WO2016147943A1 - 扁平状軟磁性粉末及びその製造方法 - Google Patents
扁平状軟磁性粉末及びその製造方法 Download PDFInfo
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- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
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Definitions
- the present invention relates to a soft magnetic flat powder used for a magnetic sheet for noise suppression used in various electronic devices and a method for producing the same.
- a magnetic sheet containing a soft magnetic flat powder has been used as an electromagnetic wave absorber and an RFID (Radio Frequency Identification) antenna.
- RFID Radio Frequency Identification
- This digitizer includes an electromagnetic induction type as disclosed in, for example, Japanese Patent Application Laid-Open No. 2011-22661 (Patent Document 1), and a high-frequency signal transmitted from a coil built in the tip of a pen-shaped position indicator is The indicated position is detected by reading with a loop coil built in the panel-shaped position detector.
- a sheet serving as a magnetic path of the high-frequency signal is disposed on the back surface of the loop coil.
- a magnetic sheet in which a soft magnetic flat powder is oriented in a resin or rubber, a sheet in which a soft magnetic amorphous alloy foil is bonded, or the like is applied.
- the entire detection panel can be made into one sheet, so that excellent uniformity can be obtained without any detection failure at the bonded portion such as an amorphous foil.
- Patent Document 2 As a method of increasing the major axis of a soft magnetic flat powder and producing a flat powder having a high aspect ratio, the organic solvent has 2 carbon atoms. A method of performing flattening using 1 to 4 monohydric alcohols has been proposed.
- JP 2011-22661 A Japanese Patent No. 4636113
- Patent Document 2 discloses the coercive force as an index of magnetic characteristics, and the index of the aspect ratio as 50% particle diameter D 50 ( ⁇ m) and coercive force Hc (A / m) of the flat soft magnetic alloy powder.
- BD bulk density
- Hc coercive force
- the coercive force is the smallest in the state of spherical powder and tends to increase as the processing proceeds.
- the cause of the transition of the coercive force is considered to be the distortion of the crystal grain size accompanying the processing and the increase in the oxygen content due to oxidation from the surrounding water.
- the former can be improved by heat treatment, but the latter reacts with the surface texture of the powder even with a very small amount of water, and therefore it is very difficult to prevent an increase in the oxygen content during processing. For the above reasons, there is a limit to the magnetic permeability obtained with the conventional flat powder.
- an object of the present invention is to provide a soft magnetic flat powder capable of realizing a particularly high magnetic permeability when used as a magnetic sheet and a method for producing the same.
- a flat powder made of an Fe—Si—Al-based alloy having an average particle size of 43 to 60 ⁇ m and a coercive force Hc measured by applying a magnetic field in the longitudinal direction of the flat powder is 106 A. / M or less, ratio of tap density to true density is 0.17 or less, oxygen content is 0.6 mass% or less, manganese content is in the range of 0.1 mass% or more and 1.0 mass% or less, and the balance Is provided with a soft magnetic flat powder, which consists entirely of inevitable impurities.
- Raw material powder production process by gas atomization method or disk atomization method A flattening process for flattening the raw material powder; Heat treating the flattened powder in a vacuum or argon atmosphere at 700 to 900 ° C .; A method for producing the soft magnetic flat powder is provided.
- Soft flat powder of the soft magnetic flat powder present invention consists Fe-Si-Al alloy powder, the average particle diameter D 50 is 43 ⁇ 60 [mu] m. If the average particle size is less than 43 ⁇ m, it is difficult to obtain a flat powder having a high aspect ratio, and the real part permeability ⁇ ′ tends to be low. Moreover, since it will become difficult to form a sheet if the average particle size becomes too large, it is not preferable.
- the average particle diameter D 50 is preferably 50 to 60 ⁇ m, particularly preferably 51 to 58 ⁇ m.
- the soft magnetic flat powder of the present invention has a coercive force Hc measured by applying a magnetic field in the longitudinal direction of 106 A / m or less.
- the coercive force Hc is preferably 90 A / m or less, more preferably 80 A / m or less.
- the lower limit of the coercive force is not particularly limited, but typically it is preferably higher than 40 A / m in terms of production conditions.
- the ratio of the tap density to the true density of the soft magnetic flat powder of the present invention is 0.17 or less.
- the ratio of tap density to true density is preferably 0.14 or less, more preferably 0.11 or less.
- the lower limit of the tap density is not particularly limited, but is typically 0.07 or more. The tap density tends to monotonously decrease as the processing progresses, and long time processing may lead to a decrease in average particle size and an increase in coercive force.
- the soft magnetic flat powder of the present invention has an oxygen concentration of 0.6% by mass or less.
- the existence form of oxygen in the soft magnetic flat powder is considered to have two forms, a grain boundary precipitated oxide and a powder surface oxide, both of which are considered to be causes of an increase in coercive force. It is not preferable that the concentration is too high.
- the oxygen concentration is preferably 0.4% by mass or less, more preferably 0.3% by mass or less.
- the lower limit of the oxygen concentration is not particularly limited, but is typically 0.1% by mass or more.
- the amount of grain boundary precipitated oxide can be lowered by suppressing the oxidation in the preparation process of the raw soft magnetic spherical powder during the production of the soft magnetic flat powder and the flat working process. Moreover, the amount of powder surface oxides can be lowered by suppressing oxidation in the flattening process and the heat treatment process.
- Zener in the steady grain growth model, when the grain size of the structure does not grow any more, the driving force for grain growth and the pinning force by fine secondary particles are equal, and the grain radius is It is proportional to the ratio of (radius of dispersed particles / phase volume fraction of dispersed particles). Details are unknown, but the low oxygen content means that the coercive force is low because the oxide pinning effect is difficult to inhibit the grain growth during heat treatment, which is advantageous in terms of magnetic properties. It is thought that it becomes.
- the soft magnetic flat powder of the present invention has a manganese concentration of 0.1% by mass or more and 1.0% by mass or less. As described above, it is considered that there are two forms of oxygen in the soft magnetic flat powder, that is, grain boundary precipitated oxide and powder surface oxide. Although details are unknown, we think about the action of manganese as follows. That is, in the conventional Sendust flat powder having a low manganese concentration, there are innumerable fine oxides of Fe, Si, and Al. On the other hand, flat powder containing an appropriate concentration of manganese preferentially adsorbs oxygen originally contained in sendust, and manganese exists as manganese oxide. Since the pinning effect hardly occurs, the coercive force is lowered, which is considered advantageous in terms of magnetic characteristics.
- the manganese concentration is preferably 0.3 mass% or more and 0.7 mass% or less, more preferably 0.4 mass% or more and 0.6 mass% or less.
- the soft magnetic flat powder of the present invention can be produced by flattening a soft magnetic alloy powder (raw material powder).
- the soft magnetic alloy powder is preferably a powder having a low coercive force value, and more preferably a powder having a high saturation magnetization value. In general, it is an Fe—Si—Al alloy that has excellent coercive force and saturation magnetization.
- Soft magnetic alloy powder is produced by various atomizing methods such as a gas atomizing method and a water atomizing method. Since it is more preferable that the amount of oxygen contained in the soft magnetic alloy powder is small, production by a gas atomization method is preferred, and production using an inert gas is more preferred. Although the disk atomizing method can be used for manufacturing without problems, the gas atomizing method is superior from the viewpoint of mass productivity.
- the particle size of the soft magnetic alloy powder used in the present invention is not particularly limited, depending on the purpose of adjusting the average particle size after flattening, the purpose of removing powder with a large amount of oxygen content, and other manufacturing purposes, It may be classified.
- the soft magnetic alloy powder (raw material powder) is flattened.
- the flat processing method For example, it can carry out using an attritor, a ball mill, a vibration mill, etc. Among these, it is preferable to use an attritor that is relatively excellent in flat processing ability.
- an inert gas when performing a dry process, it is preferable to use an organic solvent.
- the type of organic solvent is not particularly limited.
- the amount of the organic solvent added is preferably 100 parts by mass or more and more preferably 200 parts by mass or more with respect to 100 parts by mass of the soft magnetic alloy powder.
- the upper limit of the organic solvent is not particularly limited, and can be appropriately adjusted according to the desired flat powder size / shape and the balance of productivity, but is typically 500 parts by mass or less.
- the water concentration in the organic solvent is preferably 0.002 parts by mass or less with respect to 100 parts by mass of the organic solvent.
- a flattening aid may be used together with the organic solvent, it is preferably 5 parts by mass or less with respect to 100 parts by mass of the soft magnetic alloy powder in order to suppress oxidation.
- the lower limit is not particularly limited, but is typically 0.1 parts by mass or more.
- the soft magnetic flat powder is heat-treated.
- the heat treatment apparatus is not particularly limited, but the heat treatment temperature is preferably 700 ° C. to 900 ° C. By performing the heat treatment at the corresponding temperature, the coercive force is lowered and a soft magnetic flat powder with high permeability is obtained.
- limiting in particular about heat processing time It is good to select suitably according to a processing amount and productivity. In the case of long-time heat treatment, the productivity is lowered, and therefore within 5 hours is preferable.
- the soft magnetic flat powder used in the present invention is preferably heat-treated in vacuum or in an inert gas in order to suppress oxidation.
- heat treatment may be performed in a gas in nitrogen. In this case, the coercive force value increases, and the magnetic permeability tends to decrease as compared with the case of heat treatment in vacuum.
- surface-treated powder may be suitable, and the powder produced by the flat processing method of the present invention may be used during the heat treatment process or before and after the heat treatment process.
- a surface treatment step may be added as necessary.
- heat treatment may be performed in an atmosphere containing a small amount of active gas.
- Magnetic Sheet Manufacturing Method can also be performed by a conventionally proposed method. For example, it can be produced by mixing a flat powder with a solution obtained by dissolving chlorinated polyethylene or the like in toluene, and applying and drying the mixture with various presses or rolls.
- a powder having a predetermined component was prepared by a gas atomizing method or a disk atomizing method, and classified to 150 ⁇ m or less.
- Gas atomization was performed by using an alumina crucible for melting, discharging molten alloy from a nozzle having a diameter of 5 mm under the crucible, and spraying high pressure argon on the molten alloy.
- the obtained raw material powder was flattened by an attritor.
- the attritor used a ball of 4.8 mm in diameter made by SUJ2, was put into a stirring vessel together with the raw material powder and industrial ethanol, and the flattening process was carried out at a blade rotation speed of 300 rpm.
- the amount of industrial ethanol added was 200 to 500 parts by mass with respect to 100 parts by mass of the raw material powder.
- the flattening aid was not added, or 1 to 5 parts by mass with respect to 100 parts by mass of the raw material powder.
- the flat powder and industrial ethanol taken out from the stirring vessel after flattening were transferred to a stainless steel dish and dried at 80 ° C. for 24 hours.
- the flat powder thus obtained was heat-treated at 700 to 900 ° C. for 2 hours in vacuum or argon and used for various evaluations. Table 1 shows the detailed conditions when producing the flat powder.
- ⁇ Evaluation of flat powder> The average particle diameter, true density, tap density, oxygen content, nitrogen content, and coercive force of the obtained flat powder were evaluated.
- the average particle size was evaluated by a laser diffraction method, and the true density was evaluated by a gas displacement method.
- the tap density was evaluated based on the packing density when about 20 g of flat powder was filled in a cylinder having a volume of 100 cm 3 and the drop height was 10 mm and the number of taps was 200 times.
- the coercive force was measured by filling a flat container with a resin container having a diameter of 6 mm and a height of 8 mm, and magnetizing in the height direction and magnetizing in the diameter direction.
- the flat powder is flattened when magnetized in the height direction of the container and flattened when magnetized in the thickness direction of the flat powder and in the diameter direction of the container. It becomes the coercive force in the longitudinal direction of the powder.
- the applied magnetic field was 144 kA / m.
- permeability real part of complex permeability: ⁇ ′ .
- the cross section of the obtained magnetic sheet was resin-filled and polished, and from the optical microscope image, 50 powders were measured at random in the longitudinal direction length and thickness, and the ratio of the longitudinal length and thickness was averaged. The aspect ratio was used.
- No. 22 to 40 comparative example Except that the conditions during the production of the flat powder were as shown in Table 2, the production and evaluation of the flat powder and the production and evaluation of the magnetic sheet were conducted as No. 1 The same procedure as in 1 to 21 was performed.
- Comparative Example No. shown in Table 2 22 is producing the raw material powder by water atomization. For this reason, the oxygen content of the flat powder becomes high, so the magnetic permeability does not improve. Comparative Example No. In No. 23, the processing time is extended due to the influence of the excessive addition of the flattening aid, and as a result, the amount of oxygen contained increases, so the magnetic permeability does not improve. Comparative Example No. No. 24 is heat-treated in an air atmosphere, and the oxygen content is high, so the magnetic permeability does not improve. Comparative Example No. No. 25 has a high oxygen content and does not improve the permeability value.
- Comparative Example No. Nos. 26 to 28 have a higher raw material powder amount / solvent amount ratio than the examples. Therefore, the average particle diameter does not improve and the magnetic permeability does not improve. Comparative Example No. In No. 29, the average particle size is lowered by long-time processing, and the oxygen content is increased, so the magnetic permeability is not improved. Comparative Example No. No. 30 does not improve the average particle size and does not increase the magnetic permeability. Comparative Example No. Since 31 is not heat-treated and the coercive force does not decrease, the magnetic permeability is not improved.
- Comparative Example No. In Nos. 32 to 33, the heat treatment temperature is lower and the coercive force is not lowered compared to the example, so that the magnetic permeability is not improved. Comparative Example No. No. 34 has a higher heat treatment temperature than that of the example, and the permeability is not improved due to an increase in tap density ratio and coercive force due to powder aggregation. Comparative Example No. Compared with the example 35, 35 has a short processing time and is not sufficiently flattened, so the magnetic permeability is not improved. Comparative Example No. Since 36 is heat-treated in a nitrogen atmosphere and has a high coercive force, the magnetic permeability is not improved.
- Comparative Example No. No. 37 contains less manganese than in the examples, the coercive force is not lowered, and the magnetic permeability is not improved. Comparative Example No. No. 38 has an excessive amount of manganese compared to the examples, the coercive force is not lowered, and the magnetic permeability is not improved. Comparative Example No. No. 39 has a higher coercive force than the embodiment and does not improve the magnetic permeability.
- Comparative Example No. No. 40 has a larger average particle size D 50 than the examples. Therefore, sheet formation becomes difficult, the orientation of the flat powder is lowered, and the magnetic permeability is lowered.
- Example No. 1 to 21 are soft magnetic flat powders that satisfy the conditions according to the present invention. By using this soft magnetic flat powder, a magnetic sheet for an electromagnetic wave absorber having a sufficiently high magnetic permeability can be produced. It turns out that there is an effect.
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Abstract
Description
ガスアトマイズ法またはディスクアトマイズ法による原料粉末作製工程と、
前記原料粉末を扁平化する扁平加工工程と、
前記扁平加工された粉末を真空またはアルゴン雰囲気で、700~900℃で熱処理する工程と、
を備えた、前記軟磁性扁平粉末の製造方法が提供される。
本発明の軟磁性扁平粉末は、Fe-Si-Al系合金粉末からなり、その平均粒径D50が43~60μmである。平均粒径が43μm未満では、アスペクト比の高い扁平粉が得られ難く、実部透磁率μ’が低くなる傾向がある。また、平均粒径が大きくなりすぎると、シート成型が困難になるため好ましくない。平均粒径D50は、好ましくは50~60μm、特に好ましくは51~58μmである。
次に、本発明の軟磁性扁平粉末の製造方法について説明する。
<軟磁性合金粉末(原料粉末)準備工程>
本発明の軟磁性扁平粉末は、軟磁性合金粉末(原料粉末)を扁平化処理することで作製することができる。軟磁性合金粉末は、保磁力の値が低い粉末であることが好ましく、飽和磁化の値が高い粉末であることがより好ましい。一般的に、保磁力と飽和磁化の値が優れているのは、Fe-Si-Al系合金である。
次に、上記軟磁性合金粉末(原料粉末)を扁平化する。扁平加工方法は、特に制限は無く、例えば、アトライタ、ボールミル、振動ミル等を用いて行うことができる。中でも、比較的扁平加工能力に優れるアトライタを用いることが好ましい。また、乾式で加工を行う場合は、不活性ガスを用いることが好ましい。湿式で加工する場合は、有機溶媒を用いることが好ましい。有機溶媒の種類については特に限定されない。
次に、上記軟磁性扁平粉末を熱処理する。熱処理装置について特に制限は無いが、熱処理温度は700℃~900℃の条件で熱処理されることが好ましい。該当温度で熱処理を行うことによって、保磁力が低下し、高透磁率の軟磁性扁平粉末となる。また、熱処理時間について特に制限は無く、処理量や生産性に応じて適宜選択されるとよい。長時間の熱処理の場合、生産性が低下するため、5時間以内が好適である。
磁性シートの製造方法も従来提案されている方法で可能である。例えば、トルエンに塩素化ポリエチレンなどを溶解したものに扁平粉末を混合し、これを塗布、乾燥させたものを各種のプレスやロールで圧縮することで製造可能である。
<扁平粉末の作製>
ガスアトマイズ法あるいはディスクアトマイズ法により所定の成分の粉末を作製し150μm以下に分級した。ガスアトマイズは、アルミナ製坩堝を溶解に用い、坩堝下の直径5mmのノズルから合金溶湯を出湯し、これに高圧アルゴンを噴霧することで実施した。得られた原料粉末をアトライタにより扁平加工した。アトライタは、SUJ2製の直径4.8mmのボールを使用し、原料粉末と工業エタノールとともに攪拌容器に投入し、羽根の回転数を300rpmとして扁平加工を実施した。工業エタノールの添加量は、原料粉末100質量部に対し、200~500質量部とした。扁平化助剤は、添加しないか、もしくは、原料粉末100質量部に対し、1~5質量部とした。扁平加工後に攪拌容器から取り出した扁平粉末と工業エタノールをステンレス製の皿に移し、80℃で24時間乾燥させた。このようにして得た扁平粉末を真空中あるいはアルゴン中で、700~900℃で2時間熱処理し、各種の評価に用いた。なお、表1に扁平粉作製時の詳細な条件を示す。
得られた扁平粉末の平均粒径、真密度、タップ密度、酸素含有量、窒素含有量、保磁力を評価した。平均粒径はレーザー回折法、真密度はガス置換法で評価した。タップ密度は、約20gの扁平粉末を、容積100cm3のシリンダーに充填し、落下高さ10mmタップ回数200回とした時の充填密度で評価した。保磁力は直径6mm、高さ8mmの樹脂製容器に扁平粉末を充填し、この容器の高さ方向に磁化した場合と、直径方向に磁化した場合の値を測定した。なお、扁平粉末は充填された円柱の高さ方向が厚さ方向となっているため、容器の高さ方向に磁化した場合が扁平粉末の厚さ方向、容器の直径方向に磁化した場合が扁平粉末の長手方向の保磁力となる。印加磁場は144kA/mで実施した。
トルエンに塩素化ポリエチレンを溶解し、これに得られた扁平粉末を混合分散した。この分散液をポリエステル樹脂に厚さ100μm程度に塗布し常温常湿で乾燥させた。その後、130℃、15MPaの圧力でプレス加工し磁性シートを得た。磁性シートのサイズは150mm角で厚さは50μmである。なお、磁性シート中の扁平粉末の体積充填率はいずれも約50%であった。次に、この磁性シートを、外径7mm、内径3mmのドーナツ状に切り出し、インピーダンス測定器により、室温で1MHzにおけるインピーダンス特性を測定し、その結果から透磁率(複素透磁率の実数部:μ’)を算出した。さらに、得られた磁性シートの断面を樹脂埋め研磨し、その光学顕微鏡像から、長手方向の長さと厚さとをランダムに50粉末測定し、この長手方向の長さと厚さの比を平均してアスペクト比とした。
扁平粉作製時の条件を表2に示すとおりとした以外は、扁平粉の作製及び評価、並びに磁性シートの作製及び評価を、No.1~21と同様にして行なった。
Claims (9)
- Fe-Si-Al系合金からなる扁平粉末であって、平均粒径が43~60μm、扁平粉末の長手方向に磁場を印加して測定した保磁力Hcが106A/m以下、真密度に対するタップ密度の比が0.17以下、酸素含有量が0.6質量%以下、マンガン含有量が0.1質量%以上1.0質量%以下の範囲であり、残部はすべて不可避不純物からなる、軟磁性扁平粉末。
- 前記平均粒径が50~60μmである、請求項1に記載の軟磁性扁平粉末。
- 前記保磁力Hcが90A/m以下である、請求項1又は2に記載の軟磁性扁平粉末。
- 前記真密度に対するタップ密度の比が0.11以下である、請求項1~3のいずれか一項に記載の軟磁性扁平粉末。
- 前記酸素含有量が0.3質量%以下である、請求項1~4のいずれか一項に記載の軟磁性粉末。
- 前記マンガン含有量が0.3質量%以上0.7質量%以下である、請求項1~5のいずれか一項に記載の軟磁性扁平粉末。
- ガスアトマイズ法またはディスクアトマイズ法による原料粉末作製工程と、
前記原料粉末を扁平化する扁平加工工程と、
前記扁平加工された粉末を真空またはアルゴン雰囲気で、700~900℃で熱処理する工程と、
を備えた、請求項1~6のいずれか一項に記載の軟磁性扁平粉末の製造方法。 - 前記扁平加工工程の際、有機溶媒を用いた湿式で加工し、該有機溶媒の添加量が、前記原料粉末100質量部に対して100質量部以上である、請求項7に記載の製造方法。
- 前記扁平加工工程の際、扁平化助剤を用い、その使用量が、前記原料粉末100質量部に対して、5質量部以下である、請求項7又は8に記載の製造方法。
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