TWI385679B - Manufacturing method of magnetic material - Google Patents
Manufacturing method of magnetic material Download PDFInfo
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- TWI385679B TWI385679B TW97133109A TW97133109A TWI385679B TW I385679 B TWI385679 B TW I385679B TW 97133109 A TW97133109 A TW 97133109A TW 97133109 A TW97133109 A TW 97133109A TW I385679 B TWI385679 B TW I385679B
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本發明涉及一種磁性材料的製造方法，特別是涉及一種液相下磁性材料的製造方法。 The present invention relates to a method of producing a magnetic material, and more particularly to a method of producing a magnetic material in a liquid phase.
一般磁性材料的製造方法可分為固相法、氣相法和液相法。固相法製程較簡單，但是需要在高於600攝氏度的溫度下進行反應，而且得到的磁性材料較容易聚集成塊而不易分散。氣相法亦即化學氣相沈積法，該方法需要在高於200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。液相法則必須將所得到的初始產物在高於攝氏400度的溫度下進行高溫燒結，才能得到純度較高的磁性材料。 Generally, a method for producing a magnetic material can be classified into a solid phase method, a gas phase method, and a liquid phase method. The solid phase process is simpler, but requires a reaction at a temperature higher than 600 degrees Celsius, and the obtained magnetic material is more easily aggregated and not easily dispersed. The gas phase method, that is, the chemical vapor deposition method, requires a reaction at a temperature higher than 200 degrees Celsius, the reaction conditions are harsh, the processing window is small, and mass production is not easy. The liquid phase method must sinter the obtained initial product at a temperature higher than 400 ° C to obtain a magnetic material of higher purity.
本發明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。 The object of the present invention is to provide a magnetic material in a liquid phase which can be produced at a relatively low temperature and which is high in purity and easy to disperse, is easy to mass-produce, and can reduce manufacturing cost, in view of the deficiencies of the above-mentioned conventional techniques. Manufacturing method.
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括如下步驟：(1)將九水硝酸鐵與其他硝酸金屬化合物溶解於醇類溶劑中；(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60~100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，使固體 粉末中的殘留溶劑揮發，從而得到膨鬆粉末狀的磁性材料。 In order to achieve the above object, the method for producing a magnetic material provided by the present invention comprises the steps of: (1) dissolving iron nitrate nonahydrate and other metal nitrate compounds in an alcohol solvent; (2) heating the solution to 60 ° C. 100 degrees; (3) adding a chelating agent to the above solution, stirring evenly, and maintaining the heating temperature of 60-100 degrees Celsius, reacting the components in the solution and volatilizing the alcohol solvent in the solution, thereby obtaining a tan Solid powder; (4) heating the above solid powder in an oven to make a solid The residual solvent in the powder is volatilized to obtain a bulky powdery magnetic material.
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低，容易量產，製得的磁性材料純度較高且容易分散。 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 low, and mass production is easy, and the obtained magnetic material is high in purity and easy. dispersion.
本發明之技術內容、構造特徵及其所達成之目的與功效，以下詳予說明。 The technical content, structural features and the objects and effects achieved by the present invention are described in detail below.
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60~100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。 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 100 degrees Celsius, reacting the components in the solution and volatilizing the alcohol solvent in the solution, thereby obtaining a brown solid powder; (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.
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表示水解性官能基，n表示0~2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，該矽氧偶合劑可以為四乙氧基矽烷、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。 Before the solution is heated in the step (2), an oxirane coupling agent of the formula R n SiX 4-n may be added to the solution, wherein R represents an organic functional group, and X represents a hydrolyzable functional group. n represents an integer of 0 to 2, wherein when n=2, the substance represented by R may be the same or different; specifically, the anthracene coupling agent may be tetraethoxydecane, tetramethoxynonane, or triethylbenzene. One or more of oxymethyl 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.
上述磁性材料的製造方法中：所述其他硝酸金屬化 合物可以為六水硝酸鎳[Ni(NO3)2‧6H2O]、六水硝酸鋅[Zn(NO3)2‧6H2O]、五水硝酸鉍[Bi(NO3)3‧5H2O]、六水硝酸鈷[Co(NO3)3‧6H2O]、六水硝酸錳[Mn(NO3)2‧6H2O]、六水硝酸鎂[Mg(NO3)2‧6H2O]、九水硝酸鐵Fe(NO3)3‧9H2O和硝酸鋇[Ba(NO3)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1：1~1.5為宜，九水硝酸鐵與其他硝酸金屬化合物的總質量與螫合劑的質量比例以10：0.5~2為宜；所述九水硝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10：0.5~2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100~110度為宜。 In the method for producing a magnetic material, the other metal nitrate compound may be nickel nitrate hexahydrate [Ni(NO 3 ) 2 ‧6H 2 O], zinc nitrate hexahydrate [Zn(NO 3 ) 2 ‧6H 2 O], Lanthanum nitrate pentahydrate [Bi(NO 3 ) 3 ‧5H 2 O], cobalt nitrate hexahydrate [Co(NO 3 ) 3 ‧6H 2 O], manganese nitrate hexahydrate [Mn(NO 3 ) 2 ‧6H 2 O] One or more of magnesium nitrate hexahydrate [Mg(NO 3 ) 2 ‧6H 2 O], iron nitrate nonahydrate Fe(NO 3 ) 3 ‧9H 2 O and lanthanum nitrate [Ba(NO 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: 1~1.5 is suitable, the total mass of ferric nitrate and other nitrate metal compounds and the mass ratio of the chelating agent are preferably 10:0.5~2; the total mass of the ferric nitrate and other nitrate metal compounds and helium oxygen The mass ratio of the coupling agent is preferably 10:0.5~2. 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 100 to 110 degrees Celsius.
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。 The method for producing the above magnetic material will be described below with reference to a specific embodiment.
請參閱第一圖，首先取250克六水硝酸鎳(Ni(NO3)2‧6H2O)、256克六水硝酸鋅(Zn(NO3)2‧6H2O)和1389克九水硝酸鐵(Fe(NO3)3‧9H2O)，加入2500毫升乙醇溶劑中，充分攪拌均勻至完全溶解；再向溶液中加入100克四乙氧基矽烷、50克四甲氧基矽烷和50克三乙氧甲基矽烷；緩慢升溫至攝氏80度；再加入50克水，隨後加入200克螫合劑(citric acid)，充分攪拌均勻，此時溶液會劇烈冒泡，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105度的溫度下加熱12小時，以徹底除去乙醇溶劑，最終可得到膨鬆 粉末狀的鐵氧磁性材料。 Please refer to the first figure, first take 250 grams of nickel nitrate hexahydrate (Ni(NO 3 ) 2 ‧6H 2 O), 256 grams of zinc nitrate hexahydrate (Zn(NO 3 ) 2 ‧6H 2 O) and 1389 grams of nine water Iron nitrate (Fe(NO 3 ) 3 ‧9H 2 O), added to 2500 ml of ethanol solvent, stirred well until completely dissolved; then 100 g of tetraethoxy decane, 50 g of tetramethoxy decane and 50 g were added to the solution. 50 g of triethoxymethyl decane; slowly warmed to 80 ° C; add 50 g of water, then add 200 g of citric acid, stir well, then the solution will bubble vigorously, the ethanol solvent gradually evaporates. Thus, a brown solid powder was obtained; the solid powder was heated in an oven at a temperature of 105 ° C for 12 hours to completely remove the ethanol solvent, and finally a fermented ferrite material was obtained.
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在反應過程中會大量放熱，能夠提供足夠的能量，所以不需要經過進一步的高溫燒結，便可得到鐵氧磁性材料。反應中加入矽氧偶合劑，可使鐵氧磁性材料外層形成氧化矽保護層，從而形成鐵氧磁性材料/氧化矽之核/殼複合狀態的鐵氧磁性材料，藉此可以增加磁性材料的穩定性。 In the above method for producing a magnetic material of the present invention, since the chemical component in the solution generates a large amount of heat during the reaction, sufficient energy can be supplied, so that the ferrite magnetic material can be obtained without further high-temperature sintering. The addition of a cerium oxygen coupling agent in the reaction can form a protective layer of cerium oxide on the outer layer of the ferromagnetic material, thereby forming a ferrite material of a ferrite magnetic material/cerium oxide core/shell composite state, thereby increasing the stability of the magnetic material. Sex.
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低，容易量產，製得的磁性材料純度較高且容易分散。 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 low, and mass production is easy, and the obtained magnetic material is high in purity and easy. dispersion.
第一圖為本發明磁性材料的製造方法一種實施例的流程圖。 The first figure is a flow chart of an embodiment of a method of manufacturing a magnetic material of the present invention.
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