JP3867636B2 - Aluminum alloy wiring material and manufacturing method thereof - Google Patents
Aluminum alloy wiring material and manufacturing method thereof Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は、アルミニウム合金配線材及びその製造方法に係り、特に、自動車等の装置の配線材に用いられるアルミニウム合金配線材及びその製造方法に関するものである。
【０００２】
【従来の技術】
従来、自動車等の配線材の配線材料としては、機械的強度および導電率の点から、銅又は銅合金、アルミニウム又はアルミニウム合金が用いられてきた。
【０００３】
【発明が解決しようとする課題】
ところで、銅又は銅合金は、引張強さ及び導電率は高いものの、比重が高いため、銅又は銅合金からなる配線材を自動車等の装置に適用した場合、配線材の重量割合が増え、装置全体のエネルギー効率の低下を招くという問題がある。
【０００４】
また、高温環境下では、銅又は銅合金自体が軟化するため、配線材の強度が不足するという問題がある。このため、配線材の周りの環境温度が高温になる自動車、特に電気自動車においては、銅又は銅合金からなる配線材の信頼性の確保が困難であった。
【０００５】
一方、アルミニウム合金からなる配線材は、導電率が低いため、ジュール熱が発生し、エネルギー損失が大きくなってしまうという問題がある。
【０００６】
また、アルミニウム合金は、導電率が低く、かつ、引張強さが小さいため、アルミニウム合金からなる配線材の電流溶量及び機械的強度を満足させるためには、配線材の断面積を大きくする必要がある。このため、アルミニウム合金からなる配線材を自動車等の装置に適用した場合、装置全体に占める配線材の容積が大きくなって、大型化を招いてしまい、エネルギー効率を低下させてしまう。
【０００７】
さらに、アルミニウム合金からなる配線材で必要な引張強さを得ようとすると、伸びが低下してしまうことから、可撓性が低下し、屈曲寿命の低下を招くという欠点がある。
【０００８】
また、高温環境下での使用においては、銅又は銅合金と同様の理由で、信頼性の確保が困難であった。
【０００９】
以上より、自動車、特に電気自動車などに使用する配線材料としては、導電性、引張強さ、及び伸びが高いこと、また、耐熱性が良好であることが望まれている。しかしながら、従来の配線材料で、これらをすべて満足するものはなかった。
【００１０】
以上の事情を考慮して創案された本発明の目的は、導電性が良好で、引張強さ及び伸びが高く、かつ、耐熱性も良好なアルミニウム合金配線材及びその製造方法を提供することにある。
【００１１】
【課題を解決するための手段】
上記目的を達成すべく本発明に係るアルミニウム合金配線材は、純度９９．９５％以上の純アルミニウムからなる母材中にＦｅ、Ｚｒを特定の割合で添加し、化学組成が、Ｆｅ：０．２〜１．０質量％、Ｚｒ：０．０１〜０．１０質量％であり、残余がＡｌ及び不可避不純物からなる鋳造体に塑性加工および熱処理を施してなり、伸びが１０％以上であり、かつ、２８０℃の温度環境下における強度残存率が９１〜９６％であることを特徴とするアルミニウム合金配線材である。
【００１２】
以上の化学組成により、導電性が良好で、引張強さ及び伸びが高く、かつ、耐熱性も良好なアルミニウム合金配線材料が得られる。
【００１３】
一方、本発明に係るアルミニウム合金配線材の製造方法は、純度９９．９５％以上の純アルミニウムからなる母材中にＦｅ、Ｚｒを特定の割合で添加し、化学組成が、Ｆｅ：０．２〜１．０質量％、Ｚｒ：０．０１〜０．１０質量％であり、残余がＡｌ及び不可避不純物のアルミニウム合金鋳造体を形成し、その鋳造体に断面減少率が８５％以上の塑性加工および２５０〜３５０℃で１時間の熱処理を施すことにより、伸びが１０％以上であり、かつ、２８０℃の温度環境下における強度残存率が９１〜９６％である線材を形成するものである。
【００１４】
以上の製造方法により、前述した組成を有するアルミニウム合金鋳造体が得られ、その鋳造体を用いることでアルミニウム合金配線材を得ることができる。
【００１５】
【発明の実施の形態】
以下、本発明の好適一実施の形態について説明する。
【００１６】
本発明者らが鋭意研究を行った結果、所定以上の純度を有するアルミニウムに、Ｆｅ及びＺｒを特定の割合で微量添加することで、アルミニウムの特長である低比重および良好な導電性を維持しつつ、機械的強度および伸びが高く、かつ、耐熱性も良好となるということを見出し、本発明を完成するに至った。
【００１７】
具体的には、本発明に係るアルミニウム合金配線材料は、
Ｆｅを０．２〜１．０重量％、好ましくは０．２〜０．７重量％、特に好ましくは０．３〜０．６重量％、
Ｚｒを０．０１〜０．１０重量％、好ましくは０．０１〜０．０５重量％、特に好ましくは０．０２重量％前後含有し、
かつ、残余がＡｌ及び０．０５重量％以下の不可避不純物で構成されるものである。
【００１８】
一方、本発明に係るアルミニウム合金配線材の製造方法は、先ず、純度９９．９５％以上の純アルミニウムからなるＡｌ母材の溶湯中に、Ｆｅ及びＺｒを添加すると共に、それらの添加割合を調整し、前述した化学組成を有するＡｌ合金溶湯を作製する。次に、このＡｌ合金溶湯を用いて鋳造体の形成を行い、その後、その鋳造体に、断面減少率が８５％以上の塑性加工および２５０〜３５０℃で１時間の熱処理を施す。これによって、本発明に係るアルミニウム合金材料からなる配線材が得られる。
【００１９】
ここで、Ａｌ母材として、純度が９９．９５％以上の純アルミニウムを用いるのは、純度が９９．９５％よりも低いと、得られる配線材料において良好な導電率が得られないためである。
【００２０】
また、鋳造体に施す線材加工としては、特に限定するものではないが、例えば、断面減少率（減面率）が８５％以上、好ましくは９０％以上の塑性加工（冷間加工）が挙げられる。
【００２１】
次に、本発明に使用するアルミニウム合金配線材料の作用を説明する。
【００２２】
本発明に使用するアルミニウム合金配線材料は、母材となる純アルミニウムの純度と、ＦｅおよびＺｒの重量比とを規定したことにより、純アルミニウムと略同等の良好な導電率が得られ、従来のアルミニウム合金のようにジュール熱の発生に伴うエネルギー損失が多くなるということはない。よって、この配線材料を用いた配線材を適用した装置、例えば自動車などにおいては、エネルギーの高効率化、すなわちエネルギー効率の向上を図ることができる。
【００２３】
また、Ａｌ以外の元素（Ｆｅ、Ｚｒ等）の含有量は、最大でも１％強であるため、本発明に使用する配線材料の比重は純アルミニウムと略同等である。よって、この配線材料を用いた配線材を自動車等の装置に適用しても、配線材の重量割合は純アルミニウムの場合と略同等であり、その結果、装置全体の重量を小さくすることができ、エネルギー効率の向上を図ることができる。
【００２４】
また、本発明に使用する配線材料は、純アルミニウムと略同等の良好な導電率を有し、かつ、室温での引張強さは純アルミニウムよりも高いことから、配線材の電流溶量及び機械的強度を満足させるために、配線材の断面積を大きくする必要はない。よって、この配線材料を用いた配線材の断面積を小さく抑えることができ、装置全体に占める配線材の容積が小さくなり、その結果、装置の容積を小さくすることができる。
【００２５】
また、本発明に使用する配線材料は、純アルミニウムと比較して室温での引張強さは同等以上で、かつ、伸びは著しく高い。よって、この配線材料を用いた配線材の可撓性が良好となり、その結果、従来の配線材と比較して配線材の屈曲寿命が向上する。
【００２６】
また、本発明に使用する配線材料は、高温環境下においても引張強さは殆ど低下せず、高温強度が良好であることから、この配線材料を用いた配線材は高温環境下での信頼性が高い。よって、この配線材料を用いた配線材を、高温耐熱性が要求される装置、例えば電気自動車に適用すれば、自動車の信頼性を著しく向上させることができる。
【００２７】
本発明のアルミニウム合金配線材は、自動車用配線材の他にも、自動車用ハーネス、モーター用巻線、ケーブル用接続端子、その他のアッセンブリー品などにも適用することができる。
【００２８】
以上、本発明の実施の形態は、上述した実施の形態に限定されるものではなく、他にも種々のものが想定されることは言うまでもない。
【００２９】
【実施例】
次に、本発明について、実施例に基づいて説明するが、本発明に係る配線材の製造方法及び化学組成などは、これらの実施例に限定されるものではない。
【００３０】
（実施例１）
配線材料母材として純度９９．９５％のＡｌを用いて、化学組成がＡｌ-0.3Ｆｅ-0.02Ｚｒ（重量％）のアルミニウム合金を鋳造し、その鋳造体に断面減少率９０％の塑性加工（減面加工）を施して線材を形成し、その線材に２５０〜３５０℃で約１時間の熱処理を施し、アルミニウム合金配線材を作製した（試料１）。
【００３１】
（実施例２）
配線材料母材として純度９９．９５％のＡｌを用いて、化学組成がＡｌ-0.6Ｆｅ-0.02Ｚｒ（重量％）のアルミニウム合金からなる鋳造体を作製し、その後は、実施例１と同様にしてアルミニウム合金配線材を作製した（試料２）。
【００３２】
（比較例１）
配線材料として純度９９．９５％のＡｌを用いて純アルミニウム鋳造体を作製し、その後は、実施例１と同様にしてアルミニウム配線材を作製した（試料３）。
【００３３】
（比較例２）
配線材料母材として純度９９．９５％のＡｌを用いて、化学組成がＡｌ-0.3Ｆｅ（重量％）のアルミニウム合金からなる鋳造体を作製し、その後は、実施例１と同様にしてアルミニウム合金配線材を作製した（試料４）。
【００３４】
（比較例３）
配線材料母材として純度９９．９５％のＡｌを用いて、化学組成がＡｌ-0.6Ｆｅ（重量％）のアルミニウム合金からなる鋳造体を作製し、その後は、実施例１と同様にしてアルミニウム合金配線材を作製した（試料５）。
【００３５】
実施例１，２及び比較例１〜３の各配線材（試料１〜５）について、導電率（％ＩＡＣＳ）、室温（２０℃）での引張強さ（ＭＰａ）、伸び（％）、及び高温環境下（２８０℃）での強度残存率（％）を測定した。尚、高温環境下での強度残存率は、（２８０℃での引張強さ×１００／室温での引張強さ）によって求めた。各配線材のそれぞれの測定値を表１に示す。
【００３６】
【表１】
表１から明らかなように、実施例１の配線材（試料１）の導電率は６０．５％ＩＡＣＳ、常温引張強さは１２８ＭＰａであり、比較例２の配線材（試料４）と略同程度であり、特に伸び（１０％）については同等以上であった。また、実施例２の配線材（試料２）の導電率は６０．３％ＩＡＣＳ、常温引張強さは１３０ＭＰａであり、比較例３の配線材（試料５）と略同程度であり、特に伸び（１５％）については同等以上であった。ところが、試料１，２の高温環境下での強度残存率は９１％、９６％であり、試料４，５のそれ（８０％、８５％）と比較して１０％以上も向上している。このことから、試料１，２においては、Ｚｒの微量添加により高温強度（耐熱性）が改善されていることがわかる。
【００３８】
また、試料１，２と比較例１の配線材（試料３）とを比較すると、試料１，２の導電率が試料３のそれよりもやや劣る他は、常温の引張強さは同等以上であり、また、伸びについては２倍以上、高温強度については１．５倍以上となっていることがわかる。
【００３９】
以上要するに本発明によれば、純度９９．９５％以上の純アルミニウムからなる母材中にＦｅ、Ｚｒを特定の割合で添加し、その化学組成が、Ｆｅ：０．２〜１．０質量％、Ｚｒ：０．０１〜０．１０質量％であり、残余がＡｌ及び不可避不純物からなり、伸びが１０％以上であり、かつ、２８０℃の温度環境下における強度残存率が９０％以上であるアルミニウム合金配線材を用いることで、十分な導電性および引張強さを維持しつつ、可撓性が良好であり、配線材としての屈曲寿命を向上させることができるとともに、高温環境下での強度不足を防止することができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an aluminum alloy wiring material and a manufacturing method thereof , and more particularly to an aluminum alloy wiring material used for a wiring material of a device such as an automobile and a manufacturing method thereof .
[0002]
[Prior art]
Conventionally, copper or a copper alloy, aluminum or an aluminum alloy has been used as a wiring material for a wiring material of an automobile or the like from the viewpoint of mechanical strength and electrical conductivity.
[0003]
[Problems to be solved by the invention]
By the way, although copper or copper alloy has high tensile strength and electrical conductivity, since the specific gravity is high, when a wiring material made of copper or copper alloy is applied to a device such as an automobile, the weight ratio of the wiring material increases, and the device There is a problem that the overall energy efficiency is reduced.
[0004]
Moreover, since copper or copper alloy itself softens in a high temperature environment, there exists a problem that the intensity | strength of wiring material is insufficient. For this reason, it has been difficult to ensure the reliability of a wiring material made of copper or a copper alloy in an automobile in which the ambient temperature around the wiring material is high, particularly an electric vehicle.
[0005]
On the other hand, a wiring material made of an aluminum alloy has a problem that Joule heat is generated due to low conductivity, resulting in a large energy loss.
[0006]
In addition, since aluminum alloys have low electrical conductivity and low tensile strength, it is necessary to increase the cross-sectional area of the wiring material in order to satisfy the current dissolution amount and mechanical strength of the wiring material made of the aluminum alloy. There is. For this reason, when a wiring material made of an aluminum alloy is applied to a device such as an automobile, the volume of the wiring material occupying the entire device increases, leading to an increase in size and a reduction in energy efficiency.
[0007]
Furthermore, when it is intended to obtain a necessary tensile strength with a wiring material made of an aluminum alloy, the elongation is lowered, so that there is a drawback that flexibility is lowered and bending life is reduced.
[0008]
Further, in use in a high temperature environment, it has been difficult to ensure reliability for the same reason as copper or copper alloy.
[0009]
From the above, as a wiring material used for an automobile, particularly an electric automobile, etc., it is desired that conductivity, tensile strength, and elongation are high, and that heat resistance is good. However, none of the conventional wiring materials satisfy these requirements.
[0010]
The purpose of the consideration of the circumstances in the present invention that is conceived above, conductive good, high tensile strength and elongation, and that the heat resistance to provide good aluminum alloy wiring material and a manufacturing method thereof is there.
[0011]
[Means for Solving the Problems]
In order to achieve the above object, an aluminum alloy wiring material according to the present invention is obtained by adding Fe and Zr at a specific ratio to a base material made of pure aluminum having a purity of 99.95% or more, and having a chemical composition of Fe: 0.00. 2 to 1.0% by mass, Zr: 0.01 to 0.10% by mass, the remainder is made by plastic working and heat treatment to a casting made of Al and inevitable impurities, and the elongation is 10% or more, And it is an aluminum alloy wiring material characterized by the residual strength rate being 91-96% under a temperature environment of 280 ° C.
[0012]
With the above chemical composition, an aluminum alloy wiring material having good conductivity, high tensile strength and elongation, and good heat resistance can be obtained.
[0013]
On the other hand, in the method for producing an aluminum alloy wiring material according to the present invention, Fe and Zr are added in a specific ratio to a base material made of pure aluminum having a purity of 99.95% or more, and the chemical composition is Fe: 0.2. -1.0% by mass, Zr: 0.01-0.10% by mass, the remainder is formed of an aluminum alloy cast body of Al and inevitable impurities, and the cross-section reduction rate is 85% or more in the cast body By performing a heat treatment at 250 to 350 ° C. for 1 hour , a wire having an elongation of 10% or more and a residual strength ratio of 91 to 96% in a temperature environment of 280 ° C. is formed.
[0014]
By the above manufacturing method, an aluminum alloy casting having the above-described composition is obtained, and an aluminum alloy wiring material can be obtained by using the casting.
[0015]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, a preferred embodiment of the present invention will be described.
[0016]
As a result of intensive studies by the present inventors, by adding a small amount of Fe and Zr at a specific ratio to aluminum having a purity of a predetermined level or more, the low specific gravity and good conductivity that are the characteristics of aluminum are maintained. On the other hand, the present inventors have found that the mechanical strength and elongation are high and the heat resistance is also good, and the present invention has been completed.
[0017]
Specifically, the aluminum alloy wiring material according to the present invention is:
0.2 to 1.0% by weight of Fe, preferably 0.2 to 0.7% by weight, particularly preferably 0.3 to 0.6% by weight,
Zr is contained in an amount of 0.01 to 0.10% by weight, preferably 0.01 to 0.05% by weight, particularly preferably about 0.02% by weight,
In addition, the balance is composed of Al and 0.05% by weight or less of inevitable impurities.
[0018]
On the other hand, in the method for producing an aluminum alloy wiring material according to the present invention, first, Fe and Zr are added to a molten Al base material made of pure aluminum having a purity of 99.95% or more, and the addition ratio thereof is adjusted. Then, an Al alloy melt having the above-described chemical composition is prepared. Next, a cast body is formed using this Al alloy molten metal, and thereafter, the cast body is subjected to plastic working with a cross-section reduction rate of 85% or more and heat treatment at 250 to 350 ° C. for 1 hour . Thereby, a wiring material made of the aluminum alloy material according to the present invention is obtained.
[0019]
Here, pure aluminum having a purity of 99.95% or more is used as the Al base material because, if the purity is lower than 99.95%, good conductivity cannot be obtained in the obtained wiring material. .
[0020]
In addition, the wire material processing applied to the cast body is not particularly limited, and examples thereof include plastic processing (cold processing) in which the cross-section reduction rate (area reduction rate) is 85% or more, preferably 90% or more. .
[0021]
Next, the effect | action of the aluminum alloy wiring material used for this invention is demonstrated.
[0022]
The aluminum alloy wiring material used in the present invention has a good conductivity substantially equal to that of pure aluminum by prescribing the purity of pure aluminum as a base material and the weight ratio of Fe and Zr. Unlike aluminum alloys, there is no increase in energy loss due to generation of Joule heat. Therefore, in an apparatus to which a wiring material using this wiring material is applied, such as an automobile, energy efficiency can be improved, that is, energy efficiency can be improved.
[0023]
Further, since the content of elements other than Al (Fe, Zr, etc.) is a little over 1% at the maximum, the specific gravity of the wiring material used in the present invention is substantially the same as that of pure aluminum. Therefore, even if the wiring material using this wiring material is applied to a device such as an automobile, the weight ratio of the wiring material is substantially the same as that of pure aluminum, and as a result, the weight of the entire device can be reduced. , Energy efficiency can be improved.
[0024]
In addition, since the wiring material used in the present invention has a good electrical conductivity substantially equivalent to that of pure aluminum and has a higher tensile strength at room temperature than pure aluminum, It is not necessary to increase the cross-sectional area of the wiring material in order to satisfy the desired strength. Therefore, the cross-sectional area of the wiring material using this wiring material can be kept small, and the volume of the wiring material occupying the entire device is reduced. As a result, the volume of the device can be reduced.
[0025]
In addition, the wiring material used in the present invention has a tensile strength at room temperature that is equal to or higher than that of pure aluminum, and has an extremely high elongation. Therefore, the flexibility of the wiring material using this wiring material is improved, and as a result, the bending life of the wiring material is improved as compared with the conventional wiring material.
[0026]
In addition, since the wiring material used in the present invention has almost no decrease in tensile strength even in a high temperature environment, and the high temperature strength is good, the wiring material using this wiring material is reliable in a high temperature environment. Is expensive. Therefore, if the wiring material using this wiring material is applied to a device that requires high temperature heat resistance, for example, an electric vehicle, the reliability of the vehicle can be remarkably improved.
[0027]
The aluminum alloy wiring material of the present invention can be applied not only to automotive wiring materials but also to automotive harnesses, motor windings, cable connection terminals, and other assembly products.
[0028]
As mentioned above, it cannot be overemphasized that embodiment of this invention is not limited to embodiment mentioned above, and various things are assumed in addition.
[0029]
【Example】
Next, although this invention is demonstrated based on an Example, the manufacturing method, chemical composition, etc. of the wiring material which concern on this invention are not limited to these Examples.
[0030]
Example 1
An aluminum alloy having a chemical composition of Al-0.3Fe-0.02Zr (weight%) is cast using Al of 99.95% purity as a wiring material base material, and plastic processing with a cross-section reduction rate of 90% is performed on the cast body ( A wire rod was formed by performing a surface reduction process, and the wire rod was heat-treated at 250 to 350 ° C. for about 1 hour to produce an aluminum alloy wiring member (Sample 1).
[0031]
(Example 2)
A cast body made of an aluminum alloy having a chemical composition of Al-0.6Fe-0.02Zr (weight%) was produced using Al having a purity of 99.95% as the wiring material base material. Thus, an aluminum alloy wiring material was prepared (Sample 2).
[0032]
(Comparative Example 1)
A pure aluminum cast was produced using 99.95% purity Al as the wiring material, and thereafter an aluminum wiring material was produced in the same manner as in Example 1 (Sample 3).
[0033]
(Comparative Example 2)
A cast body made of an aluminum alloy having a chemical composition of Al-0.3Fe (weight%) was produced using Al having a purity of 99.95% as a wiring material base material. Thereafter, an aluminum alloy was produced in the same manner as in Example 1. A wiring material was prepared (Sample 4).
[0034]
(Comparative Example 3)
A cast body made of an aluminum alloy having a chemical composition of Al-0.6Fe (wt%) was produced using Al having a purity of 99.95% as a wiring material base material. Thereafter, an aluminum alloy was produced in the same manner as in Example 1. A wiring material was prepared (Sample 5).
[0035]
About each wiring material (samples 1-5) of Examples 1 and 2 and Comparative Examples 1 to 3, electrical conductivity (% IACS), tensile strength (MPa) at room temperature (20 ° C.), elongation (%), and The residual strength rate (%) in a high temperature environment (280 ° C.) was measured. The residual strength rate in a high temperature environment was determined by (tensile strength at 280 ° C. × 100 / tensile strength at room temperature). Table 1 shows the measured values of each wiring material.
[0036]
[Table 1]
As apparent from Table 1, the conductivity of the wiring material of Example 1 (Sample 1) is 60.5% IACS, and the tensile strength at room temperature is 128 MPa, which is substantially the same as the wiring material of Comparative Example 2 (Sample 4). In particular, the elongation (10%) was equal or better. Moreover, the electrical conductivity of the wiring material of Example 2 (Sample 2) is 60.3% IACS, and the normal temperature tensile strength is 130 MPa, which is substantially the same as that of the wiring material of Comparative Example 3 (Sample 5), and in particular, elongation (15%) was equivalent or better. However, the residual strength rates of Samples 1 and 2 in a high temperature environment are 91% and 96%, which is an improvement of 10% or more compared to those of Samples 4 and 5 (80% and 85%). From this, it can be seen that in samples 1 and 2, the high temperature strength (heat resistance) is improved by adding a small amount of Zr.
[0038]
In addition, comparing Samples 1 and 2 with the wiring material of Comparative Example 1 (Sample 3), the tensile strength at room temperature is equal to or higher than that of Sample 3 except that the conductivity of Samples 1 and 2 is slightly inferior to that of Sample 3. In addition, it can be seen that the elongation is 2 times or more and the high temperature strength is 1.5 times or more.
[0039]
In short, according to the present invention, Fe and Zr are added in a specific ratio to a base material made of pure aluminum having a purity of 99.95% or more, and the chemical composition thereof is Fe: 0.2 to 1.0% by mass. , Zr: 0.01 to 0.10% by mass, the remainder is made of Al and inevitable impurities, the elongation is 10% or more, and the residual strength rate in a temperature environment of 280 ° C. is 90% or more. By using an aluminum alloy wiring material, while maintaining sufficient electrical conductivity and tensile strength, it has good flexibility, can improve the flex life as a wiring material, and has strength in a high-temperature environment. Insufficiency can be prevented.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002220650A JP3867636B2 (en) | 2002-07-30 | 2002-07-30 | Aluminum alloy wiring material and manufacturing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002220650A JP3867636B2 (en) | 2002-07-30 | 2002-07-30 | Aluminum alloy wiring material and manufacturing method thereof |
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| Publication Number | Publication Date |
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| JP2004060006A JP2004060006A (en) | 2004-02-26 |
| JP3867636B2 true JP3867636B2 (en) | 2007-01-10 |
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