WO2010018955A2 - 저투자손실을 가지는 니켈 망간 코발트 스피넬 페라이트 제조 방법 및 이에 의해 제조된 니켈 망간 코발트 스피넬 페라이트 - Google Patents
저투자손실을 가지는 니켈 망간 코발트 스피넬 페라이트 제조 방법 및 이에 의해 제조된 니켈 망간 코발트 스피넬 페라이트 Download PDFInfo
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- WO2010018955A2 WO2010018955A2 PCT/KR2009/004441 KR2009004441W WO2010018955A2 WO 2010018955 A2 WO2010018955 A2 WO 2010018955A2 KR 2009004441 W KR2009004441 W KR 2009004441W WO 2010018955 A2 WO2010018955 A2 WO 2010018955A2
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Definitions
- the present invention relates to a ferrite manufacturing method and a ferrite produced thereby, and more particularly, to a method for producing nickel manganese cobalt spinel ferrite having a low investment loss and a low dielectric loss, and a nickel manganese cobalt spinel ferrite produced thereby.
- Ferrite is a solid solution in which alloying elements or impurities are dissolved in iron of a body-centered cubic crystal which is stable at 900 ° C. or lower.
- a metallographic term for steel since it is a solid solution based on ⁇ iron, its appearance is the same as pure iron, but it is also called silicon ferrite or silicon iron by the name of the element dissolved. Under a microscope, it is a single phase, and a mixture of the white part of ferrite and the black part of pearlite where carbon is slightly dissolved appears.
- Ferrites are used in magnetic heads such as high frequency transformers, pickups and tape recorders.
- spinel ferrite is generally used in low frequency such as EM core, low output high inductance resonance circuit, broadband transformer, and is mainly absorber due to high investment loss in high frequency region of MHz or higher. It is used as ferrite.
- spinel ferrite has a high permeability below the MHz frequency, but also a high permeability loss. Because of these characteristics, RF electronic component materials have difficulty in application due to high loss, and thus are mainly used as absorbers.
- Such spinel ferrite manufacturing methods include ball mill production, coprecipitation, sol-gel production, hydrothermal synthesis, and the like.
- a sol gel is a series of processes involving the transition from a fluidized sol to a gel exhibiting viscoelastic properties such as semi-solids.
- the hydrothermal synthesis method involves the solubility of materials, suspensions, temperatures, Refers to a method of synthesizing or growing crystals using properties that depend on pressure and concentration of solvent. Coprecipitation refers to a phenomenon in which one substance precipitates together in a solution in which two substances having similar chemical properties coexist.
- the production of spinel ferrite by sol-gel or hydrothermal synthesis method is a synthetic condition to control the temperature, pressure, PH, etc., the difficulty in mass production due to the difficult reproducibility and manufacturing method.
- the spinel ferrite manufacturing method using coprecipitation has the advantage that it can be used for mass production because it has a simple manufacturing process compared to sol gel and hydrothermal synthesis method, but it generates a large amount of waste water and waste during the washing process, and the metal salt heavy metal as a raw material for manufacturing.
- the low mass ratio occupies the disadvantage that the manufacturing cost is high.
- Another object of the present invention is to provide a nickel manganese cobalt spinel ferrite manufacturing method and a nickel manganese cobalt spinel ferrite produced by the mass production is not expensive.
- Nickel manganese cobalt spinel ferrite manufacturing method comprises the steps of providing nickel oxide (NiO), cobalt oxide (Co 3 O 4 ), manganese oxide (MnO) and iron oxide (Fe 2 O 3 ), the nickel oxide, the Wet mixing the cobalt oxide, the manganese oxide and the iron oxide in methanol, taking powder from the nickel oxide, the cobalt oxide, the manganese oxide and the iron oxide mixture, drying the powder, pulverizing the dried powder and the Heat-treating the pulverized powder.
- NiO nickel oxide
- Co 3 O 4 cobalt oxide
- MnO manganese oxide
- Fe 2 O 3 iron oxide
- nickel oxide, cobalt oxide, manganese oxide and iron oxide is provided in the mol ratio of nickel oxide, cobalt oxide, manganese oxide and iron oxide of 0.6 to 0.8: 0.005 to 0.007: 0.052 to 0.054: 1.04 to 1.06 It is characterized in that, preferably the molar ratio may be provided in a molar ratio of 0.7: 0.006: 0.053: 1.05.
- nickel oxide, cobalt oxide, manganese oxide and iron oxide is provided in the mol ratio of nickel oxide, cobalt oxide, manganese oxide and iron oxide of 0.6 to 0.8: 0.005 to 0.007: 0.057 to 0.059: 1.13 to 1.15 Characterized in that the molar ratio is preferably provided in a molar ratio of 0.76: 0.006: 0.058: 1.14.
- the wet mixing may be performed in a ball mill for 45 hours to 50 hours, and preferably for about 48 hours.
- Drying the mixture powder may be performed at 110 ° C to 130 ° C for 11 hours to 13 hours, preferably at about 120 ° C for 12 hours.
- the first heat treatment may be performed at 750 ° C. to 850 ° C., preferably at about 800 ° C.
- the second heat treatment may be performed at 1150 ° C to 1250 ° C, and preferably at about 1200 ° C.
- the second heat treatment may be performed at 1050 ° C to 1150 ° C, and preferably at about 1100 ° C.
- the third heat treatment may be performed at 1200 ° C to 1300 ° C, and preferably at about 1250 ° C.
- the third heat treatment may be performed at 1100 ° C. to 1200 ° C., and preferably at about 1150 ° C.
- nickel manganese cobalt spinel ferrite according to the invention is characterized in that it is produced by the above production method.
- Nickel manganese cobalt spinel ferrite manufacturing method and nickel manganese cobalt spinel ferrite prepared according to the present invention has a low investment loss and low dielectric loss, so it can be applied to the electronic component material at high frequencies.
- the nickel manganese cobalt spinel ferrite manufacturing method according to the present invention and the nickel manganese cobalt spinel ferrite produced thereby has the effect that not only the manufacturing process is simple but also sufficiently reproducible.
- the nickel manganese cobalt spinel ferrite manufacturing method according to the present invention and the nickel manganese cobalt spinel ferrite produced by it has the effect that not only can be produced in mass production but also expensive manufacturing unit price.
- FIG. 1 is a block diagram showing a method for preparing nickel manganese cobalt spinel ferrite according to the present invention
- FIG. 2 is a block diagram showing a method for preparing nickel manganese cobalt spinel ferrite according to a first embodiment of the present invention
- FIG. 3 is a graph showing the complex dielectric constant change in the band between 10 MHz and 1 GHz of nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention
- FIG. 4 is a graph showing the change in the complex permeability of the nickel manganese cobalt spinel ferrite in the band between 10 MHz and 1 GHz according to the first embodiment of the present invention
- FIG. 5 is a graph showing the performance of the antenna to which the nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention and the antenna to which the material of dielectric constant 40 is applied;
- FIG. 6 is a table showing the performance of the antenna to which the nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention and the antenna to which the material of dielectric constant 40 is applied;
- FIG. 7 is a block diagram showing a method of manufacturing nickel manganese cobalt spinel ferrite according to a second embodiment of the present invention.
- FIG. 1 is a block diagram showing a method for preparing nickel manganese cobalt spinel ferrite according to the present invention.
- the nickel manganese cobalt spinel ferrite manufacturing method of the present invention provides a step of providing nickel oxide, cobalt oxide, manganese oxide, iron oxide (S110), wet mixing in methanol with a ball mill (S120), in the mixture Taking powder and drying (S130), drying and grinding (S140), and heat-treating the pulverized powder (S150).
- FIG. 2 is a block diagram illustrating a method of manufacturing nickel manganese cobalt spinel ferrite according to a first embodiment of the present invention.
- nickel oxide, cobalt oxide, manganese oxide and iron oxide were weighed at a molar ratio of about 0.7: 0.006: 0.005: 1.05. Provided (S210).
- the nickel oxide, cobalt oxide, manganese oxide and iron oxide provided in this way are wet mixed in methanol (MeOH) for about 48 hours in a ball mill (S220).
- Powders are taken from the nickel oxide, cobalt oxide, manganese oxide, and iron oxide mixture and dried at about 120 ° C. for about 12 hours (S230).
- the dried powder is pulverized to have a small particle size (S240).
- the dried and pulverized powder is subjected to a first heat treatment process.
- Primary heat treatment is performed at a temperature of about 800 °C (S250).
- the process of synthesizing the spinel ferrite in the secondary heat treatment and the tertiary heat treatment performed later can be further promoted.
- the first heat-treated powder is subjected to the second heat treatment process.
- the secondary heat treatment is performed at a temperature of about 1200 ° C. (S260).
- the secondary heat-treated powder is subjected to a third heat treatment process, the third heat treatment is performed at a temperature of about 1250 °C (S270).
- nickel oxide, cobalt oxide, manganese oxide and iron oxide are synthesized as spinel ferrite.
- the present invention is not limited thereto, and the molar ratio of nickel oxide, cobalt oxide, manganese oxide, and iron oxide is 0.6 to 0.8: 0.005 to 0.007: 0.052 to 0.054: 1.04 to 1.06, wet mixing may be performed for 45 to 50 hours, and the powder may be dried at 110 ° C to 130 ° C for 11 to 13 hours.
- primary heat treatment may be performed at 750 ° C to 850 ° C
- secondary heat treatment may be performed at 1150 ° C to 1250 ° C
- tertiary heat treatment may be performed at 1200 ° C to 1300 ° C.
- FIG. 3 is a graph showing the change in complex dielectric constant of 10 to 1 GHz band of nickel manganese cobalt spinel ferrite prepared according to the first embodiment of the present invention.
- Permittivity is a universal electrical constant that appears in the equations for the physical force (coulomb force) existing between two isolated charges and the change in the characteristics of the electric field (electrical displacement) resulting from the insertion of the dielectric into the electric field. That is, it is a characteristic value representing the electrical characteristics of the insulator.
- the nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention has a dielectric loss of 0.0004 or less at 200 MHz.
- the dielectric constant is between 6 and 7.
- Permeability refers to the amount that represents the magnetic properties of a substance. In other words, it refers to the ratio of the magnetic flux flux density generated when the magnetization is affected by the magnetic field and the intensity in the vacuum of the magnetic field.
- the nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention has an investment loss of 0.04 or less at 200MHz.
- the magnetic permeability exhibits a property of between 9 and 10.
- Nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention exhibits a characteristic in which the ratio of permeability / dielectric constant is between 1.3 and 1.75.
- Nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention has a characteristic that the investment loss is very low, compared with the characteristics of the general spinel ferrite. And the permeability is higher than the permittivity.
- the nickel manganese cobalt spinel ferrite according to the manufacturing method according to the first embodiment of the present invention has a low investment loss and a low dielectric loss, and thus can be applied as an electronic component material in a high frequency region.
- nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention can be applied to the antenna substrate material.
- dielectric antennas having dielectric constants 6 to 7 have a shortening ratio of about 2.65.
- the antenna using nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention has a reduction ratio of about 8.37 due to the high dielectric constant and permeability characteristics. That is, when the nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention is used as the antenna substrate material, the antenna shortening effect is increased.
- FIG. 5 shows an application example in which nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention is applied to an antenna which is one of electronic components.
- FIG. 5 is a graph comparing resonant frequency and dB when comparing the antenna substrate material to which nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention is compared with a material having a dielectric constant of 40 having the same frequency.
- 6 is a table numerically showing their performance characteristics.
- the dB decreases downward in the resonant frequency region, indicating that the efficiency is increased, and the wide spread laterally indicates a wider bandwidth.
- the nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention has an excellent performance in efficiency and bandwidth compared to the material of the dielectric constant 40. That is, the antenna manufactured using the nickel manganese cobalt spinel ferrite of the present invention can be seen that the bandwidth is wider, the efficiency is also increased. In contrast, antennas with a dielectric constant of 40 do not appear to generate resonance due to their very low resonance.
- FIG. 7 is a block diagram illustrating a method of manufacturing nickel manganese cobalt spinel ferrite according to a second embodiment of the present invention.
- nickel oxide, cobalt oxide, manganese oxide and iron oxide were weighed at a molar ratio of about 0.76: 0.006: 0.058: 1.14.
- S710 it is preferable to use iron oxide whose average particle size is less than 1 micrometer.
- the nickel oxide, cobalt oxide, manganese oxide, and iron oxide thus provided are wet mixed in methanol (MeOH) for about 48 hours using a ball mill (S720).
- Powders are taken from the nickel oxide, cobalt oxide, manganese oxide, and iron oxide mixture and dried at about 120 ° C. for about 12 hours (S730).
- the dried powder is pulverized to have a small particle size (S740).
- the dried and pulverized powder is subjected to a first heat treatment process.
- Primary heat treatment is performed at a temperature of about 800 ° C (S750).
- the process of synthesizing the spinel ferrite in the secondary heat treatment and the tertiary heat treatment performed later can be further promoted.
- the first heat-treated powder is subjected to the second heat treatment process.
- the secondary heat treatment is performed at a temperature of about 1100 ° C. (S760).
- the secondary heat-treated powder is subjected to a third heat treatment process, the third heat treatment is performed at a temperature of about 1150 °C (S770).
- nickel oxide, cobalt oxide, manganese oxide and iron oxide are synthesized as spinel ferrite.
- the present invention is not limited thereto, and the molar ratio of nickel oxide, cobalt oxide, manganese oxide, and iron oxide is 0.6 to 0.8: 0.005 to 0.007: 0.057 to 0.059: 1.13 to 1.15, the wet mixing may be carried out for 45 to 50 hours, the powder may be dried at 110 °C to 130 °C for 11 hours to 13 hours.
- primary heat processing can be performed at 750 degreeC-850 degreeC
- secondary heat processing can be performed at 1050 degreeC-1150 degreeC
- tertiary heat processing can also be performed at 1100 degreeC-1200 degreeC.
- nickel manganese cobalt spinel ferrite according to the second embodiment of the present invention namely, iron oxide having a molar ratio of 1.13 to 1.15 is used, unlike the first embodiment of the present invention, and the second and third heat treatment temperatures are 100 ° C.
- the reduced manufactured nickel manganese cobalt spinel ferrite has an investment loss of 0.02 or less at 230 MHz as shown in FIG. 8.
- the nickel manganese cobalt spinel ferrite according to the second embodiment of the present invention has an investment loss that is reduced by 0.02 or more compared to the nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention, thereby increasing the efficiency of the antenna when applied to the antenna.
- the permittivity and permeability of the nickel manganese cobalt spinel ferrite according to the second embodiment of the present invention is 6 to 7 and 9 to 10, the same as the permittivity and permeability of nickel manganese cobalt spinel ferrite according to the first embodiment of the present invention.
- the nickel manganese cobalt spinel ferrites according to the first and second embodiments of the present invention have low investment loss and low dielectric loss, and thus can be applied to electronic component materials, specifically antenna substrate materials, and the like in the high frequency region. have.
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Abstract
Description
Claims (13)
- 저투자손실과 저유전손실을 가지는 스피넬 페라이트 제조 방법에 있어서,산화니켈, 산화코발트, 산화망간 및 산화철을 제공하는 단계;상기 산화니켈, 상기 산화코발트, 상기 산화망간 및 상기 산화철을 메탄올에서 습식 혼합하는 단계;상기 산화니켈, 상기 산화코발트, 상기 산화망간 및 상기 산화철 혼합물에서 분체를 취하여 건조하는 단계;상기 건조된 분체를 분쇄하는 단계; 및상기 분체를 열처리하는 단계;를 포함하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 1 항에 있어서,상기 분체를 열처리하는 단계에서 상기 열처리는 복수 회 진행하는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 2 항에 있어서,상기 산화니켈, 상기 산화코발트, 상기 산화망간 및 상기 산화철은 0.6 내지 0.8 : 0.005 내지 0.007 : 0.052 내지 0.054 : 1.04 내지 1.06의 몰(mol)비로 제공되는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 2 항에 있어서,상기 산화니켈, 상기 산화코발트, 상기 산화망간 및 상기 산화철은 0.6 내지 0.8 : 0.005 내지 0.007 : 0.057 내지 0.059 : 1.13 내지 1.15의 몰(mol)비로 제공되는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 4 항에 있어서,상기 산화철의 평균 입도는 1㎛ 미만인 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 1 항 내지 제 5 항 중 어느 한 항에 있어서,상기 습식 혼합하는 단계는 볼밀(ball mill)로 45시간 내지 50시간 동안 수행되는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 1 항 내지 제 5 항 중 어느 한 항에 있어서,상기 혼합물 분체를 건조하는 단계는 110℃ 내지 130℃에서 11시간 내지 13시간 동안 건조하는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 1 항 내지 제 5 항 중 어느 한 항에 있어서,상기 열처리 단계에서 첫번째 열처리는 750℃ 내지 850℃에서 행해지는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 8 항에 있어서,상기 첫번째 열처리 후 1150℃ 내지 1250℃에서 두번째 열처리가 행해지는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 8 항에 있어서,상기 첫번째 열처리 후 1050℃ 내지 1150℃에서 두번째 열처리가 행해지는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 9 항에 있어서,상기 두번째 열처리 후 1200℃ 내지 1300℃에서 세번째 열처리가 행해지는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 10 항에 있어서,상기 두번째 열처리 후 1100℃ 내지 1200℃에서 세번째 열처리가 행해지는 것을 특징으로 하는 니켈 망간 코발트 스피넬 페라이트 제조 방법.
- 제 1항 내지 제 5 항 중 어느 한 항의 방법으로 제조된 니켈 망간 코발트 스피넬 페라이트.
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JP2011521054A JP2011529436A (ja) | 2008-08-12 | 2009-08-10 | 低透磁損失を有するニッケル−マンガン−コバルト系スピネルフェライトの製造方法およびこれにより製造されたニッケル−マンガン−コバルト系スピネルフェライト |
US13/058,835 US20110147643A1 (en) | 2008-08-12 | 2009-08-10 | Method for producing nickel-manganese-cobalt spinel ferrite having low permeability loss and nickel-manganese-cobalt spinel ferrite produced thereby |
EP09806817A EP2327674A4 (en) | 2008-08-12 | 2009-08-10 | PROCESS FOR THE PRODUCTION OF NICKEL MANGANESE COBALT SPINELLE FERRITE WITH LOW LOSSES BY PERMEATION AND NICKEL MANGANESE COBALT SPINELLE FERRITE SO PRODUCED |
CN2009801294442A CN102105417A (zh) | 2008-08-12 | 2009-08-10 | 具有低透磁损失的镍锰钴尖晶石铁素体制造方法及由此方法制造的镍锰钴尖晶石铁素体 |
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CN113045304A (zh) * | 2021-03-25 | 2021-06-29 | 桂林电子科技大学 | 一种混合尖晶石结构的铁氧体吸波材料与制备方法 |
CN113548873A (zh) * | 2021-08-13 | 2021-10-26 | 新乡学院 | 一种锰钴氧化物陶瓷材料的制备方法 |
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KR101547972B1 (ko) * | 2014-01-09 | 2015-08-27 | 주식회사 이엔드디 | 니켈―코발트―망간 복합 전구체 제조 방법 |
KR102079734B1 (ko) * | 2017-01-26 | 2020-02-20 | 주식회사 엘지화학 | 산화적 탈수소화 반응용 페라이트 촉매, 이의 제조방법 및 이를 이용한 부타디엔의 제조방법 |
CN109267114B (zh) * | 2018-10-22 | 2020-08-21 | 中国科学院金属研究所 | 一种钴锰尖晶石涂层的制备方法 |
KR102638916B1 (ko) | 2018-11-15 | 2024-02-22 | 로저스코포레이션 | 고주파 자성 필름, 이의 제조 방법, 및 이의 용도 |
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US11679991B2 (en) | 2019-07-30 | 2023-06-20 | Rogers Corporation | Multiphase ferrites and composites comprising the same |
TW202116700A (zh) | 2019-09-24 | 2021-05-01 | 美商羅傑斯公司 | 鉍釕m型六方晶系鐵氧體、包含彼之組合物及複合物、及製造方法 |
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- 2009-08-10 WO PCT/KR2009/004441 patent/WO2010018955A2/ko active Application Filing
- 2009-08-10 CN CN2009801294442A patent/CN102105417A/zh active Pending
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CN113548873A (zh) * | 2021-08-13 | 2021-10-26 | 新乡学院 | 一种锰钴氧化物陶瓷材料的制备方法 |
CN113548873B (zh) * | 2021-08-13 | 2022-07-29 | 新乡学院 | 一种锰钴氧化物陶瓷材料的制备方法 |
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EP2327674A2 (en) | 2011-06-01 |
EP2327674A4 (en) | 2011-12-07 |
JP2011529436A (ja) | 2011-12-08 |
KR101045781B1 (ko) | 2011-07-04 |
KR20100020412A (ko) | 2010-02-22 |
WO2010018955A3 (ko) | 2010-07-01 |
CN102105417A (zh) | 2011-06-22 |
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