CN115142060A - High-throughput preparation method of alloy sample suitable for solidification kinetics research - Google Patents
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Abstract
The invention relates to an alloy sample high-flux preparation method suitable for solidification kinetics research, and belongs to the technical field of alloy material high-flux preparation. Conveying two or more kinds of metal powder by using a coaxial powder feeding technology, changing the conveying proportion along the deposition direction in the 3D printing process, and forming a wide-component blocky alloy sample with alloy components changing along the deposition direction on a substrate; cutting the blocky alloy sample into a plurality of sheet alloy samples along the component change direction, moving a laser beam on the surface of the sheet alloy sample along the component change direction to carry out laser remelting, completing remelting on each sheet alloy sample for two or more times, and using different laser remelting process parameters for remelting in different times so as to introduce different solidification conditions; and cutting the sheet alloy subjected to the multi-pass remelting into a plurality of strip-shaped samples perpendicular to the component change direction, so that the high-throughput preparation of the alloy sample for solidification dynamics research is realized.
Description
Technical Field
The invention relates to an alloy sample high-flux preparation method suitable for solidification kinetics research, and belongs to the technical field of alloy material high-flux preparation.
Background
In metal materials, the alloy solidification structure can greatly influence the alloy performance, especially in large samples, because the difficulty of post-treatment is increased, the solidification structure can often influence the structure after final treatment, and therefore, the control of the solidification structure is necessary in the preparation of the alloy.
There are many factors that affect the formation of the alloy solidification structure, and the composition and the solidification conditions are most critical, and the change of the composition and the solidification conditions can significantly affect the solidification structure of the alloy. For example, for a eutectic alloy material, a change in composition causes the alloy to transition from hypoeutectic to fully eutectic to hypereutectic, whereas at the same composition, a change in solidification conditions causes the alloy to transition from hypoeutectic to fully eutectic, and thus the eutectic alloy system is a highly composition sensitive, highly solidification condition sensitive material.
In the traditional method, in order to realize the preparation of solidification structure samples of eutectic system alloys with different components and different solidification conditions, a large number of alloy samples with different components need to be prepared at one time, different solidification conditions are introduced under each component, and the preparation method needs a large amount of labor time and preparation cost. Therefore, in order to realize the research on the solidification kinetics of a class of alloy systems, a method capable of quickly preparing a sample under a multi-component/multi-solidification condition is urgently needed, so that the construction of the component-solidification condition-structure relation of the system is completed.
Disclosure of Invention
Aiming at the requirement of rapid preparation of a multicomponent/multiple solidification condition sample in the current alloy solidification dynamics research, the invention provides an alloy sample high-flux preparation method suitable for the solidification dynamics research, which utilizes the characteristics of layer-by-layer forming and wide forming of a laser additive manufacturing technology (3D printing technology) and combines the characteristic of real-time controllable input proportion of various powders in coaxial powder feeding, and realizes the input of different solidification conditions by introducing laser remelting of different process conditions in different positions of an alloy sample along the component change direction on the basis of obtaining a large-size wide-component blocky alloy sample with alloy components changed along the deposition direction, thereby rapidly preparing the alloy sample with the multicomponent and multiple solidification conditions and providing a basis for a series of alloy research on the solidification tissue forming conditions.
The purpose of the invention is realized by the following technical scheme.
An alloy sample high-flux preparation method suitable for solidification kinetics research specifically comprises the following steps:
(1) Two or more metal powders are used as raw materials for preparing an alloy sample, a coaxial powder feeding technology is utilized to convey multiple metal powders, the conveying proportion of the multiple metal powders is changed along the deposition direction according to the requirement of component change in the alloy sample in the 3D printing process, and a wide-component massive alloy sample with alloy components changed along the deposition direction is formed on a substrate;
(2) Taking the bulk alloy sample from the substrate, and cutting the bulk alloy sample into a plurality of sheet alloy samples along the component change direction;
(3) The laser beam moves on the surface of the sheet alloy sample along the component change direction to realize laser remelting of different component positions of the same sheet alloy sample, wherein the laser beam moves from one end of the sheet alloy sample to the other end of the sheet alloy sample to complete the laser remelting of all different components in the sheet alloy sample, namely, complete one-pass remelting, and after one-pass remelting is completed, the technological parameters of the laser remelting are changed, next-pass remelting is carried out at different positions of the same sheet alloy sample along the component change direction or next-pass remelting is carried out on another sheet alloy sample along the component change direction, and different solidification speeds and temperature gradients in the height direction of a laser molten pool are utilized, so that different solidification conditions are introduced at the same component position of one laser molten pool along the height direction of the molten pool, and then the introduction of multiple solidification conditions is realized through the change of the laser remelting process on a plurality of sheet alloy samples;
(4) And cutting the sheet alloy sample subjected to the multi-pass remelting into a plurality of strip-shaped samples perpendicular to the component change direction, wherein different strip-shaped samples have different components, and different positions of the same strip-shaped sample have different solidification structures due to different laser remelting process parameters, so that the high-throughput preparation of the alloy sample for solidification kinetic research is realized.
In the step (1), the plurality of metal powders may be a plurality of elemental powders, a plurality of alloy powders, or a plurality of metal powders composed of elemental powders and alloy powders. Preferably, the metal powder is spherical powder with the grain diameter of 0.04-0.20 mm.
In the 3D printing process of the step (1), the diameter of a laser spot is preferably 2-6 mm, the laser power is preferably 1200-1800W, the laser scanning speed is preferably 10-30 mm/min, the deposition thickness of each layer is preferably 0.4-0.8 mm, and the fixed spacing between layers is preferably 1.5-3.0 mm (or the overlap ratio between layers is 50-80%).
Further, the conveying proportion of various metal powders is changed every 3-8 layers are deposited.
In the remelting process in the step (3), the laser power of the laser beam is preferably 400-2000W, and the moving speed of the laser beam is preferably 1-50 mm/s. Correspondingly, the thickness of the sheet alloy sample is more preferably 1.5-2.5 times of the diameter of the laser spot in the laser remelting process, and the center distance between two molten pools remelted in two adjacent passes in the same sheet alloy sample is more preferably 2-3 times of the diameter of the laser spot in the laser remelting process.
In the step (4), the sheet-shaped alloy sample is cut into a plurality of strip-shaped samples along the deposition interface among different components in the sheet-shaped alloy sample, the number of the strip-shaped samples is the same as the number of component gradient changes in the sheet-shaped alloy sample, and the thickness of each strip-shaped sample is the same as the deposition thickness of the corresponding component.
For Al 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x The system material (x is more than or equal to 0 and less than or equal to 0.5), and Al is preferably selected 0.8 Co 1 Cr 1 Fe 1 Ni 1.8 Alloy powder and Al 1.3 Co 1 Cr 1 Fe 1 Ni 2.3 Alloy powder is used as a raw material. More preferably, the conveying ratio of the two alloy powders is changed once every 3 to 5 layers of deposition, and the conveying ratio of the two alloy powders is changed according to the increasing or decreasing ratio of 0.3 to 0.7at percent of Al element atom and 0.15 to 0.35at percent of Ni element atom, and simultaneously the gradient change of Al atom percent in the range of 14.29 to 19.70at percent and the gradient change of Al atom percent in the range of 14.29 to 19.70at percent are realizedThe atomic percentage of the Ni element is changed in a gradient range from 32.14at percent to 34.85at percent.
Has the advantages that:
(1) The high-throughput preparation method provided by the invention utilizes the characteristics of layer-by-layer forming and wide forming of a 3D printing technology, combines the characteristic that the input proportion of various powders in coaxial powder feeding is controllable in real time, can use powders with different proportions on different deposition layers to realize the change of alloy components of a sample along the deposition direction, and then realizes the input of different solidification conditions by introducing laser remelting with different process conditions at different positions of the alloy sample along the component change direction on the basis of successfully preparing a large-size alloy sample with a wide component space, so that the alloy sample with multiple components and multiple solidification conditions can be quickly prepared, the quick establishment of alloy components, solidification conditions and solidification structures is completed, the optimization of the alloy components and the process conditions is accelerated, and the cost of manpower and material resources for alloy research and development is reduced.
(2) The good shape forming of the alloy sample is the premise that the layered components are controllable and the subsequent laser remelting treatment is carried out, so the process window for the good shape forming of the alloy sample is obtained by optimizing the 3D printing process parameters.
(3) According to the high-flux preparation method, the thickness of each component deposition layer can be optimized according to the requirements of sample preparation requirements, the requirement of introducing different solidification kinetic conditions is met, the operation is simple, and the applicability is strong.
(4) In the high-flux preparation method, the laser remelting process parameters which have great influence on the alloy solidification structure are selected as variables to be researched, and the solidification dynamics research of the alloy material under different laser remelting process conditions based on wide component space is completed. In addition, in the laser remelting process, the laser scanning speed determines the upper limit range of the solidification speed in a molten pool, and the change of the laser power is the premise of ensuring that a sample can be melted under different laser scanning speeds, so that a large-range and controllable laser remelting process is needed as the premise of obtaining the sample with multiple solidification conditions.
(5) If the thickness of a flaky alloy sample cut from a large-size blocky alloy sample prepared by a 3D technology is too small, laser penetrates through the flaky alloy sample, so that a normal laser molten pool cannot be obtained, and if the thickness is too large, material waste is caused, so that the thickness of the flaky alloy sample is 1.5-2.5 times of the diameter of a laser spot. In addition, the small remelting distance between two adjacent passes on the same sheet alloy sample can cause two melting baths to be overlapped together, so that a normal melting bath cannot be obtained, and the large remelting distance can cause material waste, so that the distance between the centers of the two adjacent melting baths is set to be 2-3 times of the diameter of a laser spot.
(6) For Al 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x In the material system, the solidification structure is greatly influenced by the Al and Ni content and the change of the solidification condition caused by the laser remelting process parameters, and the alloy component-solidification condition-solidification structure is quickly established by optimizing the 3D printing process parameters and the parameters of the subsequent laser remelting process, so that the research on the solidification dynamics of the alloy material based on different laser remelting process parameters in a wide component space is realized.
Drawings
FIG. 1 is a photograph of a sample of a wide composition bulk alloy obtained in step (1) of example 1 and a graph showing the gradient of the NiAl content in the bulk alloy sample.
FIG. 2 is a schematic diagram of a single pass laser remelting process.
FIG. 3 is a graph of the macro-topography of example 1 after step (3) has completed three remelting passes on different sheet alloy samples.
FIG. 4 is a schematic drawing of a sample of different solidification conditions/different composition sheet alloy samples prepared in example 1.
FIG. 5 shows Al prepared in example 1 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x Typical tissue morphology maps of system materials under different coagulation conditions/different compositions.
FIG. 6 shows Al obtained in example 1 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x The coagulated structure of the system material forms a figure.
Detailed Description
The present invention is further illustrated by the following detailed description, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available from a public source without further specification.
Example 1
With Al 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x Taking a system material (x is more than or equal to 0 and less than or equal to 0.5) as an example, the method for preparing the alloy sample with high flux for the solidification kinetics research comprises the following specific steps:
(1) Two kinds of Al with high sphericity and 0.04-0.20 mm size are used 0.8 Co 1 Cr 1 Fe 1 Ni 1.8 Alloy powder and Al 1.3 Co 1 Cr 1 Fe 1 Ni 2.3 Alloy powder as a raw material for preparing an alloy sample, two kinds of alloy powders were transported by a coaxial powder feeding technique, and the transport ratio of the two kinds of alloy powders was changed in the 3D printing process in the order of 10 0.8 Co 1 Cr 1 Fe 1 Ni 1.8 To Al 1.3 Co 1 Cr 1 Fe 1 Ni 2.3 A modified wide composition bulk alloy sample, as shown in fig. 1;
the 3D printing process comprises the following parameters: the diameter of a laser spot is 3mm, the laser power is 1200W, the laser scanning speed is 720mm/min, the deposition thickness of each layer is 0.5mm, the fixed interval is 3mm, and the conveying proportion of two kinds of alloy powder is changed every 4 layers are deposited;
(2) Taking a block alloy sample from a substrate by adopting an electric spark cutting technology, cutting off a 3D printed trace on the surface of the alloy sample by electric spark wire cutting, then cutting the block alloy sample into four sheet alloy samples with the length multiplied by the width multiplied by the thickness =30 multiplied by 25 multiplied by 6mm along the direction of component change, then removing the wire cutting trace on the surface of the sheet alloy sample by using No. 240 abrasive paper, polishing, then putting the sheet alloy sample into a beaker filled with alcohol, cleaning the sheet alloy sample for 30min by using ultrasonic waves, and drying the sheet alloy sample by blowing to obtain a pretreated sheet alloy sample;
(3) Moving a laser beam on the surface of the pretreated sheet alloy sample along the direction of component change, and moving the laser beam from one end of the sheet alloy sample to the other end of the sheet alloy sample to complete laser remelting of all different components in the sheet alloy sample, namely completing primary remelting, as shown in FIG. 2; after each pass of remelting is finished, changing the technological parameters of laser remelting, carrying out next pass of remelting at different positions of the same sheet alloy sample along the direction of component change, or carrying out next pass of remelting on another sheet alloy sample along the direction of component change, correspondingly, realizing three passes of remelting in each sheet alloy sample, wherein the center distance between molten pools remelted in two adjacent passes is 8mm, so that the introduction of different solidification conditions is realized through different technological parameters of laser remelting on a plurality of sheet alloy samples, as shown in fig. 3;
the specific technological parameters of twelve-pass remelting of four sheet alloy samples are as follows: the laser power of the first pass remelting is 400W and the moving speed is 2mm/s, the laser power of the second pass remelting is 400W and the moving speed is 5mm/s, the laser power of the third pass remelting is 600W and the moving speed is 5mm/s, the laser power of the fourth pass remelting is 600W and the moving speed is 10mm/s, the laser power of the fifth pass remelting is 800W and the moving speed is 10mm/s, the laser power of the sixth pass remelting is 800W and the moving speed is 20mm/s, the laser power of the seventh pass remelting is 1000W and the moving speed is 20mm/s, the laser power of the eighth pass remelting is 1000W and the moving speed is 40mm/s, the laser power of the ninth pass remelting is 2000W and the moving speed is 10mm/s, the laser power of the tenth pass remelting is 2000W and the moving speed is 20mm/s, the laser power of the eleventh pass remelting is 2000W and the moving speed is 40mm/s, the twelfth laser power remelting is 2000W and the moving speed is 2000 mm/s, and the distance between two adjacent remelting samples is 50 mm;
(4) As shown in fig. 4, perpendicular to the direction of component change, the sheet-like alloy sample subjected to the multi-pass remelting is cut into a plurality of strip-shaped samples according to the interval of 2mm (namely the thickness of each component deposit), different strip-shaped samples have different components, and different positions of the same strip-shaped sample have different solidification structures due to different laser remelting process parameters, namely, the high-throughput preparation of the alloy sample for solidification kinetic study is realized.
When the prepared alloy sample is subjected to structural morphology characterization, the alloy sample is ground by sand paper and polished by diamond polishing solution to prepare a metallographic sample, the structural morphology is observed by an Optical Microscope (OM) and a Scanning Electron Microscope (SEM), and the actual composition of each tissue in a molten pool of a remelted sample is analyzed by an X-ray energy spectrum analyzer (XDS) arranged on the SEM equipment, so that the integrated characterization of the composition, the solidification condition and the solidification structure of a wide-composition space sample containing different solidification kinetic conditions is completed.
Alloy component tests are carried out on the wide-component blocky alloy sample prepared in the step (1) at the position of every 1mm along the height direction of the blocky alloy sample, the blocky alloy sample really has NiAl phase content gradient change, the atomic percent of the NiAl phase content of the blocky alloy sample is gradually increased from 28 percent to about 40 percent, and the prepared blocky alloy sample is proved to have the effect that the component of the blocky alloy prepared from Al is gradually increased from Al 0.8 Co 1 Cr 1 Fe 1 Ni 1.8 Change to Al 1.3 Co 1 Cr 1 Fe 1 Ni 2.3 。
And (3) performing tissue morphology observation and component test on each sample obtained in the step (4), thereby rapidly obtaining alloy solidification structures with different components/under different solidification conditions, and selecting a typical solidification structure example in the sample, as shown in fig. 5. In the laser remelted sample, the temperature gradient (G) gradually decreases from the bottom to the top of the bath, and the solidification speed V gradually increases, so that different solidification conditions exist in each bath. As shown in fig. 5, when the NiAl content is 28.9% (at.), the bottom of the molten pool is γ -plane crystal, the middle is eutectic, and the top is γ -dendrite; when the NiAl content is 29.6 percent (at.), gamma plane crystal is arranged at the bottom of a molten pool, eutectic crystal is arranged in the middle, and gamma dendrite and eutectic crystal are arranged at the top; when the NiAl content is 31.5 percent (at.), gamma plane crystal is arranged at the bottom of a molten pool, plane eutectic crystal is arranged in the middle, and cellular eutectic crystal is arranged at the top; when the NiAl content is 32 percent (at.), the bottom of a molten pool is beta dendrite, the middle is plane eutectic, and the top is cellular eutectic; when the NiAl content is 34.7 percent (at.), the bottom of the molten pool is beta-dendritic crystal and the middle isThe top is beta dendrite + eutectic; when the NiAl content is 37.6% (at.), the bottom of the molten pool is beta dendrite, the middle is eutectic, and the top is beta dendrite. The temperature gradient and the solidification speed of each characteristic structure are obtained by calculating the solidification conditions of the areas where the solidification structures exist, and the solidification structure forming graphs of the series of alloy systems are obtained, as shown in fig. 6. Thus, based on the high-throughput preparation method of the present invention, al is completed 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x The rapid establishment of alloy components, solidification conditions and solidification structures in an alloy system provides a foundation for the research on solidification dynamics of the alloy material based on different laser remelting process parameters in a wide component space.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A high-flux preparation method of an alloy sample suitable for solidification kinetics research, the method is characterized in that: the method specifically comprises the following steps:
(1) Conveying two or more than two kinds of metal powder for preparing the alloy sample by using a coaxial powder feeding technology, changing the conveying proportion of the plurality of kinds of metal powder along the deposition direction in the 3D printing process, and forming a wide-component blocky alloy sample with alloy components changing along the deposition direction on a substrate;
(2) Taking the bulk alloy sample from the substrate, and cutting the bulk alloy sample into a plurality of sheet alloy samples along the component change direction;
(3) The laser beam moves along the component change direction on the surface of the sheet alloy sample, the laser beam moves from one end of the sheet alloy sample to the other end of the sheet alloy sample to complete laser remelting of all different components in the sheet alloy sample, namely, one-pass remelting is completed, and after one-pass remelting is completed, the technological parameters of the laser remelting are changed, and the next-pass remelting is performed along the component change direction at different positions of the same sheet alloy sample or the next-pass remelting is performed along the component change direction on the other sheet alloy sample;
(4) And cutting the sheet alloy sample subjected to the multi-pass remelting into a plurality of strip-shaped samples perpendicular to the component change direction, so as to realize high-throughput preparation of the alloy sample for solidification kinetic research.
2. The method for preparing the alloy sample suitable for the solidification kinetics research in a high-throughput manner according to claim 1, wherein the method comprises the following steps: in the step (1), the metal powder is spherical powder with the grain diameter of 0.04-0.20 mm.
3. The method for preparing the alloy sample suitable for the solidification kinetics research in a high-throughput manner according to claim 1, wherein the method comprises the following steps: in the 3D printing process of the step (1), the diameter of a laser spot is 2-6 mm, the laser power is 1200-1800W, the laser scanning speed is 10-30 mm/min, the deposition thickness of each layer is 0.4-0.8 mm, and the fixed spacing between layers is 1.5-3.0 mm.
4. The method for preparing the alloy sample suitable for the solidification kinetics research in the high throughput manner according to claim 3, wherein the method comprises the following steps: the conveying proportion of various metal powders is changed every 3-8 layers are deposited.
5. The method for preparing alloy samples suitable for solidification kinetics research with high throughput according to any one of claims 1 to 4, wherein: in the remelting process in the step (3), the laser power of the laser beam is 400-2000W, and the moving speed of the laser beam is 1-50 mm/s.
6. The method for preparing the alloy sample suitable for the solidification kinetics research in a high-throughput manner according to claim 5, wherein the method comprises the following steps: the thickness of the sheet alloy sample is 1.5-2.5 times of the diameter of the laser spot in the laser remelting process, and the center distance of the molten pool of two adjacent remelting passes in the same sheet alloy sample is 2-3 times of the diameter of the laser spot in the laser remelting process.
7. The method for preparing alloy samples suitable for solidification kinetics research with high throughput according to any one of claims 1 to 4, wherein: in the step (4), the sheet-shaped alloy sample is cut into a plurality of strip-shaped samples along the deposition interface among different components in the sheet-shaped alloy sample.
8. The method for preparing alloy samples suitable for solidification kinetics research with high throughput according to any one of claims 1 to 4, wherein: for Al 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x The system material is that x is more than or equal to 0 and less than or equal to 0.5, and Al is selected 0.8 Co 1 Cr 1 Fe 1 Ni 1.8 Alloy powder and Al 1.3 Co 1 Cr 1 Fe 1 Ni 2.3 The alloy powder is used as raw material.
9. The method for preparing the alloy sample suitable for the solidification kinetics research in a high-throughput manner according to claim 8, wherein the method comprises the following steps: the conveying proportion of the two alloy powders is changed once every 3 to 5 layers of the alloy powders are deposited, and the conveying proportion of the two alloy powders is changed according to the increasing or decreasing proportion of 0.3 to 0.7at percent of Al element atoms and 0.15 to 0.35at percent of Ni element atoms.
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| 杨森, 黄卫东, 林鑫, 苏云鹏, 周尧和: "激光快速凝固条件下Al- 5.6wt% Mn合金的组织选择规律研究", 应用激光, no. 05, pages 243 - 246 * |
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