CN110487788B - Method for evaluating small-angle grain boundary forming tendency of single crystal superalloy - Google Patents
Method for evaluating small-angle grain boundary forming tendency of single crystal superalloy Download PDFInfo
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Abstract
The invention relates to the technical field of investment casting, in particular to a method for evaluating the forming tendency of a small-angle grain boundary of a single-crystal high-temperature alloy. The evaluation method comprises the following specific steps: (1) designing variable cross-section moulds with different platform lengths and constant heights, combining ceramic materials and wax, and manufacturing corresponding mould shells; (2) preparing single crystal high temperature alloy castings of various alloys in a directional solidification furnace; (3) carrying out crystal orientation test on the single crystal high temperature alloys with different sections; (4) and analyzing the angle difference of the small-angle grain boundary in each cross section, and quantitatively evaluating the small-angle grain boundary forming capability of the single crystal high-temperature alloy. The larger the difference in angle between grain boundaries, the stronger the tendency of the alloy to form small angle grain boundaries. Therefore, on the premise of not using a simulation technology, the forming capability of the small-angle grain boundary of different single crystal high-temperature alloys can be quantitatively represented.
Description
The technical field is as follows:
the invention relates to the technical field of investment casting, in particular to a method for evaluating the forming tendency of a small-angle grain boundary of a single-crystal high-temperature alloy.
Background art:
the single crystal high temperature alloy is an indispensable key structural material for aviation, aerospace, energy, nuclear industry, petrifaction, national defense weaponry and national economic construction. As the efficiency of the engine is increasingly improved, higher requirements are put on the structure of the single crystal blade, and as the structure of the single crystal high-temperature alloy part is extremely complex, multiple times of deflection and meeting of dendrites are involved in the directional solidification process, so that a small-angle grain boundary is formed. The small-angle crystal boundary is used as a defect structure, the transverse crystal boundary is introduced again, the structural integrity of the single crystal high-temperature alloy blade is damaged, the high-temperature mechanical property of the alloy is obviously reduced, and the high-temperature mechanical property becomes a great hidden danger in the service process of the blade. The forming tendency of the small-angle grain boundary of the single crystal superalloy becomes a common problem in the research and development process of the single crystal superalloy, so that the forming tendency of the small-angle grain boundary of the single crystal superalloy needs to be evaluated in the processes of research and development of the single crystal superalloy, selection of materials of components, structural design of the components, arrangement of a casting head in the preparation process of the components, a seeding process and the like, and the improvement of the yield and the reduction of the production cost are facilitated.
The invention content is as follows:
the invention aims to provide a method for evaluating the forming tendency of the small-angle grain boundary of the single-crystal high-temperature alloy, which solves the problem that the forming tendency of the small-angle grain boundary of the single-crystal high-temperature alloy is difficult to evaluate.
The technical scheme of the invention is as follows:
the utility model provides an evaluation method of single crystal superalloy small angle grain boundary forming tendentiousness, according to directional solidification's classic theory, dendritic crystal can take place to deflect in the alloy solidification process, will form the small angle grain boundary when two dendritic crystals meet, the growth process through designing single crystal superalloy dendritic crystal at single crystal superalloy, make the meeting of different degree take place between the dendritic crystal, make it form the small angle grain boundary when the dendritic crystal of different times meets in the solidification process, adopt the mould that forms not high single crystal superalloy foundry goods, through the growth direction of adjustment dendritic crystal, make low order dendritic crystal and different dendritic crystal meet, and form the small angle grain boundary, through carrying out orientation detection and evaluation to the region that the dendritic crystal meets, evaluate the forming tendentiousness of single crystal superalloy small angle grain boundary.
According to the method for evaluating the forming tendency of the small-angle grain boundary of the single-crystal high-temperature alloy, the larger the angle value of the small-angle grain boundary is, the stronger the forming tendency of the small-angle grain boundary of the alloy is.
According to the method for evaluating the forming tendency of the small-angle grain boundary of the single crystal superalloy, a mold of a single crystal superalloy casting is in a variable cross section step shape, platforms with different lengths are arranged on the side face of a vertical main solidification path of the mold, the outer ends of two sections of platforms with different lengths which are adjacent up and down are connected through a vertical high-order dendrite growth channel, and the high-order dendrite growth channels for connecting the two sections of platforms with different lengths which are adjacent up and down are the same in size and staggered in position in sequence.
According to the method for evaluating the forming tendency of the small-angle grain boundary of the single crystal superalloy, the size of the cross section of a main solidification path is 2-20 mm, and the shape of the cross section is a square, a rectangle, a rhombus, a polygon, a circle, an ellipse or a revolving body; the cross section of the platform is square, rectangular, rhombic, polygonal, elliptical or a revolving body; the shape of the cross section of the high-order dendrite growth channel is square, rectangular, rhombic, polygonal, oval or a revolving body, the size of the cross section is 10-30 mm, and the height is 25-40 mm.
According to the method for evaluating the forming tendency of the small-angle grain boundary of the single crystal superalloy, each die is 10-30 mm long with different platforms, and the constant height between the upper and lower adjacent platforms is 25-40 mm.
The method for evaluating the small-angle grain boundary forming tendency of the single crystal superalloy gradually reduces the platform length of a die from 30mm to 10mm along a step shape along the directional solidification direction from bottom to top; wherein, the dendrites of different even times meet in the platform after the length of the platform is changed.
The evaluation method of the formation tendency of the small-angle grain boundary of the single crystal superalloy is characterized in that the evaluated material is nickel-based single crystal superalloy and is used for evaluating the influence of the platform length on the formation of the small-angle grain boundary.
The method for evaluating the forming tendency of the small-angle grain boundary of the single crystal superalloy comprises the following specific steps:
(1) mold design
The mould has a step-shaped variable cross-section structure, the mould has different platform lengths and constant heights, the platform length is gradually reduced from 30mm to 10mm along the step shape along the directional solidification direction from bottom to top, and the height of each section of platform is 25-40 mm;
(2) wax film module preparation
Pressing wax into a wax mold by using a mold, placing the wax mold in a water bath box, keeping the water temperature at 20-25 ℃ for 30-60 minutes, and bonding the wax mold with a pouring system in a radial and circumferential placement manner to assemble a wax film module;
(3) preparation of ceramic mould shell
Adding nano oxide with the mass fraction of 0.1-1% into the traditional ceramic formwork component proportion, preparing the formwork through a slurry coating process, then putting the formwork into a muffle furnace for heating, wherein the heating is 600-1000 ℃, the heating adopts a heating method of gradual temperature rise, the temperature rises from room temperature to 100-150 ℃ at the temperature rise rate of 2-5 ℃/min, the heat is preserved for 0.1-1 hour, then the formwork is tilted for 3-45 degrees and is continuously preserved for 0.1-1 hour, and then the formwork is tilted for 6-90 degrees in the opposite direction and is continuously preserved for 0.1-1 hour; heating the muffle furnace to 280-320 ℃ at the heating rate of 5-10 ℃/min, preserving heat for 0.5-2 hours, heating to 800-1000 ℃ at the heating rate of 10-20 ℃/min, preserving heat for 0.5-3 hours, and obtaining a qualified ceramic formwork;
(4) alloy casting
Under the same solidification condition, casting the single crystal high temperature alloy to prepare a single crystal high temperature alloy casting with the components;
(5) observation of small angle grain boundaries in a platform
Carrying out macroscopic corrosion and crystal orientation tests on the single crystal superalloy casting, and observing the small-angle grain boundary angle difference in the platform; and quantitatively analyzing the tendentiousness of the small-angle crystal boundary of the single crystal high-temperature alloy by comparing the platform length of the small-angle crystal boundary of different single crystal high-temperature alloys with the angle difference of the small-angle crystal boundary in the platform.
According to the method for evaluating the small-angle grain boundary forming tendency of the single crystal superalloy, the nano oxide is one or more than two of aluminum oxide, yttrium oxide, hafnium oxide, zirconium oxide, calcium oxide, titanium oxide and chromium oxide, and the size of the nano oxide is 5-50 nm.
The design idea of the invention is as follows:
the method is based on that the dendrite branching process in the alloy solidification process can generate certain deflection, 2 times of dendrite and even generations of dendrite such as 4, 6, 8 and the like grow into the platform at the same time in the single crystal high temperature alloy design, and meet in the platform, so that the forming capability of the small angle crystal boundary of the single crystal high temperature alloy with different components and different generations of dendrite can be quantitatively represented on the premise of not changing the solidification condition and the simulation technology. Therefore, the method has the greatest characteristic that the forming tendency of the small-angle grain boundary of the single-crystal high-temperature alloy can be quantitatively evaluated.
The invention has the advantages and beneficial effects that:
1. according to the invention, according to the phenomenon that small-angle grain boundaries are easily formed due to the meeting of dendrites of different generations in the solidification process of the single crystal high-temperature alloy, a mold with different platform lengths and heights is designed, the small-angle grain boundaries are formed due to the meeting of the dendrites of 2 times and dendrites of even generations such as 4, 6 and 8 through the change of the platform length and the adjustment of the height, the forming tendency of the small-angle grain boundaries of the single crystal high-temperature alloy is evaluated, and the evaluation result of the method can be used as the basis for alloy selection, single crystal component preparation process parameters and casting head design.
2. The single crystal high temperature alloy casting has different platform lengths and heights, can study the influence of the platform height on the tendency of the small angle grain boundary, and can also form the influence of the tendency of the small angle grain boundary under the condition that different dendrites meet when a single crystal sample is prepared under the same directional solidification condition, thereby being beneficial to guiding the production process of single crystal components.
3. The method is simple to operate, reasonable in design, strong in operability, low in cost and beneficial to popularization and application, and the cost in the research and development and production processes of the single crystal high-temperature alloy part can be obviously reduced.
Description of the drawings:
FIG. 1 is a schematic diagram of the evaluation structure of the small-angle grain boundary of the single crystal superalloy. In the figure, 1 is the main solidification path, 2 platforms, 2 times dendrite or 4, 6, 8 times dendrite that are arranged in different length platforms meet, 3 is the high order dendrite growth channel, is used for providing high order dendrite.
FIG. 2 is a macroscopic morphology of single crystal superalloy low angle grain boundaries.
FIG. 3 is a microstructure of single crystal superalloy low angle grain boundaries.
FIG. 4 is a graph of dendrite frequency vs. low angle grain boundaries.
The specific implementation mode is as follows:
in the specific implementation process, high-order dendrites are branched from low-order dendrites in the solidification process of the single crystal high-temperature alloy, small-angle crystal boundaries are formed when the high-order dendrites and the low-order dendrites meet, 2-order dendrites and even-numbered generation dendrites such as 4, 6 and 8 grow into a platform simultaneously in the single crystal high-temperature alloy, and the forming tendency of the small-angle crystal boundaries of the single crystal high-temperature alloy is evaluated through the angle difference of the small-angle crystal boundaries in the platform. The method comprises the following steps: (1) designing variable cross-section moulds with different platform lengths and constant heights, combining ceramic materials and wax, and manufacturing corresponding mould shells; (2) preparing single crystal high temperature alloy castings of various alloys in a directional solidification furnace; (3) carrying out crystal orientation test on the single crystal high temperature alloys with different sections; (4) and analyzing the angle difference of the small-angle grain boundary in each cross section, and quantitatively evaluating the small-angle grain boundary forming capability of the single crystal high-temperature alloy. The larger the difference in angle between grain boundaries, the stronger the tendency of the alloy to form small angle grain boundaries. Therefore, on the premise of not using a simulation technology, the forming capability of the small-angle grain boundary of different single crystal high-temperature alloys can be quantitatively represented.
The invention relates to a method for evaluating the recrystallization forming tendency of a single crystal superalloy, which comprises the following steps:
1. mold design
As shown in figure 1, the die of the single crystal superalloy casting is in a variable cross-section step shape, platforms 2 with different lengths are arranged on the side face of a vertical main solidification path 1 of the die, the outer ends of two sections of platforms 2 with different lengths which are adjacent up and down are connected through a vertical high-order dendrite growth channel 3, and the high-order dendrite growth channels 3 used for connecting the two sections of platforms 2 with different lengths which are adjacent up and down are the same in size and are staggered in sequence. Along the directional solidification direction from bottom to top, the different platform lengths are gradually reduced to 10mm from 30mm along the stairstepping, and the constant height between the upper and lower adjacent two sections of platforms is 25-40 mm, so that the directional influence of the low-angle crystal boundary formation of the single crystal high-temperature alloy is realized.
2. Wax film module preparation
Pressing paraffin into wax molds by using a mold, placing the wax molds of each single-crystal high-temperature alloy casting in a water bath box at the water temperature of 20-25 ℃ for 30-60 minutes, and bonding the wax molds with a pouring system in a radial and circumferential placement mode to assemble a wax film module.
3. Preparation of ceramic mould shell
The nano oxide with the mass fraction of 0.1-1% is added in the traditional ceramic formwork component proportion, and the nano oxide has the following effects: the sintering temperature of the ceramic shell is reduced, so that the deformation of the shell is controlled, the deformation of the platform is reduced, the deflection caused by dendritic crystal growth introduced by the deformation of the shell is eliminated, and a small-angle grain boundary is introduced. The nano oxide can be aluminum oxide, yttrium oxide, hafnium oxide, zirconium oxide, calcium oxide, titanium oxide or chromium oxide and the like, the size of the nano oxide is 5-50 nm, the formwork is prepared through a slurry hanging process, then the formwork is placed into a muffle furnace for heating, the heating is 600-1000 ℃, and a heating method of gradually raising the temperature is adopted for heating: raising the temperature from room temperature to 100-150 ℃ at a temperature rise rate of 2-5 ℃/min, preserving the heat for 0.1-1 hour, then tilting the formwork for 3-45 degrees, continuously preserving the heat for 0.1-1 hour, and then tilting the formwork for 6-90 degrees in the opposite direction, and continuously preserving the heat for 0.1-1 hour. Raising the temperature of the muffle furnace to 300 ℃ at the temperature raising rate of 5-10 ℃/min, preserving the heat for 1 hour, raising the temperature to 800-1000 ℃ at the temperature raising rate of 10-20 ℃/min, preserving the heat for 0.5-3 hours, and obtaining a qualified ceramic formwork; wherein, the effect of heating by gradually rising temperature is: the ceramic material in the shell is promoted to be fully sintered, and when the shell tilts for a certain angle, the removal of materials such as residual carbon in the wax material is facilitated, and the interference of the residual carbon in the wax material is facilitated to be removed.
4. Alloy casting
And pouring different single crystal high temperature alloys under the same solidification condition to prepare single crystal high temperature alloy castings with different wall thicknesses.
5. Observation of small angle grain boundaries in a platform
Carrying out macroscopic corrosion and crystal orientation tests on the single crystal superalloy casting, and observing the small-angle grain boundary angle difference in the platform; and quantitatively analyzing the tendentiousness of the small-angle crystal boundary of the single crystal high-temperature alloy by comparing the platform length of the small-angle crystal boundary of different single crystal high-temperature alloys with the angle difference of the small-angle crystal boundary in the platform.
The present invention will be explained in further detail below by way of examples and figures.
Examples
In the embodiment, the macro morphology of the single crystal superalloy is as shown in fig. 2, the die is in a variable cross section step shape, the die has different platform lengths and constant heights between adjacent platforms, the platform length is gradually reduced from 30mm to 10mm along the step shape along the directional solidification direction from bottom to top, and the heights between the upper and lower adjacent platforms are both 30 mm.
The method comprises the steps of adding 0.5% of nano oxide in mass percent into the traditional ceramic formwork in a formula ratio, wherein the nano oxide can be aluminum oxide, yttrium oxide, hafnium oxide, zirconium oxide, calcium oxide, titanium oxide or chromium oxide and the like, the size of the nano oxide is 5-50 nm, preparing the formwork through a slurry coating process, then putting the formwork into a muffle furnace for heating to 900 ℃, heating to 120 ℃ by adopting a heating method of gradually heating, heating to 120 ℃ from room temperature at a heating rate of 3 ℃/min, preserving heat for 0.5 hour, then tilting the formwork for 30 degrees, continuously preserving heat for 0.5 hour, and then tilting the formwork for 30 degrees in the opposite direction and continuously preserving heat for 0.5 hour. And raising the temperature of the muffle furnace to 300 ℃ at the heating rate of 8 ℃/min, preserving the heat for 1 hour, raising the temperature of the muffle furnace to 900 ℃ at the heating rate of 15 ℃/min, preserving the heat for 2 hours, and obtaining the qualified ceramic formwork.
Taking DD407 nickel-based single crystal superalloy as an example, the influence of the low-angle grain boundary forming tendency of the single crystal superalloy is introduced.
The single crystal hollow casting is a single crystal high temperature alloy casting prepared under the technological parameter conditions that the temperature of the upper and lower areas is 1500 ℃ and the pulling speed is 3 mm/min.
As shown in fig. 2-3, after determining the morphology of the macro-corrosion and the electron back scattering orientation, it can be seen that, on the first stage platform, 2 times of dendrites meet 4 times of dendrites, the value of the small angle grain boundary is about 0.5 degree, and as the platform height increases, 2 times of dendrites meet 6 times, 8 times and even number of dendrites respectively, and as the platform height increases, the angle of the small angle grain boundary in the platform becomes larger and larger.
The working process and the result of the invention are as follows:
according to the invention, by designing the moulds with different platform lengths and constant heights between adjacent platforms and preparing the single crystal high-temperature alloy casting according to the moulds, high-order dendrites meet in the platforms to form small-angle crystal boundaries, analyzing the angle difference of the small-angle crystal boundaries in the platforms with different heights, quantitatively evaluating the forming capability of the small-angle crystal boundaries of the alloy, providing a basis for selecting the single crystal high-temperature alloy with weak low-angle crystal boundary forming tendency in actual production, and simultaneously, the method is beneficial to research and development of single crystal high-temperature alloy materials and optimization of a solidification process in the preparation process of single crystal parts, and reducing the production cost.
As shown in fig. 4, it can be seen from the relationship between the number of dendrites and the small-angle grain boundaries that the angle of the small-angle grain boundaries gradually increases with the increase of the platform, and the deflection angle from the small-angle grain boundaries on the first-stage platform is about 0.5 ° to the deflection angle of the eleventh-stage platform is about 2.8 °.
The embodiment result shows that the method has the characteristics of simple preparation process, low cost and the like, can solve the problem that the tendency of the small-angle grain boundary of the single crystal high-temperature alloy is difficult to evaluate, and quantitatively evaluates the forming capability of the small-angle grain boundary of different single crystal high-temperature alloys in the directional solidification process, thereby being beneficial to research and development of single crystal high-temperature alloy materials and providing a basis for optimizing the solidification process in actual production.
Claims (6)
1. A method for evaluating the forming tendency of a single crystal high-temperature alloy low-angle grain boundary is characterized in that according to the classical theory of directional solidification, dendrites can deflect in the solidification process of an alloy, a low-angle grain boundary can be formed when two dendrites meet each other, the growth process of the dendrites of the single crystal high-temperature alloy is designed in the single crystal high-temperature alloy, so that the dendrites meet each other in different degrees, a small-angle grain boundary can be formed when the dendrites meet each other in different times in the solidification process, a die for forming single crystal high-temperature alloy castings with different heights is adopted, the growth direction of the dendrites is adjusted, so that the dendrites with the lower times meet different dendrites, the low-angle grain boundary can be formed, and the forming tendency of the single crystal high-temperature alloy low-angle grain boundary can be evaluated by carrying out orientation detection and evaluation on the regions where the dendrites meet each other;
the die of the single crystal high-temperature alloy casting is in a variable cross-section step shape, the side surface of a vertical main solidification path of the die is provided with platforms with different lengths, the outer ends of two sections of platforms with different lengths which are adjacent up and down are connected through a vertical high-order dendrite growth channel, and the high-order dendrite growth channels for connecting the two sections of platforms with different lengths which are adjacent up and down are same in size and staggered in position;
each mold is provided with different platforms with the length of 10-30 mm, and the constant height between the two adjacent platforms is 25-40 mm;
along the directional solidification direction from bottom to top, the length of the platform of the mould is gradually reduced from 30mm to 10mm along the step shape; wherein, the dendrites of different even times meet in the platform after the length of the platform is changed.
2. The method of assessing the formation tendency of the small angle grain boundaries of a single crystal superalloy as in claim 1, wherein a larger value of the angle of the small angle grain boundaries indicates a greater formation tendency of the small angle grain boundaries of the alloy.
3. The method for evaluating the forming tendency of the small-angle grain boundaries of the single-crystal superalloy according to claim 1, wherein the size of the cross section of the main solidification path is 2-20 mm, and the shape of the cross section is square, rectangular, rhombic, circular or elliptical; the cross section of the platform is square, rectangular, rhombic or elliptical; the shape of the cross section of the high-order dendrite growth channel is square, rectangular, rhombic or oval, the size of the cross section is 10-30 mm, and the height is 25-40 mm.
4. The method of assessing the propensity of single crystal superalloys to form small angle grain boundaries as recited in claim 1, wherein the material being assessed is a nickel-based single crystal superalloy and is used to assess the effect of plateau length on the formation of small angle grain boundaries.
5. The method for evaluating the forming tendency of the small-angle grain boundaries of the single-crystal superalloy according to claim 1, comprising the following steps:
(1) mold design
The mould has a step-shaped variable cross-section structure, the mould has different platform lengths and constant heights, the platform length is gradually reduced from 30mm to 10mm along the step shape along the directional solidification direction from bottom to top, and the height of each section of platform is 25-40 mm;
(2) wax film module preparation
Pressing wax into a wax mold by using a mold, placing the wax mold in a water bath box, keeping the water temperature at 20-25 ℃ for 30-60 minutes, and bonding the wax mold with a pouring system in a radial and circumferential placement manner to assemble a wax film module;
(3) preparation of ceramic mould shell
Adding nano oxide with the mass fraction of 0.1-1% into the traditional ceramic formwork component proportion, preparing the formwork through a slurry coating process, then putting the formwork into a muffle furnace for heating, wherein the heating temperature is 600-1000 ℃, the heating adopts a heating method of gradual temperature rise, the temperature rises to 100-150 ℃ from room temperature at the temperature rise rate of 2-5 ℃/min, the temperature is kept for 0.1-1 hour, then the formwork is tilted for 3-45 degrees and kept for 0.1-1 hour, and then the formwork is tilted for 6-90 degrees in the opposite direction and kept for 0.1-1 hour; heating the muffle furnace to 280-320 ℃ at the heating rate of 5-10 ℃/min, preserving heat for 0.5-2 hours, heating to 800-1000 ℃ at the heating rate of 10-20 ℃/min, preserving heat for 0.5-3 hours, and obtaining a qualified ceramic formwork;
(4) alloy casting
Under the same solidification condition, casting the single crystal high-temperature alloy to prepare a single crystal high-temperature alloy casting;
(5) observation of small angle grain boundaries in a platform
Carrying out macroscopic corrosion and crystal orientation tests on the single crystal superalloy casting, and observing the small-angle grain boundary angle difference in the platform; and quantitatively analyzing the tendentiousness of the small-angle crystal boundary of the single crystal high-temperature alloy by comparing the platform length of the small-angle crystal boundary of different single crystal high-temperature alloys with the angle difference of the small-angle crystal boundary in the platform.
6. The method for evaluating the small angle grain boundary forming tendency of the single crystal superalloy according to claim 5, wherein the nano oxide is one or more of aluminum oxide, yttrium oxide, hafnium oxide, zirconium oxide, calcium oxide, titanium oxide and chromium oxide, and the size of the nano oxide is 5-50 nm.
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