TWI706151B - Magnetic evaluation method of permanent magnetic ferrite magnet - Google Patents
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本發明係關於一種磁性評估方法,特別是關於一種永磁鐵氧體磁石的磁性評估方法。The present invention relates to a magnetic evaluation method, in particular to a magnetic evaluation method of a permanent ferrite magnet.
近年來,隨著電子零部件的小型化、輕量化以及高性能化,對於由氧化物構成的永磁鐵氧體磁體,也不斷要求具有較高的磁氣特性。作為永磁鐵氧體磁體的磁氣特性之指標一般以剩磁(Br)以及本質矯頑磁力( iH c)作為指標。一直以來,為了達到高剩磁與高本質矯頑磁力的特性,永磁鐵氧體磁體中的元素成份組成之探討一直在進行著。 In recent years, with the reduction in size, weight, and performance of electronic components, permanent ferrite magnets made of oxides are also required to have high magnetic properties. As an indicator of the magnetic properties of permanent ferrite magnets, remanence (Br) and intrinsic coercivity ( i H c ) are generally used as indicators. For a long time, in order to achieve the characteristics of high remanence and high intrinsic coercivity, the composition of elements in permanent ferrite magnets has been discussed.
永磁鐵氧體的製造過程中包含一煆燒製程,其中煆燒(預燒)製程溫度高於磁石燒結溫度,於煆燒製程中就需得到反應完全的磁性相,才能夠於後續燒結製程完成後達到良好的磁特性。因此在生產永磁鐵氧體磁石製程中,通常會在煆燒製程結束後,就須先針對煆燒磁粉進行磁特性檢測,以評估煆燒磁粉的特性。若煆燒磁粉特性良好,則較有機會達到較佳之燒結後磁特性,反之則最終燒結磁石的磁特性也會較差,因此煆燒磁粉的磁特性檢測甚為重要。就現有的磁特性檢測方法主要有兩種,分別說明如下。The manufacturing process of permanent ferrite includes a sintering process. The temperature of the sintering (pre-sintering) process is higher than the sintering temperature of the magnet. In the sintering process, a fully reacted magnetic phase is required to be completed in the subsequent sintering process After achieving good magnetic properties. Therefore, in the process of producing permanent ferrite magnets, usually after the sintering process is completed, the magnetic properties of the sintered magnetic powder must be tested to evaluate the characteristics of the sintered magnetic powder. If the sintered magnetic powder has good properties, there is a better chance of achieving better magnetic properties after sintering. On the contrary, the magnetic properties of the final sintered magnet will also be poor. Therefore, the magnetic property detection of the sintered magnetic powder is very important. There are mainly two existing magnetic property detection methods, which are explained as follows.
對於第一種方式,主要是在製作到完成磁石的階段才通過磁性量測儀器(BH Tracer)評估磁石的磁特性,以此數據回推並判斷煅燒磁粉的性能。此方式所需檢測時間較長,例如微粉碎步驟就需要1~2日的工作天;微粉碎後磁粉漿料的調漿工序以及磁粉漿料於磁場成型後生胚的乾燥步驟需0.5日的工作天;磁體的燒結工序也需要1日工作天。因此,當最終以磁性量測儀器測得燒結磁石的磁特性至少需要3天的工作天。雖然以此方式準確度較高,因為可直接得到永磁鐵氧體磁石的最終磁特性,再依此磁特性可回推並準確判定永磁鐵氧體煆燒磁粉的特性好壞,但所需檢測時間太長,無法快速得到磁特性結果,進而無法於實驗室快速調整煅燒磁粉的材料配方與製程條件。For the first method, the magnetic properties of the magnet are evaluated by the magnetic measuring instrument (BH Tracer) mainly at the stage of the magnet being manufactured, and the performance of the calcined magnetic powder can be estimated and judged based on this data. This method requires a long detection time. For example, the fine pulverization step requires 1 to 2 working days; the sizing process of the magnetic powder slurry after the fine pulverization and the drying step of the green embryo after the magnetic powder slurry is formed in the magnetic field require 0.5 days of work Days; the sintering process of the magnet also requires 1 working day. Therefore, it takes at least 3 working days when the magnetic properties of the sintered magnet are finally measured with a magnetic measuring instrument. Although the accuracy is high in this way, because the final magnetic characteristics of the permanent ferrite magnet can be directly obtained, and then the magnetic characteristics can be used to back and accurately determine the characteristics of the permanent ferrite burned magnetic powder, but it needs to be tested The time is too long to obtain the magnetic properties results quickly, and the material formula and process conditions of the calcined magnetic powder cannot be quickly adjusted in the laboratory.
對於第二種方式,主要是在通過振動樣品磁性量測儀(vibrating sample magnetometer;VSM)之檢測方式來量測煅燒磁粉的磁特性,做為評估最終燒結磁石的代用特性,再依據VSM檢測結果回推並修正所製備之煅燒磁粉的材料配方與製程條件是否需修改。另外,對於永磁鐵氧體煆燒磁粉中可能會因為煆燒步驟不完全,造成煆燒後步驟之永磁鐵氧體煆燒磁粉中可能存在少許二價鐵離子(Fe 2+),而也會貢獻煅燒料於VSM量測所得之MS值(VSM所測得之MS值單位為emu/g),但Fe 2+在磁體燒結後會造成磁特性低落。因此,需另以滴定方式確認煆燒磁粉中之二價鐵離子的含量。此外,VSM的儀器昂貴,因此此種方式雖然可節省時間,但會增加產品的成本。 The second method is mainly to measure the magnetic properties of the calcined magnetic powder through the vibrating sample magnetometer (VSM) detection method, as an evaluation of the substitute properties of the final sintered magnet, and then based on the VSM test results Push back and revise whether the material formula and process conditions of the prepared calcined magnetic powder need to be modified. In addition, for the permanent ferrite sintered magnetic powder, the sintering step may be incomplete, resulting in a small amount of ferrite ions (Fe 2+ ) in the permanent ferrite sintered magnetic powder after the sintering step. Contribute to the MS value of the calcined material measured by the VSM (the unit of the MS value measured by the VSM is emu/g), but Fe 2+ will cause the magnetic properties of the magnet to deteriorate after the magnet is sintered. Therefore, another titration method is required to confirm the content of ferrous ions in the sintered magnetic powder. In addition, VSM instruments are expensive, so although this method can save time, it will increase the cost of the product.
故,有必要提供一種永磁鐵氧體磁石的磁性評估方法,以解決習用技術所存在的問題。Therefore, it is necessary to provide a magnetic evaluation method for permanent ferrite magnets to solve the problems existing in the conventional technology.
本發明之一目的在於提供一種永磁鐵氧體磁石的磁性評估方法,通過直接對永磁鐵氧體煆燒粉體進行一分析步驟,並且比對所得的一分析飽和磁化強度與一飽和磁化強度標準值之間的差異,以判斷後續獲得的永磁鐵氧體磁石的一磁力性質是否符合標準。若符合標準,則表示該永磁鐵氧體煆燒粉體可用來繼續進行製造永磁鐵氧體磁石的步驟;若不符合標準,則表示煆燒步驟需進行調整。One object of the present invention is to provide a method for evaluating the magnetic properties of permanent ferrite magnets, by directly performing an analysis step on the sintered powder of permanent ferrite, and comparing the obtained analytical saturation magnetization with a saturation magnetization standard The difference between the values to determine whether a magnetic property of the permanent ferrite magnet obtained subsequently meets the standard. If it meets the standard, it means that the permanent ferrite sintered powder can be used to continue the process of making permanent magnet ferrite magnets; if it does not meet the standard, it means that the sintering step needs to be adjusted.
為達上述之目的,本發明提供一種永磁鐵氧體磁石的磁性評估方法,包含步驟:提供一永磁鐵氧體煆燒粉體;對該永磁鐵氧體煆燒粉體進行一分析步驟,以獲得該永磁鐵氧體煆燒粉體的一分析飽和磁化強度;以及根據一資料庫中的一飽和磁化強度標準值比對該分析飽和磁化強度,其中:當該分析飽和磁化強度大於或等於該飽和磁化強度標準值,則判斷通過該永磁鐵氧體煆燒粉體製得的一永磁鐵氧體磁石的一磁力性質符合標準;或當該分析飽和磁化強度小於該飽和磁化強度標準值,則判斷通過該永磁鐵氧體煆燒粉體製得的該永磁鐵氧體磁石的該磁力性質不符合標準。To achieve the above objective, the present invention provides a method for evaluating the magnetic properties of a permanent ferrite magnet, which includes the steps of: providing a permanent ferrite sintered powder; performing an analysis step on the permanent ferrite sintered powder to Obtain an analytical saturation magnetization of the sintered permanent magnet ferrite powder; and compare the analytical saturation magnetization according to a saturation magnetization standard value in a database, wherein: when the analytical saturation magnetization is greater than or equal to the Saturation magnetization standard value, it is judged that a magnetic property of a permanent ferrite magnet obtained by sintering powder of the permanent ferrite meets the standard; or when the analytical saturation magnetization is less than the saturation magnetization standard value, then It is judged that the magnetic properties of the permanent ferrite magnet obtained by sintering the powder of the permanent ferrite do not meet the standard.
在本發明之一實施例中,該永磁鐵氧體煆燒粉體的該分析飽和磁化強度與該永磁鐵氧體磁石的該磁力性質之間呈一正相關關係。In an embodiment of the present invention, there is a positive correlation between the analytical saturation magnetization of the permanent ferrite sintered powder and the magnetic properties of the permanent ferrite magnet.
在本發明之一實施例中,該永磁鐵氧體磁石的該磁力性質包含剩磁(Br)、矯頑磁力( bH c)、本質矯頑磁力( iH c)及最大磁能積((BH) m)中的至少一種。 In an embodiment of the present invention, the magnetic properties of the permanent ferrite magnet include remanence (Br), coercive force ( b H c ), intrinsic coercive force ( i H c ) and maximum magnetic energy product (( BH) at least one of m ).
在本發明之一實施例中,該分析步驟包含:混合0.05至0.1重量份的一黏著劑、0.08至0.12重量份的一溶劑及99.78至99.87重量份的該永磁鐵氧體煆燒粉體以形成一分析試片;以及通過一磁性量測儀器分析該分析試片,以獲得該分析飽和磁化強度。In an embodiment of the present invention, the analysis step includes: mixing 0.05 to 0.1 parts by weight of an adhesive, 0.08 to 0.12 parts by weight of a solvent, and 99.78 to 99.87 parts by weight of the permanent ferrite to burn the powder to Forming an analysis test piece; and analyzing the analysis test piece by a magnetic measuring instrument to obtain the analysis saturation magnetization.
在本發明之一實施例中,該黏著劑包含一環氧樹脂以及該溶劑包含丙酮。In an embodiment of the present invention, the adhesive includes an epoxy resin and the solvent includes acetone.
在本發明之一實施例中,提供該永磁鐵氧體煆燒粉體的步驟包含步驟:提供一混合物,其中該混合物包含一氧化鐵粉及一鍶化物;進行一煅燒步驟,對該混合物以1220至1300 oC之間的溫度持溫達50至70分鐘之間以形成一前處理物;以及對該前處理物進行一粗粉碎步驟,以使該前處理物的一平均粒徑介於2至5微米之間形成該永磁鐵氧體煆燒粉體。 In an embodiment of the present invention, the step of providing the ferrite sintered powder includes the steps of: providing a mixture, wherein the mixture includes an iron oxide powder and a strontium compound; and performing a calcining step to use the mixture Hold the temperature between 1220 and 1300 o C for 50 to 70 minutes to form a pre-treatment product; and perform a coarse pulverization step on the pre-treatment product so that an average particle size of the pre-treatment product is between The permanent ferrite sintered powder is formed between 2 to 5 microns.
在本發明之一實施例中,該混合物更包含一鈷化物及一鑭化物中的至少一種。In an embodiment of the present invention, the mixture further includes at least one of a cobalt compound and a lanthanide compound.
在本發明之一實施例中,在提供該混合物的步驟中,更包含步驟:提供一添加劑,其中該添加劑包含碳酸鈣、氧化矽、五氧化二磷以及氧化硼中的至少一種。In an embodiment of the present invention, the step of providing the mixture further includes the step of providing an additive, wherein the additive includes at least one of calcium carbonate, silicon oxide, phosphorus pentoxide, and boron oxide.
在本發明之一實施例中,在判斷該分析飽和磁化強度大於或等於該飽和磁化強度標準值的步驟後,更包含步驟:進行一細粉碎步驟,其中該細粉碎步驟係細粉碎該永磁鐵氧體煆燒粉體,以使該永磁鐵氧體煆燒粉體的一平均粒徑介於0.65至0.75微米之間。In an embodiment of the present invention, after the step of determining that the analytical saturation magnetization is greater than or equal to the standard value of the saturation magnetization, the method further comprises a step of: performing a fine pulverization step, wherein the fine pulverization step is to pulverize the permanent magnet The ferrite sintered powder, so that the average particle size of the permanent ferrite sintered powder is between 0.65 and 0.75 microns.
在本發明之一實施例中,在進行該細粉碎步驟後,更包含步驟:對該永磁鐵氧體煆燒粉體進行一磁場配向成型步驟,以形成一胚體,其中該磁場配向成型步驟的一配向磁場強度係介於1.3至1.7特斯拉之間,一成型壓力係介於3至4噸/平方公分之間,以及一成型時間係介於90至110秒之間;以及進行一燒結步驟,對該胚體以介於1220至1240 oC之間的溫度持續燒結達50至70分鐘之間,以製得該永磁鐵氧體磁石。 In an embodiment of the present invention, after the fine pulverization step is performed, the method further includes the step of: performing a magnetic field alignment forming step on the permanent ferrite sintered powder to form an embryo body, wherein the magnetic field alignment forming step The intensity of an alignment magnetic field is between 1.3 and 1.7 Tesla, a molding pressure is between 3 and 4 tons/cm², and a molding time is between 90 and 110 seconds; and sintering step, the embryo body to a temperature between 1220 to 1240 o C of sintering duration between 50 and 70 minutes to prepare the hard ferrite magnets.
為了讓本發明之上述及其他目的、特徵、優點能更明顯易懂,下文將特舉本發明較佳實施例,並配合所附圖式,作詳細說明如下。再者,本發明所提到的方向用語,例如上、下、頂、底、前、後、左、右、內、外、側面、周圍、中央、水平、橫向、垂直、縱向、軸向、徑向、最上層或最下層等,僅是參考附加圖式的方向。因此,使用的方向用語是用以說明及理解本發明,而非用以限制本發明。In order to make the above and other objects, features, and advantages of the present invention more obvious and understandable, the following will specifically cite the preferred embodiments of the present invention, together with the accompanying drawings, and describe in detail as follows. Furthermore, the directional terms mentioned in the present invention, such as up, down, top, bottom, front, back, left, right, inside, outside, side, surrounding, center, horizontal, horizontal, vertical, vertical, axial, The radial direction, the uppermost layer or the lowermost layer, etc., are only the direction of reference to the attached drawings. Therefore, the directional terms used are used to describe and understand the present invention, rather than to limit the present invention.
請參照第1圖所示,本發明一實施例之永磁鐵氧體磁石的磁性評估方法10主要包含下列步驟11至13:提供一永磁鐵氧體煆燒粉體(步驟11);對該永磁鐵氧體煆燒粉體進行一分析步驟,以獲得該永磁鐵氧體煆燒粉體的一分析飽和磁化強度(步驟12);以及根據一資料庫中的一飽和磁化強度標準值比對該分析飽和磁化強度,其中:當該分析飽和磁化強度大於或等於該飽和磁化強度標準值,則判斷通過該永磁鐵氧體煆燒粉體製得的一永磁鐵氧體磁石的一磁力性質符合標準;或當該分析飽和磁化強度小於該飽和磁化強度標準值,則判斷通過該永磁鐵氧體煆燒粉體製得的該永磁鐵氧體磁石的該磁力性質不符合標準(步驟13)。本發明將於下文逐一詳細說明實施例之上述各步驟的實施細節及其原理。Please refer to Figure 1, the
本發明一實施例之永磁鐵氧體磁石的磁性評估方法10首先係步驟11:提供一永磁鐵氧體煆燒粉體。在本步驟11中,該永磁鐵氧體煆燒粉體例如可以通過下列步驟製得:提供一混合物,其中該混合物包含一氧化鐵粉及一鍶化物;進行一煅燒步驟,對該混合物以1220至1300
oC之間的溫度持溫達50至70分鐘之間以形成一前處理物;以及對該前處理物進行一粗粉碎步驟,以使該前處理物的一平均粒徑介於2至5微米之間形成該永磁鐵氧體煆燒粉體。在一實施例中,該混合物包含一氧化鐵粉及一鍶化物。在本步驟11中,該氧化鐵粉例如可以是一市售產品,亦可以是一鋼鐵製程中所產生的副產品,例如鋼鐵在進行熱加工時需將鐵表面所生成的鐵銹去除,而該鐵銹可作為該氧化鐵粉的來源。在一實施例中,該鍶化物例如可包含碳酸鍶。值得一提的是,所提供的該混合物主要用於生成鍶系鐵氧體磁粉。該煅燒步驟主要用於使該混合物在高溫反應,進行使該前處理物符合鍶系鐵氧體磁粉的分子式。在一實施例中,該前處理物的一分子式係SrO.nFe
2O
3,其中n介於5至6之間。在另一實施例中,進行該煅燒步驟處理時的一氣氛係包含5%的氧氣。
The
在一實施例中,該混合物還可包含一鈷化物及一鑭化物中的至少一種。具體而言,鈷化物中的鈷元素或是該鑭化物中的鑭元素,其皆有助於改質鐵氧體磁粉所製成的永磁鐵氧體磁石得到更高的剩磁(Br)、矯頑磁力( iH c)和矩形度(Hk/ iH c)。在一範例中,該鈷化物例如是氧化鈷(Co 3O 4)。在另一範例中,該鑭化物例如是氧化鑭(La 2O 3)。在本實施例中,該混合物經煅燒步驟後所形成的該前處理物的一分子式係(Sr 2+ 1-xLa 3+x)O.n(Fe 3+ 12-yCo 2+ y) 2O 3,其中n介於7至9之間,以及x=2ny,其中,x=2ny是La和Co元素分別取代Sr與Fe時所需滿足的電中性條件。在一具體範例中,x例如可介於0.15與0.16之間。在一實施例中,鈷化物可在後述的添加步驟中加入。 In one embodiment, the mixture may further include at least one of a cobalt compound and a lanthanide compound. Specifically, the cobalt element in the cobalt compound or the lanthanum element in the lanthanide compound contributes to the permanent ferrite magnet made of modified ferrite powder to obtain higher remanence (Br), Coercivity ( i H c ) and squareness (Hk/ i H c ). In an example, the cobalt compound is, for example, cobalt oxide (Co 3 O 4 ). In another example, the lanthanide is, for example, lanthanum oxide (La 2 O 3 ). In this embodiment, a molecular formula (Sr 2+ 1-x La 3+x )O. n(Fe 3+ 12-y Co 2+ y ) 2 O 3 , where n is between 7 and 9, and x=2ny, where x=2ny is required when La and Co elements replace Sr and Fe respectively Meet the electrical neutrality conditions. In a specific example, x may be between 0.15 and 0.16, for example. In one embodiment, the cobalt compound may be added in the adding step described later.
在一實施例中,在提供該混合物的步驟11以及進行該煅燒步驟12之前更包含對該混合物進行一脫水步驟,其中經該脫水步驟處理後的該混合物的含水率係介於18%至24%之間。In one embodiment, before the
本發明一實施例之永磁鐵氧體磁石的磁性評估方法10接著係步驟12:對該永磁鐵氧體煆燒粉體進行一分析步驟,以獲得該永磁鐵氧體煆燒粉體的一分析飽和磁化強度。在本步驟12中,該分析步驟可包含混合0.05至0.1重量份的一黏著劑、0.08至0.12重量份的一溶劑及99.78至99.87重量份的該永磁鐵氧體煆燒粉體以形成一分析試片;以及通過一磁性量測儀器分析該分析試片,以獲得該分析飽和磁化強度。在一實施例中,該磁性量測儀器例如是市售儀器(中國計量科學研究院NIM-2000型 B-H Loop Tracer)。在另一實施例中,該分析試片例如是圓餅狀(例如直徑1公分,厚度約大於0.7公分),該分析試片的厚度需高於市售儀器所用來測試之線圈高度,例如該線圈高度約為0.5公分)。在又一實施例中,該黏著劑包含一環氧樹脂以及該溶劑包含丙酮。在再一實施例中,形成該分析試片的步驟之後及分析該分析試片的步驟之前,可將該分析試片於烤箱中以100
oC烘烤約2小時,以去除多餘水分。
The
本發明一實施例之永磁鐵氧體磁石的磁性評估方法10最後係步驟13:根據一資料庫中的一飽和磁化強度標準值比對該分析飽和磁化強度,其中:當該分析飽和磁化強度大於或等於該飽和磁化強度標準值,則判斷通過該永磁鐵氧體煆燒粉體製得的一永磁鐵氧體磁石的一磁力性質符合標準;或當該分析飽和磁化強度小於該飽和磁化強度標準值,則判斷通過該永磁鐵氧體煆燒粉體製得的該永磁鐵氧體磁石的該磁力性質不符合標準。在本步驟13中,該資料庫中的飽和磁化強度標準值例如可先通過實驗確認。具體而言,首先製作多個永磁鐵氧體煆燒粉體,並且量測該些永磁鐵氧體煆燒粉體的飽和磁化強度(例如參考步驟12的製作方式)。接著,將該些永磁鐵氧體煆燒粉體分別製作成永磁鐵氧體磁石,並且利用磁性量測儀器進行量測,以測得該些永磁鐵氧體磁石的磁力性質。最後,判斷該些永磁鐵氧體磁石的磁力性質中是否具有符合標準(例如商用標準或者國際通用標準(如JIS C2501或JIS C2502等)的特性。若符合標準,則可將對應的永磁鐵氧體煆燒粉體的飽和磁化強度作為標準值。The
另一方面,根據上述方式,本案發明人得知該永磁鐵氧體煆燒粉體的該分析飽和磁化強度與該永磁鐵氧體磁石的該磁力性質之間呈一正相關關係。因此,若是該些永磁鐵氧體磁石的磁力性質同時包含符合標準與不符合標準的樣態,則可通過數學理論去推測永磁鐵氧體煆燒粉體的飽和磁化強度的數值對應於永磁鐵氧體磁石的磁力性質的標準值為何。舉例而言,例如分析兩個不同永磁鐵氧體煆燒粉體的飽和磁化強度分別為1400 高斯 (Gauss;簡稱G)與1600 G,而此兩個不同永磁鐵氧體煆燒粉體所製得的永磁鐵氧體磁石的剩磁分別為4200G與4800G。而若是永磁鐵氧體磁石的商用標準值最低為4500G,則可推測若是永磁鐵氧體煆燒粉體的飽和磁化強度大於等於1500G時,則其所製得的永磁鐵氧體磁石應可約略落於4500G。值得一提的是,除了剩磁具有此特性之外,其它磁力性質例如矯頑磁力( bH c)、本質矯頑磁力( iH c)及最大磁能積((BH) m)亦具有類似的正相關關係。因此,在通過上述方式後,即可建立出資料庫。此外,還可根據所使用的混合物不同、製程不同或比重不同等等分門別類的建立出各種資料庫,以利隨時進行磁性評估。 On the other hand, according to the above method, the inventor of the present case learned that the analytical saturation magnetization of the permanent ferrite sintered powder has a positive correlation with the magnetic properties of the permanent ferrite magnet. Therefore, if the magnetic properties of these permanent ferrite magnets include both conforming to the standard and not conforming to the standard, mathematical theory can be used to infer that the value of the saturation magnetization of the permanent ferrite sintered powder corresponds to the permanent magnet What is the standard value of the magnetic properties of the ferrite magnet? For example, for example, the saturation magnetization of two different permanent ferrite sintered powders is 1400 Gauss (Gauss; abbreviated as G) and 1600 G, and these two different permanent ferrite sintered powders are made The permanent magnet ferrite magnets obtained have remanence of 4200G and 4800G, respectively. And if the commercial standard value of permanent ferrite magnet is at least 4500G, it can be inferred that if the saturation magnetization of the permanent ferrite sintered powder is greater than or equal to 1500G, the permanent ferrite magnet produced should be approximately Falling on 4500G. It is worth mentioning that in addition to this characteristic of remanence, other magnetic properties such as coercive force ( b H c ), intrinsic coercive force ( i H c ) and maximum magnetic energy product ((BH) m ) also have similar properties The positive correlation. Therefore, after the above method, a database can be created. In addition, various databases can be established according to different mixtures, different manufacturing processes, or different specific gravity, etc., to facilitate magnetic evaluation at any time.
由上可知,本發明實施例的永磁鐵氧體磁石的磁性評估方法根據該飽和磁化強度標準值比對該分析飽和磁化強度,即可判斷後續所獲得的永磁鐵氧體磁石的磁力性質是否符合標準。此外,由於此種分析方法可在不需進行微粉碎步驟、乾燥步驟、燒結步驟的前提下就可預先得知後續所獲得的永磁鐵氧體磁石的磁力性質是否符合標準,故可節省時間成本。再者,這種方式不需使用VSM儀器,所以也可節省產品的製作成本。另外,由於本發明實施例之永磁鐵氧體磁石的磁性評估方法中分析飽和磁化強度的單位與最後獲得的磁石之磁特性Br單位相同,不需再經過換算。因此評估方式較為簡易,且可作為永磁鐵氧體之代用特性(Alternative Characteristic)。It can be seen from the above that the magnetic evaluation method of the permanent ferrite magnet of the embodiment of the present invention can judge whether the magnetic properties of the permanent ferrite magnet obtained subsequently conform to the saturation magnetization standard value of the saturation magnetization. standard. In addition, because this analysis method can know in advance whether the magnetic properties of the permanent ferrite magnets obtained later meet the standards without the need for fine pulverization, drying, and sintering steps, it can save time and cost. . Furthermore, this method does not require the use of VSM equipment, so it can also save the production cost of the product. In addition, since the unit of analyzing the saturation magnetization in the magnetic evaluation method of the permanent ferrite magnet of the embodiment of the present invention is the same as the unit of the magnetic characteristic Br of the finally obtained magnet, no conversion is required. Therefore, the evaluation method is relatively simple and can be used as the alternative characteristic of permanent ferrite.
以下舉出數個實施例與比較例,以證明本發明實施例之永磁鐵氧體磁石的磁性評估方法確實具有上述的效果。Several examples and comparative examples are listed below to prove that the magnetic evaluation method of the permanent ferrite magnet of the examples of the present invention does have the above-mentioned effects.
實施例1Example 1
首先,將主原料氧化鐵粉(Fe 2O 3)與另一種主原料碳酸鍶(SrCO 3)以SrO·nFe 2O 3(n=5.9)之基本組成進行配料,另同時加入4.9wt%的微量添加劑La 2O 3及水進行混合後,以料球重量比為1:5的市售球磨機(Ball Mill)混磨2小時後出料得到漿料狀態的混合物,鋼球為直徑3/16英吋的無鉻軸承鋼球。接著,將上述的混合物以市售空氣壓濾機進行脫水,脫水後的混合物的含水率約21±3%。 First, the main raw material iron oxide powder (Fe 2 O 3 ) and another main raw material strontium carbonate (SrCO 3 ) are blended with the basic composition of SrO·nFe 2 O 3 (n=5.9), and 4.9wt% of After the trace additive La 2 O 3 and water are mixed, the mixture is mixed and milled with a commercially available ball mill (Ball Mill) with a weight ratio of 1:5 for 2 hours, and then the material is discharged to obtain a mixture in a slurry state. The steel ball is 3/16 in diameter. Inch chromium-free bearing steel balls. Next, the above-mentioned mixture is dehydrated with a commercially available air filter press, and the moisture content of the dehydrated mixture is about 21±3%.
接著,將脫水後的混合物進行煅燒步驟。以一市售烘乾機對該混合物進行預熱,其中烘乾機之溫度為300±10 oC,持溫時間為30至40分鐘,經過烘乾後的混合物含水率小於2%。之後,將該混合物放入一市售旋窯進行煅燒以形成一前處理物,煅燒溫度約為1230 oC,煅燒時間為1小時,且煅燒時旋窯內之氧氣含量約5%。煅燒後之前處理物尺寸約介於0.5公分及1公分之間。 Next, the dehydrated mixture is subjected to a calcination step. Preheat the mixture with a commercially available dryer, where the temperature of the dryer is 300 ± 10 o C, the temperature holding time is 30 to 40 minutes, and the moisture content of the mixture after drying is less than 2%. After that, the mixture is calcined in a commercially available rotary kiln to form a pre-treatment material. The calcination temperature is about 1230 o C, the calcination time is 1 hour, and the oxygen content in the rotary kiln is about 5%. After calcination, the size of the processed material is between 0.5 cm and 1 cm.
將經過旋窯煅燒之前處理物通過與旋窯相連結的溜管送入冷卻桶中進行冷卻。在前處理物的溫度降至90 oC以下時,通過裝置有旋風收集器之風選功能的松永式球磨機(Roller Mill)進行粗粉碎步驟以獲得永磁鐵氧體煆燒粉體,其中永磁鐵氧體煆燒粉體的平均粒徑約為2至5微米之分佈。 The processed material before being calcined in the rotary kiln is sent to the cooling barrel for cooling through the slide pipe connected with the rotary kiln. When the temperature of the pre-treatment material drops below 90 o C, a coarse pulverization step is carried out by a Roller Mill equipped with a wind separation function of a cyclone collector to obtain the permanent ferrite sintered powder, in which the permanent magnet The average particle size of the sintered oxygen powder is about 2 to 5 microns.
以市售儀器(中國計量科學研究院NIM-2000型 B-H Loop Tracer)檢測一部分的煆燒磁粉之代用特性。具體如下,將99.78至99.87重量份之永磁鐵氧體煆燒粉體,混合0.05至0.1重量份之環氧樹脂(Epoxy)做為黏著劑,混合過程中加入0.1重量份丙酮做為溶劑。在混合攪拌後,以手動乾式成型成為圓餅狀試片後(例如直徑1公分,厚度約大於0.7公分)。之後,再將試片於烤箱中以約100 oC烘烤約2小時後,再以市售儀器測量試片之飽和磁化強度(Saturation Magnetisation,Js,以Gauss為單位),所測得之JS值為1560G。 A commercially available instrument (NIM-2000 BH Loop Tracer of the Chinese Academy of Metrology) was used to detect the substitution characteristics of a part of the braised magnetic powder. The details are as follows: the permanent magnet ferrite of 99.78 to 99.87 parts by weight is sintered powder, 0.05 to 0.1 parts by weight of epoxy resin (Epoxy) is mixed as an adhesive, and 0.1 part by weight of acetone is added as a solvent during the mixing process. After mixing and stirring, it is manually dry-formed into a round cake-shaped test piece (for example, a diameter of 1 cm and a thickness of more than 0.7 cm). After that, the test piece was baked in an oven at about 100 o C for about 2 hours, and then the saturation magnetization (Saturation Magnetisation, Js, in Gauss) of the test piece was measured with a commercially available instrument, and the measured JS The value is 1560G.
之後,在剩餘部分的煆燒磁粉加入添加劑(例如Co 3O 4、CaCO 3、SiO 2或B 2O 3)中,於球磨機(Ball Mill)以料球重量比為1:12,濕式研磨25小時進一步進行細粉碎步驟,以使該改質鐵氧體磁粉的平均粒徑約為0.65至0.75微米之間,其中鋼球為直徑3/16英吋的無鉻軸承鋼球。 After that, add additives (such as Co 3 O 4 , CaCO 3 , SiO 2 or B 2 O 3 ) to the remaining part of the sintered magnetic powder, and use a ball mill with a weight ratio of 1:12 for wet grinding. A further fine pulverization step is performed for 25 hours, so that the average particle size of the modified ferrite magnetic powder is about 0.65 to 0.75 microns, and the steel ball is a chromium-free bearing steel ball with a diameter of 3/16 inches.
接著,進行(濕式)磁場配向成型步驟,使用市售的25噸之半自動濕式磁場成型機,對該該永磁鐵氧體煆燒粉體進行磁場配向成型,配向磁場強度為1.5特斯拉(Telsa),成型壓力為3.5噸/平方公分(Ton/cm 2),胚體尺寸為長度6公分、寬度4公分、拱高2公分、厚度約0.7公分之瓦片型胚體。 Next, proceed to the (wet) magnetic field alignment molding step, using a commercially available 25-ton semi-automatic wet magnetic field molding machine to perform magnetic field alignment molding on the permanent ferrite sintered powder, the alignment magnetic field intensity is 1.5 Tesla (Telsa), the molding pressure is 3.5 tons/square centimeter (Ton/cm 2 ), and the size of the embryo body is a tile-shaped embryo body with a length of 6 cm, a width of 4 cm, an arch height of 2 cm, and a thickness of about 0.7 cm.
最後,進行一燒結步驟,對該胚體以1240 oC的溫度持續燒結達60分鐘,以製得該永磁鐵氧體磁石。以市售儀器(中國計量科學研究院NIM-2000型 B-H Loop Tracer)檢測該永磁鐵氧體磁石的各個磁力性質,說明如下表一。 Finally, a sintering step, the embryo temperature of 1240 o C for 60 minutes continuous sintering, to produce the ferrite permanent magnet. The magnetic properties of the permanent ferrite magnet were tested with a commercially available instrument (NIM-2000 BH Loop Tracer of the Chinese Academy of Metrology), as described in Table 1 below.
表一
實施例2至4Examples 2 to 4
實施例2至4的製作方式與實施例1類似,惟其不同之處在於所使用的組成比例不同,煆燒溫度不同,其可參照上表一。The manufacturing methods of Examples 2 to 4 are similar to that of Example 1, but the difference lies in the different composition ratios and different sintering temperatures, which can be referred to Table 1 above.
由上表一可知,實施例1至4中的永磁鐵氧體煆燒粉體的分析飽和磁化強度確實與通過該永磁鐵氧體煆燒粉體製得的永磁鐵氧體磁石的磁力性質具有正相關。當分析飽和磁化強度越高時,則永磁鐵氧體磁石的磁力性質(例如剩磁(Br)、矯頑磁力( bH c)、本質矯頑磁力( iH c)或最大磁能積((BH) m))也隨之越高。換言之,本發明實施例的永磁鐵氧體磁石的磁性評估方法可根據該飽和磁化強度標準值比對該分析飽和磁化強度,即可判斷後續所獲得的永磁鐵氧體磁石的磁力性質是否符合標準。 From Table 1 above, it can be seen that the analytical saturation magnetization of the permanent ferrite sintered powder in Examples 1 to 4 is indeed the same as the magnetic properties of the permanent ferrite magnet obtained by the permanent ferrite sintered powder system. Positive correlation. When the saturation magnetization is analyzed, the magnetic properties of the permanent ferrite magnet (such as remanence (Br), coercive force ( b H c ), intrinsic coercive force ( i H c ) or maximum magnetic energy product (( BH) m )) is also higher. In other words, the magnetic evaluation method of the permanent ferrite magnet of the embodiment of the present invention can compare the saturation magnetization of the analysis according to the saturation magnetization standard value to determine whether the magnetic properties of the permanent ferrite magnet obtained subsequently meet the standard. .
另外要提到的是,本發明實施例的磁性評估方法適用於永磁鐵氧體的磁力性質的評估,而無法適用於軟磁材料。In addition, it should be mentioned that the magnetic evaluation method of the embodiment of the present invention is suitable for the evaluation of the magnetic properties of permanent magnet ferrite, but cannot be applied to soft magnetic materials.
雖然本發明已以較佳實施例揭露,然其並非用以限制本發明,任何熟習此項技藝之人士,在不脫離本發明之精神和範圍內,當可作各種更動與修飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。Although the present invention has been disclosed in preferred embodiments, it is not intended to limit the present invention. Anyone who is familiar with the art can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the present invention The scope of protection shall be subject to the scope of the attached patent application.
10:方法10: method
11~13:步驟11~13: Steps
第1圖是本發明一實施例之永磁鐵氧體磁石的磁性評估方法之流程方塊圖。FIG. 1 is a block diagram of the magnetic evaluation method of a permanent ferrite magnet according to an embodiment of the present invention.
10:方法 10: method
11~13:步驟 11~13: Steps
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WO2014058067A1 (en) * | 2012-10-11 | 2014-04-17 | Tdk株式会社 | Sr ferrite powder, method for manufacturing sr ferrite sintered magnet, motor, and generator |
US20150125700A1 (en) * | 2012-06-07 | 2015-05-07 | Tdk Corporation | METHOD FOR MANUFACTURING Sr FERRITE PARTICLE FOR SINTERED MAGNET, METHOD FOR USING Sr FERRITE PARTICLE, Sr FERRITE SINTERED MAGNET AND METHOD FOR MANUFACTURING SAME, AND MOTOR AND GENERATOR |
CN106116560A (en) * | 2016-06-28 | 2016-11-16 | 南通万宝实业有限公司 | The preparation method of permanent-magnet ferrite magnetic material |
TW201704769A (en) * | 2015-07-28 | 2017-02-01 | 中國鋼鐵股份有限公司 | Measuring method of powder magnetic property and measuring base thereof |
TWI636016B (en) * | 2017-10-13 | 2018-09-21 | 中國鋼鐵股份有限公司 | Methods of fabricating modified iron oxide powder and fabricating ferrite magnet |
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2019
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US20150125700A1 (en) * | 2012-06-07 | 2015-05-07 | Tdk Corporation | METHOD FOR MANUFACTURING Sr FERRITE PARTICLE FOR SINTERED MAGNET, METHOD FOR USING Sr FERRITE PARTICLE, Sr FERRITE SINTERED MAGNET AND METHOD FOR MANUFACTURING SAME, AND MOTOR AND GENERATOR |
WO2014058067A1 (en) * | 2012-10-11 | 2014-04-17 | Tdk株式会社 | Sr ferrite powder, method for manufacturing sr ferrite sintered magnet, motor, and generator |
TW201704769A (en) * | 2015-07-28 | 2017-02-01 | 中國鋼鐵股份有限公司 | Measuring method of powder magnetic property and measuring base thereof |
CN106116560A (en) * | 2016-06-28 | 2016-11-16 | 南通万宝实业有限公司 | The preparation method of permanent-magnet ferrite magnetic material |
TWI636016B (en) * | 2017-10-13 | 2018-09-21 | 中國鋼鐵股份有限公司 | Methods of fabricating modified iron oxide powder and fabricating ferrite magnet |
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