JP2021082664A - Composition for electromagnetic wave shield, sheet for electromagnetic wave shield, electromagnetic wave shield film, and electronic component device - Google Patents
Composition for electromagnetic wave shield, sheet for electromagnetic wave shield, electromagnetic wave shield film, and electronic component device Download PDFInfo
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- JP2021082664A JP2021082664A JP2019207277A JP2019207277A JP2021082664A JP 2021082664 A JP2021082664 A JP 2021082664A JP 2019207277 A JP2019207277 A JP 2019207277A JP 2019207277 A JP2019207277 A JP 2019207277A JP 2021082664 A JP2021082664 A JP 2021082664A
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- Prior art keywords
- electromagnetic wave
- wave shielding
- composition
- soft magnetic
- resin
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Images
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- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Description
本開示は、電磁波シールド用組成物、電磁波シールド用シート、電磁波シールド膜及び電子部品装置に関する。 The present disclosure relates to an electromagnetic wave shielding composition, an electromagnetic wave shielding sheet, an electromagnetic wave shielding film, and an electronic component device.
電子機器に外部から不要な電磁波が入射すると、誤作動を起こす可能性がある。そこで、電子機器には外部からの不要な電磁波をシールドする電磁波シールド材が用いられている。 If an unnecessary electromagnetic wave is incident on an electronic device from the outside, it may cause a malfunction. Therefore, an electromagnetic wave shielding material that shields unnecessary electromagnetic waves from the outside is used in electronic devices.
多くの電磁波シールド材は金属で構成されており、電磁波を反射することで電子機器を電磁波からシールドする。
しかし、一般的に用いられる金属のシールド材では低周波の磁界をほとんど反射することができず、電子機器を低周波の磁界からシールドすることが困難となる。
Many electromagnetic wave shielding materials are made of metal and reflect electromagnetic waves to shield electronic devices from electromagnetic waves.
However, a commonly used metal shield material can hardly reflect a low frequency magnetic field, and it becomes difficult to shield an electronic device from a low frequency magnetic field.
低周波の磁界から電子機器をシールドする場合、比透磁率の高い軟磁性体を用いるのが効果的である。磁界が比透磁率の高い領域を通りやすいという性質を利用し、保護したい部分に磁界が通らないようにすることで電子機器をシールドする。平面的な部分にシールド材を設ける場合は、シート又はフィルムのような形態でもよいが、表面形状の複雑な被着体にシールド材を設ける場合は、塗装のような方法で行うのが好ましい。その場合、シールド材は塗料で提供され、軟磁性体は粉末として樹脂等と一緒に混合される。 When shielding an electronic device from a low-frequency magnetic field, it is effective to use a soft magnetic material having a high relative magnetic permeability. Utilizing the property that the magnetic field easily passes through the region with high relative permeability, the electronic device is shielded by preventing the magnetic field from passing through the part to be protected. When the shielding material is provided on a flat portion, it may be in the form of a sheet or a film, but when the shielding material is provided on an adherend having a complicated surface shape, it is preferably performed by a method such as painting. In that case, the shielding material is provided as a paint, and the soft magnetic material is mixed with a resin or the like as a powder.
しかし、軟磁性体は塗料で用いられるような粒径が１０μｍ程度の大きさになると、バルクで高い比透磁率を持っていたとしてもほぼ粉末形状に依存する比透磁率になってしまう。粉末形状では、球よりもアスペクト比が大きな扁平形状のほうが高い比透磁率を持つ。 However, when the particle size of the soft magnetic material is about 10 μm as used in paints, even if the soft magnetic material has a high relative magnetic permeability in bulk, the relative magnetic permeability becomes almost dependent on the powder shape. In the powder form, the flat shape having a large aspect ratio has a higher relative permeability than the sphere.
一方、軟磁性体粉末同士の間に比透磁率の低い領域（空隙、塗料中に混合する樹脂等）が存在すると比透磁率の低い領域に磁束が漏れてしまい、シールド膜全体の比透磁率が低下してしまう。 On the other hand, if there is a region with low relative permeability (voids, resin mixed in the paint, etc.) between the soft magnetic powders, magnetic flux leaks to the region with low relative permeability, and the relative permeability of the entire shield film Will decrease.
粒径が１０μｍ程度の軟磁性体粉末を用いて高い比透磁率を得るために、アスペクト比の大きな扁平形状の軟磁性粉末をより密に充填し、磁束が漏れてしまう領域をなるべく少なくすることが試みられている（例えば、特許文献１参照）。 In order to obtain a high relative permeability using a soft magnetic powder having a particle size of about 10 μm, a flat-shaped soft magnetic powder having a large aspect ratio should be packed more densely to minimize the region where magnetic flux leaks. Has been attempted (see, for example, Patent Document 1).
扁平形状の軟磁性粒子を高密度に充填するには、プレス等の方法が考えられるが、表面形状の複雑な被着体に塗装する場合はプレスにより高密度充填化することは困難である。従って、軟磁性体扁平粉末が密に充填されず、高い比透磁率を得ることが困難となる場合がある。
また、特許文献１のように軟磁性体扁平粉末を密に充填させたとしても、未だ軟磁性体扁平粉末間には比透磁率の低い領域（空気、樹脂等）がある程度存在する。そのため、特許文献１の方法によっても高い比透磁率を得られない場合がある。
本開示は、上記従来の事情に鑑みてなされたものであり、比透磁率の高い皮膜を形成可能な電磁波シールド用組成物、並びに、この電磁波シールド用組成物を用いた電磁波シールド用シート、電磁波シールド膜及び電子部品装置を提供することを目的とする。
In order to fill the flat-shaped soft magnetic particles at high density, a method such as a press can be considered, but when painting on an adherend having a complicated surface shape, it is difficult to fill the soft magnetic particles with a high density by pressing. Therefore, the soft magnetic flat powder may not be densely packed, and it may be difficult to obtain a high relative magnetic permeability.
Further, even if the soft magnetic flat powder is densely packed as in
The present disclosure has been made in view of the above-mentioned conventional circumstances, and includes an electromagnetic wave shielding composition capable of forming a film having a high relative magnetic permeability, an electromagnetic wave shielding sheet using this electromagnetic wave shielding composition, and an electromagnetic wave. It is an object of the present invention to provide a shield film and an electronic component device.
前記課題を達成するための具体的手段は以下の通りである。
＜１＞ 軟磁性体粒子と樹脂とを含有し、
前記軟磁性体粒子の粒度分布が、少なくとも２つのピークを有する電磁波シールド用組成物。
＜２＞ 前記少なくとも２つのピークのうちの最も大粒子径側のピークの頂点が、前記粒度分布における１０μｍ以上の範囲に位置する＜１＞に記載の電磁波シールド用組成物。
＜３＞ 前記最も大粒子径側のピークに帰属する前記軟磁性体粒子についての平均アスペクト比が、２以上である＜２＞に記載の電磁波シールド用組成物。
＜４＞ 前記少なくとも２つのピークのうちの大粒子径側から２番目に位置するピークの頂点が、前記粒度分布における３μｍ以下の範囲に位置する＜１＞〜＜３＞のいずれか１項に記載の電磁波シールド用組成物。
＜５＞ 前記粒度分布における、前記最も大粒子径側のピークの頂点をＡμｍとし、前記大粒子径側から２番目に位置するピークの頂点をＢμｍとしたときに、比（Ａ／Ｂ）が、１０以上である＜１＞〜＜４＞のいずれか１項に記載の電磁波シールド用組成物。
＜６＞ 前記軟磁性体粒子が、鉄、鉄合金又はフェライトの粒子を含む＜１＞〜＜５＞のいずれか１項に記載の電磁波シールド用組成物。
＜７＞ ＜１＞〜＜６＞のいずれか１項に記載の電磁波シールド用組成物を含む樹脂組成物層を有する電磁波シールド用シート。
＜８＞ ＜１＞〜＜６＞のいずれか１項に記載の電磁波シールド用組成物により形成された電磁波シールド膜。
＜９＞ ＜８＞に記載の電磁波シールド膜により覆われた領域を有する電子部品装置。
Specific means for achieving the above-mentioned problems are as follows.
<1> Contains soft magnetic particles and resin,
An electromagnetic wave shielding composition in which the particle size distribution of the soft magnetic particles has at least two peaks.
<2> The composition for electromagnetic wave shielding according to <1>, wherein the apex of the peak on the largest particle diameter side of the at least two peaks is located in a range of 10 μm or more in the particle size distribution.
<3> The composition for electromagnetic wave shielding according to <2>, wherein the average aspect ratio of the soft magnetic particles belonging to the peak on the largest particle diameter side is 2 or more.
<4> In any one of <1> to <3>, the apex of the peak located second from the large particle diameter side of the at least two peaks is located in the range of 3 μm or less in the particle size distribution. The composition for electromagnetic wave shielding described.
<5> In the particle size distribution, the ratio (A / B) is when the apex of the peak on the largest particle size side is A μm and the apex of the peak located second from the large particle size side is B μm. 10. The composition for electromagnetic wave shielding according to any one of <1> to <4>, which is 10 or more.
<6> The composition for electromagnetic wave shielding according to any one of <1> to <5>, wherein the soft magnetic particles include iron, iron alloy, or ferrite particles.
<7> An electromagnetic wave shielding sheet having a resin composition layer containing the electromagnetic wave shielding composition according to any one of <1> to <6>.
<8> An electromagnetic wave shielding film formed by the electromagnetic wave shielding composition according to any one of <1> to <6>.
<9> An electronic component device having a region covered with the electromagnetic wave shielding film according to <8>.
本開示によれば、比透磁率の高い皮膜を形成可能な電磁波シールド用組成物、並びに、この電磁波シールド用組成物を用いた電磁波シールド用シート、電磁波シールド膜及び電子部品装置を提供することができる。 According to the present disclosure, it is possible to provide an electromagnetic wave shielding composition capable of forming a film having a high relative magnetic permeability, and an electromagnetic wave shielding sheet, an electromagnetic wave shielding film, and an electronic component device using this electromagnetic wave shielding composition. it can.
以下、本開示を実施するための形態について詳細に説明する。但し、本開示は以下の実施形態に限定されるものではない。以下の実施形態において、その構成要素（要素ステップ等も含む）は、特に明示した場合を除き、必須ではない。数値及びその範囲についても同様であり、本開示を制限するものではない。 Hereinafter, modes for carrying out the present disclosure will be described in detail. However, the present disclosure is not limited to the following embodiments. In the following embodiments, the components (including element steps and the like) are not essential unless otherwise specified. The same applies to the numerical values and their ranges, and does not limit this disclosure.
本開示において「工程」との語には、他の工程から独立した工程に加え、他の工程と明確に区別できない場合であってもその工程の目的が達成されれば、当該工程も含まれる。
本開示において「〜」を用いて示された数値範囲には、「〜」の前後に記載される数値がそれぞれ最小値及び最大値として含まれる。
本開示中に段階的に記載されている数値範囲において、一つの数値範囲で記載された上限値又は下限値は、他の段階的な記載の数値範囲の上限値又は下限値に置き換えてもよい。また、本開示中に記載されている数値範囲において、その数値範囲の上限値又は下限値は、実施例に示されている値に置き換えてもよい。
本開示において、各成分には、該当する物質が複数種含まれていてもよい。組成物中に各成分に該当する物質が複数種存在する場合、各成分の含有率又は含有量は、特に断らない限り、組成物中に存在する当該複数種の物質の合計の含有率又は含有量を意味する。
本開示において、各成分に該当する粒子には、複数種の粒子が含まれていてもよい。組成物中に各成分に該当する粒子が複数種存在する場合、各成分の粒子径は、特に断らない限り、組成物中に存在する当該複数種の粒子の混合物についての値を意味する。
本開示において「層」又は「膜」との語には、当該層又は膜が存在する領域を観察したときに、当該領域の全体に形成されている場合に加え、当該領域の一部にのみ形成されている場合も含まれる。
本開示において「（メタ）アクリル」はアクリル及びメタクリルの少なくとも一方を意味する。
本開示において、層又は膜の平均厚みは、対象となる層又は膜の５点の厚みを測定し、その算術平均値として与えられる値とする。
本開示において、層又は膜の厚みを直接測定可能な場合には、マイクロメーターを用いて測定する。一方、１つの層の厚み又は複数の層の総厚みを測定する場合には、電子顕微鏡を用いて、測定対象の断面を観察することで測定してもよい。
In the present disclosure, the term "process" includes not only a process independent of other processes but also the process if the purpose of the process is achieved even if the process cannot be clearly distinguished from the other process. ..
The numerical range indicated by using "~" in the present disclosure includes the numerical values before and after "~" as the minimum value and the maximum value, respectively.
In the numerical range described stepwise in the present disclosure, the upper limit value or the lower limit value described in one numerical range may be replaced with the upper limit value or the lower limit value of another numerical range described stepwise. .. Further, in the numerical range described in the present disclosure, the upper limit value or the lower limit value of the numerical range may be replaced with the value shown in the examples.
In the present disclosure, each component may contain a plurality of applicable substances. When a plurality of substances corresponding to each component are present in the composition, the content or content of each component is the total content or content of the plurality of substances present in the composition unless otherwise specified. Means quantity.
In the present disclosure, the particles corresponding to each component may include a plurality of types of particles. When a plurality of particles corresponding to each component are present in the composition, the particle size of each component means a value for a mixture of the plurality of particles present in the composition unless otherwise specified.
In the present disclosure, the term "layer" or "membrane" refers to only a part of the region, in addition to the case where the layer or the membrane is formed in the entire region when the region where the layer or the membrane exists is observed. The case where it is formed is also included.
In the present disclosure, "(meth) acrylic" means at least one of acrylic and methacrylic.
In the present disclosure, the average thickness of a layer or film is a value given as an arithmetic mean value obtained by measuring the thickness of five points of the target layer or film.
In the present disclosure, when the thickness of a layer or a film can be directly measured, it is measured using a micrometer. On the other hand, when measuring the thickness of one layer or the total thickness of a plurality of layers, the measurement may be performed by observing the cross section of the measurement target using an electron microscope.
＜電磁波シールド用組成物＞
本開示の電磁波シールド用組成物は、軟磁性体粒子と樹脂とを含有し、前記軟磁性体粒子の粒度分布が、少なくとも２つのピークを有するものである。電磁波シールド用組成物は、上記成分以外のその他の成分を含有してもよい。
本開示の電磁波シールド用組成物によれば、比透磁率の高い皮膜を形成可能となる。その理由は明確ではないが、以下のように推察される。
本開示の電磁波シールド用組成物では、電磁波シールド用組成物に含有される軟磁性体粒子の粒度分布が、少なくとも２つのピークを有する。軟磁性体粒子の粒度分布が少なくとも２つのピークを有するとは、つまり、軟磁性体粒子が、平均粒子径が大きな第1の粒子群と、第1の粒子群よりも平均粒子径の小さい第２の粒子群とを少なくとも含有することを示す。
電磁波シールド用組成物により形成された皮膜中において、軟磁性体粒子の第１の粒子群に帰属される粒子間の空隙に、第1の粒子群よりも平均粒子径の小さい第２の粒子群に帰属される粒子が配置されることで、軟磁性体粒子が密に充填されやすくなる。軟磁性体粒子が密に充填されることで、軟磁性体粒子間に比透磁率が低く磁束の漏れの生じやすい領域が生じにくくなる。そのため、本開示の電磁波シールド用組成物によれば、比透磁率の高い皮膜を形成可能になると推察される。
<Composition for electromagnetic wave shielding>
The composition for electromagnetic wave shielding of the present disclosure contains soft magnetic particles and a resin, and the particle size distribution of the soft magnetic particles has at least two peaks. The composition for electromagnetic wave shielding may contain other components other than the above components.
According to the electromagnetic wave shielding composition of the present disclosure, it is possible to form a film having a high relative magnetic permeability. The reason is not clear, but it can be inferred as follows.
In the electromagnetic wave shielding composition of the present disclosure, the particle size distribution of the soft magnetic particles contained in the electromagnetic wave shielding composition has at least two peaks. The particle size distribution of the soft magnetic particles has at least two peaks, that is, the soft magnetic particles have a first particle group having a large average particle size and a first particle group having a smaller average particle size than the first particle group. It is shown that it contains at least 2 particle groups.
In the film formed by the composition for electromagnetic wave shielding, the second particle group having an average particle diameter smaller than that of the first particle group in the voids between the particles belonging to the first particle group of the soft magnetic particles. By arranging the particles attributed to, the soft magnetic particles can be easily packed densely. By densely filling the soft magnetic particles, it becomes difficult for a region where the relative magnetic permeability is low and magnetic flux leakage is likely to occur between the soft magnetic particles. Therefore, according to the electromagnetic wave shielding composition of the present disclosure, it is presumed that a film having a high relative magnetic permeability can be formed.
以下、本開示の電磁波シールド用組成物を構成する成分について詳細に説明する。 Hereinafter, the components constituting the electromagnetic wave shielding composition of the present disclosure will be described in detail.
（軟磁性体粒子）
本開示の電磁波シールド用組成物は、軟磁性体粒子を含有する。
本開示で用いられる軟磁性体粒子の粒度分布は、少なくとも２つのピークを有する。軟磁性体粒子の粒度分布は、５個以下のピークを有するものであってもよく、３つのピークを有するものであってもよく、２つのピークを有するものであってもよい。
軟磁性体粒子の粒度分布は、レーザー回折法を用いて測定される。レーザー回折法は、レーザー回折式粒度分布測定装置（例えば、株式会社島津製作所、ＳＡＬＤ３０００Ｊ）を用いて行うことができる。具体的には、軟磁性体粒子を、水等の分散媒に分散させて分散液を調製する。この分散液について、レーザー回折式粒度分布測定装置を用いて体積基準の粒度分布を求める。
また、レーザー回折式粒度分布測定装置を用いて小径側から体積累積分布曲線を描いた場合に、累積５０％となる粒子径（Ｄ５０、体積平均粒子径）を、軟磁性体粒子の平均粒子径とする。
電磁波シールド用組成物から軟磁性体粒子を抽出する方法は、特に限定されるものではない。例えば、電磁波シールド用組成物を溶媒で希釈し、遠心分離により軟磁性体粒子を抽出することができる。また、電磁波シールド用組成物を燃焼し、軟磁性体粒子を灰分として得ることもできる。
(Soft magnetic particles)
The electromagnetic wave shielding composition of the present disclosure contains soft magnetic particles.
The particle size distribution of the soft magnetic particles used in the present disclosure has at least two peaks. The particle size distribution of the soft magnetic particles may have 5 or less peaks, 3 peaks, or 2 peaks.
The particle size distribution of the soft magnetic particles is measured using a laser diffraction method. The laser diffraction method can be performed using a laser diffraction type particle size distribution measuring device (for example, Shimadzu Corporation, SALD3000J). Specifically, the soft magnetic particles are dispersed in a dispersion medium such as water to prepare a dispersion liquid. For this dispersion, a volume-based particle size distribution is obtained using a laser diffraction type particle size distribution measuring device.
Further, when a volume cumulative distribution curve is drawn from the small diameter side using a laser diffraction type particle size distribution measuring device, the particle size (D50, volume average particle size) that is cumulative 50% is set to the average particle size of the soft magnetic particles. And.
The method for extracting the soft magnetic particles from the composition for electromagnetic wave shielding is not particularly limited. For example, the electromagnetic wave shielding composition can be diluted with a solvent and the soft magnetic particles can be extracted by centrifugation. It is also possible to burn the electromagnetic wave shielding composition to obtain soft magnetic particles as ash.
少なくとも２つのピークのうちの最も大粒子径側のピークの頂点は、磁性体粒子の粒度分布における１０μｍ以上の範囲に位置することが好ましく、２５μｍ以上の範囲に位置することがより好ましく、４０μｍ以上の範囲に位置することがさらに好ましい。少なくとも２つのピークのうちの最も大粒子径側のピークの頂点は、磁性体粒子の粒度分布における１５０μｍ以下の範囲に位置していてもよい。 The apex of the peak on the largest particle size side of at least two peaks is preferably located in the range of 10 μm or more, more preferably 25 μm or more, and 40 μm or more in the particle size distribution of the magnetic particles. It is more preferable to be located in the range of. The apex of the peak on the largest particle diameter side of at least two peaks may be located in the range of 150 μm or less in the particle size distribution of the magnetic particles.
磁性体粒子の粒度分布における最も大粒子径側のピークに帰属する軟磁性体粒子についての平均アスペクト比は、高い比透磁率を得る観点から、２以上であることが好ましく、１０以上であることがより好ましく、２０以上であることがさらに好ましい。磁性体粒子の粒度分布における最も大粒子径側のピークに帰属する軟磁性体粒子についての平均アスペクト比は、１００以下であってもよい。 The average aspect ratio of the soft magnetic particles belonging to the peak on the largest particle size side in the particle size distribution of the magnetic particles is preferably 2 or more, and preferably 10 or more, from the viewpoint of obtaining a high relative permeability. Is more preferable, and 20 or more is further preferable. The average aspect ratio of the soft magnetic particles belonging to the peak on the largest particle diameter side in the particle size distribution of the magnetic particles may be 100 or less.
磁性体粒子の粒度分布における最も大粒子径側のピークに帰属する軟磁性体粒子についての平均アスペクト比は、下記方法により測定される。
電磁波シールド用組成物を用いて電磁波シールド膜を形成する。電磁波シールド膜の厚み方向に平行な断面を走査型電子顕微鏡により５００倍の条件で撮影し、断面写真を得る。得られた断面写真から、長手方向の長さ（Ｌμｍ）が、最も大粒子径側のピークの頂点の値の±４０％の長さの軟磁性体粒子を、１０個選択する。選択された軟磁性体粒子の各々について、長径（Ｌμｍ）及び短径（Ｓμｍ）を測定する。なお、粒子の長径とは、粒子の外接長方形の長さをいい、粒子の短径とは、粒子の外接長方形の幅をいう。各軟磁性体粒子について、長径（Ｌμｍ）と短径（Ｓμｍ）とのアスペクト比（Ｌ／Ｓ）を求める。各軟磁性体粒子のアスペクト比（Ｌ／Ｓ）の算術平均値を、最も大粒子径側のピークに帰属する軟磁性体粒子についての平均アスペクト比とする。
The average aspect ratio of the soft magnetic particles belonging to the peak on the largest particle diameter side in the particle size distribution of the magnetic particles is measured by the following method.
An electromagnetic wave shielding film is formed using the electromagnetic wave shielding composition. A cross section parallel to the thickness direction of the electromagnetic wave shield film is photographed with a scanning electron microscope under the condition of 500 times, and a cross section photograph is obtained. From the obtained cross-sectional photograph, 10 soft magnetic particles having a length (L μm) in the longitudinal direction of ± 40% of the value of the apex of the peak on the largest particle diameter side are selected. The major axis (L μm) and minor axis (S μm) are measured for each of the selected soft magnetic particles. The major axis of the particle means the length of the circumscribed rectangle of the particle, and the minor axis of the particle means the width of the circumscribed rectangle of the particle. For each soft magnetic particle, the aspect ratio (L / S) between the major axis (L μm) and the minor axis (S μm) is determined. The arithmetic mean value of the aspect ratio (L / S) of each soft magnetic particle is defined as the average aspect ratio of the soft magnetic particles belonging to the peak on the largest particle size side.
なお、本開示で用いられる軟磁性体粒子が、平均粒子径の異なる少なくとも２種類の軟磁性体粒子の混合物である場合、最も平均粒子径の大きい軟磁性体粒子についての平均アスペクト比を、最も大粒子径側のピークに帰属する軟磁性体粒子についての平均アスペクト比としてもよい。最も平均粒子径の大きい軟磁性体粒子についての平均アスペクト比は、下記方法により測定される。
最も平均粒子径の大きい軟磁性体粒子について、走査型電子顕微鏡により５００倍の条件で撮影して電子顕微鏡写真を得る。得られた電子顕微鏡写真から、１０個の軟磁性体粒子の各々について、長径（Ｌμｍ）及び短径（Ｓμｍ）を測定する。各軟磁性体粒子について、長径（Ｌμｍ）と短径（Ｓμｍ）とのアスペクト比（Ｌ／Ｓ）を求める。各軟磁性体粒子のアスペクト比（Ｌ／Ｓ）の算術平均値を、最も平均粒子径の大きい軟磁性体粒子についての平均アスペクト比とする。
When the soft magnetic particles used in the present disclosure are a mixture of at least two types of soft magnetic particles having different average particle diameters, the average aspect ratio of the soft magnetic particles having the largest average particle diameter is the highest. It may be used as the average aspect ratio for the soft magnetic particles attributable to the peak on the large particle size side. The average aspect ratio of the soft magnetic particles having the largest average particle size is measured by the following method.
The soft magnetic particles having the largest average particle size are photographed with a scanning electron microscope under a condition of 500 times to obtain an electron micrograph. From the obtained electron micrographs, the major axis (L μm) and the minor axis (S μm) are measured for each of the 10 soft magnetic particles. For each soft magnetic particle, the aspect ratio (L / S) between the major axis (L μm) and the minor axis (S μm) is determined. The arithmetic mean value of the aspect ratio (L / S) of each soft magnetic particle is defined as the average aspect ratio of the soft magnetic particle having the largest average particle diameter.
磁性体粒子の粒度分布における少なくとも２つのピークのうちの大粒子径側から２番目に位置するピークの頂点は、軟磁性体粒子を密に充填する観点から、磁性体粒子の粒度分布における３μｍ以下の範囲に位置することが好ましく、２μｍ以下の範囲に位置することがより好ましく、１μｍ以下の範囲に位置することがさらに好ましい。少なくとも２つのピークのうちの大粒子径側から２番目に位置するピークの頂点は、磁性体粒子の粒度分布における０．０５μｍ以上の範囲に位置していてもよい。 The apex of the peak located second from the large particle diameter side of at least two peaks in the particle size distribution of the magnetic particles is 3 μm or less in the particle size distribution of the magnetic particles from the viewpoint of densely filling the soft magnetic particles. It is preferable to be located in the range of 1 μm or less, more preferably to be located in the range of 1 μm or less. The apex of the peak located second from the large particle diameter side of at least two peaks may be located in the range of 0.05 μm or more in the particle size distribution of the magnetic particles.
磁性体粒子の粒度分布における、最も大粒子径側のピークの頂点をＡμｍとし、大粒子径側から２番目に位置するピークの頂点をＢμｍとしたときに、比（Ａ／Ｂ）は、軟磁性体粒子を密に充填する観点から、１０以上であることが好ましく、２５以上であることがより好ましく、４０以上であることがさらに好ましい。比（Ａ／Ｂ）は、５００以下であってもよい。 In the particle size distribution of magnetic particles, the ratio (A / B) is soft when the apex of the peak on the largest particle size side is A μm and the apex of the peak located second from the large particle size side is B μm. From the viewpoint of densely filling the magnetic particles, it is preferably 10 or more, more preferably 25 or more, and even more preferably 40 or more. The ratio (A / B) may be 500 or less.
例えば、軟磁性体粒子の粒度分布が、少なくとも３つのピークを有する場合、少なくとも３つのピークのうちの最も大粒子径側のピークの頂点が粒度分布における１０μｍ以上の範囲に位置し、少なくとも３つのピークのうちの大粒子径側から２番目に位置するピークの頂点が粒度分布における１μｍ〜３μｍの範囲に位置し、少なくとも３つのピークのうちの大粒子径側から３番目に位置するピークの頂点が粒度分布における０．０５μｍ〜１μｍの範囲に位置することが好ましい。 For example, when the particle size distribution of the soft magnetic particles has at least three peaks, the apex of the peak on the largest particle size side of the at least three peaks is located in the range of 10 μm or more in the particle size distribution, and at least three. The apex of the peak located second from the large particle size side of the peak is located in the range of 1 μm to 3 μm in the particle size distribution, and the apex of the peak located third from the large particle size side of at least three peaks. Is preferably located in the range of 0.05 μm to 1 μm in the particle size distribution.
軟磁性体粒子を構成する材料は特に限定されるものではなく、高い比透磁率を持つ物質であればよい。軟磁性体としては、ナノ結晶系軟磁性体、アモルファス系軟磁性体、フェライト系軟磁性体等が挙げられる。
また、軟磁性体としては、鉄、鉄合金、ニッケル、ニッケル合金、コバルト、コバルト合金、フェライト等が挙げられる。
軟磁性体粒子としては、安価に入手することができることから、鉄、鉄合金又はフェライトの粒子が好ましい。
鉄合金としては、センダスト、ケイ素鋼、パーメンジュール等が挙げられる。
フェライトとしては、マンガン亜鉛フェライト、ニッケル亜鉛フェライト、銅亜鉛フェライト、コバルトフェライト、ニッケルフェライト、マグネタイト等が挙げられる。
The material constituting the soft magnetic particles is not particularly limited, and any material having a high relative magnetic permeability may be used. Examples of the soft magnetic material include nanocrystalline soft magnetic material, amorphous soft magnetic material, ferrite soft magnetic material and the like.
Examples of the soft magnetic material include iron, iron alloy, nickel, nickel alloy, cobalt, cobalt alloy, ferrite and the like.
As the soft magnetic particles, iron, iron alloy or ferrite particles are preferable because they can be obtained at low cost.
Examples of the iron alloy include sendust, silicon steel, permendur and the like.
Examples of the ferrite include manganese-zinc ferrite, nickel-zinc ferrite, copper-zinc ferrite, cobalt ferrite, nickel ferrite, magnetite and the like.
本開示において、軟磁性体粒子の粒度分布が少なくとも２つのピークを有するためには、平均粒子径の異なる少なくとも２種類の軟磁性体粒子を混合することが好ましい。平均粒子径の異なる少なくとも２種類の軟磁性体粒子の組み合わせとしては、平均粒子径が１０μｍ以上の第１の軟磁性体粒子と、平均粒子径が３μｍ以下の第２の軟磁性体粒子との組み合わせが挙げられる。この場合、平均粒子径が１０μｍ以上の第１の軟磁性体粒子が第１の粒子群に、平均粒子径が３μｍ以下の第２の軟磁性体粒子が第２の粒子群に該当する。
なお、平均粒子径が１０μｍ以上の第１の軟磁性体粒子の平均アスペクト比は、２以上であることが好ましく、１０以上であることがより好ましく、２０以上であることがさらに好ましい。第１の軟磁性体粒子の平均アスペクト比は、１００以下であってもよい。
In the present disclosure, in order for the particle size distribution of the soft magnetic particles to have at least two peaks, it is preferable to mix at least two types of soft magnetic particles having different average particle diameters. As a combination of at least two types of soft magnetic particles having different average particle diameters, a first soft magnetic particle having an average particle diameter of 10 μm or more and a second soft magnetic particle having an average particle diameter of 3 μm or less are used. Combinations can be mentioned. In this case, the first soft magnetic particle having an average particle diameter of 10 μm or more corresponds to the first particle group, and the second soft magnetic particle having an average particle diameter of 3 μm or less corresponds to the second particle group.
The average aspect ratio of the first soft magnetic particles having an average particle diameter of 10 μm or more is preferably 2 or more, more preferably 10 or more, and even more preferably 20 or more. The average aspect ratio of the first soft magnetic particles may be 100 or less.
電磁波シールド用組成物中における軟磁性体粒子の含有率は特に制限されない。例えば、電磁波シールド用組成物の固形分全体に占める軟磁性体粒子の割合は、２０質量％以上であることが好ましく、３０質量％以上であることがより好ましく、４０質量％以上であることがさらに好ましい。電磁波シールド用組成物の固形分全体に占める軟磁性体粒子の割合は、９９質量％以下であってもよい。 The content of the soft magnetic particles in the electromagnetic wave shielding composition is not particularly limited. For example, the ratio of the soft magnetic particles to the total solid content of the electromagnetic wave shielding composition is preferably 20% by mass or more, more preferably 30% by mass or more, and more preferably 40% by mass or more. More preferred. The ratio of the soft magnetic particles to the total solid content of the electromagnetic wave shielding composition may be 99% by mass or less.
本開示の電磁波シールド用組成物は、電磁波シールド用組成物の効果を阻害しない範囲内で、軟磁性体粒子以外のその他の無機粒子を含有してもよい。その他の無機粒子としては、シリカ、ベントナイト、ヘクトライト等が挙げられる。その他の無機粒子の平均粒子径は、９００ｎｍ以下であることが好ましい。また、その他の無機微粒子の含有率は、軟磁性体粒子及び必要に応じて用いられるその他の無機粒子の合計に対して３０質量％以下であることが好ましく、２０質量％以下であることがより好ましい。 The electromagnetic wave shielding composition of the present disclosure may contain other inorganic particles other than the soft magnetic particles as long as the effects of the electromagnetic wave shielding composition are not impaired. Examples of other inorganic particles include silica, bentonite, hectorite and the like. The average particle size of the other inorganic particles is preferably 900 nm or less. The content of the other inorganic fine particles is preferably 30% by mass or less, more preferably 20% by mass or less, based on the total of the soft magnetic particles and other inorganic particles used as needed. preferable.
（樹脂）
本開示の電磁波シールド用組成物は、樹脂を含有する。電磁波シールド用組成物が樹脂を含むことで、電磁波シールド用組成物から形成される電磁波シールド膜の接着性が向上する傾向にある。
(resin)
The electromagnetic wave shielding composition of the present disclosure contains a resin. When the electromagnetic wave shielding composition contains a resin, the adhesiveness of the electromagnetic wave shielding film formed from the electromagnetic wave shielding composition tends to be improved.
電磁波シールド用組成物に含まれる樹脂は、熱可塑性樹脂であっても熱硬化性樹脂であっても、これらの組み合わせであってもよい。樹脂は、接着性を示すことが好ましい。また、樹脂は、加熱により重合反応を生じうる官能基を有するモノマーの状態であっても、すでに重合したポリマーの状態であってもよい。 The resin contained in the composition for electromagnetic wave shielding may be a thermoplastic resin, a thermosetting resin, or a combination thereof. The resin preferably exhibits adhesiveness. Further, the resin may be in the state of a monomer having a functional group capable of causing a polymerization reaction by heating, or in the state of a polymer that has already been polymerized.
耐熱性の観点からは、樹脂として熱硬化性樹脂を含むことが好ましい。熱硬化性樹脂としては、エポキシ基、アクリロイル基、メタクリロイル基、ヒドロキシ基、ビニル基、カルボキシ基、アミノ基、マレイミド基、酸無水物基、チオール基、チオニル基等の官能基を有する樹脂が挙げられる。 From the viewpoint of heat resistance, it is preferable to include a thermosetting resin as the resin. Examples of the thermosetting resin include resins having a functional group such as an epoxy group, an acryloyl group, a methacryloyl group, a hydroxy group, a vinyl group, a carboxy group, an amino group, a maleimide group, an acid anhydride group, a thiol group and a thionyl group. Be done.
熱可塑性樹脂として具体的には、（メタ）アクリル樹脂、ポリウレタン樹脂、ポリスチレン樹脂、ポリエステル樹脂、フッ素樹脂、ポリイミド樹脂、ポリアミド樹脂、ポリアミドイミド樹脂、ポリエーテルイミド樹脂、ポリエーテルエーテルケトン樹脂、ポリカーボネート樹脂等が挙げられる。
熱硬化性樹脂として具体的には、エポキシ樹脂、オキサジン樹脂、ビスマレイミド樹脂、フェノール樹脂、不飽和ポリエステル樹脂、シリコーン樹脂等が挙げられる。
これら樹脂の中でも、エポキシ樹脂が好ましい。
Specifically, the thermoplastic resin includes (meth) acrylic resin, polyurethane resin, polystyrene resin, polyester resin, fluororesin, polyimide resin, polyamide resin, polyamideimide resin, polyetherimide resin, polyetheretherketone resin, and polycarbonate resin. And so on.
Specific examples of the thermosetting resin include epoxy resin, oxazine resin, bismaleimide resin, phenol resin, unsaturated polyester resin, and silicone resin.
Among these resins, epoxy resin is preferable.
エポキシ樹脂の具体例としては、例えば、ビスフェノールＡ型エポキシ樹脂、ビスフェノールＦ型エポキシ樹脂、ビスフェノールＳ型エポキシ樹脂、フェノールノボラック型エポキシ樹脂、クレゾールノボラック型エポキシ樹脂、ナフタレン型エポキシ樹脂、ビフェノール型エポキシ樹脂、ビフェニルノボラック型エポキシ樹脂及び環式脂肪族エポキシ樹脂が挙げられる。樹脂成分は、１種類を単独で使用しても、２種類以上を併用してもよい。 Specific examples of the epoxy resin include bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, phenol novolac type epoxy resin, cresol novolac type epoxy resin, naphthalene type epoxy resin, and biphenol type epoxy resin. Examples thereof include biphenyl novolac type epoxy resin and cyclic aliphatic epoxy resin. One type of resin component may be used alone, or two or more types may be used in combination.
電磁波シールド用組成物中における樹脂の含有率は特に制限されない。例えば、電磁波シールド用組成物の固形分全体に占める樹脂の割合は、５質量％〜７０質量％であることが好ましく、１０質量％〜６０質量％であることがより好ましく、１５質量％〜５０質量％であることがさらに好ましい。
また、軟磁性体粒子及び必要に応じて用いられるその他の無機粒子を除く電磁波シールド用組成物の固形分に占める樹脂の割合は、１０質量％〜９９質量％であることが好ましく、２０質量％〜９８質量％であることがより好ましく、３０質量％〜９７質量％であることがさらに好ましい。
The content of the resin in the composition for electromagnetic wave shielding is not particularly limited. For example, the proportion of the resin in the total solid content of the electromagnetic wave shielding composition is preferably 5% by mass to 70% by mass, more preferably 10% by mass to 60% by mass, and 15% by mass to 50% by mass. It is more preferably mass%.
Further, the ratio of the resin to the solid content of the electromagnetic wave shielding composition excluding the soft magnetic particles and other inorganic particles used as needed is preferably 10% by mass to 99% by mass, preferably 20% by mass. It is more preferably ~ 98% by mass, and even more preferably 30% by mass to 97% by mass.
本開示の電磁波シールド用組成物は、接着性を向上するために、樹脂の１種として、ポリビニルアルコール樹脂、水溶性セルロース等の、樹脂中に水酸基を豊富に含む水溶性の有機高分子結合剤を併用してもよい。 The composition for electromagnetic wave shielding of the present disclosure is a water-soluble organic polymer binder containing abundant hydroxyl groups in the resin, such as polyvinyl alcohol resin and water-soluble cellulose, as one of the resins in order to improve the adhesiveness. May be used together.
（硬化剤）
樹脂が熱硬化性樹脂である場合、電磁波シールド用組成物は、熱硬化性樹脂を硬化する硬化剤を含有してもよい。
硬化剤の種類は特に限定されるものではなく、熱硬化性樹脂の種類に応じて適宜選択される。
(Hardener)
When the resin is a thermosetting resin, the electromagnetic wave shielding composition may contain a curing agent that cures the thermosetting resin.
The type of the curing agent is not particularly limited, and is appropriately selected depending on the type of the thermosetting resin.
熱硬化性樹脂がエポキシ樹脂である場合、硬化剤としては、アミン系硬化剤、フェノール系硬化剤、酸無水物系硬化剤等が挙げられる。硬化剤は、液体状のものでも固体状のものでも使用可能である。
硬化剤は、１種類を単独で使用しても、２種類以上を併用してもよい。
When the thermosetting resin is an epoxy resin, examples of the curing agent include amine-based curing agents, phenol-based curing agents, and acid anhydride-based curing agents. The curing agent can be either liquid or solid.
As the curing agent, one type may be used alone, or two or more types may be used in combination.
アミン系硬化剤としては、ｍ−フェニレンジアミン、１，３−ジアミノトルエン、１，４−ジアミノトルエン、２，４−ジアミノトルエン、３，５−ジエチル−２，４−ジアミノトルエン、３，５−ジエチル−２，６−ジアミノトルエン、２，４−ジアミノアニソール等の芳香環が１個の芳香族アミン硬化剤；４，４’−ジアミノジフェニルメタン、４，４’−ジアミノジフェニルスルホン、４，４’−メチレンビス（２−エチルアニリン）、３，３’−ジエチル−４，４’−ジアミノジフェニルメタン、３，３’，５，５’−テトラメチル−４，４’−ジアミノジフェニルメタン、３，３’，５，５’−テトラエチル−４，４’−ジアミノジフェニルメタン等の芳香環が２個の芳香族アミン硬化剤；芳香族アミン硬化剤の加水分解縮合物；ポリテトラメチレンオキシドジ−ｐ−アミノ安息香酸エステル、ポリテトラメチレンオキシドジ−ｐ−アミノベンゾエート等のポリエーテル構造を有する芳香族アミン硬化剤；芳香族ジアミンとエピクロロヒドリンとの縮合物；芳香族ジアミンとスチレンとの反応生成物；などが挙げられる。 Examples of the amine-based curing agent include m-phenylenediamine, 1,3-diaminotoluene, 1,4-diaminotoluene, 2,4-diaminotoluene, 3,5-diethyl-2,4-diaminotoluene, and 3,5-. Aromatic amine curing agent with one aromatic ring such as diethyl-2,6-diaminotoluene, 2,4-diaminoanisole; 4,4'-diaminodiphenylmethane, 4,4'-diaminodiphenylsulfone, 4,4' -Methylenebis (2-ethylaniline), 3,3'-diethyl-4,4'-diaminodiphenylmethane, 3,3', 5,5'-tetramethyl-4,4'-diaminodiphenylmethane, 3,3', Aromatic amine curing agent with two aromatic rings such as 5,5'-tetraethyl-4,4'-diaminodiphenylmethane; hydrolyzed condensate of aromatic amine curing agent; polytetramethylene oxide di-p-aminobenzoic acid Aromatic amine curing agents having a polyether structure such as esters and polytetramethylene oxide di-p-aminobenzoate; condensates of aromatic diamine and epichlorohydrin; reaction products of aromatic diamine and styrene; etc. Can be mentioned.
酸無水物系硬化剤としては、無水フタル酸、無水マレイン酸、メチルハイミック酸無水物、ハイミック酸無水物、無水コハク酸、テトラヒドロ無水フタル酸、ヘキサヒドロ無水フタル酸、クロレンド酸無水物、メチルテトラヒドロ無水フタル酸、３−メチルヘキサヒドロ無水フタル酸、４−メチルヘキサヒドロ無水フタル酸、トリアルキルテトラヒドロ無水フタル酸マレイン酸付加物、ベンゾフェノンテトラカルボン酸無水物、無水トリメリット酸、無水ピロメリット酸、水素化メチルナジック酸無水物、無水マレイン酸とジエン化合物からディールス・アルダー反応で得られ、複数のアルキル基を有するトリアルキルテトラヒドロ無水フタル酸、ドデセニル無水コハク酸等の各種環状酸無水物が挙げられる。 Examples of the acid anhydride-based curing agent include phthalic anhydride, maleic anhydride, methyl hymic acid anhydride, hymic acid anhydride, succinic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, chlorendic anhydride, and methyltetrahydro. Phthalic anhydride, 3-methylhexahydrophthalic anhydride, 4-methylhexahydrophthalic anhydride, trialkyltetrahydrophthalic anhydride maleic anhydride, benzophenone tetracarboxylic acid anhydride, trimellitic anhydride, pyromellitic anhydride, Examples thereof include various cyclic acid anhydrides such as trialkyltetrahydrohydride phthalic anhydride, dodecenyl anhydride succinic acid, which are obtained by the deal alder reaction from hydride methylnadic acid anhydride, maleic anhydride and diene compound, and have a plurality of alkyl groups. ..
フェノール系硬化剤としては、フェノール化合物（例えば、フェノール、クレゾール、キシレノール、レゾルシン、カテコール、ビスフェノールＡ及びビスフェノールＦ）並びにナフトール化合物（例えば、α−ナフトール、β−ナフトール及びジヒドロキシナフタレン）からなる群より選択される少なくとも１種と、アルデヒド化合物（例えば、ホルムアルデヒド、アセトアルデヒド、プロピオンアルデヒド、ベンズアルデヒド及びサリチルアルデヒド）とを、酸性触媒下で縮合又は共縮合させて得られるノボラック樹脂；フェノール・アラルキル樹脂；ビフェニル・アラルキル樹脂；ナフトール・アラルキル樹脂；等が挙げられる。 The phenolic curing agent is selected from the group consisting of phenol compounds (eg, phenol, cresol, xylenol, resorcin, catechol, bisphenol A and bisphenol F) and naphthol compounds (eg, α-naphthol, β-naphthol and dihydroxynaphthalene). Novolak resin obtained by condensing or co-condensing at least one of the above with an aldehyde compound (for example, formaldehyde, acetaldehyde, propionaldehyde, benzaldehyde and salicylaldehyde) under an acidic catalyst; phenol-aralkyl resin; biphenyl-aralkyl. Resin; naphthol-aralkyl resin; and the like.
硬化剤の官能基（例えば、アミン系硬化剤の場合にはアミノ基の活性水素、フェノール系硬化剤の場合にはフェノール性水酸基、酸無水物系硬化剤の場合には酸無水物基）の当量数とエポキシ樹脂の当量数との比（硬化剤の当量数／エポキシ樹脂の当量数）を、０．６〜１．４の範囲に設定することが好ましく、０．７〜１．３の範囲に設定することがより好ましく、０．８〜１．２の範囲に設定することがさらに好ましい。 Functional groups of curing agents (for example, active hydrogen of amino group in the case of amine-based curing agent, phenolic hydroxyl group in the case of phenol-based curing agent, acid anhydride group in the case of acid anhydride-based curing agent) The ratio of the equivalent number to the epoxy resin equivalent number (equivalent number of curing agent / epoxy resin equivalent number) is preferably set in the range of 0.6 to 1.4, preferably 0.7 to 1.3. It is more preferable to set it in the range, and it is further preferable to set it in the range of 0.8 to 1.2.
（硬化促進剤）
電磁波シールド用組成物が熱硬化性樹脂を含有する場合、電磁波シールド用組成物は熱硬化性樹脂の硬化反応又は熱硬化性樹脂と硬化剤との硬化反応を促進する硬化促進剤を含有してもよい。
硬化促進剤の種類は特に限定されるものではなく、熱硬化性樹脂及び硬化剤の種類に応じて適宜選択される。
(Curing accelerator)
When the composition for electromagnetic wave shielding contains a thermosetting resin, the composition for electromagnetic wave shielding contains a curing accelerator that accelerates the curing reaction of the thermosetting resin or the curing reaction between the thermosetting resin and the curing agent. May be good.
The type of the curing accelerator is not particularly limited, and is appropriately selected depending on the type of the thermosetting resin and the curing agent.
硬化促進剤としては、具体的には、１，８−ジアザ−ビシクロ［５．４．０］ウンデセン−７、１，５−ジアザ−ビシクロ［４．３．０］ノネン、５，６−ジブチルアミノ−１，８−ジアザ−ビシクロ［５．４．０］ウンデセン−７等のシクロアミジン化合物；シクロアミジン化合物に無水マレイン酸、１，４−ベンゾキノン、２，５−トルキノン、１，４−ナフトキノン、２，３−ジメチルベンゾキノン、２，６−ジメチルベンゾキノン、２，３−ジメトキシ−５−メチル−１，４−ベンゾキノン、２，３−ジメトキシ−１，４−ベンゾキノン、フェニル−１，４−ベンゾキノン等のキノン化合物、ジアゾフェニルメタン、フェノール樹脂などのπ結合をもつ化合物を付加してなる分子内分極を有する化合物；ベンジルジメチルアミン、トリエタノールアミン、ジメチルアミノエタノール、トリス（ジメチルアミノメチル）フェノール等の３級アミン化合物；３級アミン化合物の誘導体；イミダゾール、２−メチルイミダゾール、２−フェニルイミダゾール、２−フェニル−４−メチルイミダゾール等のイミダゾール化合物；イミダゾール化合物の誘導体；テトラフェニルホスホニウムテトラフェニルボレート、トリフェニルホスホニウムテトラフェニルボレート、２−エチル−４−メチルイミダゾリウムテトラフェニルボレート、Ｎ−メチルモルホリニウムテトラフェニルボレート等のテトラフェニルボレート塩；テトラフェニルボレート塩の誘導体；トリフェニルホスフィン−トリフェニルボラン錯体、モルホリン−トリフェニルボラン錯体等のトリフェニルボラン錯体；などが挙げられる。硬化促進剤は、１種類を単独で使用しても、２種類以上を併用してもよい。 Specific examples of the curing accelerator include 1,8-diaza-bicyclo [5.4.0] undecene-7, 1,5-diaza-bicyclo [4.3.0] nonene, and 5,6-dibutyl. Cycloamidine compounds such as amino-1,8-diaza-bicyclo [5.4.0] undecene-7; cycloamidin compounds include maleic anhydride, 1,4-benzoquinone, 2,5-turquinone, 1,4-naphthoquinone. , 2,3-Didimethylbenzoquinone, 2,6-dimethylbenzoquinone, 2,3-dimethoxy-5-methyl-1,4-benzoquinone, 2,3-dimethoxy-1,4-benzoquinone, phenyl-1,4-benzoquinone Kinone compounds such as, diazophenylmethane, compounds having intramolecular polarization formed by adding a compound having a π bond such as phenol resin; benzyldimethylamine, triethanolamine, dimethylaminoethanol, tris (dimethylaminomethyl) phenol, etc. Tertiary amine compounds; derivatives of tertiary amine compounds; imidazole compounds such as imidazole, 2-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole; derivatives of imidazole compounds; tetraphenylphosphonium tetraphenylborate, Tetraphenylborate salts such as triphenylphosphonium tetraphenylborate, 2-ethyl-4-methylimidazolium tetraphenylborate, N-methylmorpholinium tetraphenylborate; derivatives of tetraphenylborate salt; triphenylphosphine-triphenylboran Examples thereof include a complex, a triphenylboran complex such as a morpholin-triphenylboran complex; and the like. As the curing accelerator, one type may be used alone, or two or more types may be used in combination.
硬化促進剤の含有率は、熱硬化性樹脂及び必要に応じて用いられる硬化剤の合計量に対して、０．１質量％〜１５質量％であることが好ましい。 The content of the curing accelerator is preferably 0.1% by mass to 15% by mass with respect to the total amount of the thermosetting resin and the curing agent used if necessary.
（溶剤）
本開示の電磁波シールド用組成物は、水、有機溶剤等の溶剤を含有してもよい。樹脂を充分に溶解する観点から、溶剤は有機溶剤が好ましく、電磁波シールド用組成物を付与する工程での作業性及び電磁波シールド用組成物の乾燥を抑制する観点から、５０℃以上の沸点を有している有機溶剤であることが好ましく、乾燥又は硬化時のボイドの発生を抑制する観点から３００℃以下の沸点を有している有機溶剤であることが好ましい。
(solvent)
The electromagnetic wave shielding composition of the present disclosure may contain a solvent such as water or an organic solvent. From the viewpoint of sufficiently dissolving the resin, the solvent is preferably an organic solvent, and has a boiling point of 50 ° C. or higher from the viewpoint of workability in the step of applying the electromagnetic wave shielding composition and suppressing drying of the electromagnetic wave shielding composition. It is preferably an organic solvent that has a boiling point of 300 ° C. or lower from the viewpoint of suppressing the generation of voids during drying or curing.
有機溶剤の例としては、テルピネオール、ステアリルアルコール、トリプロピレングリコールメチルエーテル、ジエチレングリコール、ジエチレングリコールモノエチルエーテル（別名、エトキシエトキシエタノール）、ジエチレングリコールモノヘキシルエーテル（別名、ヘキシルカルビトール）、ジエチレングリコールモノメチルエーテル、ジプロピレングリコール−ｎ−プロピルエーテル、ジプロピレングリコール−ｎ−ブチルエーテル、トリプロピレングリコール−ｎ−ブチルエーテル、１，３−ブタンジオール、１，４−ブタンジオール、プロピレングリコールフェニルエーテル、２−（２−ブトキシエトキシ）エタノール等のアルコール類；酢酸ブチル、クエン酸トリブチル、４−メチル−１，３−ジオキソラン−２−オン、γ−ブチロラクトン、ジエチレングリコールモノエチルエーテルアセテート、ジプロピレングリコールメチルエーテルアセテート、ジエチレングリコールモノブチルエーテルアセテート、グリセリントリアセテート等のエステル類；アセトン、メチルエチルケトン、メチルイソブチルケトン、シクロヘキサノン、イソホロン等のケトン類；シクロヘキサン等のシクロアルカン類；Ｎ−メチル−２−ピロリドン等のラクタム；フェニルアセトニトリル等のニトリル類；などを挙げることができる。溶剤は、１種類を単独で使用しても、２種類以上を併用してもよい。 Examples of organic solvents include terpineol, stearyl alcohol, tripropylene glycol methyl ether, diethylene glycol, diethylene glycol monoethyl ether (also known as ethoxyethoxyethanol), diethylene glycol monohexyl ether (also known as hexyl carbitol), diethylene glycol monomethyl ether, and dipropylene. Glycol-n-propyl ether, dipropylene glycol-n-butyl ether, tripropylene glycol-n-butyl ether, 1,3-butanediol, 1,4-butanediol, propylene glycol phenyl ether, 2- (2-butoxyethoxy) Alcohols such as ethanol; butyl acetate, tributyl citrate, 4-methyl-1,3-dioxolan-2-one, γ-butyrolactone, diethylene glycol monoethyl ether acetate, dipropylene glycol methyl ether acetate, diethylene glycol monobutyl ether acetate, glycerin Ethers such as triacetate; ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, isophorone; cycloalkanes such as cyclohexane; lactams such as N-methyl-2-pyrrolidone; nitriles such as phenylacetate; etc. be able to. As the solvent, one type may be used alone, or two or more types may be used in combination.
電磁波シールド用組成物中の溶剤の割合は、電磁波シールド用組成物がスクリーン印刷法、スプレー塗布法等の付与方法に適した粘度となる量であることが好ましい。
電磁波シールド用組成物中の溶剤の割合は、例えば、０．１質量％〜８５質量％であることが好ましく、０．５質量％〜７５質量％であることがより好ましく、１質量％〜７０質量％であることがさらに好ましい。
The ratio of the solvent in the electromagnetic wave shielding composition is preferably an amount that makes the electromagnetic wave shielding composition have a viscosity suitable for an application method such as a screen printing method or a spray coating method.
The ratio of the solvent in the composition for electromagnetic wave shielding is, for example, preferably 0.1% by mass to 85% by mass, more preferably 0.5% by mass to 75% by mass, and 1% by mass to 70% by mass. It is more preferably mass%.
（その他の成分）
本開示の電磁波シールド用組成物は、上述した成分に加え、必要に応じて当該分野で通常用いられるその他の成分をさらに含むことができる。その他の成分としては、可塑剤、分散剤、界面活性剤、チキソ剤等が挙げられる。
(Other ingredients)
The composition for electromagnetic wave shielding of the present disclosure may further contain other components usually used in the art, if necessary, in addition to the above-mentioned components. Examples of other components include plasticizers, dispersants, surfactants, thixotropic agents and the like.
（電磁波シールド用組成物の製造方法）
本開示の電磁波シールド用組成物の製造方法は、特に限定されるものではない。電磁波シールド用組成物を構成する成分を混合し、さらに撹拌、溶解、分散等の処理をすることにより得ることができる。これらの混合、撹拌、分散等のための装置としては、特に限定されるものではなく、３本ロールミル、プラネタリーミキサ、遊星式ミキサ、自転公転型撹拌装置、らいかい機、二軸混練機、薄層せん断分散機等を使用することができる。また、これらの装置を適宜組み合わせて使用してもよい。上記処理の際、必要に応じて加熱してもよい。
処理後、ろ過により電磁波シールド用組成物の最大粒径を調整してもよい。ろ過は、ろ過装置を用いて行うことができる。ろ過用のフィルタとしては、例えば、金属メッシュ、メタルフィルター及びナイロンメッシュが挙げられる。
(Manufacturing method of composition for electromagnetic wave shield)
The method for producing the composition for electromagnetic wave shielding of the present disclosure is not particularly limited. It can be obtained by mixing the components constituting the electromagnetic wave shielding composition and further performing treatments such as stirring, dissolution, and dispersion. The device for mixing, stirring, dispersing, etc. of these is not particularly limited, and a three-roll mill, a planetary mixer, a planetary mixer, a rotating / revolving stirrer, a raft machine, a twin-screw kneader, etc. A thin layer shear disperser or the like can be used. Moreover, you may use these devices in combination as appropriate. During the above treatment, it may be heated if necessary.
After the treatment, the maximum particle size of the electromagnetic wave shielding composition may be adjusted by filtration. Filtration can be performed using a filtration device. Examples of the filter for filtration include a metal mesh, a metal filter and a nylon mesh.
＜電磁波シールド用シート＞
本開示の電磁波シールド用シートは、本開示の電磁波シールド用組成物を含む樹脂組成物層を有するものである。本開示の電磁波シールド用シートは、必要に応じて、離型フィルムをさらに含んで構成されてもよい。
<Electromagnetic wave shield sheet>
The electromagnetic wave shielding sheet of the present disclosure has a resin composition layer containing the electromagnetic wave shielding composition of the present disclosure. The electromagnetic wave shielding sheet of the present disclosure may be further composed of a release film, if necessary.
樹脂組成物層は、例えば、本開示の電磁波シールド用組成物に溶剤を添加して調製されるワニス状の電磁波シールド用組成物（以下、「樹脂ワニス」ともいう）をポリエチレンテレフタレートフィルム、ポリイミドフィルム等の離型フィルム上に付与し、乾燥することで製造することができる。 As the resin composition layer, for example, a varnish-like composition for electromagnetic wave shielding (hereinafter, also referred to as “resin varnish”) prepared by adding a solvent to the electromagnetic wave shielding composition of the present disclosure is used as a polyethylene terephthalate film or a polyimide film. It can be produced by applying it on a release film such as varnish and drying it.
樹脂ワニスの付与は公知の方法により実施することができる。具体的には、コンマコート、ダイコート、リップコート、グラビアコート等の方法、アプリケーターを用いた方法などが挙げられる。所定の厚みに樹脂組成物層を形成するための樹脂ワニスの付与方法としては、ギャップ間に被塗工物を通過させるコンマコート法、ノズルから流量を調節した樹脂ワニスを塗布するダイコート法等が挙げられる。乾燥前の樹脂組成物層の厚みが５０μｍ〜５００μｍの場合には、コンマコート法を用いることが好ましい。
樹脂ワニスを付与する際には、付与される樹脂ワニスに磁界を印加してもよい。樹脂ワニスに磁界を印加することで、樹脂組成物層中において、軟磁性体粒子の第２の粒子群に帰属される粒子が第１の粒子群に帰属される粒子間の空隙に効率的に移動し、当該隙間が埋められやすい。これによってより高い比透磁率を得ることができる傾向にある。
The application of the resin varnish can be carried out by a known method. Specific examples thereof include a method such as a comma coat, a die coat, a lip coat, and a gravure coat, and a method using an applicator. As a method of applying the resin varnish for forming the resin composition layer to a predetermined thickness, a comma coating method in which the object to be coated is passed between the gaps, a die coating method in which the resin varnish whose flow rate is adjusted from the nozzle is applied, and the like are used. Can be mentioned. When the thickness of the resin composition layer before drying is 50 μm to 500 μm, it is preferable to use the comma coating method.
When applying the resin varnish, a magnetic field may be applied to the applied resin varnish. By applying a magnetic field to the resin varnish, the particles belonging to the second particle group of the soft magnetic particles efficiently fill the voids between the particles belonging to the first particle group in the resin composition layer. It moves and the gap is easily filled. As a result, a higher relative magnetic permeability tends to be obtained.
乾燥方法は、樹脂ワニス中に含まれる有機溶剤の少なくとも一部を除去できれば特に制限されず、通常用いられる乾燥方法から適宜選択することができる。
乾燥方法は、常温（例えば、２５℃）放置による乾燥、加熱乾燥又は減圧乾燥を用いることができる。加熱乾燥又は減圧乾燥には、ホットプレート、温風乾燥機、温風加熱炉、窒素乾燥機、赤外線乾燥機、赤外線加熱炉、遠赤外線加熱炉、マイクロ波加熱装置、レーザー加熱装置、電磁加熱装置、ヒーター加熱装置、蒸気加熱炉等を用いることができる。
乾燥のための温度及び時間は、使用した溶剤の種類及び量に合わせて適宜調整することができ、例えば、４０℃〜１８０℃で、１分間〜１２０分間乾燥させることが好ましい。
The drying method is not particularly limited as long as at least a part of the organic solvent contained in the resin varnish can be removed, and can be appropriately selected from the commonly used drying methods.
As a drying method, drying by leaving at room temperature (for example, 25 ° C.), heat drying or vacuum drying can be used. For heat drying or vacuum drying, hot plate, warm air dryer, hot air heating furnace, nitrogen dryer, infrared dryer, infrared heating furnace, far infrared heating furnace, microwave heating device, laser heating device, electromagnetic heating device , A heater heating device, a steam heating furnace, etc. can be used.
The temperature and time for drying can be appropriately adjusted according to the type and amount of the solvent used, and for example, it is preferable to dry at 40 ° C. to 180 ° C. for 1 minute to 120 minutes.
樹脂組成物層の平均厚みは、３μｍ〜３００μｍが好ましく、５μｍ〜２００μｍがより好ましく、１０μｍ〜１００μｍがさらに好ましい。 The average thickness of the resin composition layer is preferably 3 μm to 300 μm, more preferably 5 μm to 200 μm, and even more preferably 10 μm to 100 μm.
＜電磁波シールド膜＞
本開示の電磁波シールド膜は、本開示の電磁波シールド用組成物により形成されたものである。本開示の電磁波シールド膜は、本開示の電磁波シールド用組成物を含む樹脂組成物層であってもよい。電磁波シールド用組成物が樹脂として熱硬化性樹脂を含有する場合、本開示の電磁波シールド膜は、本開示の電磁波シールド用組成物を含む樹脂組成物層の硬化物であってもよい。
電磁波シールド膜の平均厚みは、３μｍ〜３００μｍが好ましく、５μｍ〜２００μｍがより好ましく、１０μｍ〜１００μｍがさらに好ましい。
<Electromagnetic wave shield film>
The electromagnetic wave shielding film of the present disclosure is formed by the composition for electromagnetic wave shielding of the present disclosure. The electromagnetic wave shielding film of the present disclosure may be a resin composition layer containing the composition for electromagnetic wave shielding of the present disclosure. When the electromagnetic wave shielding composition contains a thermosetting resin as a resin, the electromagnetic wave shielding film of the present disclosure may be a cured product of a resin composition layer containing the electromagnetic wave shielding composition of the present disclosure.
The average thickness of the electromagnetic wave shielding film is preferably 3 μm to 300 μm, more preferably 5 μm to 200 μm, and even more preferably 10 μm to 100 μm.
本開示の電磁波シールド膜が本開示の電磁波シールド用組成物を含む樹脂組成物層である場合、被着体の電磁波シールド膜を形成したい箇所にワニス状の電磁波シールド用組成物を付与し、乾燥することで、電磁波シールド膜を形成することができる。また、被着体の電磁波シールド膜を形成したい箇所に本開示の電磁波シールド用シートを付着することで、電磁波シールド膜を形成することができる。
電磁波シールド用組成物が樹脂として熱硬化性樹脂を含有する場合、被着体の電磁波シールド膜を形成したい箇所にワニス状の電磁波シールド用組成物を付与し、乾燥し、加熱により熱硬化性樹脂を硬化することで、電磁波シールド膜を形成することができる。また、被着体の電磁波シールド膜を形成したい箇所に本開示の電磁波シールド用シートを付着し、加熱により熱硬化性樹脂を硬化することで、電磁波シールド膜を形成することができる。
When the electromagnetic wave shielding film of the present disclosure is a resin composition layer containing the electromagnetic wave shielding composition of the present disclosure, a varnish-like electromagnetic wave shielding composition is applied to a portion of the adherend where the electromagnetic wave shielding film is desired to be formed, and dried. By doing so, an electromagnetic wave shielding film can be formed. Further, the electromagnetic wave shielding film can be formed by adhering the electromagnetic wave shielding sheet of the present disclosure to a portion where the electromagnetic wave shielding film of the adherend is desired to be formed.
When the electromagnetic wave shielding composition contains a thermosetting resin as a resin, a varnish-like electromagnetic wave shielding composition is applied to a portion of the adherend where the electromagnetic wave shielding film is desired to be formed, dried, and heated to obtain a thermosetting resin. The electromagnetic wave shield film can be formed by curing the above. Further, the electromagnetic wave shielding film can be formed by attaching the electromagnetic wave shielding sheet of the present disclosure to a portion of the adherend where the electromagnetic wave shielding film is desired to be formed and curing the thermosetting resin by heating.
被着体にワニス状の電磁波シールド用組成物を付与する方法としては、スプレー塗布法、既述のコンマコート、ダイコート、リップコート、グラビアコート等の方法、アプリケーターを用いた方法などが挙げられる。
ワニス状の電磁波シールド用組成物を乾燥する方法としては、既述の常温（例えば、２５℃）放置による乾燥、加熱乾燥又は減圧乾燥を用いることができる。
電磁波シールド用組成物又は電磁波シールド用シートに含有される熱硬化性樹脂を硬化するには、加熱処理で行ってもよいし、加熱加圧処理で行ってもよい。
加熱処理には、ホットプレート、温風乾燥機、温風加熱炉、窒素乾燥機、赤外線乾燥機、赤外線加熱炉、遠赤外線加熱炉、マイクロ波加熱装置、レーザー加熱装置、電磁加熱装置、ヒーター加熱装置、蒸気加熱炉等を用いることができる。
また、加熱加圧処理には、熱板プレス装置等を用いてもよいし、加圧しながら上述の加熱処理を行ってもよい。
加熱温度は、熱硬化性樹脂の種類によるが、８０℃以上であることが好ましく、１００℃以上であることがより好ましく、１２０℃以上であることがさらに好ましい。当該加熱温度の上限は、特に制限されないが、例えば２００℃以下である。
加熱時間は、熱硬化性樹脂の種類によるが、５分間〜２時間であることが好ましく、１０分間〜９０分間であることがより好ましく、３０分間〜６０分間であることがさらに好ましい。
被着体としては、ケーブル、建築材、後述の電子部品装置等が挙げられる。
Examples of the method of applying the varnish-like electromagnetic wave shielding composition to the adherend include a spray coating method, a method such as the above-mentioned comma coating, die coating, lip coating, and gravure coating, and a method using an applicator.
As a method for drying the varnish-like composition for electromagnetic wave shielding, the above-mentioned drying by leaving at room temperature (for example, 25 ° C.), heat drying or vacuum drying can be used.
The thermosetting resin contained in the electromagnetic wave shielding composition or the electromagnetic wave shielding sheet may be cured by heat treatment or heat and pressure treatment.
For heat treatment, hot plate, hot air dryer, hot air heating furnace, nitrogen dryer, infrared dryer, infrared heating furnace, far infrared heating furnace, microwave heating device, laser heating device, electromagnetic heating device, heater heating An apparatus, a steam heating furnace, or the like can be used.
Further, the heat plate pressing device or the like may be used for the heat and pressurization treatment, or the above-mentioned heat treatment may be performed while pressurizing.
The heating temperature depends on the type of the thermosetting resin, but is preferably 80 ° C. or higher, more preferably 100 ° C. or higher, and even more preferably 120 ° C. or higher. The upper limit of the heating temperature is not particularly limited, but is, for example, 200 ° C. or lower.
The heating time depends on the type of the thermosetting resin, but is preferably 5 minutes to 2 hours, more preferably 10 minutes to 90 minutes, and even more preferably 30 minutes to 60 minutes.
Examples of the adherend include cables, building materials, electronic component devices described later, and the like.
＜電子部品装置＞
本開示の電子部品装置は、本開示の電磁波シールド膜により覆われた領域を有するものである。
電子部品装置としては、リードフレーム、配線済みのテープキャリア、配線板、ガラス、シリコンウエハー等の支持部材に、半導体チップ、トランジスタ、ダイオード、サイリスタ等の能動素子、コンデンサ、抵抗体、抵抗アレイ、コイル、スイッチ等の受動素子などの電子部品を搭載したものが挙げられる。
電子部品及び支持部材のうちの、電磁波を発生する箇所又は電磁波の影響を受けやすい箇所を本開示の電磁波シールド膜で覆うことにより、本開示の電子部品装置を得ることができる。
電子部品又は支持部材を電磁波シールド膜で覆う方法としては、ワニス状の電磁波シールド用組成物を電磁波シールド膜で覆いたい箇所に付与し、乾燥し、必要に応じて加熱する方法が挙げられる。付与方法としては、スクリーン印刷法、スプレー塗布法等が挙げられる。ワニス状の電磁波シールド用組成物を付与する際、樹脂ワニスに磁界を印加してもよい。
乾燥条件及び乾燥方法は、既述の電磁波シールド用シートを製造する際の条件及び方法と同様である。また、加熱条件及び加熱方法は、既述の加熱により熱硬化性樹脂を硬化する際の条件及び方法と同様である。
また、電子部品又は支持部材を電磁波シールド膜で覆う方法としては、本開示の電磁波シールド用シートを電磁波シールド膜で覆いたい箇所に配置し、必要に応じて加熱する方法も挙げられる。電磁波シールド用シートの加熱条件及び加熱方法は、既述の加熱により熱硬化性樹脂を硬化する際の条件及び方法と同様である。
<Electronic component equipment>
The electronic component device of the present disclosure has a region covered by the electromagnetic wave shielding film of the present disclosure.
Electronic component devices include lead frames, pre-wired tape carriers, wiring boards, glass, support members such as silicon wafers, active elements such as semiconductor chips, transistors, diodes, and thyristors, capacitors, resistors, resistor arrays, and coils. , Those equipped with electronic components such as passive elements such as switches.
The electronic component device of the present disclosure can be obtained by covering a portion of the electronic component and the support member that generates an electromagnetic wave or a portion that is easily affected by the electromagnetic wave with the electromagnetic wave shield film of the present disclosure.
Examples of the method of covering the electronic component or the support member with the electromagnetic wave shielding film include a method of applying a varnish-like electromagnetic wave shielding composition to a portion to be covered with the electromagnetic wave shielding film, drying the electronic component or supporting member, and heating the electronic component or the supporting member as necessary. Examples of the application method include a screen printing method and a spray coating method. When applying the varnish-like electromagnetic wave shielding composition, a magnetic field may be applied to the resin varnish.
The drying conditions and drying method are the same as the conditions and methods for producing the electromagnetic wave shielding sheet described above. The heating conditions and heating method are the same as the conditions and methods for curing the thermosetting resin by heating as described above.
Further, as a method of covering the electronic component or the support member with the electromagnetic wave shielding film, there is also a method of arranging the electromagnetic wave shielding sheet of the present disclosure at a place to be covered with the electromagnetic wave shielding film and heating as necessary. The heating conditions and heating method of the electromagnetic wave shielding sheet are the same as the conditions and methods for curing the thermosetting resin by heating as described above.
本開示の電子部品装置は、支持部材と、支持部材上に配置される電子部品と、電子部品を封止する封止材の硬化物と、封止材の硬化物の表面に配置される本開示の電磁波シールド膜とを備えるものであってもよい。封止材の硬化物の表面に電磁波シールド膜を配置する場合、封止材を硬化した後に電磁波シールド膜を封止材の硬化物の表面に形成してもよいし、硬化する前の封止材の表面に電磁波シールド用組成物又は電磁波シールド用シートを配置してもよい。 The electronic component device of the present disclosure includes a support member, an electronic component arranged on the support member, a cured product of a sealing material for sealing the electronic component, and a book arranged on the surface of the cured product of the sealing material. It may be provided with the disclosed electromagnetic wave shielding film. When the electromagnetic wave shield film is arranged on the surface of the cured product of the sealing material, the electromagnetic wave shielding film may be formed on the surface of the cured product of the sealing material after the sealing material is cured, or the sealing before curing. An electromagnetic wave shielding composition or an electromagnetic wave shielding sheet may be arranged on the surface of the material.
電子部品装置は、電子部品及び支持部材を収容する筐体をさらに備えてもよい。電子部品及び支持部材が筐体内に収容される場合、筐体の内表面及び外表面の少なくとも一方を本開示の電磁波シールド膜で覆うことにより、本開示の電子部品装置を得ることができる。
筐体の内表面又は外表面を電磁波シールド膜で覆う方法は、電子部品又は支持部材を電磁波シールド膜で覆う方法と同様である。
The electronic component device may further include a housing that houses the electronic component and the support member. When the electronic component and the support member are housed in the housing, the electronic component device of the present disclosure can be obtained by covering at least one of the inner surface and the outer surface of the housing with the electromagnetic wave shielding film of the present disclosure.
The method of covering the inner surface or the outer surface of the housing with the electromagnetic wave shield film is the same as the method of covering the electronic component or the support member with the electromagnetic wave shield film.
以下、実施例により本開示をさらに具体的に説明するが、本開示は以下の実施例に限定されるものではない。 Hereinafter, the present disclosure will be described in more detail with reference to Examples, but the present disclosure is not limited to the following Examples.
［実施例］
軟磁性体扁平粒子としてＦｅ−Ｓｉ−Ａｌ合金（センダスト粉末、山陽特殊製鋼株式会社、平均粒子径４５μｍ、アスペクト比４５）を３２質量部、軟磁性体微粒子としてＦｅ３Ｏ４（戸田工業株式会社、平均粒子径０．１７μｍ）を６質量部、樹脂としてエポキシ樹脂を３７質量部、硬化促進剤としてイミダゾール化合物を２質量部、溶剤として酢酸ブチルを２３質量部混合し樹脂ワニス１を作製した。
樹脂ワニス１に含まれる軟磁性体粒子の粒度分布は、４５μｍ及び０．２μｍに２つのピークを有していた。また、５０μｍのピークに帰属する軟磁性体粒子についての平均アスペクト比は、５０であった。
樹脂ワニス１をギャップ２００μｍに設定したアプリケーターでポリイミドフィルム上に塗工し塗膜を作製した。その後、５０℃で１時間乾燥し、１５０℃で１時間硬化させて実施例の試験片を得た。
[Example]
32 parts by mass of Fe-Si-Al alloy (Sendust powder, Sanyo Special Steel Co., Ltd., average particle diameter 45 μm, aspect ratio 45) as soft magnetic flat particles, Fe 3 O 4 (Toda Kogyo Co., Ltd.) as soft magnetic fine particles A
The particle size distribution of the soft magnetic particles contained in the
The
［比較例］
軟磁性体扁平粉末としてＦｅ−Ｓｉ−Ａｌ合金（センダスト粉末、山陽特殊製鋼株式会社、平均粒子径４５μｍ、アスペクト比４５）を３２質量部、樹脂としてエポキシ樹脂を３７質量部、硬化促進剤としてイミダゾール化合物を２質量部、溶剤として酢酸ブチルを２９質量部混合し樹脂ワニス２を作製した。
樹脂ワニス２に含まれる軟磁性体粒子の粒度分布は、４５μｍに１つのピークを有していた。
樹脂ワニス２をギャップ２００μｍに設定したアプリケーターでポリイミドフィルム上に塗工し塗膜を作製した。その後、５０℃で１時間乾燥し、１５０℃で１時間硬化させて比較例の試験片を得た。
[Comparison example]
32 parts by mass of Fe-Si-Al alloy (Sendust powder, Sanyo Special Steel Co., Ltd., average particle diameter 45 μm, aspect ratio 45) as a soft magnetic flat powder, 37 parts by mass of epoxy resin as a resin, and imidazole as a curing accelerator. Resin varnish 2 was prepared by mixing 2 parts by mass of the compound and 29 parts by mass of butyl acetate as a solvent.
The particle size distribution of the soft magnetic particles contained in the resin varnish 2 had one peak at 45 μm.
The resin varnish 2 was applied onto the polyimide film with an applicator having a gap of 200 μm to prepare a coating film. Then, it was dried at 50 degreeC for 1 hour and cured at 150 degreeC for 1 hour to obtain the test piece of the comparative example.
＜評価＞
得られた試験片の比透磁率を測定した。比透磁率の測定には、キーサイト・テクノロジー社製のＥ４９９１Ａを用いた。
図１に実施例及び比較例で作製した試験片の比透磁率の測定結果を示す。軟磁性体扁平粒子と磁性体微粒子とを混合した実施例の方が比較例に比較して高い比透磁率が得られた。
<Evaluation>
The relative magnetic permeability of the obtained test piece was measured. E4991A manufactured by Keysight Technology Co., Ltd. was used for measuring the relative magnetic permeability.
FIG. 1 shows the measurement results of the relative magnetic permeability of the test pieces prepared in Examples and Comparative Examples. A higher relative magnetic permeability was obtained in the example in which the soft magnetic flat particles and the magnetic fine particles were mixed as compared with the comparative example.
以上のように、軟磁性体を原料とした電磁波シールド用組成物を作製するときに、軟磁性体扁平粒子と軟磁性体微粒子を混合して軟磁性体粒子の粒度分布が少なくとも２つのピークを有するようにすることで、電磁波シールド膜の比透磁率を高くすることができることがわかる。 As described above, when the composition for electromagnetic wave shielding using the soft magnetic material as a raw material is produced, the soft magnetic material flat particles and the soft magnetic material fine particles are mixed to obtain at least two peaks in the particle size distribution of the soft magnetic material particles. It can be seen that the relative magnetic permeability of the electromagnetic wave shielding film can be increased by having the electromagnetic wave shielding film.
Claims (9)
前記軟磁性体粒子の粒度分布が、少なくとも２つのピークを有する電磁波シールド用組成物。 Contains soft magnetic particles and resin,
An electromagnetic wave shielding composition in which the particle size distribution of the soft magnetic particles has at least two peaks.
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| JP2004349585A (en) * | 2003-05-23 | 2004-12-09 | Hitachi Metals Ltd | Method of manufacturing dust core and nanocrystalline magnetic powder |
| JP2005347449A (en) * | 2004-06-02 | 2005-12-15 | Denki Kagaku Kogyo Kk | Soft magnetic powder and application thereof |
| JP2010114407A (en) * | 2008-10-10 | 2010-05-20 | Dowa Electronics Materials Co Ltd | Mixed ferrite powder, method for manufacturing the same, and radio-wave absorber |
| JP2014013803A (en) * | 2012-07-04 | 2014-01-23 | Taiyo Yuden Co Ltd | Inductor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004349585A (en) * | 2003-05-23 | 2004-12-09 | Hitachi Metals Ltd | Method of manufacturing dust core and nanocrystalline magnetic powder |
| JP2005347449A (en) * | 2004-06-02 | 2005-12-15 | Denki Kagaku Kogyo Kk | Soft magnetic powder and application thereof |
| JP2010114407A (en) * | 2008-10-10 | 2010-05-20 | Dowa Electronics Materials Co Ltd | Mixed ferrite powder, method for manufacturing the same, and radio-wave absorber |
| JP2014013803A (en) * | 2012-07-04 | 2014-01-23 | Taiyo Yuden Co Ltd | Inductor |
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