JP6738010B2 - Nickel-based alloy with excellent high-temperature strength and high-temperature creep properties - Google Patents
Nickel-based alloy with excellent high-temperature strength and high-temperature creep properties Download PDFInfo
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本発明は、自動車用エンジン部品、特に排気バルブ等の高温雰囲気下で用いられるニッケル基合金に関する。 The present invention relates to an automobile engine component, particularly a nickel-base alloy used in a high temperature atmosphere such as an exhaust valve.
近年、自動車の燃費向上の進展には目覚しいものがあり、例えば自動車エンジンを従来よりも一回り小型化かつ軽量化し、不足する出力はターボチャージャーを組み合わせることで、その不足分の出力を補う省燃費ターボが主流になりつつある。 In recent years, there has been remarkable progress in improving fuel efficiency of automobiles.For example, by reducing the size and weight of automobile engines by a smaller amount than before, and combining the insufficient output with a turbocharger, the fuel saving to compensate for the insufficient output is achieved. Turbo is becoming mainstream.
そのような自動車用エンジン部品に用いられる材料として、例えば特許文献１では重量％で０．０１〜０．１％Ｃ、０〜０．５％Ｓｉ、０〜０．５％Ｍｎ、２３％を超えて２５％以下のＣｒ、０．５〜１．５％Ｎｂ、２．０〜３．０％Ｔｉ、１．０〜２．０％Ａｌ、４５％を超えて５０％以下のＮｉ、０．１〜１．２％Ｃｕ、０．３〜２．０％Ｗ等から構成されるニッケル基合金が開示されている。当該ニッケル基合金は、９００℃における高温引張強度に優れていること、および８００℃での長時間時効処理後でも高硬度が得られることから弁用耐熱合金として有用であることが説明されている。 As a material used for such an automobile engine part, for example, in Patent Document 1, 0.01 to 0.1% C, 0 to 0.5% Si, 0 to 0.5% Mn, and 23% by weight are used. More than 25% Cr, 0.5-1.5% Nb, 2.0-3.0% Ti, 1.0-2.0% Al, more than 45% and 50% Ni, 0 A nickel-based alloy composed of 0.1 to 1.2% Cu, 0.3 to 2.0% W, etc. is disclosed. It is described that the nickel-based alloy is useful as a heat-resistant alloy for valves because it has excellent high-temperature tensile strength at 900° C. and high hardness even after long-term aging treatment at 800° C. ..
また、特許文献２には、重量％で４０〜４９％Ｎｉ、１．２〜１．８％Ａｌ、２．０〜３．０％Ｔｉ、０．９〜７．８％Ｎｂ、１％以下のＭｏ等から構成されるニッケル基合金が開示されている。当該ニッケル基合金は、耐食性および耐摩耗性に優れていることから ディーゼルエンジン部品（特に排気バルブ部品）として有用であることが説明されている。 In addition, in Patent Document 2, 40 to 49% Ni, 1.2 to 1.8% Al, 2.0 to 3.0% Ti, 0.9 to 7.8% Nb, and 1% or less by weight%. A nickel-based alloy composed of Mo or the like is disclosed. It is described that the nickel-based alloy is useful as a diesel engine part (particularly, an exhaust valve part) because it has excellent corrosion resistance and wear resistance.
しかし、特許文献１のニッケル基合金では８００℃雰囲気下で３００時間という長時間の時効処理後でも一定の高硬度（例えば、ロックウェルのＣスケールでＨＲＣ３８〜３９）を保持していることは説明されているが、その高硬度が得られるまでに必要な時効処理の時間が比較的に長くなるという問題があった。 However, it is explained that the nickel-based alloy of Patent Document 1 maintains a certain high hardness (for example, HRC 38 to 39 on the Rockwell C scale) even after a long time aging treatment of 800 hours in an atmosphere of 800°C. However, there is a problem that the aging treatment time required until the high hardness is obtained is relatively long.
また、特許文献２のニッケル基合金も同様に８００℃近傍の時効処理を行うことでも高硬度（例えば、ロックウェルのＣスケールでＨＲＣ２７〜２８）が得られることが説明されているが、その高硬度が得られるまでに必要な時効処理の時間が比較的に長いという問題があった。 Further, it is described that the nickel-based alloy of Patent Document 2 can also obtain high hardness (for example, HRC27 to 28 on the Rockwell C scale) by similarly performing an aging treatment at around 800° C., which is high. There is a problem that the aging time required for obtaining hardness is relatively long.
さらに、上述したように自動車エンジンの小型化、軽量化に伴い、自動車用エンジンの排気ガス温度が９００〜１０００℃近傍に達する場合もあり、特許文献１および２に記載のニッケル基合金では高温強度や高温クリープ特性が不足するという問題があった。 Further, as described above, with the downsizing and weight reduction of the automobile engine, the exhaust gas temperature of the automobile engine may reach around 900 to 1000° C., and the nickel-based alloys described in Patent Documents 1 and 2 have high-temperature strength. There was a problem that the high temperature creep property was insufficient.
そこで、本発明においては従来のニッケル基合金に比べて、９００℃以上の温度域における高温強度に優れたニッケル基合金を提供することを課題とする。 Therefore, it is an object of the present invention to provide a nickel-base alloy that is superior in high temperature strength in a temperature range of 900° C. or higher as compared with the conventional nickel-base alloy.
前述した課題を解決するために、本発明に係るニッケル基合金は、重量％で、０．０１〜０．０５％Ｃ、０．１〜０．５％Ｓｉ、０．１〜０．５％Ｍｎ、０．００１〜０．０１％Ｂ、２１％Ｃｒ、０．７〜１．３％Ｎｂ、２．０〜３．２％Ｔｉ、１．２〜２．２％Ａｌ、５１％Ｎｉ、０．３〜１．０％Ｃｕ、２．５％Ｍｏ、１．０〜２．０％Ｗを含有し、残部がＦｅおよび不可避不純物からなるニッケル基合金とした。 In order to solve the above-described problems, the nickel-based alloy according to the present invention has a weight percentage of 0.01 to 0.05% C, 0.1 to 0.5% Si, and 0.1 to 0.5%. Mn, 0.001 to 0.01% B, 21% Cr , 0.7 to 1.3% Nb, 2.0 to 3.2% Ti, 1.2 to 2.2% Al, 51% Ni , A nickel-based alloy containing 0.3 to 1.0% Cu, 2.5% Mo , 1.0 to 2.0% W, and the balance being Fe and inevitable impurities was prepared.
また、本発明に係るニッケル基合金は、Ｔｉの含有量とＡｌの含有量との総和を重量％で４．０％以上とした。 In addition, in the nickel-based alloy according to the present invention , the total of the content of Ti and the content of Al is set to 4.0% or more by weight % .
本発明に係るニッケル基合金は、前述した従来のニッケル基合金に比べて、９００℃以上の高温雰囲気における引張強度が向上するという効果を奏する。また、本発明に係るニッケル基合金においては、優れた高温クリープ特性を有することができる。したがって、本発明に係るニッケル基合金は９００℃以上の高温雰囲気下に長時間晒される自動車用排気バルブ部品には好適である。 INDUSTRIAL APPLICABILITY The nickel-based alloy according to the present invention has an effect of improving the tensile strength in a high temperature atmosphere of 900° C. or higher as compared with the above-mentioned conventional nickel-based alloy. Further, the nickel-based alloy according to the present invention can have excellent high temperature creep properties. Therefore, the nickel-based alloy according to the present invention is suitable for automobile exhaust valve parts that are exposed to a high temperature atmosphere of 900° C. or higher for a long time.
本発明の実施の形態の一例について説明する。本発明に係るニッケル基合金を構成する成分およびその成分範囲を限定した理由について、以下に詳しく説明する。 An example of the embodiment of the present invention will be described. The components constituting the nickel-based alloy according to the present invention and the reasons for limiting the component range will be described in detail below.
Ｃ（炭素）の含有量は、０．０１〜０．０５重量％とする。Ｃは、Ｔｉ、Ｎｂ及びＣｒと結合して炭化物を形成し、高温強度を改善する。このような効果を得るためには、少なくとも、０.０１重量％以上の添加が必要である。しかし、過剰に添加すると、ＭＣ炭化物を多量に生成して、熱間加工性を低下させるため、上限を０．０５重量％とした。 The content of C (carbon) is 0.01 to 0.05% by weight. C combines with Ti, Nb and Cr to form a carbide, which improves the high temperature strength. In order to obtain such effects, it is necessary to add at least 0.01% by weight. However, if added excessively, a large amount of MC carbides are generated and the hot workability is deteriorated, so the upper limit was made 0.05% by weight.
Ｓｉ（ケイ素）の含有量は、０．１〜０．５重量％とする。Ｓｉは、脱酸元素として添加される。また、適量の添加は耐酸化性を改善する。しかし、過剰に添加すると延性の低下をきたすため、上限を０．５重量％とした。 The content of Si (silicon) is 0.1 to 0.5% by weight. Si is added as a deoxidizing element. Further, addition of a proper amount improves the oxidation resistance. However, if added excessively, ductility is deteriorated, so the upper limit was made 0.5% by weight.
Ｍｎ（マンガン）の含有量は、０．１〜０．５重量％とする。ＭｎもＳｉと同様に脱酸元素として添加されるが、過剰に添加すると高温強度の低下をきたすため、上限を０．５重量％とした。 The content of Mn (manganese) is set to 0.1 to 0.5% by weight. Mn is also added as a deoxidizing element like Si, but if added excessively, the high temperature strength will be deteriorated, so the upper limit was made 0.5% by weight.
Ｂ（ホウ素）の含有量は、０．００１〜０．０１重量％とする。Ｂは、結晶粒界を強化してクリープ強度を高めるほか、熱間加工性を改善する効果を持つ。このため、０.００１重量％以上の添加が必要である。しかし、過剰に添加すると結晶粒界に低融点化合物を生成して熱間加工性を害するため、上限を０.０１重量％とした。 The content of B (boron) is 0.001 to 0.01% by weight. B has the effect of strengthening the grain boundaries to increase the creep strength and improving the hot workability. Therefore, it is necessary to add 0.001% by weight or more. However, if added excessively, a low melting point compound is generated at the crystal grain boundaries to impair the hot workability, so the upper limit was made 0.01% by weight.
Ｃｒ（クロム）の含有量は、２０．０〜２３．５重量％とする。Ｃｒは、耐酸化性および耐食性を向上するのに不可欠な元素である。また、ある程度添加した場合は、針状組織が成長して耐クリープ特性の向上が認められる。しかし、過剰添加した場合、針状組織が粗大化して性能劣化を招くため、２０．０〜２３．５重量％とした。 The content of Cr (chrome) is 20.0 to 23.5% by weight. Cr is an essential element for improving the oxidation resistance and the corrosion resistance. Further, when added to some extent, an acicular structure grows and improvement in creep resistance is recognized. However, when excessively added, the needle-like structure becomes coarse and performance is deteriorated, so the content was made 20.0 to 23.5% by weight.
Ｎｂ（ニオブ）の含有量は、０．７〜１．３重量％とする。Ｎｂは、Ｎｉ３（Ａｌ，Ｔｉ，Ｎｂ）などの金属間化合物相を析出し、高温強度を向上する。また、Ｃと結合して炭化物ＮｂＣを生成し、高温硬さおよび強度の向上に寄与する。ただし、過剰添加すると材料を脆化させるので、０．７〜１．３重量％とした。 The content of Nb (niobium) is 0.7 to 1.3% by weight. Nb precipitates an intermetallic compound phase such as Ni 3 (Al, Ti, Nb) and improves high temperature strength. Further, it combines with C to form a carbide NbC, which contributes to improvement in high temperature hardness and strength. However, if added excessively, the material becomes brittle, so it was set to 0.7 to 1.3% by weight.
Ｔｉ（チタン）の含有量は、２．０〜３．２重量％とする。Ｔｉは、Ｎｉと結合して金属間化合物γ’相を形成し、オーステナイト相を強化する。Ｔｉを増量すれば強化相であるγ’相の量は増加し、高温強度は向上する。しかし、過剰に添加すると、脆化相の析出をまねいてしまい、素材の熱間成形性を阻害するので、その添加範囲を２．０〜３．２重量％に限定した。 The content of Ti (titanium) is 2.0 to 3.2% by weight. Ti combines with Ni to form an intermetallic compound γ'phase and strengthens the austenite phase. If the amount of Ti is increased, the amount of the γ'phase, which is the strengthening phase, is increased, and the high temperature strength is improved. However, if added excessively, the embrittlement phase is precipitated and the hot formability of the raw material is impaired. Therefore, the addition range is limited to 2.0 to 3.2% by weight.
Ａｌ（アルミニウム）の含有量は、１．２〜２．２重量％とする。Ａｌは、Ｎｉと結合して金属間化合物γ’相を形成し、オーステナイト相を強化する重要な元素である。Ａｌを増量すれば強化相であるγ’相の量は増加し、高温強度は向上する。しかし、過剰に添加すると、強化相が不安定となり脆化相の析出をまねく。このため、素材の熱間成形性を阻害するので、その添加範囲を１．２〜２．２重量％に限定した。 The content of Al (aluminum) is 1.2 to 2.2% by weight. Al is an important element that combines with Ni to form an intermetallic compound γ'phase and strengthen the austenite phase. If the amount of Al is increased, the amount of the γ'phase which is the strengthening phase is increased and the high temperature strength is improved. However, if added excessively, the strengthening phase becomes unstable and the embrittlement phase is precipitated. Therefore, the hot formability of the raw material is impaired, so the addition range is limited to 1.2 to 2.2% by weight.
Ｎｉ（ニッケル）の含有量は、５０〜５３重量％とする。Ｎｉは、マトリックスであるオーステナイト基地を形成するため不可欠である。また、析出強化相であるγ’相を形成し、高温強度を向上させる。強化元素を固溶させるため、ある程度の量が必要であり、添加量の下限は５０重量％以上とした。ただし、過剰添加した場合、合金のコスト上昇を招き、また耐硫化腐食性が悪化するので、上限を５３重量％とした。 The content of Ni (nickel) is 50 to 53% by weight. Ni is essential for forming an austenite matrix that is a matrix. Further, it forms a γ'phase which is a precipitation strengthening phase and improves high temperature strength. A certain amount is required to form a solid solution with the strengthening element, and the lower limit of the amount added is 50% by weight or more. However, if added excessively, the cost of the alloy increases and the sulfidation corrosion resistance deteriorates, so the upper limit was made 53 wt %.
Ｃｕ（銅）の含有量は、０．３〜１．０重量％とする。Ｃｕは、硫化物系腐食の改善を目的として添加する。過剰添加した場合は熱間脆化を生じるため、その含有量を０．３〜１．０重量％に限定した。 The content of Cu (copper) is 0.3 to 1.0% by weight. Cu is added for the purpose of improving sulfide-based corrosion. When added excessively, hot embrittlement occurs, so the content was limited to 0.3 to 1.0% by weight.
Ｍｏ（モリブデン）の含有量は、１．５〜３．０重量％とする。Ｍｏは、熱間強度を達成する析出強化相が固溶する温度範囲において、固溶強化により高温強度および高温クリープ特性を向上させる元素である。１．５重量％未満の含有量では高温強度および高温クリープ特性を向上させる効果が発現せず、３．０重量％を超える含有量では熱間加工性に有害となるために含有量を限定した。 The content of Mo (molybdenum) is 1.5 to 3.0% by weight. Mo is an element that improves the high temperature strength and the high temperature creep properties by solid solution strengthening in the temperature range in which the precipitation strengthening phase that achieves hot strength is in solid solution. When the content is less than 1.5% by weight, the effect of improving the high temperature strength and the high temperature creep property is not exhibited, and when the content exceeds 3.0% by weight, it is harmful to the hot workability, so the content is limited. ..
Ｗ（タングステン）の含有量は、１．０〜２．０重量％とする。Ｗは、熱間強度を達成する析出強化相が固溶する温度範囲において、固溶強化により高温強度および高温クリープ特性を向上させる元素である。１．０重量％未満の含有量では高温強度および高温クリープ特性を向上させる効果が発現せず、２．０重量％を超える含有量では熱間加工性に有害となるために含有量の上限を限定した。 The content of W (tungsten) is 1.0 to 2.0% by weight. W is an element that improves the high temperature strength and the high temperature creep property by solid solution strengthening in the temperature range in which the precipitation strengthening phase that achieves hot strength is in solid solution. If the content is less than 1.0% by weight, the effect of improving the high temperature strength and the high temperature creep property is not exhibited, and if the content exceeds 2.0% by weight, it becomes harmful to the hot workability, so the upper limit of the content is set. Limited
本発明に係るニッケル基合金（以下、本発明材という）および従来のニッケル基合金（以下、従来材という）を用いて、高温における引張試験を行ったので、その試験結果について説明する。本試験において、本発明材および従来材共に真空溶解炉で原材料を溶解させて鋼塊を作製し、１０５０℃で１時間の溶体化処理した後、水冷したものを用いた。試験片については、その鋼塊から直径１６ｍｍ、高さ１５ｍｍの円柱状の試験片を作製して、時効処理を行った。 A tensile test at high temperature was performed using the nickel-based alloy according to the present invention (hereinafter referred to as the present invention material) and the conventional nickel-based alloy (hereinafter referred to as the conventional material). The test results will be described. In this test, raw materials were melted in a vacuum melting furnace for both the material of the present invention and a conventional material to prepare a steel ingot, which was solution-treated at 1050° C. for 1 hour and then water-cooled. As for the test piece, a cylindrical test piece having a diameter of 16 mm and a height of 15 mm was prepared from the steel ingot and subjected to an aging treatment.
時効処理の条件については、時効温度は７５０℃、時効時間については４時間として行った。本実施例の本発明材および従来材の化学組成を表１に示す。 The aging temperature was 750° C. and the aging time was 4 hours. Table 1 shows the chemical compositions of the material of the present invention and the conventional material of this example.
使用した試験片は、平行部が直径６ｍｍ、長さ２５ｍｍとなるように、前述の鋼塊から作製した直径１６ｍｍの圧延材より切削加工して製作した。試験条件は、室温、８００℃および９００℃の計３水準の雰囲気に試験片を２０分間均熱保持した後、引張速度２ｍｍ／ｍｉｎで引張試験を行い、試験片が破断する際の強度（引張強度：単位ＭＰａ）、０．２％耐力（単位：ＭＰａ）、伸び（単位：％）および絞り（単位：％）をそれぞれ測定した。本発明材および従来材の室温、８００℃および９００℃における引張強度などの諸特性を表２〜４に示す。 The test piece used was manufactured by cutting from a rolled material having a diameter of 16 mm prepared from the above steel ingot so that the parallel part had a diameter of 6 mm and a length of 25 mm. The test conditions were as follows: the test piece was soaked and held in a total of three levels of atmosphere at room temperature, 800° C. and 900° C. for 20 minutes, and then a tensile test was performed at a pulling speed of 2 mm/min to determine the strength (tensile strength) at which the test piece broke. Strength: unit MPa), 0.2% proof stress (unit: MPa), elongation (unit: %) and drawing (unit: %) were measured. Tables 2 to 4 show various properties of the material of the present invention and the conventional material such as tensile strength at room temperature, 800°C and 900°C.
室温での引張強度は、表２に示すように本発明材は従来材に比べて引張強度および０．２％耐力ともにやや低い値となった。しかし、伸びおよび絞りについては本発明材の方が従来材に比べて、約４〜８倍の値を示す結果となった。 As shown in Table 2, the tensile strength at room temperature of the material of the present invention was slightly lower than that of the conventional material in both tensile strength and 0.2% proof stress. However, with respect to elongation and drawing, the material of the present invention has a result of showing about 4 to 8 times the value of the conventional material.
次に、８００℃における引張強度は、表３に示すように従来材が６６９ＭＰａであるのに対して、本発明材は６８９ＭＰａであり、本発明材は従来材と同等以上の引張強度であった。 Next, as shown in Table 3, the tensile strength at 800° C. of the conventional material was 669 MPa, whereas the inventive material was 689 MPa, and the inventive material had a tensile strength equal to or higher than that of the conventional material. ..
また、０．２％耐力については、本発明材が６４５ＭＰａであるのに対して、従来材は５９０ＭＰａであった。このことから、８００℃における本発明材の引張強度および０．２％耐力はともに従来材と同等以上の特性を有することがわかった。 Regarding the 0.2% proof stress, the material of the present invention was 645 MPa, whereas the conventional material was 590 MPa. From this, it was found that both the tensile strength and the 0.2% proof stress of the material of the present invention at 800° C. have characteristics equal to or higher than those of the conventional material.
また、９００℃における引張強度も表４に示すように従来材は３３６ＭＰａであったのに対して、本発明材は３９４ＭＰａであった。さらに、０．２％耐力については、本発明材が３９４ＭＰａであるのに対して、従来材は２６１ＭＰａであった。したがって、本発明材は、従来材に比べて８００〜９００℃までの高温雰囲気において優れた引張強度および０．２％耐力を示すことがわかった。 Further, as shown in Table 4, the tensile strength at 900° C. was 336 MPa for the conventional material and 394 MPa for the material of the present invention. Further, regarding the 0.2% proof stress, the material of the present invention was 394 MPa, whereas the conventional material was 261 MPa. Therefore, it was found that the material of the present invention exhibits superior tensile strength and 0.2% proof stress in a high temperature atmosphere of 800 to 900° C. as compared with the conventional material.
次に、表１に示す本発明材および従来材を用いて高温におけるクリープ試験を行い、試験片が破断するまでの時間を測定したので、その結果について説明する。使用した試験片は、前述の鋼塊を１０５０℃で溶体化処理して、引き続き７５０℃で４時間の条件で時効処理を施して、冷却後に試験片を作製した。 Next, the creep test at high temperature was performed using the present invention material and the conventional material shown in Table 1, and the time until the test piece was broken was measured. The results will be described. The used test piece was obtained by subjecting the steel ingot to solution treatment at 1050° C., followed by aging treatment at 750° C. for 4 hours, and producing a test piece after cooling.
試験片は、平行部の直径が６．４ｍｍになるように製作した。クリープ試験は、９００℃の高温雰囲気にて試験片に７０ＭＰａを負荷した状態で行い、試験片が破断するまでの時間を測定した。本発明材および従来材を用いて作製した試験片がクリープ破断するまでの時間（破断時間）、試験片の伸び（単位：％）および絞り（単位：％）を表５に示す。 The test piece was manufactured so that the diameter of the parallel portion was 6.4 mm. The creep test was performed in a high temperature atmosphere of 900° C. with a load of 70 MPa applied to the test piece, and the time until the test piece broke was measured. Table 5 shows the time (breaking time) until creep rupture, the elongation (unit: %), and the drawing (unit: %) of the test piece manufactured using the material of the present invention and the conventional material.
本発明材および従来材のクリープ破断時間は、表５に示すように従来材が１６０時間で破断したことに対して、本発明材の破断時間は２０６時間であり、従来材よりも約１．３倍のクリープ特性が得られた。また、試験片の伸びや絞りも同様に、従来材の伸びが２８％であるのに対して、本発明材の伸びは３６％であった。絞りは従来材が５９％であるのに対して、本発明材は３２％であった。以上の結果から、本発明材は、従来材よりも高温雰囲気で優れたクリープ特性を有していることがわかった。 Regarding the creep rupture time of the present invention material and the conventional material, as shown in Table 5, the conventional material ruptured in 160 hours, whereas the rupture time of the present invention material was 206 hours, which was about 1. A creep property of 3 times was obtained. Similarly, with respect to the elongation and drawing of the test piece, the elongation of the conventional material was 28%, whereas the elongation of the material of the present invention was 36%. The diaphragm was 32% for the material of the present invention, whereas the conventional material was 59%. From the above results, it was found that the material of the present invention has better creep characteristics in the high temperature atmosphere than the conventional material.
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