CN115142060B - High-flux preparation method of alloy sample suitable for solidification dynamics research - Google Patents
High-flux preparation method of alloy sample suitable for solidification dynamics research Download PDFInfo
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Abstract
The invention relates to a high-flux preparation method of an alloy sample suitable for solidification dynamics research, and belongs to the technical field of high-flux preparation of alloy materials. Conveying two or more metal powders by using a coaxial powder conveying 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 changed along the deposition direction on a substrate; cutting the massive alloy sample into a plurality of flaky alloy samples along the component change direction, enabling a laser beam to move on the surface of the flaky alloy sample along the component change direction to carry out laser remelting, and completing two or more remelting passes on each flaky alloy sample, wherein different laser remelting process parameters are used for different remelting passes, so that different solidification conditions are introduced; and cutting the sheet alloy subjected to multi-pass remelting into a plurality of strip-shaped samples perpendicular to the component change direction, namely realizing high-flux preparation of the alloy samples for solidification dynamics research.
Description
Technical Field
The invention relates to a high-flux preparation method of an alloy sample suitable for solidification dynamics research, and belongs to the technical field of high-flux preparation of alloy materials.
Background
In metal materials, the solidification structure of the alloy can have a great influence on the alloy performance, especially in large samples, and the solidification structure often affects the structure after final treatment due to the increasing difficulty of post-treatment, so that the control of the solidification structure is necessary in alloy preparation.
There are many factors that affect the formation of the solidification structure of an alloy, of which the composition and solidification conditions are the most critical, and changes in both the composition and solidification conditions can significantly affect the solidification structure of an alloy. For example, for eutectic alloy materials, a change in composition will cause the alloy to transition from hypoeutectic to full eutectic to hypereutectic, while at the same composition, a change in solidification conditions will cause the alloy to transition from hypoeutectic to full eutectic, so that the eutectic alloy system is a highly composition-sensitive, highly solidification condition-sensitive material.
In the conventional method, in order to realize the preparation of solidification structure samples of co-crystal alloys with different components and different solidification conditions, a large number of alloy samples with different components need to be prepared at one time, and different solidification conditions are introduced under each component, and the preparation method needs a large amount of manpower time and preparation cost. Therefore, in order to realize research on solidification kinetics of an alloy system, a method is needed to rapidly prepare samples with multiple components/solidification conditions, so as to complete construction of the component-solidification condition-structure relationship of the system.
Disclosure of Invention
Aiming at the requirement of rapid preparation of multi-component/multi-solidification condition samples in the current alloy solidification dynamics research, the invention provides a high-throughput preparation method of alloy samples suitable for solidification dynamics research, which utilizes the characteristics of layer-by-layer forming and wide forming of a laser additive manufacturing technology (3D printing technology), combines the characteristic of real-time controllability of the input proportion of various powder in coaxial powder feeding, and provides a basis for researching solidification structure forming conditions of a series of alloys by introducing laser remelting of different process conditions at different positions of the alloy samples along the component change direction on the basis of obtaining large-size wide-component massive alloy samples with alloy components changed along the deposition direction.
The aim of the invention is achieved by the following technical scheme.
The high-throughput preparation method of the alloy sample suitable for the solidification dynamics 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 used for conveying various metal powders, the conveying proportion of the various 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 block-shaped alloy sample with alloy components changed along the deposition direction is formed on a substrate;
(2) Removing the bulk alloy sample from the substrate and cutting the bulk alloy sample into a plurality of sheet alloy samples along a component variation direction;
(3) Moving a laser beam on the surface of a 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 is moved from one end of the sheet alloy sample to the other end to finish laser remelting of all different components in the sheet alloy sample, one-pass remelting is finished, after one-pass remelting is finished, the process parameters of the laser remelting are changed, the next-pass remelting is carried out at different positions of the same sheet alloy sample along the component change direction or the next-pass remelting is carried out on another sheet alloy sample along the component change direction, and different solidification conditions are introduced along the height direction of the molten pool at the same component of one laser molten pool by utilizing the difference of solidification speed and temperature gradient of the laser molten pool, so that the introduction of multiple solidification conditions is realized by the change of laser remelting processes of multiple-pass remelting on multiple sheet alloy samples;
(4) And cutting the sheet alloy sample subjected to multi-pass remelting into a plurality of strip samples perpendicular to the component change direction, wherein different strip samples have different components, and different positions of the same strip sample have different solidification structures due to different laser remelting process parameters, so that the high-throughput preparation of the alloy sample for solidification dynamics research is realized.
In the step (1), the plurality of metal powders may be a plurality of simple substance powders, a plurality of alloy powders, or a plurality of metal powders composed of simple substance powders and alloy powders. Preferably, the metal powder is spherical powder with the particle size of 0.04-0.20 mm.
In the 3D printing process of the step (1), the laser spot diameter 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 interlayer fixed interval is preferably 1.5-3.0 mm (or the interlayer lap joint rate is 50-80%).
Further, every time 3-8 layers are deposited, the conveying proportion of various metal powders is changed.
In the remelting process of 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 a laser spot in the laser remelting process, and the center-to-center distance of a molten pool 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-like alloy sample is cut into a plurality of strip-like samples along the deposition interface between different components in the sheet-like alloy sample, the number of the strip-like samples is the same as the number of component gradient changes in the sheet-like alloy sample, and the thickness of each strip-like 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) is preferably Al 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 proportion of the two alloy powders is changed every 3 to 5 layers 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% of the atomic percentage of the Al element and 0.15 to 0.35at% of the atomic percentage of the Ni element, and simultaneously the gradient change of 14.29at% to 19.70 at% of the atomic percentage of the Al element and the gradient change of 32.14at% to 34.85 at% of the atomic percentage of the Ni element are realized.
The beneficial effects are that:
(1) According to the high-throughput preparation method, the characteristics of layer-by-layer forming and wide forming by utilizing a 3D printing technology are utilized, the characteristic that the input proportion of various powder in coaxial powder feeding is controllable in real time is combined, the powder with different proportions can be used for different deposition layers, so that the change of alloy components of a sample along the deposition direction is realized, on the basis of successfully preparing a large-size alloy sample with a wide component space, the input of different solidification conditions is realized by introducing laser remelting with different process conditions along the component change direction at different positions of the alloy sample, so that the alloy sample with multiple components and multiple solidification conditions can be rapidly prepared, the rapid establishment of alloy components-solidification conditions-solidification structures is completed, the optimization of the alloy components and the process conditions is accelerated, and the manpower and material costs of alloy research and development are reduced.
(2) The good shape of the alloy sample is the precondition of controllable layering composition and subsequent laser remelting treatment, so that the process window for the good shape of the alloy sample is obtained by optimizing 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 requirements of introducing different solidification dynamics conditions are met, the operation is simple, and the applicability is strong.
(4) In the high-flux preparation method, the laser remelting process parameters with great influence on the alloy solidification structure are selected as variables for research, and the solidification dynamics research of the alloy material under different laser remelting process conditions based on a 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 the molten pool, and changing the laser power is a precondition for ensuring that samples can be melted at different laser scanning speeds, so that a large-range and controllable laser remelting process is required to be a precondition for obtaining samples with multiple solidification conditions.
(5) The sheet alloy sample cut from the large-size massive alloy sample prepared by the 3D technology cannot obtain a normal laser molten pool due to the fact that laser is molten through the sheet alloy sample if the thickness is too small, and material waste is caused due to the fact that the thickness is too large, and therefore the thickness of the sheet alloy sample is 1.5-2.5 times of the laser spot diameter. In addition, the too small interval between two adjacent remelting times on the same sheet alloy sample can cause the two molten pools to coincide together so as not to obtain a normal molten pool, and the too large interval can cause material waste, so that the center interval between the two adjacent molten pools is set to be 2-3 times of the laser spot diameter.
(6) For Al 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x The material system has great influence on solidification structure due to the Al and Ni content and the solidification condition change caused by laser remelting process parameters, and by optimizing the 3D printing process parameters and the parameters of the subsequent laser remelting process,and (3) rapidly establishing alloy components, solidification conditions and solidification structures, and realizing solidification dynamics research of the alloy material based on different laser remelting process parameters under a wide component space.
Drawings
FIG. 1 is a photograph of a sample of a wide-composition bulk alloy obtained in step (1) of example 1, showing a gradient of 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 morphology of example 1 after three remelting passes on different sheet alloy samples.
FIG. 4 is a schematic drawing showing sampling of flake alloy samples of different solidification conditions/different compositions 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 topography of the system material under different solidification conditions/different compositions.
FIG. 6 shows the Al obtained in example 1 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x The solidification structure of the system material forms a map.
Detailed Description
The present invention will be further described with reference to the following detailed description, wherein the processes are conventional, and wherein the starting materials are commercially available from the open market, unless otherwise specified.
Example 1
With 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) is taken as an example, and the specific steps of the high-flux preparation method of the alloy sample for the research of solidification dynamics are as follows:
(1) Two kinds of Al with high sphericity and particle size of 0.04-0.20 mm are adopted 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 for preparing alloy samples, the coaxial powder feeding technology is utilized to convey two alloy powders, andin the 3D printing process, the conveying proportion of the two alloy powders is changed according to the sequence of 10:0, 9:1, 8:2, 7:3, 6:4, 5:5, 4:6, 3:7, 2:8, 1:9 and 0:10 along the deposition direction, and alloy components are formed on a substrate along the deposition direction from Al 0.8 Co 1 Cr 1 Fe 1 Ni 1.8 To Al 1.3 Co 1 Cr 1 Fe 1 Ni 2.3 Modified wide component bulk alloy samples, as shown in fig. 1;
wherein, the technological parameters of 3D printing are as follows: 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 alloy powders is changed once every 4 layers are deposited;
(2) Removing a block alloy sample from a substrate by adopting an electric spark cutting technology, cutting off 3D printed traces on the surface of the alloy sample by adopting electric spark wire cutting, cutting the block alloy sample into four sheet alloy samples with length, width, thickness=30×25×6mm along the component change direction, removing the wire cutting traces on the surface of the sheet alloy sample by using 240# abrasive paper, polishing, placing into a beaker filled with alcohol, cleaning for 30min by using ultrasonic waves, and drying to obtain a pretreated sheet alloy sample;
(3) Moving a laser beam on the surface of the pretreated sheet alloy sample along the component change direction, and moving the laser beam from one end of the sheet alloy sample to the other end to finish laser remelting of all different components in the sheet alloy sample, namely finishing one-time remelting, as shown in fig. 2; after one pass of remelting is completed, changing the technological parameters of laser remelting, carrying out next pass of remelting along the component change direction at different positions of the same sheet alloy sample, or carrying out next pass of remelting along the component change direction on another sheet alloy sample, correspondingly, realizing three passes of remelting in each sheet alloy sample, wherein the center-to-center distance of a molten pool for two adjacent passes of remelting is 8mm, thereby realizing the introduction of different solidification conditions through different laser remelting technological parameters of multiple passes of remelting on a plurality of sheet alloy samples, as shown in figure 3;
the specific process parameters for twelve remelting passes on the four sheet alloy samples were 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 20mm/s, the laser power of the eleventh pass remelting is 2000W and the moving speed is 40mm/s, the laser power of the twelfth pass remelting is 2000W and the moving speed is 20mm/s, and the laser power of the twelfth pass remelting is 2000W and the moving speed is 50mm/s, wherein the laser power of the eighth pass remelting is 50mm/s and the same in the sample of two adjacent sheet-like;
(4) As shown in fig. 4, the sheet alloy sample subjected to the multi-pass remelting was cut into a plurality of strip samples at intervals of 2mm (i.e., the thickness of each component deposited) perpendicular to the direction of the component change, different strip samples having different components, and different positions of the same strip sample having different solidification structures due to the difference in laser remelting process parameters, i.e., high-throughput preparation of the alloy sample for solidification kinetics study was achieved.
When the prepared alloy sample is subjected to structure morphology characterization, the alloy sample is polished by sand paper and diamond polishing liquid to prepare a metallographic sample, the structure morphology is observed by an Optical Microscope (OM) and a Scanning Electron Microscope (SEM), the actual composition of each structure in a molten pool of the remelted sample is analyzed by an X-ray energy spectrum analyzer (XDS) equipped by SEM equipment, and the composition-solidification condition-solidification structure integrated characterization of the wide-composition spatial sample containing different solidification dynamics conditions is completed.
The wide-component block alloy sample prepared in the step (1) is subjected to alloy component tests at every 1mm interval along the height direction,the bulk alloy sample does have the NiAl phase content gradient change, and the atomic percentage of the NiAl phase content is gradually increased from 28 percent to about 40 percent, which proves that the prepared bulk alloy component is 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) carrying out structural morphology observation and composition testing on each sample obtained in the step (4), thereby rapidly obtaining alloy solidification structures under different compositions/different solidification conditions, and selecting a typical solidification structure example in the sample, as shown in fig. 5. In the laser remelting sample, the temperature gradient (G) gradually decreases from the bottom to the top of the melt pool, and the solidification speed V gradually increases, so that different solidification conditions exist in each melt pool. As shown in FIG. 5, when the NiAl content is 28.9% (at.), the bottom of the molten pool is gamma plane crystal, the middle is eutectic, and the top is gamma dendrite; when the content of NiAl is 29.6 percent (at.), the bottom of the molten pool is gamma plane crystal, the middle is eutectic, and the top is gamma dendrite+eutectic; when the NiAl content is 31.5 percent (at.), the bottom of the molten pool is gamma plane crystal, the middle is plane eutectic, and the top is cellular eutectic; when the NiAl content is 32% (at.), beta dendrite is arranged at the bottom of the molten pool, planar eutectic is arranged in the middle, and cellular eutectic is arranged at the top of the molten pool; when the NiAl content is 34.7 percent (at.), beta dendrites are arranged at the bottom of the molten pool, eutectic is arranged in the middle of the molten pool, and beta dendrites and eutectic are arranged at the top of the molten pool; 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. By calculating the solidification conditions of the areas where the solidification structures exist, the temperature gradient and solidification speed of each characteristic structure are obtained, and a solidification structure formation diagram of the series of alloy systems is obtained, as shown in fig. 6. Therefore, based on the high-throughput preparation method of the invention, al is completed 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x The rapid establishment of alloy composition-solidification condition-solidification structure in an alloy system provides a foundation for the solidification dynamics research of the alloy material based on different laser remelting process parameters under a wide composition space.
In summary, the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A high-throughput preparation method of an alloy sample suitable for solidification dynamics research is characterized by comprising the following steps of: the method specifically comprises the following steps:
(1) Conveying two or more metal powders for preparing alloy samples by using a coaxial powder conveying technology, depositing 3-8 layers along the deposition direction in the 3D printing process, gradually increasing or gradually decreasing the conveying proportion of a plurality of metal powders, and forming a wide-component blocky alloy sample with alloy components changed along the deposition direction on a substrate;
(2) Removing the bulk alloy sample from the substrate and cutting the bulk alloy sample into a plurality of sheet alloy samples along a component variation direction;
(3) Moving a laser beam on the surface of a sheet alloy sample along the component change direction, wherein the laser beam is moved from one end of the sheet alloy sample to the other end to finish laser remelting of all different components in the sheet alloy sample, namely finishing one-pass remelting, changing the technological parameters of laser remelting after finishing one-pass remelting, and carrying out next-pass remelting on different positions of the same sheet alloy sample along the component change direction or carrying out next-pass remelting on another sheet alloy sample along the component change direction;
in the remelting process of 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;
the thickness of the sheet alloy sample is 1.5-2.5 times of the diameter of a laser spot in the laser remelting process, and the center-to-center distance of a molten pool remelted in two adjacent passes in the same sheet alloy sample is 2-3 times of the diameter of the laser spot in the laser remelting process;
(4) And cutting the sheet alloy sample subjected to multi-pass remelting into a plurality of strip-shaped samples perpendicular to the component change direction, namely realizing high-flux preparation of the alloy sample for solidification dynamics research.
2. The method for high-throughput preparation of alloy samples suitable for coagulation kinetics studies as recited in claim 1, wherein: in the step (1), spherical powder with the particle size of 0.04-0.20 mm is selected as the metal powder.
3. The method for high-throughput preparation of alloy samples suitable for coagulation kinetics studies as recited in claim 1, wherein: in the 3D printing process of the step (1), the laser spot diameter 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 interlayer fixed interval is 1.5-3.0 mm.
4. A method of high throughput preparation of alloy samples for use in solidification kinetics studies in accordance with any one of claims 1 to 3, wherein: in step (4), the sheet alloy sample is cut into a plurality of elongated samples along a deposition interface between the different components in the sample.
5. A method of high throughput preparation of alloy samples for use in solidification kinetics studies in accordance with any one of claims 1 to 3, wherein: for Al 0.8+x Co 1 Cr 1 Fe 1 Ni 1.8+x The system material is 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 Alloy powder is used as a raw material.
6. The method for high-throughput preparation of alloy samples for coagulation kinetics study as recited in claim 5, wherein the method comprises the steps of: the conveying proportion of the two alloy powders is changed once every 3-5 layers are deposited, and the conveying proportion of the two alloy powders is changed according to the increasing or decreasing proportion of 0.3-0.7at% of Al element and 0.15-0.35at% of Ni element.
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