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TW201009856A - Manufacturing method of magnetic material - Google Patents

Manufacturing method of magnetic material Download PDF

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TW201009856A
TW201009856A TW97133109A TW97133109A TW201009856A TW 201009856 A TW201009856 A TW 201009856A TW 97133109 A TW97133109 A TW 97133109A TW 97133109 A TW97133109 A TW 97133109A TW 201009856 A TW201009856 A TW 201009856A
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magnetic material
solution
producing
nitrate
mass
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TW97133109A
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Chinese (zh)
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TWI385679B (en
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Chih-Hao Huang
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Cheng Uei Prec Ind Co Ltd
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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Abstract

The present invention discloses a method of manufacturing magnetic material. The method includes the following Steps. Step 1, dissolve ferric nitrate having H2O and other metallic nitrates in an alcohol solvent to form a solution. Step 2, heat the solution to 60 to 100 degrees Centigrade. Step 3, put citric acid into the solution so as to react with each other and make the alcohol solvent volatilized under the 60 to 100 degrees Centigrade, thus obtain brown solid powder. Step 4, further heat the solid powder with an oven so as to obtain the magnetic material having a fluffy powdery form. The method of manufacturing the magnetic material of the present invention can be achieved under a relatively lower temperature that effectively reduces the manufacture cost and facilitates the manufacture of the magnetic material. Moreover, the magnetic material manufactured by the above-mentioned method has a higher degree of purity and is easy to be dispersed.

Description

201009856 九、發明說明: 【發明所屬之技術領域】 本發月/v及種磁性材料的製造方法,特別是涉及-種液相 下磁性材料的製造方法。 【先前技術】 奴 憎的展造方法可分為固相法、氣相法和液相法。 固相法製:較簡單’但是需要在高於_攝氏度的溫度下進行反 〇 Λ而且㈣的磁性材料較容易聚集成塊而不易分散。氣相法亦 ㈣學氣相沈積法,該方法需要在高於雇攝氏度的溫度下進行 反應其反應條件較為嚴苛,加工窗口小,不易量產。液相法則 必須將所^_初始產物在高於攝氏_度的溫度下進行高溫燒 結,才能付到純度較高的磁性材料。 【發明内容】 本發月之目的在於針對上述習知技術之不足,提供一種可在 較低溫度下進行’製得的磁性材料純度較高且容易分散,容易量 產’可降低製造成本的液相下的磁性材料的製造方法。 為達成上述發明目的,本發明所提供磁性材料的製造方法包 下步驟(1)將九水硝酸鐵與其他硝酸金屬化合物溶解於醇 類洛劑令’(2)將上述溶液加熱至攝氏6〇〜1〇〇度;⑺向上述溶 液中加入螫合劑’攪拌均勻,繼續保持攝氏60〜100度的加熱溫度, 使命液中的成分發生反應並揮發掉溶液中的醇類溶劑,從而得到 棕褐色的固體財;⑷將上述固體粉末用烘箱加熱使固體粉 末中的殘留a劑揮發’從而得到膨鬆粉末狀的磁性材料。 ^如上所述,本發明磁性材料的製造方法可以在較低溫度下進 行從而可有效節省能源,降低製造成本,本方法反應條件要求 201009856 低,容易量產’製得的磁性材料純度較高且容易分散。 【實施方式】 本發明之技術内容、構造特徵及其所達成之目的與功效,以 下詳予說明。 Ο201009856 IX. Description of the Invention: [Technical Field of the Invention] The present invention relates to a method for producing a magnetic material, and more particularly to a method for producing a magnetic material in a liquid phase. [Prior Art] The method of exhibiting slaves can be divided into a solid phase method, a gas phase method, and a liquid phase method. The solid phase method is simpler: but it needs to be carried out at a temperature higher than _Celsius and the magnetic material of (4) is more easily aggregated and not easily dispersed. The gas phase method also (4) vapor deposition method, which requires a reaction at a temperature higher than the employed Celsius. The reaction conditions are harsh, the processing window is small, and mass production is not easy. The liquid phase method must be high temperature sintered at a temperature higher than _ degrees Celsius to obtain a higher purity magnetic material. SUMMARY OF THE INVENTION The purpose of this month is to provide a liquid which can be produced at a relatively low temperature and which is highly pure and easy to disperse, and is easy to mass-produce, which can reduce the manufacturing cost, in view of the deficiencies of the above-mentioned conventional techniques. A method of manufacturing a magnetic material in phase. In order to achieve the above object, the method for producing a magnetic material provided by the present invention comprises the steps (1) of dissolving iron nitrate nonahydrate and other metal nitrate compounds in an alcoholic agent to make '(2) heating the solution to 6 degrees Celsius. ~1〇〇 degree; (7) Adding a chelating agent to the above solution 'stirring uniformly, continue to maintain the heating temperature of 60 to 100 degrees Celsius, the components in the mission liquid react and volatilize the alcohol solvent in the solution, thereby obtaining a tan (4) The solid powder is heated in an oven to volatilize the residual a agent in the solid powder to obtain a bulky powdery magnetic material. ^ As described above, the method for producing the magnetic material of the present invention can be carried out at a relatively low temperature, thereby effectively saving energy and reducing the manufacturing cost. The reaction conditions of the method are required to be low at 201009856, and the mass of the magnetic material produced is high and the purity is high. Easy to disperse. [Embodiment] The technical contents, structural features, and the objects and effects achieved by the present invention will be described in detail below. Ο

本發明磁性材料的製造方法,包括步驟:(1)將九水硝酸鐵 與其他硝酸金屬化合物溶解於醇類溶劑中,得到硝酸化合物溶 液;(2)將上述溶液加熱至攝氏60〜100度;(3)向上述溶液中加 入螫合劑,攪拌均勻,繼續保持攝氏60〜1〇〇度的加熱溫度,使溶液中 的成分發生反應並揮發掉溶液中的醇類溶劑,從而得到棕褐色的 固體粉末;(4)將上述固體粉末用烘箱加熱,固體粉末中的殘留 溶劑揮發,從而得到膨鬆粉末狀的磁性材料。 在所述步驟(2)中將溶液加熱前,可以先向溶液中加入通式 為RnSiX4-n的矽氧偶合劑,其中,r表示一種有機官能基,X表 不水解性官能基’ η表示〇〜2的整數,其中當n=2時,R表示的 物質既可以相同也可以不同;具體說,該矽氧偶合劑可以爲四乙 氧基矽烷、四甲氧基矽烷、三乙氧甲基矽烷和三乙氧乙基矽烷中 的一種或多種。所述步驟(3)在向溶液中加入螫合劑前,可以先加 入適量水。 上述磁性材料的製造方法中··所述其他硝酸金屬化合物可以 爲六水硝酸鎳[Ni(N03)2 · 6H20]、六水硝酸鋅[Ζη(Ν03)2 · 6H20]、 五水硝酸鉍[Bi(N〇3)3 · 5H2〇]、六水硝酸鈷[c〇(N03)3 · 6H20]、六 水峭酸猛[Μη(Ν03)2 · 6H2〇]、六水硝酸鎂[Mg(N03)2 · 6H20]和硝 酸鋇[Ba(N〇3)2]中的一種或多種。所述醇類溶劑可以為乙醇和丙醇 中的一種或兩種。所述九水硝酸鐵的質量與其他硝酸金屬化合物 的總質量的比例以5 : 1〜2為宜,九水硝酸鐵與其他硝酸金屬化合 物的總質量與醇類溶劑的質量的比例以1 : 1〜15為宜,九水硝酸 201009856 鐵與其他石肖酸金屬化合物的總質量與螫合劑的質量比例以1() ·· 〇 5〜2 為宜,所述九水峭酸鐵與其他硝酸金屬化合物的總質量與矽氧偶合 劑的質量比例以10 : 〇.5〜2為宜。所述步驟(2)中,加熱時最好採 用緩慢加熱的方式,步驟(4)中的加熱溫度以攝氏1GG〜110度為 宜。 對上述磁性材料的製造方法,以下以一具體實施例進行說明。 清參閱第—圖,首先取250克六水硝酸鎳(Ni(N03)2.6H20)、 256克六水硝酸鋅(Ζη(Ν〇3)2·6Η2〇)和1389克九水硝酸鐵 0 (Fe⑽3)3 · 9Η20),加入2500毫升乙醇溶劑中,充分搜拌均勻 至九全溶解;再向溶液中加入1〇〇克四乙氧基石夕烧、5〇克四甲氧 基夕炫和50克二乙氧甲基矽烧;緩慢升溫至攝氏度;再加入 5〇克水,隨後加入2〇〇克螫合劑(citric扣记),充分授拌均勻,此 時办液會劇烈冒泡,乙醇溶劑逐漸蒸發,從而得到棕褐色的固體 粉末;將固體粉末採用烘箱在攝氏1〇5度的溫度下加熱12小時, 以徹底除去乙醇_,最終可得卿鬆粉末狀的鐵氧磁性材料。 上述本發明磁性材料的製造方法中,由於溶液中的化學成分 H 在反應過程中會大量放熱,㈣提供足_能1 ,所以不需要二 過進-步的高溫燒結,便可得到鐵氧磁性材料。反應中加: 偶合劑,可使鐵氧磁性材料外層形成氧切保護層,從而^ 虱磁性材料/氧化石夕之核/殼複合狀態的鐵氧磁性 ^ 加磁性材料的穩定性。 ㈣#此可以増 如上所述,本發明磁性材料的製造方法可以在 :而可有效節省能源’降低製造成本,本方法反應 低,各易量產,製得的磁性材料純度較高且容易分散。 要未 【圖式簡單說明】 圖 第-圖為本發明磁性材料的製造方法_種實施例的“The method for producing a magnetic material according to the present invention comprises the steps of: (1) dissolving iron nitrate nonahydrate and other metal nitrate compounds in an alcohol solvent to obtain a nitrate compound solution; (2) heating the solution to 60 to 100 degrees Celsius; (3) adding a chelating agent to the above solution, stirring uniformly, and maintaining the heating temperature of 60 to 1 degree Celsius, reacting the components in the solution and volatilizing the alcohol solvent in the solution, thereby obtaining a tan solid. (4) The solid powder is heated in an oven, and the residual solvent in the solid powder is volatilized to obtain a bulky powdery magnetic material. Before the solution is heated in the step (2), an oxirane coupling agent of the formula RnSiX4-n may be added to the solution, wherein r represents an organic functional group, and X represents a non-hydrolyzable functional group 'η An integer of 〇~2, wherein when n=2, the substance represented by R may be the same or different; specifically, the oxime coupling agent may be tetraethoxy decane, tetramethoxy decane, or triethoxymethyl. One or more of decane and triethoxyethyl decane. The step (3) may be carried out by adding an appropriate amount of water before adding the chelating agent to the solution. In the above method for producing a magnetic material, the other metal nitrate compound may be nickel nitrate hexahydrate [Ni(N03)2 · 6H20], zinc nitrate hexahydrate [Ζη(Ν03)2 · 6H20], lanthanum nitrate pentahydrate [ Bi(N〇3)3 · 5H2〇], cobalt nitrate hexahydrate [c〇(N03)3 · 6H20], hexahydrate sulphate [Μη(Ν03)2 · 6H2〇], magnesium nitrate hexahydrate [Mg ( One or more of N03)2 · 6H20] and cerium nitrate [Ba(N〇3)2]. The alcohol solvent may be one or both of ethanol and propanol. The ratio of the mass of the ferric nitrate nonahydrate to the total mass of the other metal nitrate compounds is preferably 5:1 to 2, and the ratio of the total mass of the ferric nitrate and other metal nitrate compounds to the mass of the alcohol solvent is 1: 1~15 is suitable, Jiuhui nitric acid 201009856 The total mass of iron and other oleic acid metal compounds and the mass ratio of the chelating agent are preferably 1 () · · 〇 5~2, the sulphur acid and other nitric acid The mass ratio of the total mass of the metal compound to the oxime coupling agent is preferably 10: 〇.5 〜2. In the step (2), the heating is preferably carried out in a slow heating manner, and the heating temperature in the step (4) is preferably in the range of 1 GG to 110 °C. The method for producing the above magnetic material will be described below with reference to a specific embodiment. See the first figure for the first step, first take 250 grams of nickel nitrate hexahydrate (Ni(N03)2.6H20), 256 grams of zinc nitrate hexahydrate (Ζη(Ν〇3)2·6Η2〇) and 1389g of ferric nitrate 9 Fe(10)3)3 · 9Η20), add 2500 ml of ethanol solvent, mix well until 9 full dissolution; then add 1 gram of tetraethoxy zebra, 5 gram of tetramethoxy oxime and 50 to the solution. Gram diethoxymethyl oxime; slowly warmed to Celsius; add 5 gram of water, then add 2 gram of chelating agent (citric deduction), fully mix evenly, at this time the liquid will bubble vigorously, ethanol The solvent was gradually evaporated to obtain a brown solid powder; the solid powder was heated in an oven at a temperature of 1 to 5 ° C for 12 hours to completely remove the ethanol, and finally a ferrite material in the form of a powder of pine powder was obtained. In the above method for producing a magnetic material according to the present invention, since the chemical component H in the solution generates a large amount of heat during the reaction, (4) the foot_energy 1 is provided, so that the high-temperature sintering of the two-pass step is not required, and the ferrite is obtained. material. In the reaction, a coupling agent is added to form an oxygen-cut protective layer on the outer layer of the ferromagnetic material, thereby improving the stability of the magnetic material/ferric oxide/magnetic composite material in the composite state of the core/shell of the oxidized stone. (4) As described above, the method for manufacturing the magnetic material of the present invention can be: and can effectively save energy 'reducing the manufacturing cost, the method has low reaction, and is easy to mass-produce, and the obtained magnetic material has high purity and is easy to disperse. . BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a manufacturing method of a magnetic material of the present invention.

Claims (1)

201009856 十、申請專利範圍: h 一種雜材料的製造方法,包括如下步驟: 中;⑴將九水硝酸鐵與其他確酸金屬化合物溶解於醇類溶劑 (2)將上述溶液加熱至攝氏60〜100度; 产」向ί述溶液中加入螫合劑,授拌均勻,繼續保持攝氏〜1 〇〇 0 ο 劑,從而得到棕褐色的固體粉末;單發掉♦液中的_員溶 (4)將上述固體粉末用烘箱加熱,使固體粉末 揮發,從而得到膨鬆粉末狀的磁性材料。 留〜1 2. 如中請專利範圍第!項所述之磁性材料的製造方法, ί其他硝酸金屬化合物爲六水硝_、六水硝酸鋅 '五水確酸^ /、水確酸#、六水硝_、六水韻錢和石肖_中的—種或多種。 3. 如申清專利範圍第j項所述之磁性材料的製造方法, 述九水石肖酸鐵的質量與其他石肖酸金屬化合物的總質量的比例為 二.1晉2 ’九水:酸鐵與其他硝酸金屬化合物的總質量與醇類溶 的質量的比例為1 : 1〜1 5 ;六永由金 m 總質量與替合劑的質量比例為:水^ 4. 如申請專·圍第丨項所述之魏材料的製造方法, 述步驟⑵在將溶液加歸,先向溶液中加人通式為R啊4 n ^石夕聽合劑,其中,R_ —種有射能基,絲林解 基,η表示0〜2的整數,其中告 吕月匕 同也可以不同。 ^田η — 2時,尺表示的物質既可以相 5. 如申請專利範圍第4項所述之磁性材料的製造方法,其中所 ,“氧偶合劑爲四乙氧基錢、四甲氧基矽烧、三乙氧甲基石夕燒 201009856 和二乙氧乙基矽烷_的一種或多種。 6·如申料職㈣4項所述之磁性材料㈣造方法 土九水韻鐵與其他硝酸金屬化合物的總質 其中所 量比例為10·· 0.5〜2。 ”夕巩偶合劑的質 7.如令請專利範圍第1項所述之磁性材料 述步驟⑴在向溶液中加入細前,先加入適量;·。方法’其中所 Ο 述步第1項所述之磁性材料的製造方法,其中 ◎驟(4)中的加熱溫度為攝氏刚〜u〇度。 I其中所 9’如中請專利範園第!項所述之 切類溶劑為乙醇和丙醇中的一種或兩種顿的I造方法,其中所 所迷步t利範圍第1項所述之磁性材料的製造方法,1中 * 中,加熱時採用緩慢加熱的方式。 ,、中201009856 X. Patent application scope: h A method for manufacturing a miscellaneous material, comprising the following steps: (1) dissolving iron nitrate nonahydrate and other acid metal compounds in an alcohol solvent (2) heating the solution to 60 to 100 degrees Celsius Adding a chelating agent to the solution, mixing it evenly, and maintaining the dosage of ~1 〇〇0 ο, to obtain a brown solid powder; the _ _ solution (4) in the ♦ solution will be The solid powder is heated in an oven to volatilize the solid powder to obtain a bulky powdery magnetic material. Leave ~1 2. Please ask for the scope of patents! The method for producing the magnetic material described in the item, ί other metal nitrate compounds are hexahydrate nitrate _, zinc nitrate hexahydrate, pentacene acid ^, water sulphur acid #, hexahydrate _, Liushui Yun and Shi Xiao One or more of _. 3. For the method of manufacturing the magnetic material described in item j of the patent scope, the ratio of the mass of the non-hydrated iron sulphate to the total mass of the other oxalic acid metal compound is 2.1 Jin 2 'nine water: acid The ratio of the total mass of iron to other nitrate metal compounds to the mass of alcohol-soluble is 1: 1 to 1 5; the ratio of the total mass of the six elements to the mass of the mixture is: water ^ 4. The method for producing the Wei material according to the item, wherein the step (2) adds the solution to the solution, and first adds a formula of R 4 4 n ^ Shi Xi listening mixture to the solution, wherein R_ is a kind of emitter energy source, silk Lin Jieji, η represents an integer of 0~2, which can be different from Lu Yueyue. ^田η - 2, the material represented by the ruler can be phased. 5. The method for producing a magnetic material as described in claim 4, wherein the "oxygen coupling agent is tetraethoxy money, tetramethoxy. One or more of simmering, triethoxymethyl zeshi burn 201009856 and diethoxyethyl decane _ 6. The magnetic material described in 4 (4) of the application materials (4) method of making soil nine water rhyme iron and other nitrate metal The total mass of the compound is in the range of 10·· 0.5~2. The mass of the Xigong coupling agent is as described in the magnetic material described in the first paragraph of the patent range (1) before adding the solution to the solution, first Add the right amount; The method of producing a magnetic material according to the above item 1, wherein the heating temperature in the step (4) is a temperature of about 0.25 deg. I, where 9’, invites the patent Fanyuan! The cutting solvent described in the above is a method for producing one or two of ethanol and propanol, wherein the method for producing the magnetic material according to the first item is in the heating method of the first item, Slow heating is used. ,,in
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