Preparation method of FGH4097 thermal diffusion coefficient standard sample

Abstract

The invention relates to a preparation method of an FGH4097 thermal diffusion coefficient standard sample, which comprises the following steps of: preparing a flaky FGH4097 standard sample candidate material by adopting a powder metallurgy and hot isostatic pressing process, carrying out uniformity test, stability test and multi-laboratory valuing by a confirmed analysis method, and carrying out statistics and assignment on data in a reasonable statistical mode to obtain the FGH4097 thermal diffusion coefficient standard sample. Finally, the FGH4097 thermal diffusion coefficient standard sample which is uniform in structure, good in thermal diffusion coefficient uniformity and stability at each temperature point, accurate and reliable in quantity value and reasonable in uncertainty evaluation is obtained.

Description

Technical Field

[0001] This invention belongs to the field of thermal analysis standard sample preparation, and relates to a method for preparing an FGH4097 thermal diffusivity standard sample. Background Technology

[0002] High-temperature alloys are indispensable key materials in the aerospace industry, hailed as the "cornerstone of engines." Their superior high-temperature strength, resistance to thermal fatigue, oxidation, and corrosion make them the preferred material for manufacturing hot-section components of aero-engines and spacecraft. FGH4097 is a nickel-based high-temperature alloy prepared using powder metallurgy, possessing advantages such as uniform microstructure, fine grains, and good hot-working deformation properties. It is mainly used in the hottest and most stress-prone parts of engines, such as turbine blades, turbine disks, guide vanes, and combustion chambers. These components need to operate reliably for extended periods in high-temperature exhaust gases exceeding 600°C, enduring enormous centrifugal forces and thermal stresses. The performance of FGH4097 high-temperature alloy directly determines the thrust, efficiency, lifespan, and safety of an engine, and is a core technological guarantee for achieving high thrust-to-weight ratios in advanced high-thrust aero-engines.

[0003] The thermal diffusivity measures the ability of a high-temperature alloy material to achieve a uniform internal temperature. It directly determines the "speed" and "efficiency" of heat transfer within a component during heating or cooling. A higher thermal diffusivity means that the internal temperature distribution reaches equilibrium more quickly when the temperature changes, i.e., it "heats up quickly and cools down quickly," and has lower internal thermal stress. Currently, GB / T22588-2008, "Measurement of Thermal Diffusivity or Thermal Conductivity by Flash Method," is the most widely used method for characterizing thermal diffusivity. While the flash method itself is an absolute analytical method, it is subject to random and systematic errors during actual measurements. Therefore, equipment calibration is necessary to ensure the accuracy and traceability of the measured values. A common method for equipment calibration is to measure standard samples / materials with the same / similar matrix; however, no reports have been found regarding FGH4097 thermal diffusivity standard samples / materials to date. Summary of the Invention

[0004] To address the aforementioned technical problems, this invention provides a method for preparing a standard sample of FGH4097 thermal diffusivity. This method can produce FGH4097 thermal diffusivity standard samples with uniform structure, good stability, and accurate values. It can be used not only for equipment calibration, quality control, and method verification of the thermal diffusivity of FGH4097 material, but also for quality control and standard sample development of other matrix-similar materials.

[0005] The technical solution of the present invention is as follows:

[0006] A method for preparing a standard sample of FGH4097 thermal diffusivity includes the following steps:

[0007] (1) Based on the FGH4097 thermal diffusivity standard sample, the following raw materials were selected: electrolytic nickel (purity greater than 99.9%), nickel foil, metallic chromium, aluminum briquettes, molybdenum bars, pure iron, pure manganese, electrolytic cobalt, nickel-titanium alloy, nickel-cerium alloy, nickel-boron alloy, nickel-niobium alloy, nickel-tungsten alloy, nickel-phosphorus alloy, sponge zirconium, high-purity silicon, pure carbon, pure tantalum, and pure hafnium.

[0008] (2) Place the electrolytic nickel (purity greater than 99.9%), molybdenum bar, electrolytic cobalt, nickel-tungsten alloy, pure iron, pure manganese, high-purity silicon, pure carbon, pure hafnium and pure tantalum from step (1) into a vacuum melting furnace in sequence, and control the melting and refining conditions until all raw materials are melted into molten liquid;

[0009] (3) Add aluminum briquettes, nickel-titanium alloy, metallic chromium, and nickel-niobium alloy to the molten liquid obtained in step (2), and control the second refining conditions until all raw materials are melted to further obtain the molten liquid;

[0010] (4) Add nickel-cerium alloy, nickel-boron alloy, nickel-phosphorus alloy and sponge zirconium wrapped with nickel foil to the molten liquid obtained in step (3), control the pouring conditions until the steel is tapped, and obtain the refined FGH4097 ingot.

[0011] (5) The FGH4097 ingot obtained in step (4) is prepared into FGH4097 powder using the plasma rotating electrode method.

[0012] (6) The FGH4097 powder obtained in step (5) is sieved in an inert gas Ar atmosphere and placed in a package to prepare FGH4097 rods by hot isostatic pressing.

[0013] (7) Heat-treat the FGH4097 bar obtained in step (6);

[0014] (8) Prepare samples of the FGH4097 bars that have undergone heat treatment in step (7) to make candidate materials for standard samples of thermal diffusivity of specified size;

[0015] (9) The candidate materials obtained in step (8) are evaluated for chemical composition uniformity in accordance with GB / T 15000.3-2023 "Standard Sample Working Guide Part 3: Standard Sample Value Determination and Uniformity and Stability Assessment" to obtain standard sample candidate materials with uniform thermal diffusivity.

[0016] (10) The candidate material of thermal diffusivity standard sample with uniform chemical composition obtained in step (9) is subjected to uniformity test, stability test, value determination and assignment by multiple laboratories in accordance with the provisions of GB / T15000 "Standard Sample Working Guide" and YS / T 409-2012 "Technical Specification for Standard Samples for Analysis of Non-ferrous Metal Products", and finally the FGH4097 thermal diffusivity standard sample with accurate value is obtained.

[0017] in,

[0018] In step (1), the composition of each raw material is as follows (by mass percentage): Al 4.90%~5.20%, B 0.010%~0.012%, C 0.04%~0.05%, Ce 0.007%~0.008%, Co 15.5%~16.0%, Cr 9.00%~9.50%, Fe 0.02%~0.03%, Mn 0.008%~0.009%, Mo 3.70%~3.80%, Mg 0.045%~0.050%, Nb 2.50%~2.60%, Hf 0.30%~0.40%, P 0.010%~0.015%, S 0.010%~0.014%, Si 0.16%~0.018%, Ta 0.20%~0.30%, Ti 1.80%~1.90%, W 5.30%~5.50%, Zr 0.011%~0.013%, balance Ni.

[0019] For example, weigh out 4.7 kg to 5.2 kg of electrolytic nickel (purity greater than 99.9%), 0.37 kg to 0.38 kg of molybdenum bars, 1.55 kg to 1.60 kg of electrolytic cobalt, 0.66 kg to 0.69 kg of nickel-tungsten alloy, 0.002 kg to 0.003 kg of pure iron, 0.0008 kg to 0.0010 kg of pure manganese, 0.016 kg to 0.018 kg of high-purity silicon, 0.003 kg to 0.005 kg of pure carbon, 0.03 kg to 0.04 kg of pure hafnium, 0.02 kg to 0.03 kg of pure tantalum, 0.5 kg to 0.6 kg of aluminum briquettes, 0.30 kg to 0.45 kg of nickel-titanium alloy, 0.9 kg to 0.95 kg of metallic chromium, 0.5 kg to 0.52 kg of nickel-niobium alloy, 0.008 kg to 0.02 kg of nickel-cerium alloy, and 0.005 kg of other materials. 0.008 kg of nickel-boron alloy, 0.005 kg of nickel-phosphorus alloy, and 0.0011 kg of sponge zirconium;

[0020] It should be noted that the purity of the metals used in this invention is no less than 99%, and the alloys are prepared in-house using the corresponding high-purity metals.

[0021] In step (2), the melting conditions are a controlled temperature of 1480℃~1620℃ and a time of 5 min~60 min, and the refining conditions are a controlled temperature of 1530℃~1580℃ and a time of 5 min~60 min under magnetic stirring. Preferably, the melting conditions are a controlled temperature of 1500℃~1600℃ and a time of 20 min~40 min; and the refining conditions are a controlled temperature of 1540℃~1560℃ and a time of 20 min~60 min.

[0022] In step (3), the temperature of the second refining is controlled at 1520℃~1570℃ and the time is 5 min~60 min; preferably, the temperature of the second refining is controlled at 1540℃~1560℃ and the time is 20 min~40 min.

[0023] In step (4), the pouring conditions are to control the temperature at 1440℃~1510℃ for 5 min~30 min under magnetic stirring; preferably, the pouring conditions are to control the temperature at 1460℃~1490℃ for 5 min~15 min.

[0024] In step (5), the particle size of FGH4097 powder prepared by the plasma rotating electrode method is between 0 μm and 250 μm;

[0025] In step (6), the powder obtained by sieving has a particle size between 50 μm and 100 μm. The pressing conditions of the hot isostatic pressing method are a pressure between 100 MPa and 200 MPa, a temperature between 1150°C and 1250°C, a holding time of 3 h to 5 h, and a cooling method of air cooling or furnace cooling.

[0026] In step (7), the heat treatment conditions are solution treatment + air cooling + two-stage aging. That is, the temperature is raised to 1100℃~1300℃ and held for 3 h~10 h, then rapidly cooled to room temperature, then the temperature is raised to 850℃~1000℃ and held for 3 h~12 h, then cooled to 600℃~850℃ and held for 8 h~36 h, and then cooled to room temperature in the furnace.

[0027] In step (8), the specified size of the candidate material for the thermal diffusivity standard sample is to prepare a disc with a diameter of 11.5 mm to 12.3 mm and a thickness of 2.3 mm to 2.8 mm;

[0028] In step (9), the chemical composition uniformity assessment is carried out by using inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry, spark discharge atomic emission spectrometry and high-frequency induction combustion-infrared absorption method to determine the content of each component in the candidate material of FGH4097 disc-shaped thermal diffusivity standard sample, and to test the uniformity of chemical composition.

[0029] In step (10), the conditions for the uniformity test, stability test and multiple laboratory value determination of the thermal diffusivity coefficient are as follows: under the atmosphere of high-purity argon, at an initial temperature of 25℃, a maximum temperature of 1000℃, and a heating rate of 10℃ / min, the average thermal diffusivity of the standard sample candidate material is measured at 100℃, 200℃, 300℃, 400℃, 500℃, 600℃, 700℃, 800℃, 900℃ and 1000℃.

[0030] In step (10), the assignment is based on GB / T 15000 "Standard Sample Working Guidelines" and YS / T 409-2012 "Technical Specifications for Standard Samples for Analysis of Non-ferrous Metal Products". Statistical methods are used to analyze the value data of multiple laboratories, outliers are removed, and the average value of the thermal diffusivity is calculated after normality test and equal precision test. The average value is then used as the standard value of the FGH4097 thermal diffusivity standard sample.

[0031] In step (10), the assignment is based on GB / T 15000 "Standard Sample Working Guidelines" and YS / T 409-2012 "Technical Specifications for Standard Samples for Analysis of Non-ferrous Metal Products", etc., using reasonable methods to evaluate the uncertainty introduced by homogeneity, the uncertainty introduced by stability and the uncertainty introduced by the fixed value, calculate the combined uncertainty and expanded uncertainty of the thermal diffusivity, and use the expanded uncertainty as the expanded uncertainty of the FGH4097 thermal diffusivity standard sample.

[0032] It should be noted that the temperature controlled in the above steps of the present invention is generally controlled within ±5°C of the corresponding temperature.

[0033] In one application, the standard sample prepared in the present invention is used in the analysis of the thermal diffusivity of FGH4097 material.

[0034] The standard samples are sealed in plastic bags, one sample per bag, and placed inside a packaging box lined with foam padding. These standard samples should be stored at room temperature and pressure, protected from light, and effective measures must be taken to prevent violent shaking during transportation.

[0035] Beneficial effects

[0036] The method for preparing FGH4097 thermal diffusivity standard samples provided by this invention produces standard samples with uniform microstructure distribution, good uniformity of thermal diffusivity, good stability of thermal diffusivity, and accurate values ​​of FGH4097 thermal diffusivity. This method can be used not only for equipment calibration, quality control, and method verification of the thermal diffusivity of FGH4097 material, but also for quality control and standard sample development of other matrix-similar materials. Specifically,

[0037] This invention uses electrolytic nickel (purity greater than 99.9%) and other metals or alloys as raw materials. By adding metals and metal alloys and using powder metallurgy + hot isostatic pressing process, flake-shaped FGH4097 standard sample candidate materials are prepared. Uniformity test, stability test and value determination by multiple laboratories are carried out by confirmed analytical methods. The data are statistically analyzed and assigned values ​​by reasonable statistical methods. Finally, FGH4097 thermal diffusivity standard sample with uniform structure, good stability, accurate and reliable values ​​and reasonable uncertainty assessment is obtained.

[0038] The standard samples prepared in this way ensure the accuracy of test results for high-temperature alloy materials with the same or similar matrix. They can also be used for instrument verification and method validation in the laboratory, making the FGH4097 thermal diffusivity test highly accurate, with small error and traceability, and also has huge market potential and value. Detailed Implementation

[0039] The present invention will be described in detail below through specific embodiments, as follows:

[0040] Example 1

[0041] The method for preparing the FGH4097 thermal diffusivity standard sample for thermal analysis of the present invention can be used for testing the thermal diffusivity, and includes the following steps:

[0042] (1) Based on the FGH4097 thermal diffusivity standard sample, design the distribution ratio and weigh the metals and alloys in the following steps (2) to (4) as raw materials for later use;

[0043] (2) Weigh out 5.0 kg of electrolytic nickel (purity greater than 99.9%), 0.375 kg of molybdenum bar, 1.57 kg of electrolytic cobalt, 0.67 kg of nickel-tungsten alloy, 0.002 kg of pure iron, 0.0008 kg of pure manganese, 0.017 kg of high-purity silicon, 0.0045 kg of pure carbon, 0.039 kg of pure hafnium, and 0.025 kg of pure tantalum, and put them into a vacuum melting furnace in sequence. The melting temperature is 1550 ℃±5℃ and the time is 20 min. The refining conditions are to control the temperature at 1555℃±5℃ under magnetic stirring until all raw materials are melted, and the time is 40 min to obtain molten liquid.

[0044] (3) In step (2), add 0.55 kg aluminum granules, 0.40 kg nickel-titanium alloy, 0.93 kg metallic chromium and 0.52 kg nickel-niobium alloy. The second refining conditions are to control the temperature at 1545℃±5℃ under magnetic stirring until all raw materials are melted, and the time is 40 min to further obtain molten liquid.

[0045] (4) Add 0.012 kg of nickel-cerium alloy, 0.008 kg of nickel-boron alloy, 0.0073 kg of nickel-phosphorus alloy, and 0.0013 kg of sponge zirconium wrapped in nickel foil to step (3). The pouring conditions are to control the temperature at 1475℃±5℃ under magnetic stirring until the steel is tapped, and the time is 10 min to obtain the refined FGH4097 ingot.

[0046] (5) The FGH4097 ingot obtained in step (4) is prepared into FGH4097 powder with a particle size between 0 μm and 250 μm using the plasma rotating electrode method.

[0047] (6) The FGH4097 powder obtained in step (5) is sieved in an inert gas Ar atmosphere, and powder with a particle size between 50 μm and 100 μm is selected and placed in a sleeve. FGH4097 rods are prepared by hot isostatic pressing. At this time, the pressing conditions of hot isostatic pressing are: pressure of 180 MPa, temperature of 1170℃±5℃, holding time of heat and pressure of 4.5 h, and cooling method of air cooling.

[0048] (7) Heat treatment of the FGH4097 bar obtained in step (6); the conditions are to heat to 970℃±5℃, hold for 9h, then cool rapidly to room temperature, continue to heat to 860℃±5℃, hold for 10h, then cool to 660℃±5℃, hold for 34h, and then cool to room temperature in the furnace.

[0049] (8) The FGH4097 rod obtained in step (7) is used to make samples. The sample specifications are φ11.5mm×2.3mm round pieces. A total of 850 pieces are made, each piece is a minimum packaging unit, and the candidate material for the standard sample of thermal diffusivity is obtained.

[0050] (9) The candidate materials obtained in step (8) are evaluated for chemical composition uniformity in accordance with GB / T 15000.3-2023 "Standard Sample Working Guide Part 3: Standard Sample Value Determination and Uniformity and Stability Assessment" to obtain standard sample candidate materials with uniform thermal diffusivity.

[0051] (10-1) The content of each component in the candidate material of the FGH4097 disc-shaped thermal diffusivity standard sample was determined by inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry, spark discharge atomic emission spectrometry, and high-frequency induction combustion-infrared absorption spectrometry to test the uniformity of chemical composition. Fifteen smallest packaging units were selected using stratified random sampling to test the uniformity of chemical composition. The statistical results are shown in Table 1.

[0052] Table 1. Statistical analysis of the chemical composition homogeneity test results of FGH4097

[0053] As shown in the table above, the F statistics of elements such as Al, B, C, Ce, Co, Cr, Fe, Hf, Mn, Mo, Mg, Nb, P, S, Si, Ti, W, and Zr are all less than the critical value of 2.04, indicating that each element is uniformly distributed in the standard sample. In other words, from the perspective of chemical composition, the FGH4097 standard sample has a uniform composition distribution and can be used as a candidate material for the preparation of thermal diffusivity standard samples.

[0054] (10-2) The candidate material for thermal diffusivity standard sample with uniform chemical composition obtained in step (10-1) is subjected to uniformity test, stability test, value determination and assignment by multiple laboratories in accordance with the provisions of GB / T 15000 "Standard Sample Working Guide" and YS / T 409-2012 "Technical Specification for Standard Samples for Analysis of Non-ferrous Metal Products". Finally, the FGH4097 thermal diffusivity standard sample with accurate value is obtained.

[0055] (10-3) The uniformity test in step (10-2) is as follows: 15 samples are randomly selected from the remaining 835 samples using a random number table. The sample is heated from an initial temperature of 25℃ to 1000℃ at a rate of 10℃ / min under a high-purity argon atmosphere. The average thermal diffusivity of the standard sample candidate material is measured at 100℃, 200℃, 300℃, 400℃, 500℃, 600℃, 700℃, 800℃, 900℃, and 1000℃. Each sample is tested three times according to the measurement procedure and sequence specified in GB / T22588-2008 "Measurement of Thermal Diffusivity or Thermal Conductivity by Flash Method". A one-way ANOVA is performed on the average thermal diffusivity of the three measurements. The statistical results are shown in Table 2.

[0056] Table 2. Statistics of uniformity test results for FGH4097 thermal diffusivity standard samples

[0057]

[0058] As shown in Table 2, the F-statistic of the average thermal diffusivity is less than the critical value of 2.04 at all measurement temperatures, indicating that the thermal diffusivity of the FGH4097 standard sample is uniform at all measurement temperatures within the range of 25℃ to 1000℃.

[0059] (10-4) The stability test in step (10-2) is as follows: Long-term stability tests are conducted in months 0, 1, 3, 6, and 12. The test conditions are as follows: two samples are randomly selected from the remaining samples for each time period. The temperature is increased from an initial temperature of 25℃ to 1000℃ at a rate of 10℃ / min. The atmosphere is high-purity argon. The average thermal diffusivity of the standard sample candidate material is measured at 100℃, 200℃, 300℃, 400℃, 500℃, 600℃, 700℃, 800℃, 900℃, and 1000℃. Each sample is tested three times according to the measurement procedure and sequence specified in GB / T22588-2008 "Measurement of Thermal Diffusivity or Thermal Conductivity by Flash Method". A linear regression model analysis is performed on the average thermal diffusivity of the six measurements. The statistical results are shown in Table 3.

[0060] Table 3. Statistics of Stability Test Results for FGH4097 Thermal Diffusion Coefficient Standard Samples

[0061]

[0062] Taking 100℃ as an example, a linear regression model was used to analyze the long-term stability of the FGH4097 thermal diffusivity standard sample at this temperature.

[0063] First, establish a linear model Y = a + bX.

[0064] The true values ​​of intercept a and slope b, b0 and b1, as well as the corresponding standard deviations s(b0) and s(b1), are obtained by using a univariate linear model-linear least squares method.

[0065] The formulas for calculating b0 and b1 are as follows:

[0066] (1)

[0067] (2)

[0068] In the formula:

[0069] x i —The i-th time point;

[0070] y i —The observation value corresponding to the i-th time point;

[0071] —The average value across all time points;

[0072] —The average of all observations.

[0073] The standard deviation s(b1) of b1 is given by the following formula:

[0074] (3)

[0075] In the formula, s is the standard deviation of each point on the straight line, calculated as follows:

[0076] (4)

[0077] The critical value of a two-tailed Student's t-distribution with n-2 degrees of freedom at a 95% confidence probability, if This indicates a significant difference between the slope b1 and 0, suggesting that the characteristic values ​​of the standard sample exhibit a significant changing trend during storage, indicating sample instability. If... If the slope does not change significantly, it can be determined with a 95% confidence probability that the characteristic value of the standard sample does not show a significant trend of change during the storage period, and the sample is stable.

[0078] Calculations show that b1 = -0.0027, s （b1） =0.0011, t 0.95,4 =3.18, therefore we know Therefore, the thermal diffusivity of the FGH4097 standard sample at 100℃ showed good stability over 12 months. Similarly, calculations were performed at other temperature points, and the results are shown in Table 4.

[0079] Table 4. Stability test results of FGH4097 thermal diffusivity standard sample; statistical analysis of linear regression model.

[0080]

[0081] As shown in Table 4, the thermal diffusivity of the FGH4097 standard sample at various temperature points from 25℃ to 1000℃ showed good stability over 12 months.

[0082] (10-5) The multiple laboratory determination values ​​in step (10-2) are as follows: Select 9 laboratories with CNAS qualifications or authority. The test conditions are as follows: randomly select 2 pieces from each laboratory from the remaining samples, heat from the initial temperature of 25℃ to 1000℃ at a heating rate of 10℃ / min, and use high-purity argon gas in the atmosphere. Measure the average thermal diffusivity of the standard sample candidate material at 100℃, 200℃, 300℃, 400℃, 500℃, 600℃, 700℃, 800℃, 900℃, and 1000℃. Each piece is tested twice according to the measurement procedure and measurement sequence specified in GB / T22588-2008 "Measurement of Thermal Diffusivity or Thermal Conductivity by Flash Method". Analyze the determination values ​​from multiple laboratories, remove outliers, and perform normal distribution test and equal precision test. Calculate the average value of the thermal diffusivity and use the average value as the standard value of the FGH4097 thermal diffusivity standard sample.

[0083] (10-6) In accordance with GB / T 15000 "Standard Sample Working Guidelines" and YS / T 409-2012 "Technical Specifications for Standard Samples for Analysis of Non-ferrous Metal Products", the uncertainty introduced by homogeneity, the uncertainty introduced by stability and the uncertainty introduced by the set value are evaluated using reasonable methods. The combined uncertainty and expanded uncertainty of the thermal diffusivity are calculated, and the expanded uncertainty is used as the expanded uncertainty of the FGH4097 thermal diffusivity standard sample.

[0084] After calculation and rounding, the standard values ​​and uncertainties of the thermal diffusivity standard sample of FGH4097 at each temperature range are shown in Table 5.

[0085] Table 5 Standard values ​​and uncertainties of thermal diffusivity of FGH4097 standard sample at various temperatures

[0086]

[0087] This standard sample was prepared using powder metallurgy and hot isostatic pressing (HIP). Based on the uniformity of composition, a standard sample for thermal diffusivity was prepared. The test range was 25℃ to 1000℃, with 100℃, 200℃, 300℃, 400℃, 500℃, 600℃, 700℃, 800℃, 900℃, and 1000℃ selected as test objects. The uniformity and stability of the thermal diffusivity were tested, and values ​​were determined by multiple laboratories. Statistical analysis showed that the thermal diffusivity of this standard sample exhibited good uniformity and stability at all temperature points, with accurate and reliable values. It can be used for quality control of the thermal diffusivity of the FGH4097 sample, providing a basis for improving the accuracy and comparability of test results, filling a market gap, possessing broad market value, and promoting the application and development of aerospace materials.

Claims

1. A method for preparing a standard sample of FGH4097 thermal diffusivity, comprising the following steps: (1) Based on the FGH4097 thermal diffusivity standard sample, the proportions were designed and the following raw materials were selected: electrolytic nickel, nickel foil, metallic chromium, aluminum briquettes, molybdenum bars, pure iron, pure manganese, electrolytic cobalt, nickel-titanium alloy, nickel-cerium alloy, nickel-boron alloy, nickel-niobium alloy, nickel-tungsten alloy, nickel-phosphorus alloy, sponge zirconium, high-purity silicon, pure carbon, pure tantalum, and pure hafnium. (2) Place the electrolytic nickel, molybdenum bar, electrolytic cobalt, nickel-tungsten alloy, pure iron, pure manganese, high-purity silicon, pure carbon, pure hafnium and pure tantalum from step (1) into a vacuum melting furnace in sequence, and control the melting and refining conditions until all raw materials are melted into molten liquid; (3) Add aluminum briquettes, nickel-titanium alloy, metallic chromium, and nickel-niobium alloy to the molten liquid obtained in step (2), and control the second refining conditions until all raw materials are melted to further obtain the molten liquid; (4) Add nickel-cerium alloy, nickel-boron alloy, nickel-phosphorus alloy and sponge zirconium wrapped with nickel foil to the molten liquid obtained in step (3), control the pouring conditions until the steel is tapped, and obtain the refined FGH4097 ingot. (5) The FGH4097 ingot obtained in step (4) is used to prepare FGH4097 powder using the plasma rotating electrode method; (6) The FGH4097 powder obtained in step (5) is sieved in an inert gas Ar atmosphere and placed in a package to prepare FGH4097 rods by hot isostatic pressing. (7) Heat-treat the FGH4097 bar obtained in step (6); (8) Prepare samples of the FGH4097 bars that have undergone heat treatment in step (7) to make candidate materials for standard samples of thermal diffusivity of specified size; (9) The candidate materials obtained in step (8) are evaluated for chemical composition uniformity in accordance with GB / T 15000.3-2023 "Standard Sample Working Guide Part 3: Standard Sample Value Determination and Uniformity and Stability Assessment" to obtain standard sample candidate materials with uniform thermal diffusivity. (10) The candidate material of thermal diffusivity standard sample with uniform chemical composition obtained in step (9) is subjected to uniformity test, stability test, value determination and assignment by multiple laboratories in accordance with the provisions of GB / T 15000 "Standard Sample Working Guide" and YS / T 409-2012 "Technical Specification for Standard Samples for Analysis of Non-ferrous Metal Products", and finally the FGH4097 thermal diffusivity standard sample with accurate value is obtained.

2. The preparation method according to claim 1, characterized in that, In step (1), the standard sample is designed with the following mass percentage distribution: Al 4.90%~5.20%, B 0.010%~0.012%, C 0.04%~0.05%, Ce 0.007%~0.008%, Co 15.5%~16.0%, Cr 9.00%~9.50%, Fe 0.02%~0.03%, Mn 0.008%~0.009%, Mo 3.70%~3.80%, Mg 0.045%~0.050%, Nb 2.50%~2.60%, Hf 0.30%~0.40%, P 0.010%~0.015%, S 0.010%~0.014%, Si 0.16%~0.018%, Ta 0.20%~0.30%, Ti 1.80%~1.90%, W 5.30%~5.50%, Zr 0.011%~0.013%, balance Ni.

3. The preparation method according to claim 1, characterized in that, In step (2), the melting conditions are a temperature controlled at 1480℃~1620℃ for 5 min~60 min; the refining conditions are a temperature controlled at 1530℃~1580℃ for 5 min~60 min under magnetic stirring.

4. The preparation method according to claim 1, characterized in that, In step (3), the second refining conditions are to control the temperature at 1520℃~1570℃ and the time at 5 min~60 min under magnetic stirring.

5. The preparation method according to claim 1, characterized in that, In step (4), the pouring conditions are to control the temperature at 1440℃~1510℃ for 5 min~30 min under magnetic stirring.

6. The preparation method according to claim 1, characterized in that, In step (5), the particle size of the FGH4097 powder is between 0 μm and 250 μm.

7. The preparation method according to claim 1, characterized in that, In step (6), the particle size of the FGH4097 powder obtained by sieving is between 50 μm and 100 μm.

8. The preparation method according to claim 1, characterized in that, In step (7), the heat treatment conditions are solution treatment + air cooling + two-stage aging, that is, heating to 1100℃~1300℃ and holding for 3h-10h, then rapidly cooling to room temperature, continuing to heat to 850℃~1000℃ and holding for 3h~12h, then cooling to 600℃~850℃ and holding for 8h-36h, and then cooling to room temperature with the furnace.

9. The preparation method according to claim 1, characterized in that, In step (8), the specified size of the candidate material for the standard sample of thermal diffusivity is a disc with a diameter of 11.5 mm to 12.3 mm and a thickness of 2.3 mm to 2.8 mm.

10. The preparation method according to claim 1, characterized in that, In step (9), the evaluation of chemical composition uniformity refers to determining the content of each component in the candidate material of the FGH4097 disc-shaped thermal diffusivity standard sample by using inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry, spark discharge atomic emission spectrometry and high-frequency induction combustion-infrared absorption method, and to test the uniformity of chemical composition.

11. The preparation method according to claim 1, characterized in that, In step (10), the conditions for the uniformity test, stability test and multiple laboratory value determination of the thermal diffusivity coefficient are as follows: initial temperature is 25℃, maximum temperature is 1000℃, heating rate is 10℃ / min, and the average thermal diffusivity of the standard sample candidate material is measured at 100℃, 200℃, 300℃, 400℃, 500℃, 600℃, 700℃, 800℃, 900℃ and 1000℃.

12. The preparation method according to claim 1, characterized in that, In step (10), the assignment of values ​​is based on GB / T 15000 "Standard Sample Working Guidelines" and YS / T 409-2012 "Technical Specifications for Standard Samples for Analysis of Non-ferrous Metal Products". Statistical methods are used to analyze the value data of multiple laboratories, outliers are removed, and the average value of the thermal diffusivity is calculated after normality test and equal precision test. The average value is then used as the standard value of the FGH4097 thermal diffusivity standard sample.

13. The preparation method according to claim 1, characterized in that, In step (10), the assignment is based on GB / T 15000 "Standard Sample Working Guidelines" and YS / T 409-2012 "Technical Specifications for Standard Samples for Analysis of Non-ferrous Metal Products". The uncertainty introduced by uniformity, the uncertainty introduced by stability and the uncertainty introduced by the fixed value are evaluated using reasonable methods. The combined uncertainty and expanded uncertainty of the thermal diffusivity are calculated, and the expanded uncertainty is used as the expanded uncertainty of the FGH4097 thermal diffusivity standard sample.

14. An application in which the FGH4097 thermal diffusivity standard sample prepared by the preparation method according to any one of claims 1 to 12 is used in the analysis of the thermal diffusivity of FGH4097 material.

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