JP3665169B2 - Manufacturing method of high strength and high ductility tungsten alloy - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明は、タングステン合金を高強度化するとともに良好な延性が得られる高強度高延性タングステン合金の製造方法に関するものである。
【０００２】
【従来の技術および発明が解決しようとする課題】
Ｗ−Ｆｅ−Ｎｉ合金は、タングステンの性質を利用して、高強度で高延性の材料として、各種用途に使用されている。この合金は、通常は、８５〜９８重量％のタングステンと、残部がバインダーとなるＮｉとＦｅからなる粉末を調製、混合した後、ＣＩＰ（冷間等方加工プレス）などによって成形体とした後に、バインダーの液相線温度以上に加熱して焼結することによって製造されている。また、用途によっては、図３に示すように、さらに強度を向上させるために、焼結合金にスエージング加工などの冷間または温間の加工強化を行い、さらに所望によりその後、後熱処理を行っている。
【０００３】
しかし、上記の方法では、高強度化は可能であるものの逆に延性が大きく低下するため、高い強度とともに良好な延性が要求される用途では、上記処理が施された合金は機械的性質としては不十分であるという問題がある。
本発明は、上記事情を背景としてなされたものであり、強度、延性ともに優れたタングステン合金が得られる高強度高延性タングステン合金の製造方法を提供することを目的とする。
【０００４】
上記課題を解決するため本発明のうち、第１の発明の高強度高延性タングステン合金の製造方法は、Ｗを重量％で８５〜９８％含有し、残部がＮｉ、Ｆｅであるタングステン合金に、加工率（断面減少率）８〜１４％とした冷間または温間加工により加工強化を与え、該加工強化後に１０００〜１２００℃の温度で中間熱処理を与え、さらに加工率（断面減少率）１６〜２２％とした冷間または温間加工により再加工強化を与え、該再加工強化後に後熱処理を施すことを特徴とする
【０００６】
さらに、第２の発明の高強度高延性タングステン合金の製造方法は、第２の発明において、加工強化と再加工強化の加工率（断面減少率）の合計が３０％以下であることを特徴とする。
【０００７】
なお、本発明が適用されるタングステン合金は、通常は焼結体として提供されるものであり、各成分粉末または合金粉末により成形体を製作し、これを焼結することにより得られる。この際に使用される粉末としては、例えばＷ粉末、その他の成分粉末ともに、３〜５μｍとするのが望ましい。これにより優れた強度と延性を得ることが一層可能になる。但し、上記焼結体を含め、上記加工強化等が施されるタングステン合金を得るまでの工程は適宜選択可能であり、本発明として特にその内容が限定されるものではない。
【０００８】
次に、上記タングステン合金に与えられる加工強化および再加工強化に際しては、その加工の種別は特に限定されず、加工強化と再加工強化において加工の種別を変えることも可能である。加工種としては、例えば、押抜き加工、スエージ加工等が採用される。また、各加工は１回で行う他に複数パスで行ってもよく、１回以上の回数で適宜のパス数が選択される。なお、加工を温間加工で行う際には、通常は４００〜６００℃の温度範囲内で行う。
【０００９】
なお、本系合金で最良の性能が得られる時の例えば引張り破壊形態は、Ｗ粒のへき開破壊とマトリックス相の延性破壊（デインプル模様を呈す）の混在である。
加工強化後、Ｗ粒の硬さを加工強化前の硬さまで落とさず、かつマトリックス相を加工強化前の硬さレベルまで落ちるような条件を選定して中間熱処理を施した後、再加工強化を施すことにより、マトリックス相は、その再加工強化の分だけ強化し、それに応じた十分な延性を受けもつと同時に、Ｗ粒の方は、再加工強化前の状態で既に強化されているため、その分だけ強度が増加する。
その結果、主として引張強さはＷ粒の強度に支配され、引張り伸び（延性）はマトリックス相の延性に支配されることから、常法に比べて、同じ延性レベルで比較すると高強度となり、見方を変えて、同じ強度レベルで比較すると高延性になる。本発明者らは従来例と異なる図３に示す工程手順を採用することにより、優れた強度および延性が確保されることを見出しており、さらには、以下の条件を定めることにより上記作用がより有効に得られることも見い出している。
【００１０】
［各条件限定理由］
（１）加工強化の加工率（８〜１４％）
加工強化時に８％以上の加工率を与えないと、Ｗ粒に十分な加工強化を与えられず、以降の工程の効果が十分に得られない。また、加工率が１４％を越えると、Ｗ粒の変形が大きくなり過ぎて十分な延性が得られなくなる。
以上の理由で加工強化の加工率を８〜１４％とするのが望ましく、同様の理由でさらに加工率の上限を１０％とするのが一層望ましい。
なお、本明細書では上記加工率は、被加工材の断面減少率を意味しており、以下に記述する加工率も全て同様である。
【００１１】
（２）中間熱処理温度（１０００〜１２００℃）
上記加工強化後、マトリックス相の硬さレベルを加工強化前と同等まで低下させるために、１０００℃以上を必要とし、かつＷ粒の硬さレベルを加工強化前より高いレベルに確保するために１２００℃以下であることが必要とされる。したがって、中間熱処理温度として１０００〜１２００℃が望ましいものとし、さらに同様の理由で１０５０〜１１５０℃を一層望ましいものとした。なお、上記作用を確実かつ効率的に得るためには、上記温度範囲における中間熱処理の処理時間を８〜１２時間とするのが望ましい。
【００１０】
（３）再加工強化の加工率（１６〜２２％）
被処理物の断面内の硬さ分布は、主に再加工強化時の加工率に支配される。したがって、被処理物の断面内が均一に加工され、結果として、硬さが分布を持たず均一になるためには再加工強化時の加工率を１６％以上にする必要がある。
また、再加工強化時の加工率が２２％を越えると、Ｗ粒の変形が大きくなり過ぎ、十分な延性が得られなくなる。
以上の理由で再加工強化の加工率を１６〜２２％とするのが望ましく、同様の理由でさらに加工率の下限を１８％、上限を２０％とするのが一層望ましい。
【００１１】
（４）加工強化と再加工強化の加工率の合計（３０％以下）
加工強化および再加工強化の加工率を上記範囲内に定めた場合でも、両者の合計が３０％を越えると、Ｗ粒への変形力が大きくなり、上記と同様にＷ粒の変形が大きくなって延性が低下する傾向がある。このため、それぞれの加工率の規定に加え、両者の合計を３０％以下とするのが望ましい。
【００１２】
（５）後熱処理
再加工強化後の合金のままでは、その機械的性質のバラツキが大きいため、このバラツキをなくし、適切な強度と延性のバランスが得られるように、再加工強化後、後熱処理を施す。なお、上記作用を得るためには、後熱処理温度を３５０℃以上とするのが望ましく、一方、１０００℃を越えると、強度が低下するため、後熱処理温度は、目的の強度レベル、延性レベルに応じて３５０〜１０００℃の範囲内で選択するのが望ましい。また、後熱処理による作用を十分かつ効率的に得るために、処理時間は８〜１２時間とするのが望ましい。
なお、高強度側を狙う場合に、強度と延性のバランスが最も良いのは３５０〜４５０℃の温度域で後熱処理を行う場合である。上記温度範囲での後熱処理は、例えば、１３０ｋｇｆ／ｍｍ2以上の強度を必要とする場合に有効であり、この場合にも１０％以上の延性（引張伸び）が確保される。
また、低強度側でかつ延性の高いレベルを狙う場合に、強度と延性のバランスが最も良いのは８００〜１０００℃の温度域で後熱処理を行う場合である。この温度範囲での加熱は、例えば１７％以上（引張伸び）の延性を必要とする場合に有効であり、この場合にも１０４〜１２８ｋｇｆ／ｍｍ2の強度が確保される。
【００１３】
【発明の実施の形態】
以下に本発明の一実施形態を図１のフローチャートを用いて説明する。
常法により製造した平均粒径約５μｍのＷ粉末９３重量％と、平均粒径約５μｍのＮｉおよびＦｅ粉末７重量％（ただし、Ｎｉ：Ｆｅ重量比が７／３）とを混合し（工程Ｐ１）、これを所定形状のゴム袋に充填して、静水圧成型によって圧縮して、５０ｍｍ径の棒状圧粉体を得る（工程Ｐ２）。この圧粉体には必要に応じて機械加工を施し、次いで、予備焼結（工程Ｐ３）、本焼結（工程Ｐ４）を行う。
予備焼結は、圧粉体を１３００〜１４００℃に加熱し、４時間保持することにより行い、本焼結は、予備焼結後の圧粉体を１４６０〜１５５０℃に加熱し、１時間保持して行う。得られた焼結体には、１１００℃×１０時間の熱処理を行い（工程Ｐ５）、その後、必要な機削りを冷間で行う（工程Ｐ６）。
その後、本発明における加工強化法として押抜き加工を加工率８〜１４％の範囲内で実施し（工程Ｐ７）、その後、１０００〜１２００℃の範囲内の温度で中間熱処理を施し（工程Ｐ８）、さらに再加工強化法として、加工率１６〜２２％の範囲内でスエージング加工を行い（工程Ｐ９）、その後、最後に３５０〜１０００℃の範囲内の温度で後熱処理を施す（工程Ｐ１０）。
【００１４】
【実施例】
上記実施形態に示す焼結体を使用して、加工強化および再加工強化の加工率と、中間熱処理および後熱処理の温度、時間を表１に示す条件に選定し、上記実施形態と同様の手順により本発明の試験材（発明材）を得た。また、比較のため、加工強化した後、直ちに後熱処理を行ったもの（従来材に相当）と、上記加工率等の条件を発明の範囲外としたものを比較材として用意した。
上記により得られた発明材および比較材について引張試験を行い、その引張強度と引張伸びを表１に合わせた示した。また、これら数値を両者の関係において図２に示した。
【００１５】
【表１】
表１及び図２から明らかなように、本発明材は、比較材に比べて強度、伸びが高い傾向を有しており、例えば、同一強度であれば、本発明材は比較材よりも高い伸び（延性）を示し、同一の伸びであれば、本発明材は比較材よりも高い強度を示している。したがって、本発明法によれば、タングステン合金の強度、延性が優れ、かつ両者が良好にバランスしていることが明らかになっている。
【００１７】
【発明の効果】
以上説明したように、本発明の高強度高延性タングステン合金の製造方法によれば、Ｗを重量％で８５〜９８％含有し、残部がＮｉ，Ｆｅを主成分としたタングステン合金に、加工強化・中間熱処理・再加工強化・後熱処理の処理を与えるので、高い強度が得られるとともに良好な延性が確保され、高強度高延性のタングステン合金が得られる。
【００１８】
また、加工強化を加工率（断面減少率）８〜１４％とした冷間または温間加工により与え、かつ該加工強化後の中間熱処理温度を１０００〜１２００℃とし、さらに再加工強化を加工率（断面減少率）１６〜２２％とした冷間または温間加工により与え、かつ該再加工強化後に後熱処理を施せば、上記効果がより確実になり、またその効果も増大する。
さらに、加工強化と再加工強化の加工率（断面減少率）の合計を３０％以下とすれば、良好な延性をより確実に確保することができる。
【図面の簡単な説明】
【図１】 本発明の一実施形態におけるフローチャートを示す図である。
【図２】 同じく実施例における引張強さと引張伸びを示すグラフである。
【図３】 本発明法および従来法の概略フローチャートを示す図である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a high-strength and highly ductile tungsten alloy that can increase the strength of a tungsten alloy and obtain good ductility.
[0002]
[Background Art and Problems to be Solved by the Invention]
W-Fe-Ni alloys are used in various applications as materials having high strength and high ductility by utilizing the properties of tungsten. This alloy is usually prepared by mixing and mixing 85-98% by weight of tungsten and the balance of Ni and Fe, the balance being binder, and then forming the molded body by CIP (cold isotropic processing press) or the like. It is manufactured by heating and sintering above the liquidus temperature of the binder. Depending on the application, as shown in FIG. 3, in order to further improve the strength, the sintered alloy is subjected to cold or warm work strengthening such as swaging, and further subjected to post heat treatment if desired. ing.
[0003]
However, in the above method, although the strength can be increased, the ductility is greatly reduced. Therefore, in applications in which good ductility is required in addition to high strength, the alloy subjected to the above treatment is a mechanical property. There is a problem of being insufficient.
The present invention has been made against the background of the above circumstances, and an object of the present invention is to provide a method for producing a high-strength, high-ductility tungsten alloy from which a tungsten alloy excellent in both strength and ductility can be obtained.
[0004]
Of the present invention for solving the above problems, the method of producing a high strength and high ductility tungsten alloy of the first invention, a W containing 85 to 98% by weight, the balance being Ni, the tungsten alloy is Fe, Work strengthening is provided by cold working or warm working with a working rate (cross-sectional reduction rate) of 8 to 14%, intermediate heat treatment is applied at a temperature of 1000 to 1200 ° C. after the working strengthening, and a working rate (cross-sectional reduction rate) of 16 It is characterized in that rework strengthening is given by cold or warm working to -22%, and post heat treatment is performed after the rework strengthening.
Furthermore, the method for producing a high-strength, high-ductility tungsten alloy according to the second invention is characterized in that, in the second invention, the sum of the processing rates (cross-sectional reduction rate) of work strengthening and rework strengthening is 30% or less. To do.
[0007]
Incidentally, tungsten alloy to which the present invention is applied, usually it is offered as a sintered body, to prepare a molded body by each component powder or alloy powder is obtained by sintering the same. As the powder used at this time, for example, both W powder and other component powders are preferably 3 to 5 μm. This makes it possible to obtain excellent strength and ductility. However, the process up to obtaining the tungsten alloy subjected to the above-described work strengthening including the sintered body can be selected as appropriate, and the content thereof is not particularly limited as the present invention.
[0008]
Next, in the processing strengthening and rework strengthening given to the tungsten alloy, the type of processing is not particularly limited, and it is also possible to change the type of processing in processing strengthening and rework strengthening. As the processing type, for example, punching processing, swaging processing, or the like is employed. In addition, each processing may be performed by a plurality of passes in addition to one, and an appropriate number of passes is selected by one or more times. In addition, when processing by warm processing, it is normally performed within the temperature range of 400-600 degreeC.
[0009]
For example, the tensile fracture mode when the best performance is obtained with this alloy is a mixture of cleavage fracture of W grains and ductile fracture of matrix phase (showing a dimple pattern).
After processing strengthening, select a condition that does not reduce the hardness of the W grains to the hardness before processing strengthening and lower the matrix phase to the hardness level before processing strengthening, and after applying intermediate heat treatment, rework strengthening By applying, the matrix phase is strengthened by the amount of the rework strengthening and receives sufficient ductility accordingly. At the same time, the W grains are already strengthened in the state before the rework strengthening, The strength increases accordingly.
As a result, the tensile strength is mainly governed by the strength of the W grains, and the tensile elongation (ductility) is governed by the ductility of the matrix phase. When compared at the same strength level, high ductility is achieved. The present inventors have found that by adopting the process procedure shown in FIG. 3 different from the conventional example, excellent strength and ductility are ensured. It has also been found that it can be obtained effectively.
[0010]
[Reason for limitation of each condition]
(1) Processing rate of processing reinforcement (8-14%)
If the processing rate of 8% or more is not given at the time of processing strengthening, sufficient processing strengthening cannot be given to the W grains, and the effects of the subsequent steps cannot be sufficiently obtained. On the other hand, when the processing rate exceeds 14%, the deformation of the W grains becomes too large and sufficient ductility cannot be obtained.
For the above reason, it is desirable to set the processing rate of processing strengthening to 8 to 14%, and it is more desirable to further set the upper limit of the processing rate to 10% for the same reason.
In the present specification, the processing rate means the cross-sectional reduction rate of the workpiece, and the processing rates described below are all the same.
[0011]
(2) Intermediate heat treatment temperature (1000-1200 ° C)
In order to reduce the hardness level of the matrix phase to the same level as that before the processing strengthening after the processing strengthening, 1200 ° C. or higher is required, and 1200 in order to secure the hardness level of the W grains higher than that before the processing strengthening. It is necessary that the temperature be below ℃. Accordingly, the intermediate heat treatment temperature is preferably 1000 to 1200 ° C, and more preferably 1050 to 1150 ° C for the same reason. In order to obtain the above action reliably and efficiently, it is desirable that the processing time of the intermediate heat treatment in the above temperature range is 8 to 12 hours.
[0010]
(3) Processing rate of rework strengthening (16-22%)
The hardness distribution in the cross section of the workpiece is mainly governed by the processing rate at the time of rework strengthening. Therefore, in order for the cross section of the workpiece to be processed uniformly and, as a result, the hardness to be uniform without distribution, the processing rate at the time of rework strengthening needs to be 16% or more.
On the other hand, if the processing rate at the time of rework strengthening exceeds 22%, the deformation of W grains becomes too large and sufficient ductility cannot be obtained.
For the above reasons, it is desirable to set the processing rate for rework strengthening to 16 to 22%, and for the same reason, it is more desirable to set the lower limit of the processing rate to 18% and the upper limit to 20%.
[0011]
(4) Total of processing rate of processing strengthening and rework strengthening (30% or less)
Even when the processing rate of processing strengthening and rework strengthening is set within the above range, if the total of both exceeds 30%, the deformation force to W grains increases, and the deformation of W grains increases as described above. Therefore, the ductility tends to decrease. For this reason, in addition to the regulation of each processing rate, it is desirable that the total of both be 30% or less.
[0012]
(5) The post-heat treatment re-strengthened alloy has a large variation in its mechanical properties, so that this variation is eliminated and an appropriate balance between strength and ductility is obtained. Apply. In order to obtain the above action, it is desirable to set the post-heat treatment temperature to 350 ° C. or higher. On the other hand, if it exceeds 1000 ° C., the strength decreases, so the post-heat treatment temperature is set to the target strength level and ductility level. Accordingly, it is desirable to select within a range of 350 to 1000 ° C. Moreover, in order to obtain the effect | action by post-heat processing fully and efficiently, it is desirable that processing time is 8 to 12 hours.
When aiming at the high strength side, the best balance between strength and ductility is when post-heat treatment is performed in the temperature range of 350 to 450 ° C. The post heat treatment in the above temperature range is effective when, for example, a strength of 130 kgf / mm 2 or more is required, and in this case, a ductility (tensile elongation) of 10% or more is ensured.
Further, when aiming at a low strength side and a high ductility level, the balance between strength and ductility is best when post-heat treatment is performed in a temperature range of 800 to 1000 ° C. Heating in this temperature range is effective, for example, when ductility of 17% or more (tensile elongation) is required, and in this case as well, a strength of 104 to 128 kgf / mm 2 is ensured.
[0013]
DETAILED DESCRIPTION OF THE INVENTION
An embodiment of the present invention will be described below with reference to the flowchart of FIG.
93 wt% of W powder having an average particle diameter of about 5 μm produced by a conventional method and 7 wt% of Ni and Fe powder having an average particle diameter of about 5 μm (where Ni: Fe weight ratio is 7/3) are mixed (process) P1), filling this into a rubber bag of a predetermined shape and compressing it by isostatic pressing to obtain a 50 mm diameter rod-shaped green compact (step P2). The green compact is machined as necessary, and then pre-sintering (process P3) and main sintering (process P4) are performed.
Pre-sintering is performed by heating the green compact to 1300 to 1400 ° C. and holding for 4 hours. In this sintering, the green compact after pre-sintering is heated to 1460 to 1550 ° C. and held for 1 hour. And do it. The obtained sintered body is heat-treated at 1100 ° C. for 10 hours (process P5), and then necessary machining is performed cold (process P6).
Thereafter, punching is performed within the range of 8 to 14% as a processing strengthening method in the present invention (step P7), and then an intermediate heat treatment is performed at a temperature within the range of 1000 to 1200 ° C. (step P8). Further, as a rework strengthening method, swaging is performed within a processing rate of 16 to 22% (step P9), and then a post heat treatment is finally performed at a temperature within a range of 350 to 1000 ° C. (step P10). .
[0014]
【Example】
Using the sintered body shown in the above embodiment, the processing rate of work strengthening and rework strengthening, the temperature and time of intermediate heat treatment and post heat treatment are selected in the conditions shown in Table 1, and the same procedure as in the above embodiment Thus, a test material (invention material) of the present invention was obtained. For comparison, a comparative material was prepared which was subjected to post-heat treatment immediately after work strengthening (corresponding to a conventional material) and a material whose processing rate and other conditions were outside the scope of the invention.
A tensile test was performed on the inventive material and the comparative material obtained as described above, and the tensile strength and tensile elongation thereof are shown in Table 1. Also, these numerical values are shown in FIG.
[0015]
[Table 1]
As is clear from Table 1 and FIG. 2, the material of the present invention tends to have higher strength and elongation than the comparative material. For example, if the strength is the same, the material of the present invention is higher than the comparative material. If it shows elongation (ductility) and is the same elongation, the material of the present invention shows higher strength than the comparative material. Therefore, according to the method of the present invention, it has been clarified that the strength and ductility of the tungsten alloy are excellent and both are well balanced.
[0017]
【The invention's effect】
As described above, according to the method for producing a high-strength and high-ductility tungsten alloy of the present invention, a tungsten alloy containing 85 to 98% by weight of W and the balance of Ni and Fe as main components is processed and strengthened. -Since intermediate heat treatment, rework strengthening, and post heat treatment are provided, high strength is obtained, good ductility is ensured, and a high strength and high ductility tungsten alloy is obtained.
[0018]
Further, the processing strengthening is given by cold or warm processing with a processing rate (cross-sectional reduction rate) of 8 to 14%, the intermediate heat treatment temperature after the processing strengthening is set to 1000 to 1200 ° C., and the rework strengthening is further performed at the processing rate. (Cross-section reduction rate) If given by cold or warm working of 16 to 22%, and if post-heat treatment is performed after the rework strengthening, the above effect becomes more reliable, and the effect also increases.
Furthermore, if the sum of the processing rates (cross-sectional reduction rate) of processing strengthening and rework strengthening is 30% or less, good ductility can be ensured more reliably.
[Brief description of the drawings]
FIG. 1 is a diagram illustrating a flowchart according to an embodiment of the present invention.
FIG. 2 is a graph showing tensile strength and tensile elongation in the example.
FIG. 3 is a diagram showing a schematic flowchart of the method of the present invention and the conventional method.
Claims (2)
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| JP03442297A JP3665169B2 (en) | 1997-02-03 | 1997-02-03 | Manufacturing method of high strength and high ductility tungsten alloy |
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| JP03442297A JP3665169B2 (en) | 1997-02-03 | 1997-02-03 | Manufacturing method of high strength and high ductility tungsten alloy |
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| JPH10219414A JPH10219414A (en) | 1998-08-18 |
| JP3665169B2 true JP3665169B2 (en) | 2005-06-29 |
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| CN115478236B (en) * | 2022-08-30 | 2023-02-28 | 广州市华司特合金制品有限公司 | Heat treatment method of high specific gravity tungsten alloy |
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