TWI728913B - Method of fabricating modified ferrite magnetic powder and method of fabricating modified ferrite magnet - Google Patents
Method of fabricating modified ferrite magnetic powder and method of fabricating modified ferrite magnet Download PDFInfo
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本發明係關於一種磁粉與磁石的製造方法，特別是關於一種改質鐵氧體磁粉的製造方法及改質鐵氧體磁石的製造方法。The present invention relates to a method for manufacturing magnetic powder and magnets, in particular to a method for manufacturing modified ferrite magnetic powder and a method for manufacturing modified ferrite magnet.
近年來，隨著電子零部件的小型化、輕量化以及高性能化，對於由氧化物構成的永磁鐵氧體磁體，也不斷要求具有較高的磁氣特性。作為永磁鐵氧體磁體的磁氣特性之指標一般以剩磁(B r)以及矯頑磁力( iH c)作為指標。一直以來，為了達到高剩磁與高矯頑磁力的特性，永磁鐵氧體磁體中的元素成分組成之探討一直在進行著。 In recent years, with the reduction in size, weight, and performance of electronic components, permanent ferrite magnets made of oxides are also required to have high magnetic properties. As an indicator of the magnetic properties of permanent ferrite magnets, remanence (B r ) and coercive force ( i H c ) are generally used as indicators. In order to achieve the characteristics of high remanence and high coercivity, the composition of elements in permanent ferrite magnets has been discussed.
另外，永磁鐵氧體磁體除了具有高剩磁與高矯頑磁力之外，矩形度(Sauareness ratio)也要盡可能的高(矩形度為：在90%的B r的時候，其磁場值(H k)相對於 iH c之比例。即，如果H k/ iH c高的話，則由外部磁場和溫度變化所引起的退磁(Demagnetization)就會比較小，也代表磁體本身的磁場配向度較高，因此能夠得到更穩定的磁氣特性。除此之外，另一個永磁鐵氧體磁體生產上的指標則是需達到減少磁體於磁場成型後之生胚產生裂紋或是燒結製程中磁體出現缺陷機率，以進一步提高永磁鐵氧體磁體量產之良率。然而，現有的永磁鐵氧體磁體的製造方法並無法同時達成上述對於磁氣性質與量產良率的要求。 In addition, permanent magnet ferrite magnets have high remanence and high coercivity, but also the Sauareness ratio should be as high as possible (rectangularity is: at 90% of B r , the magnetic field value ( The ratio of H k ) to i H c . That is, if H k / i H c is high, the demagnetization caused by the external magnetic field and temperature changes will be relatively small, which also represents the magnetic field alignment of the magnet itself It is higher, so more stable magnetic characteristics can be obtained. In addition, another indicator for the production of permanent ferrite magnets is to reduce the occurrence of cracks in the green embryo after the magnet is formed in the magnetic field or the magnet during the sintering process. The probability of occurrence of defects can further improve the yield of permanent ferrite magnets in mass production. However, the existing manufacturing methods of permanent ferrite magnets cannot simultaneously meet the above requirements for magnetic properties and mass production yield.
現有文獻中提到(例如中國發明專利申請第CN102473499A號與美國發明專利申請第US20140361214號)，要同時達到高剩磁(B r)、矯頑磁力( iH c)的同時要達到高矩形度(H k/ iH c)，需分別於製程中的微粉碎階段加入含有磷(P)之氧化物。 It is mentioned in the existing literature (for example, Chinese Invention Patent Application No. CN102473499A and U.S. Invention Patent Application No. US20140361214) that both high remanence (B r ) and coercivity ( i H c ) must be achieved while achieving high rectangularity (H k / i H c ), the oxide containing phosphorus (P) needs to be added in the fine pulverization stage of the manufacturing process.
另外，現有文獻提到(例如日本發明專利申請第JP2005336037A號與日本發明專利申請第JPH0669056A號)，要達到較佳的剩磁(B r)、矯頑磁力( iH c)等磁特性，會藉由將濕式微粉碎後的平均磁粉粒徑控制在0.7μm以下，以達到燒結後磁石之較高單磁區晶粒比例來使得磁石磁特性提升(一般來說，微粉碎後磁粉於成型、燒結後，磁粉晶粒會成長2~3倍，若磁粉晶粒於燒結後成長過多，則會超出單磁區臨界晶粒尺寸，而呈現多磁區晶粒狀態，進而造成磁特性下降)。因此若欲達到較高的燒結後磁石單磁區晶粒比例，過往的做法都會將微粉碎後平均磁粉粒徑控制的較小 (一般都是＜0.7μm)，以避免燒結後磁粉晶粒尺寸超出單磁區晶粒臨界尺寸，而永磁鐵氧磁體的單磁區晶粒尺寸則取決於永磁鐵氧體磁體材料配方組成。但是，這種作法反而會造成濕式異方向磁場成型時排水時間較久，排水難度較高，進而影響到成型良率、整體磁石良率以及提高了生產成本。 In addition, the existing literature mentions (for example, Japanese Invention Patent Application No. JP2005336037A and Japanese Invention Patent Application No. JPH0669056A) that to achieve better magnetic properties such as remanence (B r ) and coercive force ( i H c ), it will By controlling the average particle size of the wet finely pulverized magnetic powder to less than 0.7μm, in order to achieve a higher single-magnetic domain grain ratio of the sintered magnet, the magnetic properties of the magnet are improved (generally speaking, the magnetic powder after fine pulverization is formed, After sintering, the magnetic powder grains will grow by 2~3 times. If the magnetic powder grains grow too much after sintering, it will exceed the critical grain size of a single magnetic region and present a multi-magnetic region grain state, which will cause the magnetic properties to decrease). Therefore, if you want to achieve a higher ratio of sintered magnet single magnetic region grains, the previous method will control the average particle size of the finely pulverized magnetic powder to be smaller (usually <0.7μm) to avoid the sintered magnetic powder grain size Beyond the critical size of the single magnetic zone grains, the single magnetic zone grain size of the permanent magnet ferrite magnet depends on the composition of the permanent magnet ferrite magnet material. However, this method will cause longer drainage time and difficulty of drainage during wet-type different-directional magnetic field molding, which in turn affects the molding yield, the overall magnet yield, and increases the production cost.
上述的排水時間會較久的原因在於，永磁鐵氧體的濕式異方向磁場成型製程過程中，通常會將瓷漿中的水分排掉，濕式異方向磁場成型機之成型模具上模中設計有排水口與排水通道，可於成型過程中將瓷漿中的水分排掉。而通常會在成型機之成型模具上模裝上濾布及濾紙，濾布及濾紙可避免排水過程中一些較細小的磁粉被排水泵浦抽走，而造成排水口堵塞，濾布的裝設也可以進一步提升成型的良率。一般而言，濾紙每完成一模生胚的成型就會換過一次(以捲軸式自動更換)；濾布則可於每成型40~80模次再進行更換。然而，於微粉碎過程中所產生的過於細小的超微細粉(例如粒徑小於0.1微米)，會很容易於上述的成型排水過程中堵塞住濾布、濾紙的孔隙，進而導致成型模具上模中的排水口堵塞，最終會衍伸出成型時間過久、成型良率偏低、整體磁石良率下降等問題。這些超微細粉也會造成成型過程中磁場配向度偏低，進而導致磁特性剩磁(B r)、矯頑磁力( iH c)變差等不理想效應。 The reason for the longer drainage time mentioned above is that in the process of wet different-directional magnetic field forming process of permanent magnet ferrite, the water in the porcelain slurry is usually drained out, and it is in the upper mold of the wet-type different-directional magnetic field forming machine. Designed with drainage ports and drainage channels, which can drain the water in the porcelain slurry during the molding process. Usually, filter cloth and filter paper are installed on the mold of the forming machine. The filter cloth and filter paper can prevent some of the smaller magnetic particles from being drawn away by the drainage pump during the drainage process, causing the drainage port to be blocked, and the installation of the filter cloth The yield rate of molding can also be further improved. Generally speaking, the filter paper will be replaced every time a mold is formed (automatically replaced by a reel); the filter cloth can be replaced every 40 to 80 molds. However, the ultra-fine ultra-fine powder (for example, the particle size less than 0.1 micron) produced during the micro-pulverization process will easily block the pores of the filter cloth and filter paper during the above-mentioned molding and drainage process, which will lead to the upper mold of the molding die. Blockage of the drainage port in the middle will eventually cause problems such as too long molding time, low molding yield, and overall magnet yield decline. These ultra-fine powders can also cause the magnetic field alignment to be low during the molding process, which in turn leads to undesirable effects such as the remanence (B r ) of the magnetic properties and the deterioration of the coercive force (i H c ).
由上可知，已知的研究主要是針對濕式異方向磁場的磁石製造法，其並未針對乾式等方向磁場配向法進行研究。It can be seen from the above that the known research mainly focuses on the magnet manufacturing method of the wet different-directional magnetic field, and it has not conducted the research on the dry iso-directional magnetic field alignment method.
故，有必要提供一種改質鐵氧體磁粉的製造方法及改質鐵氧體磁石的製造方法，以解決習用技術所存在的問題。Therefore, it is necessary to provide a method for manufacturing modified ferrite magnetic powder and a method for manufacturing modified ferrite magnet to solve the problems existing in the conventional technology.
本發明之一目的在於提供一種改質鐵氧體磁粉的製造方法及改質鐵氧體磁石的製造方法，其係透過使用特定的組成物以及特定的煅燒溫度，以製得具有優良磁特性與高良率的產品，並且具有簡化材料配方複雜度、提高製程穩定性且降低生產成本的優點。One of the objects of the present invention is to provide a method for manufacturing modified ferrite magnetic powder and a method for manufacturing modified ferrite magnets, which are prepared by using a specific composition and a specific calcination temperature to have excellent magnetic properties and High-yield products, and have the advantages of simplifying material formulation complexity, improving process stability and reducing production costs.
為達上述之目的，本發明提供一種改質鐵氧體磁粉的製造方法，包含步驟：提供一混合物，其中該混合物包含一氧化鐵粉及一鋇化物；進行一煅燒步驟，對該混合物以1090至1100℃之間的溫度持溫達50至70分鐘之間，以形成一前處理物；以及進行一粉碎步驟，對該前處理物進行粉碎，以獲得該改質鐵氧體磁粉，其中該改質鐵氧體磁粉的一平均粒徑介於1.2至1.4微米之間。In order to achieve the above objective, the present invention provides a manufacturing method of modified ferrite magnetic powder, which includes the steps of: providing a mixture, wherein the mixture includes an iron oxide powder and a barium compound; Hold the temperature between 1100°C and 1100°C for 50 to 70 minutes to form a pre-processed object; and perform a pulverization step to pulverize the pre-processed object to obtain the modified ferrite magnetic powder, wherein An average particle size of the modified ferrite magnetic powder is between 1.2 and 1.4 microns.
在本發明一實施例中，該前處理物的一分子式係BaO．n(Fe 2O 3)，其中n介於5至6之間。 In an embodiment of the present invention, a molecular formula of the pretreatment is BaO. n(Fe 2 O 3 ), where n is between 5 and 6.
在本發明一實施例中，在提供該混合物的步驟中，更包含：提供一添加劑，其中該添加劑更包含碳酸鈣及氧化矽，並且以該混合物的一總重為100重量份計，碳酸鈣係介於0.1至0.5重量份之間；以及氧化矽係介於0.2至1.0重量份之間。In an embodiment of the present invention, the step of providing the mixture further includes: providing an additive, wherein the additive further includes calcium carbonate and silica, and based on a total weight of the mixture as 100 parts by weight, the calcium carbonate It is between 0.1 and 0.5 parts by weight; and the silicon oxide is between 0.2 and 1.0 parts by weight.
在本發明一實施例中，該煅燒步驟的一氣氛係包含5%的氧氣。In an embodiment of the present invention, an atmosphere of the calcination step contains 5% oxygen.
在本發明一實施例中，該粉碎步驟更包含：進行一粗粉碎子步驟，其中該粗粉碎子步驟係粗粉碎該前處理物，以使該前處理物的該平均粒徑介於4至6微米之間；以及進行一細粉碎子步驟，其中該細粉碎子步驟係細粉碎經該粗粉碎子步驟後的該前處理物，以使該改質鐵氧體磁粉的該平均粒徑介於1.2至1.4微米之間。In an embodiment of the present invention, the pulverization step further comprises: performing a coarse pulverization sub-step, wherein the coarse pulverization sub-step is to coarsely pulverize the pre-treatment object, so that the average particle size of the pre-treatment object is between 4 and 6 microns; and a fine pulverization sub-step, wherein the fine pulverization sub-step is to finely pulverize the pre-treatment after the coarse pulverization sub-step, so that the average particle size of the modified ferrite magnetic powder is medium Between 1.2 and 1.4 microns.
在本發明一實施例中，該氧化鐵粉的一平均粒徑介於1至1.1微米之間。In an embodiment of the present invention, an average particle size of the iron oxide powder is between 1 and 1.1 microns.
在本發明一實施例中，該鋇化物包含碳酸鋇。In an embodiment of the present invention, the barium compound includes barium carbonate.
為達上述之目的，本發明提供一種改質鐵氧體磁石的製造方法，其包含步驟：提供一改質鐵氧體磁粉，其中該改質鐵氧體磁粉係通過如上任一實施例所述之改質鐵氧體磁粉的製造方法所製成；對該改質鐵氧體磁粉進行一造粒步驟，加入濃度約10至20wt%的一黏結劑至該改質鐵氧體磁粉中以形成一黏結物，其中以該黏結物的總重為100wt%，該黏結物中的該黏結劑的固含量為5至7wt%之間；對該黏結物進行一磁場配向成型步驟，以形成一胚體，其中該磁場配向成型步驟的一配向磁場強度係介於1.3至1.7特斯拉之間，一成型壓力係介於2至4噸/平方公分之間，以及一成型時間係介於4.5至6.5秒之間；以及進行一燒結步驟，對該胚體以介於1190至1210℃之間的溫度持續燒結達50至70分鐘之間，以製得該改質鐵氧體磁石。In order to achieve the above objective, the present invention provides a method for manufacturing a modified ferrite magnet, which includes the steps of: providing a modified ferrite magnetic powder, wherein the modified ferrite magnetic powder is obtained by the method described in any of the above embodiments. The modified ferrite magnetic powder is produced by the method for manufacturing the modified ferrite magnetic powder; a granulation step is performed on the modified ferrite magnetic powder, and a binder with a concentration of about 10 to 20 wt% is added to the modified ferrite magnetic powder to form A binder, wherein the total weight of the binder is 100% by weight, and the solid content of the binder in the binder is between 5 and 7% by weight; a magnetic field alignment molding step is performed on the binder to form an embryo In the magnetic field alignment forming step, an alignment magnetic field intensity is between 1.3 and 1.7 Tesla, a forming pressure is between 2 and 4 tons/cm², and a forming time is between 4.5 and 6.5 seconds; and a sintering step is performed to continue sintering the green body at a temperature between 1190 and 1210° C. for between 50 and 70 minutes to obtain the modified ferrite magnet.
在本發明一實施例中，該黏結劑的材質包含聚乙烯醇。In an embodiment of the present invention, the material of the adhesive includes polyvinyl alcohol.
在本發明一實施例中，該磁場配向成型步驟係以一乾式等方向磁場配向法進行。In an embodiment of the present invention, the magnetic field alignment forming step is performed by a dry isotropic magnetic field alignment method.
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。In order to make the above and other objectives, features, and advantages of the present invention more obvious and understandable, the preferred embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings. Furthermore, the directional terms mentioned in the present invention, such as up, down, top, bottom, front, back, left, right, inside, outside, side, surrounding, center, horizontal, horizontal, vertical, vertical, axial, The radial direction, the uppermost layer or the lowermost layer, etc., are only the direction of reference to the attached drawings. Therefore, the directional terms used are used to describe and understand the present invention, rather than to limit the present invention.
請參照第1圖所示，本發明一實施例之改質鐵氧體磁粉的製造方法10主要包含下列步驟11至13：提供一混合物，其中該混合物包含一氧化鐵粉及一鋇化物(步驟11)；進行一煅燒步驟，對該混合物以1090至1100℃之間的溫度持溫達50至70分鐘之間，以形成一前處理物(步驟12)；以及進行一粉碎步驟，對該前處理物進行粉碎，以獲得該改質鐵氧體磁粉，其中該改質鐵氧體磁粉的一平均粒徑介於1.2至1.4微米之間(步驟13)。本發明將於下文逐一詳細說明實施例之上述各步驟的實施細節及其原理。Please refer to Figure 1, the
本發明一實施例之改質鐵氧體磁粉的製造方法10首先係步驟11：提供一混合物，其中該混合物包含一氧化鐵粉及一鋇化物。在本步驟11中，該氧化鐵粉例如可以是一市售產品，亦可以是一鋼鐵製程中所產生的副產品，例如鋼鐵在進行熱加工時需將鐵表面所生成的鐵銹去除，而該鐵銹可作為該氧化鐵粉的來源。在一範例中，該氧化鐵粉的一平均粒徑介於1至1.1微米之間。在一實施例中，該鋇化物例如可包含碳酸鋇(BaCO
3)。值得一提的是，所提供的該混合物主要用於生成鋇系鐵氧體磁粉。
The
在一實施例，在提供該混合物的步驟中，更包含：提供一添加劑，該添加劑包含碳酸鈣(CaCO 3)及氧化矽(SiO 2)中的至少一種。以下說明各種添加劑的效果，其中所涉及的重量百分比皆是以該混合物的總重為100重量份計為基准。在一實施例中，氧化鐵粉(Fe 2O 3)、鋇化物、碳酸鈣(CaCO 3)及氧化矽(SiO 2)可以透過研磨機(Attritor)進行乾式混磨約1小時(料球重量比約1:5，鋼球可使用直徑約3/16英吋的無鉻軸承鋼球)，以得到均質混合的粉體混合物。 In one embodiment, the step of providing the mixture further includes: providing an additive. The additive includes at least one of calcium carbonate (CaCO 3 ) and silicon oxide (SiO 2 ). The effects of various additives are described below, and the weight percentages involved are all based on the total weight of the mixture as 100 parts by weight. In one embodiment, iron oxide powder (Fe 2 O 3 ), barium compound, calcium carbonate (CaCO 3 ), and silicon oxide (SiO 2 ) can be dry-mixed through a grinder (Attritor) for about 1 hour (ball weight The ratio is about 1:5, and the steel ball can use a chromium-free bearing steel ball with a diameter of about 3/16 inches) to obtain a homogeneously mixed powder mixture.
碳酸鈣是一種用於促進晶粒成長的元素，於本發明中碳酸鈣之添加量例如介於0.1至0.5重量份之間(例如是0.15、0.2、0.26、0.3、0.35、0.4或0.46重量份)，當碳酸鈣添加量過多的時候(例如大於0.5重量份)，後續形成鐵氧體磁石所進行的燒結步驟中，會發生過量的晶粒增長，而導致矯頑磁力的降低。另一方面，當加入的碳酸鈣之添加量過少的時候(例如小於0.1重量份)，晶粒增長的現象會被過度抑制，進而導致與晶粒增長同時發生的取向的提高不足，最終導致剩磁(B r)低落。 Calcium carbonate is an element used to promote the growth of crystal grains. The amount of calcium carbonate added in the present invention is, for example, between 0.1 to 0.5 parts by weight (for example, 0.15, 0.2, 0.26, 0.3, 0.35, 0.4 or 0.46 parts by weight) ), when calcium carbonate is added in an excessive amount (for example, greater than 0.5 parts by weight), excessive grain growth will occur in the subsequent sintering step for forming ferrite magnets, resulting in a decrease in coercivity. On the other hand, when the added amount of calcium carbonate is too small (for example, less than 0.1 parts by weight), the phenomenon of crystal grain growth will be excessively suppressed, which in turn leads to insufficient increase in orientation that occurs at the same time as the crystal grain growth, and ultimately leads to residual Magnetism (B r ) is low.
氧化矽之添加則是用來消除燒結時的晶粒增長，本發明中之氧化矽的添加量例如介於0.2至1.0重量份之間(例如是0.3、0.4、0.5、0.52、0.6、0.7、0.8或0.9重量份)。當加入的氧化矽過少時(例如小於0.2重量份)，在燒結階段會發生過量的晶粒增長，而導致矯頑磁力降低。當加入的氧化矽過多時(例如大於1.0重量份)，在燒結階段之晶粒增長會過度消除，而導致與晶粒增長同時發生的取向之改進不足，最終而導致剩磁(B r)的下降。 The addition of silicon oxide is used to eliminate grain growth during sintering. The addition amount of silicon oxide in the present invention is, for example, between 0.2 and 1.0 parts by weight (for example, 0.3, 0.4, 0.5, 0.52, 0.6, 0.7, 0.8 or 0.9 parts by weight). When the added silicon oxide is too small (for example, less than 0.2 parts by weight), excessive grain growth will occur during the sintering stage, resulting in a decrease in coercivity. When too much silicon oxide is added (for example, more than 1.0 part by weight), the grain growth in the sintering stage will be excessively eliminated, resulting in insufficient orientation improvement that occurs at the same time as the grain growth, and ultimately resulting in remanence (B r ) decline.
本發明一實施例之改質鐵氧體磁粉的製造方法10接著係步驟12：進行一煅燒步驟，對該混合物以1090至1100℃之間的溫度持溫達50至70分鐘之間，以形成一前處理物。在本步驟12中，該煅燒步驟主要是使用於特定的溫度範圍，以使該混合物適於應用在後續的磁性產品的相關製程。若是溫度過低(例如小於1090℃)或溫度過高(例如大於1100℃)，皆無法達成上述本發明的優點及目的，例如無法製得具有優良磁特性與高良率的產品，並且不具有簡化材料配方複雜度、提高製程穩定性且降低生產成本的優點。詳細的實驗分析結果將在後面段落介紹。在另一實施例中，該前處理物的一分子式係BaO．n(Fe
2O
3)，其中n介於5至6之間(例如5.1、5.2、5.3、5.4、5.5、5.6、5.7、5.8或5.9)。在又一實施例中，進行該煅燒步驟處理時的一氣氛係包含約5%的氧氣。
The
本發明一實施例之改質鐵氧體磁粉的製造方法10接著係步驟13：進行一粉碎步驟，對該前處理物進行粉碎，以獲得該改質鐵氧體磁粉，其中該改質鐵氧體磁粉的一平均粒徑介於1.2至1.4微米之間。在本步驟13中，該粉碎步驟例如可以是分兩階段或多階段進行，以使該前處理物的一平均粒徑介於0.7至0.75微米之間。在一實施例中，該粉碎步驟包含：進行一粗粉碎子步驟，其中該粗粉碎子步驟係粗粉碎該前處理物，以使該前處理物的該平均粒徑介於4至6微米之間；以及進行一細粉碎子步驟，其中該細粉碎子步驟係細粉碎經該粗粉碎子步驟後的該前處理物，以使該改質鐵氧體磁粉的該平均粒徑介於1.2至1.4微米之間。The
這邊要提到的是，一般而言，該前處理物的一平均粒徑越小，磁氣特性越佳。但是，該前處理物中粒徑過小的部分(即大於0且小於等於0.1微米的粒徑的部分，其無法使用費氏粒徑分析儀(Fisher subsieve sizer)進行精確量測)反而有害於磁氣特性與成型良率。具體而言，粒徑過小的部分的該前處理物容易在後續燒結步驟中產生非磁性相，進而有害於磁氣特性。此外，這些磁粉中所存在粒子徑小於0.1μm的超微細粉對於生胚之成型也有很大的阻礙，因此使得成型所需壓力較大，容易導致生胚成型時間過久或是成型生坯出現裂紋，進而導致成型良率下降等現象。換言之，本發明就是藉由使用特定組成及特定參數的步驟，以減少粉碎後之磁粉中存在粒子徑小於0.1μm的超微細粉，有助於提高剩磁(B r)及矩形度(H k/ iH c)等磁性質，並且具有簡化材料配方複雜度、提高製程穩定性且降低生產成本的優點。 What I want to mention here is that, generally speaking, the smaller the average particle size of the pre-processed product, the better the magnetic properties. However, the part of the pretreatment with too small particle size (that is, the part with a particle size greater than 0 and less than or equal to 0.1 micron, which cannot be accurately measured with a Fisher subsieve sizer) is harmful to the magnetic field. Gas characteristics and molding yield. Specifically, the pre-processed product with an excessively small particle size is likely to generate a non-magnetic phase in the subsequent sintering step, which is harmful to the magnetic properties. In addition, the ultra-fine powders with particle diameters less than 0.1μm in these magnetic powders also hinder the molding of the green embryo. Therefore, the pressure required for the molding is relatively large, which easily leads to too long molding time of the green embryo or the appearance of the green body. Cracks, which in turn lead to phenomena such as a decrease in molding yield. In other words, the present invention is to reduce the existence of ultrafine particles with particle diameters less than 0.1μm in the pulverized magnetic powder by using the steps of specific composition and specific parameters, which helps to improve the remanence (B r ) and squareness (H k / i H c ) and other magnetic properties, and has the advantages of simplifying material formulation complexity, improving process stability and reducing production costs.
請參照第2圖，本發明另一實施例提出一種改質鐵氧體磁石的製造方法20，其包含步驟21至24：提供一改質鐵氧體磁粉，其中該改質鐵氧體磁粉係如上所述任一實施例的改質鐵氧體磁粉的製造方法所製成(步驟21)；對該改質鐵氧體磁粉進行一造粒步驟，加入濃度約10至20wt%的一黏結劑至該改質鐵氧體磁粉中以形成一黏結物，其中以該黏結物的總重為100wt%，該黏結物中的該黏結劑的固含量為5至7wt%之間(步驟22)；對該黏結物進行一磁場配向成型步驟，以形成一胚體，其中該磁場配向成型步驟的一配向磁場強度係介於1.3至1.7特斯拉之間，一成型壓力係介於2至4噸/平方公分之間，以及一成型時間係介於4.5至6.5秒之間(步驟23)；以及進行一燒結步驟，對該胚體以介於1190至1210℃之間的溫度持續燒結達50至70分鐘之間，以製得該改質鐵氧體磁石(步驟24)。本發明將於下文逐一詳細說明實施例之上述各步驟的實施細節及其原理。Referring to FIG. 2, another embodiment of the present invention provides a
本發明一實施例之改質鐵氧體磁石的製造方法20首先係步驟21：提供一改質鐵氧體磁粉，其中該改質鐵氧體磁粉係如上所述任一實施例的改質鐵氧體磁粉的製造方法所製成。在本步驟21中，通過上述的改質鐵氧體磁粉的製造方法10製成該改質鐵氧體磁粉。The
本發明一實施例之改質鐵氧體磁石的製造方法20接著係步驟22：對該改質鐵氧體磁粉進行一造粒步驟，加入濃度約10至20wt%的一黏結劑至該改質鐵氧體磁粉中以形成一黏結物，其中以該黏結物的總重為100wt%，該黏結物中的該黏結劑的固含量為5至7wt%之間。在本步驟22中，該黏結劑的材質例如包含聚乙烯醇(PVA)。在一實施例中，例如將進行粉碎步驟後的磁粉中加入之PVA (聚乙烯醇)水溶液(濃度15wt%)。接著，在混合過程中調整至整體PVA的固含量約為6wt%(即純PVA的固含量佔黏結物整體為6wt%)之黏結物，以高速混合機進行攪拌混合。混合後，再進行烘乾步驟以去除磁粉中過多的水份。於烘乾步驟後，再進行過篩步驟，留下平均磁粉粒度達到1.2至1.4μm之磁粉，以進行後續之磁場成型配向成型步驟。The
本發明一實施例之改質鐵氧體磁石的製造方法20接著係步驟23：對該黏結物進行一磁場配向成型步驟，以形成一胚體，其中該磁場配向成型步驟的一配向磁場強度係介於1.3至1.7特斯拉之間，一成型壓力係介於2至4噸/平方公分之間，以及一成型時間係介於4.5至6.5秒之間。在本步驟23中，主要是提供成型壓力與配向磁場，以使該改質鐵氧體磁粉成型為預定的形狀並且具有預定的磁場方向。這邊要提到的是，由於使用改質鐵氧體磁粉的製造方法10製成的該改質鐵氧體磁粉，故可使用較低的成型時間即可成型為胚體，並且具有優良的磁特性及優良的良率。在一實施例中，該磁場配向成型步驟係以一乾式等方向磁場配向法進行。The
本發明一實施例之改質鐵氧體磁石的製造方法20最後係步驟24：進行一燒結步驟，對該胚體以介於1190至1210℃之間的溫度持續燒結達50至70分鐘之間，以製得該改質鐵氧體磁石。在本步驟24中，主要是通過燒結步驟以使該胚體中的水分去除以製得改質鐵氧體磁石。The
這邊要提到的是，由於本發明實施例之改質鐵氧體磁石的製造方法20使用本發明實施例之改質鐵氧體磁粉的製造方法所製得的改質鐵氧體磁粉，其中該改質鐵氧體磁粉中的粒徑過小的部分較少。因此，在燒結步驟中不易產生非磁性相，並且在磁場配向成型步驟中所需壓力較小，生胚成型時間較短，成型生坯不易出現裂紋，進而導致成型良率高等優良效果。It should be mentioned here that since the
以下舉出數個實施例與比較例，以說明本發明實施例之改質鐵氧體磁粉的製造方法及本發明實施例之改質鐵氧體磁石的製造方法所製得的改質鐵氧體磁石確實具有上述的效果。Here are several examples and comparative examples to illustrate the method of manufacturing modified ferrite magnetic powder in the embodiment of the present invention and the modified ferrite produced by the method of manufacturing modified ferrite magnet in the embodiment of the present invention The bulk magnet does have the above-mentioned effects.
實施例1Example 1
首先，將氧化鐵粉(Fe 2O 3)、鋇化物(例如使用碳酸鋇(BaCO 3))以BaO．n(Fe 2O 3)之基本組成進行配料，其中氧化鐵粉(Fe 2O 3)的平均粒徑介於1至1.1微米之間(例如可通過費氏粒徑分析儀(fisher subsieve sizer確定D 50值來判斷)，n介於5至6之間(例如約5.4)。接著提供一添加劑，其中該添加劑更包含碳酸鈣及氧化矽，並且以該混合物的一總重為100重量份計，碳酸鈣係介於0.1至0.5重量份之間(例如使用約0.26重量份)；以及氧化矽係介於0.2至1.0重量份之間(例如使用約0.52重量份)。之後，將上述混合物及添加劑進行混合後，以料球重量比為1:5的市售研磨機(Attritor)混磨約1小時後出料(料球重量比約1:5，鋼球可使用直徑約3/16英吋的無鉻軸承鋼球)，以得到均質混合的粉體混合物。 First, the iron oxide powder (Fe 2 O 3 ), barium compound (for example, barium carbonate (BaCO 3 )) is BaO. The basic composition of n(Fe 2 O 3 ) is compounded, and the average particle size of iron oxide powder (Fe 2 O 3 ) is between 1 and 1.1 microns (for example, it can be determined by a fisher subsieve sizer D 50 value to determine), n is between 5 and 6 (for example, about 5.4). Then an additive is provided, wherein the additive further includes calcium carbonate and silicon oxide, and a total weight of the mixture is calculated as 100 parts by weight , The calcium carbonate is between 0.1 to 0.5 parts by weight (for example, about 0.26 parts by weight); and the silica is between 0.2 to 1.0 parts by weight (for example, about 0.52 parts by weight). Then, the above mixture and After the additives are mixed, use a commercially available grinder (Attritor) with a ball weight ratio of 1:5 to mix and grind for about 1 hour, and then discharge the material (the ball weight ratio is about 1:5, and the steel ball can be used with a diameter of about 3/16 inch. Inch chromium-free bearing steel balls) to obtain a homogeneously mixed powder mixture.
之後，將該混合物與添加劑放入一市售旋窯進行煅燒以形成一前處理物，煅燒溫度約為1090℃，煅燒時間約為1小時，且煅燒時旋窯內之氧氣含量約5%。After that, the mixture and additives are put into a commercially available rotary kiln for calcination to form a pre-treatment material. The calcination temperature is about 1090°C, the calcination time is about 1 hour, and the oxygen content in the rotary kiln is about 5% during calcination.
將經過旋窯煅燒之前處理物通過與旋窯相連結的溜管送入冷卻桶中進行冷卻。在前處理物的溫度降至適合的溫度以下(例如90℃以下)時，通過震動研磨機(vibration mill)進行粗粉碎子步驟，以使該前處理物的平均粒徑具有4至6μm之間的窄單峰粒徑分佈(以費氏粒徑分析儀量測)，其中在粗粉碎子步驟中所使用的研磨介質為直徑約為1cm的鐵條。The processed material before being calcined in the rotary kiln is sent to the cooling barrel for cooling through the chute connected with the rotary kiln. When the temperature of the pre-processed product falls below a suitable temperature (for example, 90°C or less), the coarse pulverization sub-step is performed by a vibration mill so that the average particle size of the pre-processed product is between 4 and 6 μm The narrow unimodal particle size distribution (measured by a Fischer particle size analyzer), wherein the grinding medium used in the coarse pulverization sub-step is an iron rod with a diameter of about 1 cm.
之後，再使用震動研磨機(vibration mill)進行細粉碎子步驟約1.5小時，以獲得改質鐵氧體磁粉，該改質鐵氧體磁粉的平均粒徑具有1.2至1.4μm之間的窄單峰粒徑分佈(以費氏粒徑分析儀量測)，其中在細粉碎子步驟中所使用的研磨介質為直徑約3/16英吋的無鉻軸承鋼球(以料球重量比約1:10進行)。After that, a vibration mill (vibration mill) is used to perform the fine pulverization sub-step for about 1.5 hours to obtain modified ferrite magnetic powder. The average particle size of the modified ferrite magnetic powder has a narrow particle size between 1.2 and 1.4 μm. Peak particle size distribution (measured with Fischer particle size analyzer), where the grinding medium used in the fine pulverization sub-step is a chromium-free bearing steel ball with a diameter of about 3/16 inches (the weight ratio of the ball is about 1 :10 proceed).
接著，對該改質鐵氧體磁粉進行一造粒步驟，加入濃度約10至20wt%的一黏結劑(例如PVA)至該改質鐵氧體磁粉中以形成一黏結物，其中以該黏結物的總重為100wt%，該黏結物中的該黏結劑的固含量為5至7wt%之間(例如約6wt%)。Next, a granulation step is performed on the modified ferrite magnetic powder, and a binder (such as PVA) with a concentration of about 10 to 20 wt% is added to the modified ferrite magnetic powder to form a binder, wherein the binder The total weight of the object is 100 wt%, and the solid content of the adhesive in the adhesive is between 5 and 7 wt% (for example, about 6 wt%).
接著，進行磁場配向成型步驟(例如乾式等方向磁場配向法)，使用市售的25噸之半自動乾式等方向磁場成型機，對該改質鐵氧體磁粉進行20顆胚體的磁場配向成型，配向磁場強度為1.5特斯拉(Telsa)，成型壓力為1.35噸/平方公分(Ton/cm 2)，成型胚件尺寸為長度約2cm、寬度約1cm、拱高約0.5cm、厚度約0.3cm的瓦片型胚體。於實施例1中，經成型20顆胚體之平均所需乾式磁場成型時間為6秒，胚體之平均良率為95%，生胚的密度為3.0g/cm 3。 Next, perform a magnetic field alignment molding step (such as dry isotropic magnetic field alignment method), using a commercially available 25-ton semi-automatic dry isotropic magnetic field molding machine to perform magnetic field alignment molding of 20 embryos of the modified ferrite powder. The alignment magnetic field strength is 1.5 Tesla (Telsa), the molding pressure is 1.35 tons/cm 2 (Ton/cm 2 ), and the size of the molded blank is about 2cm in length, 1cm in width, 0.5cm in arch height, and 0.3cm in thickness. The tile-shaped embryo body. In Example 1, the average dry magnetic field forming time required for forming 20 embryos is 6 seconds, the average yield of the embryos is 95%, and the density of the green embryos is 3.0 g/cm 3 .
最後，進行一燒結步驟，對該胚體以約1190至1210℃的溫度持續燒結達60分鐘，以製得實施例1之鐵氧體磁石。接著，利用市售儀器(中國計量科學研究院NIM-2000型 B-H Loop Tracer)量測實施例1，20顆鐵氧體磁石的各種磁氣性質，以及利用市售儀器量測磁石燒結密度，並且以平均值計算列於下表一。Finally, a sintering step is performed, and the green body is continuously sintered at a temperature of about 1190 to 1210° C. for 60 minutes to obtain the ferrite magnet of Example 1. Next, use a commercially available instrument (NIM-2000 BH Loop Tracer of the Chinese Academy of Metrology) to measure the various magnetic properties of the 20 ferrite magnets in Example 1, and to measure the sintered density of the magnet with a commercially available instrument, and The average value is calculated in Table 1 below.
表一
實施例2及比較例1至6Example 2 and Comparative Examples 1 to 6
實施例2及比較例1至6的製作方式大致上相同於實施例1，唯其不同之處在於：煅燒溫度不同；成型所需壓力不同；成型所需時間不同。之後，也對實施例2及比較例1至6進行如實施例1所進行的分析。The manufacturing methods of Example 2 and Comparative Examples 1 to 6 are substantially the same as Example 1, except that the difference lies in: the calcination temperature is different; the pressure required for molding is different; and the time required for molding is different. After that, the analysis performed in Example 1 was also performed on Example 2 and Comparative Examples 1 to 6.
根據實施例1與2及比較例1至6的分析結果可知，本發明在使用特定的原料的前提下，使用特定的煅燒溫度，可使所得到的磁石具備優良的磁特性，同時也具備極高的良率。According to the analysis results of Examples 1 and 2 and Comparative Examples 1 to 6, under the premise of using specific raw materials and using a specific calcination temperature, the obtained magnet can have excellent magnetic properties and also have extremely high magnetic properties. High yield.
具體而言，實施例1與實施例2之平均燒結密度分別已達5.01g/cm 3與5.02g/cm 3，相較於比較例1至6之燒結密度有相當明顯的提升，且其磁特性遠高於商用乾式等方向性成型磁石材之規格中值，且燒結磁石之矩形度(H k/ iH c)達41.3%與40.9% (商用材磁石規格: B r=2150±100G; bH c=1850±100Oe; iH c=3100±100Oe; (BH) max=1.2±0.1MGOe; H k/ iH c＞40%，其中規格中值一般指的是範圍中間值，例如商用材磁石規格中，B r之規格中值為2150G， bH c之規格中值為1850Oe， iH c之規格中值為3100Oe，(BH) max之規格中值為1.2MGOe)。換言之，從表一可知，使用本發明的製造方法所製得的磁石可使磁場配向程度提升。具體原因主要是，在實施例1與2中，永磁鐵氧體磁粉的煅燒溫度提高至1090至1100℃後，其主原料氧化鐵粉(Fe 2O 3)、碳酸鋇(BaCO 3)能夠起到更為完整的煅燒反應，因此煅燒後的磁粉硬度提升，使得煅燒料於細粉碎球磨製程中不易磨出＜0.1μm之過細的磁粉(此＜0.1μm之過細的磁粉無法以費氏粒徑分析儀(Fisher subsieve sizer)測得)，整體導致細粉碎球磨後所得到的磁粉之超微細磁粉比例下降，因此永磁鐵氧體磁粉於乾式等方向磁場成型過程中所需之成型壓力降低(相較於前述比較例1至4)、成型所需時間減少、成型性提高，因此成型良率、整體良率也都因此提升。此外，此煅燒反應提升之磁粉於製作成為磁石後，其整體磁特性均有改善，尤其對殘餘磁化強度(B r)影響較為明顯。 Specifically, the average sintered density of Example 1 and Example 2 have reached 5.01g/cm 3 and 5.02g/cm 3 , respectively. Compared with the sintered density of Comparative Examples 1 to 6, the sintered density has been significantly improved, and its magnetic The characteristics are much higher than the median specifications of commercial dry isotropic molded magnets, and the rectangularity (H k / i H c ) of the sintered magnet reaches 41.3% and 40.9% (commercial magnet specifications: B r = 2150 ± 100G; b H c =1850±100Oe; i H c =3100±100Oe; (BH) max =1.2±0.1MGOe; H k / i H c ＞40%, where the median value of the specification generally refers to the middle value of the range, such as commercial Among the material magnet specifications, the median specification of B r is 2150G, the median specification of b H c is 1850 Oe, the median specification of i H c is 3100 Oe, and the median specification of (BH) max is 1.2 MGOe). In other words, it can be seen from Table 1 that the magnet produced by the manufacturing method of the present invention can increase the degree of magnetic field alignment. The specific reason is mainly that, in Examples 1 and 2, after the calcination temperature of the permanent ferrite powder is increased to 1090 to 1100°C, the main raw material iron oxide powder (Fe 2 O 3 ) and barium carbonate (BaCO 3 ) can start In order to achieve a more complete calcination reaction, the hardness of the calcination magnetic powder increases, so that the calcined material is not easy to grind out too fine magnetic powder less than 0.1μm in the fine grinding ball milling process (this too fine magnetic powder less than 0.1μm cannot be As measured by the analyzer (Fisher subsieve sizer), the proportion of ultra-fine magnetic powder in the magnetic powder obtained after the fine pulverization and ball milling is reduced as a whole. Therefore, the molding pressure required for the permanent magnet ferrite powder in the dry iso-directional magnetic field molding process is reduced (corresponding to Compared with the aforementioned comparative examples 1 to 4), the molding time is reduced and the moldability is improved, so the molding yield and overall yield are also improved. In addition, the overall magnetic properties of the magnetic powder improved by the calcination reaction are improved after being made into a magnet, especially the residual magnetization (B r ) has a significant effect.
另一方面，比較例5與6使用高於實施例1與2的煅燒溫度，雖然其煅燒料於細粉碎球磨製程中不易磨出＜0.1μm之過細的磁粉(其可從成型時間與成型壓力推知)，但其無法滿足磁特性的規格中值的規定。換言之，並非使用過高的煅燒溫度反而造成磁特性不如於實施例1或2的磁特性。On the other hand, Comparative Examples 5 and 6 use a higher calcination temperature than Examples 1 and 2, although the calcined material is not easy to grind out too fine magnetic powder <0.1μm in the fine grinding ball milling process (it can be determined from the molding time and molding pressure Inferred), but it cannot meet the requirements of the median value of the magnetic characteristics. In other words, it is not that an excessively high calcination temperature causes the magnetic properties to be inferior to those of Example 1 or 2.
此外，從比較例1與2可推知，由於煅燒溫度仍偏低，其主原料氧化鐵粉(Fe 2O 3)、碳酸鋇(BaCO 3)仍無法起到完整的煅燒反應，因此煅燒後的磁粉硬度偏低，此現象使得煅燒料於細粉碎球磨製程中容易磨出＜0.1μm之過細的磁粉(此＜0.1μm之過細的磁粉無法以Fisher subsieve sizer費氏粒徑分析儀測得)，整體導致細粉碎球磨後所得到的磁粉之超微細磁粉比例較高，因此永磁鐵氧體磁粉於乾式等方向磁場成型過程中所需之成型壓力較大、成型所需時間較長、成型性較低，因此成型良率、整體良率都會因此劣化。此外，此煅燒反應不足之磁粉於製作成為磁石後，其整體磁特性均不佳，尤其對殘餘磁化強度(B r)影響更甚。另一方面，比較例1與2中，其乾式等方向性磁場成型所需壓力分別需達3.02與2.75 Ton/cm 2、成型時間分別長達23與20秒，亦代表乾式等方向磁場成型過程中，因磁粉中所含＜0.1μm之超微細磁粉比例偏高，造成所需成型壓力較大、成型時間較長，其中成型壓力較大容易使成型後的生胚產生層狀裂紋以及缺陷，而成型時間太長則會影響到生產成本，另比較例1與2中，乾式等方向磁場成型20顆生胚均出現層狀裂紋及/或缺陷，故成型後的生胚良率為0%。 In addition, it can be inferred from Comparative Examples 1 and 2, because the calcination temperature is still low, the main raw materials of iron oxide powder (Fe 2 O 3 ) and barium carbonate (BaCO 3 ) still cannot have a complete calcination reaction, so the calcined The hardness of the magnetic powder is low. This phenomenon makes the calcined material easy to grind out the magnetic powder of <0.1μm (the magnetic powder of <0.1μm cannot be measured by the Fisher subsieve sizer). The overall result is that the proportion of ultra-fine magnetic powder in the magnetic powder obtained after finely pulverized and ball-milled is relatively high. Therefore, the permanent magnet ferrite magnetic powder in the dry iso-directional magnetic field molding process requires a large molding pressure, a long molding time, and a relatively high moldability. Low, so the molding yield and overall yield will be degraded. In addition, after the magnetic powder with insufficient calcination reaction is made into a magnet, the overall magnetic properties are not good, especially the residual magnetization (B r ) is more affected. On the other hand, in Comparative Examples 1 and 2, the pressure required for dry isotropic magnetic field molding is 3.02 and 2.75 Ton/cm 2 , and the molding time is as long as 23 and 20 seconds, which also represents the dry isotropic magnetic field molding process. Among them, due to the high proportion of ultra-fine magnetic powder <0.1μm contained in the magnetic powder, the required molding pressure is relatively large and the molding time is relatively long. The high molding pressure is likely to cause lamellar cracks and defects in the green embryo after molding. If the molding time is too long, it will affect the production cost. In Comparative Examples 1 and 2, all 20 green embryos formed by dry isotropic magnetic field have lamellar cracks and/or defects, so the green yield rate after molding is 0%. .
此外，從比較例3與4可知，雖然相對於比較例1與2提升磁特性與成型良率，但由於煅燒溫度不足，故仍會在粉碎步驟的過程中磨出0.1μm之超微細磁粉。因此，參考上述對於比較例1與2之分析結果不佳的原理說明可知，比較例3與4也基於類似的理由而導致於磁特性與良率仍不佳。In addition, it can be seen from Comparative Examples 3 and 4 that although the magnetic properties and molding yield are improved compared to Comparative Examples 1 and 2, the calcination temperature is insufficient, so 0.1 μm ultrafine magnetic powder is still ground during the pulverization step. Therefore, referring to the above-mentioned explanation of the principle of poor analysis results of Comparative Examples 1 and 2, it can be seen that Comparative Examples 3 and 4 are also due to similar reasons, resulting in poor magnetic properties and yield.
綜上可知，本發明的一種改質鐵氧體磁粉的製造方法及改質鐵氧體磁石的製造方法，其特點之一在於透過使用特定的組成物以及特定的煅燒溫度，以製得具有優良磁特性與高良率的產品，並且具有簡化材料配方複雜度、提高製程穩定性且降低生產成本的優點。In summary, one of the characteristics of the manufacturing method of the modified ferrite magnetic powder and the manufacturing method of the modified ferrite magnet of the present invention lies in the use of a specific composition and a specific calcination temperature to produce a good Products with magnetic properties and high yield, and have the advantages of simplifying the complexity of material formulations, improving process stability and reducing production costs.
另外要提到的是，濕式異方向磁場配向法與乾式等方向磁場配向法的製作方式的不同，因為濕式異方向磁場配向法基本上是以一漿料形式製作，乾式等方向磁場配向法主要是粉體並搭配黏結劑。因此，濕式異方向磁場配向法中並不會考慮到對混合物所採用的煅燒溫度的不同與超微細粉(例如粒徑小於0.1微米)之間的相關性。因此，在一實施例中，本發明排除使用濕式異方向磁場配向法來進行磁場配向。Another thing to mention is that the wet different-directional magnetic field alignment method is different from the dry iso-directional magnetic field alignment method because the wet different-directional magnetic field alignment method is basically made in the form of a slurry, and the dry iso-directional magnetic field alignment method The method is mainly powder with a binder. Therefore, the wet different-directional magnetic field alignment method does not consider the correlation between the difference in the calcination temperature used for the mixture and the ultrafine powder (for example, the particle size is less than 0.1 micron). Therefore, in one embodiment, the present invention excludes the use of the wet different-directional magnetic field alignment method for magnetic field alignment.
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。Although the present invention has been disclosed in preferred embodiments, it is not intended to limit the present invention. Anyone familiar with the art can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the present invention The scope of protection shall be subject to the scope of the attached patent application.
10:方法
11~13:步驟
20:方法
21~24:步驟
10:
第1圖是本發明一實施例之改質鐵氧體磁粉的製造方法之流程方塊圖。 第2圖是本發明一實施例之改質鐵氧體磁石的製造方法之流程方塊圖。 FIG. 1 is a flow block diagram of a manufacturing method of modified ferrite magnetic powder according to an embodiment of the present invention. FIG. 2 is a block diagram of a manufacturing method of a modified ferrite magnet according to an embodiment of the present invention.
10:方法 10: method
11~13:步驟 11~13: Steps
Claims (9)
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| CN105174935A (en) * | 2015-08-31 | 2015-12-23 | 天长市中德电子有限公司 | Preparation method for rare-earth soft magnetic ferrite |
| CN110323027A (en) * | 2018-03-28 | 2019-10-11 | Tdk株式会社 | The manufacturing method of ferrite sintered magnet and ferrite sintered magnet |
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| CN105174935A (en) * | 2015-08-31 | 2015-12-23 | 天长市中德电子有限公司 | Preparation method for rare-earth soft magnetic ferrite |
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