JP2007057329A - Deterioration diagnosing method of ni-based hard metal by x-ray diffraction method and future lifetime evaluation method - Google Patents

Deterioration diagnosing method of ni-based hard metal by x-ray diffraction method and future lifetime evaluation method Download PDF

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JP2007057329A
JP2007057329A JP2005241592A JP2005241592A JP2007057329A JP 2007057329 A JP2007057329 A JP 2007057329A JP 2005241592 A JP2005241592 A JP 2005241592A JP 2005241592 A JP2005241592 A JP 2005241592A JP 2007057329 A JP2007057329 A JP 2007057329A
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nickel
diffraction
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diffraction peak
deterioration
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JP4719836B2 (en
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Kenichiro Igashira
賢一郎 井頭
Hideki Okado
英毅 尾角
Takuya Miyashita
卓也 宮下
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Kawasaki Heavy Industries Ltd
New Industry Research Organization NIRO
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New Industry Research Organization NIRO
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a creep damage diagnosing or future lifetime estimating method especially for an Ni-based hard metal capable of grasping a state even in a region large in creep damage and capable of accurately grasping the whole damage tendency, and the creep damage diagnosing or future lifetime estimating apparatus. <P>SOLUTION: The creep damage diagnosing or future lifetime estimating apparatus is constituted of a revolving sample stand 2, an X-ray irradiator 1 for emitting monochromatic X rays, an X-ray sensor 3 for measuring the intensity of X rays of a diffraction spot, a sensor position adjustment device 4 for adjusting their arrangement, a data processor 5 for inputting the output of the X-ray sensor to specify the shape of a diffraction peak, a memory device 6 for storing the shape of the diffraction peak and the function of a creep life consumption rate and an arithmetic device 7 for estimating the creep life consumption rate and the future lifetime on the basis of the shape of the diffraction peak using the function to exhibit them. After the X-ray sensor 3 aims at a predetermined diffraction spot, the sample stand 2 is relatively revolved with respect to the X-ray irradiator to measure the shape of the target diffraction peak. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、ガスタービン動静翼などに適用されるニッケル(Ni)基超合金のクリープ損傷による劣化の診断と、余寿命の評価法に関する。   The present invention relates to a diagnosis of deterioration due to creep damage of a nickel (Ni) base superalloy applied to a gas turbine rotor blade and the like, and a method for evaluating a remaining life.

最も高温まで高いクリープ破断強度を有してジェットエンジンやガスタービンの動静翼などに使用されるNi基超合金も、高温高応力環境に曝されてクリープ損傷を受け、クリープ損傷の蓄積により破壊に至る。機器設計や保全などの必要から、クリープ損傷程度の診断および損傷の程度から余寿命を推定する要求が強く、各所で各種の損傷診断法や余寿命推定法が開発されている。   Ni-base superalloys, which have high creep rupture strength up to the highest temperature and are used for moving blades and stationary blades of jet engines and gas turbines, are also subject to creep damage due to exposure to high-temperature and high-stress environments. It reaches. Due to the necessity of equipment design and maintenance, there is a strong demand for diagnosis of the extent of creep damage and estimation of the remaining life from the degree of damage, and various damage diagnosis methods and remaining life estimation methods have been developed in various places.

ニッケル基超合金は、面心立方格子型結晶構造を持つニッケル固溶体母相(γ相)内に、立方体状のニッケル基金属間化合物(γ’相)が3次元的に整然と配列した組織形態を有している。
ニッケル基超合金が高温下で長時間応力負荷される実機運転環境下で使用される間に、隣接するγ’相同士の融合による粗大化、扁平化が生じる。
A nickel-based superalloy has a structure in which cubic nickel-based intermetallic compounds (γ 'phase) are arranged in a three-dimensional order in a nickel solid solution matrix (γ phase) having a face-centered cubic lattice crystal structure. Have.
While the nickel-base superalloy is used in an actual machine operating environment where stress is applied for a long time at high temperature, coarsening and flattening occur due to the fusion of adjacent γ ′ phases.

そこで、γ’相を電子顕微鏡で観察して蓄積されたクリープダメージを評価し、余寿命を推定する組織観察法が一般化している。
しかし、組織観察法では、クリープ損傷の評価が観察者の感覚に左右され定量性が無い上、電子顕微鏡で観察できる領域が非常に狭いため全体の状態を把握できない。また、γ’相の縦横比などに現れる形状変化は、クリープダメージの小さい、寿命の0.1〜0.3程度の領域で飽和し、それ以上の大きなダメージを受けた領域では変化が小さく観察できない。さらに、電子顕微鏡で観察するにはサンプルを切り出す必要があるので、対象部材をそのまま再利用できない破壊検査となる。
Therefore, a structure observation method for estimating the remaining lifetime by observing the γ ′ phase with an electron microscope and evaluating the accumulated creep damage has been generalized.
However, in the structure observation method, the evaluation of creep damage is influenced by the observer's sense and is not quantitative, and the region that can be observed with an electron microscope is very narrow, so the whole state cannot be grasped. In addition, the shape change appearing in the aspect ratio of the γ 'phase is saturated in the region where the creep damage is small and the life is about 0.1 to 0.3, and the change is observed in the region where the damage is larger than that. Can not. Furthermore, since it is necessary to cut out a sample to observe with an electron microscope, it becomes a destructive inspection in which the target member cannot be reused as it is.

また、特許文献1にあるように、クリープ損傷が進行するに伴い磁気特性が変化することに着目してSQUID(超伝導磁束量子干渉計)を利用した劣化診断・余命推定装置が開発されている。
特許文献1に開示された方法は、測定対象を完全に消磁した後、励磁コイルとSQUID帯磁率計を用いて計測した結果をプロットした磁化曲線より、初期磁化率や残留磁化などの各種磁気特性を算出し、これらの特性からクリープ損傷程度を推定するものである。
開示方法は、原理的には部品を非破壊で評価することが可能である。しかし、実際の部品は全体が均等に劣化するのではなく、極く限られた領域でクリープ損傷が顕著に生じそこから破壊に進展するものである。したがって、測定対象全体を励磁した場合には、局部に重大な劣化があっても、劣化が問題にならない大部分の磁気特性変化の中に埋没して、検出することが困難である。
なお、本文献には、劣化が予測される部分を局所的に励磁し、磁化曲線を作成する方法が提案されているが、SQUID帯磁率計により得られる磁化曲線は、磁気コイルと測定対象部位の位置関係により敏感に変化するので、複雑な形状を有する実際の部品に適用するためには解決すべき技術課題が残っている。
Further, as disclosed in Patent Document 1, a deterioration diagnosis / life expectancy estimation device using a SQUID (superconducting magnetic flux quantum interferometer) has been developed by paying attention to the fact that magnetic characteristics change as creep damage progresses. .
In the method disclosed in Patent Document 1, various magnetic characteristics such as initial magnetic susceptibility and remanent magnetization are obtained from a magnetization curve obtained by plotting the measurement result using an excitation coil and a SQUID susceptibility meter after completely demagnetizing the measurement object. And the extent of creep damage is estimated from these characteristics.
The disclosed method can in principle evaluate parts nondestructively. However, the actual part does not deteriorate evenly as a whole, but creep damage occurs remarkably in a very limited region, and then progresses to destruction. Therefore, when the entire object to be measured is excited, it is difficult to detect it by burying it in most of the magnetic property changes where deterioration is not a problem, even if there is significant local deterioration.
In this document, a method of locally exciting a portion where deterioration is predicted and creating a magnetization curve is proposed. However, the magnetization curve obtained by the SQUID susceptibility meter includes a magnetic coil and a region to be measured. Therefore, the technical problem to be solved remains to be applied to an actual part having a complicated shape.

また、特許文献2には、X線回折ピークを利用して疲労損傷や余寿命を評価する非破壊評価方法が開示されている。
繰返し応力のために場所によって転位密度の差が生じるので格子定数も異なるようになることから、初めのうちは近接したX線回折ピークが重なって1つのピークになっていても、繰返し応力を受けているうちにピーク強度のアンバランスが大きくなってピークの非対称性が大きくなる。
文献2に開示された評価方法は、X線回折ピークプロファイルの左右非対称性が繰返し応力の繰り返し数に従って推移することに注目し、事前に実験により取得した両者の関係に照らし合わせて金属製部材の損傷度または余寿命を評価するものである。
Patent Document 2 discloses a nondestructive evaluation method for evaluating fatigue damage and remaining life using an X-ray diffraction peak.
Since the dislocation density varies depending on the location due to repetitive stress, the lattice constants also differ. Therefore, even if the adjacent X-ray diffraction peaks overlap to form one peak at the beginning, the repetitive stress is applied. In the meantime, the peak intensity imbalance increases and the asymmetry of the peak increases.
The evaluation method disclosed in Document 2 pays attention to the fact that the left-right asymmetry of the X-ray diffraction peak profile changes according to the number of repetitions of the cyclic stress, and in the light of the relationship between the two obtained in advance by experiment, It evaluates the degree of damage or remaining life.

しかし、この方法は、応力条件によって非対称度の推移の仕方が異なり、非対称度が同一でも応力レベルが異なると疲労損傷度や余寿命が異なるので、応力レベルが既知である必要がある。また、この方法の利用性は材料の結晶性質、温度、応力条件などにより変化し、アルミニウム、アルミニウム合金、鉄鋼、銅、銅合金など各種金属製部材に適用できることが分かっているが、本発明の主たる対象であるニッケル基超合金に適用できるかは不明である。
特開2001−141700号公報 特開平11−344454号公報
However, in this method, the way in which the degree of asymmetry changes depending on the stress condition, and even if the degree of asymmetry is the same, if the stress level is different, the degree of fatigue damage and the remaining life are different, so the stress level needs to be known. In addition, it has been found that the utility of this method varies depending on the crystal properties, temperature, stress conditions, etc. of the material, and can be applied to various metal members such as aluminum, aluminum alloy, steel, copper, copper alloy, etc. It is unclear whether it can be applied to the nickel-base superalloy, which is the main target.
JP 2001-141700 A JP-A-11-344454

そこで、本発明が解決しようとする課題は、余寿命が少なくなってクリープ損傷が大きい領域でも状態を把握することが可能で、観察領域が大きく全体の損傷傾向が正確に把握できる、非破壊検査が可能な、クリープ損傷診断あるいは余寿命推定方法および装置を提供することである。
特に、ニッケル基超合金を対象とする劣化診断あるいは余寿命推定方法および装置を提供することである。
Therefore, the problem to be solved by the present invention is a non-destructive inspection in which it is possible to grasp the state even in an area where the remaining life is reduced and the creep damage is large, and the entire damage tendency is accurately grasped. It is an object of the present invention to provide a creep damage diagnosis or remaining life estimation method and apparatus capable of satisfying the requirements.
In particular, it is to provide a deterioration diagnosis or remaining life estimation method and apparatus for nickel-base superalloys.

上記課題を解決するため、ニッケル固溶体母相(γ相)内にニッケル基金属間化合物析出相(γ’相)が整合的に散在してなるニッケル基超合金に使用する、本発明に係る劣化診断方法は、ニッケル基超合金の試料に単色X線を照射して離散的な回折スポットを生成し、これら回折スポットのうち予め決めた回折スポットを選択し、選択された回折スポットについて回折ピークの形状を測定し、回折ピークの分散にかかる係数がニッケル基超合金の劣化と対応する事実に基づいて、試料であるニッケル基超合金の劣化状態を診断することを特徴とする。   In order to solve the above-mentioned problems, the deterioration according to the present invention is used for a nickel-base superalloy in which nickel-base intermetallic compound precipitation phases (γ ′ phases) are consistently scattered in a nickel solid solution matrix (γ phase). The diagnostic method irradiates a sample of nickel-base superalloy with monochromatic X-rays to generate discrete diffraction spots, selects a predetermined diffraction spot among these diffraction spots, and selects a diffraction peak of the selected diffraction spot. The shape is measured, and the deterioration state of the nickel-base superalloy as a sample is diagnosed based on the fact that the coefficient concerning the dispersion of the diffraction peak corresponds to the deterioration of the nickel-base superalloy.

上記の予め決めた回折スポットは、ニッケル基金属間化合物(γ’相)の規則格子回折に起因する回折スポットであることが望ましく、ミラー指数(210)または(310)で表わされる結晶面に起因する回折光が回折光強度の点で有利である。
回折ピークは、所定の回折スポットにX線センサを置いた入射X線発生器とX線センサの組合わせに対して、試料を載せた試料台を相対的に揺動させて測定することにより得ることができる。
回折ピークの分散係数は、回折ピーク半価幅で代表することができる。また、劣化状態はクリープ寿命消費率に基づいて得ることができる。さらに、被検体であるニッケル基超合金の余寿命は、ニッケル基超合金の劣化診断方法により得られた劣化診断結果に基づいて算定することができる。
単色X線は放射光であってもよい。
The predetermined diffraction spot is preferably a diffraction spot caused by ordered lattice diffraction of a nickel-based intermetallic compound (γ ′ phase), and is caused by a crystal plane represented by a Miller index (210) or (310). The diffracted light is advantageous in terms of diffracted light intensity.
The diffraction peak is obtained by measuring the sample stage on which the sample is placed with respect to the combination of the incident X-ray generator and the X-ray sensor in which the X-ray sensor is placed at a predetermined diffraction spot. be able to.
The dispersion coefficient of the diffraction peak can be represented by the half width of the diffraction peak. Further, the deterioration state can be obtained based on the creep life consumption rate. Furthermore, the remaining life of the nickel-base superalloy that is the subject can be calculated based on the deterioration diagnosis result obtained by the nickel-base superalloy deterioration diagnosis method.
Monochromatic X-rays may be emitted light.

また、上記課題を解決するため、本発明のニッケル基超合金の劣化診断装置は、試料を把持して回動させる試料台と、単色X線をその試料台に照射する単色X線照射装置と、発生する離散的な回折スポットのX線強度を測定するX線センサと、X線照射装置と試料台とX線センサの配置を調整するセンサ位置調整装置と、X線センサの出力を入力して回折ピークの形状を特定する測定データ処理装置と、回折ピーク形状とクリープ寿命消費率の関数を格納する記憶装置と、特定された回折ピーク形状に基づき記憶装置に格納した関数を用いてクリープ寿命消費率を算出し、あるいはクリープ寿命消費率に基づいてニッケル基超合金の余寿命を推定して提示する演算装置とから構成される装置である。
本発明のニッケル基超合金の劣化診断装置は、センサ位置調整装置によりX線センサが測定対象とする回折スポットに照準を合わせた後は、試料台をX線照射装置とX線センサに対して相対的に回動させることにより対象の回折ピークの形状を測定することを特徴とする。
In order to solve the above problems, a nickel-base superalloy deterioration diagnosis apparatus according to the present invention includes a sample stage for gripping and rotating a sample, and a monochromatic X-ray irradiation apparatus for irradiating the sample stage with monochromatic X-rays. The X-ray sensor for measuring the X-ray intensity of the generated discrete diffraction spot, the sensor position adjusting device for adjusting the arrangement of the X-ray irradiation device, the sample stage and the X-ray sensor, and the output of the X-ray sensor are input. The measurement data processing device for identifying the diffraction peak shape, the storage device for storing the function of the diffraction peak shape and the creep life consumption rate, and the creep life using the function stored in the storage device based on the specified diffraction peak shape It is an apparatus composed of an arithmetic unit that calculates the consumption rate or estimates and presents the remaining life of the nickel-base superalloy based on the creep life consumption rate.
In the nickel-base superalloy deterioration diagnosis device according to the present invention, after the X-ray sensor is aimed at the diffraction spot to be measured by the sensor position adjustment device, the sample stage is placed on the X-ray irradiation device and the X-ray sensor. The shape of the diffraction peak of the object is measured by relatively rotating.

なお、本発明のニッケル基超合金の劣化診断装置において、測定する回折スポットがニッケル基金属間化合物(γ’相)結晶に起因する回折スポットであり、回折ピークの形状は回折ピーク半価幅により代表され、ニッケル基超合金の劣化状態はクリープ寿命消費率に基づいて得られるものであることが好ましい。
また、単色X線発生装置は放射光発生装置であっても良い。
In the nickel-base superalloy deterioration diagnosis apparatus of the present invention, the diffraction spot to be measured is a diffraction spot caused by a nickel-based intermetallic compound (γ ′ phase) crystal, and the shape of the diffraction peak depends on the half-value width of the diffraction peak. Typically, the deterioration state of the nickel-base superalloy is preferably obtained based on the creep life consumption rate.
Further, the monochromatic X-ray generator may be a synchrotron radiation generator.

クリープダメージの蓄積は直接的には結晶の変化、すなわち格子定数の変化や結晶の乱れ具合の変化に反映されるため、結晶の変化からクリープダメージを推定する方法は、γ’相の形態変化を観察する方法より材料学的に根元的な変化を把握することになる。
本発明のニッケル基超合金の劣化診断・余寿命推定方法および装置は、X線回折法により得られる回折ピークが結晶の格子定数や結晶の乱れの情報を含むことに基づくもので、結晶の乱れを特に反映する回折ピークを選択して、その回折ピークの弛み具合からクリープダメージの蓄積を推定する。
Since creep damage accumulation is directly reflected in crystal changes, that is, changes in lattice constants and changes in crystal turbulence, the method of estimating creep damage from crystal changes is based on changes in the morphology of the γ 'phase. The fundamental change in material will be grasped from the observation method.
The nickel-base superalloy deterioration diagnosis / remaining life estimation method and apparatus according to the present invention is based on the fact that the diffraction peak obtained by the X-ray diffraction method includes information on the crystal lattice constant and the crystal disorder. Is selected, and the accumulation of creep damage is estimated from the looseness of the diffraction peak.

回折ピークの弛み具合をピークの半価幅で定量化すると、半価幅がクリープ寿命消費率とよく対応し、特に寿命末期の領域でも半価幅が飽和することなく対応してクリープ損傷度を評価することができる。
このとき、ニッケル合金結晶に起因する回折ピークを選択すると、寿命末期領域における線形性がよく、評価が容易である。特に、ミラー指数(210)または(310)で表わされる結晶面に起因する回折スポットにおける特性が寿命消費率の測定に適している。
Quantifying the looseness of the diffraction peak by the half-value width of the peak, the half-value width corresponds well to the creep life consumption rate. Can be evaluated.
At this time, if a diffraction peak due to the nickel alloy crystal is selected, the linearity in the end of life region is good and the evaluation is easy. In particular, the characteristic in the diffraction spot due to the crystal plane represented by the Miller index (210) or (310) is suitable for the measurement of the lifetime consumption rate.

θロッキングカーブ法で測定した回折ピーク半価幅は、結晶内のポリゴニゼーションすなわち結晶の乱れを反映していて、原理的には結晶が乱れるにつれて大きくなる。回折ピーク半価幅は同じ超合金でも結晶面毎に異なるが、寿命消費率が大きい領域で回折ピーク半価幅が徐々に増加するような結晶面が存在するので、この結晶面について回折ピークを取得すれば回折ピーク半価幅に基づいて寿命消費率を的確に推定することが可能である。
ここで用いられるθロッキングカーブ法は、入射するX線と回折光を検出するセンサの角度関係を固定し、X線の照射位置を通りかつ入射X線と検出センサがなす面に垂直な軸を中心として測定対象物を揺動させることにより、測定対象物への入射X線の入射角を変化させて、得られた回折X線強度を測定対象物の揺動角度に対してプロットする方法である。
The half width of the diffraction peak measured by the θ rocking curve method reflects the polygonization within the crystal, that is, the disorder of the crystal, and in principle increases as the crystal is disturbed. Although the diffraction peak half-value width differs for each crystal surface even in the same superalloy, there is a crystal surface where the diffraction peak half-value width gradually increases in a region where the lifetime consumption rate is large. Once acquired, it is possible to accurately estimate the lifetime consumption rate based on the half width of the diffraction peak.
The θ rocking curve method used here fixes the angular relationship between the incident X-ray and the sensor that detects the diffracted light, and sets an axis that passes through the X-ray irradiation position and is perpendicular to the plane formed by the incident X-ray and the detection sensor. By oscillating the measurement object as the center, changing the incident angle of the incident X-ray to the measurement object, and plotting the obtained diffracted X-ray intensity against the oscillation angle of the measurement object is there.

本発明のニッケル基超合金の劣化診断・余寿命推定方法および装置は、非破壊分析により、クリープ損傷後半まで変化を捉えることができ、また、電子顕微鏡観察法を用いる場合より観察領域が広く、試料の状態をより正確に把握することができる。   The deterioration diagnosis / remaining life estimation method and apparatus of the nickel-base superalloy of the present invention can capture changes until the latter half of creep damage by nondestructive analysis, and has a wider observation area than when using an electron microscope observation method, The state of the sample can be grasped more accurately.

以下、本発明について実施例に基づき図面を参照して詳細に説明する。
図1はニッケル基超合金の初期組織図、図2はニッケル基超合金の初期状態の写真、図3はニッケル基超合金のクリープ後の写真、図4は本実施例のニッケル基超合金の劣化診断装置の構成を示すブロック図、図5は本実施例のニッケル基超合金の劣化診断方法の手順例を示すフロー図、図6はニッケル金属相における回折ピークを表わすグラフ、図7はニッケル金属相における別の回折ピークを表わすグラフ、図8はニッケル合金相の結晶面に係る回折ピークの変化を示すグラフ、図9はθロッキングカーブ法により得られた回折ピークを表わすグラフ、図10はθロッキングカーブ法により得た寿命消費率と回折ピーク半価幅の関係を示すグラフである。
Hereinafter, the present invention will be described in detail based on examples with reference to the drawings.
FIG. 1 is an initial structure diagram of a nickel-base superalloy, FIG. 2 is a photograph of the initial state of the nickel-base superalloy, FIG. 3 is a photograph after the creep of the nickel-base superalloy, and FIG. FIG. 5 is a flowchart showing an example of the procedure of a nickel base superalloy deterioration diagnosis method according to this embodiment, FIG. 6 is a graph showing diffraction peaks in the nickel metal phase, and FIG. 7 is nickel. 8 is a graph showing another diffraction peak in the metal phase, FIG. 8 is a graph showing a change in the diffraction peak related to the crystal plane of the nickel alloy phase, FIG. 9 is a graph showing a diffraction peak obtained by the θ rocking curve method, and FIG. It is a graph which shows the relationship between the lifetime consumption rate obtained by (theta) rocking curve method, and a diffraction peak half value width.

ニッケル基超合金は、図1に概念図として示すように、面心立方格子型の結晶構造を持つニッケル母相(γ相)内に、立方体状のニッケル基金属間化合物析出相部(γ’相)が3次元的に整然と配列した組織形態を有している。
ニッケル基超合金は、初めは図2に示すような立方体状のニッケル基金属間化合物析出相部(γ’相)が3次元的に整然と配列した構造を有するが、ガスタービンの実機運転環境下で使用される間に、隣接するγ’相同士の融合による粗大化、扁平化が生じる。
As shown in a conceptual diagram in FIG. 1, a nickel-base superalloy has a cubic nickel-base intermetallic compound precipitation phase portion (γ ′) in a nickel matrix (γ phase) having a face-centered cubic lattice type crystal structure. Phase) has a three-dimensional orderly organization.
The nickel-base superalloy initially has a structure in which cubic nickel-base intermetallic compound precipitation phases (γ ′ phases) as shown in FIG. 2 are three-dimensionally arranged, but under the actual operating environment of the gas turbine. During use, coarsening and flattening occur due to the fusion of adjacent γ ′ phases.

このように、クリープダメージの蓄積は直接的には結晶の変化に反映され、X線回折法により得られる回折ピークは、結晶の格子定数、転位や面欠陥など結晶の乱れの情報を含んでいる。
θロッキングカーブ法により得られる回折ピークの広がりは、結晶の湾曲やポリゴニゼーション、すなわち結晶に与えられるダメージを反映していると考えられ、原理的にはクリープダメージが蓄積して結晶が乱れるにつれて大きくなる。
As described above, the accumulation of creep damage is directly reflected in the change of the crystal, and the diffraction peak obtained by the X-ray diffraction method includes information on the disorder of the crystal such as the crystal lattice constant, dislocation and surface defects. .
The broadening of the diffraction peak obtained by the θ rocking curve method is thought to reflect the curvature and polygonization of the crystal, that is, the damage given to the crystal, and in principle, as creep damage accumulates and the crystal is disturbed. growing.

本実施例のニッケル基超合金の劣化診断方法は、Ni基超合金の試料にX線を照射して得られた回折ピークを観察することによって、蓄積されたクリープダメージを評価し、余寿命を推定しようとするものである。
本実施例の方法では、解析を容易にするため、析出強化型Ni基超耐熱合金のX線回折ピークのうち、析出相(γ’相)から回折されて形成する回折ピークに着目する。
The deterioration diagnosis method of the nickel-base superalloy according to the present embodiment evaluates the accumulated creep damage by observing the diffraction peak obtained by irradiating the sample of the Ni-base superalloy with X-rays, and increases the remaining life. It is something to be estimated.
In the method of this example, in order to facilitate the analysis, attention is paid to the diffraction peak formed by diffracting from the precipitation phase (γ ′ phase) among the X-ray diffraction peaks of the precipitation strengthened Ni-base superalloy.

図4は本実施例のニッケル基超合金の劣化診断装置の構成を示すブロック図である。
本実施例のニッケル基超合金劣化診断装置は、X線照射装置1、試料台2、X線検出装置3、センサ位置調整装置4、測定データ処理装置5、関数記憶装置6、評価演算装置7、プリンタ8により構成される。
FIG. 4 is a block diagram showing the configuration of the nickel-base superalloy deterioration diagnosis apparatus of this embodiment.
The nickel-base superalloy deterioration diagnosis device of this embodiment includes an X-ray irradiation device 1, a sample stage 2, an X-ray detection device 3, a sensor position adjustment device 4, a measurement data processing device 5, a function storage device 6, and an evaluation calculation device 7. The printer 8 is configured.

X線照射装置1は、単色X線を発生し試料に向けて放出する。X線照射装置1は、放射光による高強度、狭帯域のX線を供給するものであることが好ましい。特性X線を利用したり、フィルタで単色化したものを利用することもできる。
試料台2は、測定対象物9をX線照射位置に位置調整して固定すると共に、X線入射軸に対して適当な角度内で揺動させる機能を有する。揺動運動はセンサ位置調整装置4により制御される。
The X-ray irradiation apparatus 1 generates monochromatic X-rays and emits them toward a sample. It is preferable that the X-ray irradiation apparatus 1 supplies high-intensity, narrow-band X-rays by radiated light. It is also possible to use characteristic X-rays or a monochromatic filter.
The sample stage 2 has a function of adjusting the position of the measuring object 9 at the X-ray irradiation position and fixing it, and swinging it within an appropriate angle with respect to the X-ray incident axis. The swing motion is controlled by the sensor position adjusting device 4.

X線照射装置1から放出される入射X線は測定対象物9で回折して後方空間中に複数の回折スポットを生じる。回折スポットの発生位置は、測定対象物9に存在する結晶面に対応して決まっている。
X線検出装置3は、入射するX線の強度に対応する電気信号を発生する装置で、X線入射軸が常に測定対象物9の方向を向くようにしながら3次元空間中で位置変更することができる。
Incident X-rays emitted from the X-ray irradiation apparatus 1 are diffracted by the measurement object 9 to generate a plurality of diffraction spots in the rear space. The generation position of the diffraction spot is determined corresponding to the crystal plane existing on the measurement object 9.
The X-ray detection apparatus 3 is an apparatus that generates an electrical signal corresponding to the intensity of incident X-rays, and changes the position in a three-dimensional space while the X-ray incident axis always faces the direction of the measurement object 9. Can do.

センサ位置調整装置4は、X線検出装置3の入射軸をX線照射装置1のX線照射軸に対して角度調整すると共に、試料台2の傾きを調整することができる。なお、単色X線に放射光を利用してX線照射装置1を容易に動かせない場合などには、X線照射装置1を固定して試料台2とX線検出装置3の位置姿勢を調整するようにしてもよい。
測定データ処理装置5は、センサ位置調整装置4から試料台2とX線検出装置3の位置情報を入力し、X線検出装置3の測定出力を入力して、データ処理し、回折スポットにおける回折ピークの状態を解明する。
The sensor position adjustment device 4 can adjust the angle of the incident axis of the X-ray detection device 3 with respect to the X-ray irradiation axis of the X-ray irradiation device 1 and can adjust the inclination of the sample stage 2. In addition, when the X-ray irradiation apparatus 1 cannot be moved easily by using synchrotron radiation for monochromatic X-rays, the position and orientation of the sample stage 2 and the X-ray detection apparatus 3 are adjusted by fixing the X-ray irradiation apparatus 1. You may make it do.
The measurement data processing device 5 inputs the position information of the sample stage 2 and the X-ray detection device 3 from the sensor position adjustment device 4, inputs the measurement output of the X-ray detection device 3, performs data processing, and performs diffraction at the diffraction spot Elucidate the state of the peak.

関数記憶装置6は、回折ピークとクリープ寿命消費率の関係を表わす関数を記録していて、評価演算装置7の要求に応じて適宜必要な関数を供給する。
評価演算装置7は、回折ピークを解析して回折ピークの裾の広がり具合を把握し、関数記憶装置6から供給される関数を利用して測定対象物9のクリープ寿命消費率を求め、さらに測定対象物9の余寿命を求める。
プリンタ8は、評価演算装置7の評価結果を出力する。なお、プリンタ8の代りにあるいはこれに加えて液晶表示装置などの表示装置に評価結果を表示しても良い。
The function storage device 6 records a function representing the relationship between the diffraction peak and the creep life consumption rate, and supplies a necessary function as needed according to the request of the evaluation arithmetic device 7.
The evaluation calculation device 7 analyzes the diffraction peak to grasp the extent of the bottom of the diffraction peak, obtains the creep life consumption rate of the measurement object 9 using the function supplied from the function storage device 6, and further measures The remaining life of the object 9 is obtained.
The printer 8 outputs the evaluation result of the evaluation calculation device 7. Note that the evaluation result may be displayed on a display device such as a liquid crystal display device instead of or in addition to the printer 8.

図5は本実施例のニッケル基超合金の劣化診断方法の手順を表わすフロー図である。
測定対象物9であるニッケル基超合金を試料台2にセットし(S01)、単色X線を照射して回折スポットを生成する(S02)。
ニッケル基超合金は結晶粒径が1mm以上と大きく、一方、高精度測定のためX線照射面積を小さく、たとえばX線ビームサイズを0.4mm平方程度にしたいので、1個の結晶に単色X線を照射することになり、通常の粉末法で得られるような入射X線の軸を中心とした同心円(デバイシェラーリング)となる代りに、回折スポットがデバイシェラーリングとなるべき同心円上に離散的に生成する。なお、回折スポットの位置は、サンプルのセット毎に変化し予め決めることができない。
FIG. 5 is a flowchart showing the procedure of the deterioration diagnosis method for the nickel-base superalloy of this embodiment.
A nickel-base superalloy, which is the object 9 to be measured, is set on the sample stage 2 (S01), and a monochromatic X-ray is irradiated to generate a diffraction spot (S02).
The nickel-base superalloy has a crystal grain size as large as 1 mm or more, while the X-ray irradiation area is small for high-precision measurement, for example, the X-ray beam size is about 0.4 mm square. Instead of a concentric circle (Debye-Scherrer ring) centered on the axis of the incident X-ray as obtained by a normal powder method, the diffraction spot is discrete on a concentric circle that should be a Debye-Scherrer ring. Generate automatically. The position of the diffraction spot changes for each set of samples and cannot be determined in advance.

回折スポットは結晶面について固有な回折角2θを持っているので、この回折角を知っているときには、たとえば、X線検出装置3の入射軸とX線照射装置1の照射軸が測定対象物9の上で回折角2θの角度を持って交差するように固定し、X線照射装置1に対して固定したX線検出装置3をX線照射軸の回りに回転させながらセンサ出力をモニタして出力極大値を見つけることにより、ある結晶面に係る回折スポットを検出することができる。
なお、高輝度な放射光を利用するときには、イメージングプレートを使って回折スポットの位置を比較的簡単に確認することができる。
Since the diffraction spot has a unique diffraction angle 2θ with respect to the crystal plane, when the diffraction angle is known, for example, the incident axis of the X-ray detection device 3 and the irradiation axis of the X-ray irradiation device 1 are the measurement object 9. The sensor output is monitored while rotating the X-ray detector 3 fixed around the X-ray irradiation apparatus 1 around the X-ray irradiation axis. By finding the output maximum value, a diffraction spot related to a certain crystal plane can be detected.
Note that when using high-intensity synchrotron radiation, the position of the diffraction spot can be relatively easily confirmed using an imaging plate.

回折スポットにおける回折ピークの裾の広がりは、結晶に導入される欠陥の量を反映する。各回折ピークは、それぞれのクリープダメージの蓄積により広がりを呈するが、特にニッケル基金属間化合物(γ’相)の規則格子回折に起因する回折ピークの変化によく対応する。
また、回折ピークの回折角度が接近している場合には、互いの回折ピークが重なって観察されるため、それぞれの回折ピークに分割することが難しく、分離処理に観察者の恣意が含まれる可能性があるため、それぞれのピーク形状から劣化の度合いを評価する本手法では正確な評価の保証ができない。
The broadening of the bottom of the diffraction peak at the diffraction spot reflects the amount of defects introduced into the crystal. Each diffraction peak exhibits a broadening due to the accumulation of the respective creep damage, but particularly corresponds well to a change in the diffraction peak due to regular lattice diffraction of the nickel-based intermetallic compound (γ ′ phase).
In addition, when the diffraction angles of the diffraction peaks are close to each other, the diffraction peaks are observed to overlap each other, so that it is difficult to divide the diffraction peaks into the respective diffraction peaks, and the arbitration of the observer may be included in the separation process. Therefore, this method that evaluates the degree of deterioration from each peak shape cannot guarantee an accurate evaluation.

たとえば、ニッケル基超合金の一種である耐熱性能の高いMarM247のミラー指数(200)や(220)の結晶面に係る回折ピークは、それぞれ図6と図7に示したように、ニッケル固溶体相のγ相とニッケル基金属間化合物析出相のγ’相が近接して重畳しているので、回折ピークを正確に分割してそれぞれのテーリング状態を客観的に正しく評価することは極めて難しい。
図6は、MarM247のニッケル固溶体(γ相)とニッケル基金属間化合物析出相(γ’相)のピークが近接して出現するミラー指数(200)面回折ピークを例示するグラフ、また、図7は同様にピークが近接するミラー指数(220)面回折ピーク例を示したグラフである。
このため、クリープダメージの蓄積を正しく推量するためには、γ’相に係わる回折ピークであって他の回折ピークと十分に離れたピークを選択することが好ましい。
For example, as shown in FIGS. 6 and 7, the diffraction peaks associated with the crystal face of the Miller index (200) and (220) of MarM247, which is a kind of nickel-based superalloy and has high heat resistance, are shown in FIGS. 6 and 7, respectively. Since the γ ′ phase and the γ ′ phase of the nickel-based intermetallic compound precipitation phase are closely superposed, it is extremely difficult to accurately divide the diffraction peak and objectively evaluate each tailing state.
FIG. 6 is a graph illustrating a Miller index (200) plane diffraction peak in which MarM247 nickel solid solution (γ phase) and nickel-based intermetallic compound precipitation phase (γ ′ phase) appear close to each other, and FIG. Is a graph showing an example of a Miller index (220) plane diffraction peak in which peaks are similarly close.
For this reason, in order to correctly estimate the accumulation of creep damage, it is preferable to select a diffraction peak related to the γ ′ phase and sufficiently separated from other diffraction peaks.

図8は、MarM247のミラー指数(210)の結晶面に係る回折角45°付近にあるγ’相の回折ピークの変化を示すグラフである。(210)回折ではニッケル基金属間化合物析出相(γ’相)のピークのみが現れることが分かる。図8(a)はクリープテストを行う前の状態、図8(b)はある条件下でクリープテストを行っている最中の状態、図8(c)はある条件下で破損に至ったときの回折ピークの状態を表わす。
クリープダメージが蓄積する前は回折ピークのテーリングは小さいが、破損するほどクリープダメージが蓄積した図8(c)の回折ピークではピークの裾が広く開いていることが分かる。
このように、γ’相結晶の乱れに対応する回折ピークの弛みは、回折角度の変化方向に観測することによって観察することができる。
FIG. 8 is a graph showing changes in the diffraction peak of the γ ′ phase in the vicinity of the diffraction angle of 45 ° with respect to the crystal face of the MarM247 Miller index (210). In (210) diffraction, it can be seen that only the peak of the nickel-based intermetallic compound precipitation phase (γ ′ phase) appears. Fig. 8 (a) shows the state before the creep test, Fig. 8 (b) shows the state during the creep test under a certain condition, and Fig. 8 (c) shows the case where the breakage occurs under the certain condition. Represents the state of diffraction peaks.
It can be seen that the tail of the diffraction peak is small before creep damage is accumulated, but the bottom of the peak is wide open at the diffraction peak of FIG.
Thus, the loosening of the diffraction peak corresponding to the disturbance of the γ ′ phase crystal can be observed by observing in the direction of change of the diffraction angle.

しかし、X線照射軸に対し試料の姿勢を変化させて出力変化を検出するθロッキングカーブ法により得られた回折ピークについて観測することによっても評価することができる。
θロッキングカーブ法とは、被検体を照射する入射X線の方向に対する、回折X線が入射するX線検出器の向きすなわち回折角度2θを固定した後に、被検体をX線入射位置を軸として揺動させて、回折ピークにおける広がりを測定する方法である。X線発生器のX線軸とX線検出器の入射方向との交差角を回折角度2θに固定したものを、被検体に対するX線入射位置を回動軸として揺動させても同じ結果を得ることができる。
However, it can also be evaluated by observing the diffraction peak obtained by the θ rocking curve method in which the change of the sample posture with respect to the X-ray irradiation axis is detected and the output change is detected.
In the θ rocking curve method, the direction of the X-ray detector on which the diffracted X-rays are incident, that is, the diffraction angle 2θ with respect to the direction of the incident X-rays irradiating the subject is fixed, and then the subject is taken as the X-ray incident position as an axis. This is a method of measuring the spread at the diffraction peak by swinging. The same result can be obtained even when the X-ray generator X-ray axis and the X-ray detector incident direction fixed at the intersection angle of the diffraction angle 2θ are swung with the X-ray incident position with respect to the subject as the rotation axis. be able to.

図9は、ミラー指数(310)の結晶面についてθロッキングカーブ法により得られた回折ピークを表わすグラフである。横軸はX線軸に対する試料台2の傾き角、縦軸は回折スポットにおけるX線強度を表わす。
回折角度の変化に基づく回折ピークは、回折格子の面間距離の乱れに関係するものが重畳されているのに対して、姿勢変化に基づく回折ピークは、特定の格子面間隔を持つ結晶にのみ注目したもので、半価幅の増大は結晶面の傾きがばらついていることの反映であるから、ニッケル基超合金の融合化状態を評価するためにはより適切と考えられる。
なお、回折ピークの広がりを簡単に計数化する1つの方法に、半価幅(FWHM)がある。半価幅とは、ピークの高さの半分の位置におけるピークの幅を意味する。回折ピーク半価幅が大きいほどピークの広がりは大きく、結晶の乱れが大きい。
FIG. 9 is a graph showing a diffraction peak obtained by the θ rocking curve method for the crystal plane of the Miller index (310). The horizontal axis represents the tilt angle of the sample stage 2 with respect to the X-ray axis, and the vertical axis represents the X-ray intensity at the diffraction spot.
The diffraction peak based on the change in diffraction angle is superimposed on the one related to the disturbance of the interplanar distance of the diffraction grating, whereas the diffraction peak based on the change in posture is only for crystals having a specific lattice spacing. It has been noticed that the increase in the half width is a reflection of the variation in the inclination of the crystal plane, and is considered more appropriate for evaluating the fusion state of the nickel-base superalloy.
One method for easily counting the spread of diffraction peaks is the half-value width (FWHM). The half-value width means the width of the peak at a position half the height of the peak. The larger the half width of the diffraction peak, the larger the peak spread and the greater the disorder of the crystal.

図10は、Ni基超耐熱合金であるMarM247の一方向凝固材について実測した寿命消費率と回折ピーク半価幅の関係を示すグラフである。横軸は評価した試料の寿命消費率t/trを示し、縦軸はθロッキングカーブ法で得た結晶面の回折ピーク半価幅(FWHM)を示す。tは評価試料のクリープ試験時間、trは評価材料のクリープ寿命データから求めた破断寿命を表わす。   FIG. 10 is a graph showing the relationship between the lifetime consumption rate and diffraction peak half-value width measured for a unidirectionally solidified material of MarM247, which is a Ni-based superalloy. The horizontal axis represents the lifetime consumption rate t / tr of the evaluated sample, and the vertical axis represents the diffraction peak half width (FWHM) of the crystal plane obtained by the θ rocking curve method. t represents the creep test time of the evaluation sample, and tr represents the rupture life obtained from the creep life data of the evaluation material.

図10から分かるように、回折ピーク半価幅は結晶面毎に異なるが、寿命消費率が大きい領域で徐々に増加するものが存在し、これらの特性を用いれば回折ピーク半価幅に基づいて寿命消費率を推定することが可能であることが分かる。
これらの回折ピークから、隣の回折ピークから十分離れているなどの条件も加えると、γ’相に係わるミラー指数(210)および(310)で表わされる面にかかる回折ピークが最も適切と考えられる。(210)および(310)の回折ピークは、クリープ寿命消費率が0.2程度から1.0までの間、その半価幅が単調に増加しているので、クリープダメージの蓄積度合いを評価するために有効である。
As can be seen from FIG. 10, the diffraction peak half-value width varies from crystal plane to crystal plane, but there are some which gradually increase in the region where the lifetime consumption rate is large. It can be seen that the lifetime consumption rate can be estimated.
If conditions such as being sufficiently far from the adjacent diffraction peaks are added from these diffraction peaks, the diffraction peaks on the planes represented by Miller indices (210) and (310) related to the γ ′ phase are considered to be most appropriate. . The diffraction peaks of (210) and (310) have a monotonically increasing half-value width when the creep life consumption rate is about 0.2 to 1.0, so the degree of creep damage accumulation is evaluated. It is effective for.

そこで、本実施例のニッケル基超合金の劣化診断方法では、(210)など予め決めた回折スポットを選択してX線検出装置3をセットする(S03)。
次に、X線検出装置3の出力を監視しながら、θロッキングカーブ法により試料9を単色X線に対して相対的に回動させて、X線センサの出力を収集し、測定データ処理装置5で回折ピークの形状を測定する(S04)。
Therefore, in the nickel base superalloy deterioration diagnosis method of this embodiment, a predetermined diffraction spot such as (210) is selected and the X-ray detector 3 is set (S03).
Next, the output of the X-ray sensor is collected by rotating the sample 9 relative to the monochromatic X-ray by the θ rocking curve method while monitoring the output of the X-ray detection device 3, and the measurement data processing device The shape of the diffraction peak is measured at 5 (S04).

評価演算装置7は、得られた回折ピークの形状からピークの分散係数を求める(S05)。分散係数として、半価幅を用いるのが便利である。
また、予め求められ関数記憶装置6に格納されている半価幅とクリープ寿命消費率の関係を表わす関数あるいは表を適用して、先に求めた回折ピークの分散係数(半価幅)から対象材料のクリープ寿命消費率を算出する(S06)。
さらに、算出されたクリープ寿命消費率と経時時間から材料としての余寿命を推定計算して(S07)、これらの結果をプリントアウトする(S08)。
The evaluation calculation device 7 obtains a peak dispersion coefficient from the obtained diffraction peak shape (S05). It is convenient to use the half width as the dispersion coefficient.
In addition, by applying a function or table representing the relationship between the half-value width and the creep life consumption rate obtained in advance and stored in the function storage device 6, the object is obtained from the previously obtained diffraction peak dispersion coefficient (half-value width). The creep life consumption rate of the material is calculated (S06).
Further, the remaining life as a material is estimated and calculated from the calculated creep life consumption rate and elapsed time (S07), and these results are printed out (S08).

本発明の劣化診断方法および装置により、従来困難だったジェットエンジンなどの高温長時間の応力負荷状態で使用したニッケル基超合金の寿命消費率および余寿命を非破壊的手段により評価することが可能になった。   With the degradation diagnosis method and apparatus of the present invention, it is possible to evaluate the life consumption rate and remaining life of nickel-base superalloys used under high-temperature and long-time stress load conditions such as jet engines, which has been difficult in the past, by nondestructive means. Became.

ニッケル基超合金の初期組織図である。It is an initial organization chart of a nickel base superalloy. ニッケル基超合金の初期状態の写真である。It is a photograph of the initial state of a nickel base superalloy. ニッケル基超合金のクリープ後の写真である。It is the photograph after the creep of a nickel base superalloy. 本発明の1実施例に係るニッケル基超合金の劣化診断装置の構成を示すブロック図である。It is a block diagram which shows the structure of the deterioration diagnostic apparatus of the nickel base superalloy which concerns on one Example of this invention. 本実施例のニッケル基超合金の劣化診断方法の手順例を示すフロー図である。It is a flowchart which shows the example of a procedure of the deterioration diagnostic method of the nickel base superalloy of a present Example. ニッケル基超合金における(200)面回折ピークの例を表わすグラフである。It is a graph showing the example of the (200) plane diffraction peak in a nickel base superalloy. ニッケル基超合金における(220)面回折ピークの例を表わすグラフである。It is a graph showing the example of the (220) plane diffraction peak in a nickel base superalloy. 本実施例におけるニッケル基超合金の(210)面回折ピーク例を示すグラフである。It is a graph which shows the (210) plane diffraction peak example of the nickel base superalloy in a present Example. 本実施例におけるニッケル基超合金のθロッキングカーブ法により得られた回折ピークを表わすグラフである。It is a graph showing the diffraction peak obtained by the (theta) rocking curve method of the nickel base superalloy in a present Example. θロッキングカーブ法により得た寿命消費率と回折ピーク半価幅の関係を示すグラフである。It is a graph which shows the relationship between the lifetime consumption rate obtained by (theta) rocking curve method, and a diffraction peak half value width.

符号の説明Explanation of symbols

1 X線照射装置
2 試料台
3 X線検出装置
4 センサ位置調整装置
5 測定データ処理装置
6 関数記憶装置
7 評価演算装置
8 プリンタ
9 測定対象物、試料
DESCRIPTION OF SYMBOLS 1 X-ray irradiation apparatus 2 Sample stand 3 X-ray detection apparatus 4 Sensor position adjustment apparatus 5 Measurement data processing apparatus 6 Function storage apparatus 7 Evaluation operation apparatus 8 Printer 9 Measurement object and sample

Claims (11)

ニッケル固溶体母相(γ相)内にニッケル基金属間化合物析出相(γ’相)が整合的に散在してなるニッケル基超合金の試料に単色X線を照射して離散的な回折スポットを生成し、該回折スポットのうち予め決めた回折スポットを選択し、該選択された回折スポットについて前記試料を前記単色X線の入射位置を中心とし該単色X線に対して相対的に回動させて回折ピークの形状を測定し、該回折ピークの分散にかかる係数を算出し、該係数がニッケル基超合金の劣化と対応する事実に基づいて前記ニッケル基超合金の劣化状態を診断するニッケル基超合金の劣化診断方法。 A nickel-based superalloy sample in which nickel-base intermetallic compound precipitation phase (γ 'phase) is scattered in a consistent manner in a nickel solid solution matrix (γ phase) is irradiated with monochromatic X-rays to form discrete diffraction spots. A predetermined diffraction spot is selected from the diffraction spots, and the sample is rotated relative to the monochromatic X-ray with respect to the monochromatic X-ray with respect to the incident position of the monochromatic X-ray. Measuring the shape of the diffraction peak, calculating a coefficient for dispersion of the diffraction peak, and diagnosing the deterioration state of the nickel-base superalloy based on the fact that the coefficient corresponds to the deterioration of the nickel-base superalloy. Degradation diagnosis method for superalloys. 前記予め決めた回折スポットは、前記ニッケル基金属間化合物析出相(γ’相)の規則格子回折に起因する回折スポットであることを特徴とする請求項1記載のニッケル基超合金の劣化診断方法。 2. The method for diagnosing deterioration of a nickel-base superalloy according to claim 1, wherein the predetermined diffraction spot is a diffraction spot caused by regular lattice diffraction of the nickel-base intermetallic compound precipitation phase (γ ′ phase). . 前記予め決めた回折スポットは、ミラー指数(210)または(310)で表わされる結晶面に起因する回折スポットであることを特徴とする請求項1記載のニッケル基超合金の劣化診断方法。 2. The method for diagnosing deterioration of a nickel-base superalloy according to claim 1, wherein the predetermined diffraction spot is a diffraction spot caused by a crystal plane represented by a Miller index (210) or (310). 前記回折スポットのピーク形状は、入射するX線と回折光を検出するセンサの角度関係を固定し、該X線の照射位置を通りかつ該入射X線と前記検出センサがなす面に垂直な軸を中心として測定対象物を揺動させることにより、該測定対象物への入射X線の入射角を変化させて、得られた回折X線強度を前記測定対象物の揺動角度に対してプロットするθロッキングカーブ法により測定することを特徴とする請求項1から3のいずれかに記載のニッケル基超合金の劣化診断方法。 The peak shape of the diffraction spot is an axis that fixes the angle relationship between the incident X-ray and the sensor that detects the diffracted light, passes through the irradiation position of the X-ray, and is perpendicular to the plane formed by the incident X-ray and the detection sensor. The incident angle of the incident X-ray to the measurement object is changed by oscillating the measurement object around the center, and the obtained diffracted X-ray intensity is plotted against the oscillation angle of the measurement object. 4. The method for diagnosing deterioration of a nickel-base superalloy according to claim 1, wherein the deterioration is measured by a θ rocking curve method. 前記回折ピークの分散係数は、回折ピーク半価幅であることを特徴とする請求項1から4のいずれかに記載のニッケル基超合金の劣化診断方法。 The method for diagnosing deterioration of a nickel-base superalloy according to any one of claims 1 to 4, wherein the dispersion coefficient of the diffraction peak is a half-value width of the diffraction peak. 前記劣化状態は、クリープ寿命消費率に基づいて得られるものであることを特徴とする請求項1から5のいずれかに記載のニッケル基超合金の劣化診断方法。 The deterioration diagnosis method for a nickel-base superalloy according to any one of claims 1 to 5, wherein the deterioration state is obtained based on a creep life consumption rate. 請求項1から6のいずれかに記載のニッケル基超合金の劣化診断方法により得られた劣化診断結果に基づいて該ニッケル基超合金の余寿命を推定するニッケル基超合金の余寿命推定方法。 A nickel base superalloy remaining life estimation method for estimating a remaining life of a nickel base superalloy based on a deterioration diagnosis result obtained by the nickel base superalloy deterioration diagnosis method according to any one of claims 1 to 6. 前記単色X線は放射光であることを特徴とする請求項1から7のいずれかに記載のニッケル基超合金の劣化診断方法。 The method for diagnosing deterioration of a nickel-base superalloy according to any one of claims 1 to 7, wherein the monochromatic X-ray is synchrotron radiation. 試料を把持して回動させる試料台と、単色X線を前記試料台に照射する単色X線照射装置と、発生する離散的な回折スポットのX線強度を測定するX線センサと、前記X線照射装置と前記試料台と前記X線センサの配置を調整するセンサ位置調整装置と、前記X線センサの出力を入力して回折ピークの形状を特定する測定データ処理装置と、回折ピーク形状とクリープ寿命消費率の関数を格納する記憶装置と、前記特定された回折ピーク形状に基づき前記関数を用いてクリープ寿命消費率を算出してあるいは該クリープ寿命消費率に基づいて該ニッケル基超合金の余寿命を推定して提示する演算装置とから構成され、前記X線センサが測定対象とする回折スポットに照準を合わせた後は前記試料台を前記X線照射装置に対して相対的に回動させることにより対象の回折ピークの形状を測定する、ニッケル基超合金の劣化診断装置。 A sample stage for gripping and rotating the sample, a monochromatic X-ray irradiation apparatus for irradiating the sample stage with monochromatic X-rays, an X-ray sensor for measuring the X-ray intensity of the generated discrete diffraction spots, and the X A sensor position adjusting device for adjusting the arrangement of the X-ray sensor, a measurement data processing device for specifying the shape of a diffraction peak by inputting the output of the X-ray sensor, a diffraction peak shape, A storage device for storing a function of a creep life consumption rate, and calculating a creep life consumption rate using the function based on the identified diffraction peak shape or of the nickel-base superalloy based on the creep life consumption rate And an arithmetic unit that estimates and presents the remaining life, and after the X-ray sensor is aimed at a diffraction spot to be measured, the sample stage is rotated relative to the X-ray irradiation device The Measuring the shape of the diffraction peaks of interest by Rukoto, deterioration diagnosis apparatus for nickel-base superalloys. 前記測定する回折スポットは前記ニッケル基金属間化合物析出相(γ’相)の規則格子回折に起因する回折スポットであり、前記回折ピークの形状は回折ピーク半価幅により代表され、前記劣化状態はクリープ寿命消費率に基づいて得られるものであることを特徴とする請求項9記載のニッケル基超合金の劣化診断装置。 The diffraction spot to be measured is a diffraction spot due to regular lattice diffraction of the nickel-based intermetallic compound precipitation phase (γ ′ phase), the shape of the diffraction peak is represented by the half-width of the diffraction peak, and the deterioration state is The deterioration diagnosis apparatus for nickel-base superalloys according to claim 9, wherein the deterioration diagnosis apparatus is obtained based on a creep life consumption rate. 前記単色X線照射装置は放射光発生装置であることを特徴とする請求項9または10記載のニッケル基超合金の劣化診断装置。
11. The nickel-base superalloy deterioration diagnosis device according to claim 9, wherein the monochromatic X-ray irradiation device is a synchrotron radiation generator.
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