傳統的乾壓燒結法(Press-and-sinter process),其係先將具有所需成分之合金粉末與潤滑劑混合均勻後,將之填充至模具之中,接著在常溫施以所需之壓力令粉末成形,成為具有一定強度的胚體,後續將胚體加熱去除潤滑劑後最後經過高溫燒結,即可得到所要之金屬軟磁材料;由於以上製程皆可自動化完成,因此具有原料便宜、模具費用低、製程簡單等優點。 一般來說,在傳統乾壓燒結製程中,為了使金屬軟磁材料達到優良的機械或物理性質,燒結後金屬軟磁材料的密度應越高越好,此也代表燒結前的胚體(又稱生胚)密度應越高越好。此外,高生胚密度的胚體在經過燒結後,其尺寸收縮量將較低生胚密度的胚體少,因此高生胚密度的工件其尺寸穩定性較佳。 一般要得到高密度的生胚除了成形時的壓力必須夠大以外,粉末本身之特性也具有關鍵性,粉末本身之形狀、大小及內部結構等均對粉末成形能力有直接之影響,而由於小粒徑之粉末的表面積大,燒結驅動力高,因此可在燒結後得到高密度的軟磁材料,但利用小粒徑之粉末進行乾壓燒結製程時,由於其粉末間的接觸點較多、摩擦力較大、壓縮性(Compressibility,代表壓縮至高密度之能力)差,且成形性(Compactibility,代表粉末間之結合力)不佳,因此必需倚靠較高之成形壓力,才能達到所要之胚體密度,但過大壓力卻又容易造成胚體離開模具時產生之回彈(Spring back)量加大,而產生分層(Delamination)現象;再者,過大的成形壓力會造成模具快速損耗,且為提供較高的成形壓力,其所需之機具、價格亦較高。另外,小粒徑之粉末因流動性不佳,無法以自動化之方式將粉末充填入模穴,更進一步造成製造成本的增加。 另一方面,如使用大粒徑之粉末,則尚有其他問題的產生。以現有技術來說,若製作Fe-0.45P(即磷的重量百分比為0.45 wt.%,其餘為鐵和不可避免的雜質)之軟磁材料,係使用粒徑較大的鐵粉混合粒徑較小之磷化三鐵(Fe3 P)粉,前者之平均粒徑約70µm,後者之平均粒徑約為5µm。此種混合粉末之流動性佳且具有良好的視密度,故適合採用上述之傳統乾壓燒結法,其生胚密度約在6.4 g/ cm3 至 7.1 g/cm3 之間,依據美國金屬粉末工業聯盟(Metal Powder Industry Federation,簡稱MPIF) 標準35(MPIF Standard 35)之記載,此生胚經燒結後之密度僅在6.8 g/ cm3 至 7.4 g/ cm3 之間。由此可見,上述之傳統乾壓燒結製程並無法達到高燒結密度,原因即為粉末之粒徑過大。 除傳統乾壓燒結法外,習知技術中,亦有採用金屬粉末射出成形製程(Metal Injection Molding,簡稱MIM)者,由於此種製程並無涉及乾壓,而是利用射出的方式成形生胚,故可採用細的金屬顆粒。也因此,粉末之流動性與視密度對燒結密度的影響不大。舉例而言,若是製備Fe-3Si軟磁材料,一般係使用粒徑較小之鐵粉及Fe-Si預合金粉,此混合粉與約30 vol.%至40 vol.%之黏結劑混練後再以射出成形機射出生胚,生胚密度約為4.5 g/ cm3 至 5.5 g/ cm3 之間,經脫脂步驟將黏結劑去除後,剩下之金屬胚體以高溫燒結即可得到高密度工件。依據MPIF Standard 35之記載,燒結後密度約為7.5 g/ cm3 ,且具有良好的磁特性。雖採用MIM製程,可得到符合需求的軟磁材料,且無論是燒結密度、磁特性均優於傳統乾壓燒結法,但MIM製程所需的成本,約為乾壓燒結法的10倍。除了成本問題外,MIM製程尚有尺寸不易控制的問題,具體而言,因MIM生胚密度低而燒結密度高,其燒結後的線收縮(linear shrinkage)量大,通常高於12%,因此不易控制工件的尺寸。 綜上,習知技術所採用之傳統乾壓燒結法,係無法達到高燒結密度,且所得到之軟磁材料,其磁性不佳;又習知技術所採用的MIM製程,則具有高成本以及尺寸控制不易之問題。Due to the high inductive magnetism (B S ) and low coercive force (H C ) properties of metal soft magnetic materials, it has been widely used in electronics and electromagnetic related industries. Its application in industry began in the late 19th century. With the rise of the power industry and telecommunications technology, low-carbon steels have been used to manufacture motor machinery and transformers, and fine iron powder, iron oxide, and fine iron wire have been used in the core of the inductor coil in the telephone line. By the beginning of the 20th century, a silicon steel sheet was developed instead of low carbon steel, which improved the efficiency of the transformer and reduced the loss. Until now, the silicon steel sheet still ranks first in the metal soft magnetic materials for the power industry. One of the common methods for preparing metal soft magnetic materials is the conventional press-and-sinter process, which firstly mixes the alloy powder with the desired composition and the lubricant, and then fills it into the mold. Then, applying the required pressure at normal temperature to form the powder into a body body having a certain strength, and then heating the body body to remove the lubricant and finally sintering at a high temperature, thereby obtaining the desired metal soft magnetic material; Automated completion, so it has the advantages of cheap raw materials, low mold cost, and simple process. Generally speaking, in the conventional dry pressing sintering process, in order to achieve excellent mechanical or physical properties of the metal soft magnetic material, the density of the soft magnetic material of the metal after sintering should be as high as possible, which also represents the embryo body before sintering (also referred to as raw The higher the density of the embryo should be. In addition, the embryo body with high embryo density has less embryo shrinkage after firing, and the height of the embryo density is better. Generally, it is necessary to obtain a high-density green embryo. In addition to the pressure at the time of forming, the characteristics of the powder itself are also critical. The shape, size and internal structure of the powder itself have a direct influence on the powder forming ability, and The powder of the particle size has a large surface area and a high driving force for sintering, so that a high-density soft magnetic material can be obtained after sintering, but when a dry-sintering process is performed using a powder having a small particle diameter, since the contact points between the powders are large, friction The force is large, the compressibility (compressibility, representing the ability to compress to high density) is poor, and the compactness (representing the bonding force between the powders) is not good, so it is necessary to rely on the higher forming pressure to achieve the desired embryo density. However, if the pressure is too high, it will easily cause the spring back to increase when the embryo body leaves the mold, and the delamination phenomenon will occur. Moreover, the excessive forming pressure will cause the mold to be quickly depleted and provided. The higher forming pressure, the higher the required equipment and price. In addition, the small particle size powder cannot be filled into the cavity by an automated method due to poor fluidity, which further increases the manufacturing cost. On the other hand, if a powder having a large particle size is used, there are still other problems. In the prior art, if a soft magnetic material of Fe-0.45P (that is, the weight percentage of phosphorus is 0.45 wt.%, and the balance is iron and unavoidable impurities) is used, the mixed particle diameter of the iron powder having a larger particle diameter is used. Small phosphating triiron (Fe 3 P) powder having an average particle diameter of about 70 μm and an average particle diameter of the latter of about 5 μm. The mixed powder has good fluidity and good apparent density, so it is suitable to adopt the above-mentioned conventional dry pressing sintering method, and the green density is about 6.4 g/cm 3 to 7.1 g/cm 3 , according to the American metal powder. According to the Metal Powder Industry Federation (MPIF) Standard 35 (MPIF Standard 35), the density of this green embryo after sintering is only between 6.8 g/cm 3 and 7.4 g/cm 3 . It can be seen that the above conventional dry pressing sintering process cannot achieve a high sintered density because the particle size of the powder is too large. In addition to the conventional dry-pressure sintering method, in the prior art, a metal injection molding process (MIM) is also used. Since the process does not involve dry pressing, the injection process is used to form the green embryo. Therefore, fine metal particles can be used. Therefore, the fluidity and apparent density of the powder have little effect on the sintered density. For example, if a Fe-3Si soft magnetic material is prepared, generally, a small particle size iron powder and a Fe-Si prealloy powder are used, and the mixed powder is mixed with about 30 vol.% to 40 vol.% of the binder. The embryo is shot by an injection molding machine, and the density of the raw embryo is between 4.5 g/cm 3 and 5.5 g/cm 3 . After the binder is removed by the degreasing step, the remaining metal body is sintered at a high temperature to obtain a high density. Workpiece. According to MPIF Standard 35, the density after sintering is about 7.5 g/cm 3 and has good magnetic properties. Although the MIM process is used, soft magnetic materials can be obtained according to requirements, and both the sintered density and the magnetic properties are superior to the conventional dry-pressure sintering method, but the cost required for the MIM process is about 10 times that of the dry-pressure sintering method. In addition to the cost problem, the MIM process has problems in that the size is not easy to control. Specifically, since the MIM has a low density of embryos and a high sintered density, the amount of linear shrinkage after sintering is large, usually higher than 12%. It is difficult to control the size of the workpiece. In summary, the conventional dry-pressure sintering method adopted by the prior art cannot achieve high sintering density, and the obtained soft magnetic material has poor magnetic properties; and the MIM process adopted by the prior art has high cost and size. Control difficult problems.

本發明之主要目的,在於解決習知利用傳統乾壓成形技術之金屬軟磁材料的密度不高、磁性質不佳等問題,以及習知利用MIM製程之成本過高和燒結後尺寸難以掌握之問題。 為達上述目的,本發明提供一種高密度粉末冶金金屬軟磁材料的製備方法,其包含以下步驟: S1:提供一含鐵且具金屬軟磁性質的起始粉末,該起始粉末平均粒徑介於1微米至15微米之間,且鐵的來源為一羰基鐵粉; S2:利用一噴霧造粒製程自該起始粉末取得一噴霧造粒粉末,該噴霧造粒粉末具有一接近球形之粉末形貌且平均粒徑介於40微米至100微米之間; S3:將該噴霧造粒粉末置入一模具中,並令該噴霧造粒粉末維持在一介於20℃至150℃之成形溫度下接受一介於300MPa至1000MPa之間的成形壓力而形成一胚體;以及 S4:將該胚體加熱至1100℃至1400℃之間並於一保護氣氛中予以燒結而得到一金屬軟磁材料。 為達上述目的,本發明另提供一種高密度粉末冶金金屬軟磁材料的製備方法,其包含以下步驟: S1:提供一含鐵且具金屬軟磁性質的起始粉末,該起始粉末平均粒徑介於1微米至15微米之間,且該起始粉末為一預合金粉; S2:利用一噴霧造粒製程自該起始粉末取得一噴霧造粒粉末,該噴霧造粒粉末具有一接近球形之粉末形貌且平均粒徑介於40微米至100微米之間; S3:將該噴霧造粒粉末置入一模具中,並令該噴霧造粒粉末維持在一介於20℃至150℃之間的成形溫度下接受一介於300MPa至1000MPa之間的成形壓力而形成一胚體;以及 S4:將該胚體加熱至1100℃至1400℃之間並於一保護氣氛中予以燒結而得到一金屬軟磁材料。 本發明利用該噴霧造粒製程得到的該噴霧造粒粉末,由於呈球狀,係具有優異的流動性、成形性與壓縮性,相較於未噴霧造粒之粉末可使用乾壓燒結製程且令該胚體具有高生胚密度,如此一來,最終燒結得到之該金屬軟磁材料,無論是相對密度或磁性質,均有較一般使用粗粉及傳統乾壓、燒結製程者更為優異的表現;同時,因該製備方法採用乾壓成形技術,與金屬粉末射出成形相較之下又具有低製造成本之優點,同時因生胚密度比MIM製程取得的生胚密度高,故亦可避免收縮量過大、尺寸不易控制之問題。The main object of the present invention is to solve the problems of low density and poor magnetic properties of conventional metal soft magnetic materials using conventional dry press forming technology, and the problem that the cost of using the MIM process is too high and the size after sintering is difficult to grasp. . In order to achieve the above object, the present invention provides a method for preparing a high-density powder metallurgy metal soft magnetic material, which comprises the following steps: S1: providing an iron-containing and metal soft magnetic starting powder, the average particle size of the starting powder is Between 1 micrometer and 15 micrometers, and the source of iron is a carbonyl iron powder; S2: a spray granulation powder is obtained from the starting powder by a spray granulation process, the spray granulated powder has a powder shape close to a spherical shape Appearance and average particle size between 40 microns and 100 microns; S3: placing the spray granulated powder in a mold and maintaining the spray granulated powder at a forming temperature of between 20 ° C and 150 ° C Forming a body with a forming pressure of between 300 MPa and 1000 MPa; and S4: heating the body to between 1100 ° C and 1400 ° C and sintering in a protective atmosphere to obtain a metal soft magnetic material. In order to achieve the above object, the present invention further provides a method for preparing a high-density powder metallurgy metal soft magnetic material, comprising the following steps: S1: providing an iron-containing and metal soft magnetic starting powder, the average particle size of the starting powder Between 1 micrometer and 15 micrometers, and the starting powder is a pre-alloyed powder; S2: obtaining a spray granulated powder from the starting powder by a spray granulation process, the spray granulated powder having a nearly spherical shape The powder has a morphology and an average particle diameter of between 40 μm and 100 μm; S3: placing the spray granulated powder in a mold and maintaining the spray granulated powder at a temperature between 20 ° C and 150 ° C Forming a forming pressure between 300 MPa and 1000 MPa to form an embryo body; and S4: heating the body to between 1100 ° C and 1400 ° C and sintering in a protective atmosphere to obtain a metal soft magnetic material . The spray granulated powder obtained by the spray granulation process of the present invention has excellent fluidity, formability and compressibility because it is spherical, and a dry pressing sintering process can be used compared to the powder which is not spray granulated. The embryo body has a high green embryo density, so that the metal soft magnetic material obtained by the final sintering, whether it is a relative density or a magnetic property, is superior to the general coarse powder and the conventional dry pressing and sintering process. At the same time, because the preparation method adopts dry pressing forming technology, it has the advantages of low manufacturing cost compared with the metal powder injection molding, and at the same time, the density of the raw embryo is higher than that of the MIM process, so shrinkage can be avoided. The problem is too large and the size is not easy to control.

有關本發明之詳細說明及技術內容,現就配合圖示說明如下: 請參閱『圖1』所示,『圖1』為本發明之步驟流程示意圖,步驟S1先提供一含鐵且具金屬軟磁性質的起始粉末,該起始粉末之平均粒徑較佳地小於15微米(µm)。於本發明之一實施例中,該起始粉末之鐵的主要來源為一羰基鐵粉,而該羰基鐵粉的碳含量可小於0.05 wt.%;於本發明之另一實施例中,該起始粉末可為元素粉、化合物粉、母合金粉或其混合粉。此外,該起始粉末之成分可包括鐵與至少一添加元素,該添加元素選自於磷、矽、鈷、釩、鎳、鉬及其組合所組成之群組。舉例而言,該起始粉末可為鐵磷混合粉末(Fe-P)、鐵矽混合粉末(Fe-Si)、鐵鈷混合粉末(Fe-Co)、鐵鈷釩混合粉末(Fe-Co-V)、鐵鎳混合粉末(Fe-Ni)或鐵鎳鉬混合粉末(Fe-Ni-Mo)等具軟磁性之金屬粉末或具上述成分之合金粉末。 於本發明之其他實施例中,該起始粉末之磷的重量百分比可介於0.4 wt.%至0.9 wt.%之間,其餘為鐵及不可避免之雜質;或者該起始粉末之矽的重量百分比可介於2 wt.%至6 wt.%之間,其餘為鐵及不可避免之雜質;或者該起始粉末之鈷的重量百分比可介於48 wt.%至52 wt.%之間,釩的重量百分比低於3 wt.%,其餘為鐵及不可避免之雜質;或者該起始粉末之鎳的重量百分比可介於48 wt.%至52 wt.%之間,其餘為鐵及不可避免之雜質;或者該起始粉末之鎳的重量百分比可介於77 wt.%至83 wt.%之間,鉬的重量百分比可低於5 wt.%,其餘為鐵及不可避免之雜質。 步驟S2係對該起始粉末進行一噴霧造粒製程,自該起始粉末取得一噴霧造粒粉末,該噴霧造粒粉末具有一接近球形之粉末形貌且平均粒徑介於40微米至100微米之間。於本實施例中,步驟S2中係對該起始粉末添加一黏結劑和水而混合形成一混合物,該黏結劑可為阿拉伯膠、甲基纖維素、聚乙烯醇、聚乙二醇或其混合物。經該噴霧造粒製程後,該噴霧造粒粉末可具有介於40微米至100微米之間的平均粒徑,且粉末形貌接近球形,此將有利於改善粉末之流動性、壓縮性、視密度與成形性。 步驟S3係將該噴霧造粒粉末置入一模具中,並令該噴霧造粒粉末維持在一成形溫度下並接受一成形壓力而形成一胚體。於本實施例中,該成形溫度介於20℃至150℃之間,該成形壓力介於300 MPa至1000 MPa之間,並可視需求於該噴霧造粒粉末先添加一潤滑劑,該潤滑劑可為白蠟、硬脂酸或硬脂酸鋅或其他潤滑劑,再將該噴霧造粒粉末置入該模具中。一般而言,該模具包含中模、上沖以及下沖,該上沖以及該下沖之間係形成一容置該噴霧造粒粉末之模穴空間,而於本實施例中,係可透過對該模具之該中模、該上沖或該下沖進行加熱,而利用該模具之熱傳導使該噴霧造粒粉末維持在20℃至150℃之間;或者,亦可對容納該噴霧造粒粉的餵粉盒(feedshoe)及輸送該噴霧造粒粉之輸送管以電熱或油熱方式加熱該噴霧造粒粉末,使該噴霧造粒粉末維持在20℃至150℃之間。 步驟S4係先進行一脫脂步驟,將該胚體加熱至一脫脂溫度,以去除該潤滑劑或該黏結劑,或採用其他化學方法脫脂,完成後再升溫至一燒結溫度而得到一金屬軟磁材料。於本實施例中,步驟S4可於一真空爐或一氣氛爐進行,如採用該氣氛爐,則應通入一還原氣氛,該還原氣氛含有氫氣或裂解氨,該燒結溫度為1100℃至1400℃之間。此外,經過步驟S4所得到之該金屬軟磁材料,其相對密度係高於94 %。 為進一步具體說明本發明高密度粉末冶金金屬軟磁材料的製備方法之內容,請續參閱下述依據本發明進行之實施例以及採用其他技術進行之比較例:實施例 1 本實施例之起始粉末為一鐵鈷混合粉末(Fe-50Co),係選用羰基鐵粉與鈷粉兩種元素粉之混合,鈷佔50 wt.%,其餘為鐵,且羰基鐵粉中的碳含量小於0.05 wt.%,其與鈷粉之平均粒徑皆小於10 µm,由於粉末太細,其流動性及視密度均無法以MPIF之標準測試法量測。在進行噴霧造粒製程前,該鐵鈷混合粉末(Fe-50Co)先與一黏結劑與水均勻混合,該黏結劑為聚乙烯醇及聚乙二醇,且添加量占金屬粉之1.0 wt.%,經過噴霧造粒製程所得到之一噴霧造粒粉末的平均粒徑為75 µm,且形貌接近球形,因此,此造粒粉已具流動性,以MPIF Standard 03標準測試法所測得之流動性為30 sec/50g,MPIF Standard 04標準測試法所測得之視密度為2.1 g/ cm3 。之後,先將該噴霧造粒粉末與一潤滑劑混合,該潤滑劑為白臘,添加量為0.1 wt.%,再將該噴霧造粒粉末置於一模具中,令該噴霧造粒粉末維持在35℃,並以600 MPa之成形壓力對該噴霧造粒粉末施壓而形成一胚體,胚體密度為6.2 g/cm³。接下來,將該胚體置於氣氛爐中,並通入含有75 vol.%氫氣及25 vol.%氮氣之裂解氨還原氣氛,先持溫於300℃至600℃之間以除去該黏結劑與該潤滑劑後,於1355℃的溫度下燒結2小時,而得到一Fe-50Co金屬軟磁材料,該Fe-50Co金屬軟磁材料之密度為7.89 g/cm³,相對密度為94.2 %,碳含量小於0.01 wt.%,感應磁束密度BS 為2.17 T (Tesla),矯頑磁力HC 為 89 A/m,最大導磁率μmax 為6790。由此製程所得Fe-50Co軟磁之密度及磁性質均比MPIF Standard 35 for Metal Injection Molded Parts中由金屬射出成形製程所製得之工件佳且生產成本也較低。比較例 1 比較例1與實施例1的差異在於,比較例1並未以噴霧造粒製程形成該噴霧造粒粉末,而是直接將該鐵鈷混合粉末(Fe-50Co)添加一潤滑劑,該潤滑劑為白臘,添加量為0.6 wt.%(由於粉末流動性不佳,故相較於實施例1需添加較多的量),但即使如此,其流動性仍無法量測,其視密度也無法量測。之後,對該鐵鈷混合粉末(Fe-50Co)以手動方式將粉填入模穴,再進行乾壓成形製程。然嘗試利用300 MPa至1000 MPa之間的成形壓力進行乾壓製程時,發現均無法順利形成胚體,胚體易裂成數片。此處所稱之利用300 MPa至1000 MPa之間的成形壓力,係指分別嘗試使用300 MPa、400 MPa、500 MPa、600 MPa、700 MPa、800 MPa、900 MPa、1000 MPa之成形壓力。 由以上可知,比較例1之鐵鈷混合粉末(Fe-50Co)的壓縮性以及成形性較差,即使增加成形壓力至1000 MPa,仍無法壓製出外形完整之該胚體;反觀,依據本發明製備方法的實施例1則可完整壓製出該胚體,並且進行燒結步驟後所得到的該Fe-50Co金屬軟磁材料亦具有高相對密度以及良好之磁性質。實施例 2 本實施例之起始粉末為一鐵鈷釩混合粉末(Fe-49Co-2V),係選用預合金粉,鈷佔49 wt.%,釩佔2 wt.%,其餘為鐵,平均粒徑為12 µm,經過使用與實施例1相同之噴霧造粒製程及黏結劑所得到之一噴霧造粒粉末的平均粒徑為78 µm,且形貌接近球形。取得該噴霧造粒粉末後,在未加潤滑劑之情形下將該噴霧造粒粉末置於一模具中,令該噴霧造粒粉末維持在室溫,即25℃,並以800 MPa之成形壓力對該噴霧造粒粉末施壓而形成一胚體,胚體密度為6.4 g/cm³。接下來,將該胚體置於氣氛爐中,並通入氫氣氣氛,先於550℃持溫2小時脫脂以除去該黏結劑,然後於1340℃的溫度下燒結1.5小時,而得到一Fe-49Co-2V金屬軟磁材料,該Fe-49Co-2V金屬軟磁材料之密度為7.81 g/cm³,相對密度為94 %,感應磁束密度BS 為1.85 T,矯頑磁力HC 為320 A/m,碳含量小於0.01 wt.%,最大導磁率μmax 為1740。比較例 2 比較例2與實施例2的差異在於,比較例2並未以噴霧造粒製程形成該噴霧造粒粉末,而是直接於該鐵鈷釩預合金粉末(Fe-49Co-2V)添加一潤滑劑,該潤滑劑為白臘,添加量為0.5 wt.%(由於粉末流動性不佳,故相較於實施例2需添加該潤滑劑),但即使如此,其流動性仍無法量測,其視密度也無法量測。之後,對該鐵鈷釩預合金粉末(Fe-49Co-2V)進行乾壓成形製程。然嘗試利用300 MPa至1000 MPa之間的成形壓力進行乾壓製程時,發現均無法順利形成胚體。 由以上可知,比較例2之鐵鈷釩混合粉末(Fe-49Co-2V)的壓縮性以及成形性較差,即使增加成形壓力至1000 MPa,仍無法壓製出外形完整之該胚體;反觀,依據本發明製備方法的實施例2則可完整壓製出該胚體,並且進行燒結步驟後所得到的該Fe-49Co-2V金屬軟磁材料亦具有高相對密度以及良好之鐵磁性質。實施例 3 本實施例之起始粉末為一鐵磷混合粉末(Fe-0.45P),係選用磷化三鐵(Fe3 P)粉與羰基鐵粉之混合,此磷化三鐵(Fe3 P)粉為化合物粉,其磷佔15.6 wt.%,其餘為鐵,而羰基鐵粉為元素粉,其中的碳含量為0.7 wt.%,且羰基鐵粉與磷化三鐵粉之平均粒徑皆小於10 µm,混合後粉末之磷含量為0.45 wt%。經過使用與實施例1相同之噴霧造粒製程及黏結劑所得到之一噴霧造粒粉末的平均粒徑為65 µm,且形貌接近球形。之後,先將該噴霧造粒粉末與一潤滑劑混合,該潤滑劑為白臘,添加量為0.3 wt.%,再將該噴霧造粒粉末置於一模具中,令該噴霧造粒粉末維持在60℃,並以700 MPa之成形壓力對該噴霧造粒粉末施壓而形成一胚體,胚體密度為6.54 g/cm³。接下來,將該胚體至於氣氛爐中,並通入裂解氨與氮氣之混合氣氛,其中氫氣佔10 vol.%,氮氣佔90 vol.%,先於550℃持溫2小時以除去該黏結劑及該潤滑劑,然後於1340℃的溫度下燒結1.5小時,而得到一Fe-0.45P金屬軟磁材料,該Fe-0.45P金屬軟磁材料之密度為7.80 g/cm³,相對密度為99 %,碳含量小於0.01 wt.%,感應磁束密度BS 為1.75 T,矯頑磁力HC 為 40 A/m,最大導磁率μmax 為12400。比較例 3 比較例3與實施例3的差異在於,比較例3並未以噴霧造粒製程形成該噴霧造粒粉末,而是選用一鐵磷混合粉末(Fe-0.45P),其為傳統乾壓成形製程所用之水噴霧鐵粉與磷化三鐵(Fe3 P)粉之混合粉,磷佔0.45 wt.%,水噴霧鐵粉中的碳含量小於0.05 wt.%,其平均粒徑為80 µm,該磷化三鐵粉末之平均粒徑為5 µm,此混合粉具有流動性,適合用於傳統乾壓燒結製程。先將該鐵磷混合粉末(Fe-0.45P)與一潤滑劑混合,該潤滑劑為白臘,添加量為0.75 wt.%,再將該混合粉末置於一模具中,令該粉末維持在室溫,即25℃,並以600 MPa之成形壓力對該粉末施壓而形成一胚體,胚體密度為6.9 g/cm³。接下來,將該胚體置於氣氛爐中,並通入含有75 vol.%氫氣及25 vol.%氮氣之裂解氨還原氣氛,於1120℃(傳統乾壓成形、燒結製程最常用溫度)的溫度下燒結1小時,而得到一Fe-0.45P金屬軟磁材料,該Fe-0.45P金屬軟磁材料之密度為7.12 g/cm³,相對密度為90.4 %,碳含量小於0.01 wt.%,感應磁束密度BS 為1.25 T,矯頑磁力HC 為125 A/m,最大導磁率μmax 為3400。 由以上可知,比較例3以傳統乾壓燒結製程及粉末所形成之Fe-0.45P金屬軟磁材料不論在相對密度、感應磁束密度、矯頑磁力和最大導磁率皆遜於實施例3之Fe-0.45P金屬軟磁材料。實施例 4 本實施例之起始粉末為一鐵矽混合粉末(Fe-3Si),係選用鐵矽母合金粉(Fe-7Si)與羰基鐵粉之混合,此鐵矽母合金粉中矽佔7 wt.%,其餘為鐵,而羰基鐵粉為元素粉,其中的碳含量小於0.05 wt.%,於該鐵矽混合粉末(Fe-3Si)中,矽佔3 wt.%,其餘為鐵,且羰基鐵粉之平均粒徑為5.3 µm,該鐵矽母合金粉(Fe-7Si)之平均粒徑為12 µm。在進行噴霧造粒製程前,該鐵矽混合粉末(Fe-3Si)先與一黏結劑與水均勻混合,該黏結劑為聚乙烯醇及聚乙二醇,且總添加量為0.7 wt.%,經過噴霧造粒製程所得到之一噴霧造粒粉末的平均粒徑為56 µm,且形貌接近球形。之後,將該噴霧造粒粉末置於一模具中,令該噴霧造粒粉末維持在120℃,並以400 MPa之成形壓力對該噴霧造粒粉末施壓而形成一胚體,胚體密度為6.35 g/cm³。接下來,將該胚體置於氣氛爐中,並通入裂解氨氣氛,先持溫2小時於550℃以除去該黏結劑後,於1320℃的溫度下燒結2小時,而得到一Fe-3Si金屬軟磁材料,該Fe-3Si金屬軟磁材料之密度為7.55 g/cm³,相對密度為98.5%,碳含量小於0.03 wt.%,感應磁束密度BS 為1.9 T,矯頑磁力HC 為 70 A/m,最大導磁率μmax 為7100。比較例 4 比較例4與實施例4的差異在於,比較例4並未以噴霧造粒製程形成該噴霧造粒粉末,而是選用一市售適用於傳統乾壓燒結製程之水噴霧鐵粉與鐵矽母合金粉之混合粉末,矽佔3.0 wt.%,其餘為鐵,該混合粉之平均粒徑為75 µm。之後,使用傳統乾壓成形製程,先將該鐵矽混合粉末(Fe-3Si)與一潤滑劑混合,該潤滑劑為白臘,添加量為0.8 wt.%,再將該粉末置於一模具中,令該粉末維持在室溫,即25℃,並以700 MPa之成形壓力對該粉末施壓而形成一胚體,胚體密度為6.8 g/cm³。接下來,將該胚體置於氣氛爐中,並通入含有75 vol.%氫氣及25 vol.%氮氣之裂解氨還原氣氛,先持溫2小時於550℃以除去該潤滑劑後,再於1320℃的溫度下燒結2小時,而得到一Fe-3Si金屬軟磁材料,該Fe-3Si金屬軟磁材料之密度為7.0 g/cm³,相對密度為91.3 %,碳含量小於0.03 wt.%,感應磁束密度BS 為1.2 T,矯頑磁力HC 為95 A/m,最大導磁率μmax 為4000。 由以上可知,比較例4以傳統乾壓燒結法所形成之Fe-3Si金屬軟磁材料不論在相對密度、感應磁束密度、矯頑磁力和最大導磁率皆遜於實施例4之Fe-3Si金屬軟磁材料。實施例 5 本實施例之起始粉末為一鐵磷混合粉末(Fe-0.8P),將磷化三鐵(Fe3 P)粉與羰基鐵粉混合,此磷化三鐵(Fe3 P)粉為化合物粉,其磷佔15.6 wt.%,其餘為鐵,而羰基鐵粉為元素粉,其碳含量小於0.05 wt.%,且羰基鐵粉與磷化三鐵粉之平均粒徑皆小於10 µm。混合後粉末之磷含量為0.8 wt.%。該Fe-0.8P混合粉末先與一黏結劑與水均勻混合,該黏結劑為聚乙烯醇及聚乙二醇,且總添加量為0.7 wt.%,經過噴霧造粒製程後將該噴霧造粒粉末與一潤滑劑混合,該潤滑劑為硬脂酸,添加量為0.2 wt.%,再將該噴霧造粒粉末置於一模具中,令該噴霧造粒粉末維持在95℃,並以800 MPa之成形壓力對該噴霧造粒粉末施壓而形成一胚體,胚體密度為6.55 g/cm³。接下來,將該胚體置於真空爐中,先持溫2小時於550℃以除去該黏結劑及該潤滑劑後,並於1300℃的溫度下燒結1.5小時,而得到一Fe-0.8P金屬軟磁材料,該Fe-0.8P金屬軟磁材料之密度為7.80 g/cm³,相對密度為99%,碳含量小於0.01 wt.%,感應磁束密度BS 為1.65 T,矯頑磁力HC 為53 A/m,最大導磁率μmax 為11600。比較例 5 本比較例之起始粉末與實施例5相同,但採用金屬粉末射出成形(MIM)之方法。先將該磷化三鐵(Fe3 P)粉與羰基鐵粉混合粉末與一黏結劑混合,該黏結劑為石蠟、硬脂酸及聚乙烯的混合體,總添加量為8.0 wt.%,其中聚乙烯約3.0 wt.%,然後再採用金屬射出成形製程取得一胚體,胚體密度為5.1 g/cm³。將該胚體置於正更烷溶劑中去除該黏結劑中的石蠟及硬脂酸。接下來,將該胚體置於真空爐中,並於300℃至550℃之間將殘留的黏結劑燒除,然後在1300℃的溫度下燒結1.5小時,而得到一Fe-0.8P金屬軟磁材料,該Fe-0.8P金屬軟磁材料之密度為7.80 g/cm³,相對密度為99 %,碳含量約0.03 wt.%,感應磁束密度BS 為1.55 T,矯頑磁力HC 為 45 A/m,最大導磁率μmax 為11000。 由以上可知,雖然實施例5與比較例5之該Fe-0.8P金屬軟磁材料的性質接近,但因實施例5中所使用的該黏結劑及該潤滑劑總共僅需1.0 wt.%,較比較例5之8 wt.%少很多,實施例5除了具有較低的原料成本外,亦可省去額外之溶劑脫脂製程,因此可降低製造成本,此外,亦可省去處理溶劑之環保問題。又由於比較例5之MIM製程使用約3 wt.%的聚乙烯,故需長時間之加熱脫脂製程以燒除聚乙烯;且實施例5係採用一般的乾壓成形製程,但比較例5需採用金屬射出成形製程,後者之製程及模具成本明顯高出許多,整體觀之,實施例5之總製程成本較比較例5低了35%。 此外,由於實施例5中,該黏結以及該潤滑劑總共僅1.0 wt.%,生胚密度可達6.55 g/cm³,亦即金屬粉之體積比約82.5 vol.%,相較於比較例5,生胚密度為5.1 g/cm³。該黏結劑有8.0 wt.%,金屬粉之體積比約59.7 vol.%,因此,實施例5之該Fe-0.8P金屬軟磁材料燒結後達到99 vol.%密度時的線性收縮率僅5.9%,而比較例5之該Fe-0.8P金屬軟磁材料的線性收縮率高達15.5%,導致其尺寸穩定性不佳,不良率大幅提昇。實施例 6 本實施例之起始粉末為一鐵鎳混合粉末(Fe-50Ni),係選用羰基鐵粉與羰基鎳粉兩種元素粉之混合,鎳佔50 wt.%,其餘為鐵,且羰基鐵粉與羰基鎳粉中的碳含量皆小於0.05 wt.%,兩種金屬粉之平均粒徑皆小於10 µm,由於粉末太細,其流動性及視密度均無法量測。在進行噴霧造粒製程前,該鐵鎳混合粉末(Fe-50Ni)先與一黏結劑與水均勻混合,該黏結劑為聚乙烯醇及聚乙二醇,且添加量總共為0.7 wt.%,經過噴霧造粒製程所得到之一噴霧造粒粉末的平均粒徑為74 µm,且形貌接近球形,因此,此造粒粉已具流動性,以MPIF Standard 03標準測試法所測得之流動性為31 sec/50g,MPIF Standard 04標準測試法所測得之視密度為2.2 g/ cm3 。之後,再將該噴霧造粒粉末置於一模具中,令該噴霧造粒粉末維持在60℃,並以500 MPa之成形壓力對該噴霧造粒粉末施壓而形成一胚體,胚體密度為6.5 g/cm³。接下來,將該胚體置於真空爐中,並通入少量氬氣,氬氣之分壓約0.05大氣壓,先持溫於300℃至600℃之間以除去該黏結劑後,於1350℃的溫度下燒結2小時,而得到一Fe-50Ni金屬軟磁材料,該Fe-50Ni金屬軟磁材料之密度為7.95 g/cm³,相對密度為95 %,碳含量小於0.01 wt.%,感應磁束密度BS 為1.45 T,矯頑磁力HC 為 16 A/m,最大導磁率μmax 為27000。由此製程所得Fe-50Ni金屬軟磁之生產成本比由金屬射出成形製程所製得之工件低,而磁性質則與MPIF Standard 35 for Metal Injection Molded Parts中由金屬粉末射出成形製程所製得工件之磁性質相當。比較例 6 比較例6與實施例6的差異在於,比較例1並未以噴霧造粒製程形成該噴霧造粒粉末,而是直接將該鐵鎳混合粉末(Fe-50Ni)添加一潤滑劑,該潤滑劑為白臘,添加量為0.8 wt.%,但其流動性仍無法量測,其視密度也無法量測。之後,對該混合粉末以手動方式將粉填入模穴,再進行乾壓成形製程。然嘗試利用300 MPa至1000 MPa之間的成形壓力進行乾壓製程時,發現均無法順利形成胚體,胚體易裂成數片。 由以上可知,比較例6之鐵鎳混合粉末(Fe-50Ni)的壓縮性以及成形性較差,即使增加成形壓力至1000 MPa,仍無法壓製出外形完整之該胚體;反觀,依據本發明製備方法的實施例6則可完整壓製出該胚體,並且進行燒結步驟後所得到的該Fe-50Ni金屬軟磁材料亦具有高相對密度以及良好之磁性質。實施例 7 本實施例之起始粉末為一鐵鎳鉬混合粉末(Fe-79Ni-4Mo),係選用羰基鐵粉、羰基鎳粉與鉬粉三種元素粉之混合,鎳佔79 wt.%,鉬佔4 wt.%,其餘為鐵,羰基鐵粉的碳含量為0.8 wt.%,羰基鎳粉與鉬粉的碳含量皆小於0.05 wt.%,三種金屬粉之平均粒徑皆小於10 µm,由於粉末太細,其流動性及視密度均無法量測。在進行噴霧造粒製程前,該鐵鎳鉬混合粉末(Fe-79Ni-4Mo)先與一黏結劑與水均勻混合,該黏結劑為聚乙烯醇及聚乙二醇,且添加量總共為0.8 wt.%,經過噴霧造粒製程所得到之一噴霧造粒粉末的平均粒徑為72 µm,且形貌接近球形,因此,此造粒粉已具流動性,以MPIF Standard 03標準測試法所測得之流動性為32 sec/50g,MPIF Standard 04標準測試法所測得之視密度為2.3 g/ cm3 。之後,先將該噴霧造粒粉末與一潤滑劑混合,該潤滑劑為白臘,添加量為0.2 wt.%,再將該噴霧造粒粉末置於一模具中,令該噴霧造粒粉末維持在室溫(27℃),並以500 MPa之成形壓力對該噴霧造粒粉末施壓而形成一胚體,胚體密度為6.3 g/cm³。接下來,將該胚體置於氣氛爐中,並通入氫氣氣氛,先持溫於300℃至600℃之間以除去該黏結劑與該潤滑劑後,於1350℃的溫度下燒結2小時,而得到一Fe-79Ni-4Mo金屬軟磁材料,該Fe-79Ni-4Mo金屬軟磁材料之密度為8.3 g/cm³,相對密度為95 %,碳含量小於0.01 wt.%,感應磁束密度BS 為0.8 T,矯頑磁力HC 為 89 A/m,最大導磁率μmax 為120000。比較例 7 本比較例之起始粉末與實施例7相同,但採用金屬粉末射出成形(MIM)之方法。先將該鐵鎳鉬混合粉末(Fe-79Ni-4Mo)與一黏結劑混合,該黏結劑為石蠟、硬脂酸及聚乙烯的混合體,總添加量為8.0 wt.%,其中聚乙烯約3.0 wt.%,然後再採用金屬射出成形製程取得一胚體,胚體密度為5.3 g/cm³。將該胚體置於正更烷溶劑中去除該黏結劑中的石蠟及硬脂酸。接下來,將該胚體置於氣氛爐中,並通入氫氣氣氛,並於300℃至600℃之間將殘留的黏結劑燒除,然後在1350℃的溫度下燒結2小時,而得到一Fe-79Ni-4Mo金屬軟磁材料,該Fe-79Ni-4Mo金屬軟磁材料之密度為8.25 g/cm³,相對密度為94 %,感應磁束密度BS 為0.8 T,矯頑磁力HC 為 95 A/m,最大導磁率μmax 為115000。 由以上可知,雖然實施例7與比較例7之該Fe-79Ni-4Mo金屬軟磁材料的性質接近,但因實施例7中所使用的該黏結劑及該潤滑劑較比較例7少,實施例7除了具有較低的原料成本外,亦可省去額外之脫脂製程成本也不需處理溶劑之環保問題。實施例7係採用一般的乾壓成形製程,但比較例7採用金屬射出成形製程,後者製程及模具成本明顯高出許多,整體觀之,實施例7之總製程成本較比較例7低了約35%。 此外,由於實施例7中,生胚密度可達6.3 g/cm³,相較於比較例5,生胚密度為5.3 g/cm³,因此,實施例7之該Fe-79Ni-4Mo金屬軟磁材料燒結後的線性收縮率低於比較例7之Fe-79Ni-4Mo金屬軟磁材料的線性收縮率,導致實施例7之尺寸穩定性較佳,良率大幅提昇。 綜上所述,本發明具有下列特點: 一、本發明利用該噴霧造粒製程得到的該噴霧造粒粉末,由於呈球狀且含黏結劑,係具有優異的流動性、成形性與壓縮性,可改善習知以細粉生產金屬軟磁材料時在傳統乾壓製備方法中因流動性、成形性與壓縮性不佳而不易成形之問題。 二、承上,由於本發明之該胚體具有高生胚密度,且使用小於15微米之起始粉末,使得最終燒結得到之該金屬軟磁材料,無論是相對密度或磁性質,均有較傳統乾壓燒結製備方法更為優異的表現。 三、本發明利用該噴霧造粒製程得到的該噴霧造粒粉末,由於呈球狀,係具有優異的流動性、成形性與壓縮性,可直接以傳統乾壓製備方法製作金屬軟磁,可降低以習知金屬射出成形製程生產金屬軟磁材料之成本且可改善金屬射出成形生產金屬軟磁材料之尺寸穩定性不佳,良率不高之問題。The detailed description and technical contents of the present invention will now be described as follows: Please refer to FIG. 1 and FIG. 1 is a schematic flow chart of the steps of the present invention. Step S1 first provides an iron-containing and metal-soft magnetic The starting powder of the nature, the starting powder preferably has an average particle size of less than 15 micrometers (μm). In an embodiment of the present invention, the main source of iron of the starting powder is a carbonyl iron powder, and the carbon content of the carbonyl iron powder may be less than 0.05 wt.%; in another embodiment of the present invention, The starting powder may be an elemental powder, a compound powder, a master alloy powder or a mixed powder thereof. Further, the composition of the starting powder may include iron and at least one additional element selected from the group consisting of phosphorus, cerium, cobalt, vanadium, nickel, molybdenum, and combinations thereof. For example, the starting powder may be iron-phosphorus mixed powder (Fe-P), iron-iron mixed powder (Fe-Si), iron-cobalt mixed powder (Fe-Co), iron-cobalt-vanadium mixed powder (Fe-Co- V), a soft magnetic metal powder such as an iron-nickel mixed powder (Fe-Ni) or an iron-nickel-molybdenum mixed powder (Fe-Ni-Mo) or an alloy powder having the above composition. In other embodiments of the present invention, the weight percentage of phosphorus of the starting powder may be between 0.4 wt.% and 0.9 wt.%, the balance being iron and unavoidable impurities; or the enthalpy of the starting powder. The weight percentage may be between 2 wt.% and 6 wt.%, the balance being iron and unavoidable impurities; or the weight percentage of cobalt of the starting powder may be between 48 wt.% and 52 wt.%. The weight percentage of vanadium is less than 3 wt.%, and the balance is iron and unavoidable impurities; or the weight percentage of nickel of the starting powder may be between 48 wt.% and 52 wt.%, and the balance is iron and Inevitable impurities; or the weight percentage of nickel of the starting powder may be between 77 wt.% and 83 wt.%, the weight percentage of molybdenum may be less than 5 wt.%, and the balance is iron and inevitable impurities . Step S2 is a spray granulation process of the starting powder, and a spray granulated powder having a nearly spherical powder morphology and an average particle diameter of 40 micrometers to 100 is obtained from the starting powder. Between microns. In this embodiment, in step S2, a binder and water are added to the starting powder to form a mixture, and the binder may be gum arabic, methyl cellulose, polyvinyl alcohol, polyethylene glycol or mixture. After the spray granulation process, the spray granulated powder may have an average particle diameter of between 40 micrometers and 100 micrometers, and the powder morphology is close to a spherical shape, which is advantageous for improving the fluidity, compressibility, and visual properties of the powder. Density and formability. In step S3, the spray granulated powder is placed in a mold, and the spray granulated powder is maintained at a forming temperature and subjected to a forming pressure to form an embryo body. In this embodiment, the forming temperature is between 20 ° C and 150 ° C, the forming pressure is between 300 MPa and 1000 MPa, and a lubricant may be added to the spray granulated powder according to requirements. It may be white wax, stearic acid or zinc stearate or other lubricant, and the spray granulated powder may be placed in the mold. In general, the mold comprises a middle mold, an upper punch and an undershoot, and the upper punch and the lower punch form a cavity space for accommodating the spray granulated powder, and in the embodiment, the permeable medium is permeable. Heating the middle mold, the upper punch or the lower punch of the mold, and maintaining the spray granulated powder between 20 ° C and 150 ° C by heat conduction of the mold; or alternatively, granulating the spray The powder feedshoe and the delivery tube conveying the spray granulated powder heat the spray granulated powder electrically or oil-heated to maintain the spray granulated powder between 20 ° C and 150 ° C. Step S4 is first performing a degreasing step, heating the embryo body to a degreasing temperature to remove the lubricant or the binder, or degreasing by other chemical methods, and then heating to a sintering temperature to obtain a metal soft magnetic material. . In this embodiment, step S4 may be performed in a vacuum furnace or an atmosphere furnace. If the atmosphere furnace is used, a reducing atmosphere containing hydrogen or cracked ammonia may be introduced, and the sintering temperature is 1100 ° C to 1400. Between °C. Further, the metal soft magnetic material obtained in the step S4 has a relative density of more than 94%. In order to further specifically describe the content of the method for preparing the high-density powder metallurgy metal soft magnetic material of the present invention, please refer to the following examples according to the present invention and comparative examples using other techniques: Example 1 : The start of the present embodiment The powder is an iron-cobalt mixed powder (Fe-50Co), which is a mixture of carbonyl iron powder and cobalt powder. Cobalt accounts for 50 wt.%, the balance is iron, and the carbon content of the carbonyl iron powder is less than 0.05 wt. .%, the average particle size of the cobalt powder is less than 10 μm. Since the powder is too fine, its fluidity and apparent density cannot be measured by the MPIF standard test method. Before the spray granulation process, the iron-cobalt mixed powder (Fe-50Co) is uniformly mixed with a binder and water. The binder is polyvinyl alcohol and polyethylene glycol, and the added amount is 1.0 wt of the metal powder. .%, one of the spray granulation powders obtained by the spray granulation process has an average particle size of 75 μm and a morphology close to a spherical shape. Therefore, the granulated powder has fluidity and is measured by the MPIF Standard 03 standard test method. The resulting fluidity is 30 sec/50g, and the apparent density measured by the MPIF Standard 04 standard test method is 2.1 g/cm 3 . Thereafter, the spray granulated powder is first mixed with a lubricant, which is white wax, added in an amount of 0.1 wt.%, and the spray granulated powder is placed in a mold to maintain the spray granulated powder. The spray granulated powder was pressed at 35 ° C and at a forming pressure of 600 MPa to form an embryo body having a bulk density of 6.2 g/cm 3 . Next, the embryo body is placed in an atmosphere furnace, and a reducing ammonia reducing atmosphere containing 75 vol.% of hydrogen and 25 vol.% of nitrogen is introduced, and the temperature is first maintained between 300 ° C and 600 ° C to remove the binder. After sintering with the lubricant, it was sintered at a temperature of 1355 ° C for 2 hours to obtain a Fe-50Co metal soft magnetic material having a density of 7.89 g/cm 3 , a relative density of 94.2 %, and a carbon content of less than 94.2 %. 0.01 wt.%, the induced magnetic flux density B S was 2.17 T (Tesla), the coercive force H C was 89 A/m, and the maximum magnetic permeability μ max was 6790. The density and magnetic properties of the Fe-50Co soft magnetic material obtained by the process are better than those of the metal injection molding process in the MPIF Standard 35 for Metal Injection Molded Parts, and the production cost is also low. Comparative Example 1 : The difference between Comparative Example 1 and Example 1 is that Comparative Example 1 does not form the spray granulated powder by a spray granulation process, but directly adds a lubricant to the iron-cobalt mixed powder (Fe-50Co). The lubricant is white wax and the addition amount is 0.6 wt.% (due to the poor fluidity of the powder, it is required to add more than the first embodiment), but even then, the fluidity cannot be measured. Its apparent density cannot be measured. Thereafter, the iron-cobalt mixed powder (Fe-50Co) was manually filled into the cavity by a powder, and then subjected to a dry press forming process. However, when attempting to use the forming pressure between 300 MPa and 1000 MPa for dry pressing, it was found that the embryo body could not be formed smoothly, and the embryo body was easily broken into several pieces. The use of the forming pressure between 300 MPa and 1000 MPa as referred to herein means the forming pressures of 300 MPa, 400 MPa, 500 MPa, 600 MPa, 700 MPa, 800 MPa, 900 MPa, and 1000 MPa, respectively. From the above, the iron-cobalt mixed powder (Fe-50Co) of Comparative Example 1 has poor compressibility and formability, and even if the forming pressure is increased to 1000 MPa, the embryo body having a complete shape cannot be pressed; in other words, it is prepared according to the present invention. In the first embodiment of the method, the embryo body can be completely pressed, and the Fe-50Co metal soft magnetic material obtained after the sintering step also has high relative density and good magnetic properties. Example 2 : The starting powder of the present embodiment is an iron-cobalt-vanadium mixed powder (Fe-49Co-2V), which is a pre-alloyed powder, cobalt accounts for 49 wt.%, vanadium accounts for 2 wt.%, and the rest is iron. The average particle diameter was 12 μm, and the spray granulated powder obtained by the same spray granulation process and binder as in Example 1 had an average particle diameter of 78 μm and a morphology close to a spherical shape. After obtaining the spray granulated powder, the spray granulated powder is placed in a mold without adding a lubricant, and the spray granulated powder is maintained at room temperature, that is, 25 ° C, and is formed at a pressure of 800 MPa. The spray granulated powder was pressed to form an embryo body having a density of 6.4 g/cm3. Next, the embryo body was placed in an atmosphere furnace, and subjected to a hydrogen atmosphere, degreased at 550 ° C for 2 hours to remove the binder, and then sintered at a temperature of 1340 ° C for 1.5 hours to obtain a Fe- 49Co-2V metal soft magnetic material, the Fe-49Co-2V metal soft magnetic material has a density of 7.81 g/cm3, a relative density of 94%, an induced magnetic flux density B S of 1.85 T, and a coercive force H C of 320 A/m. The carbon content is less than 0.01 wt.%, and the maximum magnetic permeability μ max is 1,740. Comparative Example 2 : The difference between Comparative Example 2 and Example 2 is that Comparative Example 2 does not form the spray granulated powder by a spray granulation process, but directly on the iron-cobalt-vanadium prealloyed powder (Fe-49Co-2V). A lubricant is added, the lubricant is white wax, and the addition amount is 0.5 wt.% (the lubricant is added compared to Example 2 because of poor fluidity of the powder), but even so, the fluidity cannot be obtained. Measurement, its apparent density can not be measured. Thereafter, the iron-cobalt-vanadium prealloyed powder (Fe-49Co-2V) was subjected to a dry press forming process. However, when attempting to perform a dry pressing process using a forming pressure of between 300 MPa and 1000 MPa, it was found that the embryo body could not be formed smoothly. From the above, the iron-cobalt-vanadium mixed powder of Comparative Example 2 (Fe-49Co-2V) has poor compressibility and formability, and even if the forming pressure is increased to 1000 MPa, the embryo body having a complete shape cannot be pressed; In the second embodiment of the preparation method of the present invention, the embryo body can be completely pressed, and the Fe-49Co-2V metal soft magnetic material obtained after the sintering step also has high relative density and good ferromagnetic properties. Example 3 : The starting powder of the present embodiment is an iron-phosphorus mixed powder (Fe-0.45P), which is a mixture of phosphating triiron (Fe 3 P) powder and carbonyl iron powder, and the phosphating triiron (Fe) 3 P) powder is a compound powder, the phosphorus accounts for 15.6 wt.%, the rest is iron, and the carbonyl iron powder is elemental powder, wherein the carbon content is 0.7 wt.%, and the average of carbonyl iron powder and phosphating tri-iron powder The particle size is less than 10 μm, and the phosphorus content of the powder after mixing is 0.45 wt%. One of the spray granulated powders obtained by the same spray granulation process and binder as in Example 1 had an average particle diameter of 65 μm and a morphology close to a spherical shape. Thereafter, the spray granulated powder is first mixed with a lubricant, which is white wax, added in an amount of 0.3 wt.%, and the spray granulated powder is placed in a mold to maintain the spray granulated powder. The spray granulated powder was pressed at 60 ° C and at a forming pressure of 700 MPa to form an embryo body having a bulk density of 6.54 g/cm 3 . Next, the embryo body is placed in an atmosphere furnace, and a mixed atmosphere of cracked ammonia and nitrogen is introduced, wherein hydrogen accounts for 10 vol.%, nitrogen accounts for 90 vol.%, and the temperature is maintained at 550 ° C for 2 hours to remove the bond. The lubricant and the lubricant are then sintered at a temperature of 1340 ° C for 1.5 hours to obtain a Fe-0.45P metal soft magnetic material having a density of 7.80 g/cm 3 and a relative density of 99 %. The carbon content is less than 0.01 wt.%, the induced magnetic flux density B S is 1.75 T, the coercive force H C is 40 A/m, and the maximum magnetic permeability μ max is 12,400. Comparative Example 3 : The difference between Comparative Example 3 and Example 3 is that Comparative Example 3 does not form the spray granulated powder by a spray granulation process, but an iron-phosphorus mixed powder (Fe-0.45P), which is a conventional The mixed powder of water sprayed iron powder and phosphating triiron (Fe 3 P) powder used in the dry press forming process, phosphorus accounts for 0.45 wt.%, and the carbon content in the water sprayed iron powder is less than 0.05 wt.%, and the average particle diameter thereof At 80 μm, the average particle size of the phosphide powder is 5 μm, and the mixed powder has fluidity and is suitable for use in a conventional dry pressing sintering process. First, the iron-phosphorus mixed powder (Fe-0.45P) is mixed with a lubricant, which is white wax, added in an amount of 0.75 wt.%, and the mixed powder is placed in a mold to maintain the powder in the mold. The powder was pressed at room temperature, i.e., 25 ° C, at a forming pressure of 600 MPa to form an embryo body having a density of 6.9 g/cm 3 . Next, the embryo body is placed in an atmosphere furnace, and a reducing ammonia reducing atmosphere containing 75 vol.% of hydrogen and 25 vol.% of nitrogen is introduced at 1120 ° C (the most common temperature for conventional dry pressing and sintering processes). Sintering at temperature for 1 hour, to obtain a Fe-0.45P metal soft magnetic material having a density of 7.12 g/cm3, a relative density of 90.4%, a carbon content of less than 0.01 wt.%, and an induced magnetic flux density. B S is 1.25 T, the coercive force H C is 125 A/m, and the maximum magnetic permeability μ max is 3400. It can be seen from the above that the Fe-0.45P metal soft magnetic material formed by the conventional dry pressing sintering process and the powder of Comparative Example 3 is inferior to the Fe-- of Example 3 regardless of the relative density, the induced magnetic flux density, the coercive force and the maximum magnetic permeability. 0.45P metal soft magnetic material. Example 4 : The starting powder of the present embodiment is a mixed powder of iron (Fe-3Si), which is selected from the mixture of iron-base alloy powder (Fe-7Si) and carbonyl iron powder. It accounts for 7 wt.%, the rest is iron, and the carbonyl iron powder is elemental powder, wherein the carbon content is less than 0.05 wt.%. In the iron strontium mixed powder (Fe-3Si), strontium accounts for 3 wt.%, and the rest is Iron, and the average particle diameter of the carbonyl iron powder is 5.3 μm, and the average particle diameter of the iron-base alloy powder (Fe-7Si) is 12 μm. Before the spray granulation process, the iron slag mixed powder (Fe-3Si) is uniformly mixed with a binder and water, the binder is polyvinyl alcohol and polyethylene glycol, and the total addition amount is 0.7 wt.%. One of the spray granulated powders obtained by the spray granulation process has an average particle diameter of 56 μm and a morphology close to a spherical shape. Thereafter, the spray granulated powder is placed in a mold, the spray granulated powder is maintained at 120 ° C, and the spray granulated powder is pressed at a forming pressure of 400 MPa to form an embryo body having a density of the embryo body. 6.35 g/cm3. Next, the embryo body was placed in an atmosphere furnace, and passed through a cracked ammonia atmosphere, and the temperature was first maintained at 550 ° C for 2 hours to remove the binder, and then sintered at a temperature of 1320 ° C for 2 hours to obtain a Fe- 3Si metal soft magnetic material, the Fe-3Si metal soft magnetic material has a density of 7.55 g/cm3, a relative density of 98.5%, a carbon content of less than 0.03 wt.%, an induced magnetic flux density B S of 1.9 T, and a coercive force H C of 70 A/m, the maximum magnetic permeability μ max is 7100. Comparative Example 4 : The difference between Comparative Example 4 and Example 4 is that Comparative Example 4 does not form the spray granulated powder by a spray granulation process, but a commercially available water spray iron powder suitable for a conventional dry pressing sintering process is selected. The mixed powder with the iron samarium alloy powder, 矽 accounted for 3.0 wt.%, and the balance was iron, and the average particle size of the mixed powder was 75 μm. Thereafter, using a conventional dry press forming process, the iron slag mixed powder (Fe-3Si) is first mixed with a lubricant, which is white wax, added in an amount of 0.8 wt.%, and the powder is placed in a mold. The powder was maintained at room temperature, i.e., 25 ° C, and the powder was pressed at a forming pressure of 700 MPa to form an embryo body having a density of 6.8 g/cm 3 . Next, the embryo body is placed in an atmosphere furnace, and a reducing ammonia reducing atmosphere containing 75 vol.% of hydrogen and 25 vol.% of nitrogen is introduced, and the lubricant is removed by holding the temperature for 2 hours at 550 ° C. Sintering at a temperature of 1320 ° C for 2 hours, to obtain a Fe-3Si metal soft magnetic material, the density of the Fe-3Si metal soft magnetic material is 7.0 g / cm3, the relative density is 91.3%, the carbon content is less than 0.03 wt.%, induction The magnetic flux density B S was 1.2 T, the coercive force H C was 95 A/m, and the maximum magnetic permeability μ max was 4000. From the above, the Fe-3Si metal soft magnetic material formed by the conventional dry-pressure sintering method of Comparative Example 4 is inferior to the Fe-3Si metal soft magnetic material of Example 4 regardless of the relative density, the induced magnetic flux density, the coercive force and the maximum magnetic permeability. material. Example 5: Example of the present embodiment the starting powder is an iron-phosphorus mixed powder (Fe-0.8P), iron phosphide (Fe 3 P) mixed with a carbonyl iron powder, the iron phosphide (Fe 3 P Powder is compound powder, its phosphorus accounts for 15.6 wt.%, the rest is iron, and carbonyl iron powder is elemental powder, its carbon content is less than 0.05 wt.%, and the average particle size of carbonyl iron powder and phosphating triiron powder are Less than 10 μm. The phosphorus content of the mixed powder was 0.8 wt.%. The Fe-0.8P mixed powder is uniformly mixed with a binder and water. The binder is polyvinyl alcohol and polyethylene glycol, and the total addition amount is 0.7 wt.%. After the spray granulation process, the spray is made. The granulated powder is mixed with a lubricant which is stearic acid in an amount of 0.2 wt.%, and the spray granulated powder is placed in a mold, and the spray granulated powder is maintained at 95 ° C, and The spray granulated powder was pressed at a forming pressure of 800 MPa to form an embryo body having a density of 6.55 g/cm3. Next, the embryo body was placed in a vacuum furnace, first held at 550 ° C for 2 hours to remove the binder and the lubricant, and sintered at a temperature of 1300 ° C for 1.5 hours to obtain a Fe-0.8P. The metal soft magnetic material has a density of 7.80 g/cm 3 , a relative density of 99%, a carbon content of less than 0.01 wt.%, an induced magnetic flux density B S of 1.65 T, and a coercive force H C of 53. A/m, the maximum magnetic permeability μ max is 11600. Comparative Example 5 : The starting powder of this comparative example was the same as that of Example 5, but a metal powder injection molding (MIM) method was employed. First, the mixed powder of phosphating iron (Fe 3 P) powder and carbonyl iron powder is mixed with a binder, and the binder is a mixture of paraffin, stearic acid and polyethylene, and the total addition amount is 8.0 wt.%. The polyethylene is about 3.0 wt.%, and then an embryo body is obtained by a metal injection molding process, and the density of the embryo body is 5.1 g/cm3. The embryo body is placed in a normal hexane solvent to remove paraffin and stearic acid from the binder. Next, the embryo body is placed in a vacuum furnace, and the residual binder is burned off between 300 ° C and 550 ° C, and then sintered at a temperature of 1300 ° C for 1.5 hours to obtain a Fe-0.8P metal soft magnetic. The Fe-0.8P metal soft magnetic material has a density of 7.80 g/cm3, a relative density of 99%, a carbon content of about 0.03 wt.%, an induced magnetic flux density B S of 1.55 T, and a coercive force H C of 45 A/ m, the maximum magnetic permeability μ max is 11,000. It can be seen from the above that although the properties of the Fe-0.8P metal soft magnetic material of Example 5 and Comparative Example 5 are close, the total amount of the adhesive and the lubricant used in Example 5 is only 1.0 wt.%. In Comparative Example 5, 8 wt.% is much less. In addition to the lower raw material cost, the embodiment 5 can also eliminate the additional solvent degreasing process, thereby reducing the manufacturing cost and, in addition, eliminating the environmental problem of treating the solvent. . Moreover, since the MIM process of Comparative Example 5 uses about 3 wt.% of polyethylene, it takes a long time to heat the degreasing process to burn off the polyethylene; and Example 5 uses a general dry press forming process, but Comparative Example 5 requires The metal injection molding process is used, and the latter process and mold cost are significantly higher. As a whole, the total process cost of the embodiment 5 is 35% lower than that of the comparative example 5. In addition, since the bonding and the lubricant are only 1.0 wt.% in total in Example 5, the density of the raw embryos can reach 6.55 g/cm3, that is, the volume ratio of the metal powder is about 82.5 vol.%, compared with Comparative Example 5. The density of raw embryos was 5.1 g/cm3. The binder has a volume ratio of 8.0 wt.% and a metal powder of about 59.7 vol.%. Therefore, the linear shrinkage of the Fe-0.8P metal soft magnetic material of Example 5 at a density of 99 vol.% after sintering is only 5.9%. The linear shrinkage of the Fe-0.8P metal soft magnetic material of Comparative Example 5 was as high as 15.5%, resulting in poor dimensional stability and a large increase in the defect rate. Example 6 : The starting powder of the present embodiment is an iron-nickel mixed powder (Fe-50Ni), which is a mixture of two kinds of elemental powders of carbonyl iron powder and nickel carbonyl powder, nickel accounts for 50 wt.%, and the rest is iron. Moreover, the carbon content in both the carbonyl iron powder and the carbonyl nickel powder is less than 0.05 wt.%, and the average particle diameters of the two metal powders are all less than 10 μm. Since the powder is too fine, the fluidity and apparent density cannot be measured. Before the spray granulation process, the iron-nickel mixed powder (Fe-50Ni) is uniformly mixed with a binder and water, and the binder is polyvinyl alcohol and polyethylene glycol, and the total amount is 0.7 wt.%. One of the spray granulation powders obtained by the spray granulation process has an average particle diameter of 74 μm and a morphology close to a spherical shape. Therefore, the granulated powder has fluidity and is measured by the MPIF Standard 03 standard test method. The fluidity is 31 sec/50g, and the apparent density measured by the MPIF Standard 04 standard test method is 2.2 g/cm 3 . Thereafter, the spray granulated powder is placed in a mold, the spray granulated powder is maintained at 60 ° C, and the spray granulated powder is pressed at a forming pressure of 500 MPa to form an embryo body, and the embryo body density It is 6.5 g/cm3. Next, the embryo body is placed in a vacuum furnace, and a small amount of argon gas is introduced, and the partial pressure of argon gas is about 0.05 atm, and the temperature is first maintained between 300 ° C and 600 ° C to remove the binder, at 1350 ° C. Sintering at a temperature of 2 hours to obtain a Fe-50Ni metal soft magnetic material having a density of 7.95 g/cm3, a relative density of 95%, a carbon content of less than 0.01 wt.%, and an induced magnetic flux density B. S is 1.45 T, the coercive force H C is 16 A/m, and the maximum magnetic permeability μ max is 27,000. The production cost of the Fe-50Ni metal soft magnetic obtained by the process is lower than that of the workpiece obtained by the metal injection molding process, and the magnetic material is the workpiece obtained by the metal powder injection molding process in the MPIF Standard 35 for Metal Injection Molded Parts. The magnetic properties are equivalent. Comparative Example 6 : The difference between Comparative Example 6 and Example 6 is that Comparative Example 1 does not form the spray granulated powder by a spray granulation process, but directly adds a lubricant to the iron-nickel mixed powder (Fe-50Ni). The lubricant is white wax and the addition amount is 0.8 wt.%, but the fluidity is still unmeasurable, and the apparent density cannot be measured. Thereafter, the powder is manually filled into the cavity by the powder, and then subjected to a dry press forming process. However, when attempting to use the forming pressure between 300 MPa and 1000 MPa for dry pressing, it was found that the embryo body could not be formed smoothly, and the embryo body was easily broken into several pieces. From the above, the iron-nickel mixed powder (Fe-50Ni) of Comparative Example 6 has poor compressibility and formability, and even if the forming pressure is increased to 1000 MPa, the embryo body having a complete shape cannot be pressed; in other words, it is prepared according to the present invention. In the sixth embodiment of the method, the embryo body can be completely pressed, and the Fe-50Ni metal soft magnetic material obtained after the sintering step also has high relative density and good magnetic properties. Example 7 : The starting powder of the present embodiment is an iron-nickel-molybdenum mixed powder (Fe-79Ni-4Mo), which is a mixture of carbonyl iron powder, nickel carbonyl powder and molybdenum powder, and nickel accounts for 79 wt.%. Molybdenum accounts for 4 wt.%, the rest is iron, the carbon content of carbonyl iron powder is 0.8 wt.%, the carbon content of nickel carbonyl powder and molybdenum powder are less than 0.05 wt.%, and the average particle diameter of all three metal powders is less than 10 Μm, since the powder is too fine, its fluidity and apparent density cannot be measured. Before the spray granulation process, the iron-nickel-molybdenum mixed powder (Fe-79Ni-4Mo) is uniformly mixed with a binder and water, and the binder is polyvinyl alcohol and polyethylene glycol, and the total amount is 0.8. Wt.%, one of the spray granulation powders obtained by the spray granulation process has an average particle size of 72 μm and a nearly spherical shape. Therefore, the granulated powder has fluidity and is tested by the MPIF Standard 03 standard method. The measured fluidity was 32 sec/50g, and the apparent density measured by the MPIF Standard 04 standard test method was 2.3 g/cm 3 . Thereafter, the spray granulated powder is first mixed with a lubricant, the lubricant is white wax, and the addition amount is 0.2 wt.%, and the spray granulated powder is placed in a mold to maintain the spray granulated powder. The spray granulated powder was pressed at room temperature (27 ° C) at a forming pressure of 500 MPa to form an embryo body having a bulk density of 6.3 g/cm 3 . Next, the embryo body is placed in an atmosphere furnace, and a hydrogen atmosphere is introduced, and the temperature is maintained between 300 ° C and 600 ° C to remove the binder and the lubricant, and then sintered at a temperature of 1350 ° C for 2 hours. And obtaining a Fe-79Ni-4Mo metal soft magnetic material having a density of 8.3 g/cm 3 , a relative density of 95%, a carbon content of less than 0.01 wt.%, and an induced magnetic flux density B S of 0.8 T, the coercive force H C was 89 A/m, and the maximum magnetic permeability μ max was 120,000. Comparative Example 7 : The starting powder of this comparative example was the same as that of Example 7, but a metal powder injection molding (MIM) method was employed. First, the iron-nickel-molybdenum mixed powder (Fe-79Ni-4Mo) is mixed with a binder, which is a mixture of paraffin, stearic acid and polyethylene, and the total addition amount is 8.0 wt.%, wherein the polyethylene is about 3.0 wt.%, and then a metal injection molding process was used to obtain an embryo body with a density of 5.3 g/cm3. The embryo body is placed in a normal hexane solvent to remove paraffin and stearic acid from the binder. Next, the embryo body is placed in an atmosphere furnace, and a hydrogen atmosphere is introduced, and the residual binder is burned off between 300 ° C and 600 ° C, and then sintered at a temperature of 1350 ° C for 2 hours to obtain a Fe-79Ni-4Mo metal soft magnetic material, the Fe-79Ni-4Mo metal soft magnetic material has a density of 8.25 g/cm3, a relative density of 94%, an induced magnetic flux density B S of 0.8 T, and a coercive force H C of 95 A/ m, the maximum magnetic permeability μ max is 115,000. From the above, although the properties of the Fe-79Ni-4Mo metal soft magnetic material of Example 7 and Comparative Example 7 are similar, the binder used in Example 7 and the lubricant are less than Comparative Example 7, and the examples are In addition to lower raw material costs, it also eliminates the need for additional degreasing process costs and environmental issues. The seventh embodiment adopts a general dry press forming process, but the comparative example 7 employs a metal injection molding process, and the latter process and mold cost are significantly higher. As a whole, the total process cost of the embodiment 7 is lower than that of the comparative example 7. 35%. Further, since the density of the green embryo was up to 6.3 g/cm3 in Example 7, the density of the green embryo was 5.3 g/cm3 as compared with Comparative Example 5, and therefore, the Fe-79Ni-4Mo metal soft magnetic material of Example 7 was sintered. The linear shrinkage ratio after that was lower than that of the Fe-79Ni-4Mo metal soft magnetic material of Comparative Example 7 resulted in better dimensional stability of Example 7, and the yield was greatly improved. In summary, the present invention has the following features: 1. The spray granulated powder obtained by the spray granulation process of the present invention has excellent fluidity, formability and compressibility due to its spherical shape and containing a binder. It can improve the conventional problem that the production of metal soft magnetic materials by fine powder is not easy to form due to poor fluidity, formability and compressibility in the conventional dry pressing preparation method. 2. In conclusion, since the embryo body of the present invention has a high green density and uses a starting powder of less than 15 micrometers, the metal soft magnetic material obtained by final sintering, whether of relative density or magnetic properties, is more conventionally dried. The pressure sintering preparation method is more excellent in performance. 3. The spray granulated powder obtained by the spray granulation process of the present invention has excellent fluidity, formability and compressibility because it has a spherical shape, and can directly form a metal soft magnetic body by a conventional dry pressing preparation method, which can be reduced. The cost of producing a metal soft magnetic material by a conventional metal injection molding process can improve the dimensional stability of the metal soft magnetic material produced by metal injection molding, and the yield is not high.

S1~S4‧‧‧步驟S1~S4‧‧‧ steps

圖1,為本發明之步驟流程示意圖。FIG. 1 is a schematic flow chart of the steps of the present invention.

S1~S4‧‧‧步驟 S1~S4‧‧‧ steps

Claims (18)

一種高密度粉末冶金金屬軟磁材料的製備方法,其包含以下步驟: S1:提供一含鐵且具金屬軟磁性質的起始粉末,該起始粉末平均粒徑介於1微米至15微米之間,且鐵的來源為一羰基鐵粉; S2:利用一噴霧造粒製程自該起始粉末取得一噴霧造粒粉末,該噴霧造粒粉末具有一接近球形之粉末形貌且平均粒徑介於40微米至100微米之間; S3:將該噴霧造粒粉末置入一模具中,並令該噴霧造粒粉末維持在一介於20℃至150℃的成形溫度下接受一介於300MPa至1000MPa之間的成形壓力而形成一胚體;以及 S4:將該胚體加熱至1100℃至1400℃之間並於一保護氣氛中予以燒結而得到一金屬軟磁材料。A method for preparing a high-density powder metallurgy metal soft magnetic material, comprising the steps of: S1: providing an iron-containing and metal soft magnetic starting powder, the starting powder having an average particle diameter of between 1 micrometer and 15 micrometers, And the source of iron is a carbonyl iron powder; S2: a spray granulation powder is obtained from the starting powder by a spray granulation process, the spray granulated powder has a nearly spherical powder morphology and an average particle size of 40 Between micrometers and 100 micrometers; S3: placing the spray granulated powder in a mold, and maintaining the spray granulated powder at a forming temperature of between 20 ° C and 150 ° C to receive a flow between 300 MPa and 1000 MPa Forming pressure to form an embryo body; and S4: heating the body body to between 1100 ° C and 1400 ° C and sintering in a protective atmosphere to obtain a metal soft magnetic material. 如申請專利範圍第1項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之成分包括鐵與至少一添加元素,該添加元素選自於磷、矽、鈷、釩、鎳、鉬及其組合所組成之群組。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 1, wherein the component of the starting powder comprises iron and at least one additive element selected from the group consisting of phosphorus, antimony, cobalt, vanadium, A group of nickel, molybdenum, and combinations thereof. 如申請專利範圍第1項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末選自於元素粉、化合物粉及母合金粉所組成之群組。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 1, wherein the starting powder is selected from the group consisting of elemental powder, compound powder and master alloy powder. 如申請專利範圍第1項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中於步驟S4中,該保護氣氛係一真空環境或一還原氣氛,該還原氣氛選自於氫氣、裂解氨、氬氣及氮氣所組成之群組。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 1, wherein in the step S4, the protective atmosphere is a vacuum environment or a reducing atmosphere, and the reducing atmosphere is selected from the group consisting of hydrogen, pyrolysis ammonia, A group consisting of argon and nitrogen. 如申請專利範圍第2項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之磷的重量百分比介於0.4 wt.%至0.9 wt.%之間,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 2, wherein the weight percentage of phosphorus of the starting powder is between 0.4 wt.% and 0.9 wt.%, and the balance is iron and not Avoid impurities. 如申請專利範圍第2項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之矽的重量百分比介於2 wt.%至6 wt.%之間,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 2, wherein the weight percentage of the starting powder is between 2 wt.% and 6 wt.%, and the balance is iron and not Avoid impurities. 如申請專利範圍第2項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之鈷的重量百分比介於48 wt.%至52 wt.%之間,釩的重量百分比低於3 wt.%,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 2, wherein the weight percentage of cobalt of the starting powder is between 48 wt.% and 52 wt.%, and the weight percentage of vanadium is low. At 3 wt.%, the balance is iron and unavoidable impurities. 如申請專利範圍第2項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之鎳的重量百分比介於48 wt.%至52 wt.%之間,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 2, wherein the weight percentage of nickel of the starting powder is between 48 wt.% and 52 wt.%, and the balance is iron and not Avoid impurities. 如申請專利範圍第2項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之鎳的重量百分比介於77 wt.%至83 wt.%之間,鉬的重量百分比低於5 wt.%,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 2, wherein the weight percentage of nickel of the starting powder is between 77 wt.% and 83 wt.%, and the weight percentage of molybdenum is low. At 5 wt.%, the balance is iron and unavoidable impurities. 如申請專利範圍第1項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該羰基鐵粉的碳含量小於0.05 wt.%。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 1, wherein the carbonyl iron powder has a carbon content of less than 0.05 wt.%. 一種高密度粉末冶金金屬軟磁材料的製備方法,其包含以下步驟: S1:提供一含鐵且具金屬軟磁性質的起始粉末,該起始粉末平均粒徑介於1微米至15微米之間,且該起始粉末為一預合金粉; S2:利用一噴霧造粒製程自該起始粉末取得一噴霧造粒粉末,該噴霧造粒粉末具有一接近球形之粉末形貌且平均粒徑介於40微米至100微米之間; S3:將該噴霧造粒粉末置入一模具中,並令該噴霧造粒粉末維持在一介於20℃至150℃之間的成形溫度下接受一介於300MPa至1000MPa之間的成形壓力而形成一胚體;以及 S4:將該胚體加熱至1100℃至1400℃之間並於一保護氣氛中予以燒結而得到一金屬軟磁材料。A method for preparing a high-density powder metallurgy metal soft magnetic material, comprising the steps of: S1: providing an iron-containing and metal soft magnetic starting powder, the starting powder having an average particle diameter of between 1 micrometer and 15 micrometers, And the starting powder is a pre-alloyed powder; S2: obtaining a spray granulated powder from the starting powder by a spray granulation process, the spray granulated powder having a nearly spherical powder morphology and an average particle diameter Between 40 micrometers and 100 micrometers; S3: placing the spray granulated powder in a mold, and maintaining the spray granulated powder at a forming temperature between 20 ° C and 150 ° C to receive a range of 300 MPa to 1000 MPa Forming pressure between the forming body; and S4: heating the body to between 1100 ° C and 1400 ° C and sintering in a protective atmosphere to obtain a metal soft magnetic material. 如申請專利範圍第11項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之成分包括鐵與至少一添加元素,該添加元素選自於磷、矽、鈷、釩、鎳、鉬及其組合所組成之群組。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 11, wherein the component of the starting powder comprises iron and at least one additive element selected from the group consisting of phosphorus, antimony, cobalt, vanadium, A group of nickel, molybdenum, and combinations thereof. 如申請專利範圍第11項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中於步驟S4中,該保護氣氛係一真空環境或一還原氣氛,該還原氣氛選自於氫氣、裂解氨、氬氣及氮氣所組成之群組。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 11, wherein in the step S4, the protective atmosphere is a vacuum environment or a reducing atmosphere, and the reducing atmosphere is selected from the group consisting of hydrogen, pyrolysis ammonia, A group consisting of argon and nitrogen. 如申請專利範圍第12項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之磷的重量百分比介於0.4 wt.%至0.9 wt.%之間,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 12, wherein the weight percentage of phosphorus of the starting powder is between 0.4 wt.% and 0.9 wt.%, and the balance is iron and not Avoid impurities. 如申請專利範圍第12項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之矽的重量百分比介於2 wt.%至6 wt.%之間,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 12, wherein the weight percentage of the starting powder is between 2 wt.% and 6 wt.%, and the balance is iron and not Avoid impurities. 如申請專利範圍第12項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之鈷的重量百分比介於48 wt.%至52 wt.%之間,釩的重量百分比低於3 wt.%,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 12, wherein the weight percentage of cobalt of the starting powder is between 48 wt.% and 52 wt.%, and the weight percentage of vanadium is low. At 3 wt.%, the balance is iron and unavoidable impurities. 如申請專利範圍第12項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之鎳的重量百分比介於48 wt.%至52 wt.%之間,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 12, wherein the weight percentage of nickel of the starting powder is between 48 wt.% and 52 wt.%, and the balance is iron and not Avoid impurities. 如申請專利範圍第12項所述之高密度粉末冶金金屬軟磁材料的製備方法,其中該起始粉末之鎳的重量百分比介於77 wt.%至83 wt.%之間,鉬的重量百分比低於5 wt.%,其餘為鐵及不可避免之雜質。The method for preparing a high-density powder metallurgy metal soft magnetic material according to claim 12, wherein the weight percentage of nickel of the starting powder is between 77 wt.% and 83 wt.%, and the weight percentage of molybdenum is low. At 5 wt.%, the balance is iron and unavoidable impurities.
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