CN117110128A - Quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy - Google Patents

Quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy Download PDF

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CN117110128A
CN117110128A CN202311380449.0A CN202311380449A CN117110128A CN 117110128 A CN117110128 A CN 117110128A CN 202311380449 A CN202311380449 A CN 202311380449A CN 117110128 A CN117110128 A CN 117110128A
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赵文侠
李刚
王剑
周静怡
张佩佩
刘昌奎
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AECC Beijing Institute of Aeronautical Materials
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Abstract

The application provides a quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy, which comprises the following steps: mass M to be pretreated 1 The alloy sample of (2) is put into 1% citric acid-1% ammonium sulfate aqueous solution for electrolysis, and after the electrolysis is finished, the alloy sample is washed and dried to constant weight, and is marked as M 2 The method comprises the steps of carrying out a first treatment on the surface of the Soaking the obtained sample in 5-20% hydrochloric acid aqueous solution, performing ultrasonic treatment, cleaning, drying to constant weight, and marking as M 3 The method comprises the steps of carrying out a first treatment on the surface of the Filtering the ultrasonic hydrochloric acid aqueous solution to obtain filtrate and a filter membrane with residues; the filter membrane with the residue was dried to constant weight and designated M 4 The mass of the residue was designated M 5 ，M 5 =M 4 -filter membrane mass; gamma' -phase mass ratio)=X 100. The method can obtain the mass ratio of the strengthening phase gamma' -in the alloy, and fills the blank of the alloy microstructure characterization technology in the aspect of three-dimensional quantitative distribution.

Description

Quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy
Technical Field
The application belongs to the technical field of quantitative tests, and particularly relates to a quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy.
Background
The development of aeroengines with higher service temperature requirements continues to require the use of nickel-based, cobalt-based and iron-based superalloys as structural materials. The microstructure of superalloys has been widely studied and information about their microstructure and properties can be found in many papers. Briefly, superalloys are characterized by a face centered cubic (fcc) austenitic matrix (γ) that is precipitation hardened by solid solution strengthening and carbide and Geometrically Close Packed (GCP) phases such as the γ' phase.
In the new generation of high pressure turbine disk materials for aeroengines represented by nickel-based powder superalloy, the preparation process is complex due to high self alloying degree, and the requirement on the content control precision of the second phase in the material is high, especially the gamma' -phase playing a main strengthening role, for example: the technical requirement of the first generation of nickel-based powder superalloy Ren 95 in the United states is that the mass fraction of gamma ' -phase is 50%, the mass fraction of gamma ' -phase of the second generation of nickel-based powder superalloy Ren 88DT with damage tolerance is 37%, and the mass fraction of gamma ' -phase of the third generation of nickel-based powder superalloy Ren 104 is 51%. The requirements of the powder superalloy of the soviet union on the gamma '-phase are consistent with the requirements of the United states and Europe on the gamma' -phase, the gamma '-phase mass ratio of the first-generation nickel-based powder superalloy EP962P is 50 percent, and the gamma' -phase mass ratio of the second-generation nickel-based powder superalloy EP741NP is 60 percent.
In the reported file data, the gamma-phase in the alloy is regulated and controlled by adopting the mass percentage, the conventional quantitative metallographic method based on the principle of stereology can only obtain the area percentage of the second phase in the two-dimensional plane, and then the method is based on the stereologyGeneral rule A A = V V Under the condition that the second phase in the material is uniformly distributed, the volume ratio (volume percent) of the second phase in the material can be equivalent to the calculation of the area ratio of the second phase content in the two-dimensional plane image, but the mass percent of the second phase cannot be obtained, and the ratio of chemical elements in each phase cannot be accurately obtained, so that the development and application of the alloy, particularly the nickel-based powder superalloy with higher alloying degree, are not hindered.
Disclosure of Invention
In view of the above, the present application aims to provide a quantitative test method for the mass fraction of gamma '-phase in nickel-based powder superalloy, which can obtain the mass ratio of the strengthening phase gamma' -phase in the nickel-based powder superalloy in the alloy, and fill the blank of the microstructure characterization technology of the alloy in terms of three-dimensional quantitative distribution.
The electrochemical extraction phase is utilized to make the alloy matrix be in an activated or over-passivated state to be dissolved by utilizing the difference of different polarization characteristics-stable potential or anode passivation behaviors in the alloy. The extracted phase is at a potential below its steady-state potential or, although the potential exceeds its steady-state potential, enters an anodic passivation state without being ionized.
FIG. 1 is a schematic view of an electrolytic device used in the present application, wherein 1 is a beaker with a volume of 700mL;2 is a cathode cylinder, 3 is a container, and 4 is an alloy sample; 5 is a circulating cooling component, 6 is a platinum wire-cathode, 7 is a pipe plug, 8 is a pipe plug, 9 is electrolyte, 10 is a pipe plug, 11 is a platinum wire-anode, and 12 is a reference electrode; the present application performs electrolysis in the electrolysis apparatus shown in fig. 1.
The application provides a quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy, which comprises the following steps:
1) Mass M to be pretreated 1 Placing a nickel-based powder superalloy sample in a 1% citric acid-1% ammonium sulfate aqueous solution for electrolysis, wherein the current density of electrolysis is 0.02-0.03A/cm 2 The time is 2-4 hours, the alloy sample is cleaned after the electrolysis is finished, and the alloy sample is dried to constant weight and is marked as M 2 ；
2) Step 1) The obtained sample is continuously soaked in 5-20vol% hydrochloric acid aqueous solution, ultrasonic treatment is carried out until no particles are attached to the surface of the sample, deionized water and ethanol are adopted for cleaning, drying is carried out until the weight is constant, and the sample is marked as M 3 ；
3) Filtering the hydrochloric acid aqueous solution after ultrasonic treatment in the step 2) to obtain filtrate and a filter membrane with residues; the filter membrane with the residue was dried to constant weight and designated M 4 The mass of the residue was designated M 5 ，M 5 = M 4 -filter membrane mass;
the gamma' -phase mass ratio is calculated using the following formula:
gamma' -phase mass ratio) = />× 100。
In the application, the percentages of the 1% citric acid-1% ammonium sulfate aqueous solution, the 5-20% hydrochloric acid aqueous solution, the 10% hydrochloric acid-methanol electrolyte and the 0.5% citric acid solution are all represented by volume percent. The M is 1 、M 2 、M 3 、M 4 And M 5 Is in g.
In order to remove residues on the surface of an alloy sample, such as grease, adsorbed dust and the like, the application preferably needs to electrolyze 10% hydrochloric acid-methanol reagent at a lower (-5 to-10 ℃) temperature before gamma' -phase electrolytic extraction, so as to ensure accurate measurement in the subsequent test process.
Specifically, the mass M 1 The pretreatment of the nickel-based powder superalloy sample specifically comprises:
electrolyzing the alloy sample in 10% hydrochloric acid-methanol electrolyte for 14-16 min at-5 to-10deg.C with current density of 0.1A/cm 2 Cleaning, drying and weighing to obtain pretreated mass M 1 Is a sample of the alloy.
In a specific embodiment, the time of pretreatment electrolysis is 15min; the electrolysis temperature is-10 ℃; the current density was 0.1A/cm 2 。
The surface of the pretreated alloy sample is silver and bright, smooth and free of abnormal bulges. The application adopts an analytical balance to carry out constant weight weighing on the alloy sample.
In the specific embodiment of the application, the nickel-based powder superalloy uses second phase precipitation hardening as a metal material of a main strengthening mechanism, and the second phase generated in the nickel-based powder superalloy, such as gamma' -phase, carbide phase, boride phase and the like, can be used for strengthening the performance of the alloy material, especially the high-temperature performance, to play a positive effect.
Mass M to be pretreated in the application 1 Placing the nickel-based powder superalloy sample in 1% citric acid-1% ammonium sulfate aqueous solution for electrolysis; the application utilizes ammonium sulfate-citric acid aqueous solution to quantitatively extract gamma ' -phase in nickel-based powder superalloy, in the electrolytic process, matrix phase gamma is completely dissolved in electrolyte, but because of anodic protection effect, gamma ' -phase and trace phases (carbide, boride and the like) in the alloy are firmly adsorbed on the surface of a sample, based on chemical separation technology, hydrochloric acid with a certain concentration is adopted to heat and ultrasonically oscillate, a second phase (the general name of separating out matrix phase gamma in the alloy) adsorbed on the surface of the sample is completely separated from the hydrochloric acid solution, and according to the characteristic that gamma ' -phase is dissolved in reducing acid, gamma ' -phase is separated from other trace phases, and the mass ratio of gamma ' -phase in the alloy is obtained by a weightlessness method.
FIG. 2 is a graph of residual morphology of an alloy sample after different treatment methods; wherein (a) and (b) are residual morphology after ultrasonic vibration treatment, and (c) and (d) are residual morphology after ox horn knife scraping treatment. Fig. 2 illustrates that the physical separation method is not applicable under anodic protection, but only chemical separation is adopted so that the second phase adhered to the surface of the sample due to anodic protection is sufficiently detached.
The target phase is kept on the anode as insoluble precipitate through ionization, in the multiphase ionization extraction process, the most common and difficult to treat condition is pollution of matrix gamma phase, the gamma' -phase and the matrix gamma phase in the nickel-based superalloy are very close to each other in chemical property and electrochemical property, although factors influencing polarization characteristics can be regulated by adjusting electrolyte components, current density and the like, in the oxygen-containing acid electrolyte, when the conditions are satisfied＜E＜/>Time (+)>For matrix gamma phase overpassivation potential, +.>The gamma '-phase is subjected to passivation potential), the gamma' -phase can be quantitatively extracted, but the pollution of the gamma-phase of the matrix can be introduced due to the fact that the current density is too high or too low. When meeting->＜E＜/>（/>Is the stable potential of matrix gamma phase, +.>Is the stable potential of the second phase), the matrix is activated to dissolve, and the second phase remains in the precipitate. Three factors affecting the electrolytic extraction process: electrolysis temperature, current density and electrolysis time, in order to find the optimal electrolysis conditions, the application designs orthogonal experiments or adopts a preferred method, and the optimal experimental result is obtained by using the minimum experiment times. And verifying whether the electrolysis parameter selection is accurately determined according to the polarization curve of each phase, firstly determining the polarization characteristics of each phase in the alloy in the electrolyte before the test, finding out the proper dissolution potential range, and carrying out constant current electrolysis in the potential range. The application utilizes a constant current method to obtain linear polarization curves of a nickel-based powder superalloy matrix phase and a second phase in a specific electrolyte, obtains optimal current density based on the yield of a target phase, and under the condition, the dissolution rate of the matrix phase is highest, and the target phase is in a passivation protection state. In the application, the current density of electrolysis is 0.02-0.03A/cm 2 For 2h4h; the temperature of electrolysis is 10-25 ℃; in a specific embodiment, the electrolytic current density is 0.02A/cm 2 Or 0.03A/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The electrolysis time was 4h or 2 hours. FIG. 3 is a surface appearance of an alloy sample after electrolysis.
After the electrolysis is completed, the alloy sample is cleaned, dried to constant weight and marked as M 2 . The application preferably adopts 0.5 percent citric acid solution to clean three times after the electrolysis is finished, and distilled water is used for cleaning three alloy samples.
The method comprises the steps of continuously soaking the sample obtained in the step 1) in 5-20% hydrochloric acid aqueous solution, carrying out ultrasonic treatment until no particles adhere to the surface of the sample, cleaning by adopting deionized water and ethanol, and drying to constant weight.
The soaking temperature is 60-80 ℃, and the soaking time is 10-15 min; the method is characterized in that the method is immersed in a hot hydrochloric acid solution in an ultrasonic mode, the ultrasonic wave is changed from gray black to silver bright color until the surface of a sample is changed from gray black, the condition of the surface of the sample recovered to pretreatment is visually checked to be that the removal of particles attached to the surface is finished, and the surface topography of a sample after hydrochloric acid treatment and cleaning is shown in fig. 4, and fig. 4 is a graph of the surface topography of the sample.
The application adopts deionized water and ethanol to clean the alloy sample after hydrochloric acid aqueous solution treatment, carries out low-temperature air drying, and carries out constant weight weighing, and is marked as M 3 。
The application pumps and filters the hydrochloric acid aqueous solution after ultrasonic treatment to obtain filtrate and a filter membrane with residues; the filter membrane with the residue was dried to constant weight and designated M 4 The mass of the residue was designated M 5 ，M 5 = M 4 -filter membrane mass.
The gamma' -phase mass ratio is calculated by adopting the following formula:
gamma' -phase mass ratio) = />× 100。
The application adopts XRD to analyze the collected residues; XRD analysis conditions were: cu target, accelerating voltage 40kv, tube voltage 40mA, scanning step length 0.02 DEG, 2 theta scanning range 20-120 deg. The alloy is nickel-based powder superalloy; the measured nickel-based powder superalloy contains 35.1-37.1wt% of gamma' -phase.
The application preferably filters the ultrasonic hydrochloric acid aqueous solution, the obtained filtrate is transferred into a 100mL volumetric flask, and the mass fraction or mass concentration of the elements of aluminum, cobalt, chromium, iron, molybdenum, niobium, titanium, tungsten, zirconium and nickel are obtained by utilizing ICP chemical analysis means according to the content range of the elements of aluminum, cobalt, chromium, tungsten, zirconium and nickel in the sample.
FIG. 5 is a schematic diagram of a flow chart of analysis of gamma prime phase mass fraction and elemental composition in accordance with certain embodiments of the present application; the method specifically comprises the following steps: after sample preparation, 10% HCl-CH was used 3 OH surface cleaning, deionized water cleaning for 5min, constant weight, and M 1 The method comprises the steps of carrying out a first treatment on the surface of the By 1% (NH) 4 ） 2 SO 4 -1%C 6 H 8 O 7 Deionized water electrolysis, deionized water washing for 5min, vacuum drying, constant weight, designated as M 2 The method comprises the steps of carrying out a first treatment on the surface of the Placing the sample in 100mL of 5-20% HCl aqueous solution at 60-80 ℃ and carrying out ultrasonic vibration to obtain an ultrasonic hydrochloric acid aqueous solution and an ultrasonic sample, carrying out vacuum drying on the ultrasonic sample, and marking the ultrasonic sample as M 3 The method comprises the steps of carrying out a first treatment on the surface of the Performing vacuum suction filtration on the hydrochloric acid aqueous solution after ultrasonic treatment, and performing ICP chemical element analysis on filtrate; vacuum drying the filter membrane residue after vacuum filtration, and marking as M 4 The mass of the residue was designated M 5 ，M 5 = M 4 -filter membrane mass; XRD analysis of the residue was performed.
The application provides a quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy, which comprises the following steps: 1) Mass M to be pretreated 1 Placing a nickel-based powder superalloy sample in a 1% citric acid-1% ammonium sulfate aqueous solution for electrolysis, wherein the current density of electrolysis is 0.02-0.03A/cm 2 The time is 2-4 hours, the alloy sample is cleaned after the electrolysis is finished, and the alloy sample is dried to constant weight and is marked as M 2 The method comprises the steps of carrying out a first treatment on the surface of the 2) Continuously soaking the sample obtained in the step 1) in 5-20vol% hydrochloric acid aqueous solution, performing ultrasonic treatment until no particles adhere to the surface of the sample, cleaning with deionized water and ethanol, drying to constant weight, and marking as M 3 The method comprises the steps of carrying out a first treatment on the surface of the 3) Filtering the hydrochloric acid aqueous solution after ultrasonic treatment in the step 2) to obtain filtrate and a filter membrane with residues; will carry residuesThe filter was dried to constant weight and designated M 4 The mass of the residue was designated M 5 ，M 5 = M 4 -filter membrane mass; the gamma' -phase mass ratio is calculated using the following formula: gamma' -phase mass ratio) = X 100. The method can obtain the mass ratio of the strengthening phase gamma' -in the nickel-based powder superalloy in the alloy, and fills the blank of the alloy microstructure characterization technology in the aspect of three-dimensional quantitative distribution.
Drawings
FIG. 1 is a schematic view of an electrolytic device employed in the present application;
FIG. 2 is a graph of residual morphology of an alloy sample after different treatment methods;
FIG. 3 is a surface appearance of an alloy coupon after electrolysis;
FIG. 4 is a graph showing the surface morphology of a sample after hydrochloric acid treatment and cleaning;
fig. 5 is a schematic diagram of a flow chart of analysis of gamma prime phase mass ratio and elemental composition according to some embodiments of the application.
Detailed Description
In order to further illustrate the present application, the following examples are provided to describe in detail a quantitative measurement method for the gamma prime phase mass fraction in a nickel-based powder superalloy, which is not to be construed as limiting the scope of the present application.
Example 1
1. Pretreatment of
Electrolyzing the alloy sample with electrolyte A (10% hydrochloric acid-methanol) for 15min, controlling the pretreatment temperature at-10deg.C, adjusting the voltage, and controlling the current density at 0.1A/cm 2 . Taking out, cleaning, drying, visually inspecting sample to obtain silver bright color, smooth and free of abnormal protrusions, weighing with analytical balance, and marking the mass as M 1 ；
2. Electrolysis
Adding a certain amount of electrolyte B (1% citric acid-1% ammonium sulfate aqueous solution) and a cathode into an electrolytic tankThe cartridge was placed in an electrolysis beaker and a standard sample was suspended as an anode in the center of the cathode cartridge with a platinum wire and immersed to a depth of about 60mm. The power switch is turned on, and the voltage is adjusted to control the current density to be 0.025A/cm 2 . The electrolysis time is controlled at 3 h according to the actual situation. After the electrolytic extraction, the surface morphology of the sample is shown in figure 3;
3. cleaning
After the electrolysis is finished, taking out the anode test bar, cleaning the anode test bar in 0.5% citric acid solution for three times, and after cleaning the anode test bar in distilled water for three times, drying the anode test bar in vacuum at low temperature, weighing the anode test bar at constant weight, and marking the mass as M 2 ；
4. Separation
Soaking in 100mL of 20% hydrochloric acid aqueous solution (60 ℃) for 15min. Directly carrying out ultrasonic treatment on the hot hydrochloric acid solution and the test bar until the surface of the sample is changed from gray black to silver bright color, taking out the test bar, and visually checking that the surface of the sample is recovered to a state when the pretreatment is finished, namely, the removal of the particles attached to the surface is finished (see figure 4);
5. weighing
After replacing another clean beaker and washing the test bar with deionized water for several times, washing the test bar with absolute ethyl alcohol, drying by low-temperature blowing, weighing again with constant weight, and recording the mass as M 3 。
6. Suction filtration
Placing the cleaned hydrochloric acid solution in a vacuum filtration device, selecting polytetrafluoroethylene filter membranes with diameters of 45mm and phi 0.1 mu m as the filtration device, and transferring the filtered solution into a 100mL volumetric flask. Drying the filter membrane residues at low temperature under vacuum, weighing at constant weight, and marking the mass as M 4 The mass of the collected residues is M 5 = M 4 -filter membrane mass;
XRD analysis
Placing the collected residues in an X-ray diffractometer, selecting a Cu target, and testing the conditions: the accelerating voltage is 40kv, the tube voltage current is 40mA, the scanning step length is 0.02 DEG, and the 2 theta scanning range is 20-120 deg.
8. Result calculation
Gamma' -phase mass ratio) = />× 100。
TABLE 1 gamma prime phase mass fraction in Nickel-based powder superalloys in example 1
Example 1 M 1 (g) M 2 (g) M 3 (g) M 4 (g) Filter membrane quality (g) M 5 (g) Gamma prime phase mass ratio (wt%)
Group 1 37.6417 37.5475 37.4907 0.0021 0.0006 0.0015 36.62
Group 2 37.2173 37.1244 37.0705 0.0024 0.0006 0.0018 35.49
Group 3 36.6486 36.5576 36.5036 0.0028 0.0006 0.0022 35.72
Group 4 36.0571 35.9627 35.9075 0.0023 0.0006 0.0017 35.76
Example 2
1. Pretreatment of
Electrolyzing the alloy sample with electrolyte A (10% hydrochloric acid-methanol) for 15min, controlling the pretreatment temperature at-10deg.C, adjusting the voltage, and controlling the current density at 0.1A/cm 2 . Taking out, cleaning, drying, visually inspecting sample to obtain silver bright color, smooth and free of abnormal protrusions, weighing with analytical balance, and marking the mass as M 1 ；
2. Electrolysis
Adding a certain amount of electrolyte B (1% citric acid-1% ammonium sulfate aqueous solution) into an electrolytic tank, placing a cathode barrel into an electrolytic beaker,the standard sample was suspended as an anode in the center of the cathode tube with a platinum wire and immersed to a depth of about 60mm. The power switch is turned on, and the voltage is adjusted to control the current density to be 0.02A/cm 2 . The electrolysis time is controlled to be 4h according to the actual situation. After the electrolytic extraction, the surface morphology of the sample is shown in figure 3;
3. cleaning
After the electrolysis is finished, taking out the anode test bar, cleaning the anode test bar in 0.5% citric acid solution for three times, and after cleaning the anode test bar in distilled water for three times, drying the anode test bar in vacuum at low temperature, weighing the anode test bar at constant weight, and marking the mass as M 2 ；
4. Separation
Soaking in 100mL of 20% hydrochloric acid aqueous solution (60 ℃) for 15min. Directly carrying out ultrasonic treatment on the hot hydrochloric acid solution and the test bar until the surface of the sample is changed from gray black to silver bright color, taking out the test bar, and visually checking that the surface of the sample is recovered to a state when the pretreatment is finished, namely, the removal of the particles attached to the surface is finished (see figure 4);
5. weighing
After replacing another clean beaker and washing the test bar with deionized water for several times, washing the test bar with absolute ethyl alcohol, drying by low-temperature blowing, weighing again with constant weight, and recording the mass as M 3 。
6. Suction filtration
Placing the cleaned hydrochloric acid solution in a vacuum filtration device, selecting polytetrafluoroethylene filter membranes with diameters of 45mm and phi 0.1 mu m as the filtration device, and transferring the filtered solution into a 100mL volumetric flask. Drying the filter membrane residues at low temperature under vacuum, weighing at constant weight, and marking the mass as M 4 The mass of the collected residues is M 5 = M 4 -filter membrane mass;
XRD analysis
Placing the collected residues in an X-ray diffractometer, selecting a Cu target, and testing the conditions: the accelerating voltage is 40kv, the tube voltage current is 40mA, the scanning step length is 0.02 DEG, and the 2 theta scanning range is 20-120 deg.
8. Result calculation
Gamma' -phase mass ratio) = />× 100。
TABLE 2 gamma prime phase Mass ratio in Nickel-based powder superalloys in example 2
Example 2 M 1 (g) M 2 (g) M 3 (g) M 4 (g) Filter membrane quality (g) M 5 (g) Gamma prime phase mass ratio (wt%)
Group 1 35.5946 35.5011 35.4442 0.0018 0.0006 0.0012 37.03
Group 2 36.3227 36.2292 36.1723 0.0021 0.0006 0.0015 36.84
Group 3 35.7424 35.6474 35.5906 0.0024 0.0006 0.0018 36.23
Group 4 35.1653 35.0711 35.0142 0.0029 0.0006 0.0023 36.14
Example 3
1. Pretreatment of
Electrolyzing the alloy sample with electrolyte A (10% hydrochloric acid-methanol) for 15min, controlling the pretreatment temperature at-5deg.C, adjusting the voltage, and controlling the current density at 0.1A/cm 2 . Taking out, cleaning, drying, visually inspecting sample to obtain silver bright color, smooth and free of abnormal protrusions, weighing with analytical balance, and marking the mass as M 1 ；
2. Electrolysis
Adding a certain amount of electrolyte B (1% citric acid-1% ammonium sulfate aqueous solution) into an electrolytic tank, placing a cathode barrel into an electrolytic beaker, and hanging a standard sample as an anode by using a platinum wireThe immersion depth was about 60mm in the center of the cathode tube. The power switch is turned on, and the voltage is adjusted to control the current density to be 0.03A/cm 2 . The electrolysis time was controlled at 2h according to the actual conditions. After the electrolytic extraction, the surface morphology of the sample is shown in figure 3;
3. cleaning
After the electrolysis is finished, taking out the anode test bar, cleaning the anode test bar in 0.5% citric acid solution for three times, and after cleaning the anode test bar in distilled water for three times, drying the anode test bar in vacuum at low temperature, weighing the anode test bar at constant weight, and marking the mass as M 2 ；
4. Separation
Soaking in 100mL of 20% hydrochloric acid aqueous solution (60 ℃) for 15min. Directly carrying out ultrasonic treatment on the hot hydrochloric acid solution and the test bar until the surface of the sample is changed from gray black to silver bright color, taking out the test bar, and visually checking that the surface of the sample is recovered to a state when the pretreatment is finished, namely, the removal of the particles attached to the surface is finished (see figure 4);
5. weighing
After replacing another clean beaker and washing the test bar with deionized water for several times, washing the test bar with absolute ethyl alcohol, drying by low-temperature blowing, weighing again with constant weight, and recording the mass as M 3 。
6. Suction filtration
Placing the cleaned hydrochloric acid solution in a vacuum filtration device, selecting polytetrafluoroethylene filter membranes with diameters of 45mm and phi 0.1 mu m as the filtration device, and transferring the filtered solution into a 100mL volumetric flask. Drying the filter membrane residues at low temperature under vacuum, weighing at constant weight, and marking the mass as M 4 The mass of the collected residues is M 5 = M 4 -filter membrane mass;
XRD analysis
Placing the collected residues in an X-ray diffractometer, selecting a Cu target, and testing the conditions: the accelerating voltage is 40kv, the tube voltage current is 40mA, the scanning step length is 0.02 DEG, and the 2 theta scanning range is 20-120 deg.
8. Result calculation
Gamma' -phase mass ratio) = />× 100。
TABLE 3 gamma prime phase mass fraction in Nickel-based powder superalloys in example 3
Example 3 M 1 (g) M 2 (g) M 3 (g) M 4 (g) Filter membrane quality (g) M 5 (g) Gamma prime phase mass ratio (wt%)
Group 1 34.5635 34.4700 34.4148 0.0022 0.0006 0.0016 36.05
Group 2 31.0436 30.9504 30.8964 0.0029 0.0006 0.0023 35.12
Group 3 37.4678 37.3746 37.3178 0.0027 0.0006 0.0021 36.47
Group 4 34.0678 33.9748 33.9180 0.0024 0.0006 0.0018 36.72
As can be seen from the above examples, the present application provides a quantitative test method for gamma-prime phase mass fraction in nickel-based powder superalloy, comprising the following steps: 1) Mass M to be pretreated 1 The nickel-based powder superalloy sample is put into 1vol% citric acid-1 vol% ammonium sulfate aqueous solution for electrolysis, and the current density of electrolysis is 0.02-0.03A/cm 2 The time is 2-4 hours, the alloy sample is cleaned after the electrolysis is finished, and the alloy sample is dried to constant weight and is marked as M 2 The method comprises the steps of carrying out a first treatment on the surface of the 2) Continuously soaking the sample obtained in the step 1) in 5-20vol% hydrochloric acid aqueous solution, performing ultrasonic treatment until no particles adhere to the surface of the sample, cleaning with deionized water and ethanol, drying to constant weight, and marking as M 3 The method comprises the steps of carrying out a first treatment on the surface of the 3) Filtering the hydrochloric acid aqueous solution after ultrasonic treatment in the step 2) to obtain filtrateAnd a filter membrane with residue; the filter membrane with the residue was dried to constant weight and designated M 4 The mass of the residue was designated M 5 ，M 5 = M 4 -filter membrane mass; the gamma' -phase mass ratio is calculated using the following formula: gamma' -phase mass ratio) = />X 100. The method can obtain the mass ratio of the strengthening phase gamma' -in the nickel-based powder superalloy in the alloy, and fills the blank of the alloy microstructure characterization technology in the aspect of three-dimensional quantitative distribution. The method is not only applied to nickel-based powder superalloy, but also can be applied to quantitative extraction and analysis of precipitated phases in other types of alloys.
The foregoing is merely a preferred embodiment of the present application and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present application, which are intended to be comprehended within the scope of the present application.

Claims (7)

1. A quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy comprises the following steps:
1) Mass M to be pretreated 1 The nickel-based powder superalloy sample is put into 1vol% citric acid-1 vol% ammonium sulfate aqueous solution for electrolysis, and the current density of electrolysis is 0.02-0.03A/cm 2 The time is 2-4 hours, the alloy sample is cleaned after the electrolysis is finished, and the alloy sample is dried to constant weight and is marked as M 2 ；
2) Continuously soaking the sample obtained in the step 1) in 5-20vol% hydrochloric acid aqueous solution, performing ultrasonic treatment until no particles adhere to the surface of the sample, cleaning with deionized water and ethanol, drying to constant weight, and marking as M 3 ；
3) Filtering the hydrochloric acid aqueous solution after ultrasonic treatment in the step 2) to obtain filtrate and a filter membrane with residues; the filter membrane with the residue was dried to constant weight and designated M 4 The mass of the residue was designated M 5 ，M 5 = M 4 -filteringFilm quality;
the gamma' -phase mass ratio is calculated using the following formula:
gamma' -phase mass ratio) = />× 100。
2. The quantitative test method according to claim 1, wherein the mass M 1 The pretreatment of the nickel-based powder superalloy sample specifically comprises:
electrolyzing the nickel-based powder superalloy sample in 10% hydrochloric acid-methanol electrolyte for 14-16 min at-5 to-10 ℃ with the electrolytic current density of 0.1A/cm 2 Cleaning, drying and weighing to obtain pretreated mass M 1 Nickel-based powder superalloy samples of (a).
3. The quantitative test method according to claim 1, wherein the soaking temperature in the step 2) is 60-80 ℃ and the soaking time is 10-15 min.
4. The quantitative test method according to claim 1, wherein the suction filtration in the step 3) is performed by using a polytetrafluoroethylene filter membrane having a membrane diameter of 45mm and a pore size of 0.1. Mu.m.
5. The quantitative test method according to claim 1, wherein the step 1) is performed by washing three times with a 0.5vol% citric acid solution after the completion of the electrolysis, and washing three times with distilled water.
6. The quantitative test method according to claim 1, wherein the nickel-based powder superalloy comprises 35.1-37.1 wt% of strengthening phase γ'.
7. The quantitative test method according to claim 1, wherein the residue in step 3) is analyzed by XRD;
XRD analysis conditions were: cu target, accelerating voltage 40kV, tube voltage 40mA, scanning step length 0.02 DEG, 2 theta scanning range 20-120 deg.
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