415860 五、發明説明（1 ) 本發明是關於鐵為主之拾全 粉末’特別是，本發明是關於 一種鐵為主之粉末’其可用於制供姑 備軟磁材料，當其同時用 於高低頻率時具有改良的特性。 鐵為主之粒子長久以來在粉末冶金學上被視為一種結 構組成分製造的基本材料’鐵為主的粉末首先於高壓下置 於印模中鎮模，以生成所需之形狀，缚模過程之後，結構 組成份通常會進行燒結步驟以給予該組成分必須之強度。 磁鐵核心部分亦可藉由粉末冶金方法而製備，但用於 此法之鐵為主的粒子通常會在周圍覆蓋一層絕緣體材質。 鐵核心組成分之二個主要特徵為其本身透磁性及核心 耗損特性。一種材質的透磁性即表示其被磁化的能力或其 帶有磁通量能力。透磁性定義為誘導的磁通量對磁力或磁 場強度之比值，當一種磁性材質曝露於一快速變化的磁場 中時’核心的能量會因發生滯後耗損以及/或渦流耗損而 減少*滯後耗損是因必須消耗能量以克服鐵被保留在成分 之磁力而造成’而渦流耗損是因核心成分產生電流而引 起，而此電流是因交流電（AC)之電流改變所致。 經濟部中央標率局貝工消費合作社印裝 j 一 n -S- - ^^1 ^^1 — - - -·- ^^1 » i -- . .1 ^^1 m. -II (請先閲讀背面之注意事項再填寫本頁) 磁核心組成份是由薄片層之不銹鋼所製成，但該成份 很難製成小而複雜的形狀，且在高頻率下常造成大量核心 耗損。這些薄層為主的核心由於必須只能在薄片層平面上 帶有磁通量以避免造成大量的渦流耗損，而在應用上受到 限制。燒結金屬粉末已取代薄層不鎸鋼而用於磁核心組成 物，但這些燒結部分仍具有高的核心耗損量，並基本上受 限於以直流電操作。 -4- 本紙浪尺度適用中國國家標率（CNS ) A4規格（210X297公釐> A7 B7 415860 五、發明説明（2 ) 利用經包覆之以鐵為主的粉末來進行磁力核心組成份 之粉末冶金製造研究，已經直接導致鐵粉末組成份之開 發’此可增強其物理與磁特性且對其他特性亦無不良影 響。需求的特性包括通過一延伸頻率範圍之高磁透性、高 壓強度 '低核心耗損量及對壓縮鑄模技術之適用性β 當鑄模一應用AC電源之核心成份時，一般會需要該 等鐵粒子具有一電氣絕緣塗層，以減少核心耗損。 應用於鐵粒子之不同型式的絕緣體包覆物均揭露於文 獻中" 根據DE 1291028所述’鐵粉以一種磷酸溶液處理，隨 後再清洗與乾燥，該方法之特徵在於鐵粉具有大小至多為 10之尺寸，且此粉末，除了磷酸外，亦用鉻酸處理。該專 利公告案並未揭露利用該鐵粉所製備之材質的磁性質。 在本領域中的另一篇專利公告案係為DE2825235，其 揭露一種由為氧化物層所包覆之粒子所構的鐵粉末，該粒 子的大小介於0_05至〇.15nm之間，且該粒子具有一屬氧化 物包覆層’該包覆層以粒子之重量來計算，含有重量為〇3 至0.8%的氧。該氧化物包覆層係可藉由在空氣中加熱或 化學的氧化作用而得到’但卻未揭露經包覆之粒子的方法 參數以及分析結果。由實例中可計算出，所得之透磁性係 介於30至35之範圍内。 歐洲專利申請案第434669號是關於一種磁性粉末，在 其中一電氣絕緣包覆層係分隔開磁力粉末粒子，該粒子之 平均大小為10〜300以m ’且包覆每個粒子之絕緣想钟質之 泰紙張尺度適用中國國家標準（CNS ) A4規格（23〇x29·?公瘦） I 1--- - 1 二；I -I - 衣 - I —I— I - » 、1T (請先閲讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消賢合作社印製 經濟部中央標準局貝工消費合作社印製 415860 A7 ______^B7______ 五、發明説明（3 ) 包含有一連績絕緣薄層，該薄層具有小於等於10 β m之厚 度’且此薄層包含一種金屬碱氧化物或其降解產物。 W〇 95/29490揭露一種使用基於配置於水中之磷酸的 方法所得到絕緣體層。 最後DE專利第3439397號揭露一種以磷酸鹽包覆物來 達電氣絕緣作用之鐵粒子，此包覆物可為磷酸鎂或磷酸 鋅，絕緣磷酸鹽包覆物必須為鐵粒子重量的0.1至0.15% 間。該專利公告案之第1實例更詳細揭露，該電氣絕緣包 覆物係藉由將鐵粒子與溶於丙酮之89%的鱗酸溶液相混合 而製得β比較根據WO專利所製備之粉末與根據DE專利所 得到之粉末，可顯示出DE專利之絕緣層含有比WO專利申 請案之粉末更多的氧及磷酸。 現今十分意外的發現藉由本發明之新低氧粉末可以明 顯地改良其特性，此特性包括強度，密度，誘導性與磁透 性並伴隨低的耗損量》 該新粉末是以一種基本粉末為基礎，其必須由純鐵所 組成且必須為一種商業上可獲得之經水霧化的鐵粉末或一 種呈圓形、不規則狀或扁平狀顆粒的海編鐵粉末。一般不 規則狀或經水霧化且可使用之粒子實例，係為瑞典霍加納 斯股份有限公司之ABC 100及ASC 100系列的粉末β基本 粉末之粒子大小需視最後使用之粉末而定，一般小於2〇〇 仁m且最好小於丨5〇 # m。對高頻率而言，使用粒子尺寸小 於450从m較佳。最好大部分鐵為主之粉末的粒子大小係大 於lOym。根據本發明，該基本粉末係含有一氧包覆物或 _________ 本紙ίΜ賴相®家料（⑽）A4· ( 21Qx 297公瘦）~~~ ~~ 1^1^1 ^n^i— ^^^^1 (請先閲讀背面之注意事項再填寫本頁) 經濟部中央標率局員工消費合作社印製 415860 a? ___B7 五、發明説明（4 ) 者障壁，該新粉末係具有一明顯的新特性，即在於與基本 粉末比較時該新粉末之氧含量稍高，更特別的是新粉末中 氧之含量係較基本粉末為高至多重量之0,2%，較好為0.15 %。 一般相信粒子之表面構造與組成份對新粉末之特性極 為重要’基於此新粉末以ESC A方法加以研究（£^· "Proceedings of the sixth international conference on X-ray optics and micro-analysis", University of Tokyo Press, 1972, p 385-392 and 393-398 or "Solid state Chemistry and its applications" by Anthony R. West, Published by John Wilew and Sons, 1984, p 86 and p 92-96)。根據該方法◦ : P 之比 值應小於30且大於1 ’較好是此比值應小於i5且大於2,最 好為小於10且大於3 b 新粉末粒子之表面障壁的另一個重要特性為其厚度， 利用 AES方法（cf. The publication "Solid state chemistr and its applications" referred to above)發現絕緣障壁或包覆應 小於10 nm較好小於70 nm且最好小於50 nm。 本發明絕緣包覆物是藉由被配置於有機溶劑中之碟酸 處理基本粉末一段時間使足以得到所指示之含量而應用於 該基本粉末上。有機溶劑中之磷酸濃度應明顯低於揭露於 DE專利中之濃度且介於〇·5至50%間，較好介於〇 5至2〇 % ’最好介於1至5% »新粉末可藉由混合磷酸與基本粉 末一段時間以達到指標值而獲得之。 根據本發明之新穎以鐵為主之粉末可與重量約〇.1至1 -----------j_-__ 本紙張尺度適用中關家標準（CNS) M規格（^獻297公楚） -----^---^-----β--. ------訂------t .(請先聞讀背面之注意^項再填寫本頁) 415860 A7 B7 五、發明説明（ 經濟部中央標準局貝工消費合作社印製 %之潤滑劑组合且在填塞步驟前可任意與有機熱凝或熱塑 樹脂組合，潤滑劑之代表實例為Kenolube®，H wax, EBS及 硬脂酸鹽，諸如鋅硬脂酸鹽，有機樹脂可選自Peracit，U tenn 群。 填塞可在達到1000 MPa之一般壓力下進行，且p可在 環境溫度或高溫下進行。 本發明將藉由下列實驗加以說明。 1公斤的ABS 100_30粉末樣品其來自瑞典霍加納期股 份有限公司且是商業上可取得的樣品，藉由正墙酸及乙醇 進行包覆步驟’將其量在2.5至120毫升/公斤之間變化之 鐵為主的叔末與此溶液混合’經過一段時間使足以得到— 由氧磷酸所構成之包覆物。將樣品乾燥以去除溶劑，利用 ESCA分析所得到的粉末顯示，以該水溶液所得到之粉束 其0 . P之比值約為3〇，而根據本發明之方法所得到之比 值介於5至10之間。 樣品的化學分析揭露’利用該水溶液所製得之粉末其 氧含量大於0.2%，高於基本粉末，但是根據本發明之方 法所製備之粉末，其氧含量低於〇 2%，高於基本粉末。 樣品經AES分析顯示所有樣品之氧化物厚度均小於1〇〇 nm 0 下表即新粉末，以A表示之結果摘要，並與其他非本 發明之粉末比較。 ___% 1 表 I樣品I氧/读~~~早|爸厣子 金部氧I添;^氣丨全部磷丨添如^ 本紙狀^適财關家標率7^7^7雜（21£)Χ297$ (請先閲讀背面之注意事項再填寫本頁) .装- -Φ • A7 415860 五、發明説明（6 ) _______B7 (%) (%) ~ 含 量 含量 量 基本 粉末 0 0.00 53.98 0.067 0 0.003 0 樣品 A4 9.3 5.83 53.98 0.070 0.003 0.004 0.001 樣品 A3 6.95 5.91 41.13 0.093 h0.026 0.014 .011 樣品 A2 4.6 13.49 61.92 0.171 0.104 0.048 0.045 參考 樣品B 30 9.69 54.43 0.214 0.147 0.013 0,010 0 / P比值是利用ESCA測定，其乃利用KRATOS ASIXHS光譜儀並以單色AJ為又_射線源，κα = ΐ486.6 eV ; 〜395nm β 0與Ρ之含量以化學分析法測定之。 參考樣品B (Ref.B)係為由一水溶液所製得之樣品。 第2表是揭露本發明之新粉末及非本發明之粉末的溼 強度與密度之比較，該粉末於8〇〇 MPa下填塞且添加0,6% 之Kenolube為潤滑劑。 - - - —^1. I - - I^i ^^1 !—......—'*衣- --n ^―* · - - 1 ^^1 (請先聞讀背面之注$項再填^^本頁) ‘ 經濟部中央橾隼局貝工消費合作社印製 本紙張尺度適用中國國家標率（CNS丨A4規格（2IOX297公釐） 415860 A7 B7 五、發明說明（7 ) 第 2 表 材暂 fy. --5__ 溼強度（N/mm2) 密度（g/cm3) ... 參考樣品B 26.71 7.25 樣品 39.55 7.31 參考樣品C 19.24 7.14 參考樣品C(Ref. C)為根據DE專利3439397號之方法製 備的樣品。 圖式簡要說明 根據本發明所製備的低氧粉末樣品，其對磁力特性之 改良效果說明於第1圖中，該粉末以Esc A方法測得之〇 / P比值定義之，該樣品在8〇〇 MPa下進行填塞並將填塞 樣品在500°C下加熱30分鐘，Ref. B表示利用該水溶液所 製備之相同鐵為主之粉末，由結果可明顯看出本發明之新 低氧鐵粉末之特性顯著改善。 第2圖揭露改良之效果為揭露於第丄圖之樣品全部氧 含量之函數。 (請先閱讀背面之注意事項再填窝本頁) 裝----l·---訂------— — 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 10415860 V. Description of the invention (1) The present invention relates to iron-based powders. In particular, the present invention relates to an iron-based powder. It can be used for preparing soft magnetic materials. Has improved characteristics at frequency. Iron-based particles have long been regarded as a basic material for structural composition in powder metallurgy. 'Iron-based powders are first placed in a stamper under high pressure to produce the required shape and mold After the process, the structural component is usually subjected to a sintering step to give the component the necessary strength. The core of the magnet can also be prepared by powder metallurgy, but the iron-based particles used in this method are usually covered with a layer of insulator material. The two main characteristics of the iron core composition are its magnetic permeability and core wear characteristics. The permeability of a material means its ability to be magnetized or its ability to carry magnetic flux. Permeability is defined as the ratio of the induced magnetic flux to the magnetic force or magnetic field strength. When a magnetic material is exposed to a rapidly changing magnetic field, the core energy will be reduced due to hysteresis loss and / or eddy current loss. Consumption of energy to overcome the magnetic force caused by the iron being retained in the composition ', and the eddy current loss is caused by the current generated by the core component, and this current is caused by the change of the current of the alternating current (AC). Printed by Shellfish Consumer Cooperative, Central Standards Bureau, Ministry of Economic Affairs j n n -S--^^ 1 ^^ 1 —---·-^^ 1 »i-. .1 ^^ 1 m. -II (Please Read the notes on the back before filling this page.) The magnetic core component is made of a thin layer of stainless steel, but it is difficult to make small and complex shapes, and it often causes a lot of core wear at high frequencies. These thin layer-based cores are limited in application because they must only carry magnetic flux on the plane of the thin layer layer to avoid causing large eddy current losses. Sintered metal powder has been used in magnetic core compositions instead of thin stainless steel, but these sintered parts still have high core losses and are basically limited to DC operation. -4- This paper scale is applicable to China National Standard (CNS) A4 specification (210X297 mm > A7 B7 415860) V. Description of the invention (2) Use coated iron-based powder for magnetic core components Research on powder metallurgy has directly led to the development of iron powder components. 'This can enhance its physical and magnetic properties and has no adverse effects on other properties. The required properties include high magnetic permeability and high voltage strength through an extended frequency range' Low core loss and applicability to compression mold technology β When the core components of the AC power supply are used in the mold, the iron particles will generally need an electrical insulation coating to reduce core losses. Different types of iron particles The insulator coverings are disclosed in the literature " According to DE 1291028, the iron powder is treated with a phosphoric acid solution, and then washed and dried. The method is characterized in that the iron powder has a size of at most 10, and the powder In addition to phosphoric acid, it is also treated with chromic acid. The patent publication does not disclose the magnetic properties of the material prepared using the iron powder. In the art Another patent publication is DE2825235, which discloses an iron powder composed of particles coated with an oxide layer. The size of the particles is between 0_05 and 0.15nm, and the particles have a kind of oxidation "The coating layer is calculated based on the weight of the particles and contains 0 to 0.8% by weight of oxygen. The oxide coating layer can be obtained by heating or chemical oxidation in air" but However, the method parameters and analysis results of the coated particles have not been disclosed. It can be calculated from the examples that the obtained magnetic permeability is in the range of 30 to 35. European Patent Application No. 434669 is about a magnetic powder. One of the electrical insulation coatings separates the magnetic powder particles. The average size of the particles is 10 to 300 m ', and the insulation of each particle that covers the particles. The paper size of Thai paper is applicable to China National Standard (CNS) A4. Specifications (23〇x29 ·? Male thin) I 1 ----1 2; I -I-clothing-I —I— I-», 1T (Please read the precautions on the back before filling this page) Central Ministry of Economic Affairs Standards Bureau staff Xiaoxian Cooperative Printed Ministry of Economy Central Printed by the Zhuhai Bureau Shellfish Consumer Cooperative Co., Ltd. 415860 A7 ______ ^ B7______ 5. Description of the Invention (3) Contains a continuous insulation thin layer having a thickness of 10 β m or less' and this thin layer contains a metal alkali oxide Or its degradation product. W095 / 29490 discloses an insulator layer obtained by using a method based on phosphoric acid disposed in water. Finally, DE Patent No. 3439397 discloses an iron particle with a phosphate coating to achieve electrical insulation. The coating can be magnesium phosphate or zinc phosphate, and the insulating phosphate coating must be between 0.1 and 0.15% by weight of the iron particles. The first example of the patent publication discloses in more detail that the electrical insulation coating is prepared by mixing iron particles with 89% quassic acid solution in acetone to obtain β The powder obtained according to the DE patent shows that the insulation layer of the DE patent contains more oxygen and phosphoric acid than the powder of the WO patent application. It is very surprising today that the new low-oxygen powder of the present invention can significantly improve its characteristics, including properties such as strength, density, inducibility and magnetic permeability with low loss. "The new powder is based on a basic powder. It must consist of pure iron and must be a commercially available water-atomized iron powder or a sea weave iron powder with round, irregular or flat particles. Examples of particles that are generally irregular or water atomized and can be used are powders of the β basic powder of the ABC 100 and ASC 100 series of Sweden's Hoganas Co., Ltd. The particle size depends on the final powder used. Generally Less than 200 μm and preferably less than 50 μm. For high frequencies, it is better to use particle sizes smaller than 450 to m. Preferably, the particle size of most iron-based powders is greater than lOym. According to the present invention, the basic powder contains an oxygen coating or _________ paper ΜΜ 赖 相 ® home material (⑽) A4 · (21Qx 297 male thin) ~~~ ~~ 1 ^ 1 ^ 1 ^ n ^ i— ^^^^ 1 (Please read the notes on the back before filling out this page) Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 415860 a? ___B7 V. Description of the invention (4) The barrier of the new powder is obvious. The new characteristic is that the oxygen content of the new powder is slightly higher when compared with the basic powder. More specifically, the oxygen content of the new powder is up to 0.2% by weight, and preferably 0.15%. It is generally believed that the surface structure and composition of the particles are extremely important for the characteristics of the new powder. Based on this, the new powder is studied by the ESC A method (£ ^ · " Proceedings of the sixth international conference on X-ray optics and micro-analysis ", University of Tokyo Press, 1972, p 385-392 and 393-398 or " Solid state Chemistry and its applications " by Anthony R. West, Published by John Wilew and Sons, 1984, p 86 and p 92-96). According to this method: the ratio of P should be less than 30 and greater than 1 ', preferably this ratio should be less than i5 and greater than 2, preferably less than 10 and greater than 3 b. Another important characteristic of the surface barrier of new powder particles is its thickness Using the AES method (cf. The publication " Solid state chemistr and its applications " referred to above), it was found that the insulation barrier or cladding should be less than 10 nm, preferably less than 70 nm, and preferably less than 50 nm. The insulating coating of the present invention is applied to the base powder by treating the base powder with a dish acid disposed in an organic solvent for a period of time sufficient to obtain the indicated content. The concentration of phosphoric acid in the organic solvent should be significantly lower than the concentration disclosed in the DE patent and is between 0.5 and 50%, preferably between 0.05 and 20% 'preferably between 1 and 5% »New powder It can be obtained by mixing phosphoric acid with basic powder for a period of time to reach the target value. According to the novel iron-based powder according to the present invention, the weight can be about 0.1 to 1 ----------- j _-__ This paper size is applicable to the Zhongguanjia Standard (CNS) M specification (^ 297 Gongchu) ----- ^ --- ^ ----- β--. ------ Order ------ t. (Please read the notes on the back ^ before filling in This page) 415860 A7 B7 V. Description of the invention (% of lubricant combinations printed by the Shell Standard Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs and can be combined with organic thermosetting or thermoplastic resins before the filling step. Representative examples of lubricants are Kenolube®, H wax, EBS, and stearates, such as zinc stearate, organic resins can be selected from the Peracit, U tenn group. Packing can be performed at a general pressure of 1000 MPa, and p can be at ambient temperature or It is carried out at high temperature. The present invention will be explained by the following experiments. A 1 kg ABS 100_30 powder sample from Sweden's Hoganana Phase Co., Ltd. is a commercially available sample, and the coating step is performed with ortho-acid and ethanol. 'Mix this iron-based uncle whose amount varies between 2.5 and 120 ml / kg with this solution' over a period of time sufficient to obtain-from the oxygen phosphorus The coating is formed. The sample is dried to remove the solvent, and the powder obtained by the ESCA analysis shows that the powder bundle obtained by the aqueous solution has a ratio of 0. 0 to about 30, and is obtained according to the method of the present invention. The ratio is between 5 and 10. The chemical analysis of the sample revealed that the powder prepared from the aqueous solution has an oxygen content greater than 0.2%, which is higher than the basic powder, but the powder prepared according to the method of the present invention has an oxygen content Less than 0%, higher than the basic powder. AES analysis of the samples shows that the oxide thickness of all samples is less than 100nm. 0 The following table is a new powder, a summary of the results indicated by A, and other powders other than the present invention. Comparison. ___% 1 Table I Sample I Oxygen / Reading ~~~ Early | Dad-in-law Gold Department Oxygen I; ^ Gas 丨 All phosphorus 丨 Add as ^ Paper-like ^ Shicai Guan Family Standard Rate 7 ^ 7 ^ 7 Miscellaneous (21 £) × 297 $ (Please read the precautions on the back before filling out this page). Packing--Φ • A7 415860 V. Description of the invention (6) _______B7 (%) (%) ~ Basic content 0 0.00 53.98 0.067 0 0.003 0 Sample A4 9.3 5.83 53.98 0.070 0.003 0.004 0.001 Sample A3 6.9 5 5.91 41.13 0.093 h0.026 0.014 .011 Sample A2 4.6 13.49 61.92 0.171 0.104 0.048 0.045 Reference Sample B 30 9.69 54.43 0.214 0.147 0.013 0,010 0 / P ratio is measured using ESCA, which is using a KRATOS ASIXHS spectrometer with a monochrome AJ as And _ ray source, κα = ΐ486.6 eV; ~ 395nm The content of β 0 and P was determined by chemical analysis. Reference sample B (Ref. B) is a sample prepared from an aqueous solution. Table 2 discloses the comparison of the wet strength and density of the new powder of the present invention and the powder of the present invention. The powder was packed at 800 MPa and Kenolube was added as a lubricant at 0.6%. ---— ^ 1. I--I ^ i ^^ 1! —......— '* 衣---n ^ ― * ·--1 ^^ 1 (Please read the note on the back first $ Item refill ^^ this page) 'The paper size printed by the Central Bureau of the Ministry of Economic Affairs, Shellfish Consumer Cooperative Co., Ltd. The paper size is applicable to China's national standard (CNS 丨 A4 specification (2IOX297 mm) 415860 A7 B7 V. Description of invention (7) The second sheet is temporarily fy. --5__ Wet strength (N / mm2) Density (g / cm3) ... Reference sample B 26.71 7.25 Sample 39.55 7.31 Reference sample C 19.24 7.14 Reference sample C (Ref. C) is based on DE The sample prepared by the method of Patent No. 3439397. The figure briefly illustrates the effect of improving the magnetic characteristics of the low oxygen powder sample prepared according to the present invention in the first figure. The powder is measured by the Esc A method. The ratio is defined. The sample is stuffed at 800 MPa and the stuffed sample is heated at 500 ° C for 30 minutes. Ref. B represents the same iron-based powder prepared by using the aqueous solution. It can be clearly seen from the results The characteristics of the new low-oxygen iron powder of the present invention are significantly improved. The effect of the improvement shown in Figure 2 is a function of the total oxygen content of the sample disclosed in Figure VII. (Please read the precautions on the back before filling in this page.) Packing ---- l · --- Order ------------ — Printed by the Intellectual Property Bureau of the Ministry of Economic Affairs, Consumer Cooperatives Paper size applies to China Standard (CNS) A4 size (210 X 297 mm) 10