WO2016075953A1 - 高温部材の温度推定方法、準安定正方相の含有量測定方法、劣化判定方法 - Google Patents
高温部材の温度推定方法、準安定正方相の含有量測定方法、劣化判定方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 75
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 title claims abstract description 29
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/10—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/0088—Radiation pyrometry, e.g. infrared or optical thermometry in turbines
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/02—Constructional details
- G01J5/04—Casings
- G01J5/046—Materials; Selection of thermal materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/10—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors
- G01J2005/103—Absorbing heated plate or film and temperature detector
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/80—Calibration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/63—Specific applications or type of materials turbine blades
Definitions
- the present invention relates to a temperature estimation method for a high temperature member, a metastable square phase content measurement method, and a degradation determination method.
- Patent Document 1 discloses a temperature at which the amount of M phase (monoclinic phase) contained in TBC is measured using X-ray diffraction, and the surface temperature of TBC is calculated based on the measured amount of monoclinic phase. An estimation method is described.
- the TBC is initially composed of a tough crystal called a T ′ phase (metastable square phase: Tetragonal® Prime).
- T ′ phase metalstable square phase: Tetragonal® Prime
- T ′ phase metalstable square phase: Tetragonal® Prime
- C phase cubic phase
- T phase tetragonal phase
- M phase monoclinic phase
- Patent Document 1 focuses on the content of the monoclinic phase (M phase) generated after the temperature of the TBC decreases, but focuses on the content of the T ′ phase and includes T in the TBC. If the degree of decomposition of the 'phase is examined and the temperature can be estimated based on the content of the T' phase, it is considered that a more accurate TBC surface temperature can be estimated. However, no such temperature estimation method has been proposed so far.
- the present invention provides a temperature estimation method, a metastable square phase content measurement method, and a degradation determination method that can solve the above-described problems.
- the temperature estimation method measures the content of the metastable square phase contained in the coating layer formed on the surface of the high temperature member by X-ray diffraction or Raman spectroscopy, and measures the content. Based on the content of the metastable tetragonal phase, the surface temperature of the high temperature member is estimated.
- the temperature estimation method includes a plurality of test members for a plurality of coating layers subjected to heat treatment for a plurality of heating times and a plurality of heating times determined for each of a plurality of predetermined heating temperatures.
- Each of the plurality of tests by Rietveld analysis of each of the diffraction results measured by the line diffraction method and the diffraction results by the X-ray diffraction method for members whose metastable tetragonal phase, tetragonal phase and cubic phase content are known in advance.
- the measurement result of the measurement member by the X-ray diffraction method, and the metastable square phase, the square phase, and the cubic phase in advance Performing a Rietveld analysis of the diffraction result by X-ray diffraction method for a member whose content is known, calculating the content of the metastable square phase contained in the measurement member, and heating the measurement member Calculating the heating temperature of the measurement member based on the time, the calculated content of the metastable square phase contained in the measurement member, and the relational expression.
- the temperature estimation method includes a plurality of test members for a plurality of coating layers subjected to heat treatment for a plurality of heating times and heat treatments determined for each of a plurality of predetermined heating temperatures.
- Each of the plurality of tests by Rietveld analysis of each of the diffraction results measured by the line diffraction method and the diffraction results by the X-ray diffraction method for members whose metastable tetragonal phase, tetragonal phase and cubic phase content are known in advance.
- the step of calculating the correlation between the characteristic amount of the spectrum and the content of the metastable tetragonal phase contained in each of the calculated test members, and the coating subjected to heat treatment at a heating temperature equal to or higher than a predetermined temperature A measurement member of a layer, and when the heating time in the heat treatment is known, the spectral feature obtained by measuring the measurement member by Raman spectroscopy and the correlation, The step of calculating the content of the metastable square phase contained in the measurement member, the heating time of the measurement member, the calculated content of the metastable square phase contained in the measurement member, and the relational expression Calculating the heating temperature of the measurement member based on the above.
- the relational expression is based on the fact that the decomposition amount of the metastable square phase and the 1/4 power of the heating time are in a linear relationship.
- the metastable tetragonal phase content measurement method is a method of measuring the metastable tetragonal phase content contained in the coating layer formed on the surface of the high temperature member, Each of the diffraction results measured by the X-ray diffractometry for the coating layer measurement member subjected to the heat treatment at a heating temperature equal to or higher than a predetermined temperature, and the contents of the metastable square phase, the square phase, and the cubic phase in advance A step of calculating a content of a metastable square phase contained in each of the plurality of measurement members by performing Rietveld analysis of a diffraction result of the known member by an X-ray diffraction method;
- the metastable tetragonal phase content measurement method is a method of measuring the metastable tetragonal phase content contained in the coating layer formed on the surface of the high temperature member,
- Each of the diffraction results measured by the X-ray diffraction method for a plurality of test members for the plurality of coating layers subjected to heat treatment for a plurality of heating times determined for each of a plurality of predetermined heating temperatures, and a metastable square phase in advance Calculating the content of the metastable tetragonal phase contained in each of the plurality of test members by Rietveld analysis of the diffraction result by X-ray diffractometry for a member whose content of the square phase and the cubic phase is known And a correlation between a characteristic amount of a spectrum obtained by measuring the plurality of test members by Raman spectroscopy and a content of the metastable square phase contained in each of the calculated test members.
- a measuring member of the coating layer that has been heat-treated at a heating temperature equal to or higher than a predetermined temperature, and the measuring member is subjected to Raman spectroscopy when the heating time in the heat-treatment is known And calculating the content of the metastable square phase contained in the measurement member based on the feature amount of the spectrum obtained by the measurement and the correlation.
- the deterioration determination method calculates the content of the metastable square phase contained in the measurement member by the above-described metastable square phase content measurement method, and the measurement member
- the deterioration degree of the high temperature member is calculated based on a predetermined correspondence relationship between the content of the metastable square phase contained in and the deterioration degree of the high temperature member.
- the surface temperature of the high temperature member can be estimated.
- FIG. 1 is a schematic view of a high temperature member in a first embodiment according to the present invention.
- FIG. 2 is a diagram for explaining a change in the crystal structure of the topcoat layer of the high temperature member in the first embodiment according to the present invention.
- the surface of the heat-resistant alloy layer as a base material has low thermal conductivity for the purpose of improving heat insulation and durability.
- Thermal spray coating is applied by spraying a thermal spray material (for example, a ceramic material having low thermal conductivity).
- TBC Thermal spray coating
- the turbine blade 1 is composed of a high temperature member 10.
- the high temperature member 10 is formed of a base material 11 made of a heat resistant alloy and a thermal barrier coating (TBC) layer 12.
- TBC thermal barrier coating
- the thermal barrier coating layer 12 is formed of a metal bond coat layer 13 for improving adhesion and oxidation resistance with the base material 11 and a ceramic top coat layer 14 for improving thermal barrier properties.
- the FIG. 2 shows how the YSZ crystal structure of the topcoat layer changes with the operating time of the gas turbine when YSZ (yttria stabilized zirconia) is used as an example of the topcoat layer. .
- the sprayed YSZ is a tough crystal called a T ′ phase (metastable tetragonal phase) generated by quenching almost 100%. Therefore, almost all YSZ at the start of operation of the gas turbine is occupied by the T ′ phase.
- the T ′ phase is relatively stable, but when it is exposed to a high temperature exceeding 1200 ° C., it is gradually decomposed into a T phase (tetragonal phase) and a C phase (cubic phase).
- the T ′ phase is decomposed into the T phase and the C phase
- the YSZ of the top coat layer 14 formed on the surface of the high temperature member 10 includes the T ′ phase, T Phase and C phase
- the T phase is stable at high temperatures, but decomposes into an M phase (monoclinic phase) and a C phase when cooled to about 600 ° C. or lower. Therefore, when the operation period of the gas turbine ends and the operation is stopped, the YSZ is gradually cooled. Therefore, the T phase is decomposed, and the YSZ at the time of the operation stop includes the T ′ phase, the T phase, and the M phase. Phase and C phase are mixed.
- the cooling rate at this time affects the decomposition of the T phase into the M phase and the C phase. Since the surface temperature of the top coat layer 14 of the turbine blade 1 is also related to the cooling method of the turbine blade 1, for example, it is very useful information in designing the gas turbine, and it is important to obtain an accurate temperature as much as possible. It is. For example, when the surface temperature of TBC is estimated based on the contents of T phase and M phase, since the contents are affected by the cooling rate of the turbine, there is a possibility that an accurate temperature at a high temperature cannot be estimated.
- the surface temperature of the topcoat layer 14 during operation of the gas turbine can be estimated based on the content (remaining amount) of the T ′ phase
- the content of the T ′ phase affects, for example, the cooling rate of the turbine. Therefore, the surface temperature of the TBC can be estimated more accurately.
- a method for estimating the surface temperature of the topcoat layer 14 during heating based on the content of the T ′ phase is provided.
- the surface temperature of the topcoat layer 14 is referred to as a TBC surface temperature.
- FIG. 3 is a first diagram illustrating derivation of a relational expression among the content of the T ′ phase, the heating time, and the TBC surface temperature in the first embodiment according to the present invention.
- FIG. 3 is a diagram for explaining the creation of base data for identifying the content of the T ′ phase contained in the topcoat layer 14.
- the TBC surface temperature is estimated based on the content of the T ′ phase contained in the topcoat layer 14. Therefore, it is important to accurately know the content of the T ′ phase of the TBC to be measured. Therefore, in the present embodiment, base data is created by using, as a sample, a test piece of the topcoat layer 14 exposed to various temperatures for various times.
- a heat treatment is performed in which a test piece of the topcoat layer 14 having the same composition as the actual machine is heated to a predetermined temperature for a predetermined time.
- the predetermined temperature is, for example, 1100 ° C., 1200 ° C., 1300 ° C., 1400 ° C.
- the predetermined time is, for example, 100 hours, 1000 hours, or 10000 hours.
- the X-ray diffraction measurement is performed on each of the test pieces subjected to the heat treatment under these various conditions, and the diffraction result [measured XRD (X-ray diffraction) profile] is accumulated.
- the T ′ phase, T phase, M phase, and C phase included in the test piece can be identified from the measurement result by the X-ray diffraction method, but the lattice constants of T ′ phase, T phase, and C phase are close.
- the peaks of the measurement results overlap and it is difficult to identify the T ′ phase, the T phase, and the C phase. Therefore, the T ′ phase, T phase, and C phase of the test piece are identified by Rietveld analysis.
- the measured XRD profile of each test piece and the theoretical XRD profile created in advance are analyzed by, for example, full pattern fitting by the nonlinear least square method, and the theoretical XRD profile that fits most accurately is obtained.
- the theoretical XRD profile is a theoretical value of a diffraction result by an X-ray diffraction method generated by simulation or the like for each pattern assuming various patterns of T ′ phase, T phase, and C phase.
- the contents of the T ′ phase, T phase, and C phase of the test piece are assumed for the determined theoretical XRD profile. The content is determined.
- FIG. 4 is a second diagram illustrating the derivation of the relational expression among the T ′ phase content, the heating time, and the TBC surface temperature in the first embodiment according to the present invention.
- FIG. 5 is a third diagram illustrating the derivation of the relational expression among the T ′ phase content, the heating time, and the TBC surface temperature in the first embodiment according to the present invention.
- FIG. 6 is a fourth diagram illustrating the derivation of the relational expression among the T ′ phase content, the heating time, and the TBC surface temperature in the first embodiment according to the present invention.
- the vertical axis (1- ⁇ T′-YSZ ) in FIG. 4 indicates the amount of decomposition of the T ′ phase contained in the test piece.
- the horizontal axis represents a value obtained by raising the time (t) during which the test piece was heat-treated to the 1/4 power.
- the diamond points indicate the data of the test piece heat-treated at 1100 ° C.
- the square points are 1200 ° C
- the triangular points are 1300 ° C
- the round points are 1400 ° C.
- the data of the test piece performed are shown. As shown in FIG.
- the value obtained by dividing the decomposition amount (reduction amount) of the T ′ phase accompanying the heat treatment and the heat treatment time (t) to a 1 ⁇ 4 power has a linear relationship.
- the decomposition amount of the T ′ phase and the 1 ⁇ 4 power treatment time (t) can be expressed by the following equations.
- FIG. 5 is a table summarizing the heating temperature (T) and the value of the slope k of the above equation (1).
- T heating temperature
- 1 / T is the reciprocal of the absolute temperature of T (unit: K).
- lnk is log e k.
- the heating temperature (T) can be calculated by the equation (4).
- the heating temperature (T) is the temperature of the furnace when the test piece of the topcoat layer is charged into the furnace, for example, and can be regarded as the TBC surface temperature in the actual machine. That is, if the content of the T ′ phase contained in the actual topcoat layer 14 is obtained, the TBC surface temperature can be obtained by the equation (4).
- the processing in the preparation stage of this embodiment is the processing in the preparation stage of this embodiment.
- the measured XRD profile of each test piece subjected to the heat treatment under the various conditions described with reference to FIG. 3 and the inclusion of the T ′ phase, T phase, and C phase for each test piece after the heat treatment The relationship between the amount (particularly the content of the T ′ phase) and the relationship between the content of the T ′ phase, the heating time, and the TBC surface temperature described with reference to FIGS. 4 to 6 [Formula (4) ] Is obtained.
- FIG. 7 is a flowchart of the TBC surface temperature estimation method according to the first embodiment of the present invention.
- Steps S11 to S13 are preparatory steps. Since these processes are as described above, they will be briefly described.
- a plurality of test pieces of the topcoat layer 14 are prepared, and a test piece obtained by performing heat treatment for a predetermined time at a predetermined temperature for each test piece is created (step S11).
- each test piece is measured by the X-ray diffraction method, and the T ′ phase, T phase, C phase, and M phase are identified from the diffraction pattern of the diffraction result, and the content of each phase is obtained.
- theoretical diffraction results (theoretical XRD profiles) for various T ′ phase, T phase, and C phase content patterns. )
- a relational expression between the T ′ phase content, the heating time, and the TBC surface temperature during heating is derived by the procedure described with reference to FIGS. 3 to 6 (step S13).
- the TBC surface temperature of the actual machine is estimated.
- a TBC (top coat layer) to be measured is obtained from a gas turbine after operation.
- X-ray diffraction and Rietveld analysis are performed on the obtained measurement target TBC as in step S12.
- the target to be fitted with the measurement result of the measurement target TBC by the X-ray diffraction method is the content of the T ′ phase, the T phase, and the C phase
- the test piece analyzed in step S12 The diffraction result by the X-ray diffraction method may be used, or the theoretical XRD profile may be used. Thereby, the content of the T ′ phase in the measurement target TBC is obtained (step S14).
- the content of the T ′ phase calculated in step S14 and the operation time of the gas turbine in the relational expression [for example, equation (4)] of the T ′ phase content calculated in step S13, the heating time, and the TBC surface temperature. Is assigned. It is assumed that the operation time of the gas turbine is known.
- the substituted expression is solved for the TBC surface temperature (T), and the TBC surface temperature is calculated (step S15).
- the calculated value is an estimated value of the surface temperature of the topcoat layer 14 during operation (heating) of the gas turbine according to the present embodiment.
- the content of the T ′ phase of the topcoat layer 14 can be accurately obtained by X-ray diffraction and Rietveld analysis. Further, the T ′ phase is decomposed into a stable T phase governed by a diffusion phenomenon in a high temperature environment, the decomposition rate at that time changes according to the temperature, and the decrease amount of the T ′ phase at each temperature and the TBC That the heating time of 1 ⁇ 4 is linearly related (FIG.
- FIG. 8 is a diagram showing the relationship between the position of the Raman peak and the content of the T ′ phase in the second embodiment according to the present invention.
- the vertical axis in FIG. 8 is the position of the Raman peak, and the horizontal axis is the content of the T ′ phase.
- 144cm -1, 252cm -1, 258cm -1 linear focused on Raman peak located near 463cm -1, as shown in FIG. 8 and rearranging the relationship of the Raman peak positions with T'-phase content of these neighboring A relationship was obtained.
- FIG. 9 is a diagram showing the relationship between the half-value width of the Raman peak and the content of the T ′ phase in the second embodiment according to the present invention.
- the vertical axis in FIG. 9 is the half width of the Raman peak, and the horizontal axis is the content of the T ′ phase.
- Figure 8 Similar to 144cm -1, 252cm -1, 258cm -1 , focused on Raman peak near 463cm -1, and rearranging the relationship of the half value width and T'-phase content of the Raman peaks of these neighboring FIG A linear relationship as shown in FIG.
- FIG. 10 is a diagram showing the relationship between the intensity ratio of the Raman peak and the content of the T ′ phase in the second embodiment according to the present invention.
- the vertical axis in FIG. 10 is the Raman peak intensity ratio, and the horizontal axis is the content of the T ′ phase.
- measurement by Raman spectroscopy is performed on a test piece whose T ′ phase content is known by the same X-ray diffraction method and Rietveld analysis as in the first embodiment.
- the characteristic amount (peak position, half width, peak intensity ratio) of the spectrum of the measurement result is extracted, and a correlation (for example, FIGS. 8 to 10) between the extracted characteristic amount and the content of the T ′ phase is obtained.
- a relational expression [Expression (4)] among the content of the T ′ phase, the heating time, and the TBC surface temperature is obtained.
- Step S11 to S13 are preparatory steps. These processes are the same as in the first embodiment. That is, the test piece which heat-processed on various conditions is created (step S11), and content, such as T 'layer, is calculated
- Raman spectroscopic measurement is next performed on each test piece. Focusing on a predetermined Raman peak of the measurement result obtained by Raman spectroscopy, the correlation between the Raman peak position, the half-value width of the Raman peak, and the Raman peak intensity ratio and the content of the T ′ phase obtained in step S12 Organizing the relationship, the relationship between the Raman peak position and the T ′ phase content (for example, FIG. 8), the relationship between the half width of the Raman peak and the T ′ phase content (for example, FIG. 9), the Raman peak intensity ratio and the T At least one of the relational expressions of the 'phase content (for example, FIG. 10) is calculated for each focused Raman peak (step S16).
- the above is the preparation stage in this embodiment.
- the TBC surface temperature of the high-temperature member 10 of the actual machine is estimated.
- a TBC (top coat layer) to be measured is obtained from a gas turbine after operation. Measurement by Raman spectroscopy is performed on the obtained measurement target TBC. Then, from the measurement result, at least one of the Raman peak position, the Raman peak half width, and the peak intensity ratio is obtained for the measurement target TBC (step S17).
- the Raman peak position, the Raman peak half width, and the peak intensity ratio obtained in step S17 are substituted into the corresponding relational expression calculated in step S16, and the content of the T ′ phase contained in the measurement target TBC is calculated ( Step S18).
- the substituted expression is solved for the TBC surface temperature (T), and the TBC surface temperature is calculated (step S15).
- the calculated value is an estimated value of the TBC surface temperature during heating according to the present embodiment.
- the first embodiment Rietveld analysis was performed in order to obtain the content of the T ′ phase contained in the actual topcoat layer 14.
- Rietveld analysis often takes time and effort.
- the content of the T ′ phase contained in the actual topcoat layer 14 by using Raman spectroscopy that can be performed relatively easily by anyone instead of the X-ray diffraction method and Rietveld analysis. Ask for. Therefore, if the preparation stage is completed, the content of the T ′ phase can be obtained relatively easily. Further, if the content of the T ′ phase is obtained, the TBC surface temperature can be calculated as in the first embodiment. Therefore, according to the present embodiment, in addition to the effects of the first embodiment, the surface temperature of the TBC can be estimated more easily regardless of human skills.
- Raman spectroscopy measurement can be performed on a turbine blade while it is mounted on an actual machine.
- the TBC surface temperature can be estimated by the following method.
- a method for estimating the surface temperature according to the third embodiment will be described with reference to FIGS.
- the heat treatment is performed on the test piece of the top coat layer 14 under various conditions.
- the measurement by a Raman spectroscopy is performed with respect to the test piece after heat processing.
- the Raman spectrum obtained by the measurement is fitted with a Gaussian function and a Lorentz function to obtain a Raman peak position, a full width at half maximum, and a peak intensity.
- FIG. 12 to FIG. 14 are examples of results obtained by arranging measured values by Raman spectroscopy using LMP using actual test pieces (T: heating temperature, t: heat treatment time).
- FIG. 12 is a diagram showing the relationship between the Raman peak position and the LMP value in the third embodiment.
- 252cm -1, 258cm -1, 463cm -1 focusing on the Raman peak located near 635cm -1, and rearranging the relationship between the Raman peak and LMP value of these near obtained linear relationship as shown in FIG. 12 It was.
- FIG. 13 is a diagram illustrating the relationship between the half-value width of the Raman peak and the LMP value in the third embodiment.
- the vertical axis in FIG. 13 is the half width of the Raman peak, and the horizontal axis is the LMP value.
- 144cm -1, the 258cm -1, 321cm -1, focusing on the Raman peak located near 463cm -1 organize the relationship between the half width and LMP value of the Raman peak of these near straight line as shown in FIG. 13 A relationship was obtained.
- FIG. 14 is a diagram showing the relationship between the intensity ratio of the Raman peak and the LMP value in the third embodiment.
- the vertical axis in FIG. 14 is the Raman peak intensity ratio, and the horizontal axis is the LMP value.
- a linear relationship as shown in FIG. 14 was obtained.
- the relationship between the result of measurement by Raman spectroscopy using these test pieces and the LMP value is recorded. The above is the preparation stage process.
- the TBC surface temperature of the actual machine is estimated.
- a TBC to be measured is obtained, and the measurement target TBC is measured by Raman spectroscopy.
- at least one of the Raman peak position, the Raman peak half width, and the peak intensity ratio for the measurement target TBC is obtained from the measurement result.
- the Raman peak position is obtained, the LMP value of the measurement target TBC is obtained from the relationship illustrated in FIG.
- the Raman peak half width is obtained, the LMP value of the measurement target TBC is obtained from the relationship illustrated in FIG.
- the peak intensity ratio is obtained, the LMP value of the measurement target TBC is obtained from the relationship illustrated in FIG.
- T ⁇ [5 + ln (t)] LMP value obtained based on FIGS. 12 to 14 (5)
- Equation (5) the TBC surface temperature according to the third embodiment can be obtained.
- 4388466 discloses a laser type in which the TBC side of a test piece is heated by a laser beam, and the base material on the back side of the test piece (the side opposite to the side on which TBC is applied) is cooled with a cooling gas.
- a method is described in which a predetermined thermal load is repeatedly applied to a test piece by a thermal cycle test apparatus, and the number of repetitions when TBC peeling occurs is evaluated as a thermal cycle life. Using this method, for example, a heat load is repeatedly applied to a test piece for a heat resistance test until TBC peeling occurs.
- the X-ray diffraction method and the Rietveld analysis are performed on the test piece every predetermined number of times to obtain the content of the T ′ phase contained in the TBC of the test piece.
- the content of the T ′ phase contained in the TBC of the test piece is determined using the measurement result of the Raman spectroscopy with respect to the TBC of the test piece and the relational expression obtained in step S16.
- the relationship between the number of repetitions and the degree of deterioration is defined from the number of repetitions when TBC peeling occurs (for example, if the TBC peels after 100 times, the degree of deterioration is 50% at 50 times).
- the correspondence relationship between the content of the T ′ phase and the degree of deterioration is recorded.
- the TBC to be measured is obtained from the actual machine, and the content of the T ′ phase of the measurement target TBC is calculated by the same method as in the first embodiment or the second embodiment. Then, it is possible to determine the degree of deterioration of the actual turbine member based on the correspondence relationship between the content of the T ′ phase and the degree of deterioration created in advance using a test piece for a heat resistance test.
- YSZ has been described as an example of the material of the topcoat layer 14, but the present invention is not limited to this.
- oxides that can partially stabilize zirconia (ZrO 2 ) (alkaline such as MgO and CaO, light rare earth such as Sc 2 O 3 and Y 2 O 3 , La 2 O 3 , Ce 2) O 3 , Pr 2 O 3 , Nd 2 O 3 , Pm 2 O 3 , Sm 2 O 3 , Eu 2 O 3 , Gd 2 O 3 , Tb 2 O 3 , Dy 2 O 3 , Ho 2 O 3 , Er 2
- It may be a stabilized zirconia (for example, YbSZ) containing one kind or two or more kinds of heavy rare earth such as O 3 , Tm 2 O 3 , Yb 2 O 3 , Lu 2 O 3 .
- test piece of the top coat layer 14 is an example of a test member.
- the measurement target TBC is an example of a measurement member.
- the surface temperature of the high temperature member can be estimated.
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Abstract
Description
本願は、2014年11月12日に、日本に出願された特願2014-229619号に基づき優先権を主張し、その内容をここに援用する。
以下、本発明の第一実施形態による制御システムを図1~図6を参照して説明する。
図1は、本発明に係る第一実施形態における高温部材の概略図である。
図2は、本発明に係る第一実施形態における高温部材のトップコート層の結晶構造の変化を説明する図である。
ガスタービンの動静翼、分割環、燃焼器などの高温に曝される高温部材には、母材となる耐熱合金層の表面に、遮熱性及び耐久性を向上させる目的で、熱伝導率の低い溶射材(例えば、熱伝導率の低いセラミックス系材料)を溶射して遮熱コーティング(TBC)が施されている。図1において、タービン翼1は、高温部材10で構成されている。高温部材10は、耐熱合金製の母材11と、遮熱コーティング(TBC)層12から形成される。さらに、遮熱コーティング層12は、母材11との密着性および耐酸化性を向上するための金属製のボンドコート層13と、遮熱性を向上するセラミックス製のトップコート層14とから形成される。図2は、トップコート層の一例としてYSZ(イットリア安定化ジルコニア)を用いた場合の、トップコート層のYSZの結晶構造が、ガスタービンの運転時間と共に変化している様子を示したものである。
図3は、トップコート層14に含まれるT´相の含有量を同定するためのベースデータの作成を説明する図である。上述のとおり、本実施形態では、トップコート層14に含まれるT´相の含有量に基づいてTBC表面温度を推定する。従って、測定対象となるTBCのT´相の含有量を正確に知ることが重要である。その為、本実施形態では、さまざまな温度に、さまざまな時間だけ曝したトップコート層14の試験片をサンプルとして、ベースデータを作成する。まず、実機と同じ組成を有するトップコート層14の試験片を所定時間、所定温度に加熱する加熱処理を行う。所定温度とは、例えば、1100℃、1200℃、1300℃、1400℃である。所定時間とは、例えば、100時間、1000時間、10000時間などである。次に、これら様々な条件で加熱処理を行った試験片のそれぞれに対してX線回折法による測定を行い、回折結果[測定XRD(X-ray diffraction)プロファイル]を蓄積する。ここで、X線回折法による測定結果によって試験片に含まれるT´相、T相、M相、C相を同定できればよいが、T´相、T相、C相については、格子定数が近く、測定結果のピークが重なり、T´相、T相、C相を同定することが難しい。そこで、リートベルト解析によって、試験片のT´相、T相、C相を同定する。
図4は、本発明に係る第一実施形態におけるT´相の含有量と加熱時間とTBC表面温度との関係式の導出を説明する第二の図である。
図5は、本発明に係る第一実施形態におけるT´相の含有量と加熱時間とTBC表面温度との関係式の導出を説明する第三の図である。
図6は、本発明に係る第一実施形態におけるT´相の含有量と加熱時間とTBC表面温度との関係式の導出を説明する第四の図である。
図4は、本発明に係る第一実施形態におけるT´相の分解量と加熱処理時間との関係を示している。
図4の縦軸(1-αT´-YSZ)は、試験片に含まれるT´相の分解量を示している。横軸は、試験片を加熱処理した時間(t)を1/4乗した値である。また、ひし型の点は、1100℃で加熱処理を行った試験片のデータを示し、同様に四角の点は1200℃、三角の点は1300℃、丸の点は1400℃でそれぞれ加熱処理を行った試験片のデータを示している。図4に示すように、1100~1400℃の各温度において,熱処理に伴うT´相の分解量(減少量)と加熱処理時間(t)を1/4乗した値は直線関係にある。各温度において、直線の傾きをkとすると、T´相の分解量と加熱処理時間(t)の1/4乗は、次式で表すことができる。
また、図6により1/Tとlnkの関係を満足する直線の式を求めると次式(3)が求められる。
y=-8692.7x+3.9126 ・・・(3)
さらに、切片のlnk0=3.9126、傾きのQ/R=-8692.7[Rは気体定数:8.31J/(mol・K)]から、k0=50.0、Q=7.2×105J/molを求めることができる。この値を式(2)に代入すると次式(4)を得る。
図7は、本発明に係る第一実施形態におけるTBC表面温度推定方法のフローチャートである。
ステップS11~S13までは、準備段階の処理である。これらの処理については上述のとおりであるので簡単に説明する。まず、トップコート層14の試験片を複数用意し、それぞれの試験片について所定の温度で所定時間だけ加熱処理を行った試験片を作成する(ステップS11)。次に、各試験片についてX線回折法による測定を行い、回折結果の回折パターンからT´相、T相、C相、M相を同定し、各相の含有量を求める。但し、T´相、T相、C相については、X線回折法による同定が難しいので、様々なT´相、T相、C相の含有量のパターンに対する理論的な回折結果(理論XRDプロファイル)を用いたリートベルト解析によって各相の含有量を求める(ステップS12)。次に、図3~図6を用いて説明した手順でT´相の含有量と加熱時間と加熱時におけるTBC表面温度との関係式を導出する(ステップS13)。
次にステップS13で算出したT´相の含有量と加熱時間とTBC表面温度の関係式[例えば、式(4)]にステップS14で求めたT´相の含有量とガスタービンの運転時間とを代入する。ガスタービンの運転時間は、既知であるとする。代入した式をTBC表面温度(T)について解き、TBC表面温度を算出する(ステップS15)。算出した値が本実施形態によるガスタービン運転時(加熱時)におけるトップコート層14の表面温度の推定値である。
本実施形態では、X線回折法とリートベルト解析によってトップコート層14のT´相の含有量を正確に求めることができる。また、T´相が高温環境において拡散現象に支配され安定なT相に分解されること、そのときの分解速度が温度に応じて変わること、またそれぞれの温度におけるT´相の減少量とTBCの加熱時間の1/4乗が線形関係にある(図4)ことと、アレニウスの式[k=A×exp(-Q/RT)、A:定数、Q:活性化エネルギー、R:気体定数、T:絶対温度]から、T´相の含有量と加熱時間とTBC表面温度の関係式[例えば、式(4)]を求めることができる。これにより、T´相の含有量のみに基づいてTBC層温度を推定する事ができる。従って、例えば、ガスタービンの冷却速度等による影響を受けることなく、より精度の高い表面温度を推定することができる。
以下、本発明の第二実施形態による温度推定方法を図8~図11を参照して説明する。
第二実施形態では、測定対象とするTBCのT´相の含有量を算出するにあたって、ラマン分光法による測定を行う。本実施形態では、まず、第一実施形態と同様に、様々な条件で加熱処理を行った実機と同じ組成を有する試験片に対してX線回折法及びリートベルト解析を行い、それぞれの試験片におけるT´相の含有量を求める。次にT´相の含有量がわかった各試験片に対してラマン分光法による測定を行う。そして、ラマン分光法の測定結果とT´相の含有量を対応付けて記録する。
次に実際の試験片を用いて上記のラマン分光法による測定を行った結果を図8~図11を用いて説明する。
図8の縦軸は、ラマンピークの位置であり、横軸はT´相の含有量である。144cm-1、252cm-1、258cm-1、463cm-1付近に位置するラマンピークに着目し、これらの近傍のラマンピーク位置とT´相含有量の関係を整理すると図8に示すような直線関係が得られた。
図9の縦軸は、ラマンピークの半値幅であり、横軸はT´相の含有量である。図8と同様に144cm-1、252cm-1、258cm-1、463cm-1付近のラマンピークに着目し、これらの近傍のラマンピークの半値幅とT´相含有量の関係を整理すると図9に示すような直線関係が得られた。
図10の縦軸は、ラマンピークの強度比であり、横軸はT´相の含有量である。144cm-1のピーク強度と463cm-1のピーク強度の比(144cm-1のピーク強度÷463cm-1のピーク強度)、144cm-1のピーク強度と635cm-1のピーク強度の比(144cm-1のピーク強度÷653cm-1のピーク強度)、463cm-1のピーク強度と635cm-1のピーク強度の比(463cm-1のピーク強度÷635cm-1のピーク強度)に着目し、これらのピーク強度比とT´相含有量の関係を整理すると図10に示すような直線関係が得られた。
図11に、本発明に係る第二実施形態におけるTBC表面温度推定方法のフローチャートを示す。
ステップS11~S13までは、準備段階の処理である。これらの処理については第一実施形態と同様である。つまり、様々な条件で加熱処理を行った試験片を作成し(ステップS11)、各試験片についてX線回折法及びリートベルト解析によってT´層などの含有量を求める(ステップS12)。次に、T´相の含有量と加熱時間と加熱時におけるTBC表面温度との関係式を導出する(ステップS13)。
次に、ステップS17で求めたラマンピーク位置、ラマンピーク半値幅、ピーク強度比をステップS16で算出した対応する関係式に代入し、測定対象TBCに含まれるT´相の含有量を算出する(ステップS18)。次に、ステップS13で求めたT´相の含有量と加熱時間とTBC表面温度との関係式[例えば、式(4)]にステップS18で算出したT´相の含有量と既知であるガスタービンの運転時間を代入する。代入した式をTBC表面温度(T)について解き、TBC表面温度を算出する(ステップS15)。算出した値が本実施形態による加熱時のTBC表面温度の推定値である。
その他、次のような方法でもTBC表面温度を推定することができる。第三実施形態の表面温度の推定方法を図12~図14を用いて説明する。
まず、第一実施例と同様にトップコート層14の試験片に対して様々な条件で加熱処理を行う。次に加熱処理後の試験片に対して、ラマン分光法による測定を行う。次に、測定して得られたラマンスペクトルを、ガウス関数、ローレンツ関数によりフィッティングし、ラマンピークの位置、半値幅、ピーク強度を得る。次にラマンピークの位置、半値幅、強度のそれぞれと、加熱処理時間と、加熱温度をラーソンミラーパラメータ(LMP=T[5+ln(t)])で整理する。
図12~図14は、実際の試験片を用いてラマン分光法による測定値をLMPで整理した結果の一例である(T:加熱温度、t:加熱処理時間)。
図12の縦軸は、ラマンピーク位置であり、横軸はLMP値(=T[5+ln(t)])である。252cm-1、258cm-1、463cm-1、635cm-1付近に位置するラマンピークに着目し、これらの近傍のラマンピークとLMP値の関係を整理すると、図12に示すような直線関係が得られた。
図13の縦軸は、ラマンピークの半値幅であり、横軸はLMP値である。144cm-1、258cm-1、321cm-1、463cm-1付近に位置するラマンピークに着目し、これらの近傍のラマンピークの半値幅とLMP値の関係を整理すると、図13に示すような直線関係が得られた。
図14の縦軸は、ラマンピークの強度比であり、横軸はLMP値である。144cm-1のピーク強度と463cm-1のピーク強度の比、144cm-1のピーク強度と635cm-1のピーク強度の比、463cm-1のピーク強度と635cm-1のピーク強度の比に着目し、これらのピーク強度比とLMP値の関係を整理すると、図14に示すような直線関係が得られた。
これら試験片を用いてラマン分光法による測定を行った結果とLMP値との関係を記録する。以上が準備段階の処理である。
T×[5+ln(t)]= 図12~図14に基づいて得たLMP値
・・・(5)
式(5)を、Tについて解くと、第三実施形態によるTBC表面温度を求めることができる。
ところで、T´相の含有量は熱サイクル耐久性と高い相関関係があることが知られている(R.A.Miller.et al.,American Ceramic Society Bulletin,62(12),1355,1983)。この性質と、第一~三実施形態のT´相の含有量の測定方法を利用すると高温部材10の劣化判定を行うことができる。
例えば、実機と同じ母材の上に、実機と同じTBCを形成した耐熱試験用の試験片を用意し、この試験片に実機のタービン部材と同様の熱負荷を与えて、試験片の劣化度を調べる。例えば、日本国特許第4388466号公報には、試験片のTBC側をレーザ光によって加熱し、試験片の裏側(TBCが施された側と反対側)の母材を冷却ガスで冷却するレーザ式熱サイクル試験装置によって、試験片に所定の熱負荷を繰り返し与え、TBCの剥離が生じた時点での繰り返し回数を熱サイクル寿命として評価する方法が記載されている。この方法を利用して、例えば、耐熱試験用の試験片に、TBCの剥離が生じるまで繰り返し熱負荷を与える。このとき、所定回数ごとに、第一実施形態と同様に、この試験片に対してX線回折法及びリートベルト解析を行って試験片のTBCに含まれるT´相の含有量を求める。あるいは、第二実施形態と同様にして、この試験片のTBCに対するラマン分光法の測定結果とステップS16で得た関係式とを用いて、試験片のTBCに含まれるT´相の含有量を求める。また、TBCの剥離が生じたときの繰り返し回数から、繰り返し回数と劣化度との関係を定義し(例えば、100回でTBCが剥離したとすると、50回では劣化度50%とするなど)、そして、T´相の含有量と劣化度との対応関係を記録する。
次に、実機から測定対象とするTBCを入手し、第一実施形態又は第二実施形態と同様の方法で、測定対象TBCのT´相の含有量を算出する。すると、予め耐熱試験用の試験片を用いて作成したT´相の含有量と劣化度との対応関係に基づいて、実機のタービン部材の劣化度合いを判定することができる。
10 高温部材
11 母材
12 遮熱コーティング層
13 ボンドコート層
14 トップコート層
Claims (7)
- 高温部材の表面に形成されたコーティング層に含まれる準安定正方相の含有量をX線回折法又はラマン分光法によって測定し、測定した前記準安定正方相の含有量に基づいて、前記高温部材の表面温度を推定する温度推定方法。
- 定められた複数の加熱温度ごとに定められた複数の加熱時間、加熱処理を行った複数の前記コーティング層の試験用部材についてX線回折法によって測定した回折結果のそれぞれと、予め準安定正方相と正方相と立方相との含有量が既知である部材に対するX線回折法による回折結果をリートベルト解析して前記複数の試験用部材それぞれに含まれる準安定正方相の含有量を算出し、それぞれの前記試験用部材に対応する加熱温度及び加熱時間及び準安定正方相の含有量のデータを蓄積し、前記蓄積したデータに基づいて、前記試験用部材に対する加熱時間と加熱温度と準安定正方相の含有量との関係式を算出するステップと、
所定の温度以上の加熱温度で加熱処理を行った前記コーティング層の測定用部材であって、前記加熱処理における加熱時間が既知である場合に、前記測定用部材のX線回折法による回折結果と、予め準安定正方相と正方相と立方相との含有量が既知である部材についてのX線回折法による回析結果をリートベルト解析して、前記測定用部材に含まれる準安定正方相の含有量を算出するステップと、
前記測定用部材の加熱時間と、前記算出した前記測定用部材に含まれる準安定正方相の含有量と、前記関係式に基づいて前記測定用部材の加熱温度を算出するステップ、
を有する請求項1に記載の温度推定方法。 - 定められた複数の加熱温度ごとに定められた複数の加熱時間、加熱処理を行った複数の前記コーティング層の試験用部材についてX線回折法によって測定した回折結果のそれぞれと、予め準安定正方相と正方相と立方相との含有量が既知である部材に対するX線回折法による回折結果をリートベルト解析して前記複数の試験用部材それぞれに含まれる準安定正方相の含有量を算出し、それぞれの前記試験用部材に対応する加熱温度及び加熱時間及び準安定正方相の含有量のデータを蓄積し、前記蓄積したデータに基づいて、前記試験用部材に対する加熱時間と加熱温度と準安定正方相の含有量との関係式を算出するステップと、
前記複数の試験用部材をラマン分光法によって測定した結果のスペクトルの特徴量と、前記算出した試験用部材のそれぞれに含まれる準安定正方相の含有量との相関関係を算出するステップと、
所定の温度以上の加熱温度で加熱処理を行った前記コーティング層の測定用部材であって、前記加熱処理における加熱時間が既知である場合に、前記測定用部材をラマン分光法によって測定して得たスペクトルの特徴量と、前記相関関係に基づいて、前記測定用部材に含まれる準安定正方相の含有量を算出するステップと、
前記測定用部材の加熱時間と、前記算出した前記測定用部材に含まれる準安定正方相の含有量と、前記関係式に基づいて前記測定用部材の加熱温度を算出するステップ、
を有する請求項1に記載の温度推定方法。 - 前記関係式は、準安定正方相の分解量と加熱時間の1/4乗とが直線関係であることに基づく、
請求項2又は請求項3に記載の温度推定方法。 - 高温部材の表面に形成されたコーティング層に含まれる準安定正方相の含有量を測定する方法であって、
所定の温度以上の加熱温度で加熱処理を行った前記コーティング層の測定用部材についてX線回折法によって測定した回折結果のそれぞれと、予め準安定正方相と正方相と立方相との含有量が既知である部材に対するX線回折法による回折結果をリートベルト解析して前記複数の測定用部材それぞれに含まれる準安定正方相の含有量を算出するステップを有する、
準安定正方相の含有量測定方法。 - 高温部材の表面に形成されたコーティング層に含まれる準安定正方相の含有量を測定する方法であって、
定められた複数の加熱温度ごとに定められた複数の加熱時間、加熱処理を行った複数の前記コーティング層の試験用部材についてX線回折法によって測定した回折結果のそれぞれと、予め準安定正方相と正方相と立方相との含有量が既知である部材に対するX線回折法による回折結果をリートベルト解析して前記複数の試験用部材それぞれに含まれる準安定正方相の含有量を算出するステップと、
前記複数の試験用部材をラマン分光法によって測定した結果のスペクトルの特徴量と、前記算出した試験用部材のそれぞれに含まれる準安定正方相の含有量との相関関係を算出するステップと、
所定の温度以上の加熱温度で加熱処理を行った前記コーティング層の測定用部材であって、前記加熱処理における加熱時間が既知である場合に、前記測定用部材をラマン分光法によって測定して得たスペクトルの特徴量と、前記相関関係に基づいて、前記測定用部材に含まれる準安定正方相の含有量を算出するステップ、
を有する準安定正方相の含有量測定方法。 - 請求項5又は請求項6に記載の準安定正方相の含有量測定方法によって前記測定用部材に含まれる準安定正方相の含有量を算出し、
前記測定用部材に含まれる準安定正方相の含有量と前記高温部材の劣化度との予め定められた対応関係に基づいて、前記高温部材の劣化度を算出する、
劣化判定方法。
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