A6 B6 213492 五、發明說明（; 本發明係間於一種磁性金屬粉末的安定化方法，更特別的，係關於一 安定化方法，其可使處理後之磁性金属扮末具優良之安定性及分散性。 磁性金屬粉末廣泛應用於較高纪錄密度之錄影帶、錄音帶和磁碟月上 ’然而高記錄密度須很細之磁性金屬粉末，但粉末太細會有分散的困難， 且磁性金屬粉末非常容易氣化甚至起火燃燒，因此如何提高磁性金屬粉末 的安定性和分散性是急欲解決的問題。 曰本公開特許公報第Μ-wo⑽號揭窀了 Μ熱處理法來提高磁性金屬 粉末的安定性，此法須嚴格地控制熱處理的溫度和被熱處理物接觸之氣體 ，所得之磁性金屬粉末的保磁力約J5卯〇e,飽和磁化量約J如emw/g， 在讨候性試驗ί仰。C,相對漏度9似/?//下7天）後飽和磁化量約 112emu/g 〇曰本公開特許公報第Μ-烈犯似號揭露了以環狀腊肪族之一級胺化合物 被復於金屬粒子表面來提高其安定性，所得之磁性金屬粉末之饱和磁化责 約』24emu/g，在耐候性試驗（仰。c，相對濕度9狀/?//下7天）後飽和 磁化量約JJOemu/g，以上所得之磁性金屬粉末的安定性仍不足夠。 本發明之目的爲在提供具有優良之安定性及分散性之磁性金屬粉末的 安定化方法。 依據本發明方法，其為遺原磁性金屬扮末，將磁性金屬粉末在隔絕空 氣下浸清在有機溶刻中，直到磁性金屬粉末表面形成氣化層後，再將所得 之磁性金屬粉末與鈦鼗偶合則溶液充分攪拌，使磁性金屬粉末表面均勻吸 附一層鈦啟偶合則後，在空氣下乾燥之。 於本發明方法中，所謂遣原步驟係指長釉U〜U wm，短軸 〜O.Wum的針狀a-fe00//在空氣下聣水形成^ fe/3，之後在氮氟氣 流流量= 0.2 7/mh, 4卯。〇下J〜2小時轉變爲黑色厂勺〇4再遣原成 ot-fe磁性金屬粉末；將磁性金屬粉末在隔絕空氣下浸清在有機溶則步邾 ’係指將磁性金屬扮末置入遣原壚中並通氮氣，溫度保持在50-c以下， 使金屬粉末與空氣隔絕，再以導管注入有機溶則直完全埯沒該金屬粉末。 有機溶則之沸點若太低則揮發快速使鐵粉曝露於空氣中，所以須選擇沸點 甲 4(210X297 公发） (請先聞讀背面之注意事項再瑱寫本頁) .裝. .緣. 經濟部中央榡準局印$ A6 B6 2134^2 五、發明説明（ ） 较高之有機溶則（沸點大於JOO°C者），藉該有機溶則使慢揮發使磁性金 屬粉末表面與空氟接觸進而形成氣化膜（豉基j，有機溶則揮發速度直接影 響磁性金屬扮末之氣化速度與厚度，氧化脓成份爲與/τ~〇4之混合 物’膜厚爲30〜50埃；而在鈦漿偶合刻溶液步驟主要爲鈦氩偶合則中之 鍵，會與磁性金屬粉末表面之蹀基形成化學鍵結（爲一疏水性官能基) ，靠此疏水性官能基可令磁性金屬粉末在有機溶刻中分散均勻，並且該化 學鍵結可有效阻隔空氣與磁性金屬扮末接觸，進而提高磁性金屬粉末之抗 氡化力，以達安定磁性金屬粉末之功效。 於本發明方法中，所使用之鈦氬偶合刻其結構通式如下： (R1—〇)m—Ti (Ο —X—只之—, /7=J〜3 其中\和&爲由破數4〜仞之垸基組成，/爲暹自包含垸基、硤基 、磺睃氬、酚類和磷睃里的族群之一者，y爲熱固性官能基其烏選自包含 甲基丙烯基和胺類的族群之一者，鈦敷偶合則溶液由鈦氩偶合則和有機溶 刻所组成，有機溶創▼為甲笨或二甲笨，且鈦里偶合則溶液之濃度為介於 至，较佳之濃度爲找至，鈦氬偶合則常做爲固液 懸浮系統中之分散則或稿定剞，因此可提高磁性金屬粉末的安定性和分散 性。 本發明之內容將經由以下之例子作進一步之說明： 實施例1 經 »-ίτ :叱 部 中 央 標 準 Μ 印 (請先閲讀背面之注意事項再填寫本頁} 取20g針狀a-fe00H (長軸〇1〜〇3um短軸〇 〇1〜〇〇3_), 在溫度3〇0°C之空氟中稅水形成a-fe2〇3，然後在流量ο』溫 度4仰C之氩氣氟流下J〜£小時形成α-fe之磁性金屬粉末，直到該磁 性金屬粉末冷卻至5irc以下，於隖絕空氣下加入甲笨使磁性金屬粉末浸沒 在該溶則中，直到該溶則在空氣下完全揮發爲止。取結構式如下： 甲4(210X 297公发） A6 B6 2134C2 .五、發明說明（ > CH£ ^ CH—CH2〇—CH^ q q I ii ii CH3CH2—C—CH2—〇—Ti(〇—P—〇—P(〇C8H17)2)3 (LICA38)A6 B6 213492 V. Description of the invention (; The present invention is interposed between a method of stabilizing magnetic metal powder, and more particularly, it relates to a method of stabilizing, which can make the processed magnetic metal have excellent stability and Dispersibility. Magnetic metal powder is widely used in video tapes, audio tapes and magnetic discs with higher recording density. However, high recording density requires very fine magnetic metal powder, but if the powder is too fine, it will be difficult to disperse, and magnetic metal powder It is very easy to gasify or even ignite and burn, so how to improve the stability and dispersibility of magnetic metal powder is an urgent problem to be solved. Japanese Patent Publication No. M-wo⑽ revealed the M heat treatment method to improve the stability of magnetic metal powder This method requires strict control of the temperature of the heat treatment and the gas in contact with the object to be heat treated. The coercive force of the resulting magnetic metal powder is about J590m, and the saturation magnetization is about J, such as emw / g. .C, relative leakage 9% /? // Next 7 days) After saturation magnetization is about 112emu / g The compound is coated on the surface of the metal particles to improve its stability. The saturation magnetization of the resulting magnetic metal powder is about 24emu / g in the weather resistance test (Yang.c, relative humidity 9 /// Next 7 days) The amount of post-saturation magnetization is about JJOemu / g, and the stability of the magnetic metal powder obtained above is still insufficient. The object of the present invention is to provide a method for stabilizing magnetic metal powder having excellent stability and dispersibility. According to the method of the present invention, it is left as the original magnetic metal, and the magnetic metal powder is immersed in organic dissolution etching under the shielded air until the vaporized layer is formed on the surface of the magnetic metal powder, and then the obtained magnetic metal powder and titanium In the case of chelating coupling, the solution is fully stirred, so that the magnetic metal powder surface is evenly adsorbed with a layer of titanium to start coupling, and then it is dried in air. In the method of the present invention, the so-called stepping process refers to the needle-shaped a-fe00 of the long glaze U ~ U wm and the short axis ~ O. Wum /// formed under the air ^ fe / 3, and then the flow of nitrogen and fluorine gas flow = 0.2 7 / mh, 490. 〇Under J ~ 2 hours, it will be converted into black factory spoon. 〇4 Re-transform the original into ot-fe magnetic metal powder; immerse the magnetic metal powder in an organic solution under the isolation of air, then bu yong 'means to put the magnetic metal into the end Dissolve the nitrogen and keep the temperature below 50-c to isolate the metal powder from the air, and then inject organic solution through the catheter to completely disappear the metal powder. If the boiling point of the organic solvent is too low, the volatilization will quickly expose the iron powder to the air, so you must choose the boiling point A 4 (210X297 public issue) (please read the precautions on the back before writing this page). . Printed by the Central Bureau of Economics of the Ministry of Economic Affairs. $ A6 B6 2134 ^ 2 5. Description of the invention () Higher organic dissolution (boiling point greater than JOO ° C), by which the slow dissolution of the magnetic metal powder surface and empty Fluorine contacts to form a vaporized film (豉 基 j, organic solution, the volatilization rate directly affects the vaporization rate and thickness of the magnetic metal at the end, and the oxidized pus component is a mixture with / τ ~ 〇4) The film thickness is 30 ~ 50 Angstroms ; The coupling solution step in the titanium paste is mainly titanium-argon coupling, which will form a chemical bond (a hydrophobic functional group) with the radical on the surface of the magnetic metal powder. By this hydrophobic functional group can make the magnetic metal The powder is evenly dispersed in the organic solution etching, and the chemical bonding can effectively block the contact between the air and the magnetic metal, thereby improving the resistance to radonization of the magnetic metal powder, so as to stabilize the effect of the magnetic metal powder. In the method of the present invention, Used The general structure of titanium-argon coupling engraving is as follows: (R1—〇) m—Ti (Ο —X— Zhizhi—, / 7 = J ~ 3 where \ and & are composed of broken numbers 4 ~ / It is one of the ethnic groups in Siam self-contained emulsyl group, ketyl group, sulfonium argon, phenols and phosphoric acid, y is a thermosetting functional group and its group is selected from one of the groups containing methacryl groups and amines, Titanium coating coupling is composed of titanium argon coupling and organic dissolution etching, organic solvent wound ▼ is methyl stupid or dimethyl stupid, and in titanium coupling, the concentration of the solution is between to, the preferred concentration is to find, titanium Argon coupling is often used as the dispersion rule or draft in the solid-liquid suspension system, so it can improve the stability and dispersibility of the magnetic metal powder. The content of the present invention will be further explained by the following examples: Example 1 »-Ίτ: Chibe Central Standard M seal (please read the precautions on the back before filling in this page) Take 20g needle-shaped a-fe00H (long axis 〇1 ~ 〇3um short axis 〇〇1 ~ 〇〇3_), in A-fe2〇3 is formed in the tax water at a temperature of 300 ° C in empty fluorine, and then the α-fe is formed under a flow rate of argon gas at a temperature of 4 ° C under J ~ £ hours. Metal powder until the magnetic metal powder is cooled to below 5irc, add Jiaben under the air to immerse the magnetic metal powder in the solution until the solution is completely volatilized under air. Take the structural formula as follows: A 4 (210X 297 public) A6 B6 2134C2. V. Description of the invention (> CH £ ^ CH-CH2〇-CH ^ qq I ii ii CH3CH2-C-CH2-CH-Ti (〇-P-〇-P ( 〇C8H17) 2) 3 (LICA38)
I I CH之二 CH一CH2〇 —CH2 〇ff 之故敗偶合势l(美铒KENRICH PETROCHEMICALS INC.公司產品编说LICA38) 2d«溶於甲笨中，形成鈦里偶合則溶液，將上述所得之磁性金屬粉末置於 此溶液中，混合均勻後遽去液體於空氣中乾燥之。所得之安定化磁性金屬 粉末經振動試料嗖磁力計f測定磁場為5X0e j測試結果爲飽和磁化量（σ s >> J38emu/g，抗磁力f/Zc)為J65〇〇e ,經耐候性試驗（6iTC ,相對濕度 90°C則下7天）後飽和磁化量降低爲jjsemu/g ,飽和磁化量衰減率為 其結果如表一所示。 實施例2 重複實施例1之操作條件及步驊，惟其鈦氩偶合則之濃度為3.5α%， 所得之磁性金屬粉末之測試條件如實施例1所述，結果如表一所示。 實施例3 重複實施例1之操作條件及步鶊，惟其鈦風偶合則（產品來源如實施 例1，產品编號/·Κ/Ι97 J之結構式改變如下： CH2=CH—CH2〇—CH2II CH 2 CH-CH2〇-CH2 〇ff's failure coupling potential l (US Erken KENRICH PETROCHEMICALS INC. Product editor LICA38) 2d «dissolve in a stupid, to form a titanium coupling solution, the above obtained The magnetic metal powder is placed in this solution, mixed evenly, and then the liquid is removed and dried in the air. The obtained stabilized magnetic metal powder was measured by a vibrating sample swish magnetometer f to determine the magnetic field is 5X0e j. The test result is the saturation magnetization (σ s > > J38emu / g, coercive force f / Zc) is J65〇〇e, after weathering After the sex test (6iTC, relative humidity 90 ° C, then 7 days), the saturation magnetization decreased to jjsemu / g, and the saturation magnetization attenuation rate is shown in Table 1. Example 2 The operating conditions and steps of Example 1 were repeated, but the concentration of titanium-argon coupling was 3.5α%. The test conditions of the obtained magnetic metal powder were as described in Example 1, and the results are shown in Table 1. Example 3 The operating conditions and steps of Example 1 were repeated, but the titanium wind coupling was used (the product source is as in Example 1, the structural formula of the product number / · Κ / Ι97 J was changed as follows: CH2 = CH—CH2〇—CH2
I CH 3CH 2~C~CH 2—0—T i(〇—C6H4—NH2)3 (LICA97)I CH 3CH 2 ~ C ~ CH 2—0—T i (〇—C6H4—NH2) 3 (LICA97)
I CH2=CH—CH2〇~CH2 甲 4(210X297 公犮） 請先閲讀背面之注意事項再填寫本頁) .5t· .蟓. 經濟部中央標準局印$1I CH2 = CH—CH2〇 ~ CH2 A 4 (210X297 Gonglu) Please read the precautions on the back before filling out this page. .5t ·. 蟓. Printed by the Central Bureau of Standards of the Ministry of Economic Affairs $ 1
2134C :飞 A6 五、發明說明（ ) 所得之磁性金屬粉末之測試條件如實施例i所述，結果如表一所示。 锖先聞绅背面之注意事項再填寫本頁) 比較實例1 σ-fe磁性金4粉末的製锖如實施例1之操作條件及步邾，但不施以 甲笨和鈦鬣偶合則處理，導致a_fe磁性金屬粉末產生自發性燃燒，結果 如表一所示。 比較實例2 a-fe磁性金属粉末的製備如實施例1之操作條件及步驟後，僅以甲 笨處理不加鈦盥偶合則，所得磁性金屬粉末特性如表一所示。 比較實例3 a-fe磁性金屬粉末的製備如實施例1之操作條件及步邾後，僅以鈦 啟偶合則處理不加f笨，所得磁性金屬粉末特性如表一所示。 表一 實施例 處理條件 處理後之特性 職生嫌後之特性 (60°C, 90%RH，7天) as(emu/g) 表減率 as(emu/g) Hc(Oe) as(emu/g) 1 2wt% LICA38 138 1650 118 14.5% 2 3.5wt% LICA38 133 1630 114 14.3% 3 2wt% LICA97 138 1660 117 15.2% 比较實例1 未加處理 饋生職 比较實例2 只加甲笨 130 1600 97 25.4% 比较實例3 只加飲盥偶合则 102 1400 71 30.4% 甲 4 (210X297 乂韙） A6 B6 五、洤明説明ί ) 由表一數據得知，經本發明方法處理遇之磁性金屬粉末比未處理或只 施以部份處理有較高之飽和磁化责，在經耐候性試驗印°c，相對滋度9敗 /?//之條件7天後之測試結果頤示，經本發明方法處理後之磁性金屬扮末有 较低之衰減皁，相對即提高磁性金屬粉末的安定性。又有待言者，凡依本 發明申請專利範团之特徵及精神所做之各種變化及修飾，皆應可屬本發明 涵蓋之範固〇 請先閱讀背面之注专事項再填寫本頁) 經濟部中央標準局印製 甲4(2ΐ〇χ 297 2超）2134C: Fei A6 V. Description of the invention () The test conditions of the obtained magnetic metal powder are as described in Example i, and the results are shown in Table 1. Please read the notes on the back of the gentry first, and then fill out this page) Comparative Example 1 The preparation of σ-fe magnetic gold 4 powder is performed as in the operating conditions and steps of Example 1, but it is not treated by the coupling of Jiaben and Titanium, This resulted in spontaneous combustion of a_fe magnetic metal powder. The results are shown in Table 1. Comparative Example 2 Preparation of a-fe magnetic metal powder After the operating conditions and steps of Example 1, only the treatment with methylbenzene and no titanium coupling was performed. The characteristics of the obtained magnetic metal powder are shown in Table 1. Comparative Example 3 Preparation of a-fe magnetic metal powder As in the operating conditions and steps of Example 1, only coupling with titanium is performed without treatment, and the characteristics of the obtained magnetic metal powder are shown in Table 1. Table 1 Examples of treatment conditions The characteristics of the post-treatment students (60 ° C, 90% RH, 7 days) as (emu / g) Table decrease rate as (emu / g) Hc (Oe) as (emu / g) 1 2wt% LICA38 138 1650 118 14.5% 2 3.5wt% LICA38 133 1630 114 14.3% 3 2wt% LICA97 138 1660 117 15.2% 25.4% Comparative Example 3 Only drinking and drinking couplet 102 1400 71 30.4% A 4 (210X297 乂 韪) A6 B6 V. Description of the source) According to the data in Table 1, the magnetic metal powder treated by the method of the present invention is better than Treatment or only partial treatment has a higher saturation magnetization responsibility. After the weather resistance test prints ° C, the relative humidity is 9 failures /? // The test results are shown after 7 days, after treatment by the method of the present invention The magnetic metal has lower attenuation soap, which relatively improves the stability of the magnetic metal powder. It remains to be said that all changes and modifications made according to the characteristics and spirit of the patent application group of the present invention should be included in the scope of the invention. Please read the notes on the back and then fill out this page) Economy The Central Bureau of Standards of the People's Republic of China prints Armor 4 (2 × 297 2)