TWI437590B - Wide temperature type and low hysteresis coefficient of the magnetic core manufacturing methods - Google Patents
Wide temperature type and low hysteresis coefficient of the magnetic core manufacturing methods Download PDFInfo
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本發明是有關於一種磁蕊的製造方法,特別是指一種寬溫型且低磁滯係數之磁蕊的製造方法。The present invention relates to a method for manufacturing a magnetic core, and more particularly to a method for manufacturing a magnetic core having a wide temperature type and a low hysteresis coefficient.
非對稱數位式用戶線路(Asymmetric Digital Subscriber Line,ADSL)是現有資訊傳輸主流,其中,傳輸用的寬頻變壓器更是ADSL的必要配備,因此,連帶使得用以寬頻傳輸的磁蕊需求量大增。Asymmetric Digital Subscriber Line (ADSL) is the mainstream of existing information transmission. Among them, the broadband transformer for transmission is a necessary equipment for ADSL. Therefore, the demand for magnetic core for broadband transmission is greatly increased.
然而,由於ADSL的使用區域遍布全球,因此,用以寬頻傳輸之磁蕊不僅在常溫(25℃)下要能夠達成其導磁率(Permeability,μ)的要求,甚至在-40℃~100℃的環境溫度下,其導磁率(μi-40℃~100℃ )也要能儘量維持一定,使導磁率隨溫度的變化率(亦即導磁率溫度係數)愈小愈能穩定控制磁路。再者,隨著ADSL的傳輸距離愈來愈長,因此,必需減少用以寬頻傳輸之磁蕊的磁滯係數(ηB),才能達成傳輸時分離度高、不失真及穩定性佳之要求。However, since the use area of ADSL is spread all over the world, the magnetic core used for broadband transmission is required to achieve the permeability (μ) of the magnetic core at room temperature (25 ° C), even at -40 ° C to 100 ° C. At ambient temperature, the magnetic permeability (μi -40 ° C ~ 100 ° C ) should be maintained as much as possible, so that the smaller the rate of change of magnetic permeability with temperature (that is, the temperature coefficient of magnetic permeability), the more stable the control of the magnetic circuit. Furthermore, as the transmission distance of ADSL is longer and longer, it is necessary to reduce the hysteresis coefficient (ηB) of the magnetic core for broadband transmission, so as to achieve high separation, no distortion and good stability in transmission.
參閱圖1、2,現有低磁滯係數錳鋅軟磁磁粉在25℃~100℃之間的導磁率介於3100~3600之間,相對磁滯係數是介於0.29×10-6 ~0.32×10-6 之間,但是,現有低磁滯係數錳鋅軟磁磁粉是-40℃時的導磁率偏低僅有1907,而且在-40℃~10℃之間的磁滯係數竟高達0.44×10-6 ~1.16×10-6 之間。Referring to Figures 1 and 2, the magnetic permeability of the existing low hysteresis coefficient Mn-Zn soft magnetic powder between 25 °C and 100 °C is between 3100 and 3600, and the relative hysteresis coefficient is between 0.29×10 -6 and 0.32×10. Between -6 , however, the existing low hysteresis coefficient Mn-Zn soft magnetic powder is only 1907 when the magnetic permeability is low at -40 °C, and the hysteresis coefficient between -40 °C and 10 °C is as high as 0.44×10 - 6 ~ 1.16 × 10 -6 .
同時現有低磁滯係數錳鋅軟磁磁粉在-20℃~25℃之間的導磁率溫度係數(α-20℃~25℃ )的絕對值高達3×10-6 ,也容易造成訊號傳輸失真,因此,現有低磁滯係數錳鋅軟磁磁粉並不適用寒帶地區。At the same time, the absolute value of the magnetic permeability temperature coefficient (α -20 ° C ~ 25 ° C ) of the existing low hysteresis coefficient Mn - Zn soft magnetic powder between -20 ° C and 25 ° C is as high as 3 × 10 -6 , which is also likely to cause signal transmission distortion. Therefore, the existing low hysteresis coefficient manganese-zinc soft magnetic powder is not suitable for the cold zone.
為改善上述現有低磁滯係數錳鋅軟磁磁粉的缺點,相關業者研發出如中華人民共和國公開第CN101894650A號「一種寬溫高磁導率低失真軟磁鐵氧體」發明專利申請案,其主成分的莫耳百分比以氧化物計算為:52.7~53.5mol%的氧化鐵(Fe2 O3 )、22.5~24mol%的氧化鋅(ZnO),其餘的氧化錳(MnO);副成分的重量百分比以氧化物計算為:0.08~0.2wt%的氧化錫(SnO2 )、0.04~0.06wt%的氧化鈣(CaO),以及0.04~0.06wt%氧化釩(V2 O5 )。In order to improve the above-mentioned shortcomings of the existing low hysteresis coefficient Mn-Zn soft magnetic magnetic powder, the related art has developed a patent application for a wide temperature, high magnetic permeability and low distortion soft ferrite as disclosed in the Chinese Patent Publication No. CN101894650A, the main component of which is The percentage of moles is calculated as oxides: 52.7 to 53.5 mol% of iron oxide (Fe 2 O 3 ), 22.5 to 24 mol% of zinc oxide (ZnO), and the remaining manganese oxide (MnO); The oxide is calculated as: 0.08 to 0.2 wt% of tin oxide (SnO 2 ), 0.04 to 0.06 wt% of calcium oxide (CaO), and 0.04 to 0.06 wt% of vanadium oxide (V 2 O 5 ).
該寬溫高磁導率低失真軟磁鐵氧體於10KHz、-55℃~85℃的導磁率(μi10KHz、-55℃~85℃ )大於5000,常溫磁滯係數(ηB25℃ )小於0.3×10- 6/mT。The magnetic permeability of the wide temperature, high magnetic permeability and low distortion soft ferrite at 10KHz, -55°C to 85°C (μi 10KHz, -55°C to 85°C ) is greater than 5000, and the hysteresis coefficient at room temperature (ηB 25°C ) is less than 0.3. ×10 - 6/mT.
由上述可知,利用材料成分配比的改變,以開發出適用於寬溫度範圍之高導磁率低磁滯係數的磁蕊,確實為相關業者努力的目標。From the above, it has been found that the use of a change in the distribution ratio of the material to develop a magnetic core having a high magnetic permeability and a low hysteresis coefficient suitable for a wide temperature range is indeed an objective of the related art.
因此,本發明之目的,即在提供一種寬溫型且低磁滯係數之磁蕊的製造方法。Accordingly, it is an object of the present invention to provide a method of manufacturing a magnetic core having a wide temperature type and a low hysteresis coefficient.
於是,本發明寬溫型且低磁滯係數之磁蕊的製造方法,包含下列步驟:(A)將一主原料進行煆燒,該主原料含有總合為100 mol%的氧化鐵、氧化錳與氧化鋅,其中,氧化鐵為52.35mol%~52.55 mol%,而氧化錳與氧化鋅之莫耳百分比之比值介於1.35~1.38之間;(B)將一副原料加入該主原料成為一混合料,其中,該副原料含有佔該混合料0.04wt%的氧化鈣,與佔該混合料0.02 wt%的氧化鋯;(C)將該混合料進行研磨且添加黏結劑形成顆粒;(D)利用模具將顆粒成型為生胚;(E)將該生胚燒結成磁蕊。Therefore, the method for producing a wide-temperature and low hysteresis magnetic core of the present invention comprises the following steps: (A) calcining a main raw material containing 100 mol% of iron oxide and manganese oxide in total And zinc oxide, wherein the iron oxide is 52.35mol%~52.55 mol%, and the ratio of the molar percentage of manganese oxide to zinc oxide is between 1.35 and 1.38; (B) adding a raw material to the main raw material to become a a mixture, wherein the auxiliary material contains 0.04% by weight of calcium oxide of the mixture, and 0.02% by weight of zirconia; (C) grinding the mixture and adding a binder to form particles; (D) The mold is used to form the pellet into a green embryo; (E) the green embryo is sintered into a magnetic core.
本發明的有益效果在於:利用主原料、副原料與黏結劑的成分配比,經煆燒、混合、研磨、造粒、成型...等過程後燒結成磁蕊,使該磁蕊於-40℃~100℃之導磁率介於3200~4800之間,且-20℃~25℃之導磁率溫度係數的絕對值小於7.0×10-7 ,而25℃~60℃導磁率溫度係數的絕對值小於0.45×10-7 ,-40℃~100℃之磁滯係數小於0.75×10-6 ,以及25℃之磁滯係數小於0.6×10-6 。The beneficial effects of the invention are: using the distribution ratio of the main raw material, the auxiliary raw material and the bonding agent, and sintering into a magnetic core after being calcined, mixed, ground, granulated, formed, etc., so that the magnetic core is in- The magnetic permeability of 40 ° C ~ 100 ° C is between 3200 ~ 4800, and the absolute value of the temperature coefficient of permeability of -20 ° C ~ 25 ° C is less than 7.0 × 10 -7 , and the absolute temperature coefficient of magnetic permeability of 25 ° C ~ 60 ° C The value is less than 0.45×10 -7 , the hysteresis coefficient of -40°C~100°C is less than 0.75×10 -6 , and the hysteresis coefficient of 25°C is less than 0.6×10 -6 .
有關本發明之前述及其他技術內容、特點與功效,在以下配合參考圖式之一個較佳實施例的詳細說明中,將可清楚的呈現。The above and other technical contents, features and advantages of the present invention will be apparent from the following detailed description of the preferred embodiments.
參閱圖3,本發明寬溫型且低磁滯係數之磁蕊的製造方法之較佳實施例,首先,如步驟21所示,將一主原料經900℃煆燒,該主原料含有總合為100 mol%的氧化鐵(Fe2 O3 )、氧化錳(MnO)與氧化鋅(ZnO),其中,氧化鐵為52.35mol%~52.55mol%,而氧化錳與氧化鋅之莫耳百分比之比值介於1.35~1.38之間。Referring to FIG. 3, in a preferred embodiment of the method for manufacturing a wide-temperature and low hysteresis magnetic core of the present invention, first, as shown in step 21, a main raw material is calcined at 900 ° C, and the main raw material contains a total of It is 100 mol% of iron oxide (Fe 2 O 3 ), manganese oxide (MnO) and zinc oxide (ZnO), wherein iron oxide is 52.35 mol% to 52.55 mol%, and the percentage of molybdenum oxide and zinc oxide is The ratio is between 1.35 and 1.38.
接下來,如步驟22所示,將一副原料加入該主原料成為一混合料,其中,該副原料含有佔該混合料0.04wt%的氧化鈣(CaO)、佔該混合料0.02 wt%的氧化鋯(ZrO2 )、佔該混合料0.02wt%至0.08 wt%的氧化鈦(TiO2 ),與佔該混合料0.02 wt%至0.05 wt%的氧化鈷(CoO)。Next, as shown in step 22, a raw material is added to the main raw material to form a mixture, wherein the auxiliary raw material contains 0.04% by weight of calcium oxide (CaO) of the mixture, and 0.02% by weight of the mixture. Zirconium oxide (ZrO 2 ), 0.02 wt% to 0.08 wt% of titanium oxide (TiO 2 ), and 0.02 wt% to 0.05 wt% of cobalt oxide (CoO) based on the mixture.
其中,添加氧化鈣與氧化鋯能增加晶界電阻,而添加氧化鈦與氧化鈷則是用以改善低溫的導磁率與磁滯係數。Among them, the addition of calcium oxide and zirconia can increase the grain boundary resistance, while the addition of titanium oxide and cobalt oxide is used to improve the magnetic permeability and hysteresis coefficient of low temperature.
然後,如步驟23所示,將該混合料進行濕式研磨且添加1wt%聚乙烯醇(Polyvinyl Alcohol)作為黏結劑,並經手工過篩形成粒徑介於80μm~240μm之間的顆粒。Then, as shown in step 23, the mixture was wet-milled and 1 wt% of polyvinyl alcohol (Polyvinyl Alcohol) was added as a binder, and manually sieved to form particles having a particle diameter of between 80 μm and 240 μm.
接著,如步驟24所示,利用模具將顆粒成型為生胚。最後,如步驟25所示,將該生胚燒結成磁蕊,其中,燒結時的氧含量是依據平衡氧分壓理論:AP=log(PO2 )+14540/(T+273)調整,其中,AP為氣氛參數、PO2 代表平衡氧分壓,T代表操作溫度,其中,高導磁率錳鋅軟磁的AP為8.0,而平衡氧分壓在加熱至900℃後由21%降至4%~8%。Next, as shown in step 24, the granules are formed into green embryos using a mold. Finally, as shown in step 25, the green embryo is sintered into a magnetic core, wherein the oxygen content during sintering is adjusted according to the equilibrium oxygen partial pressure theory: AP=log(PO 2 )+14540/(T+273), wherein AP is the atmospheric parameter, PO 2 represents the equilibrium oxygen partial pressure, and T represents the operating temperature, wherein the high permeability MnZn soft magnetic AP is 8.0, and the equilibrium oxygen partial pressure is reduced from 21% to 4% after heating to 900 °C. ~8%.
於本實施例中,是先以每小時100℃的加熱速率將生胚加熱至500℃,接下來改以每小時200℃的加熱速率將生胚由500℃加熱至900℃,再以每小時250℃的加熱速率將生胚由900℃加熱至1350℃,然後持溫2至4小時候,之後以每小時200℃的冷卻速率將生胚冷卻至1100℃,最後是以每小時240℃的冷卻速率將已冷卻至1100℃的生胚冷卻至室溫(25℃)。In this embodiment, the green body is first heated to 500 ° C at a heating rate of 100 ° C per hour, and then the raw embryo is heated from 500 ° C to 900 ° C at a heating rate of 200 ° C per hour, and then hourly. The heating rate of 250 ° C heats the green embryo from 900 ° C to 1350 ° C, then holds the temperature for 2 to 4 hours, then cools the raw embryo to 1100 ° C at a cooling rate of 200 ° C per hour, and finally cools at 240 ° C per hour. The raw embryos cooled to 1100 ° C were cooled to room temperature (25 ° C).
為驗證本發明之功效,發明人分別以表一中實施例1、實施例2與實施例3之成分配比與平衡氧分壓,配合圖3中的製造方法對應製成三種磁蕊,並利用導磁率量測設備Agilent-4284A(LCR meter)於100KHz下對所述磁蕊進行檢測,其結果如表二所示。In order to verify the efficacy of the present invention, the inventors respectively produced the three magnetic cores according to the distribution ratios of the first embodiment, the second embodiment and the third embodiment, and the equilibrium oxygen partial pressure in accordance with the manufacturing method in FIG. The magnetic core was detected at 100 KHz using a magnetic permeability measuring device Agilent-4284A (LCR meter), and the results are shown in Table 2.
其中,表二中的比較例即為現有低磁滯係數錳鋅軟磁磁粉的量測結果,而實施例1、實施例2與實施例3則代表是對應表一中之實施例1、實施例2與實施例3之成分配比與平衡氧分壓所製成的磁蕊、μi-40℃~100℃ 是-40℃~100℃的導磁率、μi25℃ 是25℃的導磁率、α-20℃~25℃ 是-20℃~25℃的導磁率溫度係數、α25℃~60℃ 是25℃~60℃的導磁率溫度係數、ηB-40℃~100℃ 是-40℃~100℃的磁滯係數,而ηB25℃ 是常溫磁滯係數。The comparative example in Table 2 is the measurement result of the existing low hysteresis coefficient Mn-Zn soft magnetic magnetic powder, and the first embodiment, the second embodiment and the third embodiment represent the embodiment 1 in the first embodiment. 2, the distribution ratio of Example 3 and the balance of oxygen partial pressure, μi -40 ° C ~ 100 ° C is -40 ° C ~ 100 ° C permeability, μi 25 ° C is 25 ° C permeability, α -20 ° C ~ 25 ° C is -20 ° C ~ 25 ° C magnetic permeability temperature coefficient, α 25 ° C ~ 60 ° C is 25 ° C ~ 60 ° C magnetic permeability temperature coefficient, ηB -40 ° C ~ 100 ° C is -40 ° C ~ 100 The hysteresis coefficient of °C, and ηB 25 °C is the room temperature hysteresis coefficient.
由表二可知,以本發明的製造方法所製成之磁蕊(即實施例1、實施例2與實施例3),無論是在是-40℃~100℃或25℃的導磁率,以及-20℃~25℃與25℃~60℃的導磁率溫度係數,皆優於較現有低磁滯係數錳鋅軟磁磁粉。As can be seen from Table 2, the magnetic cores produced by the manufacturing method of the present invention (i.e., Example 1, Example 2 and Example 3), whether at a magnetic permeability of -40 ° C to 100 ° C or 25 ° C, The magnetic permeability coefficients of -20 ° C ~ 25 ° C and 25 ° C ~ 60 ° C are better than the existing low hysteresis coefficient Mn - Zn soft magnetic powder.
雖然,以本發明的製造方法所製成之磁蕊,在常溫磁滯係數方面略大於現有低磁滯係數錳鋅軟磁磁粉,但是,以本發明的製造方法所製成之磁蕊,在-40℃~100℃的磁滯係數的變化率明顯小於現有低磁滯係數錳鋅軟磁磁粉。Although the magnetic core produced by the manufacturing method of the present invention is slightly larger than the conventional low hysteresis coefficient manganese zinc soft magnetic powder in terms of the room temperature hysteresis coefficient, the magnetic core produced by the manufacturing method of the present invention is - The rate of change of hysteresis coefficient from 40 °C to 100 °C is significantly smaller than that of the existing low hysteresis coefficient manganese-zinc soft magnetic powder.
由上述可知,以本發明的製造方法,確實可以製造出較現有低磁滯係數錳鋅軟磁磁粉的更為廣泛適用溫度範圍,且傳輸效能上也更為穩定的磁蕊。As apparent from the above, according to the production method of the present invention, it is possible to manufacture a magnetic core which is more widely applicable than the conventional low hysteresis coefficient manganese-zinc soft magnetic powder and which is more stable in transmission efficiency.
綜上所述,本發明寬溫型且低磁滯係數之磁蕊的製造方法利用主原料、副原料與黏結劑的成分配比,經煆燒、混合、研磨、造粒...等過程後燒結成磁蕊,使該磁蕊於-40℃~100℃之導磁率介於3200~4800之間、且-20℃~25℃之導磁率溫度係數的絕對值小於7.0×10-7 、而25℃~60℃導磁率溫度係數的絕對值小於0.45×10-7 、-40℃~100℃之磁滯係數小於0.75×10-6 ,以及25℃之磁滯係數小於0.6×10-6 ,故確實能達成本發明之目的。In summary, the method for manufacturing a magnetic core having a wide temperature type and a low hysteresis coefficient according to the present invention utilizes a process ratio of a main raw material, an auxiliary material, and a binder, and is subjected to processes such as calcination, mixing, grinding, granulation, and the like. After sintering into magnetic core, the magnetic permeability of the magnetic core between -40 ° C ~ 100 ° C is between 3200 ~ 4800, and the absolute value of the magnetic permeability temperature coefficient of -20 ° C ~ 25 ° C is less than 7.0 × 10 -7 , The absolute value of the magnetic permeability coefficient of 25 ° C ~ 60 ° C is less than 0.45 × 10 -7 , the hysteresis coefficient of -40 ° C ~ 100 ° C is less than 0.75 × 10 -6 , and the hysteresis coefficient of 25 ° C is less than 0.6 × 10 -6 Therefore, the object of the present invention can be achieved.
惟以上所述者,僅為本發明之較佳實施例而已,當不能以此限定本發明實施之範圍,即大凡依本發明申請專利範圍及發明說明內容所作之簡單的等效變化與修飾,皆仍屬本發明專利涵蓋之範圍內。The above is only the preferred embodiment of the present invention, and the scope of the invention is not limited thereto, that is, the simple equivalent changes and modifications made by the scope of the invention and the description of the invention are All remain within the scope of the invention patent.
21...將一主原料進行煆燒twenty one. . . Burning a main raw material
22...將一副原料加入該主原料成為一混合料twenty two. . . Adding a pair of raw materials to the main raw material to form a mixture
23...將該混合料進行研磨造粒twenty three. . . Grinding and granulating the mixture
24...將顆粒成型為生胚twenty four. . . Forming the granule into a green embryo
25...將該生胚燒結成磁蕊25. . . Sintering the raw embryo into a magnetic core
圖1是一關係圖,說明現有低磁滯係數錳鋅軟磁磁粉之導磁率與溫度的關係;1 is a relational diagram showing the relationship between the magnetic permeability and the temperature of a conventional low hysteresis coefficient manganese-zinc soft magnetic powder;
圖2是另一關係圖,說明現有低磁滯係數錳鋅軟磁磁粉之磁滯係數與溫度的關係;及2 is another relationship diagram illustrating the relationship between hysteresis coefficient and temperature of a conventional low hysteresis coefficient manganese-zinc soft magnetic powder;
圖3是一流程圖,說明本發明寬溫型且低磁滯係數之磁蕊的製造方法之較佳實施例。Fig. 3 is a flow chart showing a preferred embodiment of the method for producing a wide-temperature and low hysteresis magnetic core of the present invention.
21...將一主原料進行煆燒twenty one. . . Burning a main raw material
22...將一副原料加入該主原料成為一混合料twenty two. . . Adding a pair of raw materials to the main raw material to form a mixture
23...將該混合料進行研磨造粒twenty three. . . Grinding and granulating the mixture
24...將顆粒成型為生胚twenty four. . . Forming the granule into a green embryo
25...將該生胚燒結成磁蕊25. . . Sintering the raw embryo into a magnetic core
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| TW101103595A TWI437590B (en) | 2012-02-03 | 2012-02-03 | Wide temperature type and low hysteresis coefficient of the magnetic core manufacturing methods |
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| TW (1) | TWI437590B (en) |
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