TW201001450A - Constituents and manufacturing method for ferrites that has high saturated magnetic flux density and low sintering temperature - Google Patents

Constituents and manufacturing method for ferrites that has high saturated magnetic flux density and low sintering temperature Download PDF

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TW201001450A
TW201001450A TW97123896A TW97123896A TW201001450A TW 201001450 A TW201001450 A TW 201001450A TW 97123896 A TW97123896 A TW 97123896A TW 97123896 A TW97123896 A TW 97123896A TW 201001450 A TW201001450 A TW 201001450A
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Taiwan
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oxide
magnetic flux
flux density
hours
oxidized
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TW97123896A
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Chinese (zh)
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ming-yan Xie
shao-xiong Huang
Rui-Min Zhong
shao-hui Lu
Xun-De Lin
Kun-Qi Chen
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Tai Tech Advanced Electronics Co Ltd
Mag Layers Scient Technics Co
Chilisin Electronics Corp
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Priority to TW97123896A priority Critical patent/TW201001450A/en
Publication of TW201001450A publication Critical patent/TW201001450A/en

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Abstract

This invention provides constituents and manufacturing method for ferrites that has high saturated magnetic flux density and low sintering temperature. It comprises a mixture of Fe2O3 (iron oxide) 62-67wt%, NiO (nickel oxide) 15-25wt%, ZnO (zinc oxide) 6-15wt%, and CuO (copper oxide) 5-12wt%, furthermore, added with a small amount of Li2CO3(lithium carbonate) 0.05wt%, MgO(magnesium oxide) 0.05wt%, Bi2O3 (bismuth oxide) 0.4wt%. The mixture is mixed by a ball grinding mill for 2 to 4 hours and then dried; after that it is calcined for 2 hours at 700 DEG C to 750 DEG C and ground in the ball grinding mill for another 8 hours. The fine magnetic powder is then added with PVA 0.8wt% and formed into small pellets. The small pellets is placed into a shape-forming mould and pressed with a molding press, then heated at 350 DEG C to 550 DEG C to remove grease and sintered at 890 DEG C, 900 DEG C, 910 DEG C to obtain inductance magnetic core material. The sintered compact temperature is reduced to 890 DEG C by adding the small amount of Li2CO3(lithium carbonate), MgO(magnesium oxide) and Bi2O3(bismuth oxide). Moreover, stable sintering density and saturated magnetic flux density can be obtained at temperature range between 890 DEG C to 910 DEG C can obtain.

Description

201001450 九、發明說明: 【發明所屬之技術領域】 本發明係為一種高飽和磁束密度且低溫燒結之鐵氧體組成物及方法, 尤指一種可藉由本發明中添加微量Li£〇3 (碳酸鋰)、MgO (氧化鎂)及Bi2〇3 (氧化叙)後,而可降低燒結緻密之溫度至89〇°C,同時於890〇C至910。。 溫度範圍可具有穩定的燒結密度與高飽和磁束密度之方法。 【先前技術】 電機、電子、通訊產品走向輕、薄、短、小與多功能之趨勢,因此高 密度岗效率是基本要求,同時也要求薄型化的設計,因而提昇電子線路與 零組件之裝配密度,同時也造成更嚴重之電磁干擾(EMI)的問題,因此小 型、薄型化的電感器與磁珠被廣泛地使用於輕、薄、短、小的電子通訊產 品,所以薄型化之積層晶片電感磁珠元件也成為電子產品中不可或缺之重 要零件; 這些電感、磁珠元件都是使用鐵氧磁體材料(Ferrite) 需要在HHKTC以上之溫度才能燒結,而晶片電感、磁珠則因為需要與銀導 體同時燒結,銀導體聽點是9的,所以必需將⑼電感、磁珠燒結溫度 降至_°C ’傳統上各電感廠商大多是以添加錯來達到低溫燒結之目的·,但 ^ H ^ ^ ^ f , (Restricti〇n 〇f Hazard〇us201001450 IX. Description of the Invention: [Technical Field] The present invention relates to a ferrite composition and method for sintering at a high saturation magnetic flux density and low temperature, and more particularly to a method for adding a trace amount of Li 〇 3 (carbonic acid) by the present invention. After lithium), MgO (magnesium oxide) and Bi2〇3 (oxidation), the temperature of sintering compaction can be lowered to 89 ° C, and at 890 ° C to 910. . The temperature range can have a method of stable sintered density and high saturation magnetic flux density. [Prior Art] Motor, electronics, and communication products are trending toward light, thin, short, small, and versatile. Therefore, high-density efficiency is a basic requirement, and a thin design is required, thereby improving the assembly of electronic circuits and components. Density, but also caused more serious electromagnetic interference (EMI) problems, so small, thin inductors and magnetic beads are widely used in light, thin, short, and small electronic communication products, so thin laminated wafers Inductor bead components have also become an indispensable part in electronic products; these inductors and bead components use ferrite magnets (Ferrite) to be sintered at temperatures above HHKTC, while chip inductors and beads are needed because of the need. Simultaneous sintering with silver conductor, silver conductor hearing point is 9, so it is necessary to reduce (9) inductance, magnetic bead sintering temperature to _ ° C 'Traditionally, most inductor manufacturers are adding the wrong to achieve the purpose of low temperature sintering ·, but ^ H ^ ^ ^ f , (Restricti〇n 〇f Hazard〇us

Substance,祕)與「廢電機電子設備指令」⑽咖❿咖―-EleCtr〇nic E_随t,麵),以管制電機電子& 面影響;歐盟的RoHS及丽這兩項指令嚴格限制產品中錯、鑛、采、六 201001450 價鉻及多演化合物等有害物質之成分,如今在_指令之下,電感及腿 元件也必織魏,所財低溫⑽〇。〇燒結且無触在猶上是相當大的 挑戰; 按’日本專利特開2004_161527號公報内提到無錯化的錄辞鐵氧體組 成是 12-20m〇le%的 Fe2〇3,10-25 mole%的 Zn0,其餘 m〇1_ _(合計 1〇〇 mole%),而添加的副成份是〇.卜_%的_,〇· 〇卜衞_灿邊卜加t% 的MgO ’此鐵氧體組成是在95(rc—11〇〇t,燒結2小時才會燒結緻密,作 為繞線電感的磁蕊,此糊雜是絲化的鐵氧體,但纽*是低溫_ C燒結,也不是作為積層晶片電感磁珠的材料組成·, 又日本專利JP2000109325提出以鐵化合物、錄化合物、銅化合物以及 辞化合物齡後’峨,然後粉碎而製成軸職氧雜料,其中鐵化合 物使用比表面積8.5m2/g以上之粉體,混合後粉體比表面積i〇m2/g以上,煆 燒後粉體比表面積5.Gm2/g以上,粉碎後粉體比表面積恤%以上,可以 在900C下低溫燒結緻密,而NiCuZnferrite鐵氧體粉末的比表面積愈大, 代表鐵氧體粉末峰縣小,而愈小練賴氧雜末在製作為積層晶片 電感與磁珠,不官是在漿料的分贼生胚的製作是愈不料控制的,因此 較大粒徑的NiCuZnfe油e鐵氧體粉末即是較小的比表面積之观麵* 鐵氧體粉末是有利於積層晶片電感與磁珠的製作; 因此’本案發明人4監於上述習知技術之缺失,因而乃亟思加以創新開 發’終於研發出-種可藉由本發明中添加微量[祕(碳酸鐘)、_ (氧化 鎮)及Bi2〇3 (氧化祕)後,而可降低燒結緻密之溫度至89〇。〇,同時於_ 201001450 C至91GC溫度細可具有穩定的燒結密度與高飽和磁賴度之方法。 【發明内容】 本發明之主要目的係提供一種一種高飽和磁束密度且低溫燒結之鐵氧 體組成物及方法,其係包含: 將科取Fe2〇3 (氧化鐵)62_67wt%、隱(氧化錄)15_25wt%、Zn〇 (氧 化辞)6-15wt%及CuO (氧化銅)5—12wt%混合,並添加微量之Li2C〇3 (碳酸 鋰)0. 05wt%、MgO (氧化鎂)〇· 〇5wt%、Bi2〇3 (氧化麵)侃%後,以球磨 機混合2~4小時後經烘乾,並以7〇(rc~75(rc煆燒2小時後,再以球磨機進 行8小時粉碎’將已球磨過細粉碎的磁體粉末加入〇· 8社%的pvA做混合造 粒’並製成細小造粒粉顆粒,再將其係置人成麵具,經成顏機加壓成 型’經再350°C〜55(TC脫脂後在89(TC、900°C、91(TC燒結成為電感磁蕊 體材料; 藉由本發明巾添加微量Lim (碳酸M)、MgQ (氧化⑹及脳3 (氧 化叙)後,而可降低燒結緻密之溫度至89〇。〇,同時於_。匚至_。〇溫度 範圍可制具有歡的燒結密度與高飽和磁束密度。 【實施方式】 為使貝審查員方便簡捷瞭解本發明之其他特徵内容與優點及其所達 成之功效能夠更為顯現,茲將本發明配合附圖,詳細說明如下·· 请參閱第-、二圖所示,本發明之主要目的係提供一種一種高飽和磁 束密度且低溫燒結之鐵氧體組成物及方法,其係由下列重量百分比之原料 與方法製成: 8 201001450 第一步驟·混合’其主要組成物為Fe2〇3 (氧化鐵)犯—❿伐、削(氧 化鎳)15-25禮、ZnO (氧化辞)6_15wt%、Cu〇 (氧化銅)5_12.,混合 添加微量Li2C〇3 (碳酸鐘)〇. 05wt%、Mg〇 (氧化鎖)〇.、脳3 (氧化 鉍)0.4wt%’再加入150c_c·去離子水、;L100g碳鋼珠之不鏽鋼磨球罐中, 同時加入O.lg之水溶性分散劑,並以球磨機混合2〜4小時後即可得漿料; 第二步驟:假燒,將第一步驟之漿料放入烘箱中,並以阶供乾,再 將烘乾後之粉舰過60目_祕化,而職不輯之粉末,並將該粉末 Γ 置入高溫爐中,以4°C/min的升溫速率加熱至700。〇750。(:維持2小時假 燒,經煆燒後之粉末再以60目篩網顆粒化,而形成不結塊之粉末; 第三步驟··粉碎,將第二步驟之粉末再以15〇c. c.去離子水、簡g碳 鋼珠之不鏽鋼磨球罐中之球磨條件進行粉碎,其球磨粉碎時間為8小時後 得到祕,並將職料放人烘箱85t烘乾,且打散職關罐卩為乾燥球 磨的NiCuZnFerrite鐵氧體粉末,該乾燥球磨的NiCuZnFerrite鐵氧體粉 末其比表面積為3. 0m2/g~4. Om2/g ; l 細轉:造粒’取第三轉之乾燥球磨的NiCuZnFeirite鐵氧體粉 末20g,加入5c. c.的4wt%之聚乙稀醇(p〇lyvinylene也〇}1〇1)以卿 混合機混合10分鐘,再經85t:烘乾3〇分鐘後,以顆粒機顆粒過6〇目筛網, 即得到造粒之NiCuZnFerrite鐵氧體粉末; 第五步驟·· ’再將第四步驟的造粒之NiCuZnFerrite鐵氧體粉末 4. 〇克’置入環狀模具内,該環狀模具為外徑2 〇 cm、内# 〇 cm,再將環 狀模具置於壓難20()() kg/on2纏力將造崎職成環狀生胚體; 9 201001450 第六步驟:燒結,將第五步驟之環狀生胚體置入燒結爐内,先以緩慢2 。(:她之加熱升溫速度下’升溫至35(rc〜55(rc停留2小時,將環狀生胚 體内之有機黏結劑完全脫脂後’在以4t:/min之加熱升溫速度,升溫至咖 C停留2小時餅止升溫燒結’絲賴船體材料,可依需求將燒結溫 度調整為 89(TC、90(TC 或 91(TC ; 藉由本發明中添加微量Li2C〇3 (碳酸鐘)、_ (氧化錢)及仏〇3 (氧 化絲)後,而可降低燒結緻密之溫度至89(rc,同時於89〇t至⑽。c溫度 範圍可具有穩定的燒結密度與高飽和磁束密度; 再依下列各個實施例加以詳述本發明之特徵、目的及優點; 實施例-:秤取純度99.3%以上的氧化物粉末純(氧化鐵)65.6社 %、削(氧化錄)2G. 5社%、ZnO (氧化鋅)6. 9wt%、Cu()(氧化鋼)7. _Substance, secret) and the "Waste Electrical and Electronic Equipment Directive" (10) coffee machine - EleCtr〇nic E_ with t, surface), to control motor electronics &surface; EU's RoHS and Li are strictly restricted products In the wrong, mining, mining, six 201001450 price of chromium and multi-component compounds and other harmful substances, now under the _ directive, the inductance and leg components will also weave Wei, the low temperature (10) 〇. Sintering and non-touching are quite a challenge; as mentioned in the 'Japanese Patent Laid-Open No. 2004_161527, the error-free recording ferrite composition is 12-20 m〇le% of Fe2〇3,10- 25 mole% of Zn0, the rest of m〇1_ _ (total 1〇〇 mole%), and the added sub-component is 〇. _% of _, 〇· 〇 卫 _ _ bian bian plus t% of MgO 'this The composition of ferrite is 95 (rc - 11 〇〇t, sintering will be dense for 2 hours after sintering, as the magnetic core of the winding inductance, this paste is a filamentized ferrite, but New York is low temperature _ C sintering Nor is it a material composition of a laminated chip inductive magnetic bead. Moreover, Japanese Patent No. JP2000109325 proposes an iron compound, a recorded compound, a copper compound, and a compound after ageing, and then pulverized to form a shaft oxygen compound, wherein the iron compound When the powder having a specific surface area of 8.5 m 2 /g or more is used, the specific surface area of the powder after mixing is i 〇 m 2 /g or more, and the specific surface area of the powder after calcination is 5. Gm 2 /g or more, and the specific surface area of the powder after pulverization is more than or equal to Low temperature sintering at 900C, and the larger the specific surface area of NiCuZnferrite ferrite powder, representing ferrite powder Fengxian is small, and the smaller the lyophobic slag is made into laminated chip inductors and magnetic beads, the unsuccessful is the production of the squid embryo in the slurry is more uncontrolled, so the larger particle size NiCuZnfe oil e Ferrite powder is a small surface area of the specific surface area * Ferrite powder is beneficial to the fabrication of laminated chip inductors and magnetic beads; therefore, the inventor of the present invention is in charge of the lack of the above-mentioned conventional techniques, and thus is thinking Innovative development has finally been developed. By adding a small amount of [secret (carbon clock), _ (oxidized town) and Bi2〇3 (oxidation secret) in the present invention, the temperature of sintering compaction can be lowered to 89 〇. At the same time, the temperature of _201001450 C to 91GC may have a stable sintered density and a high saturation magnetic latitude. SUMMARY OF THE INVENTION The main object of the present invention is to provide a ferrite composition with high saturation magnetic flux density and low temperature sintering. And method, comprising: taking Fe2〇3 (iron oxide) 62_67wt%, hidden (oxidation record) 15_25wt%, Zn〇 (oxidation) 6-15wt% and CuO (copper oxide) 5-12wt% mixed , and added a trace of Li2C〇3 (lithium carbonate) 0. 05 After wt%, MgO (magnesium oxide) 〇·〇5wt%, Bi2〇3 (oxidized surface)侃%, after mixing for 2~4 hours in a ball mill, drying, and 7〇(rc~75(rc煆烧2) After an hour, it was pulverized by a ball mill for 8 hours. 'The ball-milled finely pulverized magnet powder was added to 〇·8% of pvA for mixing granulation' and made into fine granulated powder granules, which were then placed into a mask. Pressurized by a forming machine to pass through 350 ° C ~ 55 (TC degreased at 89 (TC, 900 ° C, 91 (TC sintered into an inductive magnetic core material; by adding a trace of Lim (carbonic acid M) by the towel of the present invention After MgQ (oxidation (6) and 脳3 (oxidation), the temperature of sintering compaction can be lowered to 89 〇. Oh, at the same time _.匚 to _. The 〇 temperature range allows for a sintered density and a high saturation magnetic flux density. [Embodiment] In order to facilitate the simple and easy understanding of the other features and advantages of the present invention and the effects achieved thereby, the present invention will be described in detail with reference to the accompanying drawings. As shown, the main object of the present invention is to provide a ferrite composition and method for high-saturation magnetic flux density and low-temperature sintering, which are made of the following raw materials and methods by weight: 8 201001450 First step · Mixing' Its main composition is Fe2〇3 (iron oxide) - ❿ cutting, cutting (nickel oxide) 15-25, ZnO (oxidation) 6_15wt%, Cu〇 (copper oxide) 5_12., mixed with trace Li2C〇3 (carbonic acid) 〇. 05wt%, Mg〇 (oxidized lock) 〇., 脳3 (铋 铋) 0.4wt% 'Add 150c_c·deionized water; L100g carbon steel ball in stainless steel grinding ball jar, while adding O .lg water-soluble dispersant, and mixed in a ball mill for 2~4 hours to obtain the slurry; the second step: fake burning, the first step of the slurry is placed in the oven, and the order is dry, and then After drying, the powder ship has passed 60 mesh _ secret, and the powder is not And Γ powder into the high-temperature furnace, the temperature rise rate of 4 ° C / min was heated to 700. 〇 750. (: Maintain 2 hours of smoldering, the powder after simmering is granulated by a 60 mesh screen to form a non-caking powder; the third step smashing, the powder of the second step is further 15 cc The ball milling conditions in the stainless steel grinding ball jar of ionized water and simple carbon steel ball are pulverized, the ball milling time is 8 hours, the secret is obtained, and the material is placed in an oven for drying at 85t, and the cans are dried for drying. Ball-milled NiCuZnFerrite ferrite powder, the dry-milled NiCuZnFerrite ferrite powder has a specific surface area of 3.0 m2 / g ~ 4. Om2 / g; l fine rotation: granulation 'take the third turn of the dry ball milled NiCuZnFeirite iron 20 g of oxygen powder, adding 4 wt% of polyethylene glycol (p〇lyvinylene 〇}1〇1) of 5c.c., mixed with a mixer for 10 minutes, and then subjected to 85t: drying for 3 minutes, after granules The granules pass through the 6 mesh screen to obtain the granulated NiCuZnFerrite ferrite powder; the fifth step ·· 'The fourth step of granulating NiCuZnFerrite ferrite powder 4. 〇克' is placed in the ring mold Inside, the annular mold has an outer diameter of 2 〇cm, inner # 〇cm, and then the annular mold is placed under pressure 20 () () Kg/on2 entanglement force will form the ring-shaped raw body body; 9 201001450 The sixth step: sintering, the fifth step of the ring-shaped embryo body into the sintering furnace, first with a slow 2 (: her heating At the heating rate, the temperature was raised to 35 (rc~55 (rc stayed for 2 hours, after the organic binder in the ring-shaped embryo was completely degreased), and the temperature was raised at 4 t:/min, and the temperature was raised to the coffee C for 2 hours. The cake is heated and sintered, and the slag material can be adjusted to 89 (TC, 90 (TC or 91 (TC; by adding a small amount of Li2C〇3 (carbonic acid), _ (oxidized money) by the present invention) And 仏〇3 (oxidized wire), can reduce the temperature of sintering compaction to 89 (rc, while at the same time from 89 〇t to (10). c temperature range can have stable sintered density and high saturation magnetic flux density; The features, objects, and advantages of the present invention are exemplified in detail. Example:: An oxide powder having a purity of 99.3% or more is weighed (iron oxide) 65.6%, cut (oxidized) 2G. 5%, ZnO (oxidized) Zinc) 6. 9wt%, Cu () (oxidized steel) 7. _

分別將這些原材料以上述之步驟進行製作,最後將所得到之電感磁芯 體材料分職結至89G°C、咖。(:、91(TC之燒結溫度,等爐冷㈣環狀試/ 以阿基米德原理之方法量測得NiCuZnFerrite燒结體的密许 、口 疝厌,以 LCR meter 測量導磁率ui,以磁滯曲線儀測量飽和磁束密度bs,如下表 201001450 實施例 燒結條件 測量密度 初導磁率 飽和磁束密度 (〇c*小時) (g/cm3) (@1ΜΗζ) (Gauss) 1 ~ 890*2 4.08 13 叫 753 1 900*2 4.19 15 864 1 910*2 4.28 17 1119 1A 890*2 4.86 45 Ί 2886 1A 900*2 5.08 61 3293 1A 910*2 5.22 70 3542 1B 890*2 5.22 51 3386 1B 900*2 5.26 54 3533 1B 910*2 5.26 54 3423 1C 890*2 5.24 50 3253 1C 「900*2 5.27 51 3264 1C 皂 910*2 5.27 54 r 3393 表二、不同重量百分比添加物之測量密度r初導磁率束密度 在實施例1至1C的粉末比表面積測量是3. 52至3. 87(m2/g),遠低於 8,5(m2/g),表示無鉛化的NiCuZnferrite鐵氧體粉末不需要球磨至太小的粉 末即可於900C燒結敏欲’也有利於積層晶片電感、磁珠生胚薄片的製作 與網印等製程; °青參閱上表一所示,而在燒結溫度900 C時,實施例1B至1C的材料 组’有添加0.05wt%以上的MgO、0.4wt%的吼2〇3與〇.05wt%以上的Li2C〇3, 相較於無添加MgO、Bi2〇3與Li£〇3的結果,其燒結密度高於5 2〇(g/cm3), 同時在燒結溫度於890-910 C的溫度範圍,其燒結密度介於 5.22〜5.28(g/cm3),且其初導磁率介於51〜54,故其燒結密度與初導磁率對於 燒結溫度於890-910t的溫度變化是穩定的; 實施例二:秤取純度99. 3%以上的氧化物粉末㈣3 (氧化鐵)65.侃 %、_ (氧化錄)15. 4wt%、ZnO (氧化辞)12· 3wt%、Cu〇 (氧化銅)6. 9社 % ’且分別量取添加物的組成配置加入,如丁表三所示: 201001450 實施例 材料組成添加物重量百分比(〇/〇) 鐵氧磁體粉末 Li2C03 Mg〇 Bi2〇3 比表面積(m2/g) 2 0 0 0 3.49 2A 0.05 0.05 0.2 3.92 2B 0.05 0.05 ~ 0.4 3.92 2C 0.1 0.1 0.4 3.80 表三、實施例二中添加物重量百分比(%) 分別將這些原材料與實施例一之相同步驟進行製作,最後將所得到之 電感磁芯體材料分別燒結至890X:、900°c、9HTC之燒結溫度,等爐冷取出 環狀試片,以阿基米德原理之方法量測得NiCuZnFerrite燒結體的密度,以 LCR meter測量導磁率ui,以磁滯曲線儀測量飽和磁束密度Bs,如下表四 所示: 實施例 燒結條件 (C*小時) 測量密度 (g/cm3) 初導磁率 (@1ΜΗζ) 飽和磁束密度(Gauss) 2 890*2 4.14 27 1559 2 900*2 4.27 34 1973 2_ 910*2— 4.36 39 2221 2A 890*2 4.98 116 3685 2A — 900*2 5.15 159 4018 2A 910*2 5.25 169 4150 2B 890*2 5.23 108 3955 nr 900*2 5.26 112 4048 2B 910*2 5.29 121 4115 2C 890*2 5.25 105 3951 2C 900*2 5.28 112 4069 |_2C 卜 910*2 5.28 140 4078 表四、不同重量百分比添加物之測量密度、初導磁率及飽和磁束密度 請參閱上表四所示,而在燒結溫度9〇〇°C時,實施例2B至2C的結果 中,有添加 〇_〇5wt%以上的 MgO、0.4wt%的 Bi203與 0.05wt%以上的 Li2C〇3, 相較於無添加Mg〇、Bi2〇3與Li£〇3的編號2之實驗結果較佳,其燒結密度 12 201001450 高於5辱办同時在燒結溫度物。⑽此的溫度範圍,其燒結密度 "於5.23〜5.29(gW),且其初導磁率介於⑽〜⑵,故其燒結密度與初導 磁率對於燒結溫度於㈣以呢的溫度變化是穩定的; 本發明可進—步’無科胁靴下魏,製成賴晶片磁珠與電 感;又本發明亦可進-步與溶劑、分散劑、有機塑化劑、黏結劑混合,以 刮刀成型製作成生胚薄片’於生胚薄片網印銀導電膏,積層堆疊與熱壓, 脫脂後與銀導電膏共燒製作成積層晶片電感與磁珠元件。 為使本發明更加_岐進步性與實祕,贿先前技術作—比較分 析如下: 習用缺失: 1、 無法在低溫(90(Tc)下燒結。 2、 鐵氧體粉末的比表面積愈大,代表鐵氧體粉末的錄愈小,而愈小 粒徑的鐵氧體粉末在製作為積層晶片電感與磁珠,不管是在漿料的分散或 生胚的製作不容易控制。 本發明優點: 1、 可於低溫燒結。 2、 鐵氧體粉末不需要球磨至太小的粉末’即可於9〇〇。。燒結緻密。 3、 具有穩定的燒結密度與高飽和磁束密度。 【圖式簡單說明】 第圖係為本發明之組成物混合示意圖。 第二圖係為本發明之添加微量組成物示意圖。 【主要元件符號說明】 13These raw materials were separately produced in the above-mentioned steps, and finally the obtained inductive magnetic core material was divided into 89 G ° C, coffee. (:, 91 (the sintering temperature of TC, the furnace cooling (four) ring test / the method of Archimedes principle measured the density of the NiCuZnFerrite sintered body, mouth 疝, measured by the LCR meter permeability ui, The hysteresis curve meter measures the saturation magnetic flux density bs as shown in the following table 201001450. Example Sintering conditions Measurement Density Initial permeability Magnetic flux density (〇c*hour) (g/cm3) (@1ΜΗζ) (Gauss) 1 ~ 890*2 4.08 13 753 1 900*2 4.19 15 864 1 910*2 4.28 17 1119 1A 890*2 4.86 45 Ί 2886 1A 900*2 5.08 61 3293 1A 910*2 5.22 70 3542 1B 890*2 5.22 51 3386 1B 900*2 5.26 54 3533 1B 910*2 5.26 54 3423 1C 890*2 5.24 50 3253 1C "900*2 5.27 51 3264 1C Soap 910*2 5.27 54 r 3393 Table 2, Measurement Density of Different Weight Percent Additives r Initial Magnetic Flux Density The specific surface area measurement of the powders of Examples 1 to 1C was 3.52 to 3.87 (m2/g), which was much lower than 8,5 (m2/g), indicating that the lead-free NiCuZnferrite ferrite powder did not need to be ball-milled to Too small powder can be sintered at 900C. It is also beneficial for the fabrication of laminated wafer inductors, magnetic bead green sheets and screen printing. ° see the above Table 1, and at the sintering temperature of 900 C, the material group of Examples 1B to 1C has added 0.05 wt% or more of MgO, 0.4 wt% of 吼2〇3 and 〇.05 wt% or more. Li2C〇3, compared with the results of no addition of MgO, Bi2〇3 and Li£〇3, the sintering density is higher than 5 2〇(g/cm3), and the sintering temperature is in the temperature range of 890-910 C. The sintered density is between 5.22 and 5.28 (g/cm3), and the initial magnetic permeability is between 51 and 54, so the sintered density and the initial permeability are stable for the temperature change of the sintering temperature of 890-910 t; The oxide powder of the purity of 99.3% or more is taken. (4) 3 (iron oxide) 65. 侃%, _ (oxidation record) 15. 4wt%, ZnO (oxidation) 12·3wt%, Cu〇 (copper oxide) 6. 9%%' and separately measure the composition of the additive, as shown in Table 3: 201001450 Example Material Composition Additive Weight Percent (〇/〇) Ferrite Magnet Powder Li2C03 Mg〇Bi2〇3 Specific Surface Area (m2 /g) 2 0 0 0 3.49 2A 0.05 0.05 0.2 3.92 2B 0.05 0.05 ~ 0.4 3.92 2C 0.1 0.1 0.4 3.80 Table 3, the weight percentage (%) of the additives in the second example These raw materials were fabricated in the same manner as in the first embodiment. Finally, the obtained inductive magnetic core materials were respectively sintered to a sintering temperature of 890X:, 900 ° C, and 9 HTC, and the annular test piece was taken out in a furnace to obtain an Aki. The density of the NiCuZnFerrite sintered body was measured by the Mead principle method, the magnetic permeability ui was measured by the LCR meter, and the saturation magnetic flux density Bs was measured by a hysteresis curve meter as shown in the following Table 4: Example Sintering conditions (C* hours) Measurement density (g/cm3) Initial permeability (@1ΜΗζ) Saturation magnetic flux density (Gauss) 2 890*2 4.14 27 1559 2 900*2 4.27 34 1973 2_ 910*2— 4.36 39 2221 2A 890*2 4.98 116 3685 2A — 900 *2 5.15 159 4018 2A 910*2 5.25 169 4150 2B 890*2 5.23 108 3955 nr 900*2 5.26 112 4048 2B 910*2 5.29 121 4115 2C 890*2 5.25 105 3951 2C 900*2 5.28 112 4069 |_2C 910*2 5.28 140 4078 Table 4, measured density, initial permeability and saturation magnetic flux density of different weight percentage additives, please refer to Table 4 above, and at the sintering temperature of 9 ° C, Examples 2B to 2C As a result, there is added 〇_〇 5 wt% or more of MgO, 0.4 wt% Bi203 and 0.05wt% or more of Li2C〇3 are better than the experimental results of No. 2 without added Mg〇, Bi2〇3 and Li£〇3, and the sintered density 12 201001450 is higher than 5 in the same time at the sintering temperature. Things. (10) The temperature range, the sintered density " at 5.23~5.29 (gW), and its initial permeability is between (10) and (2), so the sintered density and the initial permeability are stable for the temperature change of the sintering temperature in (4) The invention can be further advanced into a step by step, and the rotor is made of a magnetic bead and an inductor; and the invention can also be further mixed with a solvent, a dispersant, an organic plasticizer and a binder to form a doctor blade. The raw embryonic sheet is made into a silver-plated conductive paste on the green sheet, laminated and hot pressed, and co-fired with silver conductive paste after degreasing to form a laminated chip inductor and magnetic bead element. In order to make the invention more progressive and practical, the previous technical work of bribes is comparatively analyzed as follows: Lack of use: 1. It cannot be sintered at low temperature (90 (Tc). 2. The larger the specific surface area of the ferrite powder, The smaller the recording of the ferrite powder, the smaller the particle size of the ferrite powder is made into the laminated chip inductor and the magnetic bead, which is not easy to control in the dispersion of the slurry or the production of the green embryo. Advantages of the invention: 1. It can be sintered at low temperature. 2. The ferrite powder does not need to be ball milled to a powder that is too small to be 9 〇〇. Sintering is dense. 3. It has stable sintered density and high saturation magnetic flux density. DESCRIPTION OF THE DRAWINGS The figure is a schematic diagram of the composition of the composition of the present invention. The second figure is a schematic diagram of the added trace composition of the present invention.

Claims (1)

201001450 十、申請專利範圍: 1、 一種高飽和磁束密度且低溫燒結之鐵氧體組成物,其係由下列重量 百分比之原料所組成: Fe2〇3 (氧化鐵)62_67wt%、Ni〇 (氧化鎳)15_25社%、Zn〇 (氧化鋅) 6 15wt/。CuO (氧化銅)5-l2wt%、以及 Li2C〇3 (碳酸艘)〇. 〇5wt%、MgO (氧 化鎮)0· 05wt%、Bi2〇3 (氧化銘)〇. 4wt%。 2、 一種高飽和磁束密度且低溫燒結之鐵氧體方法,其係包含: 將科取 Fe2〇3 (氧化鐵)62_67wt%、_ (氧化錦)15_25wt%、Zn〇 (氧 化鋅)6-15wt%及CuO (氧化銅)5_版%混合’並添加微量之Li2C〇3 (碳酸 鐘)0· 05wt%、MgO (氧化鎂)〇. Q5wt%、馳(氧化⑷◦·侃%後以球磨 機/昆σ 2 4小時後經供乾,並以7〇〇。〇〜75〇。〇烺燒2小時後,再以球磨機進 行叙碎將已球磨過細粉碎的磁體粉末加入〇. 的PM做混合造粒,並 製成細小造粒粉顆粒’再將其係置人成型模具’經·壓機加壓成型,經 再351TC〜55(TC脫脂後在89(rc、9〇(rc、91(rc燒結成為電感蕊體材料。 3依申凊專利範圍第2項所敘述之一種高飽和磁束密度且低溫燒結之 鐵氧體方法,其中該球磨_體粉末之比表面積為3. G(m2/g)至4. G(m2/g)。 14201001450 X. Patent application scope: 1. A ferrite composition with high saturation magnetic flux density and low temperature sintering, which is composed of the following raw materials by weight: Fe2〇3 (iron oxide) 62_67wt%, Ni〇 (nickel oxide) ) 15_25%, Zn〇 (zinc oxide) 6 15wt/. CuO (copper oxide) 5-l2wt%, and Li2C〇3 (carbonate) 〇. 5wt%, MgO (oxidized town) 0. 05wt%, Bi2〇3 (oxidized) 〇. 4wt%. 2. A ferrite method of high saturation magnetic flux density and low-temperature sintering, comprising: taking Fe2〇3 (iron oxide) 62_67wt%, _(oxidized bromine) 15_25wt%, Zn〇(zinc oxide) 6-15wt % and CuO (copper oxide) 5_ version% mixed 'and add a small amount of Li2C〇3 (carbonic acid clock) 0· 05wt%, MgO (magnesium oxide) 〇. Q5wt%, Chi (oxidized (4) ◦·侃% after ball mill / Kun σ 2 After 4 hours, it is supplied and dried, and it is 7 〇〇. 〇~75 〇. After simmering for 2 hours, it is smashed by a ball mill to add the ball milled finely pulverized magnet powder to 〇. PM for mixing. Granulation, and made into small granulated powder particles 'and then placed into a human molding die' pressurization by press, after 351TC ~ 55 (TC degreasing after 89 (rc, 9 〇 (rc, 91 (rc Sintered to be an inductive core material. 3 A high-saturation magnetic flux density and a low-temperature sintering ferrite method according to the second aspect of the invention, wherein the specific surface area of the ball-milling powder is 3. G (m2/g) ) to 4. G(m2/g). 14
TW97123896A 2008-06-26 2008-06-26 Constituents and manufacturing method for ferrites that has high saturated magnetic flux density and low sintering temperature TW201001450A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI414484B (en) * 2011-12-09 2013-11-11 Ind Tech Res Inst Ferrite magnetic materials
US9414534B2 (en) 2012-06-05 2016-08-09 Industrial Technology Research Institute EMI shielding device and manufacturing method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI414484B (en) * 2011-12-09 2013-11-11 Ind Tech Res Inst Ferrite magnetic materials
US9414534B2 (en) 2012-06-05 2016-08-09 Industrial Technology Research Institute EMI shielding device and manufacturing method thereof
TWI562718B (en) * 2012-06-05 2016-12-11 Ind Tech Res Inst Emi shielding device and manufacturing method thereof

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