CN112525916B - Method for displaying harmful phase of isothermal forging die material for turbine disc - Google Patents
Method for displaying harmful phase of isothermal forging die material for turbine disc Download PDFInfo
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Abstract
The invention discloses a method for displaying a harmful phase of an isothermal forging die material for a turbine disc, which aims to solve the problem that the harmful phase of the isothermal forging die material for the turbine disc can only display a phase boundary and cannot distinguish a phase lining from a matrix by adopting traditional chemical reagent acid etching. The component characteristics of the harmful phase are fully utilized, the nano light-transmitting film is formed through high-precision polishing, heating at a lower temperature and heat preservation processes, so that the harmful phase and the matrix form obviously different phase contrast optical interference effects, and obvious interference color differences are formed, and thus, the harmful phase is clearly distinguished and displayed integrally relative to the matrix. The method can realize high-sensitivity identification, automatic identification and quantitative statistics of the harmful phase in the high-temperature alloy by using an image analyzer, is successfully applied to display and quantitative characterization of the harmful phase of the isothermal forging die material for the turbine disc at present, and can also be used for distinguishing and displaying a precipitated phase and a matrix of other metal materials.
Description
Technical Field
The invention discloses a method for displaying harmful phases of isothermal forging die materials for turbine discs, and belongs to the technical field of high-temperature alloys.
Background
The high-temperature alloy mainly refers to an advanced metal structure material which can be used for a long time in a high-temperature environment with the temperature of more than 600 ℃ and a complex stress environment, and has the comprehensive properties of excellent high-temperature strength, environmental resistance, good fatigue resistance, fracture toughness and the like. High temperature alloys are used in large quantities for the manufacture of hot end components of aircraft engines, known as "the heart of gas turbines". In addition, the high-temperature alloy is also a key material of a gas turbine for ship power and power generation, a carrier rocket engine, a hot end part of an ultra-supercritical power station unit, the chemical field, an isothermal forging die and ocean engineering equipment. The turbine disk is an important core hot end part of an aeroengine, the operating condition of the turbine disk is extremely severe, the turbine disk bears complex thermal and mechanical loads in flight, the stress and the temperature of each part are different, and therefore the turbine disk material is required to have enough mechanical properties, and particularly, the turbine disk material needs to have fatigue and durability as high as possible and good creep resistance in the service temperature range. At present, most of advanced gas turbines adopt powder high-temperature alloy to prepare turbine disc parts, and isothermal forging is not performed on the turbine disc in forming, so that the performance and the service life of isothermal forging die materials become key factors for preparing the turbine disc. The existing turbine disk isothermal forging die material occasionally generates harmful phases such as thick hard and brittle carbide phases in the preparation process, the size can reach dozens of micrometers, the shape also has sharp corners, the shape is equivalent to inclusions in high-temperature alloy, and the performance and the service life of the die are directly influenced. Isothermal forging dies exhibiting detrimental carbide phases have been found to exhibit a reduction in tensile strength at 1100 ℃ of about 50MPa and a 50% reduction in endurance life at 1100 ℃. Therefore, the identification display and quantitative characterization of the harmful phase of the isothermal forging die material for the turbine disk have important significance. In the manufacturing process of the large-size isothermal forging die, because the section is thick and the cooling speed is low, severe macro segregation sometimes occurs, and harmful phases and uneven distribution characteristics are caused. To accurately measure the average content of the harmful phase, a proper magnification factor should be selected, and at least hundreds of fields of view should be measured to obtain good statistics, and an automatic image analyzer is usually adopted. An important limiting factor in using this method is whether highly contrast images of the detrimental phases and the matrix can be obtained to avoid false or missed detections in automatic detection. Therefore, a high-quality single phase in the matrix shows a harmful phase, which is of great significance.
Disclosure of Invention
The invention provides a method for displaying harmful phases of an isothermal forging die nickel-based superalloy material for a turbine disc aiming at overcoming the defects in the prior art, and aims to solve the problem that the harmful phases of the isothermal forging die material for the turbine disc can only display phase boundaries, but phase contrast and a matrix cannot be distinguished. The method can realize high-sensitivity identification, automatic identification and quantitative statistics of the harmful phase in the high-temperature alloy by using an image analyzer, is successfully applied to display and quantitative characterization of the harmful phase of the isothermal forging die material for the turbine disc at present, and can also be used for distinguishing and displaying a precipitated phase and a matrix of other metal materials.
The purpose of the invention is realized by the following technical scheme:
according to the method for displaying the harmful phase of the isothermal forging die nickel-based superalloy material for the turbine disc, firstly, residual stress removal polishing is carried out on a sample of the isothermal forging die material for the turbine disc, then the sample of the isothermal forging die material for the turbine disc is placed into a heating furnace which is preheated to 400-500 ℃, heat preservation is carried out for 15-45min, the sample is taken out and naturally cooled to room temperature, and a light-transmitting film with the thickness of 40-80nm and a matrix of the sample of the isothermal forging die material for the turbine disc are formed on the harmful phase on the surface of the sample of the isothermal forging die material for the turbine disc, so that an optical interference effect which is obviously different is formed.
In practice, the detrimental phases of the isothermal forging die material specimens for turbine disks include coarse hard brittle tungsten-rich carbide phases.
In implementation, the step of polishing the isothermal forging die material sample for the turbine disk by removing residual stress is as follows:
firstly, grinding the metallographic grinding surface of an isothermal forging die material sample for a turbine disc by using 100-200# abrasive paper, and then washing the surface of the sample by using running water;
step two, grinding the metallographic grinding surface of the turbine disc by using 400-1200# abrasive paper from small to large, fully flushing the sample with running water after each abrasive paper is ground, flatly turning the sample by 90 degrees, then grinding the next abrasive paper, and grinding off the scratch of the previous abrasive paper;
step three, selecting navy woolen as polishing fabric to polish the metallographic phase grinding surface of the isothermal forging die material sample for the turbine disc, soaking the polishing fabric by using precipitated and filtered purified water, then covering the polishing disc, setting the rotation speed of the polishing disc to be 200-400 r/min, then selecting grinding paste or spraying suspension liquid with the particle size of polishing grinding material to be 1-3 mu m to polish for 1-3min, and then washing for 0.5-2min by using running water; the step is rough polishing to ensure grinding amount and finish;
step four, setting the rotation speed of the polishing disk to be 200-400 r/min, selecting high-concentration water suspension of medical superfine MgO powder as an abrasive, polishing the metallographic grinding surface of the isothermal forging die material sample for the turbine disk, adding the uniformly stirred abrasive for 3-4 times at intervals of 0.5-1min during polishing, flushing the metallographic grinding surface with running water for 0.5-1min after polishing for 1-3min, and performing fine polishing to ensure that the highest smooth finish and a residual strain-free layer are obtained; and after polishing, wiping the metallographic ground surface of the isothermal forging die material sample for the turbine disc by using a cotton ball soaked with alcohol, and simultaneously blowing the metallographic ground surface to be dry by using a blower to obtain the isothermal forging die material sample for the turbine disc without residual stress.
Further, in the first step, the deformation layer and the burned layer left by the isothermal die material sample for cutting the turbine disk should be ground off.
Further, in the third step, the polishing abrasive with the granularity of 1-3 mu m is artificial diamond grinding paste or Al 2 O 3 Spraying the suspension.
Further, in the fourth step, the proportion of the high-concentration water suspension of the medical superfine MgO powder is 100ml H 2 O+2g MgO。
Furthermore, in the second step, the sequence of the sand paper and the sand is 400#, 800# and 1000# from small to large.
In the implementation, the isothermal forging die material sample for the turbine disk is cut by using a mechanical grinding wheel or a wire cut electrical discharge machine.
In the implementation, the metallographic phase ground surface of the isothermal forging material sample for the wheel disc is upwards put into a heat-resistant ceramic crucible and covered, then the crucible is put into a heating furnace, and the crucible is taken out and the cover is opened when the crucible is cooled.
When metallographic observation is carried out on the isothermal forging die material sample for the turbine disc without residual stress finally obtained under an optical microscope, the harmful phase is observed to be blue in color and is obviously different from a white and bright alloy matrix, so that not only is the contrast difference between the harmful phase and the matrix obtained in a gray image mode, but also the obvious color difference can be obtained in a color mode, and the harmful phase is displayed in a clear single phase. Not only the contrast difference (in the black and white grayscale image mode), but also the color difference (in the color mode). The method can realize high-sensitivity identification and automatic identification of an image analyzer and quantitative statistics of the size and the content of the harmful phase in the high-temperature alloy, and is successfully applied to display and quantitative characterization of the harmful phase of the isothermal forging die material for the turbine disc at present.
The technical scheme of the invention has the characteristics and the technical effects that:
the display of harmful phases in the traditional high-temperature alloy usually adopts metallographic reagents consisting of various mixed acids, displays phase boundaries through chemical action corrosion, outlines the harmful phases, but has no obvious contrast between the interior of the harmful phases and a matrix. Thus, conventional chemical acid etching can only reveal phase boundaries and phase contrast and matrix cannot be distinguished. And if the alkali etching reagent is adopted to display harmful phases, the whole body is dark black, and the contrast with loose defects cannot be distinguished. The method of the technical scheme is based on the phase contrast interference principle, utilizes the chemical composition difference of the harmful phase and the matrix phase, and enables the harmful phase and the alloy matrix to form characteristic nanometer light-transmitting films with different thicknesses through high-precision polishing, lower-temperature heating and heat preservation processes, so that the harmful phase and the alloy matrix form obviously different optical interference effects and obviously different interference chromatic aberration, and the integral clear display of the harmful phase different from the matrix is realized. The method can realize high-sensitivity identification, automatic identification and quantitative statistics of the harmful phase in the high-temperature alloy by using an image analyzer, is successfully applied to display and quantitative characterization of the harmful phase of the isothermal forging die material for the turbine disc at present, and can also be used for distinguishing and displaying a precipitated phase and a matrix of other metal materials.
Compared with an acidic corrosion reagent, the technical scheme of the invention not only can display the outline and the phase boundary, but also can integrally highlight the harmful phase in a single phase to form uniform contrast different from a matrix, and is safe and environment-friendly because no chemical reagent is adopted;
in order to realize the single-phase display of harmful phases, the finish requirement of the metallographic grinding surface of the sample of the isothermal forging die material for the turbine disc is extremely high, so that multi-stage fine grinding and polishing are adopted, and the last stage adopts a little adopted superfine medical MgO suspension liquid, so that a high-finish surface without a residual strain layer is favorably formed, and the phenomenon that the surface of the sample generates dirty false colors and strain marks when the sample is heated and insulated finally due to the existence of the strain layer is prevented;
according to the technical scheme, the nanoscale interference film with the appropriate thickness is formed by appropriate heating and heat preservation on the basis of the high-finish surface, and different optical interference effects and colors can be formed due to the fact that the harmful phase and the substrate have different film thicknesses, so that the harmful phase whole body (non-contour boundary) and the substrate are displayed in a distinguishing mode.
The heating temperature is too low or the heat preservation time is too short, the thickness of the interference film is thin, the color of a harmful phase under an optical metallographic phase deviates from a characteristic color, and a good contrast can not be formed between the harmful phase and a matrix; however, when the substrate is heated at a high temperature for a long time, the formed oxide film is too thick, the light transmittance is insufficient, the thickness capable of forming optical interference is missed, the characteristic color is dark, and proper contrast relative to the substrate cannot be obtained. The proper heating temperature and time obtained by experiments are within the range of 400-500 ℃/15-45min, and the color contrast with uniform and vivid harmful phase and matrix can be obtained.
The technical scheme of the invention has the advantages of simple method and low cost, only needs a common heating furnace, lower heating temperature and shorter heat preservation time, can form a nano interference film with a certain thickness and has an integral uniform blue characteristic, forms a sharp contrast with a white and bright substrate of a matrix alloy, displays and distinguishes harmful phases in a high-quality single phase, and has the advantages of saving subsequent image processing cost by high-quality development of the harmful phases with single striking characteristic color, improving detection efficiency and accuracy and laying a foundation for microscopic observation and high-precision identification and high-efficiency quantitative analysis of an image analyzer.
Detailed Description
The technical solution of the present invention will be further described with reference to the following examples:
example 1
The method for displaying the harmful phase of the isothermal forging die material for the turbine disc by adopting the method comprises the following steps:
(1) Cutting a nickel-based high-temperature alloy sample of the isothermal forging die material for the turbine disc by adopting a mechanical grinding wheel or electrospark wire-electrode cutting;
(2) Grinding a metallographic grinding surface by using No. 200 abrasive paper, grinding a deformation layer and a burn layer left by cutting the sample, and then washing the surface of the sample by using running water;
(3) Grinding the metallographic surface by using 400# abrasive paper, 800# abrasive paper and 1000# abrasive paper in three grades from small to large, fully washing with running water after finishing one abrasive paper, flatly rotating the sample by 90 degrees and then grinding the next abrasive paper;
(4) Selecting admiralty as polishing fabric, soaking the polishing fabric in pure water after precipitation and filtration, covering the polishing fabric on a polishing disc at a rotating speed of 300 r/min, and selecting 3 mu m Al as polishing abrasive 2 O 3 Spraying the suspension, polishing for 2min, and washing with flowing water for 1min;
(5) The rotation speed of the polishing disk is 300 r/min, the grinding material is high-concentration water suspension of medical superfine MgO powder, and the proportion is 100ml H 2 Stirring O +2g of MgO powder uniformly, adding MgO suspension uniformly stirred for 4 times at intervals of 1min during polishing, washing for 0.5min by using running water after polishing for 3min, wiping the polished surface by using a cotton ball soaked with alcohol, and drying by using a blower at the same time to obtain a turbine disc isothermal forging die material sample without a residual strain layer fine polished surface;
(6) And (3) putting the polished sample with the ground surface facing upwards into a heat-resistant ceramic crucible and covering, putting the crucible into a heating furnace which is preheated to 400 ℃ in advance, preserving the heat for 40min, taking out the crucible, naturally cooling to the room temperature, and opening a crucible cover to take out the sample.
(7) The metallographic observation is carried out on the sample under an optical microscope, and harmful phases M can be seen 6 The C carbide is blue in color and different from white alloy matrix, and the harmful phase is displayed in clear single phase. The sample treated by the method can be further applied to high-sensitivity identification, automatic identification and quantitative statistics of harmful phases in the high-temperature alloy by an image analyzer.
Example 2
The method for displaying the harmful phase of the isothermal forging die material for the turbine disc is completed by adopting the method disclosed by the invention as follows:
(1) Cutting a nickel-based high-temperature alloy sample of the isothermal forging die material for the turbine disc by adopting mechanical grinding wheel cutting or electrospark wire-electrode cutting;
(2) Grinding a metallographic grinding surface by using No. 200 abrasive paper, grinding a deformation layer and a burn layer left by cutting a sample, and then washing the surface of the sample by using running water;
(3) Grinding the metallographic surface by using 400# abrasive paper, 800# abrasive paper and 1000# abrasive paper in three grades from small to large, fully washing with running water after finishing one abrasive paper, flatly rotating the sample by 90 degrees and then grinding the next abrasive paper;
(4) Selecting admiralty as a polishing fabric, soaking the polishing fabric in purified water after precipitation and filtration, covering the polishing fabric on a polishing disc at a rotating speed of 300 revolutions per minute, selecting 3-micron artificial diamond grinding paste as a polishing abrasive, polishing for 2min, and then washing for 1min by running water;
(5) The rotation speed of the polishing disk is 300 r/min, the grinding material is high-concentration water suspension of medical superfine MgO powder, and the proportion is 100ml H 2 Stirring O +2g of MgO powder uniformly, adding MgO suspension uniformly stirred for 4 times at intervals of 1min during polishing, washing for 0.5min by using running water after polishing for 3min, wiping the polished surface by using a cotton ball soaked with alcohol, and drying by using a blower at the same time to obtain a turbine disc isothermal forging die material sample without a residual strain layer fine polished surface;
(6) And putting the polished sample with the ground surface facing upwards into a heat-resistant ceramic crucible and covering, putting the crucible into a heating furnace preheated to 470 ℃ in advance, preserving the heat for 20min, taking out the crucible, naturally cooling to room temperature, and opening a crucible cover to take out the sample.
(7) Metallographic observation is carried out on the sample under an optical microscope, and a harmful phase M can be seen 6 The C carbide is blue in color and different from white alloy matrix, and the harmful phase is displayed in clear single phase. The sample treated by the method can be further applied to high-sensitivity identification, automatic identification and quantitative statistics of harmful phases in the high-temperature alloy by an image analyzer.
Example 3
The method for displaying the harmful phase of the isothermal forging die material for the turbine disc is completed by adopting the method disclosed by the invention as follows:
(1) Cutting a nickel-based high-temperature alloy sample of the isothermal forging die material for the turbine disc by adopting mechanical grinding wheel cutting or electrospark wire-electrode cutting;
(2) Grinding a metallographic grinding surface by using No. 200 abrasive paper, grinding a deformation layer and a burn layer left by cutting the sample, and then washing the surface of the sample by using running water;
(3) Grinding the metallographic surface by using 400# abrasive paper, 800# abrasive paper and 1000# abrasive paper in three grades from small to large, fully washing with running water after each abrasive paper is ground, flatly turning the sample by 90 degrees and then grinding the next abrasive paper;
(4) Selecting admiralty as polishing fabric, soaking the polishing fabric in purified water after precipitation and filtration, covering the polishing fabric on a polishing disc at the rotating speed of 300 revolutions per minute, and selecting 3 mu m Al as polishing abrasive 2 O 3 Spraying the suspension, polishing for 2min, and washing with flowing water for 1min;
(5) The rotation speed of the polishing disk is 300 r/min, the grinding material is high-concentration water suspension of medical superfine MgO powder, and the proportion is 100ml H 2 Stirring O +2g of MgO powder uniformly, adding MgO suspension uniformly stirred for 4 times at intervals of 1min during polishing, washing for 0.5min by using running water after polishing for 3min, wiping the polished surface by using a cotton ball soaked with alcohol, and blowing by using a blower at the same time to obtain a turbine disc isothermal forging die material sample without a residual strain layer and a finely polished surface;
(6) And putting the polished sample into a heat-resistant ceramic crucible with the ground surface facing upwards and covering, putting the crucible into a heating furnace preheated to 500 ℃ in advance, preserving the heat for 15min, taking out the crucible, naturally cooling to room temperature, and opening the crucible cover to take out the sample.
(7) Metallographic observation is carried out on the sample under an optical microscope, and a harmful phase M can be seen 6 The C carbide is blue in color and different from white alloy matrix, and the harmful phase is displayed in clear single phase. The sample treated by the method can be further applied to high-sensitivity identification, automatic identification and quantitative statistics of harmful phases in the high-temperature alloy by an image analyzer.
Different temperatures are matched with different heat preservation time combinations, so that longer heat preservation time is needed when the temperature is lower, and the heat preservation time can be shortened when the temperature is relatively higher. The embodiment proves that the above scheme can obtain satisfactory interference colors, thereby effectively displaying harmful phases.
Claims (4)
1. A method for displaying harmful phases of an isothermal forging die material for a turbine disk, wherein the harmful phases of a sample of the isothermal forging die material for the turbine disk comprise thick hard and brittle tungsten-rich carbide phases, and is characterized in that: firstly, polishing a sample of the isothermal forging die material for the turbine disc, then putting the sample of the isothermal forging die material for the turbine disc into a heating furnace which is preheated to 400-500 ℃, preserving heat for 15-45min, taking out the sample and naturally cooling to room temperature, so that a light-transmitting film with the thickness of 40-80nm is formed by a harmful phase on the surface of the sample of the isothermal forging die material for the turbine disc, and an optical interference effect which is obviously different from that of a matrix of the sample of the isothermal forging die material for the turbine disc can be formed under the observation of an optical microscope, thereby realizing the integral clear and uniform display and quantitative analysis of the harmful phase without false color and strain mark which is different from the matrix;
the method for polishing the residual stress of the isothermal forging die material sample for the turbine disc comprises the following steps:
firstly, grinding the metallographic grinding surface of a turbine disc isothermal forging die material sample by using 100-200# abrasive paper, and then washing the surface of the sample by using running water;
step two, grinding the metallographic grinding surface of the turbine disc by using 400-1200# abrasive paper from small to large, fully flushing the sample with running water after each abrasive paper is ground, flatly turning the sample by 90 degrees, then grinding the next abrasive paper, and grinding off the scratch of the previous abrasive paper;
step three, selecting admiralty as polishing fabric to polish the metallographic grinding surface of the isothermal forging die material sample for the turbine disc, soaking the polishing fabric in precipitated and filtered purified water, covering the polishing disc, setting the rotating speed of the polishing disc to be 200-400 r/min, and selecting artificial diamond grinding paste or Al with the granularity of 1-3 mu m as polishing abrasive 2 O 3 Spraying the suspension for 1-3min, and washing with running water for 0.5-2min;
step four, setting the rotation speed of a polishing disc to be 200-400 r/min, selecting a medical superfine MgO powder aqueous suspension as an abrasive, polishing the metallographic ground surface of the isothermal forging die material sample for the turbine disc, adding the abrasive uniformly stirred for 3-4 times at intervals of 0.5-1min during polishing, washing the metallographic ground surface of the isothermal forging die material sample for the turbine disc for 0.5-1min by using running water after polishing for 1-3min, wiping the metallographic ground surface of the isothermal forging die material sample for the turbine disc by using a cotton ball soaked with alcohol after polishing, and simultaneously blowing the metallographic ground surface by using a blower to obtain the isothermal forging die material sample for the turbine disc without residual stress;
the medical superfine MgO powder aqueous suspensionThe mixture ratio of (A) is 100ml H 2 O+2g MgO。
2. The method for indicating harmful phases in isothermal forging die material for turbine disks according to claim 1, wherein: in the first step of residual stress removal polishing, a deformation layer and a burn layer left by an isothermal forging die material sample for cutting a turbine disc should be ground.
3. The method for indicating a harmful phase of an isothermal die forging material for a turbine disk according to claim 1, wherein: in the step two of removing residual stress and polishing, the sequence of sand paper and sand is 400#, 800# and 1000# from small to large.
4. The method for indicating harmful phases in isothermal forging die material for turbine disks according to claim 1, wherein: the isothermal forging die material sample for the turbine disc is cut by a mechanical grinding wheel or an electric spark wire.
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