JPH0356289B2 - - Google Patents
Info
- Publication number
- JPH0356289B2 JPH0356289B2 JP62091971A JP9197187A JPH0356289B2 JP H0356289 B2 JPH0356289 B2 JP H0356289B2 JP 62091971 A JP62091971 A JP 62091971A JP 9197187 A JP9197187 A JP 9197187A JP H0356289 B2 JPH0356289 B2 JP H0356289B2
- Authority
- JP
- Japan
- Prior art keywords
- nickel
- bonding
- diffusion bonding
- phase
- alloy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 96
- 239000000956 alloy Substances 0.000 claims description 48
- 229910052759 nickel Inorganic materials 0.000 claims description 46
- 229910045601 alloy Inorganic materials 0.000 claims description 45
- 229910052782 aluminium Inorganic materials 0.000 claims description 32
- 238000009792 diffusion process Methods 0.000 claims description 31
- 229910052721 tungsten Inorganic materials 0.000 claims description 26
- 238000001816 cooling Methods 0.000 claims description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 20
- 229910000601 superalloy Inorganic materials 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 14
- 239000010937 tungsten Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 36
- 230000008018 melting Effects 0.000 description 16
- 238000002844 melting Methods 0.000 description 16
- 238000005304 joining Methods 0.000 description 12
- 239000010410 layer Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 230000007423 decrease Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 229910052796 boron Inorganic materials 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000009864 tensile test Methods 0.000 description 4
- 230000000881 depressing effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910001080 W alloy Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、高温部品用材料であるニツケル基超
合金の接合に用いる接合用合金の製造方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing a joining alloy used for joining nickel-based superalloys, which are materials for high-temperature parts.
ガスタービン動翼等の高温部品用材料であるニ
ツケル基超合金の接合技術が近年その重要性が高
まつている。
The importance of bonding technology for nickel-based superalloys, which are materials for high-temperature parts such as gas turbine rotor blades, has increased in recent years.
従来ニツケル基超合金の接合に関しては特開昭
47−33850号公報に記載の液相拡散接合が主に用
いられている。この接合方法は、ニツケル基超合
金である被接合物の接合面間に被接合物より融点
の低いNi−ＢあるいはNi−Ｂ−Ｘ系（ここでＸ
はNi、Ｂ以外の合金元素を示す）組成の合金薄
板、コーテイング層又はスパツタ層等を有する接
合用合金層を配置し、被接合物の有点より低く接
合用合金層の融点より高い温度範囲にて、接合応
力を与えて、真空中あるいは不活性ガス雰囲気中
等で被接合物を接合する方法である。 Regarding joining of conventional nickel-based superalloys, JP-A-Sho
Liquid phase diffusion bonding described in Japanese Patent No. 47-33850 is mainly used. This joining method uses Ni-B or Ni-B-X (here, X
(indicates an alloying element other than Ni or B), a bonding alloy layer having a coating layer, a sputter layer, etc. is placed, and the temperature range is lower than the point of the object to be bonded and higher than the melting point of the bonding alloy layer. In this method, bonding stress is applied to the objects to be bonded in a vacuum or an inert gas atmosphere.
この接合方法の特徴は接合用合金層にボロン等
の融点降下元素を含んだ低融点合金組成材を用い
ることにあり、接合時に接合用合金層を溶融する
とともに被接合物の接合界面を部分溶融させて接
合する。その結果として接合部分は被接合物より
融点の低い合金組成で形成されることになる。高
温強度と融点とは一般に比例する傾向があり、こ
の方法における接合部分の高温強度は被接合物よ
り弱くなつている。 The feature of this joining method is that a low melting point alloy composition containing melting point depressing elements such as boron is used for the joining alloy layer, which melts the joining alloy layer and partially melts the joining interface of the objects to be joined. and join. As a result, the joint portion is formed of an alloy composition having a lower melting point than the objects to be joined. High-temperature strength and melting point generally tend to be proportional, and the high-temperature strength of the bonded portion in this method is weaker than that of the objects to be bonded.
その対策として、接合後に熱処理を施し、接合
部の融点降下元素を接合母材全体に拡散させて接
合部分の融点降下元素料を少なくすることによつ
て接合部分の融点を上げることが提案されてい
る。 As a countermeasure, it has been proposed to increase the melting point of the joint by applying heat treatment after joining and diffusing the melting point depressing element in the joint into the entire joining base material, thereby reducing the amount of the melting point depressing element in the joint. There is.
しかしこの方法に於ける接合用合金層は、融点
を降下させる必要があるためボロンやシリコン等
の合金元素を必ず含む必要がある。また、ニツケ
ル基超合金において高温強度を高めるのに最も重
要なアルミニウムやアルミニウムと同様の効果が
あるチタン、ニオビウム、タンタル等の合金は、
接合用合金層の融点を高めるという理由で接合用
合金層には実質的に含めることができない。 However, the bonding alloy layer in this method must necessarily contain an alloying element such as boron or silicon because it is necessary to lower the melting point. In addition, alloys such as aluminum, titanium, niobium, and tantalum, which have the same effect as aluminum, are the most important for increasing high-temperature strength in nickel-based superalloys.
It cannot be substantially included in the bonding alloy layer because it increases the melting point of the bonding alloy layer.
その結果、接合用合金層はボロンやシリコンの
添加により融点を下げることと、高温強度向上に
必要な元素を含んでいないことにより接合部の高
温強度が低下するという問題があつた。 As a result, the bonding alloy layer has a problem in that the melting point is lowered by adding boron or silicon, and the high-temperature strength of the bonded portion is reduced because it does not contain elements necessary for improving high-temperature strength.
さらに、一製品において接合面積が多くある場
合、ボロン等を多く含んだ接合用合金層を多量用
いることになるため、ボロン等の融点降下元素が
製品使用中に製品全体に拡散していき、製品の中
に含まれるボロン等の平均濃度を高める。そのた
め製品を構成している材料の融点が下がり、製品
自体の高温強度を低下させるという問題もあつ
た。これらの問題の対策としては、被接合物の接
合界面に液相を生成しない固相拡散接合方法を適
用する必要がある。 Furthermore, if a product has a large bonding area, a large amount of bonding alloy layer containing a large amount of boron etc. will be used, so elements that lower the melting point such as boron will diffuse throughout the product during use. Increases the average concentration of boron, etc. contained in As a result, there was a problem in that the melting point of the materials constituting the product decreased and the high-temperature strength of the product itself decreased. As a countermeasure to these problems, it is necessary to apply a solid-phase diffusion bonding method that does not generate a liquid phase at the bonding interface of the objects to be bonded.
しかしながら、この固相拡散接合方法では被接
合物の接合面同志を直接、あるいは接合用合金層
を介して接触させ、原子面間に凝集力が働く距離
まで密着させる必要があり、そのためには大きな
接合応力を必要とするという問題があつた。 However, in this solid-phase diffusion bonding method, it is necessary to bring the surfaces of the objects to be bonded into contact with each other directly or through a bonding alloy layer, and to bring them into close contact with each other to a distance where a cohesive force is exerted between the atomic surfaces. There was a problem that bonding stress was required.
本発明の目的は、前記の問題点を解消し、ニツ
ケル基超合金の拡散接合時に高い接合応力を必要
としない拡散接合用ニツケル基合金の製造方法を
提供することにある。 SUMMARY OF THE INVENTION An object of the present invention is to provide a method for manufacturing a nickel-based alloy for diffusion bonding that eliminates the above-mentioned problems and does not require high bonding stress during diffusion bonding of a nickel-based superalloy.
本発明は、ニツケル基超合金からなる被接合物
の接合面間に挿入して拡散接合を行う拡散接合用
ニツケル基合金の製造方法において、アルミニウ
ム16〜22原子％、タングステン0.5〜５原子％及
び残部ニツケルからなる組成を有する溶湯を102
〓／秒以上の冷却速度で寒冷凝固させることを特
徴とする拡散接合用ニツケル基合金の製造方法に
ある。
The present invention provides a method for manufacturing a nickel-based alloy for diffusion bonding in which nickel-based superalloys are inserted between bonding surfaces of objects to be bonded to perform diffusion bonding. 10 2 molten metal with a composition of nickel
The present invention provides a method for producing a nickel-based alloy for diffusion bonding, which is characterized by cold-solidifying at a cooling rate of 0/sec or more.
拡散接合用ニツケル基合金に含まれるアルミニ
ウムは平衡相としてNi3Alの組成、L12構造を有
するガンマプライム相となつて析出し、高温強度
を強化する。
Aluminum contained in a nickel-based alloy for diffusion bonding precipitates as a gamma prime phase having a composition of Ni 3 Al and an L 12 structure as an equilibrium phase, thereby enhancing high-temperature strength.
しかし、アルミニウムを含有する拡散接合用ニ
ツケル基合金にタングステンを添加した溶融ニツ
ケル基合金を急速に冷却して凝固することにより
ニツケル基合金の結晶粒が微細になり、かつ非平
衡相を形成し前記ガンマプライマ相を析出させな
い。 However, by rapidly cooling and solidifying a molten nickel-based alloy containing aluminum and tungsten added to a nickel-based alloy for diffusion bonding, the crystal grains of the nickel-based alloy become fine and a non-equilibrium phase is formed. Prevents precipitation of gamma primer phase.
結晶粒が微細になることにより高温強度が低下
し、更に非平衡相を形成することから平衡相とし
てのガンマプライマ相を析出せず、そのため高温
強度が低下する。従つて、拡散接合用ニツケル基
合金の高温強度の低下は、拡散接合時の接合応力
を大巾に低下させる。 As the crystal grains become finer, the high-temperature strength decreases, and since a non-equilibrium phase is formed, the gamma primer phase as an equilibrium phase is not precipitated, resulting in a decrease in the high-temperature strength. Therefore, a decrease in the high temperature strength of the nickel-based alloy for diffusion bonding significantly reduces the bonding stress during diffusion bonding.
本発明の実施例では、拡散接合用ニツケル基合
金として、Ni−15at％〜22.5at％Al合金材とNi
−20at％Al−0.5〜5at％Ｗ合金材を試作し、試験
調査を行つた。
In the embodiment of the present invention, Ni-15at% to 22.5at%Al alloy material and Ni-based alloy material for diffusion bonding are used.
-20at%Al-0.5~5at%W alloy material was prototyped and tested and investigated.
合金の溶解は、所定の組成に配合した材料をア
ルゴンガス雰囲気下で溶解し、凝固は急速凝固法
の一種である双ロール法により、ロール周速15
ｍ／secの速度で回転している双ロール間に溶解
した合金を石英製ノズルから噴出させて凝固させ
た。 The alloy is melted by melting the materials blended to a predetermined composition in an argon gas atmosphere, and solidified by the twin roll method, which is a type of rapid solidification method, at a roll peripheral speed of 15.
The alloy melted between twin rolls rotating at a speed of m/sec was jetted from a quartz nozzle and solidified.
作成されたニツケル基合金は、巾10mm、厚さ
0.1mmの薄帯状の形状をしており、操作型顕微鏡
で合金組織中の二次デンドラアイトアーム間隔を
測定したところ0.5μｍ程度であり、102K／sec以
上の冷却速度で凝固していることが確認できた。 The nickel-based alloy created is 10mm wide and thick.
It has a thin strip shape of 0.1 mm, and when the distance between secondary dendrite arms in the alloy structure was measured using an operating microscope, it was about 0.5 μm, and it solidified at a cooling rate of 10 2 K/sec or more. I was able to confirm that there was.
拡散接合を行う場合は、上記の如くにして作成
されたニツケル基合金の薄帯をニツケル基超合金
である被接合物の接合面間に挿入し、１×
10-4Torr以下の高真空雰囲気下で、1000℃以上
の温度で拡散接合するのが好ましい。なおその時
の接合応力としては0.5〜3Kgf／mm2が適当な範囲
であり、その接合時間は0.5〜２時間で十分であ
る。 When performing diffusion bonding, the thin strip of nickel-based alloy prepared as described above is inserted between the joining surfaces of the nickel-based superalloy to be joined, and
Diffusion bonding is preferably performed at a temperature of 1000°C or higher in a high vacuum atmosphere of 10 -4 Torr or lower. Note that the bonding stress at this time is in an appropriate range of 0.5 to 3 Kgf/mm 2 , and the bonding time of 0.5 to 2 hours is sufficient.
上記の如く、本実施例で作成された拡散接合用
のニツケル基合金の高温強度について調査した結
果を第１図に示す。 As mentioned above, FIG. 1 shows the results of investigating the high temperature strength of the nickel-based alloy for diffusion bonding produced in this example.
第１図は引張り試験での歪速度を変化させて、
拡散接合時の接合温度領域である1100℃で高温引
張り試験を行つた場合の歪速度と最大真応力の関
係を示す。 Figure 1 shows that by changing the strain rate in the tensile test,
The relationship between strain rate and maximum true stress is shown when a high-temperature tensile test is conducted at 1100°C, which is the bonding temperature range during diffusion bonding.
まず、前記ニツケル基合金中のアルミニウムの
効果について説明すると、第１図に示すように、
Ni−17.5at％Al、Ni−20at％Alを102K／sec以上
の冷却速度で凝固させた材料の試験結果は商用ニ
ツケル基超合金であるRene80やIN738LCと同等
の最大真応力で表わされる応力で変形しているこ
とがわかる。前記の最大真応力は、引張試験にお
いて試験片の各瞬間の断面積でその時の外力を割
つた値、即ち真応力のうち最大の値を示すもの
で、最大真応力の低い程低い応力で変形すること
を表わす。 First, to explain the effect of aluminum in the nickel-based alloy, as shown in Figure 1,
Test results for materials made of Ni-17.5at%Al and Ni-20at%Al solidified at a cooling rate of 10 2 K/sec or higher are expressed in maximum true stress equivalent to commercial nickel-based superalloys Rene 80 and IN738LC. It can be seen that it is deformed due to stress. The maximum true stress mentioned above is the value obtained by dividing the external force at each moment by the cross-sectional area of the test piece at each instant in a tensile test, that is, the maximum value of the true stress.The lower the maximum true stress, the lower the stress. It means to do something.
Rene80やIN738LCに含まれているガンマプラ
イム相の量はアルミニウム量にして約15at％であ
ることから、それ以上のアルミニウム量にして高
温強度が更に高くなる組成にしても、102K／sec
以上の冷却速度で凝固させることにより低応力化
させることが出来ることがわかる。 Since the amount of gamma prime phase contained in Rene80 and IN738LC is approximately 15 at% in terms of aluminum content, even if the composition has a higher aluminum content and higher high-temperature strength, it will still yield 10 2 K/sec.
It can be seen that stress can be reduced by solidifying at the above cooling rate.
これは上記の冷却速度で凝固されたため結晶粒
が微細になり、そのため高温強度が低下したもの
である。結晶粒を微細化できるのはアルミニウム
量が16〜22at％の組成範囲であつて、ガンマプラ
イム相の量が64〜88vol％の範囲である。 This is because the crystal grains became fine because they were solidified at the above-mentioned cooling rate, resulting in a decrease in high-temperature strength. Crystal grains can be refined in a composition range in which the amount of aluminum is 16 to 22 at% and the amount of gamma prime phase is in a range of 64 to 88 vol%.
第４ａ図〜第４ｄ図に、ニツケルに、アルミニ
ウムを15〜22.5at％含んだものを102K／sec以上
の冷却速度で凝固し、接合温度に対応する1100℃
で30分間加熱した場合のミクロ組織を示すが、ア
ルミニウムが15at％と22.5at％のものでは結晶粒
が粗粒化していることが認められる。そのため、
第１図で示したNi−15at％Alの応力は、小さい
歪速度範囲ではRene80やIN738LCより高くなつ
ているのである。 Figures 4a to 4d show that nickel containing 15 to 22.5 at% aluminum is solidified at a cooling rate of 10 2 K/sec or higher to 1100°C, which corresponds to the bonding temperature.
The microstructures obtained when heated for 30 minutes are shown, and it can be seen that the crystal grains are coarser in those with aluminum content of 15 at% and 22.5 at%. Therefore,
The stress of Ni-15at%Al shown in Figure 1 is higher than that of Rene 80 and IN738LC in the small strain rate range.
一般にニツケル基超合金において強度、特に高
温強度に最も大きな効果を示すのはNi3Alで示さ
れ、L12構造をもつガンマプライム相である。 In general, in nickel-based superalloys, the gamma prime phase shown by Ni 3 Al, which has the L 12 structure, has the greatest effect on strength, especially high-temperature strength.
また、通常のニツケル基超合金ではガンマプラ
イム相が40〜80vol％含まれる。この量のガンマ
プライム量を形成するのに必要なアルミニウムは
10〜20at％となる。ニツケル基超合金では一般に
ガンマプライム相が多くなる程強度は高くなり、
そのためアルミニウム量が多くなる程強度上有利
となる。 In addition, normal nickel-based superalloys contain 40 to 80 vol% of gamma prime phase. The aluminum required to form this amount of gamma prime is
It will be 10~20at%. Generally speaking, the more gamma prime phase there is in a nickel-based superalloy, the higher its strength becomes.
Therefore, the greater the amount of aluminum, the more advantageous it becomes in terms of strength.
ニツケル基超合金の拡散接合を考える場合、被
接合物のアルミニウム量が10〜20at％であること
から、それより高いアルミニウム量として16〜
22at％を試験の対象範囲とした。その理由はアル
ミニウム量が16at％より少ない場合は接合部の高
温強度が低下するため接合部としては好ましくな
く、22at％よりも多い場合は接合部が脆くなる傾
向を有するからである。 When considering diffusion bonding of nickel-based superalloys, since the aluminum content of the material to be bonded is 10 to 20 at%, a higher aluminum content of 16 to 20 at% is considered.
The target range of the test was 22at%. The reason for this is that if the aluminum content is less than 16 at%, the high temperature strength of the joint will decrease, making it undesirable for the joint, while if it is more than 22 at%, the joint will tend to become brittle.
次に、ニツケル基合金中のタングステンの効果
について説明すると、第１図に示すように
102K／sec以上の冷却速度で凝縮したNi−20at％
Al−1at％Ｗは、Rene80やIN738LCと比べて試
験温度1100℃で1/5の応力で変形可能であり、ま
たタングステンを添加しないNi−20at％Alと比
べても約1/3以下で変形可能になつていることが
わかる。これはタングステン添加により非平衡相
が形成されたため大巾な応力低下が実現したもの
である。 Next, to explain the effect of tungsten in nickel-based alloys, as shown in Figure 1,
Ni−20at% condensed at a cooling rate of 10 2 K/sec or higher
Al-1at%W can be deformed with 1/5 stress at the test temperature of 1100℃ compared to Rene80 and IN738LC, and can be deformed with about 1/3 or less compared to Ni-20at%Al without tungsten added. I see that it is becoming possible. This is because a non-equilibrium phase was formed due to the addition of tungsten, resulting in a large stress reduction.
ニツケル基合金にタングステンを添加して
102K／sec以上の冷却速度で凝固させると非平衡
相が形成されることについて、第２図、第３ａ図
〜３ｄ図により説明する。 Adding tungsten to nickel-based alloy
The formation of a non-equilibrium phase when solidified at a cooling rate of 10 2 K/sec or more will be explained with reference to FIGS. 2 and 3a to 3d.
ニツケル基合金では、アルミニウムが含有され
ている場合Ni3Alで示されるガンマプライム相が
析出するが、通常5at％以上アルミニウムが含有
されている場合はＸ線回折でガンマプライム相の
ピークを認めることが出来る。なおＸ線回折は物
質にＸ線を通すとその物質の結晶によりＸ線が散
乱されて回折され、その干渉効果により回折Ｘ線
の強度が変化するという現象を応用して、試料を
回転させ異なつた角度で回折する回折Ｘ線の強度
を計測することにより特定物質の存在の有無を知
ることの出来る試験方法である。 In nickel-based alloys, if aluminum is contained, a gamma prime phase, indicated by Ni 3 Al, precipitates, but if aluminum is contained at 5 at% or more, a gamma prime phase peak can be observed in X-ray diffraction. I can do it. X-ray diffraction applies the phenomenon that when X-rays are passed through a substance, the X-rays are scattered and diffracted by the substance's crystals, and the intensity of the diffracted X-rays changes due to the interference effect. This is a test method that allows you to determine the presence or absence of a specific substance by measuring the intensity of diffracted X-rays diffracted at an angle.
第２図は冷却速度102K／sec以上で凝固したNi
−20at％Al材のＸ線回折結果であるが、ピーク
１で示した所（2θ＝24.8゜ガンマプライム相の固
有ピークが現れている。 Figure 2 shows Ni solidified at a cooling rate of 10 2 K/sec or higher.
The X-ray diffraction results for the -20 at% Al material show peak 1 (2θ = 24.8°, where the characteristic peak of the gamma prime phase appears).
それに対して、下記のいずれも冷却速度
102K／sec以上で凝固した、第３ａ図〜第３ｄ図
に示す、Ni−20at％Al−0.5at％Ｗ、Ni−20at％
WAl−1at％Ｗ、Ni−20at％Al−2at％Ｗおよび
Ni−20at％Al−5at％Ｗには、2θ＝24.8゜の所にガ
ンマプライム相の生成を示すピークが現われてい
ない。このことは上記のニツケル基合金にタング
ステンが添加されたことにより非平衡相が形成さ
れていることを意味している。 On the other hand, both of the following cooling rates
Ni-20at%Al-0.5at%W, Ni-20at% shown in Figures 3a to 3d solidified at 10 2 K/sec or higher
WAl-1at%W, Ni-20at%Al-2at%W and
In Ni-20at%Al-5at%W, no peak indicating the formation of gamma prime phase appears at 2θ=24.8°. This means that a non-equilibrium phase is formed due to the addition of tungsten to the above-mentioned nickel-based alloy.
このタングステン添加により冷却速度102K／
sec以上で凝固したNi−20at％Al1at％Ｗは第１
図に示すようにRene80やIN738LCと比べて1100
℃で約1/5の応力で変形可能であり、またタング
ステンを添加しないNi−20at％Alと比べても約
１／３以下で変形可能になつていることがわかる。 With this addition of tungsten, the cooling rate is 10 2 K/
Ni-20at%Al1at%W solidified at sec or more is the first
1100 compared to Rene80 and IN738LC as shown in the figure.
It can be seen that it can be deformed with about 1/5 of the stress at ℃, and can be deformed with about 1/3 or less of the stress compared to Ni-20at%Al which does not contain tungsten.
以上の如く、タングステンを添加したNi−
16at％〜22at％合金は、冷却速度102K／sec以上
で凝固させると非平衡相が形成され、アルミニウ
ムの含有量が高くて高温強度の高い組成材でもガ
ンマプライム相が形成されないため高温強度が極
めて低くなり、低い接合応力でニツケル基合金の
拡散接合が可能となる。なお、タングステン添加
により形成された非平衡相は接合後の熱処理で平
衡相に戻るが、その場合には平衡相として高強度
を示すようになる。 As mentioned above, tungsten-doped Ni−
When 16 at% to 22 at% alloys are solidified at a cooling rate of 10 2 K/sec or higher, a non-equilibrium phase is formed, and even in compositions with high aluminum content and high high temperature strength, no gamma prime phase is formed, resulting in low high temperature strength. becomes extremely low, making diffusion bonding of nickel-based alloys possible with low bonding stress. Note that the non-equilibrium phase formed by adding tungsten returns to an equilibrium phase by heat treatment after bonding, but in that case, it comes to exhibit high strength as an equilibrium phase.
タングステンもニツケル基合金においては固溶
強化をはかる代表的元素であるため、タングステ
ン添加による強度低下あるいは融点低下による強
度低下は生じない。 Since tungsten is also a typical element for solid solution strengthening in nickel-based alloys, there is no decrease in strength due to the addition of tungsten or a decrease in strength due to a decrease in melting point.
以上の如く、Ｗを含有しないものはガンマプラ
イム相が形成されるが、W0.5〜5at％を含むもの
はいずれにもガンマプライム相は形成されず、そ
のため強度の低下が大きくなることが明らかであ
る。従つて、0.5at％未満ではガンマプライム相
の生成をなくす効果がなく、また5at％を越えて
加えてもガマプライム相の生成を抑制する作用の
他に逆にそれ自身による強化作用が生じるので
5at％以下とすべきである。 As mentioned above, it is clear that the gamma prime phase is formed in those that do not contain W, but the gamma prime phase is not formed in any of those that contain 0.5 to 5 at% W, and therefore the strength decreases significantly. It is. Therefore, if it is less than 0.5 at%, it will not have the effect of eliminating the formation of gamma prime phase, and even if it is added in excess of 5 at%, in addition to the effect of suppressing the generation of gamma prime phase, it will also have a reinforcing effect by itself.
It should be less than 5at%.
また、102K／sec以下の冷却速度で凝固させた
場合は非平衡相が形成されなくなると同時に、結
晶粒を微細化させにくくなるためふさわしくな
い。なお本実施例では102K／sec以上の冷却速度
で凝固させる手段として双ロール法を用いたが、
この他にも単ロール法、スパツタ法、溶射法、化
学蒸着法（CDC法）、急速凝固粉末焼結材等を用
いても上記と同様な冷却速度が得られる。 Furthermore, solidification at a cooling rate of 10 2 K/sec or less is not suitable because no non-equilibrium phase is formed and at the same time it becomes difficult to refine the crystal grains. In this example, a twin roll method was used as a means of solidifying at a cooling rate of 10 2 K/sec or more, but
In addition, the same cooling rate as above can be obtained by using a single roll method, a sputtering method, a thermal spray method, a chemical vapor deposition method (CDC method), a rapidly solidified powder sintered material, and the like.
なお、本実施例で示した前記ニツケル基合金を
用いた拡散接合は固相での拡散接合に主眼を置い
たものであるが、被接合物の接合面間に挿入され
た前記ニツケル基合金が接合温度の高温域で溶融
して液相拡散接合の状態になつた場合において
も、接合応力が更に低くなるのみでなく、その拡
散接合用ニツケル基合金がアルミニム16〜22at％
含むことにより接合部が被接合物と同等あるいは
それ以上の量のガンマプライム相を析出する組成
となつているので、接合部の高温強度が被接合物
より低下することがなく、更に同時に、固溶強化
をはかる主要元素でもあるタングステンも含んで
いるので接合部の高温強度は更に高くなる。 The diffusion bonding using the nickel-based alloy shown in this example focuses on diffusion bonding in a solid phase, but the nickel-based alloy inserted between the bonding surfaces of the objects to be bonded is Even in the case of melting in the high temperature range of the bonding temperature and entering the state of liquid phase diffusion bonding, not only does the bonding stress become even lower, but the nickel-based alloy for diffusion bonding is 16 to 22 at% aluminum.
By including the gamma prime phase in the joint, the composition is such that the gamma prime phase precipitates in an amount equal to or greater than that of the objects to be joined, so the high-temperature strength of the joint does not decrease compared to that of the objects to be joined, and at the same time, it has a strong Since it also contains tungsten, which is a major element for strengthening the weld, the high-temperature strength of the joint is further increased.
従つて、本発明による拡散接合用ニツケル基合
金を、上述の如く液相における拡散接合に用いる
ことも本発明の技術範囲に含まれる。 Therefore, it is also within the technical scope of the present invention to use the nickel-based alloy for diffusion bonding according to the present invention for diffusion bonding in the liquid phase as described above.
本発明の構成によれば、平衡相においてガンマ
プライム相を生成して高強度を示す組成を有する
ニツケル基合金を、被接合物の接合面間に挿入し
て拡散接合することにより、低い接合応力で接合
することができ、かつ、接合部を熱処理により平
衡相に戻すことにより被接合物と同等あるいはそ
れ以上の高温強度を有する接合部を得ることがで
きる。
According to the configuration of the present invention, a nickel-based alloy having a composition that generates a gamma prime phase in the equilibrium phase and exhibits high strength is inserted between the joint surfaces of the objects to be joined and diffusion bonded, thereby reducing the joining stress. By returning the bonded portion to an equilibrium phase through heat treatment, it is possible to obtain a bonded portion having high-temperature strength equal to or greater than that of the objects to be bonded.
また、非平衡相形成に効果を示したタングステ
ンは、平衡相では固溶強化元素として高温強度の
向上に役立つている。 In addition, tungsten, which has shown an effect on non-equilibrium phase formation, is useful for improving high-temperature strength as a solid solution strengthening element in the equilibrium phase.
従つて、本発明の拡散接合用ニツケル基合金を
使用してニツケル基超合金の拡散接合を行うこと
により、高温で稼働するタービン等の運転温度の
上昇が可能となり、より高い運転効率が得られ
る。 Therefore, by performing diffusion bonding of a nickel-based superalloy using the nickel-based alloy for diffusion bonding of the present invention, it is possible to increase the operating temperature of turbines, etc. that operate at high temperatures, and higher operating efficiency can be obtained. .
第１図は1100℃における本発明のニツケル基合
金と商用ニツケル基超合金を含む比較材との高温
引張試験結果を示す図であり、第２図は102K／
sec以上の冷却速度で凝固したNi−20at％Al材の
Ｘ線回折結果を示す図であり、第３ａ図は本発明
によるNi−20at％Al−0.5at％ＷのＸ線回折結果
を示す図であり、第３ｂ図は本発明によるNi−
20at％Al−1at％ＷのＸ線回折結果を示す図であ
り、第３ｃ図は本発明によるNi−20at％Al−2at
％ＷのＸ線回折結果を示す図であり、第３ｄ図は
本発明によるNi−20at％Al−5at％ＷのＸ線回折
結果を示す図であり、第４ａ図は102K／sec以上
の冷却速度で凝固し1100℃で30分間加熱された
Ni−15at％Alのミクロ組織を示す写真であり、
第４ｂ図は102K／sec以上の冷却速度で凝固し
1100℃で30分間加熱されたNi−17.5at％Alのミ
クロ組織を示す写真であり、第４ｃ図は102K／
sec以上の冷却速度で凝固し1100℃で30分間加熱
されたNi−20at％Alのミクロ組織を示す写真で
あり、第４ｄ図は102K／sec以上の冷却速度で凝
固し1100℃で30分間加熱されたNi−22.5at％Al
のミクロ組織を示す写真である。
Figure 1 shows the results of a high-temperature tensile test at 1100°C between the nickel-based alloy of the present invention and a comparative material containing a commercial nickel-based superalloy, and Figure 2 shows the results at 10 2 K/
Fig. 3a is a diagram showing the X-ray diffraction results of Ni-20at%Al material solidified at a cooling rate of sec or more, and Fig. 3a is a diagram showing the X-ray diffraction results of Ni-20at%Al-0.5at%W according to the present invention. and FIG. 3b shows the Ni-
It is a figure showing the X-ray diffraction result of 20at%Al-1at%W, and Figure 3c is a figure showing the X-ray diffraction result of Ni-20at%Al-2at according to the present invention.
%W, FIG. 3d is a diagram showing the X-ray diffraction results of Ni-20at%Al-5at%W according to the present invention, and FIG. 4a is a diagram showing the X-ray diffraction results of Ni- 20at %Al-5at%W according to the present invention. Solidified at a cooling rate of
It is a photograph showing the microstructure of Ni−15at%Al,
Figure 4b shows solidification at a cooling rate of 10 2 K/sec or higher.
This is a photograph showing the microstructure of Ni-17.5at%Al heated at 1100°C for 30 minutes, and Figure 4c is a photograph showing the microstructure of Ni-17.5at%Al heated at 102K /
This is a photograph showing the microstructure of Ni-20at%Al solidified at a cooling rate of 102 K/sec or more and heated at 1100°C for 30 minutes. Ni−22.5at%Al heated for minutes
This is a photograph showing the microstructure of.
Claims (1)
間に挿入して拡散接合を行う拡散接合用ニツケル
基合金の製造方法において、アルミニウム16〜22
原子％、タングステン0.5〜５原子％及び残部ニ
ツケルからなる組成を有する溶湯を102〓／秒以
上の冷却速度で急冷凝固させることを特徴とする
拡散接合用ニツケル基合金の製造方法。1. In a method for manufacturing a nickel-based alloy for diffusion bonding in which diffusion bonding is performed by inserting a nickel-based superalloy between the bonding surfaces of objects to be bonded, aluminum 16 to 22
1. A method for producing a nickel-based alloy for diffusion bonding, which comprises rapidly solidifying a molten metal having a composition of 0.5 to 5 atomic % tungsten, and the balance nickel at a cooling rate of 10 2 /sec or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9197187A JPS63259043A (en) | 1987-04-16 | 1987-04-16 | Nickel based alloy for diffusion bonding and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9197187A JPS63259043A (en) | 1987-04-16 | 1987-04-16 | Nickel based alloy for diffusion bonding and its production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63259043A JPS63259043A (en) | 1988-10-26 |
| JPH0356289B2 true JPH0356289B2 (en) | 1991-08-27 |
Family
ID=14041418
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9197187A Granted JPS63259043A (en) | 1987-04-16 | 1987-04-16 | Nickel based alloy for diffusion bonding and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63259043A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0613743B2 (en) * | 1987-11-19 | 1994-02-23 | 工業技術院長 | Solid-state joining method for nickel-base superalloys |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS50148222A (en) * | 1974-05-04 | 1975-11-27 | ||
| JPS5891144A (en) * | 1974-08-07 | 1983-05-31 | アライド・コ−ポレ−シヨン | Amorphous metal alloy having high crystalline temperature and high hardness |
-
1987
- 1987-04-16 JP JP9197187A patent/JPS63259043A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS50148222A (en) * | 1974-05-04 | 1975-11-27 | ||
| JPS5891144A (en) * | 1974-08-07 | 1983-05-31 | アライド・コ−ポレ−シヨン | Amorphous metal alloy having high crystalline temperature and high hardness |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63259043A (en) | 1988-10-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4710235A (en) | Process for preparation of liquid phase bonded amorphous materials | |
| US4426033A (en) | Ductile titanium-copper brazing alloy | |
| US6616032B1 (en) | Brazing composition and method for brazing parts made of alumina-based materials with said composition | |
| US5068084A (en) | Columnar grain superalloy articles | |
| EP1444388A1 (en) | Mcraly-coating | |
| WO2003035946A1 (en) | Method of growing a mcraly-coating and an article coated with the mcraly-coating | |
| JP2001507758A (en) | High temperature protective coating | |
| KR20130010878A (en) | Braze foil for high-temperature brazing and methods for repairing or producing components using said braze foil | |
| US6692586B2 (en) | High temperature melting braze materials for bonding niobium based alloys | |
| JPH0613743B2 (en) | Solid-state joining method for nickel-base superalloys | |
| Choi et al. | Effect of In addition on Sn-3.5 Ag solder and joint with Cu substrate | |
| JPH0356289B2 (en) | ||
| US6720086B1 (en) | Liquid interface diffusion bonding of nickel-based superalloys | |
| Dinkel et al. | New boron and silicon free single crystal-diffusion brazing alloys | |
| JPS6125773B2 (en) | ||
| JPH0569890B2 (en) | ||
| FR2672905A1 (en) | COATINGS FORMING PROTECTION BARRIERS AGAINST OXIDATION, CONTAINING A COMPATIBILITY LAYER. | |
| US6740176B2 (en) | Single crystal seed alloy | |
| JP2001501256A (en) | Nickel-based alloys and their products | |
| JPH0569891B2 (en) | ||
| JPS62158597A (en) | Manufacture of multicomponent system congruent melting solder material | |
| Gale et al. | Ni3Al based composite interlayers for wide gap transient liquid phase bonding of NiAl–Hf single crystals to a nickel base superalloy | |
| Laux et al. | Development of Ni–Mn-based alloys for the fast epitaxial braze-repair of single-crystalline nickel-based superalloys | |
| JPS63266036A (en) | Ni based alloy | |
| JPH05263178A (en) | Manufacture of high strength niobium alloy and niobium alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |