CN114964961A - Preparation method of standard sample of thermal expansion coefficient of nickel-based superalloy and standard sample - Google Patents

Preparation method of standard sample of thermal expansion coefficient of nickel-based superalloy and standard sample Download PDF

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CN114964961A
CN114964961A CN202210547144.3A CN202210547144A CN114964961A CN 114964961 A CN114964961 A CN 114964961A CN 202210547144 A CN202210547144 A CN 202210547144A CN 114964961 A CN114964961 A CN 114964961A
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毕经亮
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Ncs Testing Technology Co ltd
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Abstract

The invention discloses a preparation method of a standard sample of a nickel-based superalloy thermal expansion coefficient and the standard sample, wherein the method comprises the following steps: s100, designing chemical components; s200, smelting raw materials; s300, forging, wherein the high-temperature alloy ingot is forged into a plurality of metal round rods with preset sizes; s400, performing heat treatment, wherein the metal round bar is placed in a vacuum heat treatment furnace and is subjected to circulation for a plurality of times according to the steps of heating, heat preservation and tempering; s500, naturally aging, wherein the metal round bar is placed in a conventional storage room for more than a preset time; s600, performing primary uniformity detection; s700, processing a sample, wherein a metal round bar is processed into a cylindrical finished product sample with a preset size; next, each cylindrical finished sample was packaged as an independent unit. The standard sample prepared by the method can meet the requirements of thermal expansion performance analysis of metal materials and quality control of a thermal expansion instrument, and fills the blank of the related standard sample field in the domestic and foreign fields.

Description

Preparation method of standard sample of thermal expansion coefficient of nickel-based superalloy and standard sample
Technical Field
The invention relates to the technical field of characterization of metal materials and thermophysical properties, in particular to a preparation method of a standard sample of a nickel-based superalloy thermal expansion coefficient and the standard sample.
Background
The material shows the characteristic of expansion or contraction due to the change of the lattice size in the heating or cooling process, so the research on the thermal expansion coefficient (thermal expansion performance) of the material is very important for the fields of mechanical manufacturing and processing, instruments and meters, aerospace and other industries. The thermal expansion coefficient is one of the basic physical properties of the material and one of the performance indexes which must be characterized for determining the application dimension and depth of the material.
The more mature and popular commercial instruments currently used to characterize thermal expansion performance are pusher-rod (ram-method) thermal dilators, interferometric dilators, thermo-mechanical analyzers, and the like. Although the instruments are distributed in various departments and institutions, universities, enterprise laboratories and the like, little attention is paid to whether the measurement results of the instruments are accurate, whether the measurement results are consistent in different time and space, whether the measurement results can be traced, the operation states of the instruments and the like. The standard sample of thermal expansion coefficient is the key to solve the relevant measurement and measurement problems of the instrument, and the evaluation of the whole performance of the instrument by using the standard sample is a more applicable method and is more accepted by the experimenters.
The development of a metal material standard sample which is suitable for high temperature and has a certain thermal expansion coefficient gradient is necessary for meeting the performance evaluation of a thermal expansion instrument, the check of personnel, the comparison of methods and the like, particularly for the analysis standard of the thermal expansion coefficient of a metal material.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a preparation method of a standard sample of a nickel-based superalloy thermal expansion coefficient and the standard sample.
In a first aspect, a method for preparing a standard sample of the thermal expansion coefficient of a nickel-based superalloy is provided, which comprises the following steps:
s100, designing chemical components,
wherein the design value of the mass percent of each component is as follows: 2-4% of Mn, 6-9% of Cr, 1-4% of Fe, 4-6% of W and 80-84% of Ni;
s200, smelting the raw materials,
adding electrolytic pure manganese, electrolytic pure chromium sheets, industrial pure iron, pure tungsten and pure nickel into a vacuum smelting furnace according to a designed proportion for smelting to obtain a high-temperature alloy ingot;
s300, forging and processing,
forging a high-temperature alloy ingot into a plurality of metal round rods with preset sizes;
s400, carrying out heat treatment,
placing the metal round bar in a vacuum heat treatment furnace, and performing circulation for a plurality of times according to the steps of heating, heat preservation and tempering;
s500, naturally aging,
wherein, the metal round bar is placed in a conventional storage room for more than a preset time;
s600, carrying out primary uniformity detection,
wherein, the metal round bar is subjected to tissue inspection, chemical composition segregation inspection and thermal expansion coefficient inspection;
next, rejecting round bar samples which are unqualified in the uniformity initial inspection;
s700, processing the sample,
processing a metal round bar into a cylindrical finished product sample with a preset size;
next, each cylindrical finished sample was packaged as an independent unit.
Optionally, in S600, the uniformity initial checking step includes:
s601, sampling at two ends of a metal round rod, cutting to a height of not less than 5mm, and inspecting macrostructure and grain size after grinding, polishing and corroding the cut sample section;
s602, sampling the head, the middle and the tail of a metal round bar, intercepting each section to have a height of not less than 20-30 mm, performing component segregation test on elements easy to segregate such as C, Si, Mn, Cr, Fe and S by using a direct-reading spectrometer, and performing 10 times of measurement at the head, the middle and the tail respectively to obtain an average value and a standard deviation, wherein when the range of the average value of the three position measurements is less than the repeatability limit r specified by a high-temperature alloy determination spark discharge atomic emission spectrometry, the segregation test is considered to be qualified;
s603, processing three small materials sampled from the head, the middle and the tail of the metal round rod into 3 small samples with the diameter of 6-8 mm and the length of not less than 20-30 mm, testing the 3 small samples according to the same fixed value measuring method, and determining that the uniformity initial test passes when the data of three groups of temperature points meet the repeatability requirement of the expected design.
Optionally, the method further comprises:
s800, uniformity inspection, wherein the method comprises the following steps:
s801, size uniformity inspection: measuring the diameter and the length of the sample, and determining whether the verticality meets the requirement;
s802, thermal expansion coefficient magnitude uniformity test: selecting n samples from a finished product, testing each sample once to obtain a first data set, randomly selecting 1 sample from the n samples each time, repeating the test on the selected samples m times to obtain a second data set, and verifying the uniformity by adopting a single-factor variance analysis method;
s803, when the variance between the groups in the uniformity study among the bottles is larger than the variance in the groups, the standard deviation among the bottles and the uncertainty component caused by the non-uniformity among the bottles are calculated by the following formula:
Figure BDA0003653041660000031
when the interclass variance in the interclass uniformity study is less than the intraclass variance, the following formula is used to calculate the standard deviation between bottles and the uncertainty component due to interclass non-uniformity:
Figure BDA0003653041660000032
wherein, MS among Representing variance between groups, i.e. first dataVariance of group, MS within Denotes the intra-group variance, i.e. the variance of the measured repeatability of the second data set, V denotes the degree of freedom, s bb Denotes the standard deviation, u, between bottles bb Representing the component of uncertainty due to inter-vial non-uniformity, n represents the number of observations, n 0 Represents the number of valid units, which equals n when no data is missing;
s804, after the thermal expansion coefficient results of all temperature points of the first data set and the second data set are summarized, the uniformity of the standard sample is evaluated by a single-factor variance method, and if the statistic value F is less than a critical value F (n-1, m-1) 0.05 Then, it indicates that there is no significant difference in the inter-group variation compared to the intra-group variation, and the candidate standard sample is uniform, wherein F represents the statistical value of the F distribution, n-1 represents the degree of freedom of the first data group, m-1 represents the degree of freedom of the second data group, 0.05 represents the significance level, F (n-1, m-1) 0.05 F test critical values when the significance level is 0.05 and the degrees of freedom between groups and in groups are n-1 and m-1 respectively;
s805, comparing the relative standard deviation of the first data set and the second data set with the design requirement, and determining the uniformity.
Optionally, the method further comprises:
s900, standard sample valuing, wherein the standard sample valuing comprises the following steps:
s901, selecting a cooperation fixed value in a plurality of tests;
s902, determining a measurement method, wherein the initial temperature is set to be 20 ℃ or 30 ℃, the temperature range is 1050 ℃ at most, and the average thermal expansion coefficients of 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ and 1000 ℃ are respectively measured;
s903, setting the temperature rise rate to be 5 ℃/min, and selecting N 2 Or other inert atmosphere protection;
s904, collecting the data of each laboratory, and carrying out fixed value inspection;
and S905, summarizing laboratory data after the constant value inspection is passed, calculating a total average value and a standard deviation, and taking the average value of unit average values of the constant values as a standard value.
Optionally, after S905, the method further includes:
and S906, performing polynomial linear fitting on the obtained data to obtain a fitting equation of the thermal expansion coefficient and the temperature correlation.
Optionally, after the laboratory data are summarized in S904, a quantitative test is performed, including:
s9041, after all data are collected, all fixed value analysis data are tested by a Charcot-Wilkeley method for normality, if a statistic W > W (0.05, n) or W (0.01, n), each group of data is in a normal distribution or an approximate normal distribution, wherein W represents a normal statistic, 0.05 represents a significance level, 0.01 represents a significance level, n represents the number of the measured data groups, W (0.05, n) represents a normal statistic with the number of the measured data groups being n when the significance level is 0.05, and W (0.01, n) represents a normal statistic with the number of the measured data groups being n when the significance level is 0.01;
s9042, after all data are gathered, carrying out abnormal value inspection on the average value of each laboratory by using a Grabbs inspection method, and judging that the Grabbs inspection is qualified if the values of the fixed-value data of the thermal expansion coefficients of each temperature point, the Grabbs inspection statistics Gmax and Gmin are both smaller than a critical value G (0.05, n) or G (0.01, n), wherein Gmin represents a Grabbs minimum value, Gmax represents a Grabbs maximum value, 0.05 represents a significance level, 0.01 represents a significance level, n represents the number of measured data groups, G (0.05, n) represents a Grabbs critical value with the number of data groups being n when the significance level is 0.05, and G (0.01, n) represents a Grabbs critical value with the number of data groups being n when the significance level is 0.01;
s9043, after all data are gathered, performing equal precision test on all constant value data by using a Kokelen valve, and if the Cokelen test statistic value C of each temperature point constant value data is smaller than a critical value C0.05(n) or C0.01(n), indicating that the Kokelen test is qualified, wherein C represents a Kokelen statistic, 0.05 represents a significance level, 0.01 represents a significance level, n represents the number of measured data sets, C0.05(n) represents a Kokelen critical value with the number of data sets n measured when the significance level is 0.05, and C0.01(n) represents a Kokelen critical value with the number of data sets n measured when the significance level is 0.01.
Optionally, the method further comprises:
s10, stability assessment, comprising:
s1001, evaluating the second data set by adopting a trend analysis method, wherein a basic model of stability research is as follows:
Y＝β 0 +β 1 X+ε
wherein X is the number of measurements, Y is the coefficient of thermal expansion value corresponding to each measurement, and beta 0 、β 1 Is a regression coefficient; ε is the random error component;
s1002, carrying out linear regression on the thermal expansion coefficient measured value and the corresponding measuring times to obtain a slope b 1 And the standard deviation s (b) of the slope 1 ) Verifying the significance of the slope change by using a t-test method when b 1 Absolute value less than or equal to t 0.95,(n-2) S (b1), indicating that the slope is not significant and no instability is observed, wherein 0.95 represents the confidence probability, n-2 represents the degree of freedom, t 0.95,(n-2) Representing a t-test value with a confidence probability of 0.95 and a degree of freedom of n-2.
S1003, evaluating the significance of regression by using a one-factor variance method, and when the F test value is not more than F (1, n-2) 0.05 It was shown that regression was not significant, i.e. no tendency to instability occurred, where 1 is the degree of freedom of regression, n-2 is the degree of freedom of residual, 0.05 is the level of significance, F (1, n-2) 0.05 F-test cut-off values representing a significance level of 0.05 and regression and residual degrees of freedom of 1 and n-2, respectively, were calculated as follows:
linearly regressing the measured value of the thermal expansion coefficient and the corresponding measuring times to obtain a linear variance Y-b 0 +b 1 X, number of measurements X i Carrying into an equation to obtain a regression value
Figure BDA0003653041660000051
Separately calculating the variance MS of the regression reg Variance s of sum residual 2 Then, then
Figure BDA0003653041660000052
Optionally, the method further comprises:
s11, stability monitoring, including:
s1101, measuring data at least three times in tracking monitoring for not less than one year;
s1102, if the difference value between each measured value and the mean value is less than or equal to U, the standard sample is stable in the observation period;
s1103, if the range of the repeated measurement or the accumulated measurement is less than or equal to 2U, the standard sample is stable in the observation period.
Optionally, the method further comprises:
s12, uncertainty evaluation, comprising:
s1201, calculating the uncertainty of the synthesis standard by the following formula:
Figure BDA0003653041660000053
wherein:
Figure BDA0003653041660000054
wherein u is CRM Standard uncertainty, u, representing the magnitude of each characteristic char Representing the uncertainty, u, arising from the measurement of each characteristic quantity bb Representing the uncertainty, u, introduced by the inter-bottle heterogeneity counted by the homogeneity test for each characteristic quantity lts Representing the long-term stability uncertainty, u, of each characteristic magnitude sts Representing short-term stability uncertainty of each characteristic quantity value, S representing single measurement standard deviation of constant value statistics, and n representing number of measured data groups;
s1202, the calculation formula of the expansion uncertainty of each characteristic quantity value is as follows: u-ku CRM ，
Wherein U represents the expansion uncertainty of each characteristic magnitude, k is an inclusion factor, U CRM Indicating the standard uncertainty for each characteristic magnitude.
In a second aspect, there is provided a standard sample manufactured according to the method for preparing a standard sample of a nickel-base superalloy thermal expansion coefficient according to any of the above.
The invention can have the following beneficial effects:
the standard sample prepared by the preparation method of the nickel-based superalloy thermal expansion coefficient standard sample can meet the requirements of thermal expansion performance analysis of metal materials and quality control of a thermal expansion instrument, can be reused, has the relative standard deviation of repeated measurement of the thermal expansion coefficient of each temperature point not more than 10 percent and the relative expansion uncertainty not more than 5 percent of the value of the point, and fills the blank in the field of related standard samples in the fields of home and abroad.
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The accompanying drawings, which are included to provide a further understanding of embodiments of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of a method for preparing a standard sample of the coefficient of thermal expansion of a nickel-based superalloy according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a sampling site for uniformity initial inspection according to an embodiment of the present invention;
FIG. 3 is a statistical result diagram of a constant value test provided in accordance with an embodiment of the present invention;
FIG. 4 is a graph of constant data and a linear fit curve according to an embodiment of the present invention;
FIG. 5 is a graph of second data set uniformity test results provided in accordance with an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail and completely with reference to the following detailed description of the invention and the accompanying drawings. It is to be understood that the described embodiments are merely some embodiments of the invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making creative efforts based on the embodiments of the present invention, belong to the protection scope of the present invention.
The following examples are given to further illustrate embodiments of the present invention, but the present invention is not limited to the following examples.
The technical problem to be solved by the invention is to provide a preparation method of a standard sample of the thermal expansion coefficient of the nickel-based superalloy, which meets the requirements of thermal expansion performance analysis of metal materials and quality control of a thermal expansion instrument. The standard sample developed by the method fills the blank of the related standard sample field in the domestic and foreign fields.
The thermal expansion coefficient characteristic magnitude is designed as follows: the constant temperature points are average thermal expansion coefficients of 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ and 1000 ℃, respectively. The relative standard deviation of multiple repeated measurements of the coefficient of thermal expansion at each temperature point is no greater than 10%, and the relative expansion uncertainty is no greater than 5% of the magnitude at that point.
The nickel-based superalloy has stable chemical components, uniform tissue structure, phase transition temperature higher than 1000 ℃, reusability under specified conditions and small oxidation weight gain, and is an ideal candidate material for a metal thermal expansion coefficient standard sample. Based on this, in a first aspect, an embodiment of the present invention provides a method for preparing a standard sample of a nickel-based superalloy with a thermal expansion coefficient, including the following steps:
and S100, designing chemical components.
Figure BDA0003653041660000061
Figure BDA0003653041660000071
The design value of the mass percent of each component is as follows: 2-4% of Mn, 6-9% of Cr, 1-4% of Fe, 4-6% of W and 80-84% of Ni;
and S200, smelting raw materials.
Adding electrolytic pure manganese, electrolytic pure chromium sheets, industrial pure iron, pure tungsten and pure nickel into a 500kg vacuum smelting furnace according to a designed proportion for smelting to obtain the high-temperature alloy ingot.
And S300, forging.
Wherein, the high-temperature alloy ingot is forged into a plurality of metal round rods with the diameter (15-20) mm and the length of about 1 m.
S400, heat treatment.
Wherein, the metal round bar is placed in a vacuum heat treatment furnace, and the steps of temperature rise, heat preservation and tempering are carried out for a plurality of times of circulation. Illustratively, the mixture is heated to 1050 ℃ at a certain heating rate, is subjected to heat preservation for 30min, is tempered, and is heated again after the temperature is reduced to 100 ℃, the heat preservation and the tempering are carried out, and the total number of 10 cycles is obtained.
And S500, naturally aging.
Wherein the metal round bar is placed in a conventional storage room for not less than 6 months.
S600, performing primary uniformity detection.
Wherein, the metal round bar is subjected to a structure test, a chemical composition segregation test and a thermal expansion coefficient test. Further comprising:
s601, sampling at two ends of the metal round rod, wherein the cutting height is not less than 5mm, and inspecting the macroscopic structure and the grain size after grinding, polishing and corroding the cut sample section.
S602, sampling the head, the middle and the tail of a metal round bar, intercepting each section to a height of not less than 20-30 mm, carrying out component segregation test on elements easy to segregate such as C, Si, Mn, Cr, Fe and S by using a direct-reading spectrometer, respectively carrying out 10 times of measurement at the head, the middle and the tail to obtain an average value and a standard deviation, and considering that the segregation test is qualified when the range of the average value of the three position measurements is less than the repeatability limit r specified by a high-temperature alloy determination spark discharge atomic emission spectrometry (namely the direct-reading spectrometer);
s603, processing three small materials sampled from the head, the middle and the tail of the metal round rod into 3 small samples with the diameter (6-8) mm and the length not less than (20-30) mm, testing the 3 small samples according to the same fixed value measuring method, and determining that the uniformity initial test passes when the data of three groups of temperature points meet the repeatability requirement of the expected design.
And S700, processing the sample.
Wherein the uniformity of the passingProcessing the initially inspected metal round bar into
Figure BDA0003653041660000072
Cylindrical finished samples of 6mm by 25mm, each as an individual packaging unit. During processing, the smooth end surfaces of the two sides are noticed, and the flatness is high, so that the thermal expansion instrument can be conveniently attached to a push rod of the thermal expansion instrument.
S800, uniformity inspection, wherein dimensional uniformity inspection and thermal expansion coefficient inspection are included
S801, size uniformity inspection: the diameter and length of the sample were measured with a vernier caliper, wherein the diameters were measured at the upper, middle and lower portions of the sample, respectively, to check for deviation of the diameters. When the maximum deviation of the diameter is not more than 0.05mm, the verticality of the sample can be considered to meet the requirement.
S802, the thermal expansion coefficient value is uniformly checked. Different from a standard sample taking chemical components as characteristic quantity values, the sample has only 1 independent packaging unit, and uniformity test research in a bottle cannot be carried out; in addition, unlike the standard sample having mechanical properties (tensile strength, impact energy, etc.) as characteristic values, which can be used only once, the sample can be repeatedly used several times under predetermined conditions. The single measurement time is 3.5h, and the test result can be influenced by the factors such as the contact between the sample and the push rod and the like caused by the condition change caused by frequent sample replacement. Therefore, a unique uniformity verification method was devised as follows: selecting n samples from the finished product, testing each sample once to obtain a first data set, then randomly selecting 1 sample from the n samples each time, repeating the test on the selected samples m times to obtain a second data set, and verifying the uniformity by adopting a single-factor variance analysis method. n, m can be determined by those skilled in the art according to actual requirements, and can be, for example, 10, 11, 12, etc.
By the design, the requirement of sample uniformity inspection can be met, the repeatability of the method can be verified, m times of tests are carried out through random sampling, and the later-period assessment of the uncertainty in the bottle is facilitated.
The first sample uniformity evaluation method is given by S803 below:
s803, when the interclass variance (i.e., the variance of the first data set) in the study of the uniformity between bottles is greater than the intraclass variance (i.e., the variance of the second data set), the standard deviation between bottles and the uncertainty component due to the heterogeneity between bottles are calculated using the following equations:
Figure BDA0003653041660000081
when the measurement method used for uniformity evaluation has poor repeatability, MS may be caused among Less than MS within . When the interclass variance in the interclass uniformity study is less than the intraclass variance, the following formula is used to calculate the standard deviation between bottles and the uncertainty component due to interclass non-uniformity:
Figure BDA0003653041660000082
wherein, MS among Representing the interclass variance, i.e. the variance of the first data set, MS within Denotes the intra-group variance, i.e. the variance of the measured repeatability of the second data set, V denotes the degree of freedom, s bb Denotes the standard deviation, u, between bottles bb Representing the component of uncertainty due to inter-vial non-uniformity, n representing the number of observations, n 0 Representing the number of valid units, which is equal to n when no data is missing.
A second sample uniformity evaluation method is given by S804 below:
s804, after the thermal expansion coefficient results of all temperature points of the first data set and the second data set are summarized, a single-factor variance method is used (the uniformity of the standard sample is evaluated, if the statistic value F is less than a critical value F (n-1, m-1) 0.05 Then, it indicates that there is no significant difference in the inter-group variation compared to the intra-group variation, and the candidate standard sample is uniform, wherein F represents the statistical value of the F distribution, n-1 represents the degree of freedom of the first data group, m-1 represents the degree of freedom of the second data group, 0.05 represents the significance level, F (n-1, m-1) 0.05 F-test cut-off values at a significance level of 0.05, with n-1 and m-1 degrees of freedom between and within groups, respectively.
A third sample uniformity evaluation method is given in S805 below:
and S805, comparing the relative standard deviation of the first data set and the second data set with the design requirement, wherein the standard deviation is within the design requirement, and the uniformity of the characterization sample is good.
In practical use, the uniformity test can be performed by any one, two or three of the above three methods, which is not limited in this embodiment.
S900, standard sample valuing, wherein the standard sample valuing comprises the following steps:
and S901, selecting a cooperative fixed value in a plurality of tests. A mode of cooperative valuing of a plurality of laboratories is adopted, and the number of laboratories is not less than 8; the measuring instrument covers mainstream instrument manufacturers and models.
S902, determining a measurement method, wherein the initial temperature is set to be 20 ℃ or 30 ℃, the temperature range is 1050 ℃ at most, and the average thermal expansion coefficients of 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ and 1000 ℃ are respectively measured;
s903, setting the temperature rise rate to be 5 ℃/min, and selecting N 2 Or other inert atmosphere. Note that 20 ℃ or 30 ℃ is selected as the starting temperature, and the temperature needs to be kept for a period of time and then increased.
And S904, correcting the equipment before formal testing to ensure that the drift of the instrument does not influence the test result. The pillars were defined with alumina, and the sample was attached to the pillars. After the data in each laboratory are collected, the data are checked for fixed values. It should be noted that: if the laboratory-provided data has significant outliers or does not meet statistical requirements, it is retained unless specifically necessary to retest or cull the process. The fixed value test specifically comprises:
s9041, after all data are collected, all fixed value analysis data are tested by a Charcot-Wilkeley method for normality, if a statistic W > W (0.05, n) or W (0.01, n), each group of data is in a normal distribution or an approximate normal distribution, wherein W represents a normal statistic, 0.05 represents a significance level, 0.01 represents a significance level, n represents the number of the measured data groups, W (0.05, n) represents a normal statistic with the number of the measured data groups being n when the significance level is 0.05, and W (0.01, n) represents a normal statistic with the number of the measured data groups being n when the significance level is 0.01.
S9042, after all data are gathered, performing abnormal value test on the average value of each laboratory by using a Grabbs test method, and judging that the Grabbs test is qualified if the values of the fixed-value data of the thermal expansion coefficients of each temperature point, the Grabbs test statistics Gmax and Gmin are both smaller than a critical value G (0.05, n) or G (0.01, n), wherein Gmin represents a Grabbs minimum value, Gmax represents a Grabbs maximum value, 0.05 represents a significance level, 0.01 represents a significance level, n represents the number of measured data groups, G (0.05, n) represents a Grabbs critical value with the number of data groups being n when the significance level is 0.05, and G (0.01, n) represents a Grabbs critical value with the number of data groups being n when the significance level is 0.01.
S9043, after all data are gathered, performing equal precision test on all constant value data by using a Kokelen valve, and if the Cokelen test statistic value C of each temperature point constant value data is smaller than a critical value C0.05(n) or C0.01(n), indicating that the Kokelen test is qualified, wherein C represents a Kokelen statistic, 0.05 represents a significance level, 0.01 represents a significance level, n represents the number of measured data sets, C0.05(n) represents a Kokelen critical value with the number of data sets n measured when the significance level is 0.05, and C0.01(n) represents a Kokelen critical value with the number of data sets n measured when the significance level is 0.01.
And S905, summarizing laboratory data after the constant value inspection is passed, calculating a total average value and a standard deviation, and taking the average value of unit average values of the constant values as a standard value.
And S906, performing polynomial linear fitting on the obtained data to obtain a fitting equation of the thermal expansion coefficient and the temperature correlation. By the design, the thermal expansion coefficients of more temperature points can be obtained, and the general range of the material is improved. A polynomial of degree 5 may be selected as the hypothesis function in linear fitting.
S10, stability assessment, comprising:
s1001, a trend analysis method is adopted to evaluate a second data set, and a basic model of stability research is as follows:
Y＝β 0 +β 1 X+ε
wherein X is the number of measurements, Y is the coefficient of thermal expansion value corresponding to each measurement, and beta 0 、β 1 Is a regression coefficient; ε is the random error component. After the measurement data are substituted for solving, beta can be calculated 0 、β 1 、ε。
Wherein the slope estimate b 1 Calculated using the formula:
Figure BDA0003653041660000101
estimate of intercept b 0 Calculated using the formula:
Figure BDA0003653041660000102
s(b 1 ) Is b is 1 Is calculated using the following formula:
Figure BDA0003653041660000103
the first stability evaluation mode is given by S1002 below:
s1002, performing linear regression on the thermal expansion coefficient measured value and the corresponding measuring times to obtain a slope b 1 And the standard deviation s (b) of the slope 1 ) Verifying the significance of the slope change by using a t-test method when b 1 Absolute value less than or equal to t 0.95,(n-2) S (b1), indicating that the slope is not significant and no instability is observed, wherein 0.95 represents the confidence probability, n-2 represents the degree of freedom, t 0.95,(n-2) Representing a t-test value with a confidence probability of 0.95 and a degree of freedom of n-2.
The second stability evaluation mode is given by S1003 below:
s1003, evaluating the significance of regression by using a one-factor variance method, and when the F test value is not more than F (1, n-2) 0.05 It indicates that the regression was not significant, i.e., there was no instabilityTrends appeared where 1 is the degree of freedom of regression, n-2 is the degree of freedom of residual, 0.05 is the level of significance, F (1, n-2) 0.05 F-test cut-off values representing a significance level of 0.05 and regression and residual degrees of freedom of 1 and n-2, respectively, were calculated as follows:
linearly regressing the measured value of the thermal expansion coefficient and the corresponding measuring times to obtain a linear variance Y-b 0 +b 1 X, number of measurements X i Carrying into an equation to obtain a regression value
Figure BDA0003653041660000114
Separately calculating the variance MS of the regression reg Variance s of sum residual 2 Then, then
Figure BDA0003653041660000111
In addition, the thermal expansion coefficient is related to the chemical composition and the structure of the metal material, the chemical composition of the main elements of the nickel-based superalloy is very stable, and the content of the nickel-based superalloy does not change in the past decades of experience and literature data. The microstructure of the nickel-based superalloy does not change so much after heat treatment to affect the measurement result, so that the material can be considered to be stable, and the physical property of the material is stable enough to ensure the property of thermal expansion.
S11, stability monitoring, comprising:
s1101, measuring data at least three times in tracking monitoring for not less than one year;
s1102, if the difference between each measured value and the mean value is less than or equal to U, that is, | x CRM -x meas When | ≦ U, it indicates that the standard sample is stable in the observation period.
S1103, if the range of the repeated measurement or the accumulated measurement is less than or equal to 2U, the standard sample is stable in the observation period.
S12, uncertainty evaluation, comprising:
s1201, the uncertainty of the synthesis standard generally considers the following aspects: uncertainty mu due to the constant value process char Uncertainty mu due to inhomogeneity bb Uncertainty mu due to short-term stability sts And uncertainty mu due to long-term stability lts The synthesis standard uncertainty was calculated by the following formula:
Figure BDA0003653041660000112
wherein:
Figure BDA0003653041660000113
wherein u is CRM Standard uncertainty, u, representing the magnitude of each characteristic char Representing the uncertainty, u, caused by the measurement of each characteristic quantity bb Representing the uncertainty, u, introduced by the inter-bottle heterogeneity counted by the homogeneity test for each characteristic quantity lts Representing the long-term stability uncertainty, u, of each characteristic magnitude sts And (3) representing the short-term stability uncertainty of each characteristic quantity value, S representing the standard deviation of single measurement of constant value statistics, and n representing the number of measured data groups.
In the above formula, uncertainty μ due to short-term stability and long-term stability sts And mu lts Can be ignored, u char The uncertainty u of the inhomogeneity can be calculated from the formula given above bb I.e. standard deviation s of non-uniformity bb It can be calculated from the formula given in S803.
S1202, the calculation formula of the expansion uncertainty of each characteristic quantity value is as follows: u-ku CRM ，
Wherein U represents the expansion uncertainty of each characteristic magnitude, k is an inclusion factor, U CRM Indicating the standard uncertainty for each characteristic magnitude.
The steps of the preparation method of the nickel-based superalloy thermal expansion coefficient standard sample are described in detail with reference to specific examples as follows:
1) the chemical components are designed as follows:
element(s) C Si Mn Cr Fe W Ni
Measured value/%) 0.017 0.115 2.54 6.90 1.55 5.72 83.1
2) The processing size of the raw material sample rod is 20mm in diameter and 1.5m in length.
3) And (3) checking the tissue structure: the defects of cracks, shrinkage cavities, bubbles, center porosity and the like are not found; the grain size is 2.5 grade.
4) The chemical composition segregation test data is as follows:
Figure BDA0003653041660000121
Figure BDA0003653041660000131
a schematic diagram of the three sampling positions of the head, middle and tail can be seen in fig. 2.
5) The initial inspection data for the uniformity of the thermal expansion coefficient are as follows:
unit x 10 -6 ℃ -1
Figure BDA0003653041660000132
6) All samples were processed: processing the metal round bar into
Figure BDA0003653041660000134
The total number of the cylindrical finished product samples of 6mm multiplied by 25mm is 120, and each sample is used as an independent packaging unit.
7) And (3) uniformity inspection: uniformity test data at 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ and 1000 ℃, and the following figure is an example of an F test at 100 ℃.
100 ℃ homogeneity test data statistics (unit 10) -6 ℃ -1 )
Figure BDA0003653041660000133
Figure BDA0003653041660000141
In the above table, a represents data of the first data group, and B represents data of the second data group.
8) And (4) summarizing uniformity test results:
statistical summary of homogeneity test/. times.10 -6 /K
Temperature range/. degree.C A S A B S B F s bb
30～100 13.22 0.26 13.03 0.16 2.46 0.1897
30～200 14.00 0.19 13.93 0.13 2.02 0.1277
30～300 14.43 0.16 14.45 0.13 1.50 0.0898
30～400 14.81 0.14 14.88 0.13 1.09 0.0372
30～500 15.15 0.12 15.23 0.13 0.786 0.0858
30～600 15.56 0.12 15.66 0.12 0.866 0.0791
30～700 15.92 0.12 16.05 0.11 1.16 0.0426
30～800 16.26 0.14 16.42 0.11 1.60 0.0841
30～900 16.58 0.19 16.80 0.13 2.27 0.1342
30～1000 16.95 0.16 17.16 0.13 1.39 0.0798
In the above table, A represents the mean value of 11 samples tested in the first data set, S A Represents the standard deviation of the test of 11 samples in the first data set; b represents the mean of 11 tests of 1 sample in the second data set, S B Represents the standard deviation of 11 tests on 1 sample in the second data set; f represents a variance test statistic value, and the critical value of F is 2.98; s bb Indicating the standard deviation between bottles.
9) And (3) uniformity inspection:
Figure BDA0003653041660000142
Figure BDA0003653041660000151
in the above table, a-RSD represent the uniformity test data for the first data set and B-RSD represent the uniformity test data for the second data set.
A second data set homogeneity check chart can be seen in fig. 5.
10) Fixed value and uncertainty:
Figure BDA0003653041660000152
the statistical results of the valuing test can be seen in fig. 3.
11) The coefficient of thermal expansion for any temperature within the temperature interval can be represented by a 5 th order polynomial fit:
α(10 -6 ℃ -1 )＝10.3533+0.03183t-9.8814×10 -5 t 2 +1.6627×10 -7 t 3 -1.3514×10 - 10 t 4 +4.2308×10 -14 t 5
the linear fit curve can be seen in fig. 4.
12) And (3) stability test: look-up table t 0.95,10 Was 2.23. When b is 1 Absolute value not greater than t 0.95,10 ·s(b 1 ) It can be stated that the slope is insignificant.
Figure BDA0003653041660000153
Figure BDA0003653041660000161
In a second aspect, embodiments of the present invention provide a standard sample manufactured according to any one of the methods for preparing a nickel-based superalloy thermal expansion coefficient standard sample described above.
Finally, it should be noted that: the above embodiments and examples are only for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments and examples, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments and examples can be modified, or some of the technical features can be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments and examples of the present invention.

Claims (10)

1. The preparation method of the standard sample of the thermal expansion coefficient of the nickel-based superalloy is characterized by comprising the following steps:
s100, designing chemical components,
wherein the design value of the mass percent of each component is as follows: 2-4% of Mn, 6-9% of Cr, 1-4% of Fe, 4-6% of W and 80-84% of Ni;
s200, smelting the raw materials,
adding electrolytic pure manganese, electrolytic pure chromium sheets, industrial pure iron, pure tungsten and pure nickel into a vacuum smelting furnace according to a designed proportion for smelting to obtain a high-temperature alloy ingot;
s300, forging and processing the blank,
forging a high-temperature alloy ingot into a plurality of metal round rods with preset sizes;
s400, carrying out heat treatment,
placing the metal round bar in a vacuum heat treatment furnace, and performing circulation for a plurality of times according to the steps of heating, heat preservation and tempering;
s500, naturally aging,
wherein, the metal round bar is placed in a conventional storage room for more than a preset time;
s600, carrying out primary uniformity detection,
wherein, the metal round bar is subjected to tissue inspection, chemical composition segregation inspection and thermal expansion coefficient inspection;
next, rejecting round bar samples which are unqualified in the uniformity initial inspection;
s700, processing the sample,
processing a metal round bar into a cylindrical finished product sample with a preset size;
next, each cylindrical finished sample was packaged as an independent unit.
2. The method for preparing the standard sample of the thermal expansion coefficient of the nickel-based superalloy as claimed in claim 1, wherein the step of performing uniformity initial inspection, which is S600, comprises:
s601, sampling at two ends of a metal round rod, cutting the metal round rod to be not less than 5mm in height, and inspecting macroscopic structure and grain size after grinding, polishing and corroding the cut sample section;
s602, sampling the head, the middle and the tail of a metal round bar, intercepting each section to have a height of not less than 20-30 mm, performing component segregation test on elements easy to segregate such as C, Si, Mn, Cr, Fe and S by using a direct-reading spectrometer, and performing 10 times of measurement at the head, the middle and the tail respectively to obtain an average value and a standard deviation, wherein when the range of the average value of the three position measurements is less than the repeatability limit r specified by a high-temperature alloy determination spark discharge atomic emission spectrometry, the segregation test is considered to be qualified;
s603, processing three small materials sampled from the head, the middle and the tail of the metal round rod into 3 small samples with the diameter of 6-8 mm and the length of not less than 20-30 mm, testing the 3 small samples according to the same fixed value measuring method, and determining that the uniformity initial test passes when the data of three groups of temperature points meet the repeatability requirement of the expected design.
3. The method for preparing the standard sample of the thermal expansion coefficient of the nickel-based superalloy as claimed in claim 2, further comprising:
s800, uniformity inspection, wherein the method comprises the following steps:
s801, size uniformity inspection: measuring the diameter and the length of the sample, and determining whether the verticality meets the requirement;
s802, thermal expansion coefficient magnitude uniformity test: selecting n samples from a finished product, testing each sample once to obtain a first data set, randomly selecting 1 sample from the n samples each time, repeating the test on the selected samples m times to obtain a second data set, and verifying the uniformity by adopting a single-factor variance analysis method;
s803, when the variance between the groups in the uniformity study among the bottles is larger than the variance in the groups, the standard deviation among the bottles and the uncertainty component caused by the non-uniformity among the bottles are calculated by the following formula:
Figure FDA0003653041650000021
when the interclass variance in the interclass uniformity study is less than the intraclass variance, the following formula is used to calculate the standard deviation between bottles and the uncertainty component due to interclass non-uniformity:
Figure FDA0003653041650000022
wherein, MS among Representing the interclass variance, i.e. the variance of the first data set, MS within Denotes the intra-group variance, i.e. the variance of the measured repeatability of the second data set, V denotes the degree of freedom, s bb Denotes the standard deviation, u, between bottles bb Representing the component of uncertainty due to inter-vial non-uniformity, n representing the number of observations, n 0 Represents the number of valid units, which equals n when no data is missing;
s804, after the thermal expansion coefficient results of all temperature points of the first data set and the second data set are summarized, the uniformity of the standard sample is evaluated by a single-factor variance method, and if the statistic value F is less than a critical value F (n-1, m-1) 0.05 Then, it indicates that there is no significant difference in the inter-group variation compared to the intra-group variation, and the candidate standard sample is uniform, wherein F represents the statistical value of the F distribution, n-1 represents the degree of freedom of the first data group, m-1 represents the degree of freedom of the second data group, 0.05 represents the significance level, F (n-1, m-1) 0.05 F test critical values when the significance level is 0.05 and the degrees of freedom between groups and in groups are n-1 and m-1 respectively;
s805, comparing the relative standard deviation of the first data set and the second data set with the design requirement, and determining the uniformity.
4. The method for preparing the standard sample of the thermal expansion coefficient of the nickel-based superalloy as claimed in claim 3, further comprising:
s900, standard sample valuing, wherein the standard sample valuing comprises the following steps:
s901, selecting a cooperation fixed value in a plurality of tests;
s902, determining a measurement method, wherein the initial temperature is 20 ℃ or 30 ℃, the temperature range is 1050 ℃ at the maximum, and the average thermal expansion coefficients of 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ and 1000 ℃ are respectively measured;
s903, setting the temperature rise rate to be 5 ℃/min, and selecting N 2 Or other inert atmosphere protection;
s904, collecting the data of each laboratory, and carrying out fixed value inspection;
and S905, summarizing laboratory data after the constant value inspection is passed, calculating a total average value and a standard deviation, and taking the average value of unit average values of the constant values as a standard value.
5. The method for preparing the standard sample of the thermal expansion coefficient of the nickel-based superalloy as claimed in claim 4, wherein after step S905, the method further comprises:
and S906, performing polynomial linear fitting on the obtained data to obtain a fitting equation of the thermal expansion coefficient and the temperature correlation.
6. The method for preparing the standard sample of the thermal expansion coefficient of the nickel-based superalloy as claimed in claim 5, wherein the step of collecting the laboratory data in step S904 and performing a fixed value test comprises:
s9041, after all data are gathered, all definite value analysis data are tested by a Charcot-Wilkeley method to analyze the normality of the data, if a statistic W > W (0.05, n) or W (0.01, n), the data are in normal distribution or approximate normal distribution, wherein W represents normal statistic, 0.05 represents significance level, 0.01 represents significance level, n represents measured data group number, W (0.05, n) represents normal statistic with n data group number measured when the significance level is 0.05, and W (0.01, n) represents normal statistic with n data group number measured when the significance level is 0.01;
s9042, after all data are gathered, carrying out abnormal value inspection on the average value of each laboratory by using a Grabbs inspection method, and judging that the Grabbs inspection is qualified if the values of the fixed-value data of the thermal expansion coefficients of each temperature point, the Grabbs inspection statistics Gmax and Gmin are both smaller than a critical value G (0.05, n) or G (0.01, n), wherein Gmin represents a Grabbs minimum value, Gmax represents a Grabbs maximum value, 0.05 represents a significance level, 0.01 represents a significance level, n represents the number of measured data groups, G (0.05, n) represents a Grabbs critical value with the number of data groups being n when the significance level is 0.05, and G (0.01, n) represents a Grabbs critical value with the number of data groups being n when the significance level is 0.01;
s9043, after all data are gathered, performing equal precision test on all constant value data by using a Kokelen method, and if the Cokelen test statistic value C of each temperature point constant value data is smaller than a critical value C0.05(n) or C0.01(n), indicating that the Kokelen test is qualified, wherein C represents a Kokelen statistic, 0.05 represents a significance level, 0.01 represents a significance level, n represents the number of measured data sets, C0.05(n) represents a Kokelen critical value with the number of data sets being n when the significance level is 0.05, and C0.01(n) represents a Kokelen critical value with the number of data sets being n when the significance level is 0.01.
7. The method for preparing the standard sample of the thermal expansion coefficient of the nickel-based superalloy as claimed in claim 6, further comprising:
s10, stability assessment, comprising:
s1001, evaluating the second data set by adopting a trend analysis method, wherein a basic model of stability research is as follows:
Y＝β 0 +β 1 X+ε
wherein X is the number of measurements, Y is the coefficient of thermal expansion value corresponding to each measurement, and beta 0 、β 1 Is a regression coefficient; ε is the random error component;
s1002, expanding heatPerforming linear regression on the expansion coefficient measurement value and the corresponding measurement times to obtain a slope b 1 And the standard deviation s (b) of the slope 1 ) Verifying the significance of the slope change by using a t test method when b 1 Absolute value less than or equal to t 0.95,(n-2) S (b1), indicating that the slope is not significant and no instability is observed, wherein 0.95 represents the confidence probability, n-2 represents the degree of freedom, t 0.95,(n-2) A t test value representing a confidence probability of 0.95 and a degree of freedom of n-2;
s1003, evaluating the significance of regression by using a one-factor variance method, and when the F test value is not more than F (1, n-2) 0.05 It was shown that regression was not significant, i.e. no tendency to instability occurred, where 1 is the degree of freedom of regression, n-2 is the degree of freedom of residual, 0.05 is the level of significance, F (1, n-2) 0.05 F-test cut-off values representing a significance level of 0.05 and regression and residual degrees of freedom of 1 and n-2, respectively, were calculated as follows:
linearly regressing the measured value of the thermal expansion coefficient and the corresponding measuring times to obtain a linear variance Y-b 0 +b 1 X, number of measurements X i Carrying into an equation to obtain a regression value
Figure FDA0003653041650000041
Separately calculating the variance MS of the regression reg Variance s of sum residual 2 Then, then
Figure FDA0003653041650000042
8. The method for preparing the standard sample of the thermal expansion coefficient of the nickel-based superalloy as claimed in claim 7, further comprising:
s11, stability monitoring, comprising:
s1101, measuring data at least three times in tracking monitoring for not less than one year;
s1102, if the difference value between each measured value and the mean value is less than or equal to U, the standard sample is stable in the observation period;
s1103, if the range of the repeated measurement or the accumulated measurement is less than or equal to 2U, the standard sample is stable in the observation period.
9. The method for preparing the standard sample of the thermal expansion coefficient of the nickel-based superalloy as claimed in claim 8, further comprising:
s12, uncertainty evaluation, comprising:
s1201, calculating the uncertainty of the synthesis standard by the following formula:
Figure FDA0003653041650000043
wherein:
Figure FDA0003653041650000051
wherein u is CRM Standard uncertainty, u, representing the magnitude of each characteristic char Representing the uncertainty, u, arising from the measurement of each characteristic quantity bb Representing the uncertainty, u, introduced by the inter-bottle heterogeneity counted by the homogeneity test for each characteristic quantity lts Representing the long-term stability uncertainty, u, of each characteristic magnitude sts Representing short-term stability uncertainty of each characteristic quantity value, S representing single measurement standard deviation of constant value statistics, and n representing number of measured data groups;
s1202, the calculation formula of the expansion uncertainty of each characteristic quantity value is as follows: u-ku CRM ，
Wherein U represents the extended uncertainty of each characteristic magnitude, k is an inclusion factor, U CRM Indicating the standard uncertainty for each characteristic magnitude.
10. A standard sample manufactured by the method for preparing a nickel-base superalloy thermal expansion coefficient standard sample according to any one of claims 1 to 9.
CN202210547144.3A 2022-05-19 2022-05-19 Preparation method of standard sample of thermal expansion coefficient of nickel-based superalloy and standard sample Pending CN114964961A (en)

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