TWI901261B - Nickel copper zinc ferrite and manufacturing method and use thereof - Google Patents
Nickel copper zinc ferrite and manufacturing method and use thereofInfo
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Abstract
Description
本發明係有關一種鎳銅鋅鐵氧體,尤指一種具有特定組成之鎳銅鋅鐵氧體。本發明亦有關一種鎳銅鋅鐵氧體之製備方法及應用於高頻微波通訊領域之用途。The present invention relates to a nickel-copper-zinc ferrite, particularly a nickel-copper-zinc ferrite having a specific composition. The present invention also relates to a method for preparing the nickel-copper-zinc ferrite and its application in high-frequency microwave communications.
鎳銅鋅鐵氧體(NiCuZn ferrite)係一種常見的磁性材料,由於其在空氣中燒結後具有高導磁率、低介電常數及低介電損耗等優異之性能,因此,鎳銅鋅鐵氧體常被用於3C系統之濾波功能。近年來,隨著科技不斷的進步,微波通信技術之發展亦日趨成熟,因此,以磁性材料作為微波元件之重要組成部分,扮演著至關重要之角色,且已被廣泛應用於微波領域中,例如應用於無線射頻辨識系統(radio frequency identification, RFID)之短距離通訊領域中。Nickel-copper-zinc-ferrite (NiCuZn ferrite) is a common magnetic material. Due to its excellent properties, such as high magnetic permeability, low dielectric constant, and low dielectric loss after sintering in air, NiCuZn ferrite is often used for filtering in 3C systems. In recent years, with the continuous advancement of technology, the development of microwave communication technology has also matured. Therefore, magnetic materials, as key components of microwave components, play a vital role and have been widely used in the microwave field, such as in the short-range communication field of wireless radio frequency identification (RFID) systems.
在現有技術中,鎳銅鋅鐵氧體被廣泛用於製作天線,以提高通信距離及靈敏度,其中鎳銅鋅鐵氧體之高導磁率可增強磁場,從而提高接收器之感應電壓,及鎳銅鋅鐵氧體之低介電常數及低介電損耗可減少信號之阻抗匹配問題,進而提高整體性能。In existing technology, nickel copper zinc ferrite is widely used to make antennas to improve communication distance and sensitivity. The high magnetic permeability of nickel copper zinc ferrite can enhance the magnetic field, thereby increasing the induced voltage of the receiver. The low dielectric constant and low dielectric loss of nickel copper zinc ferrite can reduce the impedance matching problem of the signal, thereby improving overall performance.
然而,針對更遠距離之通訊需求,RFID所使用之MHz頻段已不敷使用。由於高頻微波信號具有(1)更短之波長,能夠更容易地穿透諸如建築物及樹木等較厚之障礙物與地形,及(2)較佳之直線傳播能力,因此,高頻微波信號於開放區域中傳輸時,其信號衰減較低,可實現較長距離的通信。因此,需開發GHz頻段用材料以應用於諸如衛星通信、雷達、無線電、無線電視及無線網絡等需穿透建築物及更遠距離之通訊領域。However, for longer-distance communication needs, the MHz band used by RFID is no longer sufficient. Because high-frequency microwave signals have (1) shorter wavelengths, which can more easily penetrate thicker obstacles and terrain such as buildings and trees, and (2) better straight-line propagation capabilities, high-frequency microwave signals have lower signal attenuation when transmitted in open areas, enabling longer-distance communication. Therefore, it is necessary to develop materials for the GHz band for applications in communication fields such as satellite communications, radar, radio, wireless television, and wireless networks that need to penetrate buildings and longer distances.
應用於高頻微波通信中之材料的規範要求非常嚴格,其需具備介於4400 G與4430 G之間的高飽和磁化強度(4πMs)及介於210 Oe與240 Oe之間的窄鐵磁共振線寬(ΔH)之微波特性,以確保通訊設備之可靠性。此外,現有技術亦需使用量測技術及量測成本相當高之檢測儀器來量測材料之飽和磁化強度(4πMs)及鐵磁共振線寬(ΔH),造成用於高頻微波通信中之材料之製備成本提高的問題。Materials used in high-frequency microwave communications face stringent specifications. They must possess microwave properties such as a high saturation magnetization (4πMs) between 4400 and 4430 G and a narrow ferromagnetic resonance linewidth (ΔH) between 210 Oe and 240 Oe to ensure the reliability of communications equipment. Furthermore, existing technologies require the use of measurement techniques and costly instrumentation to measure the saturation magnetization (4πMs) and ferromagnetic resonance linewidth (ΔH), increasing the manufacturing costs of materials used in high-frequency microwave communications.
因此,基於上述現有技術之缺點,開發出一種可應用於高頻微波通信之鎳銅鋅鐵氧體及其製備方法,並降低量測鎳銅鋅鐵氧體之飽和磁化強度(4πMs)及鐵磁共振線寬(ΔH)之成本係本領域亟待解決之問題。Therefore, based on the above-mentioned shortcomings of the existing technology, developing a nickel-copper-zinc ferrite and its preparation method that can be applied to high-frequency microwave communications, and reducing the cost of measuring the saturation magnetization intensity (4πMs) and ferromagnetic resonance linewidth (ΔH) of nickel-copper-zinc ferrite are urgent problems to be solved in this field.
為解決上述現有技術之問題,本發明之目的在於提供一種鎳銅鋅鐵氧體之製備方法,藉由混合特定配方之Fe2O3、CuO、Ni2O3及ZnO來製得可應用於高頻微波通訊領域之元件的鎳銅鋅鐵氧體。To solve the above problems of the prior art, the present invention aims to provide a method for preparing nickel-copper-zinc ferrite by mixing Fe 2 O 3 , CuO, Ni 2 O 3 and ZnO in a specific formula to produce nickel-copper-zinc ferrite suitable for components in the field of high-frequency microwave communications.
本發明之另一目的在於提供一種可應用於高頻微波通訊領域之元件的鎳銅鋅鐵氧體。Another object of the present invention is to provide a nickel-copper-zinc ferrite that can be used in components in the field of high-frequency microwave communications.
本發明之另一目的在於提供一種鎳銅鋅鐵氧體之用途,可透過量測鎳銅鋅鐵氧體之μi、Bs、矩形比(Squareness;SQ;Br/Bs)及Hc之磁特性來預測鎳銅鋅鐵氧體之飽和磁化強度(4πMs)、鐵磁共振線寬(ΔH)及介電損耗角正切(tanδ)等微波特性,以及由該鎳銅鋅鐵氧體所製得之元件於Ka波段(27 GHz至30 GHz)之微波範圍中的S11(回波損失)與S21(插入損失)的微波特性,以達到降低量測鎳銅鋅鐵氧體及該元件之微波特性之成本的目的。Another object of the present invention is to provide a use of nickel-copper-zinc ferrite. By measuring the magnetic properties of the nickel-copper-zinc ferrite, such as μ i , Bs, squareness ratio (SQ; Br/Bs), and Hc, the microwave properties of the nickel-copper-zinc ferrite, such as saturated magnetization (4πMs), ferromagnetic resonance linewidth (ΔH), and dielectric loss tangent (tanδ), can be predicted. Furthermore, the microwave properties of components made from the nickel-copper-zinc ferrite, such as S 11 (return loss) and S 21 (insertion loss), in the Ka-band (27 GHz to 30 GHz) microwave range can be predicted. This reduces the cost of measuring the microwave properties of nickel-copper-zinc ferrite and the components.
為了達成上述目的,本發明提供一種鎳銅鋅鐵氧體之製備方法,包括:步驟1:秤取Fe2O3、CuO、Ni2O3及ZnO,並混合,以得到第一混合物;其中以第一混合物之總莫耳數計,Fe2O3之莫耳百分濃度係介於51 mol%與53 mol%之間,及CuO之莫耳百分濃度係介於8.0 mol%與9.5 mol%之間,以及Ni2O3與ZnO之莫耳百分濃度的比值係介於0.8與1.0之間;步驟2:利用球磨機將第一混合物與研磨球及水進行濕式混合1小時,以得到第一漿料;步驟3:將第一漿料進行烘乾,並於空氣中進行煅燒,以得到磁粉;步驟4:以磁粉之總重量計,將介於0.03 wt%與0.08 wt%之間的CaO、介於0.05 wt%與0.15 wt%之間的SiO2、介於0.03wt%與0.08 wt%之間的MgO、介於0.05wt%與0.15 wt%之間的Mn3O4及介於0.1 wt%與0.3 wt%之間的Bi2O3加入磁粉中,以得到第二混合物,之後利用振動研磨機將第二混合物與研磨球及水進行濕式研磨至約1.1 μm,以得到第二漿料;以及步驟5:將第二漿料進行烘乾後所得到之粉體填入塑膠模套內進行冷均壓(cold isostatic press, CIP),並於1000℃之空氣中進行燒結,以得到鎳銅鋅鐵氧體。To achieve the above-mentioned object, the present invention provides a method for preparing nickel-copper-zinc ferrite, comprising: step 1: weighing Fe 2 O 3 , CuO, Ni 2 O 3 and ZnO, and mixing them to obtain a first mixture; wherein, based on the total molar number of the first mixture, the molar percentage concentration of Fe 2 O 3 is between 51 mol% and 53 mol%, the molar percentage concentration of CuO is between 8.0 mol% and 9.5 mol%, and the molar percentage concentration of Ni 2 O 3 is between 10.0 mol% and 10.0 mol%. 3 and ZnO is between 0.8 and 1.0; step 2: wet-mixing the first mixture with grinding balls and water in a ball mill for 1 hour to obtain a first slurry; step 3: drying the first slurry and calcining it in air to obtain magnetic powder; step 4: adding between 0.03 wt% and 0.08 wt% of CaO, between 0.05 wt% and 0.15 wt% of SiO 2 , between 0.03 wt% and 0.08 wt% of MgO, between 0.05 wt% and 0.15 wt% of Mn 3 O 4 and between 0.1 wt% and 0.3 wt% of Bi 2 O 4 based on the total weight of the magnetic powder. 3 is added to the magnetic powder to obtain a second mixture, which is then wet-milled with grinding balls and water using a vibratory mill to a particle size of approximately 1.1 μm to obtain a second slurry; and Step 5: The second slurry is dried to obtain a powder, which is then filled into a plastic mold sleeve and subjected to cold isostatic pressing (CIP). The powder is then sintered at 1000°C in air to obtain nickel-copper-zinc ferrite.
在一具體實施例中,在該步驟3中,煅燒之溫度係介於700℃與900℃之間,及煅燒之時間係介於0.5小時與2小時之間。In one embodiment, in step 3, the calcination temperature is between 700°C and 900°C, and the calcination time is between 0.5 hours and 2 hours.
在一具體實施例中,在步驟4中,第二混合物:研磨球:水之比例為1:20:2至1:40:4,及濕式研磨之時間係介於0.5分鐘與60分鐘之間。In one embodiment, in step 4, the ratio of the second mixture: grinding balls: water is 1:20:2 to 1:40:4, and the wet grinding time is between 0.5 minutes and 60 minutes.
在一具體實施例中,在步驟5中,燒結之溫度係介於980℃與1200℃之間,及燒結之時間係介於1小時與3小時之間。In one embodiment, in step 5, the sintering temperature is between 980°C and 1200°C, and the sintering time is between 1 hour and 3 hours.
本發明另提供一種鎳銅鋅鐵氧體之製備方法所製得之鎳銅鋅鐵氧體,其中鎳銅鋅鐵氧體具有介於300與350之間的μi、介於4150 G與4250 G之間的Bs、介於0.5與0.85之間的Br/Bs(SQ),及介於0.6 Oe與1.2 Oe之間的Hc之磁特性。The present invention also provides a nickel-copper-zinc ferrite prepared by a method for preparing nickel-copper-zinc ferrite, wherein the nickel-copper-zinc ferrite has magnetic properties of μ i between 300 and 350, Bs between 4150 G and 4250 G, Br/Bs (SQ) between 0.5 and 0.85, and Hc between 0.6 Oe and 1.2 Oe.
在一具體實施例中,鎳銅鋅鐵氧體具有介於4400 G與4430 G之間的飽和磁化強度(4πMs)、介於210 Oe與240 Oe之間的鐵磁共振線寬(ΔH),及小於 0.001的介電損耗角正切(tanδ)的微波特性。In one embodiment, the nickel copper zinc ferrite has microwave properties of a saturation magnetization (4πMs) between 4400 G and 4430 G, a ferromagnetic resonance linewidth (ΔH) between 210 Oe and 240 Oe, and a dielectric loss tangent (tan δ) less than 0.001.
在一具體實施例中,鎳銅鋅鐵氧體所製得之元件於Ka波段(27 GHz至30 GHz)之微波範圍中,具有S11(回波損失)> -18 dB及S21(插入損失),及S21(插入損失)> 0.5 dB之微波特性。In one embodiment, a device made of nickel copper zinc ferrite has microwave characteristics of S 11 (return loss) > -18 dB and S 21 (insertion loss) > 0.5 dB in the microwave range of the Ka band ( 27 GHz to 30 GHz).
本發明另提供一種鎳銅鋅鐵氧體之用途,可利用相對簡單之100 KHz量測鎳銅鋅鐵氧體之μi、Bs、矩形比(Squareness;SQ;Br/Bs)及Hc之磁特性,來預測鎳銅鋅鐵氧體之飽和磁化強度(4πMs)、鐵磁共振線寬(ΔH)及介電損耗角正切(tanδ)之微波特性,進而預測鎳銅鋅鐵氧體是否適用於高頻微波領域中。The present invention also provides a use for nickel-copper-zinc ferrite. By using the relatively simple 100 kHz measurement of the nickel-copper-zinc ferrite's magnetic properties, including μ i , Bs, squareness ratio (SQ; Br/Bs), and Hc, the microwave properties of the nickel-copper-zinc ferrite, including saturation magnetization (4πMs), ferromagnetic resonance linewidth (ΔH), and dielectric loss tangent (tanδ), can be predicted. This, in turn, allows the suitability of the nickel-copper-zinc ferrite for use in high-frequency microwave applications to be determined.
在一具體實施例中,利用量測鎳銅鋅鐵氧體之μi、Bs、矩形比(Squareness;SQ;Br/Bs)及Hc之磁特性或鎳銅鋅鐵氧體之飽和磁化強度(4πMs)、鐵磁共振線寬(ΔH)及介電損耗角正切(tanδ)之微波特性的結果,來預測由鎳銅鋅鐵氧體所製得之元件於Ka波段(27 GHz至30 GHz)之微波範圍中的S11(回波損失)與S21(插入損失)的微波特性,進而預測由鎳銅鋅鐵氧體所製得之元件是否適用於高頻微波領域中。In one embodiment, the magnetic properties of NCuZnF, including μi , Bs, squareness ratio (SQ; Br/Bs), and Hc, or the microwave properties of NCuZnF, including saturated magnetization (4πMs), ferromagnetic resonance linewidth (ΔH), and dielectric loss tangent (tanδ), are measured to predict the microwave properties of S11 (return loss) and S21 (insertion loss) of NCuZnF devices in the Ka-band (27 GHz to 30 GHz) microwave range. Furthermore, the suitability of NCuZnF devices for use in high-frequency microwave applications is predicted.
在一具體實施例中,鎳銅鋅鐵氧體可應用於高頻微波通訊領域之元件中。In one embodiment, nickel copper zinc ferrite can be used in components in the field of high-frequency microwave communications.
本發明透過特定莫耳百分濃度之Fe2O3、CuO、Ni2O3及ZnO,並添加CaO、SiO2、Bi2O3、MgO及Mn3O4等副成分,可製得具旋磁特性(高導磁率及高飽和磁束密度)之鎳銅鋅鐵氧體,藉由加入銅元素,可進一步優化鎳銅鋅鐵氧體之旋磁特性,並使其可應用於高頻微波通訊領域之元件中;及其中CaO可增加晶界電阻,MgO可增加晶粒電阻,及Bi2O3可促進晶粒成長。The present invention utilizes specific molar percentage concentrations of Fe₂O₃ , CuO, Ni₂O₃ , and ZnO , along with the addition of auxiliary components such as CaO, SiO₂ , Bi₂O₃ , MgO, and Mn₃O₄ , to produce nickel-copper- zinc ferrite with gyromagnetic properties (high magnetic permeability and high saturated magnetic flux density). The addition of copper further optimizes the gyromagnetic properties of the nickel-copper-zinc ferrite, enabling its application in components used in high-frequency microwave communications. CaO increases grain boundary resistance, MgO increases grain resistance, and Bi₂O₃ promotes grain growth.
此外,本發明可利用相對簡單之100 KHz來量測鎳銅鋅鐵氧體之μi、Bs、矩形比(Squareness;SQ;Br/Bs)及Hc等磁特性,來達到預測鎳銅鋅鐵氧體之飽和磁化強度(4πMs)、鐵磁共振線寬(ΔH)及介電損耗角正切(tanδ),並加速組裝合格之Ka波段所需之S11(回波損失)與S21(插入損失)之微波特性需求的目的,解決現有技術無法製得可應用於高頻微波通訊領域之鎳銅鋅鐵氧體,及必須透過高成本之量測技術來量測鎳銅鋅鐵氧體之磁特性及量測鎳銅鋅鐵氧體元件於Ka波段所需之S11(回波損失)與S21(插入損失)之微波特性之問題。In addition, the present invention can use a relatively simple 100 kHz frequency to measure the magnetic properties of nickel copper zinc ferrite, such as μ i , Bs, squareness ratio (SQ; Br/Bs) and Hc, to predict the saturation magnetization intensity (4πMs), ferromagnetic resonance linewidth (ΔH) and dielectric loss tangent (tanδ) of nickel copper zinc ferrite, and accelerate the assembly of qualified Ka-band S 11 (return loss) and S 21 The purpose of this research is to address the microwave characteristics of nickel-copper-zinc-ferrite (NiCuZnF) components, which are unable to produce NiCuZnF for use in high-frequency microwave communications. Existing technologies are unable to produce NiCuZnF, which is suitable for use in high-frequency microwave communications. High-cost measurement techniques are required to measure the magnetic properties of NiCuZnF, as well as the microwave characteristics of S11 (return loss) and S21 (insertion loss) required for NiCuZnF components in the Ka band.
以下係藉由特定之具體實施例說明本發明之實施方式,熟習此技術之人士可藉由本說明書所揭示之內容瞭解本發明之其他優點與功效。然而,本發明中所揭示之例示性實施例僅出於說明之目的,不應被視為限制本發明之範圍。換言之,本發明亦可藉由其他不同的具體實施例加以施行或應用,本說明書中的各項細節亦可基於不同的觀點與應用,在不悖離本發明之精神下進行各種修飾與變更。The following describes the implementation of the present invention through specific embodiments. Those skilled in the art will appreciate the other advantages and benefits of the present invention through the disclosures herein. However, the exemplary embodiments disclosed herein are for illustrative purposes only and should not be construed as limiting the scope of the present invention. In other words, the present invention may be implemented or applied through various other specific embodiments, and the details in this specification may be modified and altered based on different viewpoints and applications without departing from the spirit of the present invention.
除非本文另有說明,否則說明書及所附申請專利範圍中所使用之單數形式「一」及「該」包括複數個體。除非本文另有說明,否則說明書及所附申請專利範圍中所使用之術語「或」包括「及/或」之含義。Unless otherwise specified herein, the singular forms "a," "an," and "the" used in the specification and the appended claims include plural forms. Unless otherwise specified herein, the term "or" used in the specification and the appended claims includes the meaning of "and/or."
製備例1 製備第一鎳銅鋅鐵氧體樣品及第一鎳銅鋅鐵氧體元件Preparation Example 1 Preparation of the First NiCuZnFerrite Sample and the First NiCuZnFerrite Component
參見第1圖,第一鎳銅鋅鐵氧體樣品及第一鎳銅鋅鐵氧體元件之製備方法包括:步驟1:秤取適當重量之Fe2O3、CuO、Ni2O3及ZnO,並混合,以得到第一混合物;其中以第一混合物之總莫耳數計,Fe2O3及CuO之莫耳百分濃度分別為51.4 mol%及9.1 mol%,以及Ni2O3與ZnO之莫耳百分濃度的比值為1.0;步驟2:利用球磨機將第一混合物與研磨球及水進行濕式混合1小時,以得到第一漿料;其中第一混合物與研磨球及水之比例為250 g:1600 g:500 cc;步驟3:將第一漿料進行烘乾,並於空氣中進行煅燒,以得到磁粉;其中煅燒之溫度及時間分別為850℃及2小時;步驟4:以磁粉之總重量計,將0.05 wt%之CaO、0.1 wt%之SiO2、0.2 wt%之Bi2O3、0.06 wt%之MgO及0.1 wt%之Mn3O4加入磁粉中,以得到第二混合物,之後利用振動研磨機將第二混合物與研磨球及水進行濕式研磨30分鐘至約1.1 μm,以得到第二漿料;其中第二混合物與研磨球及水之比例為250 g:3000 g:500 cc;步驟5:將第二漿料進行烘乾後所得到之粉體填入直徑為45 mm及長度為100 mm之塑膠模套內,於2200 kgf/cm2之條件下進行冷均壓,並於1000℃之空氣中進行燒結3小時,以得到第一鎳銅鋅鐵氧體;以及步驟6:將第一鎳銅鋅鐵氧體進行研磨加工,以製得合適之形狀及尺寸之第一鎳銅鋅鐵氧體樣品(即,磁芯)及使用於高頻微波通訊領域之第一鎳銅鋅鐵氧體元件。Referring to FIG. 1 , the preparation method of the first nickel-copper-zinc ferrite sample and the first nickel-copper-zinc ferrite element includes: step 1: weighing appropriate weights of Fe 2 O 3 , CuO, Ni 2 O 3 and ZnO, and mixing them to obtain a first mixture; wherein, based on the total molar number of the first mixture, the molar percentage concentrations of Fe 2 O 3 and CuO are 51.4 mol% and 9.1 mol%, respectively, and the molar percentage concentration ratio of Ni 2 O 3 to ZnO is 1.0; step 2: wet-mixing the first mixture with grinding balls and water in a ball mill for 1 hour to obtain a first slurry; wherein the ratio of the first mixture to the grinding balls and water is 250 g:1600 g:500 g. cc; Step 3: Drying the first slurry and calcining it in air to obtain magnetic powder; wherein the calcination temperature and time are 850°C and 2 hours respectively; Step 4: Based on the total weight of the magnetic powder, 0.05 wt% of CaO, 0.1 wt% of SiO 2 , 0.2 wt% of Bi 2 O 3 , 0.06 wt% of MgO and 0.1 wt% of Mn 3 O 4 are added to the magnetic powder to obtain a second mixture, and then the second mixture is wet-milled with grinding balls and water using a vibration mill for 30 minutes to about 1.1 μm to obtain a second slurry; wherein the ratio of the second mixture to grinding balls and water is 250 g:3000 g:500 cc; Step 5: Filling the powder obtained by drying the second slurry into a plastic mold sleeve with a diameter of 45 mm and a length of 100 mm, cold-isolating the mold sleeve at 2200 kgf/ cm² , and sintering the mold sleeve at 1000°C in air for 3 hours to obtain a first nickel-copper-zinc ferrite; and Step 6: Grinding the first nickel-copper-zinc ferrite to produce a first nickel-copper-zinc ferrite sample (i.e., a magnetic core) of suitable shape and size and a first nickel-copper-zinc ferrite component for use in high-frequency microwave communications.
製備例2 製備第二鎳銅鋅鐵氧體樣品、第三鎳銅鋅鐵氧體樣品、第二鎳銅鋅鐵氧體元件及第三鎳銅鋅鐵氧體元件Preparation Example 2 Preparation of a second nickel-copper-zinc-ferrite sample, a third nickel-copper-zinc-ferrite sample, a second nickel-copper-zinc-ferrite element, and a third nickel-copper-zinc-ferrite element
第二鎳銅鋅鐵氧體樣品、第三鎳銅鋅鐵氧體樣品、第二鎳銅鋅鐵氧體元件及第三鎳銅鋅鐵氧體元件之製備方法概同於第一鎳銅鋅鐵氧體樣品及第一鎳銅鋅鐵氧體元件之製備方法,差異在於:於步驟1中所秤取之Fe2O3、CuO、Ni2O3及ZnO之重量不同,以於步驟5得到第二鎳銅鋅鐵氧體及第三鎳銅鋅鐵氧體,及於步驟6得到第二鎳銅鋅鐵氧體樣品、第三鎳銅鋅鐵氧體樣品、第二鎳銅鋅鐵氧體元件及第三鎳銅鋅鐵氧體元件。The preparation methods of the second NiCuZnFerrite sample, the third NiCuZnFerrite sample, the second NiCuZnFerrite element and the third NiCuZnFerrite element are similar to the preparation methods of the first NiCuZnFerrite sample and the first NiCuZnFerrite element. The difference is that the Fe2O3 , CuO, Ni2O weighed in step 1 3 and ZnO by weight, so as to obtain a second nickel copper zinc ferrite and a third nickel copper zinc ferrite in step 5, and to obtain a second nickel copper zinc ferrite sample, a third nickel copper zinc ferrite sample, a second nickel copper zinc ferrite device and a third nickel copper zinc ferrite device in step 6.
比較例 製備第四鎳銅鋅鐵氧體樣品、第五鎳銅鋅鐵氧體樣品、第六鎳銅鋅鐵氧體樣品、第四鎳銅鋅鐵氧體元件、第五鎳銅鋅鐵氧體元件及第六鎳銅鋅鐵氧體元件Comparative Example: Preparation of a fourth nickel-copper-zinc-ferrite sample, a fifth nickel-copper-zinc-ferrite sample, a sixth nickel-copper-zinc-ferrite sample, a fourth nickel-copper-zinc-ferrite device, a fifth nickel-copper-zinc-ferrite device, and a sixth nickel-copper-zinc-ferrite device
第四鎳銅鋅鐵氧體樣品、第五鎳銅鋅鐵氧體樣品、第六鎳銅鋅鐵氧體樣品、第四鎳銅鋅鐵氧體元件、第五鎳銅鋅鐵氧體元件及第六鎳銅鋅鐵氧體元件之製備方法概同於第一鎳銅鋅鐵氧體樣品及第一鎳銅鋅鐵氧體元件之製備方法,差異在於:於步驟1中所秤取之Fe2O3、CuO、Ni2O3及ZnO之重量不同,以於步驟5得到第四鎳銅鋅鐵氧體、第五鎳銅鋅鐵氧體及第六鎳銅鋅鐵氧體,及於步驟6得到第四鎳銅鋅鐵氧體樣品、第五鎳銅鋅鐵氧體樣品、第六鎳銅鋅鐵氧體樣品、第四鎳銅鋅鐵氧體元件、第五鎳銅鋅鐵氧體元件及第六鎳銅鋅鐵氧體元件。茲將製備第一鎳銅鋅鐵氧體樣品至第六鎳銅鋅鐵氧體樣品時,於步驟1中所秤取之Fe2O3及CuO之莫耳百分濃度,及Ni2O3及ZnO之莫耳百分濃度的比值整理於表1中。表1 製備第一鎳銅鋅鐵氧體樣品至第六鎳銅鋅鐵氧體樣品時所秤取之Fe2O3及CuO之莫耳百分濃度,及Ni2O3及ZnO之莫耳百分濃度的比值
實施例1 量測第一鎳銅鋅鐵氧體樣品至第六鎳銅鋅鐵氧體樣品之磁特性與標準微波特性,以及第一鎳銅鋅鐵氧體元件至第六鎳銅鋅鐵氧體元件於Ka波段之S11(回波損失)與S21(插入損失)之微波特性Example 1: Magnetic properties and standard microwave properties of the first to sixth NiCuZnFerrite samples were measured, as well as the microwave properties of S11 (return loss) and S21 (insertion loss) of the first to sixth NiCuZnFerrite elements in the Ka band.
將製備例1、製備例2及比較例所得到之第一鎳銅鋅鐵氧體樣品至第六鎳銅鋅鐵氧體樣品進行磁特性分析及標準微波特性分析,其中第一鎳銅鋅鐵氧體樣品至第六鎳銅鋅鐵氧體樣品係研磨加工成T16(外徑×內徑×厚度 = 16×6×8 mm),以量測μi、Bs、Br/Bs(SQ)及Hc等磁特性。此外,第一鎳銅鋅鐵氧體樣品至第六鎳銅鋅鐵氧體樣品係研磨加工成圓盤狀(ø = 12.73 mm及厚度=1.53 mm)以量測飽和磁化強度(4πMs)、加工成圓球狀(ø = 1.56 mm)以量測鐵磁共振線寬(ΔH),及加工成棒狀(ø = 1.27 mm及L > 20 mm)以量測介電損耗角正切(tanδ)等微波特性。再者,將第一鎳銅鋅鐵氧體元件至第六鎳銅鋅鐵氧體元件於Ka波段(27 GHz至30 GHz)之微波範圍中進行S11(回波損失)與S21(插入損失)之微波特性分析。Magnetic properties and standard microwave properties analysis were performed on the first to sixth NiCuZnFerrite samples obtained in Preparation Example 1, Preparation Example 2, and the comparative example. The first to sixth NiCuZnFerrite samples were ground into T16 (outer diameter × inner diameter × thickness = 16 × 6 × 8 mm) to measure magnetic properties such as μi, Bs, Br/Bs (SQ), and Hc. In addition, the first to sixth NiCuZnFerrite samples were ground into discs (ø = 12.73 mm and thickness = 1.53 mm) to measure the saturation magnetization (4πMs), spheres (ø = 1.56 mm) to measure the ferromagnetic resonance linewidth (ΔH), and rods (ø = 1.27 mm and L > 20 mm) to measure microwave properties such as the dielectric loss tangent (tanδ). Furthermore, the microwave characteristics of S 11 (return loss) and S 21 (insertion loss) of the first to sixth nickel-copper-zinc-ferrite devices were analyzed in the microwave range of the Ka band (27 GHz to 30 GHz).
參見表2,結果顯示相較於第四鎳銅鋅鐵氧體樣品、第五鎳銅鋅鐵氧體樣品及第六鎳銅鋅鐵氧體樣品,第一鎳銅鋅鐵氧體樣品、第二鎳銅鋅鐵氧體樣品及第三鎳銅鋅鐵氧體樣品具有μi> 300(介於300與350之間)、Bs > 4000 G(介於4150 G與4250 G之間)、Br/Bs(SQ)介於0.5與0.85之間,及Hc < 0.85 Oe(介於0.6 Oe與1.2 Oe之間)等良好的磁特性。此外,相較於第四鎳銅鋅鐵氧體樣品、第五鎳銅鋅鐵氧體樣品及第六鎳銅鋅鐵氧體樣品,第一鎳銅鋅鐵氧體樣品、第二鎳銅鋅鐵氧體樣品及第三鎳銅鋅鐵氧體樣品具有飽和磁化強度(4πMs)介於4400 G與4430 G之間、鐵磁共振線寬(ΔH)介於210 Oe與240 Oe之間,及介電損耗角正切(tanδ) < 0.001等良好的標準微波特性。再者,相較於第四鎳銅鋅鐵氧體元件、第五鎳銅鋅鐵氧體元件及第六鎳銅鋅鐵氧體元件,第一鎳銅鋅鐵氧體元件、第二鎳銅鋅鐵氧體元件及第三鎳銅鋅鐵氧體元件於Ka波段(27 GHz至30 GHz)之微波範圍中具有符合規格要求之S11(回波損失)> -18 dB及S21(插入損失) > 0.5 dB之良好的微波特性。表2 第一鎳銅鋅鐵氧體樣品至第六鎳銅鋅鐵氧體樣品之磁特性及標準微波特性,及第一鎳銅鋅鐵氧體元件至第六鎳銅鋅鐵氧體元件於Ka波段之S11(回波損失)與S21(插入損失)之等微波特性分析的結果
註:底線表示所得到之鎳銅鋅鐵氧體樣品不具良好的磁特性及標準微波特性。Note: The bottom line indicates that the obtained nickel-copper-zinc ferrite sample does not have good magnetic properties and standard microwave properties.
實施例2 觀察第一鎳銅鋅鐵氧體樣品及第六鎳銅鋅鐵氧體樣品之微觀組織Example 2 Observation of the microstructure of the first nickel-copper-zinc ferrite sample and the sixth nickel-copper-zinc ferrite sample
參見第2圖,利用顯微鏡觀察第一鎳銅鋅鐵氧體樣品及第六鎳銅鋅鐵氧體樣品之微觀組織,結果顯示相較於第一鎳銅鋅鐵氧體樣品,第六鎳銅鋅鐵氧體樣品具有較差之孔洞緻密性。Referring to Figure 2, the microstructures of the first and sixth nickel-copper-zinc ferrite samples were observed under a microscope. The results show that the sixth nickel-copper-zinc ferrite sample has poorer pore density than the first nickel-copper-zinc ferrite sample.
由上可知,本發明之鎳銅鋅鐵氧體之製備方法透過將特定莫耳百分濃度之Fe2O3、CuO、Ni2O3及ZnO混合後,進行濕式混合、煅燒、濕式研磨及燒結等步驟後可得到具有μi> 300(介於300與350之間)、Bs > 4000 G(介於4150 G與4250 G之間)、Br/Bs(SQ)介於0.5與0.85之間,及Hc < 0.85 Oe(介於0.6 Oe與1.2 Oe之間)等良好磁特性,及飽和磁化強度(4πMs)介於4400 G與4430 G之間、鐵磁共振線寬(ΔH)介於210 Oe與240 Oe之間,及介電損耗角正切(tanδ) < 0.001等良好的標準微波特性之鎳銅鋅鐵氧體樣品。此外,第一鎳銅鋅鐵氧體元件、第二鎳銅鋅鐵氧體元件及第三鎳銅鋅鐵氧體元件於Ka波段(27 GHz至30 GHz)之微波範圍中具有符合規格要求之S11(回波損失)> -18 dB,及S21(插入損失)> 0.5 dB之良好的微波特性。As can be seen from the above, the preparation method of the nickel-copper-zinc ferrite of the present invention can obtain good magnetic properties such as μ i > 300 (between 300 and 350), Bs > 4000 G (between 4150 G and 4250 G), Br/Bs (SQ) between 0.5 and 0.85, and Hc < 0.85 Oe (between 0.6 Oe and 1.2 Oe), and saturated magnetization (4πMs) between 4400 G and 4430 G by mixing Fe 2 O 3 , CuO, Ni 2 O 3 and ZnO with specific molar percentage concentrations, and then performing wet mixing, calcining, wet grinding and sintering. The nickel-copper-zinc-ferrite samples exhibit excellent standard microwave characteristics, including a ferromagnetic resonance linewidth (ΔH) between 210 Oe and 240 Oe, a dielectric loss tangent (tanδ) less than 0.001. Furthermore, the first, second, and third nickel-copper-zinc-ferrite components exhibit excellent microwave characteristics in the Ka-band (27 GHz to 30 GHz) with S 11 (return loss) greater than -18 dB and S 21 (insertion loss) greater than 0.5 dB, meeting specification requirements.
因此,本發明透過特定莫耳百分濃度之Fe2O3、CuO、Ni2O3及ZnO,並添加CaO、SiO2、Bi2O3、MgO及Mn3O4等副成分,可製得具旋磁特性(高導磁率及高飽和磁束密度)之鎳銅鋅鐵氧體,藉由加入銅元素,可進一步優化鎳銅鋅鐵氧體之旋磁特性,並使其可應用於高頻微波通訊領域之元件中;及其中CaO可增加晶界電阻,MgO可增加晶粒電阻,及Bi2O3可促進晶粒成長。Therefore, the present invention achieves nickel- copper-zinc ferrite ( NiCuZn ) with gyromagnetic properties ( high permeability and high saturated magnetic flux density) by using specific molar percentage concentrations of Fe₂O₃ , CuO , Ni₂O₃ , and ZnO, and by adding auxiliary components such as CaO, SiO₂, Bi₂O₃ , MgO, and Mn₃O₄ . The addition of copper further optimizes the gyromagnetic properties of NiCuZn ferrite, enabling its application in components used in high-frequency microwave communications. CaO increases grain boundary resistance, MgO increases grain resistance, and Bi₂O₃ promotes grain growth.
此外,本發明可利用相對簡單之100 KHz來量測鎳銅鋅鐵氧體之μi、Bs、矩形比(Squareness;SQ;Br/Bs)及Hc等磁特性,來達到預測在現有技術中必須使用高成本之量測技術之鎳銅鋅鐵氧體之飽和磁化強度(4πMs)、鐵磁共振線寬(ΔH)及介電損耗角正切(tanδ),並加速組裝合格之Ka波段所需之S11(回波損失)與S21(插入損失)之微波特性需求的目的,解決現有技術無法製得可應用於高頻微波通訊領域之鎳銅鋅鐵氧體,及必須透過高成本之量測技術來量測鎳銅鋅鐵氧體之磁特性及量測鎳銅鋅鐵氧體元件於Ka波段所需之S11(回波損失)與S21(插入損失)之微波特性之問題。In addition, the present invention can use a relatively simple 100 kHz frequency to measure the magnetic properties of nickel-copper-zinc ferrite, such as μ i , Bs, squareness ratio (SQ; Br/Bs), and Hc, to predict the saturation magnetization intensity (4πMs), ferromagnetic resonance linewidth (ΔH), and dielectric loss tangent (tanδ) of nickel-copper-zinc ferrite, which require high-cost measurement technology in existing technology. It also accelerates the S 11 (echo loss) and S 21 required for qualified Ka-band assembly. The purpose of this research is to address the microwave characteristics of nickel-copper-zinc-ferrite (NiCuZnF) components, which are unable to produce NiCuZnF for use in high-frequency microwave communications. Existing technologies are unable to produce NiCuZnF, which is suitable for use in high-frequency microwave communications. High-cost measurement techniques are required to measure the magnetic properties of NiCuZnF, as well as the microwave characteristics of S11 (return loss) and S21 (insertion loss) required for NiCuZnF components in the Ka band.
上述實施例僅例示性說明本發明之鎳銅鋅鐵氧體及其製備方法與用途,而非用於限制本發明。任何熟習此項技術之人士皆可在不違背本發明之精神及範疇下,對上述實施例進行修飾與改變。因此,本發明之權利保護範圍,應如後述之申請專利範圍所載。The above embodiments are merely illustrative of the nickel-copper-zinc ferrite, its preparation method, and uses of the present invention and are not intended to limit the present invention. Any person skilled in the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention shall be as set forth in the patent application described below.
第1圖係本發明之第一鎳銅鋅鐵氧體樣品及第一鎳銅鋅鐵氧體元件之製備方法的步驟流程圖。第2A圖及第2B圖分別係利用顯微鏡觀察本發明之第一鎳銅鋅鐵氧體樣品及比較例之第六鎳銅鋅鐵氧體樣品之微觀組織的結果圖。Figure 1 is a flow chart of the steps involved in preparing the first nickel-copper-zinc ferrite sample and the first nickel-copper-zinc ferrite device of the present invention. Figures 2A and 2B are microscopic observations of the microstructures of the first nickel-copper-zinc ferrite sample of the present invention and the sixth nickel-copper-zinc ferrite sample of the comparative example, respectively.
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| TW201819308A (en) * | 2016-11-21 | 2018-06-01 | 中國鋼鐵股份有限公司 | Nickel-copper-zinc ferrite powder and method for fabricating the same |
| CN110540422A (en) * | 2019-08-22 | 2019-12-06 | 江门江益磁材有限公司 | Nickel-copper-zinc ferrite powder and preparation method and application thereof |
| CN116283265A (en) * | 2023-04-14 | 2023-06-23 | 电子科技大学 | Low temperature sintered NiCuZn power ferrite and its preparation method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201819308A (en) * | 2016-11-21 | 2018-06-01 | 中國鋼鐵股份有限公司 | Nickel-copper-zinc ferrite powder and method for fabricating the same |
| CN110540422A (en) * | 2019-08-22 | 2019-12-06 | 江门江益磁材有限公司 | Nickel-copper-zinc ferrite powder and preparation method and application thereof |
| CN116283265A (en) * | 2023-04-14 | 2023-06-23 | 电子科技大学 | Low temperature sintered NiCuZn power ferrite and its preparation method |
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