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JP4936233B2 - Flat Fe-based alloy powder for magnetic shield - Google Patents
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JP4936233B2 - Flat Fe-based alloy powder for magnetic shield - Google Patents

Flat Fe-based alloy powder for magnetic shield Download PDF

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JP4936233B2
JP4936233B2 JP2008261356A JP2008261356A JP4936233B2 JP 4936233 B2 JP4936233 B2 JP 4936233B2 JP 2008261356 A JP2008261356 A JP 2008261356A JP 2008261356 A JP2008261356 A JP 2008261356A JP 4936233 B2 JP4936233 B2 JP 4936233B2
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based alloy
flat
alloy powder
particle size
powder
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JP2009074176A (en
Inventor
修司 飛田
和則 五十嵐
耕一郎 森本
銀矢 石黒
康明 吉岡
和美 泉谷
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Dai Nippon Printing Co Ltd
Mitsubishi Materials Corp
NTT Inc
NTT Inc USA
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Dai Nippon Printing Co Ltd
Mitsubishi Materials Corp
Nippon Telegraph and Telephone Corp
NTT Inc USA
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Description

この発明は、各種の磁気記録装置や電子機器などを磁場や電磁波の悪影響から保護するための磁気シールド層や磁気シールドシートなどの形成に用いられる偏平状Fe基合金粉末に関するものである。   The present invention relates to a flat Fe-based alloy powder used for forming a magnetic shield layer, a magnetic shield sheet, and the like for protecting various magnetic recording devices and electronic devices from the adverse effects of magnetic fields and electromagnetic waves.

従来、磁気シールド用偏平状Fe基合金粉末として、例えば特開平3−295206号公報に記載されるように、原子%で(以下、%は原子%を示す)、
SiおよびAlの内の1種または2種:18〜30%、
Cr:19%以下(0を含まず)、
を含有し、残りがFeと不可避不純物からなる組成を有し、かつX線回折で体心立方型結晶構造を示すものが知られている。また、上記従来の磁気シールド用偏平状Fe基合金粉末は、その他多くのものが、実用に際して、
平均厚さ(以下、「d」で示す):0.02〜0.6μm、
粒度分布計によって求められた粒径の小さい方から重量を累計して50%になったときの粒径(以下、「D50」で示す):3〜60μm、
アスペクト比(D50/d):20〜500、
の粒度に調整されて使用されることも良く知られるところである。
Conventionally, as a flat Fe-based alloy powder for a magnetic shield, for example, as described in JP-A-3-295206, in atomic% (hereinafter,% indicates atomic%),
One or two of Si and Al: 18-30%,
Cr: 19% or less (excluding 0),
In which the balance is composed of Fe and inevitable impurities, and shows a body-centered cubic crystal structure by X-ray diffraction. In addition, the above-mentioned conventional flat Fe-based alloy powders for magnetic shields,
Average thickness (hereinafter referred to as “d”): 0.02 to 0.6 μm,
Particle size when the weight is accumulated from the smaller particle size determined by the particle size distribution meter to 50% (hereinafter referred to as “D 50 ”): 3 to 60 μm,
Aspect ratio (D 50 / d): 20 to 500
It is also well known that the particle size is adjusted to be used.

一方、近年の磁気記録装置や電子機器の多機能化、小型化および高出力化と共にコストダウンに対する要求が激しく、これに伴ない、磁気シールド性能の一段の向上、並びに磁気シールド層および磁気シールドシートなどの一層の薄肉化のため、より高い飽和磁化およびより低い保磁力を示す磁気シールド用粉末を一層低価格で提供するように求められている。   On the other hand, there is a strong demand for cost reduction along with multifunction, miniaturization and high output of recent magnetic recording devices and electronic devices. Accordingly, magnetic shield performance and magnetic shield layer and magnetic shield sheet are further improved. Therefore, it is required to provide a magnetic shielding powder exhibiting higher saturation magnetization and lower coercive force at a lower price.

そこで、本発明者等は、上述のような観点から、上記従来の磁気シールド用偏平状Fe基合金粉末よりも一層高い飽和磁化および一層低い保磁力を示す磁気シールド用粉末を一層低価格で提供すべく研究を行なった結果、
(a)前記従来の磁気シールド用偏平状Fe基合金粉末において、さらにNi:0.1〜30%を含有せしめると、飽和磁化が一層向上すると同時に保磁力が低下し、磁気シールド用粉末として優れた磁気シールド性能を示す、
(b)一般に従来の磁気シールド用偏平状Fe基合金粉末は保磁力を低減させるために偏平化処理後熱処理が施されるが、従来の磁気シールド用偏平状Fe基合金粉末にさらにNi:0.1〜30%を添加すると偏平化処理後に熱処理を施さなくても従来以上の低保磁力を実現でき、熱処理工程の省略によるコストダウンを行うことができる、
(c)前記Ni:0.1〜30%を含有した磁気シールド用偏平状Fe基合金粉末は、熱処理無しでも従来以上の低保磁力を実現できるが、偏平化処理後の熱処理を行うと、保磁力が一層低減し、飽和磁化が一層向上する、
(d)このNi:0.1〜30%を含む磁気シールド用粉末の粒度は、従来と同じd:0.02〜0.6μm、D50:3〜60μm、D50/d:20〜500の範囲に調整すればよい、などの研究結果を得たのである。
In view of the above, the inventors of the present invention provide magnetic shield powder that exhibits higher saturation magnetization and lower coercivity than the conventional flat Fe-based alloy powder for magnetic shield, at a lower price. As a result of research,
(A) In the above-described conventional flat Fe-based alloy powder for magnetic shielding, when Ni: 0.1 to 30% is further added, the saturation magnetization is further improved and the coercive force is lowered, and it is excellent as a magnetic shielding powder. Show magnetic shielding performance,
(B) In general, the conventional flat Fe-based alloy powder for magnetic shield is subjected to a heat treatment after flattening treatment in order to reduce the coercive force. .1-30% can be added to achieve a lower coercive force than before without performing a heat treatment after the flattening treatment, and the cost can be reduced by omitting the heat treatment step.
(C) The flat Fe-based alloy powder for magnetic shield containing Ni: 0.1 to 30% can achieve a lower coercive force than before even without heat treatment, but when heat treatment after flattening treatment is performed, The coercive force is further reduced and the saturation magnetization is further improved.
(D) The particle size of the magnetic shielding powder containing Ni: 0.1 to 30% is the same as that of the conventional d: 0.02 to 0.6 μm, D 50 : 3 to 60 μm, D 50 / d: 20 to 500 The research results were obtained, such as adjusting to the range of.

この発明は、上記の研究結果にもとづいてなされたものであって、
(1)Al:15〜35%、Ni:0.1〜30%、Cr:0.1〜6%を含有し、残りがFeと不可避不純物からなる組成を有する磁気シールド用偏平状Fe基合金粉末、
(2)Al:15〜35%、Ni:0.1〜30%、Cr:0.1〜6%を含有し、残りがFeと不可避不純物からなる組成、並びにd:0.02〜0.6μm、D50:3〜60μm、D50/d:20〜500の範囲に調整された粒度を有する磁気シールド用偏平状Fe基合金粉末、に特徴を有するものである。
This invention was made based on the above research results,
(1) A flat Fe-based alloy for a magnetic shield having a composition containing Al: 15 to 35%, Ni: 0.1 to 30%, Cr: 0.1 to 6%, and the remainder consisting of Fe and inevitable impurities Powder,
(2) Al: 15 to 35%, Ni: 0.1 to 30%, Cr: 0.1 to 6%, with the remainder consisting of Fe and inevitable impurities, and d: 0.02 to 0. It is characterized by a flat Fe-based alloy powder for magnetic shielding having a particle size adjusted to 6 μm, D 50 : 3 to 60 μm, and D 50 / d: 20 to 500 .

この発明の磁気シールド用偏平状Fe基合金粉末は、Al:15〜35%、Ni:0.1〜30%、Cr:0.1〜6%を含有し、残りがFeと不可避不純物からなる組成を有するFe基合金溶湯を水アトマイズ法により粉末化し、得られた粉末に対して、通常の条件で分級、偏平化を行い、必要に応じて熱処理を施しさらに分級を施す。すなわち前記水アトマイズ粉末を分級により50μm以下の粒径とし、これをアトライタで偏平化した後、必要に応じてAr雰囲気中、350〜750℃の温度に所定時間保持の熱処理を施し、引続いて分級を行なって、
d:0.02〜0.6μm、
50:3〜60μm、
50/d:20〜500、
に粒度調整することにより製造することができる。
The flat Fe-based alloy powder for magnetic shield of the present invention contains Al: 15 to 35%, Ni: 0.1 to 30%, Cr: 0.1 to 6%, and the remainder is composed of Fe and inevitable impurities. The molten Fe-based alloy having a composition is pulverized by a water atomization method, and the obtained powder is classified and flattened under normal conditions, and subjected to heat treatment as necessary, and further classified. That is, the particle size of the water atomized powder is reduced to 50 μm or less by classification, and after flattening with an attritor, a heat treatment is performed at a temperature of 350 to 750 ° C. for a predetermined time in an Ar atmosphere as necessary. Perform classification,
d: 0.02 to 0.6 μm,
D 50 : 3 to 60 μm,
D 50 / d: 20~500,
It can be manufactured by adjusting the particle size.

つぎに、この発明の偏平状Fe基合金粉末の組成を上記の通りに限定した理由を説明する。
(a) Al
Alには、偏平化時に保磁力を増大させない作用があるが、その含有量が15%未満では所望の低い保磁力が得られないため、すぐれた磁気シールド性能を確保することができない。一方、その含有量が35%を越えると飽和磁化が急激に低下する。従って、この発明の偏平状Fe基合金粉末に含まれるSiを15〜35%(望ましくは20〜30%)含有するように定めた。
Next, the reason why the composition of the flat Fe-based alloy powder of the present invention is limited as described above will be described.
(A) Al
Al does not increase the coercive force during flattening, but if the content is less than 15%, a desired low coercive force cannot be obtained, so that excellent magnetic shielding performance cannot be ensured. On the other hand, when the content exceeds 35%, the saturation magnetization rapidly decreases. Therefore, it is determined to contain 15 to 35% (desirably 20 to 30%) of Si contained in the flat Fe-based alloy powder of the present invention.

(b) Ni
Niには、耐食性を向上させ、もって錆や変色の発生を防止する作用があり、加えてFeと同様に強磁性があるためにFeと置換しても大きく飽和磁化を低下させず、さらに偏平化時に保磁力を増大させない作用があるが、その含有量が0.1%未満では所望の低い保磁力を確保することができず、一方、その含有量が30%を越えると飽和磁化が低下し、所望の高い飽和磁化を得ることが難しくなる。従って、この発明の偏平状Fe基合金粉末に含まれるNi含有量は0.1〜30%(一層望ましくは0.4〜20%)と定めた。
(B) Ni
Ni has the effect of improving corrosion resistance and thus preventing the occurrence of rust and discoloration. In addition, since it has ferromagnetism like Fe, even if it is replaced with Fe, the saturation magnetization is not greatly reduced, and further flattening is achieved. Although the coercive force is not increased at the time of formation, if the content is less than 0.1%, the desired low coercive force cannot be secured, while if the content exceeds 30%, the saturation magnetization decreases. In addition, it becomes difficult to obtain a desired high saturation magnetization. Therefore, the Ni content contained in the flat Fe-based alloy powder of the present invention is determined to be 0.1 to 30% (more desirably 0.4 to 20%).

(c) Cr
Crは、Niと共存させることにより耐食性を一層向上させ、もって錆や変色の発生を防止する作用があるが、その含有量が0.1%未満では通常の所望のすぐれた耐食性および低い保磁力を確保することができず、一方、その含有量が6%を越えると飽和磁化が低下し、磁気シールド性能の低下が避けられなくなる。従って、この発明の偏平状Fe基合金粉末に含まれるCr含有量は0.1〜6%(一層望ましくは1〜5%)と定めた。
(C) Cr
Cr has the effect of further improving the corrosion resistance by coexisting with Ni and thus preventing the occurrence of rust and discoloration. However, if its content is less than 0.1%, it usually has excellent desired corrosion resistance and low coercive force. On the other hand, if the content exceeds 6%, the saturation magnetization is lowered, and the magnetic shield performance is inevitably lowered. Therefore, the Cr content contained in the flat Fe-based alloy powder of the present invention is determined to be 0.1 to 6% (more desirably 1 to 5%).

(d) 粒度
この発明の偏平状Fe基合金粉末は、従来と同じd:0.02〜0.6μm、D50:3〜60μm、D50/d:20〜500の範囲に調整すればよいが、d:0.05〜0.3μm、D50:5〜20μm、D50/d:50〜300の範囲に調整することが一層好ましい。
(D) Particle size The flat Fe-based alloy powder of this invention may be adjusted to the same ranges as d: 0.02 to 0.6 μm, D 50 : 3 to 60 μm, and D 50 / d: 20 to 500. but, d: 0.05~0.3μm, D 50: 5~20μm, D 50 / d: it is more preferably adjusted to a range of 50 to 300.

上述のように、この発明の偏平状Fe基合金粉末は、熱処理しなくても保磁力が低く、高い飽和磁化を示すので、熱処理工程を省略することによる製造コストを削減することができ、また、特にすぐれた磁気シールド性能を必要とする場合のみ、熱処理した偏平状Fe基合金粉末を使用すればよく、低価格化と共に磁気シールド性能の一層の向上に寄与するばかりでなく、磁気シールド層や磁気シールドシートなどの薄肉化を可能にするなど電子産業の発展に大いに貢献し得るものである。   As described above, the flat Fe-based alloy powder of the present invention has a low coercive force even without heat treatment and exhibits high saturation magnetization, so that the manufacturing cost can be reduced by omitting the heat treatment step. The heat-treated flat Fe-based alloy powder may be used only when particularly excellent magnetic shielding performance is required, which not only contributes to lowering the price but also improving the magnetic shielding performance. It can contribute greatly to the development of the electronics industry, such as enabling thinning of magnetic shield sheets.

つぎに、この発明の偏平状Fe基合金粉末を実施例により具体的に説明する。
実施例1
原料として、Fe−Al合金、Fe−Cr合金、溶解用ニッケル、および電解鉄を用意し、これら原料を高周波誘導炉にてそれぞれ表1に示される成分組成をもったFe基合金溶湯を調製し、この溶湯を水アトマイズ法により粉末化し、分級して40μm以下の粒径を有する粉末とし、ついでこれをアトライタで偏平化した後、ただちに分級を行なって同じく表1に示される粒度に調整することにより本発明偏平状Fe基合金粉末(以下、本発明粉末という)1〜6を製造した。
この結果得られた本発明粉末1〜6の保磁力および飽和磁化を測定し、この測定結果を表1に示した。
従来例1
原料として、Fe−Al合金、Fe−Cr合金および電解鉄を用意し、これら原料を高周波誘導炉にてそれぞれ表1に示される成分組成をもったFe基合金溶湯を調製し、この溶湯を水アトマイズ法により粉末化し、分級して40μm以下の粒径を有する粉末とし、ついでこれをアトライタで偏平化した後、Ar雰囲気中、350〜750℃の範囲内の所定温度に2時間保持の熱処理を施し、さらに分級を行なって同じく表1に示される粒度に調整することにより従来偏平状Fe基合金粉末(以下、従来粉末という)1を製造した。
Next, the flat Fe-based alloy powder of the present invention will be specifically described with reference to examples.
Example 1
Prepare Fe-Al alloy, Fe-Cr alloy, melting nickel, and electrolytic iron as raw materials, and prepare Fe-based alloy melts having the component compositions shown in Table 1 in the high frequency induction furnace. The molten metal is pulverized by the water atomization method, classified into a powder having a particle size of 40 μm or less, then flattened with an attritor, and immediately classified to adjust the particle size as shown in Table 1. Thus, the flat Fe-based alloy powders of the present invention (hereinafter referred to as the present powder) 1 to 6 were produced.
The coercive force and saturation magnetization of the obtained powders 1 to 6 of the present invention were measured, and the measurement results are shown in Table 1.
Conventional Example 1
Fe-Al alloy, Fe-Cr alloy and electrolytic iron are prepared as raw materials, and Fe-based alloy melts having the component compositions shown in Table 1 are prepared from these raw materials in a high-frequency induction furnace, respectively. Powdered by the atomizing method, classified to a powder having a particle size of 40 μm or less, then flattened with an attritor, and then heat treated for 2 hours at a predetermined temperature in the range of 350 to 750 ° C. in an Ar atmosphere. Then, classification was performed and the particle size shown in Table 1 was adjusted to produce a conventional flat Fe-based alloy powder (hereinafter referred to as conventional powder) 1.

実施例1で得られた本発明粉末1〜6および従来例1で得られた従来粉末1の保磁力および飽和磁化を測定し、この測定結果を表1に示した。   The coercive force and saturation magnetization of the inventive powders 1 to 6 obtained in Example 1 and the conventional powder 1 obtained in Conventional Example 1 were measured, and the measurement results are shown in Table 1.

Figure 0004936233
Figure 0004936233

表1に示される結果から、NiおよびCrを共に含有する熱処理無しの本発明粉末1〜6は、Crのみを含有する熱処理を施した従来粉末1に比して、保磁力が低く、一段と高い飽和磁化を示すことが明らかである。   From the results shown in Table 1, the inventive powders 1 to 6 containing both Ni and Cr without heat treatment have lower coercive force and higher than the conventional powder 1 subjected to heat treatment containing only Cr. It is clear that it exhibits saturation magnetization.

実施例2
実施例1で作製した本発明粉末1〜6と同じ成分組成をもったFe基合金溶湯を調製し、アトマイズ法により粉末化し、分級して40μm以下の粒径を有する粉末とし、ついでこれをアトライタで偏平化した後、Ar雰囲気中、350〜750℃の範囲内の所定温度に2時間保持の条件の熱処理を施し、さらに分級を行なって本発明粉末1〜6と同じ表2に示される粒度に調整することにより本発明粉末7〜12を製造し、得られた本発明粉末7〜12の保磁力および飽和磁化を測定し、この測定結果を表2に示した。
Example 2
An Fe-based alloy molten metal having the same composition as the powders 1 to 6 of the present invention prepared in Example 1 was prepared, pulverized by the atomizing method, and classified into a powder having a particle size of 40 μm or less. After flattening, the heat treatment was carried out at a predetermined temperature in the range of 350 to 750 ° C. in an Ar atmosphere for 2 hours, followed by classification, and the particle size shown in Table 2 which is the same as that of the present powders 1 to 6 The powders 7 to 12 of the present invention were produced by adjusting the coercive force and the coercive force and saturation magnetization of the obtained powders 7 to 12 of the present invention were measured. The measurement results are shown in Table 2.

Figure 0004936233
Figure 0004936233

表2に示される結果から、偏平化したのち熱処理して得られた本発明粉末7〜12は、同じ成分組成の熱処理しない本発明粉末1〜6に比べて保磁力が一層低く、飽和磁化が一層向上していることが分かる。   From the results shown in Table 2, the inventive powders 7 to 12 obtained by heat treatment after flattening have lower coercive force and saturation magnetization than the inventive powders 1 to 6 of the same component composition that are not heat-treated. It turns out that it is improving further.

Claims (2)

原子%で、
Al:15〜35%、
Ni:0.1〜30%、
Cr:0.1〜6%、
を含有し、残りがFeと不可避不純物からなる組成を有することを特徴とする磁気シールド用偏平状Fe基合金粉末。
Atomic%
Al: 15-35%
Ni: 0.1 to 30%,
Cr: 0.1 to 6%,
A flat Fe-based alloy powder for magnetic shielding, characterized in that it has a composition comprising Fe and inevitable impurities.
原子%で、
Al:15〜35%、
Ni:0.1〜30%、
Cr:0.1〜6%、
を含有し、残りがFeと不可避不純物からなる組成、並びに、
平均厚さd:0.02〜0.6μm、
粒度分布計によって求められた粒径の小さい方から重量を累計して50%になったときの粒径D50:3〜60μm、
アスペクト比(D50/d):20〜500、
に調整された粒度を有することを特徴とする磁気シールド用偏平状Fe基合金粉末。
Atomic%
Al: 15-35%
Ni: 0.1 to 30%,
Cr: 0.1 to 6%,
And the balance of Fe and inevitable impurities, and
Average thickness d: 0.02 to 0.6 μm,
Particle size D 50 when the weight is accumulated from the smaller particle size determined by the particle size distribution meter to 50%: 3 to 60 μm,
Aspect ratio (D 50 / d): 20 to 500
A flat Fe-based alloy powder for magnetic shielding, characterized by having a grain size adjusted to
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JPS63285912A (en) * 1987-05-18 1988-11-22 Riken Corp Soft magnetic powder
JP2523388B2 (en) * 1990-04-12 1996-08-07 ティーディーケイ株式会社 Method for producing soft magnetic powder for magnetic shield and magnetic shield material
JP3094727B2 (en) * 1993-03-19 2000-10-03 三菱マテリアル株式会社 Powder for magnetic shielding
JP3094728B2 (en) * 1993-03-19 2000-10-03 三菱マテリアル株式会社 Powder for magnetic shielding

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