CN105717118A - Method for determining nickel-based single crystal high-temperature alloy residual segregation - Google Patents
Method for determining nickel-based single crystal high-temperature alloy residual segregation Download PDFInfo
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Abstract
The invention provides a method for determining nickel-based single crystal high-temperature alloy residual segregation. By means of a manufactured metallographic specimen, primary dendrite distance of nickel-based single crystal high-temperature alloy is measured, and mass fraction distribution of all elements on all points of the nickel-based single crystal high-temperature alloy are measured on the manufactured metallographic specimen through a dot matrix method. The segregation directions of the elements are determined according to obtained mass fractions of the elements on the measurement points. A computer simulates solution treatment to obtain distribution of the elements after solution treatment, and accordingly the residual segregation ratios of Al, Ta, W and Re elements are obtained respectively. According to the method, experiments and simulation are combined so that residual segregation of the high-temperature alloy can be accurately and quickly predicted after solution treatment, cost of solution treatment research is reduced, and the period of solution treatment research is shortened. The mode that the mass fraction distribution of the elements on the points is obtained through the dot matrix method has the advantage of being large in specimen number, and result deviation caused by large errors in common representing methods is prevented.
Description
Technical field
The present invention relates to nickel base superalloy field, specifically a kind of method simulating calculating nickel base superalloy remnants segregation.
Background technology
Nickel base superalloy (hereinafter referred to as high temperature alloy) is the high temperature alloy at the temperature more than 650 DEG C with nickel for matrix (content is generally higher than 50%) with good strength, creep-resistant property and antioxidation, resistance to corrosion.In order to improve the temperature capability of high temperature alloy, eliminate this weak link of crystal boundary, develop into single crystal super alloy.Along with the development of single crystal super alloy, solid solution strengthening effect and the creep diffusion rate of progressively adding refractory element increase alloy put forward heavy alloyed mechanical behavior under high temperature.High temperature alloy in process of setting owing to the segregation coefficient of wherein each element is different, different positive and negative segregation element can segregation in various degree in interdendritic, dendrite does.Segregation is crossed conference and is caused the problems such as uneven, the TCP phase precipitation of γ ' granular size, serious harm high temperature alloy performance.In order to eliminate segregation, high temperature alloy through solution treatment, will at high temperature allow alloy each element full and uniformization spread.But along with the refractory element of single crystal super alloy gets more and more, solution treatment difficulty constantly increases, after solution treatment, remaining segregation cannot be avoided.Therefore Accurate Determining remnants segregation is particularly important.The as cast condition segregation of alloy measures generally can use metallographic method dry to the dendrite distinguishing alloy and interdendritic regions measures both composition respectively, calculates segregation ratio.But the arborescent structure of alloy can disappear after solution treatment, it is impossible to distinguish dendrite by metallographic method and do and interdendritic.Now can measure the remaining segregation of alloy by dot matrix, but need the some quantity measured a lot, substantial amounts of time and cost can be spent.Along with the development of computer technology and corresponding data base, calculating simulation technology becomes more and more quick and accurate, utilizes the remaining segregation of the method Accurate Prediction alloy of calculating simulation can be substantially reduced experimental cost and time.
" JablonskiPD et al. is at Metallurgical&MaterialsTransactionsB, 2009, document HomogenizingaNickel-BasedSuperalloy:ThermodynamicandKine ticSimulationandExperimentalResults is delivered on 40 (2) " adopt Thermo-Calc and Dictra simulation to calculate the remaining segregation of a kind of Nimonic105 alloy, but its initial segregation is to obtain with the Scheil model in Thermo-Calc software, but the segregation that this model obtains and actual segregation differ greatly, the deviation that follow-up remaining segregation calculates can be caused.
" LiuG et al. is at MetallurgicalandMaterialsTransactionsA; 2011; 42 (9) publish an article EffectsofReandRuonthesolidificationcharacteristicsofnick el-basesingle-crystalsuperalloys ", remaining segregation after adopting dot matrix to survey a kind of single crystal super alloy heat treatment in literary composition, but the method for the pure experiment of method comparing simulation can consume substantial amounts of time and fund more.
That mentions meaning that in high temperature alloy, segregation alleviates and a kind of high temperature alloy remnants segregation in Chinese patent CN103276333A alleviates method, but does not describe the assay method of remaining segregation.
US Patent No. 20050217426A1 describes the remaining segregation impact on high temperature alloy, but the assay method of remaining segregation is not described.
US Patent No. 20060016527A1 describes remaining segregation to the impact of incipient melting in high temperature alloy heat treatment process, but the assay method of remaining segregation is not described.
Summary of the invention
For the remaining segregation determined after solution treatment in high temperature alloy, the present invention proposes a kind of method determining nickel-base high-temperature single crystal alloy remnants segregation.
Of the present invention determine that nickel-base high-temperature single crystal alloy element remnants segregation refers to most important 4 kinds of segregation element Al, Ta, W and Re in nickel-base high-temperature single crystal alloy；Comprise the concrete steps that:
Step 1, prepares metallographic specimen.
Step 2, measures the primary dendritic spacing of nickel-base high-temperature single crystal alloy: measured the primary dendritic spacing of nickel-base high-temperature single crystal alloy by the metallographic specimen made.
When measuring the primary dendritic spacing of nickel-base high-temperature single crystal alloy, will corrode on sample surfaces by the proportions caustic brush of 1:2:3 with nitric acid, Fluohydric acid. and glycerol.Etching time is 10s.
Step 3, measures the mass fraction distribution of all elements of nickel-base high-temperature single crystal alloy: measure each element mass fraction distribution on nickel-base high-temperature single crystal alloy each point on the metallographic specimen made by dot matrix.
It is choose a foursquare region on metallographic specimen surface with scanning electron microscope that described dot matrix measures each element mass fraction distribution on nickel-base high-temperature single crystal alloy each point on the metallographic specimen made, and includes a complete arborescent structure in this region.In selected region, determine the measurement point of 100 with the supporting energy disperse spectroscopy of scanning electron microscope, and make described 100 measurement points be distributed in this region.Measure these 100 mass fractions measuring the upper all elements of point with energy disperse spectroscopy, respectively obtain each mass fraction measuring the upper all elements of point.The mass fraction distribution of nickel-base high-temperature single crystal alloy is obtained according to each position distribution measuring point.
Step 4, sorts out the segregation direction of Al, Ta, W and Re element in nickel-base high-temperature single crystal alloy: determine the segregation direction of element according to element mass fraction measuring point each in step 3.
If being arranged in dendrite to do the content of each element element measuring point more than being positioned on interdendritic and measuring this constituent content a little, then it is positioned at dendrite described in and does that to measure this element put be negative segregation element.Otherwise, if being arranged in dendrite to do the content of each element element measuring point less than being positioned on interdendritic and measuring this constituent content a little, then it is positioned at dendrite described in and does that to measure this element put be normal segregation element.
Step 5, simulates solution treatment, to obtain the distribution of each element after solution treatment:
The I each element mass fraction distribution of nickel-base high-temperature single crystal alloy step 3 obtained and solution treatment system action initial condition are input in Dictra software.
The primary dendritic spacing of II nickel-base high-temperature single crystal alloy step 2 obtained is input in Dictra software as diffusion length, to simulate each element diffusion process in solution treatment.
III reads nickel-base high-temperature single crystal alloy distribution of each element mass fraction after solution treatment in Dictra software analog result.
The solution treatment system of described simulation is: nickel-base high-temperature single crystal alloy, from the room temperature ramp to 1250 DEG C with 10 DEG C/min, is incubated 1h.After insulation terminates, it is incubated 1h with the ramp of 1 DEG C/min to 1290 DEG C.After insulation terminates, continue to be incubated 2h with the ramp to 1300 DEG C of 1 DEG C/min.After insulation terminates, continue to be incubated with the ramp to 1310 DEG C of 1 DEG C/min 3h, then be incubated 5h with the ramp to 1320 DEG C of 1 DEG C/min, be finally incubated 10h with the ramp of 1 DEG C/min to 1330 degree Celsius.Insulation terminates rear air cooling to room temperature.
Step 6, it is determined that Al, Ta, W and Re element remaining segregation ratio:
Described determine Al, four kinds of elements of Ta, W and Re remaining segregation than time:
The first step, the distribution according to after the solution treatment that step 5 obtains four kinds of element mass fractions, take the meansigma methods of four kinds of all mass fractions of element respectively, respectively obtain the mass fraction meansigma methods of four kinds of elements；
Second step, if classifying as the mass fraction mass fraction meansigma methods more than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is interdendritic composition.
If classifying as the mass fraction mass fraction meansigma methods less than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is also dendrite dry ingredients.
3rd step, if classifying as the mass fraction mass fraction meansigma methods more than this W element of the W element of negative segregation element, then the mass fraction of this W element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is dendrite dry ingredients.
If classifying as the mass fraction mass fraction meansigma methods less than this W element of the W element of normal segregation element, then the mass fraction of this W element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is also interdendritic composition.
4th step, takes the meansigma methods of all dendrite dry ingredients of Al element, obtains the average assay that this Al element dendrite is dry.The average assay that the dendrite of Ta element, W element and Re element is done is determined successively by the method for the dry average assay of the described Al of determination element dendrite.
Take the meansigma methods of all interdendritics composition of Al element, obtain this interdendritic average assay of Al element.The interdendritic average assay of Ta element, W element and Re element is determined successively by the method for the described Al of determination element interdendritic average assay.
5th step, the average assay that the dendrite of the Al element that use is determined is done is divided by the interdendritic average assay of this Al element, and k is compared in the remaining segregation namely obtaining this Al elementAl。
By the dry average assay of the dendrite of the Ta element the determined interdendritic average assay divided by this Ta element, k is compared in the remaining segregation namely obtaining this Ta elementTa。
By the dry average assay of the dendrite of the W element the determined interdendritic average assay divided by this W element, k is compared in the remaining segregation namely obtaining this W elementW。
By the dry average assay of the dendrite of the Re element the determined interdendritic average assay divided by this Re element, k is compared in the remaining segregation namely obtaining this Re elementRe。
After solution treatment, the arborescent structure of high temperature alloy disappears, and remaining segregation need to measure by dot matrix.In the process of research solution treatment, it is often necessary to the remaining segregation after repetitive measurement difference solution treatment, and the dot matrix every time used needs to expend substantial amounts of time and cost.The present invention utilizes the method that experiment and simulation combine fast and accurately to predict the high temperature alloy remaining segregation after solution treatment, the method utilizing the present invention as shown in Figure 1 has only to measure the initial as cast condition segregation of an alloy by dot matrix, just can predict the remaining segregation of alloy after various different solution treatment, greatly reduce cost and the cycle of solution treatment research and development.Additionally for the ratio that the method that typicallys represent of segregation ratio is two values, but the result that dot matrix obtains has that sample is many and energy disperse spectroscopy exists the feature of certain error, the present invention is directed to the dry average assay of this feature proposition dendrite divided by interdendritic average assay to represent segregation ratio, namely make use of the advantage that dot matrix sample is many, prevent again and the method for typicallying represent is worth most the excessive result error caused of error.
Fig. 1 is that in embodiment 1, the simulation of Dictra software calculates Al, the four kinds of element mass fractions of Ta, W and Re distribution results on arborescent structure after high temperature alloy solution treatment.In figure: curve 1 is the mass fraction of Al element distribution results on arborescent structure, described curve 1 illustrates the remaining segregation situation of Al element after solution treatment, for calculating the remaining segregation of Al element than providing data；Curve 2 is the mass fraction of Ta element distribution results on arborescent structure, and described curve 2 illustrates the remaining segregation situation of Ta element after solution treatment, for calculating the remaining segregation of Ta element than providing data；Curve 3 is the mass fraction of W element distribution results on arborescent structure, and described curve 3 illustrates the remaining segregation situation of W element after solution treatment, for calculating the remaining segregation of W element than providing data；Curve 4 is the mass fraction of Re element distribution results on arborescent structure, and described curve 4 illustrates the remaining segregation situation of Re element after solution treatment, for calculating the remaining segregation of Re element than providing data.
Fig. 2 is that in embodiment 2, the simulation of Dictra software calculates Al, the four kinds of element mass fractions of Ta, W and Re distribution results on arborescent structure after high temperature alloy solution treatment.In figure: curve 5 is the mass fraction of Al element distribution results on arborescent structure, described curve 5 illustrates the remaining segregation situation of Al element after solution treatment, for calculating the remaining segregation of Al element than providing data；Curve 6 is the mass fraction of Ta element distribution results on arborescent structure, and described curve 6 illustrates the remaining segregation situation of Ta element after solution treatment, for calculating the remaining segregation of Ta element than providing data；Curve 7 is the mass fraction of W element distribution results on arborescent structure, and described curve 7 illustrates the remaining segregation situation of W element after solution treatment, for calculating the remaining segregation of W element than providing data；Curve 8 is the mass fraction of Re element distribution results on arborescent structure, and described curve 8 illustrates the remaining segregation situation of Re element after solution treatment, for calculating the remaining segregation of Re element than providing data.
Fig. 3 is that in embodiment 3, the simulation of Dictra software calculates Al, the four kinds of element mass fractions of Ta, W and Re distribution results on arborescent structure after high temperature alloy solution treatment.In figure: curve 9 is the mass fraction of Al element distribution results on arborescent structure, described curve 9 illustrates the remaining segregation situation of Al element after solution treatment, for calculating the remaining segregation of Al element than providing data；Curve 10 is the mass fraction of Ta element distribution results on arborescent structure, and described curve 10 illustrates the remaining segregation situation of Ta element after solution treatment, for calculating the remaining segregation of Ta element than providing data；Curve 11 is the mass fraction of W element distribution results on arborescent structure, and described curve 11 illustrates the remaining segregation situation of W element after solution treatment, for calculating the remaining segregation of W element than providing data；Curve 12 is the mass fraction of Re element distribution results on arborescent structure, and described curve 12 illustrates the remaining segregation situation of Re element after solution treatment, for calculating the remaining segregation of Re element than providing data.
Accompanying drawing explanation
Fig. 1 is that in embodiment 1, the simulation of Dictra software calculates Al, the four kinds of element mass fractions of Ta, W and Re distribution results on arborescent structure after high temperature alloy solution treatment.In figure: curve 1 is the mass fraction of Al element distribution results on arborescent structure；Curve 2 is the mass fraction of Ta element distribution results on arborescent structure；Curve 3 is the mass fraction of W element distribution results on arborescent structure；Curve 4 is the mass fraction of Re element distribution results on arborescent structure.
Fig. 2 is that in embodiment 2, the simulation of Dictra software calculates Al, the four kinds of element mass fractions of Ta, W and Re distribution results on arborescent structure after high temperature alloy solution treatment.In figure: curve 5 is the mass fraction of Al element distribution results on arborescent structure；Curve 6 is the mass fraction of Ta element distribution results on arborescent structure；Curve 7 is the mass fraction of W element distribution results on arborescent structure；Curve 8 is the mass fraction of Re element distribution results on arborescent structure.
Fig. 3 is that in embodiment 3, the simulation of Dictra software calculates Al, the four kinds of element mass fractions of Ta, W and Re distribution results on arborescent structure after high temperature alloy solution treatment.In figure: curve 9 is the mass fraction of Al element distribution results on arborescent structure；Curve 10 is the mass fraction of Ta element distribution results on arborescent structure；Curve 11 is the mass fraction of W element distribution results on arborescent structure；Curve 12 is the mass fraction of Re element distribution results on arborescent structure.
Fig. 4 is the flow chart of the present invention.
Detailed description of the invention
Embodiment 1
The present embodiment is a kind of method determining nickel-base high-temperature single crystal alloy element remnants segregation.Described determination nickel-base high-temperature single crystal alloy element remnants segregation refers to most important 4 kinds of segregation element Al, Ta, W and Re in nickel-base high-temperature single crystal alloy.
Namely the present embodiment calculates the remaining segregation ratio of Al, four kinds of elements of Ta, W and Re.
Described nickel-base high-temperature single crystal alloy is as cast condition, it is made up of Cr, Mo, Al, Co, W, Re, Ta, Hf, C, B and Ni, its nominal composition is: the content of Cr is 3.6%, the content of Mo is 1.8%, and the content of Al is 5.7%, and the content of Co is 9%, the content of W is 6%, the content of Re is 4%, and the content of Ta is 8%, and surplus is Ni.Described percentage ratio is mass percent.
The step that is embodied as of the present embodiment is:
Step 1, prepares metallographic specimen: nickel-base high-temperature single crystal alloy to be measured is sampled.Use sand papering sample surfaces, with polishing cloth, specimen surface is polished.
Step 2, measures the primary dendritic spacing of nickel-base high-temperature single crystal alloy: measured the primary dendritic spacing of nickel-base high-temperature single crystal alloy by the metallographic specimen made.
The proportions caustic of 1:2:3 is pressed with nitric acid, Fluohydric acid. and glycerol.Dip the caustic of preparation with Cotton Gossypii, uniformly brush corrodes on sample surfaces.Etching time is 10s.With the primary dendritic spacing of optical microscope measuring nickel-base high-temperature single crystal alloy after etching.In the present embodiment, primary dendritic spacing is 130 microns.
Step 3, measures the mass fraction distribution of all elements of nickel-base high-temperature single crystal alloy: measured each element mass fraction distribution of nickel-base high-temperature single crystal alloy by the metallographic specimen made.
Each element mass fraction distribution of nickel-base high-temperature single crystal alloy is measured, specifically: choose a foursquare region on metallographic specimen surface with scanning electron microscope, and in this region, include a complete arborescent structure by dot matrix.In selected region, determine the measurement point of 100 with the supporting energy disperse spectroscopy of scanning electron microscope, and make described 100 measurement points be distributed in this region.Measure these 100 mass fractions measuring the upper all elements of point with energy disperse spectroscopy, respectively obtain each mass fraction measuring the upper all elements of point.The mass fraction distribution of nickel-base high-temperature single crystal alloy is obtained according to each position distribution measuring point.
Step 4, sorts out the segregation direction of Al, Ta, W and Re element in nickel-base high-temperature single crystal alloy: determine the segregation direction of element according to element mass fraction measuring point each in step 3.If being arranged in dendrite to do the content of each element element measuring point more than being positioned on interdendritic and measuring this constituent content a little, be positioned at described in then dendrite do measure point this element be negative segregation element, in the present embodiment, it is 8.2 that W element does certain content measuring point at dendrite, the content measuring point in interdendritic is 4.8, therefore in nickel-base high-temperature single crystal alloy, W element is negative segregation element.Otherwise, if being arranged in dendrite to do the content of each element element measuring point less than being positioned on interdendritic and measuring this constituent content a little, be positioned at described in then dendrite do measure point this element be normal segregation element, in the present embodiment, it is 6.2 that Ta element does certain content measuring point at dendrite, the content measuring point in interdendritic is 10.5, therefore Ta element is normal segregation element in nickel-base high-temperature single crystal alloy.
Categorized element segregation direction, in the nickel-base high-temperature single crystal alloy of the present embodiment, Al and Ta element is normal segregation element, and W and Re element is negative segregation element.
Step 5, simulates solution treatment, to obtain the distribution of each element after solution treatment:
First, each element mass fraction distribution of nickel-base high-temperature single crystal alloy step 3 obtained and solution treatment system action initial condition are input in Dictra software.In the present embodiment, the solution treatment system of simulation is: nickel-base high-temperature single crystal alloy, from the room temperature ramp to 1250 DEG C with 10 DEG C/min, is incubated 1h.After insulation terminates, it is incubated 1h with the ramp of 1 DEG C/min to 1290 DEG C.After insulation terminates, continue to be incubated 2h with the ramp to 1300 DEG C of 1 DEG C/min.After insulation terminates, continue to be incubated with the ramp to 1310 DEG C of 1 DEG C/min 3h, then be incubated 5h with the ramp to 1320 DEG C of 1 DEG C/min, be finally incubated 10h with the ramp of 1 DEG C/min to 1330 degree Celsius.Insulation terminates rear air cooling to room temperature.
Secondly, the primary dendritic spacing of nickel-base high-temperature single crystal alloy step 2 obtained is input in Dictra software as diffusion length, can simulate each element diffusion process in solution treatment.
Finally, Dictra software analog result reads nickel-base high-temperature single crystal alloy distribution of each element mass fraction after solution treatment, as shown in Figure 1.In Fig. 1, vertical coordinate is the mass fraction of nickel-base high-temperature single crystal alloy element.
Step 6, it is determined that Al, Ta, W and Re element remaining segregation ratio:
Described determine Al, four kinds of elements of Ta, W and Re remaining segregation than time:
The first step, the distribution according to after the solution treatment that step 5 obtains four kinds of element mass fractions, take the meansigma methods of four kinds of all mass fractions of element respectively, respectively obtain the mass fraction meansigma methods of four kinds of elements；
Second step, if classifying as the mass fraction mass fraction meansigma methods more than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is interdendritic composition.
If classifying as the mass fraction mass fraction meansigma methods less than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is also dendrite dry ingredients.
3rd step, if classifying as the mass fraction mass fraction meansigma methods more than this W element of the W element of negative segregation element, then the mass fraction of this W element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is dendrite dry ingredients.
If classifying as the mass fraction mass fraction meansigma methods less than this W element of the W element of normal segregation element, then the mass fraction of this W element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is also interdendritic composition.
4th step, takes the meansigma methods of all dendrite dry ingredients of Al element, obtains the average assay that this Al element dendrite is dry.The average assay that the dendrite of Ta element, W element and Re element is done is determined successively by the method for the dry average assay of the described Al of determination element dendrite.
Take the meansigma methods of all interdendritics composition of Al element, obtain this interdendritic average assay of Al element.The interdendritic average assay of Ta element, W element and Re element is determined successively by the method for the described Al of determination element interdendritic average assay.
5th step, the average assay that the dendrite of the Al element that use is determined is done is divided by the interdendritic average assay of this Al element, and k is compared in the remaining segregation namely obtaining this Al elementAl。
By the dry average assay of the dendrite of the Ta element the determined interdendritic average assay divided by this Ta element, k is compared in the remaining segregation namely obtaining this Ta elementTa。
By the dry average assay of the dendrite of the W element the determined interdendritic average assay divided by this W element, k is compared in the remaining segregation namely obtaining this W elementW。
By the dry average assay of the dendrite of the Re element the determined interdendritic average assay divided by this Re element, k is compared in the remaining segregation namely obtaining this Re elementRe。
In the present embodiment, k is compared in the remaining segregation of Al elementAl=0.93, k is compared in the remaining segregation of Ta elementTa=0.90, k is compared in the remaining segregation of W elementW=1.16, k is compared in the remaining segregation of Re elementRe=1.50.
In order to assess the result of simulation, nickel-base high-temperature single crystal alloy remaining segregation ratio of element to be measured after solution treatment has been surveyed by dot matrix, and table 1 being listed in the remaining segregation that obtains of simulation than comparing result, the contrast through table 1 can be seen that simulation predicts the remaining segregation ratio after solution treatment accurately.
Embodiment 2
The present embodiment is a kind of method determining nickel-base high-temperature single crystal alloy element remnants segregation.Described determination nickel-base high-temperature single crystal alloy element remnants segregation refers to most important 4 kinds of segregation element Al, Ta, W and Re in nickel-base high-temperature single crystal alloy.
Namely the present embodiment calculates the remaining segregation ratio of Al, four kinds of elements of Ta, W and Re.
Described nickel-base high-temperature single crystal alloy is as cast condition, it is made up of Cr, Mo, Al, Co, W, Re, Ta, Hf, C, B and Ni, its nominal composition is: the content of Cr is 3.5%, the content of Mo is 1.7%, and the content of Al is 5.75%, and the content of Co is 9.1%, the content of W is 6%, the content of Re is 4%, and the content of Ta is 8%, and surplus is Ni.Described percentage ratio is mass percent.
The step that is embodied as of the present embodiment is:
Step 1, prepares metallographic specimen: nickel-base high-temperature single crystal alloy to be measured is sampled.Use sand papering sample surfaces, with polishing cloth, specimen surface is polished.
Step 2, measures the primary dendritic spacing of nickel-base high-temperature single crystal alloy: measured the primary dendritic spacing of nickel-base high-temperature single crystal alloy by the metallographic specimen made.
The proportions caustic of 1:2:3 is pressed with nitric acid, Fluohydric acid. and glycerol.Dip the caustic of preparation with Cotton Gossypii, uniformly brush corrodes on sample surfaces.Etching time is 10s.With the primary dendritic spacing of optical microscope measuring nickel-base high-temperature single crystal alloy after etching.In the present embodiment, primary dendritic spacing is 130 microns.
Step 3, measures the mass fraction distribution of all elements of nickel-base high-temperature single crystal alloy: measured each element mass fraction distribution of nickel-base high-temperature single crystal alloy by the metallographic specimen made.
Each element mass fraction distribution of nickel-base high-temperature single crystal alloy is measured, specifically: choose a foursquare region on metallographic specimen surface with scanning electron microscope, and in this region, include a complete arborescent structure by dot matrix.In selected region, determine the measurement point of 100 with the supporting energy disperse spectroscopy of scanning electron microscope, and make described 100 measurement points be distributed in this region.Measure these 100 mass fractions measuring the upper all elements of point with energy disperse spectroscopy, respectively obtain each mass fraction measuring the upper all elements of point.The mass fraction distribution of nickel-base high-temperature single crystal alloy is obtained according to each position distribution measuring point.
Step 4, sorts out the segregation direction of Al, Ta, W and Re element in nickel-base high-temperature single crystal alloy: determine the segregation direction of element according to element mass fraction measuring point each in step 3.If being arranged in dendrite to do the content of each element element measuring point more than being positioned on interdendritic and measuring this constituent content a little, be positioned at described in then dendrite do measure point this element be negative segregation element, in the present embodiment, it is 7.6 that W element does certain content measuring point at dendrite, the content measuring point in interdendritic is 4.2, therefore in nickel-base high-temperature single crystal alloy, W element is negative segregation element.Otherwise, if being arranged in dendrite to do the content of each element element measuring point less than being positioned on interdendritic and measuring this constituent content a little, be positioned at described in then dendrite do measure point this element be normal segregation element, in the present embodiment, it is 6.7 that Ta element does certain content measuring point at dendrite, the content measuring point in interdendritic is 11.2, therefore Ta element is normal segregation element in nickel-base high-temperature single crystal alloy.
Categorized element segregation direction, in the nickel-base high-temperature single crystal alloy of the present embodiment, Al and Ta element is normal segregation element, and W and Re element is negative segregation element.
Step 5, simulates solution treatment, to obtain the distribution of each element after solution treatment:
First, each element mass fraction distribution of nickel-base high-temperature single crystal alloy step 3 obtained and solution treatment system action initial condition are input in Dictra software.In the present embodiment, the solution treatment system of simulation is: nickel-base high-temperature single crystal alloy is from the room temperature ramp to 1230 DEG C with 10 DEG C/min, after the ramp of 60 DEG C/h to 1290 DEG C, continues to be incubated 15h with the ramp to 1330 DEG C of 2.5 DEG C/h.Insulation terminates rear air cooling to room temperature.
Secondly, the primary dendritic spacing of nickel-base high-temperature single crystal alloy step 2 obtained is input in Dictra software as diffusion length, can simulate each element diffusion process in solution treatment.
Finally, Dictra software analog result reads nickel-base high-temperature single crystal alloy distribution of each element mass fraction after solution treatment, as shown in Figure 1.In Fig. 1, vertical coordinate is the mass fraction of nickel-base high-temperature single crystal alloy element.
Step 6, it is determined that Al, Ta, W and Re element remaining segregation ratio:
Described determine Al, four kinds of elements of Ta, W and Re remaining segregation than time:
The first step, the distribution according to after the solution treatment that step 5 obtains four kinds of element mass fractions, take the meansigma methods of four kinds of all mass fractions of element respectively, respectively obtain the mass fraction meansigma methods of four kinds of elements；
Second step, if classifying as the mass fraction mass fraction meansigma methods more than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is interdendritic composition.
If classifying as the mass fraction mass fraction meansigma methods less than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is also dendrite dry ingredients.
3rd step, if classifying as the mass fraction mass fraction meansigma methods more than this W element of the W element of negative segregation element, then the mass fraction of this W element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is dendrite dry ingredients.
If classifying as the mass fraction mass fraction meansigma methods less than this W element of the W element of normal segregation element, then the mass fraction of this W element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is also interdendritic composition.
4th step, takes the meansigma methods of all dendrite dry ingredients of Al element, obtains the average assay that this Al element dendrite is dry.The average assay that the dendrite of Ta element, W element and Re element is done is determined successively by the method for the dry average assay of the described Al of determination element dendrite.
Take the meansigma methods of all interdendritics composition of Al element, obtain this interdendritic average assay of Al element.The interdendritic average assay of Ta element, W element and Re element is determined successively by the method for the described Al of determination element interdendritic average assay.
5th step, the average assay that the dendrite of the Al element that use is determined is done is divided by the interdendritic average assay of this Al element, and k is compared in the remaining segregation namely obtaining this Al elementAl。
By the dry average assay of the dendrite of the Ta element the determined interdendritic average assay divided by this Ta element, k is compared in the remaining segregation namely obtaining this Ta elementTa。
By the dry average assay of the dendrite of the W element the determined interdendritic average assay divided by this W element, k is compared in the remaining segregation namely obtaining this W elementW。
By the dry average assay of the dendrite of the Re element the determined interdendritic average assay divided by this Re element, k is compared in the remaining segregation namely obtaining this Re elementRe。
In the present embodiment, k is compared in the remaining segregation of Al elementAl=0.94, k is compared in the remaining segregation of Ta elementTa=0.91, k is compared in the remaining segregation of W elementW=1.14, k is compared in the remaining segregation of Re elementRe=1.48.
In order to assess the result of simulation, nickel-base high-temperature single crystal alloy remaining segregation ratio of element to be measured after solution treatment has been surveyed by dot matrix, and table 1 being listed in the remaining segregation that obtains of simulation than comparing result, the contrast through table 1 can be seen that simulation predicts the remaining segregation ratio after solution treatment accurately.
Embodiment 3
The present embodiment is a kind of method determining nickel-base high-temperature single crystal alloy element remnants segregation.Described determination nickel-base high-temperature single crystal alloy element remnants segregation refers to most important 4 kinds of segregation element Al, Ta, W and Re in nickel-base high-temperature single crystal alloy.
Namely the present embodiment calculates the remaining segregation ratio of Al, four kinds of elements of Ta, W and Re.
Described nickel-base high-temperature single crystal alloy is as cast condition, it is made up of Cr, Mo, Al, Co, W, Re, Ta, Hf, C, B and Ni, its nominal composition is: the content of Cr is 3.62%, the content of Mo is 1.83%, and the content of Al is 5.7%, and the content of Co is 9%, the content of W is 6%, the content of Re is 4.1%, and the content of Ta is 8%, and surplus is Ni.Described percentage ratio is mass percent.
The step that is embodied as of the present embodiment is:
Step 1, prepares metallographic specimen: nickel-base high-temperature single crystal alloy to be measured is sampled.Use sand papering sample surfaces, with polishing cloth, specimen surface is polished.
Step 2, measures the primary dendritic spacing of nickel-base high-temperature single crystal alloy: measured the primary dendritic spacing of nickel-base high-temperature single crystal alloy by the metallographic specimen made.
The proportions caustic of 1:2:3 is pressed with nitric acid, Fluohydric acid. and glycerol.Dip the caustic of preparation with Cotton Gossypii, uniformly brush corrodes on sample surfaces.Etching time is 10s.With the primary dendritic spacing of optical microscope measuring nickel-base high-temperature single crystal alloy after etching.In the present embodiment, primary dendritic spacing is 130 microns.
Step 3, measures the mass fraction distribution of all elements of nickel-base high-temperature single crystal alloy: measured each element mass fraction distribution of nickel-base high-temperature single crystal alloy by the metallographic specimen made.
Each element mass fraction distribution of nickel-base high-temperature single crystal alloy is measured, specifically: choose a foursquare region on metallographic specimen surface with scanning electron microscope, and in this region, include a complete arborescent structure by dot matrix.In selected region, determine the measurement point of 100 with the supporting energy disperse spectroscopy of scanning electron microscope, and make described 100 measurement points be distributed in this region.Measure these 100 mass fractions measuring the upper all elements of point with energy disperse spectroscopy, respectively obtain each mass fraction measuring the upper all elements of point.The mass fraction distribution of nickel-base high-temperature single crystal alloy is obtained according to each position distribution measuring point.
Step 4, sorts out the segregation direction of Al, Ta, W and Re element in nickel-base high-temperature single crystal alloy: determine the segregation direction of element according to element mass fraction measuring point each in step 3.If being arranged in dendrite to do the content of each element element measuring point more than being positioned on interdendritic and measuring this constituent content a little, be positioned at described in then dendrite do measure point this element be negative segregation element, in the present embodiment, it is 7.8 that W element does certain content measuring point at dendrite, the content measuring point in interdendritic is 4.7, therefore in nickel-base high-temperature single crystal alloy, W element is negative segregation element.Otherwise, if being arranged in dendrite to do the content of each element element measuring point less than being positioned on interdendritic and measuring this constituent content a little, be positioned at described in then dendrite do measure point this element be normal segregation element, in the present embodiment, it is 6.3 that Ta element does certain content measuring point at dendrite, the content measuring point in interdendritic is 10.8, therefore Ta element is normal segregation element in nickel-base high-temperature single crystal alloy.
Categorized element segregation direction, in the nickel-base high-temperature single crystal alloy of the present embodiment, Al and Ta element is normal segregation element, and W and Re element is negative segregation element.
Step 5, simulates solution treatment, to obtain the distribution of each element after solution treatment:
First, each element mass fraction distribution of nickel-base high-temperature single crystal alloy step 3 obtained and solution treatment system action initial condition are input in Dictra software.In the present embodiment, the solution treatment system of simulation is: nickel-base high-temperature single crystal alloy, from the room temperature ramp to 1250 DEG C with 10 DEG C/min, is incubated 1h.After insulation terminates, it is incubated 1h with the ramp of 1 DEG C/min to 1290 DEG C.After insulation terminates, continue to be incubated 2h with the ramp to 1300 DEG C of 1 DEG C/min.After insulation terminates, continue to be incubated with the ramp to 1310 DEG C of 1 DEG C/min 3h, then be incubated 5h with the ramp to 1320 DEG C of 1 DEG C/min, be finally incubated 20h with the ramp of 1 DEG C/min to 1330 degree Celsius.Insulation terminates rear air cooling to room temperature.
Secondly, the primary dendritic spacing of nickel-base high-temperature single crystal alloy step 2 obtained is input in Dictra software as diffusion length, can simulate each element diffusion process in solution treatment.
Finally, Dictra software analog result reads nickel-base high-temperature single crystal alloy distribution of each element mass fraction after solution treatment, as shown in Figure 1.In Fig. 1, vertical coordinate is the mass fraction of nickel-base high-temperature single crystal alloy element.
Step 6, it is determined that Al, Ta, W and Re element remaining segregation ratio:
Described determine Al, four kinds of elements of Ta, W and Re remaining segregation than time:
The first step, the distribution according to after the solution treatment that step 5 obtains four kinds of element mass fractions, take the meansigma methods of four kinds of all mass fractions of element respectively, respectively obtain the mass fraction meansigma methods of four kinds of elements；
Second step, if classifying as the mass fraction mass fraction meansigma methods more than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is interdendritic composition.
If classifying as the mass fraction mass fraction meansigma methods less than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is also dendrite dry ingredients.
3rd step, if classifying as the mass fraction mass fraction meansigma methods more than this W element of the W element of negative segregation element, then the mass fraction of this W element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is dendrite dry ingredients.
If classifying as the mass fraction mass fraction meansigma methods less than this W element of the W element of normal segregation element, then the mass fraction of this W element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is also interdendritic composition.
4th step, takes the meansigma methods of all dendrite dry ingredients of Al element, obtains the average assay that this Al element dendrite is dry.The average assay that the dendrite of Ta element, W element and Re element is done is determined successively by the method for the dry average assay of the described Al of determination element dendrite.
Take the meansigma methods of all interdendritics composition of Al element, obtain this interdendritic average assay of Al element.The interdendritic average assay of Ta element, W element and Re element is determined successively by the method for the described Al of determination element interdendritic average assay.
5th step, the average assay that the dendrite of the Al element that use is determined is done is divided by the interdendritic average assay of this Al element, and k is compared in the remaining segregation namely obtaining this Al elementAl。
By the dry average assay of the dendrite of the Ta element the determined interdendritic average assay divided by this Ta element, k is compared in the remaining segregation namely obtaining this Ta elementTa。
By the dry average assay of the dendrite of the W element the determined interdendritic average assay divided by this W element, k is compared in the remaining segregation namely obtaining this W elementW。
By the dry average assay of the dendrite of the Re element the determined interdendritic average assay divided by this Re element, k is compared in the remaining segregation namely obtaining this Re elementRe。
In the present embodiment, k is compared in the remaining segregation of Al elementAl=0.94, k is compared in the remaining segregation of Ta elementTa=0.91, k is compared in the remaining segregation of W elementW=1.12, k is compared in the remaining segregation of Re elementRe=1.47.
In order to assess the analog result of each embodiment that the present invention proposes, survey nickel-base high-temperature single crystal alloy remaining segregation ratio of element to be measured after solution treatment by dot matrix, and the remaining segregation ratio that the remaining segregation obtained with simulation obtains than with experiment has been contrasted.Comparing result is listed in table 1.By the contrast of table 1 it can be seen that the present invention predicts the remaining segregation ratio after solution treatment accurately.
The each embodiment of table 1. is simulated and tests the segregation comparison ratio obtained
Claims (4)
1. the method determining nickel-base high-temperature single crystal alloy remnants segregation, it is characterised in that described determination nickel-base high-temperature single crystal alloy element remnants segregation refers to most important 4 kinds of segregation element Al, Ta, W and Re in nickel-base high-temperature single crystal alloy；Comprise the concrete steps that:
Step 1, prepares metallographic specimen；
Step 2, measures the primary dendritic spacing of nickel-base high-temperature single crystal alloy: measured the primary dendritic spacing of nickel-base high-temperature single crystal alloy by the metallographic specimen made；
Step 3, measures the mass fraction distribution of all elements of nickel-base high-temperature single crystal alloy: measure each element mass fraction distribution on nickel-base high-temperature single crystal alloy each point on the metallographic specimen made by dot matrix；
Step 4, sorts out the segregation direction of Al, Ta, W and Re element in nickel-base high-temperature single crystal alloy: determine the segregation direction of element according to element mass fraction measuring point each in step 3；
If being arranged in dendrite to do the content of each element element measuring point more than being positioned on interdendritic and measuring this constituent content a little, then it is positioned at dendrite described in and does that to measure this element put be negative segregation element；Otherwise, if being arranged in dendrite to do the content of each element element measuring point less than being positioned on interdendritic and measuring this constituent content a little, then it is positioned at dendrite described in and does that to measure this element put be normal segregation element；
Step 5, simulates solution treatment, to obtain the distribution of each element after solution treatment:
The I each element mass fraction distribution of nickel-base high-temperature single crystal alloy step 3 obtained and solution treatment system action initial condition are input in Dictra software；
The primary dendritic spacing of II nickel-base high-temperature single crystal alloy step 2 obtained is input in Dictra software as diffusion length, to simulate each element diffusion process in solution treatment；
III reads nickel-base high-temperature single crystal alloy distribution of each element mass fraction after solution treatment in Dictra software analog result；
Step 6, it is determined that Al, Ta, W and Re element remaining segregation ratio:
Described determine Al, four kinds of elements of Ta, W and Re remaining segregation than time:
The first step, the distribution according to after the solution treatment that step 5 obtains four kinds of element mass fractions, take the meansigma methods of four kinds of all mass fractions of element respectively, respectively obtain the mass fraction meansigma methods of four kinds of elements；
Second step, if classifying as the mass fraction mass fraction meansigma methods more than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is interdendritic composition；
If classifying as the mass fraction mass fraction meansigma methods less than this Al element of the Al element of normal segregation element, then the mass fraction of this Al element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Ta element of the Ta element of normal segregation element, then the mass fraction of this Ta element is also dendrite dry ingredients；
3rd step, if classifying as the mass fraction mass fraction meansigma methods more than this W element of the W element of negative segregation element, then the mass fraction of this W element is dendrite dry ingredients；Equally, if classifying as the mass fraction mass fraction meansigma methods more than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is dendrite dry ingredients；
If classifying as the mass fraction mass fraction meansigma methods less than this W element of the W element of normal segregation element, then the mass fraction of this W element is interdendritic composition；Equally, if classifying as the mass fraction mass fraction meansigma methods less than this Re element of the Re element of normal segregation element, then the mass fraction of this Re element is also interdendritic composition；
4th step, takes the meansigma methods of all dendrite dry ingredients of Al element, obtains the average assay that this Al element dendrite is dry；The average assay that the dendrite of Ta element, W element and Re element is done is determined successively by the method for the dry average assay of the described Al of determination element dendrite；
Take the meansigma methods of all interdendritics composition of Al element, obtain this interdendritic average assay of Al element；The interdendritic average assay of Ta element, W element and Re element is determined successively by the method for the described Al of determination element interdendritic average assay；
5th step, the average assay that the dendrite of the Al element that use is determined is done is divided by the interdendritic average assay of this Al element, and k is compared in the remaining segregation namely obtaining this Al elementAl；
By the dry average assay of the dendrite of the Ta element the determined interdendritic average assay divided by this Ta element, k is compared in the remaining segregation namely obtaining this Ta elementTa；
By the dry average assay of the dendrite of the W element the determined interdendritic average assay divided by this W element, k is compared in the remaining segregation namely obtaining this W elementW；
By the dry average assay of the dendrite of the Re element the determined interdendritic average assay divided by this Re element, k is compared in the remaining segregation namely obtaining this Re elementRe。
2. the method determining nickel-base high-temperature single crystal alloy remnants segregation as claimed in claim 1, it is characterized in that, when measuring the primary dendritic spacing of nickel-base high-temperature single crystal alloy, will corrode on sample surfaces by the proportions caustic brush of 1:2:3 with nitric acid, Fluohydric acid. and glycerol；Etching time is 10s.
3. the method determining nickel-base high-temperature single crystal alloy remnants segregation as claimed in claim 1, it is characterised in that the solution treatment system of described simulation is: nickel-base high-temperature single crystal alloy, from the room temperature ramp to 1250 DEG C with 10 DEG C/min, is incubated 1h；After insulation terminates, it is incubated 1h with the ramp of 1 DEG C/min to 1290 DEG C；After insulation terminates, continue to be incubated 2h with the ramp to 1300 DEG C of 1 DEG C/min；After insulation terminates, continue to be incubated with the ramp to 1310 DEG C of 1 DEG C/min 3h, then be incubated 5h with the ramp to 1320 DEG C of 1 DEG C/min, be finally incubated 10h with the ramp of 1 DEG C/min to 1330 degree Celsius；Insulation terminates rear air cooling to room temperature.
4. the method determining nickel-base high-temperature single crystal alloy remnants segregation as claimed in claim 1, it is characterized in that, it is choose a foursquare region on metallographic specimen surface with scanning electron microscope that described dot matrix measures each element mass fraction distribution on nickel-base high-temperature single crystal alloy each point on the metallographic specimen made, and includes a complete arborescent structure in this region；In selected region, determine the measurement point of 100 with the supporting energy disperse spectroscopy of scanning electron microscope, and make described 100 measurement points be distributed in this region；Measure these 100 mass fractions measuring the upper all elements of point with energy disperse spectroscopy, respectively obtain each mass fraction measuring the upper all elements of point；The mass fraction distribution of nickel-base high-temperature single crystal alloy is obtained according to each position distribution measuring point.
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