CN109082710B - Preparation method of nickel-based single crystal superalloy test rod with chemical components distributed in continuous gradient manner - Google Patents
Preparation method of nickel-based single crystal superalloy test rod with chemical components distributed in continuous gradient manner Download PDFInfo
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- CN109082710B CN109082710B CN201811079655.7A CN201811079655A CN109082710B CN 109082710 B CN109082710 B CN 109082710B CN 201811079655 A CN201811079655 A CN 201811079655A CN 109082710 B CN109082710 B CN 109082710B
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/52—Alloys
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
Abstract
The invention discloses a preparation method of a nickel-based single crystal superalloy test rod with chemical components distributed in a continuous gradient manner, and belongs to the technical field of metal material preparation. The method uses high-melting-point single crystal alloy placed at the lower end of a mould shell as seed crystals and realizes single crystal growth by a directional solidification process. In the state that the two alloys are completely molten, the two alloy liquids are mutually mixed through convection or diffusion, so that the alloy components are changed, and a component gradient is generated. The method can realize the centimeter-level component gradient distribution in the nickel-based single crystal sample and can meet the requirements of research on macroscopic mechanical properties such as durability, creep deformation and the like.
Description
Technical Field
The invention relates to the technical field of metal material preparation, in particular to a preparation method of a nickel-based single crystal superalloy test rod with chemical components distributed in a continuous gradient manner.
Background
In 6 months of 2011, the ' Materials Genome Initiative (MGI) is proposed in the lecture of the university of kangsu-meilong with the topic of ' advanced manufacturing partnership ', and the general aim of the method is to improve the speed of new Materials from discovery to application by at least one time and reduce the cost by at least one half by utilizing the breakthrough in material simulation calculation, high-throughput experiments and data mining in recent years. MGI represents a new model for future advanced material development. In recent years, the Chinese edition of the 'material genome project' is also started in China, and the material genome technology is vigorously developed. A high-throughput preparation technology, which is one of the material genome technologies, has been remarkably developed. The high-flux preparation method of the metal material has various methods, including a combined material chip technology, a powder metallurgy method, a 3D printing method, a new device developed based on common smelting casting, a diffusion multi-element method and the like. Wherein, the combined material chip technology is not suitable for the field of high-temperature alloy; the method for powder metallurgy, 3D printing, new devices developed based on common smelting and casting and the like realizes gradient change of material components by controlling the precise proportion of raw material powder components, and the obtained materials are all polycrystalline alloys; although the diffusion multi-node method can prepare single crystal samples with gradient distribution of components, the distribution distance of the gradient components is narrow (about 200 μm), and the requirements of macroscopic mechanical property (such as endurance and creep) research cannot be met. At present, a high-flux preparation method suitable for the nickel-based single crystal superalloy is not reported.
Disclosure of Invention
The invention aims to provide a preparation method of a nickel-based single crystal superalloy test rod with chemical components in continuous gradient distribution, which can realize the gradient distribution of the components in a centimeter level in a nickel-based single crystal sample and can meet the requirements of research on macroscopic mechanical properties such as durability, creep deformation and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a nickel-based single crystal superalloy test rod with chemical components in continuous gradient distribution is characterized in that the content of an element A in the chemical components of the alloy is in gradient distribution, and the content of other elements except nickel is kept unchanged; the preparation method of the nickel-based single crystal superalloy test rod comprises the following steps:
(1) preparing a formwork: the mold shell comprises a mold shell base plate and an alumina tube for bearing a nickel-based single crystal high-temperature alloy test bar, wherein a hole is drilled in the mold shell base plate, and the alumina tube is inserted into the hole in the mold shell base plate and is fixed (can be fixed by adopting paint);
(2) preparing an alloy bar: respectively preparing an alloy bar with the element A content of a1 and an alloy bar with the element A content of a2 according to the distribution range of the element A content in the target alloy test bar, wherein alloy components with relatively high melting points are prepared into single-crystal alloy bars, and the requirement is not made when the melting points are low; the diameter of the alloy bar is slightly smaller than the inner diameter of the alumina tube on the formwork; meanwhile, the monocrystalline alloy bar with high melting point component is used as seed crystal, and the length is more than 3 cm; after being butted, the two bars are placed in an alumina tube;
(3) preparing a nickel-based single crystal superalloy test rod with chemical components distributed in a continuous gradient manner: the high-speed solidification (HRS) method is adopted for preparation, firstly, the mould shell is fixed on a water-cooling disc and is placed in a heat preservation furnace; the temperature and the smelting time of the holding furnace are determined according to the contact surface type of the test bars with two components, the vacuum degree in the furnace is less than or equal to 1Pa, and the drawing rate of the directional solidification is 3-6 mm/min.
In the step (1), the mould shell chassis is prepared by a traditional method, and is obtained by coating, air-drying, dewaxing and grinding a disc-shaped wax mould by using a coating; the material of the alumina tube is high-purity alumina, the inner diameter of the alumina tube is selected according to the size of the required test bar, and the number of the alumina tubes is determined according to the experiment requirement.
In the step (2), the element A is any one of main elements except nickel in the nickel-based single crystal superalloy; the distribution range of the weight percentage content of the element A in the target alloy test bar is a 1-a 2%, and a1 is less than a2(a1 is the lower limit of the content, and a2 is the upper limit of the content).
In the step (2), the high-melting-point bar serving as the seed crystal is placed at the lower part of the alumina tube, the other bar is placed at the upper part of the alumina tube, and the contact surfaces of the two bars are ensured to be clean and attached.
In the step (2), when two bars are butted, the contact surface is a flat surface or a wedge surface; the straight surface means that the contact surface is perpendicular to the axial direction of the alumina tube, and the wedge-shaped surface means that the angle formed by the contact surface and the axial direction of the alumina tube is 0-90 degrees.
In the step (2), when two bars are butted, the selection principle of the contact surface is as follows: when the density of the high-melting-point bar is less than that of the low-melting-point bar, the contact surface is a flat surface; when the density of the high-melting-point bar is greater than that of the low-melting-point bar, the contact surface is a wedge-shaped surface; the height of the wedge-facet depends on the length of the desired gradient component.
In the step (3), the selection principle of the temperature of the holding furnace and the smelting time is as follows: when the contact surface is flat and straight, the temperature of the holding furnace is 50-100 ℃ higher than the melting point of the bar with the high melting point at the lower end, and the smelting time is 20-40 min; when the contact surface is a wedge surface, the temperature of the holding furnace is 100-150 ℃ higher than the melting point of the bar with the high melting point at the lower end, and the smelting time is 2-4 h.
The principle of the invention is as follows:
the high melting point single crystal alloy is used as seed crystal, and the single crystal growth is realized through the directional solidification process. In the state that the two alloys are completely molten, the two alloy liquids are mutually mixed through convection or diffusion, so that the alloy components are changed, and a component gradient is generated. When the density of the upper-end low-melting-point alloy is higher than that of the lower-end high-melting-point alloy, the two alloy liquids can generate convection and are mixed with each other, so that the alloy components are changed, and the component gradient is generated. At the moment, the contact surface of the two alloys is a straight surface, and the speed and the distance of the convection of the alloy liquid are controlled by shortening the smelting time by reducing the temperature of the holding furnace. When the density of the upper-end low-melting-point alloy is smaller than that of the lower-end high-melting-point alloy, the alloy liquid does not generate convection, the contact surface of the two alloys is a wedge-shaped surface, and the two alloys are fused in the radial direction through diffusion of elements in the alloy liquid. In the wedge-shaped contact section of the two alloys, the proportion of the two alloys in any cross section is different, so that a composition gradient is generated. Because the diffusion rate of the elements is slow, the temperature of the holding furnace is increased, and the smelting time is increased to ensure the sufficiency of radial diffusion.
The invention has the following beneficial effects:
(1) the preparation method of the nickel-based single crystal superalloy test rod with chemical components in continuous gradient distribution, provided by the invention, can be used for preparing single crystal samples with multiple components in gradient distribution at one time, greatly improves the preparation efficiency of the single crystal samples for experiments, reduces the experiment cost, and belongs to a high-throughput preparation method.
(2) The mould shell adopted by the invention has a simple structure, is easy to prepare, can adjust the diameter and the number of the single crystal test rods according to actual needs, and has great flexibility.
(3) In the nickel-based single crystal alloy test bar prepared by the invention, the distribution distance of gradient components can reach the centimeter level, and the nickel-based single crystal alloy test bar can be used for processing samples with durability, creep deformation and the like and used for high-throughput characterization research on mechanical properties.
Drawings
FIG. 1 is a schematic flow chart of the production process of the present invention; in the figure: 1-alumina tube, 2-mould shell base plate, 3-water cooling plate, 4-heating body, 5-high melting point alloy bar and 6-low melting point alloy bar.
FIG. 2 is a graph showing the results of analyzing the composition of a tantalum content gradient single crystal test rod according to example 1 of the present invention.
FIG. 3 is a result of analyzing the composition of a single crystal test rod having a gradient change in chromium content according to example 2 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following examples, but the scope of the present invention is not limited to the following examples.
Example 1:
the embodiment is a preparation method of a nickel-based single crystal superalloy test rod with tantalum (Ta) content in continuous gradient distribution, and the method comprises the following specific steps:
(1) preparing a formwork: the mould shell chassis 2 is prepared by adopting a traditional method and obtaining the mould shell chassis after coating, air drying, dewaxing and grinding the disc-shaped wax mould by paint. The mold shell for holding the single crystal test rods uses a high-purity alumina tube with the inner diameter of 10mm, the length of 150mm and the number of 4 tubes. Drilling a hole on the bottom plate of the formwork, inserting an alumina tube 1, and fixing by using paint.
(2) Preparing an alloy bar: according to the designed gradient change range (5-9 wt%) of the Ta content, the alloy with two components of 5 wt% Ta and 9 wt% Ta is prepared respectively, and the specific components are shown in Table 1. The alloy containing 5 wt% of Ta has high melting point and is prepared into a single crystal test rod with the diameter of 16 mm; the alloy containing 9 wt% of Ta is smelted into an alloy ingot. The two alloys are processed into bars with the diameter of 9.8mm, the length of the bars is 6cm, and the contact surface is processed into a flat surface. Two alloy bars are put into an alumina tube on a mould shell, a high-melting-point alloy bar 5 containing 5 wt% of Ta is placed at the lower end, a low-melting-point alloy bar 6 containing 9 wt% of Ta is placed at the upper end, and the contact surfaces of the two test bars are ensured to be clean and attached.
TABLE 1 chemical composition (wt%) of the two alloys used in example 1
| Alloy (I) | Cr | Co | W | Mo | Ta | Al | Re | Ru | Ni |
| 5Ta | 3.5％ | 8％ | 6％ | 1.5％ | 5％ | 6％ | 5％ | 3％ | Surplus |
| 9Ta | 3.5％ | 8％ | 6％ | 1.5％ | 9％ | 6％ | 5％ | 3％ | Surplus |
(3) Directional solidification of gradient component test bars: the gradient component single crystal test bar is prepared by a high speed solidification (HRS) method. The mould shell is fixed on a water-cooling disc 3 and is lifted into a heat preservation furnace, and a heating body 4 in the heat preservation furnace heats the mould shell. The temperature of the holding furnace is 1480 ℃, the smelting time is 30min, and the vacuum degree in the furnace is less than or equal to 1 Pa. After the smelting is finished, the mould shell is pulled out from the heat preservation furnace at the pulling speed of 3mm/min, and the nickel-based single crystal superalloy test bar with the required Ta content in continuous gradient distribution is obtained.
The energy spectrum of a scanning electron microscope is used for analyzing the components of the longitudinal section of the single crystal test bar with the Ta content gradient, and the result is shown in FIG. 2. As can be seen, the Ta content gradient varies by about 25mm over a range of about 5 to 8.5 wt%.
Example 2:
the embodiment is a preparation method of a nickel-based single crystal superalloy test rod with continuous gradient distribution of chromium (Cr) content, which comprises the following specific steps:
(1) preparing a formwork: the preparation of the mould shell chassis adopts a traditional method, and the disc-shaped wax mould is obtained by coating, air-drying, dewaxing and grinding. The mold shell for holding the single crystal test rods uses a high-purity alumina tube with the inner diameter of 6mm, the length of 150mm and the number of 4 tubes. Drilling a hole on the bottom plate of the formwork, inserting an alumina tube, and fixing by using paint.
(2) Preparing an alloy bar: according to the gradient change range (2.5-6 wt%) of Cr content, the alloy with two components of 2.5 wt% Cr and 6 wt% Cr is prepared, and the specific components are shown in Table 2. 2.5 wt% of Cr alloy has high melting point and is prepared into a single crystal test rod with the diameter of 16 mm; 6 wt% Cr alloy is smelted into alloy ingot. The two alloys are processed into test bars with the diameter of 5.8mm, the length of each test bar is 6cm, the contact surface is processed into a wedge-shaped surface, and the height of the wedge-shaped surface is 25 mm. Two alloy test bars are put into a mould shell, a 2.5 wt% Cr test bar is placed at the lower end, a 6 wt% Cr test bar is placed at the upper end, and the contact surfaces of the two test bars are ensured to be clean and attached.
Table 2 chemical composition (wt%) of two alloys used in example 2
| Alloy (I) | Cr | Co | W | Mo | Ta | Al | Re | Ru | Ni |
| 2.5Cr | 2.5％ | 8％ | 5％ | 1％ | 8％ | 6％ | 5％ | 3 | Surplus |
| 6Cr | |||||||||
| 6％ | 8％ | 5％ | 1％ | 8％ | 6％ | 5％ | 3％ | Surplus |
(3) Directional solidification of gradient component test bars: the gradient component single crystal test bar is prepared by a high speed solidification (HRS) method. Fixing the mould shell on a water-cooling disc, and lifting the mould shell into a heat preservation furnace. The temperature of the holding furnace is 1550 ℃, the smelting time is 2 hours, and the vacuum degree in the furnace is less than or equal to 1 Pa. After the smelting is finished, the mould shell is pulled out from the heat preservation furnace at the pulling speed of 5mm/min, and the nickel-based single crystal superalloy test bar with the required Cr content in continuous gradient distribution is obtained.
The analysis of the components of the longitudinal section of the Cr content gradient single crystal test bar using the energy spectrum of a scanning electron microscope is shown in FIG. 3. As can be seen from the figure, the distance of the Cr content gradient is about 20mm, and the variation range is about 2.5-6 wt%.
Claims (2)
1. A preparation method of a nickel-based single crystal superalloy test rod with chemical components distributed in a continuous gradient manner is characterized by comprising the following steps: the nickel-based single crystal superalloy with the chemical components in continuous gradient distribution is characterized in that the content of an element A in the chemical components of the alloy is in gradient distribution, and the content of other elements except the nickel and the element A is kept unchanged; the element A is Ta or Cr; the distribution range of the weight percentage content of the element A in the target alloy test bar is a 1-a 2%, and a1 is less than a 2; the preparation method of the nickel-based single crystal superalloy test rod comprises the following steps:
(1) preparing a formwork: the mold shell comprises a mold shell base plate and an alumina tube for bearing a nickel-based single crystal high-temperature alloy test bar, wherein a hole is drilled in the mold shell base plate, and the alumina tube is inserted into the hole in the mold shell base plate and is fixed; the mould shell chassis is prepared by a traditional method, and is obtained by coating, air-drying, dewaxing and grinding a disc-shaped wax mould by using a coating; the material of the alumina tube is high-purity alumina, the inner diameter of the alumina tube is selected according to the size of the required test bar, and the number of the alumina tubes is determined according to the experimental requirement;
(2) preparing an alloy bar: respectively preparing an alloy bar with the element A content of a1 and an alloy bar with the element A content of a2 according to the distribution range of the element A content in the target alloy test bar, wherein alloy components with relatively high melting points are prepared into single-crystal alloy bars, and the requirement is not made when the melting points are low; meanwhile, the monocrystalline alloy bar with high melting point component is used as seed crystal, and the length is more than 3 cm; after being butted, the two bars are placed in an alumina tube;
(3) preparing a nickel-based single crystal superalloy test rod with chemical components distributed in a continuous gradient manner: adopting a high-speed solidification method HRS preparation, firstly fixing a mould shell on a water-cooling disc, and placing the mould shell into a heat preservation furnace; the temperature and the smelting time of the holding furnace are determined according to the contact surface type of the test bars with two components, the vacuum degree in the furnace is less than or equal to 1Pa, and the drawing rate of the directional solidification is 3-6 mm/min;
in the step (2), when two bars are butted, the contact surface is a flat surface or a wedge surface; the straight surface is that the contact surface is vertical to the axial direction of the alumina tube, and the wedge-shaped surface is that the angle formed by the contact surface and the axial direction of the alumina tube is 0-90 degrees;
in the step (2), when two bars are butted, the selection principle of the contact surface is as follows: when the density of the high-melting-point bar is less than that of the low-melting-point bar, the contact surface is a flat surface; when the density of the high-melting-point bar is greater than that of the low-melting-point bar, the contact surface is a wedge-shaped surface; the height of the wedge-shaped surface is determined according to the length of the required gradient component;
in the step (3), the selection principle of the temperature of the holding furnace and the smelting time is as follows: when the contact surface is flat and straight, the temperature of the holding furnace is 50-100 ℃ higher than the melting point of the bar with the high melting point at the lower end, and the smelting time is 20-40 min; when the contact surface is a wedge surface, the temperature of the holding furnace is 100-150 ℃ higher than the melting point of the bar with the high melting point at the lower end, and the smelting time is 2-4 h.
2. The method for preparing a Ni-based single crystal superalloy test rod having a chemical composition continuously graded according to claim 1, wherein: in the step (2), a high-melting-point bar serving as a seed crystal is placed at the lower part of the alumina tube, the other bar is placed at the upper part of the alumina tube, and the contact surfaces of the two bars are ensured to be clean and attached; the diameter of the alloy bar is slightly smaller than the inner diameter of the alumina tube on the formwork.
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| CN109811405B (en) * | 2019-03-28 | 2020-10-27 | 西北工业大学 | Preparation method of Nb-Si-based ultrahigh-temperature alloy component gradient test piece |
| CN111364096B (en) * | 2020-03-30 | 2021-01-22 | 上海交通大学 | Substrate-triggered single crystal high-temperature alloy directional solidification process |
| CN111979582B (en) * | 2020-08-21 | 2021-05-07 | 西北工业大学 | Preparation method of single crystal superalloy with gradient structure |
| CN114346180B (en) * | 2022-01-07 | 2023-02-24 | 西安交通大学 | Method for controlling mosaic defects of single crystal high-temperature alloy blade |
| CN114934312A (en) * | 2022-05-18 | 2022-08-23 | 中南大学 | Device and method for manufacturing high-throughput sample and gradient functional material |
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