JP2014513753A5

JP2014513753A5 -

Info

Publication number: JP2014513753A5
Application number: JP2013551417A
Authority: JP
Filing date: 2012-01-30
Publication date: 2015-07-23
Anticipated expiration: 2032-01-30

Description

更に別の実施形態において、本発明は、非晶質材料を成形する急速コンデンサ放電装置に関する。１つのそのような実施形態において、非晶質材料のサンプルは、実質的に均一な断面を有する。別のそのような実施形態において、少なくとも２つの電極は、非晶質材料のサンプルに電気エネルギ供給源を接続する。そのような実施形態において、電極は、実質的に均一な接続が電極とサンプルの間に形成されるようにサンプルに取り付けられる。更に別のそのような実施形態において、動的電界の電磁表皮深さは、装填物の半径、幅、厚み、及び長さと比較して大きい。 In yet another embodiment, the present invention relates to a rapid capacitor discharge device for molding an amorphous material. In one such embodiment, the sample of amorphous material has a substantially uniform cross section. In another such embodiment, the at least two electrodes connect an electrical energy source to the sample of amorphous material. In such embodiments, the electrode is attached to the sample such that a substantially uniform connection is formed between the electrode and the sample. In yet another such embodiment, the electromagnetic skin depth of the dynamic electric field is large compared to the load radius, width, thickness, and length.

更に別の実施形態において、本発明は、
・実質的に均一な断面を有する強磁性非晶質金属のサンプルを準備する段階と、
・電気エネルギの量子を生成及び放出することができる電気エネルギ供給源とサンプルを電気的に接触させる段階と、
・サンプルを通じて均一に電気エネルギの量子を放出し、ガラス転移温度と非晶質金属の平衡融点の間の処理温度までサンプルの全体を急速かつ均一に加熱し、電気エネルギの量子の放出が、サンプルにおいて電界を生成し、動的電界の電磁表皮深さが、サンプルの半径、幅、厚み、及び長さと比較して大きいが、電流パルスの立上り時間が、冷却不足液体領域において最適形成温度で非晶質金属を結晶化させることに関連付けられた時間を超えない段階と、
・加熱されたサンプルが依然としてガラス転移温度と平衡融点の間の温度にある間に加熱されたサンプルを成形するために変形力を印加する段階と、
・非晶質材料のガラス転移温度未満の温度に物品を冷却する段階と、
を含む急速コンデンサ放電を使用して磁気非晶質金属を急速かつ均一に加熱する方法に関する。 In yet another embodiment, the present invention provides:
Providing a sample of a ferromagnetic amorphous metal having a substantially uniform cross-section;
Electrically contacting the sample with an electrical energy source capable of generating and emitting quantum of electrical energy;
Emission of electrical energy quanta uniformly throughout the sample, heating the entire sample rapidly and uniformly to a processing temperature between the glass transition temperature and the equilibrium melting point of the amorphous metal, and the emission of electrical energy quanta The electromagnetic skin depth of the dynamic electric field is large compared to the radius, width, thickness and length of the sample, but the rise time of the current pulse is not optimal at the optimal formation temperature in the undercooled liquid region. Not exceeding the time associated with crystallizing the crystalline metal;
Applying a deformation force to shape the heated sample while the heated sample is still at a temperature between the glass transition temperature and the equilibrium melting point;
Cooling the article to a temperature below the glass transition temperature of the amorphous material;
To rapidly and uniformly heat a magnetic amorphous metal using a rapid capacitor discharge comprising:

更に別の実施形態において、本発明は、
・実質的に均一な断面を有する強磁性非晶質金属のサンプルと、
・電気エネルギ供給源と、
・非晶質材料のサンプルに電気エネルギ供給源を接続し、実質的に密接な接続が電極とサンプルの間に形成されるようにサンプルに取り付けられた少なくとも２つの電極と、
・サンプルとの形成関係に配置された成形ツールと、
を含み、
・電気エネルギ供給源が、ガラス転移温度と非晶質金属の平衡融点の間の処理温度までサンプルの全体を均一に加熱するのに十分な電気エネルギの量子を生成及び放出することができ、電気エネルギの量子の放出が、サンプルにおいて電界を生成し、動的電界の電磁表皮深さが、サンプルの半径、幅、厚み、及び長さと比較して大きいが、電流パルスの立上り時間が、冷却不足液体領域において最適形成温度で非晶質金属を結晶化させることに関連付けられた時間を超えず、
・成形ツールが、加熱されたサンプルをネット形状物品に形成するのに十分な変形力を印加することができる、
強磁性非晶質金属を急速に加熱する急速コンデンサ放電装置に関する。 In yet another embodiment, the present invention provides:
A sample of ferromagnetic amorphous metal having a substantially uniform cross-section;
An electrical energy source;
Connecting an electrical energy source to a sample of amorphous material and at least two electrodes attached to the sample such that a substantially intimate connection is formed between the electrode and the sample;
A molding tool arranged in a forming relationship with the sample;
Including
An electrical energy source can generate and emit quantum of electrical energy sufficient to uniformly heat the entire sample to a processing temperature between the glass transition temperature and the equilibrium melting point of the amorphous metal, The quantum emission of energy creates an electric field in the sample, and the electromagnetic skin depth of the dynamic electric field is large compared to the radius, width, thickness, and length of the sample, but the rise time of the current pulse is undercooled Not exceed the time associated with crystallizing the amorphous metal at the optimum formation temperature in the liquid region,
The molding tool can apply sufficient deformation force to form a heated sample into a net-shaped article;
The present invention relates to a rapid capacitor discharge device for rapidly heating a ferromagnetic amorphous metal.

容量放電中に円筒体内の電流が均一であるには、動的電界の電磁表皮深さΛがサンプルに関連付けられた寸法（半径、長さ、幅、又は厚み）の特性と比較して大きいことが必要である。円筒体の例では、関連の特徴的な寸法は、明らかに装填物の半径及び深さＲ及びＬであると考えられる。この条件は、Λ＝［ρ₀τ／μ₀］^1/2≧Ｒ（Ｌ）の時に満たされる。ここで、τはコンデンサの「ＲＣ」時定数であり、サンプルシステムμ₀＝４π×１０^-7（ヘンリー／ｍ）は空き領域の誘電率である。Ｒ及びＬ〜１ｃｍに対して、これは、τ＞１０〜１００μｓを意味する。このような一般的な寸法及び非晶質合金の抵抗率の値を使用して、これには、適切にサイズ設定をされた典型的に約１０，０００μＦのキャパシタンス又はそれよりも大きいコンデンサが必要である。 In order for the current in the cylinder to be uniform during capacitive discharge, the electromagnetic skin depth Λ of the dynamic electric field must be large compared to the dimensions (radius, length, width or thickness) characteristics associated with the sample. is necessary. In the cylinder example, the relevant characteristic dimensions are clearly considered to be the charge radius and depth R and L. This condition is satisfied when Λ = [ρ ₀ τ / μ ₀ ] ^1/2 ≧ R (L). Here, τ is the “RC” time constant of the capacitor, and the sample system μ ₀ = 4π × 10 ⁻⁷ (Henry / m) is the permittivity of the empty area. For R and L˜1 cm, this means τ> 10-100 μs. Using these general dimensions and resistivity values for amorphous alloys, this requires a suitably sized capacitor of typically about 10,000 μF or larger. It is.

上述したように、加熱を通して均一な温度を維持するために、電流のエネルギ消散は、金属ガラス装填物を通して均一でなければならず、従って、印加された電界は、断面にわたって金属ガラス装填物に通過すべきである。電界の通過の尺度は、表皮深さΛであり、表皮深さΛは、外部的に印加された電界が材料内で１／ｅまで低下する距離として定義され、良導体に対して次式；
Λ＝［ρ₀τ／μ_rμ₀］^1/2 （式６）
のように与えられ、ここで、τは、電流パルスの増加に関連付けられた時定数であり、ρ₀は金属ガラスの抵抗率であり、μ₀は空き領域の透磁率であり、μ_rは金属ガラスの比透磁率である。上述したように、均一な加熱をもたらすために、金属ガラス装填物の寸法は、Λより遥かに小さいものであるべきである。ＲＣＤＦに利用される一般的な放電時間τ_RCは、約１ｍｓである。非磁性金属ガラスに約２００μΩ−ｃｍの一般的な抵抗率及びμ_r≒１の比透磁率を使用すると、表皮深さは、約４０ｍｍである。このような表皮深さが入手可能な金属ガラスの実用的な寸法よりも遥かに大きいので、均一な加熱が保証されることになる。しかし、強磁性金属ガラスは、典型的には遥かに高い比透磁率（１０²〜１０⁴のμ_r）を有し、０．５〜５ｍｍの範囲の表皮深さΛが発生する。これらの表皮深さは、従って、金属ガラス装填物の実用的なサイズに相当する。その結果、約１ｍｓの従来の時間尺度で機能するＲＣＤＦを使用して強磁性ガラスを処理した時に不均一な加熱が発生することになる。 As mentioned above, in order to maintain a uniform temperature throughout the heating, the energy dissipation of the current must be uniform through the metallic glass charge, so that the applied electric field passes through the metallic glass charge across the cross section. Should. Measure of the passage of the electric field is the skin depth lambda, the skin depth lambda is defined as the distance external to the applied electric field is reduced in the material to 1 / e, the following expression for a good conductor;
Λ = [ρ ₀ τ / μ _r μ ₀ ] ^1/2 (Formula 6)
Where τ is the time constant associated with the increase in current pulse, ρ ₀ is the resistivity of the metallic glass, μ ₀ is the permeability of the free space, and μ _r is It is the relative permeability of metallic glass. As noted above, the size of the metallic glass charge should be much smaller than Λ to provide uniform heating. A typical discharge time τ _RC used for RCDF is about 1 ms. Using a typical resistivity of about 200 μΩ-cm and a relative permeability of μ _r ≈1 for non-magnetic metallic glass, the skin depth is about 40 mm. Such skin depth is much larger than the practical dimensions of available metallic glass, so that uniform heating is guaranteed. However, ferromagnetic metallic glasses typically have a much higher relative permeability (10 ² to 10 ⁴ of the mu _r), the skin depth in the range of 0.5 to 5 mm lambda occurs. These skin depths therefore correspond to a practical size of the metallic glass charge. As a result, non-uniform heating occurs when the ferromagnetic glass is processed using RCDF that functions on a conventional time scale of about 1 ms.

従って、一実施形態において、本発明は、パルスの時間を長くし、従って、電流パルスτの増加に関連付けられた時定数を増加させ、その結果、表皮深さ（Λ）を増加させることにより、非磁性金属ガラスの処理において達成される電磁表皮深さに同等の比較的大きい電磁表皮深さをもたらすことに関する。それによって高い比透磁率を有する金属ガラス合金を容量放電で均一に加熱することができる。しかし、パルス立上り時間は、冷却不足液体領域での最適形成温度で金属ガラスを結晶化させるのに要する時間（典型的に強磁性ガラスに対して０．１〜１ｓ間）に接近したり上回ったりすべきではない。好ましくは、電流パルスの立上り時間は、１ｍｓと１００ｍｓの間である。 Thus, in one embodiment, the present invention increases the time of the pulse, thus increasing the time constant associated with the increase in current pulse τ, and consequently increasing the skin depth (Λ), It relates to providing a relatively large electromagnetic skin depth equivalent to the electromagnetic skin depth achieved in the processing of non-magnetic metallic glass. Thereby, a metallic glass alloy having a high relative magnetic permeability can be uniformly heated by capacitive discharge. However, the pulse rise time approaches or exceeds the time required to crystallize the metallic glass at the optimum forming temperature in the undercooled liquid region (typically between 0.1 and 1 s for ferromagnetic glass). should not do. Preferably, the rise time of the current pulse is between 1 ms and 100 ms.

このような磁気金属ガラスをオーム加熱する方法の一実施形態において、容量放電τのパルスの立上り時間は長くされ、従って、金属ガラス装填物に印加された周波数を低減し、表皮深さΛを増加させる。Ｒ、Ｌ、及びＣが、それぞれ回路の抵抗、インダクタンス、及びキャパシタンスである直列ＲＬＣ回路の減衰係数は、ζ＝（Ｒ／２）√（Ｃ／Ｌ）により与えられる。以下のようにパルス立上り時間を伸張することによって表皮深さを増加させることができる。
・システム応答がネーパー周波数により支配された場合に、パルス立上り時間は、τ＝２Ｌ／Ｒで判断される。従って、回路に付加的なインダクタンスを導入することによって表皮深さを増加させることができる。例えば、放電回路と直列にワイヤのループ又はコイルの形態でインダクタを追加することによってこれをもたらすことができる。
・システム応答が角度周波数により支配された場合に、パルス立上り時間は、τ＝√（ＬＣ）により決まる。従って、回路に付加的なインダクタンス及び／又は付加的なキャパシタンスを導入することによって表皮深さを増加させることができる。例えば、放電回路と直列にワイヤのループ又はコイルの形態でインダクタを追加することにより、及び／又は放電回路と直列に付加的なコンデンサを追加することによってこれをもたらすことができる。 In one embodiment of the method for ohmic heating such a magnetic metallic glass, the rise time of the pulse of capacitive discharge τ is lengthened, thus reducing the frequency applied to the metallic glass charge and increasing the skin depth Λ. Let The attenuation coefficient of a series RLC circuit where R, L, and C are the circuit resistance, inductance, and capacitance, respectively, is given by ζ = (R / 2) √ (C / L). The skin depth can be increased by extending the pulse rise time as follows.
If the system response is dominated by the Naper frequency, the pulse rise time is determined by τ = 2L / R. Therefore, the skin depth can be increased by introducing additional inductance into the circuit. For example, this can be done by adding an inductor in the form of a wire loop or coil in series with the discharge circuit.
When the system response is dominated by angular frequency, the pulse rise time is determined by τ = √ (LC). Thus, the skin depth can be increased by introducing additional inductance and / or additional capacitance into the circuit. This can be achieved, for example, by adding an inductor in the form of a wire loop or coil in series with the discharge circuit and / or by adding an additional capacitor in series with the discharge circuit.

急速放電が行われる前に金属ガラス装填物の温度を上げることによって表皮深さを増加させることができる。強磁性金属ガラスの場合に、比透磁率は、温度の増加と共に下がり、キュリー温度よりも高い温度でほぼ１の値に到達する。強磁性ガラスのキュリー温度は、典型的には、あらゆる塑性成形又は結晶化が行われることなく低い透磁率値までの予熱を可能にするようにガラス転移よりも低い。従って、一実施形態において、強磁性金属ガラス装填物は、キュリー温度よりも高いがガラス転移温度よりも低い温度まで比較的遅い容量放電パルスにより加熱され、その後の加熱及び形成に向けて急速容量放電を受ける。 The skin depth can be increased by raising the temperature of the metallic glass charge before rapid discharge takes place. In the case of a ferromagnetic metallic glass, the relative permeability decreases with increasing temperature and reaches a value of approximately 1 at a temperature higher than the Curie temperature. The Curie temperature of ferromagnetic glasses is typically lower than the glass transition to allow preheating to low permeability values without any plastic forming or crystallization. Thus, in one embodiment, the ferromagnetic metallic glass charge is heated by a relatively slow capacity discharge pulse to a temperature above the Curie temperature but below the glass transition temperature, followed by a rapid capacity discharge for subsequent heating and formation. Receive.

サンプルＡ及びＢの最終形状が、図１４ｂ及び１４ｃに示されている。図１４ｂで分るように、小さいインダクタンス及びキャパシタンスに関連付けられた高周波数（短い立上り時間τ）により、結果的に非常に不均一な形状（サンプルＡ）の一部が発生し、非常に不均一な加熱という結果は、装填物サイズと比較すると小さい表皮深さに帰するものであった。これとは対照的に、図１４ｃで分るように、大きいインダクタンス及びキャパシタンスに関連付けられた低周波数（長い立上り時間τ）により、かなり均一なディスク状の部分（サンプルＢ）が得られ、かなり均一な加熱という結果は、より大きい表皮深さに関連するものであった。非晶質装填物に対する示差熱測定走査及び低周波急速容量放電（サンプルＢ）により製造された成形ディスクが図１５に示されている。結晶化（曲線の下の区域）のエンタルピーの大きさから、サンプルＢの成形ディスクは、本質的に完全に非晶質であると結論付けることができる。 The final shapes of samples A and B are shown in FIGS. 14b and 14c. As can be seen in FIG. 14b, the high frequency (short rise time τ) associated with small inductance and capacitance results in the generation of a part of a very non-uniform shape (sample A), which is very non-uniform. The result of proper heating was attributed to a small skin depth compared to the charge size. In contrast, as can be seen in FIG. 14c, the low frequency (long rise time τ) associated with large inductance and capacitance results in a fairly uniform disk-like part (sample B), which is fairly uniform. The result of proper heating was associated with a greater skin depth . A shaped disc produced by differential calorimetric scanning and low frequency rapid capacitive discharge (Sample B) for an amorphous charge is shown in FIG. From the magnitude of enthalpy of crystallization (the area under the curve), it can be concluded that the molded disk of Sample B is essentially completely amorphous.

Claims

A method of rapidly and uniformly heating magnetic metallic glass using rapid capacitor discharge,
Preparing a sample of ferromagnetic metallic glass formed by metallic glass forming alloy having a uniform in a flat cross section,
Electrically contacting the sample with an electrical energy source capable of generating and releasing electrical energy;
Uniformly emit electrical energy through said sample, the uniformly heating the sample to a processing temperature between the glass transition temperature of the metallic glass and the equilibrium melting point of the metallic glass forming alloy, the release of the electrical energy, the An electric field is generated in the sample, and the electromagnetic skin depth of the generated dynamic electric field is large compared to the radius, width, thickness, and length of the sample, but the rise time of the current pulse due to the discharge of electric energy Not exceeding the time required for crystallization of the sample at the optimal formation temperature in the undercooled liquid region;
Applying a deformation force to form the heated sample while the heated sample is still at a temperature between the glass transition temperature of the metallic glass and the equilibrium melting point of the metallic glass-forming alloy. When,
Cooling the sample to a temperature below the glass transition temperature of the metallic glass;
A method comprising the steps of:

The method of claim 1, wherein the metallic glass has a resistivity that does not increase with temperature.

The method of claim 1, wherein the temperature of the sample is increased at a rate of at least 500 K / sec.

The metallic glass has a relative change in resistivity per unit of temperature change (S) not greater than ¹ × 10 ⁻⁴ ° C. and a resistivity (ρ ₀ ) at room temperature between 80 and 300 μΩ-cm. The method according to claim 1.

The method of claim 1, wherein the electrical energy is at least 100 J and the rise time of the current pulse is between 1 ms and 100 ms.

The treatment temperature A method according to claim 1, characterized in that between in between the equilibrium melting point of the glass transition temperature and the metallic glass forming alloy of the metallic glass.

The treatment temperature A method according to claim 1, wherein the viscosity of the heated sample is temperature of one to 10 ⁴ Pa-s.

The sample A method according to claim 1, characterized in that there are no defects.

The method of claim 1, wherein the rise time of the current pulse is controlled by increasing the inductance of an electrical circuit.

The method of claim 9, wherein the inductance is increased by adding an inductor in series with the sample.

The method of claim 1, wherein the time constant of the discharge is controlled by increasing the capacitance of an electrical circuit.

The method of claim 1, further comprising the step of preheating the sample to higher preheat temperature than the Curie temperature before releasing the electrical energy.

The method according to claim 12, wherein the preheating temperature is higher than the Curie temperature and lower than the glass transition temperature.

The method of claim 12, wherein the pre-heat treatment is performed using capacitive discharge pulses.

The method of claim 1, wherein the step of releasing the electrical energy is performed through at least two electrodes connected to opposite ends of the sample.

The method of claim 1, wherein the deforming force on the heated sample is applied after the release of the electrical energy is completed.

A rapid capacitor discharge device for rapidly heating a ferromagnetic metal glass,
A sample having a uniform in a flat section of metallic glass formed of metallic glass forming alloy,
An electrical energy source;
At least two electrodes attached to the sample such that the metallic glass of the electrical energy source to the sample interconnected, contact between the electrode and the sample connection is formed,
A molding tool arranged in a forming relationship with the sample;
Including
The electrical energy source may generate and emit sufficient electrical energy to uniformly heat the sample to a processing temperature between the glass transition temperature of the metallic glass and the equilibrium melting point of the metallic glass forming alloy. can, release of the electrical energy to generate an electric field in the sample, the electromagnetic skin depth of the generated the dynamic field, the sample radius, width, but larger than the thickness, and length, electrical The rise time of the current pulse due to the release of energy does not exceed the time required for crystallization of the metallic glass at the optimum formation temperature in the undercooled liquid region,
The molding tool can apply a deformation force sufficient to form the heated sample into a net-shaped article,
A device characterized by that.

18. The method of claim 17 , wherein the molding tool is selected from the group consisting of an injection mold, dynamic forging, stamp forging, and blow molding mold.

The apparatus of claim 17 , wherein the forming tool is at least partially formed from at least one of the electrodes.

The forming tool, the tool higher than the key Jury temperature, and to claim 17, further comprising a temperature-controlled heating element for heating to a temperature below the glass transition temperature of the metallic glass The device described.

The apparatus of claim 17 , wherein the metallic glass has a resistivity that does not increase with temperature.

The apparatus of claim 17 , wherein the temperature of the sample increases at a rate of at least 500 K / sec.

The metallic glass has a relative change in resistivity per unit of temperature change (S) not greater than ¹ × 10 ⁻⁴ ° C. and a resistivity (ρ ₀ ) at room temperature between 80 and 300 μΩ-cm. The apparatus of claim 17 .

The apparatus of claim 17 , wherein the electrical energy is at least 100 J and the rise time of the current pulse is between 1 ms and 100 ms.

The treatment temperature is, apparatus according to claim 17, characterized in that between in between the equilibrium melting point of the glass transition temperature and the metallic glass forming alloy of the metallic glass.

The treatment temperature is, apparatus according to claim 17, wherein the viscosity of the heated sample is temperature of one to 10 ⁴ Pas-sec.

The samples, according to claim 17, characterized in that there is no defect.

Electrode material, Cu, Ag, or Ni, or at least 95 at% of Cu, according to claim 17, characterized in that it is selected from a group consisting of an alloy containing one of Ag, or Ni Equipment.

29. The apparatus of claim 28 , wherein the rise time of the current pulse is modified by increasing circuit inductance.

30. The apparatus of claim 29 , wherein the time constant of the discharge is modified by adding at least one additional inductor in series with the sample.

30. The apparatus of claim 28 , wherein the time constant of the discharge is modified by increasing the capacitance of the circuit.

The source according to claim 17, characterized in that it is further configured to supply a preheating discharge that is configured to preheat the sample to higher preheat temperature than the Curie temperature before releasing the electrical energy The device described in 1.

The apparatus according to claim 32 , wherein the preheating temperature is higher than the Curie temperature and lower than the glass transition temperature.