CN112666335A - Method for representing performance of high-flux molybdenum alloy multi-scale micro-area - Google Patents
Method for representing performance of high-flux molybdenum alloy multi-scale micro-area Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 28
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 80
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Abstract
The invention discloses a method for representing the performance of a high-flux molybdenum alloy multi-scale micro-area, which comprises the steps of dividing a molybdenum alloy prepared in a high-flux mode into a pure section and a transition section, equally dividing the transition section into a plurality of small areas according to obvious component change of the component transition section, carrying out multi-scale representation on the molybdenum alloy micro-area shape, the micro-area corrosion potential, the micro-area hardness and the micro-area components, and establishing the relationship between lanthanum oxide content-molybdenum alloy grain size-corrosion resistance-hardness. According to the method, a large amount of molybdenum alloy data are obtained by using a small sample and are used for constructing and optimizing a machine learning model, and the high-throughput characterization of the molybdenum alloy is realized by combining a high-throughput experiment and a test means commonly used in a laboratory in a multi-scale manner.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and relates to a method for representing the performance of a high-flux molybdenum alloy multi-scale micro-area.
Background
Molybdenum is a rare refractory metal, has high melting point and elastic modulus, good electric and heat conducting performance, low thermal expansion coefficient, and good acid and alkali resistance and liquid metal corrosion resistance, is widely applied to various fields such as aerospace, mechanical manufacturing, power electronics, ferrous metallurgy, medical appliances, illumination, energy chemical industry, military industry and the like, and is an indispensable high-temperature-resistant material. With the development of science and technology, particularly the demand of national defense is higher and higher, higher requirements are put forward on the comprehensive performance of the molybdenum alloy.
However, research and development of materials are a long process, the traditional research and development method of new materials is a trial and error method, and scientific researchers determine the composition of the material components based on own knowledge and relevant experience accumulation. Reviewing the development and application history of the entire industrial technology and materials, the development of new generation materials generally requires a considerable amount of time. Therefore, shortening the period from research and development to application of materials, accelerating the research and development speed of materials, and reducing the research and development cost of materials become important for research in various countries.
In the process of high-throughput preparation and research and development of the metal matrix composite, a high-throughput characterization technology is required to rapidly detect the components, the morphology, the tissue, the performance and the interface of a large number of samples prepared by the high-throughput technology, and the detection result is used for reverse optimization of the high-throughput technology and rapid screening of a conforming system. The rapid, accurate and low-cost acquisition of material information is an important standard for measuring high-throughput characterization technology of materials.
Because the components of the metal matrix composite are more complex than metals, in the aspect of characterization technology, a multi-dimensional, multi-field and multi-scale synchronous acquisition technology aiming at the components, the shapes, the tissues, the structures and the performances of a single sample of the metal matrix composite and a rapid characterization technology aiming at the components, the shapes, the tissues and the structures of an array sample are still lacked.
At present, few reports on the performance characterization of the molybdenum alloy material micro-area are reported, and in order to realize the multi-dimensional and multi-scale characterization of the performance of the molybdenum alloy, a method for multi-scale characterization of the performance of the high-flux molybdenum alloy micro-area is provided.
Disclosure of Invention
The invention aims to provide a method for representing the performance of a high-flux molybdenum alloy multi-scale micro-area, which is used for carrying out multi-scale performance test analysis such as microstructure-component-corrosion resistance-hardness on molybdenum alloy component transition areas with different fixed components prepared by high flux. The method realizes the high-throughput characterization of the molybdenum alloy by combining the common test means in the laboratory in a multi-scale manner, and has the advantages of short test period, convenient experiment and low cost.
The invention is realized by the following technical scheme:
the invention provides a method for representing the performance of a high-flux molybdenum alloy multi-scale micro-area, which comprises the following steps:
preparing molybdenum alloy rods doped with rare earth metal oxides with different mass fractions by a powder metallurgy solid-liquid doping mode, preparing molybdenum powder doped with the rare earth metal oxides with different mass fractions into a molybdenum rod in a component gradient mode, and taking a component transition region formed between two different components as a strip sample;
polishing the surface of the strip sample of the component transition area obtained in the step 1, removing surface scratches, and corroding the surface by using a molybdenum alloy corrosive liquid;
the surface of the molybdenum strip is uniformly divided into a plurality of small square areas with the size of 1 multiplied by 1mm, the small areas on the surface of the sample are scanned by using an electron microscope and an electron energy spectrum, and molybdenum alloy microstructures with different doping components and the contents of rare earth metal oxides in different areas are obtained by respectively photographing;
counting the sizes of the crystal grains in different areas, and establishing a relation between the content of the rare earth metal oxide and the size of the crystal grains of the molybdenum alloy;
step 3, representing the corrosion resistance of the high-flux molybdenum alloy micro-area:
polishing the surface of the strip sample of the component transition area obtained in the step 1, removing surface scratches, and scanning the surface of the sample by using a scanning Kelvin probe measurement method to obtain a change data point of the metal surface potential;
equally dividing the surface of the sample into a plurality of units by taking 1 x 1mm as a unit, and calculating the average potential value of each unit; corresponding the corrosion resistance data of the surface of the sample with the content of the rare earth metal oxide and the size of the molybdenum alloy crystal grain in the step 2, and establishing a relation between the content of the rare earth metal oxide, the size of the molybdenum alloy crystal grain and the corrosion resistance;
step 4, representing the hardness of the high-flux molybdenum alloy micro-area:
polishing the surface of the strip sample in the component transition area obtained in the step (1), removing surface scratches, equally dividing the surface of the molybdenum strip into a plurality of small square areas of 1 multiplied by 1mm, and testing the surface hardness of the sample by using a Vickers hardness tester with the set pressure value of 300g and the indentation time of 15 s;
taking more than 3 points for testing in each small area, and taking the average value as the hardness value of the area; the hardness value is in one-to-one correspondence with the rare earth metal oxide components, grain size and corrosion resistance, and the relationship between the content of the rare earth metal oxide, the grain size of the molybdenum alloy, the corrosion resistance and the hardness is established;
and (3) corresponding the data points of the characteristics of the content of the rare earth metal oxide, the grain size of the molybdenum alloy, the corrosion resistance and the hardness, which are measured in the steps, one by one, and expanding the data points into a multi-scale performance database of the rare earth molybdenum alloy by means of machine learning.
Preferably, the rare earth metal oxide is lanthanum oxide or cerium oxide.
Preferably, the molybdenum alloy corrosive liquid is prepared from 10% of potassium ferricyanide and 10% of sodium hydroxide in percentage by mass.
Preferably, in the step 2, the surface of the sample is corroded for 40-60s at room temperature.
Preferably, the scanning kelvin probe measurement method scans the sample surface with a step size of 0.1mm, i.e. a potential value is taken every 0.1 mm.
Preferably, the mass fraction of the rare earth metal oxide in a composition transition region formed between different compositions is distributed in a way that the content is gradually increased from low to high or gradually decreased from high to low, and the multi-scale performance corresponding to each region is changed.
Preferably, the relationship between the rare earth metal oxide content and the grain size of the molybdenum alloy is such that the grain size of the molybdenum alloy decreases with increasing rare earth metal oxide content.
Preferably, the relationship between the content of the rare earth metal oxide and the size of the molybdenum alloy crystal grains and the corrosion resistance is that as the content of the rare earth metal oxide increases, the size of the molybdenum alloy crystal grains decreases and the corrosion resistance increases.
Preferably, the relationship between the content of the rare earth metal oxide-the grain size of the molybdenum alloy-the corrosion resistance-the hardness is that as the content of the rare earth metal oxide increases, the grain size decreases, the corrosion resistance increases and the hardness increases.
The invention has the following technical effects:
1) the invention prepares molybdenum alloy with different component gradients by utilizing high flux so as to obtain transition zone samples with different components, and can obtain samples with doping component contents which are uniformly changed in a single direction by a single doping mode.
2) The high-throughput experiment is combined with a multi-scale characterization means, a large amount of molybdenum alloy multi-scale performance data is obtained by using a small sample, a plurality of groups of multi-scale data can be obtained by using one sample, the manufacturing cost of a large amount of alloy materials can be saved, and a large amount of data can be obtained by using a small amount of samples.
3) The multi-scale synchronous representation of the components, the morphology, the performance and the like of the molybdenum alloy is realized, and the obtained data is utilized to establish the relation of the performance characteristics of all dimensions of the molybdenum alloy by a machine learning method, so that the research and development efficiency of the high-performance molybdenum alloy is greatly improved.
Drawings
FIGS. 1a-1b are schematic diagrams of the distribution of the components and the transition zone of the components of the molybdenum alloy of the present invention;
FIG. 2 is a sample processing shape during characterization;
FIG. 3 is a schematic representation of a sample micro-characterization zone;
FIG. 4 is a diagram showing lanthanum oxide content versus grain size;
FIG. 5 is a diagram showing lanthanum oxide content-size-potential;
fig. 6 is a diagram showing lanthanum oxide content-hardness-potential.
Detailed Description
The present invention is further described below in conjunction with the following embodiments and the accompanying drawings, it being understood that the drawings and the following embodiments are illustrative of the invention only and are not limiting.
The invention provides a method for representing the performance of a high-flux molybdenum alloy multi-scale micro-area, which comprises the following steps:
a batch of molybdenum alloy rods doped with rare earth metal oxides (lanthanum oxide or cerium oxide) with different mass fractions are prepared in a powder metallurgy solid-liquid doping mode, and in the preparation process, molybdenum powder doped with lanthanum oxide or cerium oxide with different mass fractions is placed in the same mold in a component gradient mode to prepare a molybdenum rod, and particularly, the molybdenum rod is shown in figure 1 a. Due to the stacking of different components, the components of each section of the molybdenum rod are changed in a gradient manner, a component transition area is necessarily formed between two different components, and samples of the two component transition areas are taken, as shown in fig. 1 b. To facilitate the subsequent process characterization of the samples, the samples were processed into strip samples as shown in fig. 2.
The molybdenum alloy used for testing is prepared by a high-flux powder metallurgy solid-liquid doping mode, molybdenum powder with different doping components is placed into the same die once and then subjected to isostatic pressing to obtain the molybdenum alloy with different components and transition regions, and because the powder with different components is mutually permeated to form the component transition regions, the mass fraction of lanthanum oxide or cerium oxide in the region has the distribution condition that the content is gradually increased from low to high or gradually decreased from high to low. Due to the characteristic that the components are uniformly changed, the multi-scale performance corresponding to each area is changed, which is the key for the feasibility of the characterization method.
and (2) polishing the surface of the sample obtained in the step (1) by using sand paper and a polishing machine to remove surface scratches, and corroding the surface of the sample for 40-60s at room temperature by using molybdenum alloy corrosive liquid prepared from 10 mass percent of potassium ferricyanide and sodium hydroxide.
In one embodiment, the 7mm by 20mm molybdenum strip surface is evenly divided into 140 small square areas of 1mm by 1mm as shown in FIG. 3. 140 small areas on the surface of the SEM + EDS (scanning electron microscope + electron energy spectrum) sample are respectively photographed and subjected to component analysis, and the microstructure of the molybdenum alloy with different doping components and the content of doped lanthanum oxide or cerium oxide in 140 different areas are obtained. Observing the microstructure of different areas, and counting the grain sizes of the different areas, thereby establishing the relationship between the content of lanthanum oxide or cerium oxide and the grain size of the molybdenum alloy, and reducing the grain size of the molybdenum alloy along with the increase of the content of lanthanum oxide or cerium oxide.
The size of the transition zone and the equally divided small area of x 1mm are only used for illustration of the method, and the size in the specific implementation process is determined by the size of the sample intercepted by the transition into segments and the actual experimental requirements.
Step 3, representing the corrosion resistance of the high-flux molybdenum alloy micro-area:
and (3) polishing the surface of the sample by using sand paper and a polishing machine, removing surface scratches, and scanning the surface of the sample by using SKP (scanning Kelvin probe measurement technology), wherein the scanning step length is 0.1mm, namely, a potential value is taken every 0.1 mm. A model graph of the change in metal surface potential and data points were obtained, as shown in FIG. 4. The data was processed, divided into 140 cells in units of 1mm × 1mm, and the average potential value was calculated for each cell. And (3) corresponding the corrosion resistance data of the surface of the sample with the content of lanthanum oxide or cerium oxide and the grain size of the molybdenum alloy in the step (2), and establishing a relation between the content of lanthanum oxide or cerium oxide-the grain size of the molybdenum alloy-corrosion resistance, wherein the grain size of the molybdenum alloy is reduced and the corrosion resistance is enhanced along with the increase of the content of lanthanum oxide or cerium oxide.
Step 4, representing the hardness of the high-flux molybdenum alloy micro-area:
the surface of the sample was polished by sandpaper and a polishing machine to remove scratches on the surface, and the surface of the sample was divided into 140 small areas of 1mm × 1 mm. The surface hardness of the sample was measured with a Vickers hardness tester, set at a pressure value of 300g, and an indentation time of 15 seconds. In order to reduce the error, 3 to 5 points are taken for each small area to be tested, and the average value is taken to be the hardness value of the point. And (3) counting the hardness values of 140 micro-areas, drawing a three-dimensional graph as shown in fig. 5, and carrying out one-to-one correspondence between the hardness values and the lanthanum oxide or cerium oxide components, the grain size and the corrosion resistance to establish the relationship between the lanthanum oxide or cerium oxide content, the molybdenum alloy grain size, the corrosion resistance and the hardness, wherein the grain size is reduced, the corrosion resistance is enhanced and the hardness is increased along with the increase of the lanthanum oxide content.
and (3) correspondingly setting 140 data points of the characteristics of the molybdenum alloy grain size, the second phase distribution, the lanthanum oxide component, the corrosion potential and the hardness, which are measured in the steps, one by one, and expanding the data points into a rare earth molybdenum alloy multi-scale performance database by means of machine learning.
The following different examples are given to further illustrate the invention.
Example 1
The molybdenum alloy used in this embodiment is a lanthanum oxide-doped molybdenum alloy prepared in a high-throughput manner, wherein a molybdenum alloy sample and a lanthanum oxide doping content are schematically shown in fig. 1a, the molybdenum alloy prepared in a high-throughput powder metallurgy manner is shown in the figure, the mass fraction of lanthanum oxide in the alloy changes in a stepwise increase from 0% to 0.9%, a light-color part in the figure is a lanthanum oxide component pure region, and a dark-color region is a lanthanum oxide component transition region. The present embodiment selects the composition transition section with the lanthanum oxide doping quality fraction of 0.3% -0.4%, as shown in figure 1b # 1.
(1) Characterization of high-flux molybdenum-lanthanum alloy micro-area micro-morphology and components
1) For convenience of experiment, the figure 1b
The bar sample of about 20mm in length was processed into a long sample of 20 mm. times.7 mm. times.4 mm, as shown in FIG. 2. The surface of a 7mm by 20mm molybdenum bar was equally divided into 140 small square areas of 1mm by 1mm as shown in figure 3.
2) And (3) polishing the surface of the sample by using sand paper and a polishing machine, removing surface scratches, corroding the surface by using a molybdenum alloy corrosive liquid prepared from 10 mass percent of potassium ferricyanide and sodium hydroxide, and corroding for 50s at room temperature.
3) 140 small areas on the surface of the SEM + EDS (scanning electron microscope + electron energy spectrum) sample are respectively used for photographing and component analysis, and the microstructure of the molybdenum alloy with different doping components and the content of doped lanthanum oxide in 140 different areas are obtained. Observing the microstructure of different areas, and counting the grain sizes of the different areas so as to establish the relationship between the lanthanum oxide content and the molybdenum alloy grain size, wherein FIG. 4 is a schematic diagram showing the change of the grain size along with the lanthanum oxide content.
(2) Molybdenum lanthanum alloy micro-area electrochemical characterization
And (3) polishing the surface of the sample by using sand paper and a polishing machine, removing surface scratches, and scanning the surface of the sample by using SKP (scanning Kelvin probe measurement technology) to obtain a change data point of the metal surface potential. The data was processed, divided into 140 cells in units of 1mm × 1mm, and the average potential value was calculated for each cell. And (3) corresponding the corrosion data with the components and the grain data in the step (2) to establish a relationship between the components, grain size and corrosion resistance, and FIG. 5 is a schematic diagram showing the change of the grain size and the corrosion potential along with the lanthanum oxide content.
(3) Hardness characterization of molybdenum-lanthanum alloy micro-region
The surface of the sample was polished by sandpaper and a polishing machine to remove scratches on the surface, and the surface of the sample was divided into 140 small areas of 1mm × 1 mm. The surface hardness of the sample was measured with a Vickers hardness tester, set at a pressure value of 300g, and an indentation time of 15 seconds. In order to reduce the error, 3 to 5 points are taken for each small area to be tested, and the average value is taken to be the hardness value of the point. And (3) counting the hardness values of 140 micro-areas, drawing a three-dimensional graph as shown in fig. 5, and establishing a relationship between the hardness values and the lanthanum oxide components, namely grain size and corrosion resistance, and the relationship between the components, namely grain size, corrosion resistance and hardness, wherein fig. 6 is a schematic diagram of the change of the molybdenum alloy hardness and the corrosion potential along with the lanthanum oxide content.
(4) Sorting data to build database
And (3) correspondingly setting 140 data points of the characteristics of the molybdenum alloy grain size, the second phase distribution, the lanthanum oxide component, the corrosion potential and the hardness, which are measured in the steps, one by one, and expanding the data points into a rare earth molybdenum alloy multi-scale performance database by means of machine learning.
Example 2
The molybdenum alloy used in this embodiment is a lanthanum oxide-doped molybdenum alloy prepared in a high-throughput manner, wherein a molybdenum alloy sample and a lanthanum oxide doping content are schematically shown in fig. 1a, the molybdenum alloy prepared in a high-throughput powder metallurgy manner is shown in the figure, the mass fraction of lanthanum oxide in the alloy changes in a stepwise increase from 0% to 0.9%, a light-color part in the figure is a lanthanum oxide component pure region, and a dark-color region is a lanthanum oxide component transition region. The present embodiment selects the composition transition section with the lanthanum oxide doping quality fraction of 0.5% -0.6%, as shown in figure 1b # 2.
(1) Characterization of high-flux molybdenum-lanthanum alloy micro-area micro-morphology and components
1) For convenience of experiment, the following FIG. 1
The bar sample of about 20mm in length was processed into a long sample of 20 mm. times.7 mm. times.4 mm, as shown in FIG. 2. The surface of a 7mm by 20mm molybdenum bar was equally divided into 140 small square areas of 1mm by 1mm as shown in figure 3.
2) And (3) polishing the surface of the sample by using sand paper and a polishing machine, removing scratches on the surface, corroding the surface by using a molybdenum alloy corrosion solution prepared from 10% of potassium ferricyanide and 10% of sodium hydroxide in percentage by mass, and corroding the surface for 60s at room temperature.
3) 140 small areas on the surface of the SEM + EDS (scanning electron microscope + electron energy spectrum) sample are respectively used for photographing and component analysis, and the microstructure of the molybdenum alloy with different doping components and the content of doped lanthanum oxide in 140 different areas are obtained. And observing the microstructures of different areas, and counting the grain sizes of the different areas and the distribution condition of the second phase particles, thereby establishing the relationship between the lanthanum oxide content and the grain sizes of the molybdenum alloy and the distribution condition of the second phase particles.
(2) Molybdenum lanthanum alloy micro-area electrochemical characterization
And (3) polishing the surface of the sample by using sand paper and a polishing machine, removing surface scratches, and scanning the surface of the sample by using SKP (scanning Kelvin probe measurement technology) to obtain a change model diagram and data points of the metal surface potential. The data was processed, divided into 140 cells in units of 1mm × 1mm, and the average potential value was calculated for each cell. And (3) corresponding the corrosion data with the components and the crystal grain data in the step (2) to establish the relationship between the components, the crystal grain size and the corrosion resistance.
(3) Hardness characterization of molybdenum-lanthanum alloy micro-region
The surface of the sample was polished by sandpaper and a polishing machine to remove scratches on the surface, and the surface of the sample was divided into 140 small areas of 1mm × 1 mm. The surface hardness of the sample was measured with a Vickers hardness tester, set at a pressure value of 300g, and an indentation time of 15 seconds. In order to reduce the error, 3 to 5 points are taken for each small area to be tested, and the average value is taken to be the hardness value of the point. And (3) counting the hardness values of 140 micro-areas, and corresponding the hardness values to the lanthanum oxide components, the grain sizes and the corrosion resistance one by one to establish the relationship between the components, the grain sizes, the corrosion resistance and the hardness.
(4) Sorting data to build database
And (3) correspondingly setting 140 data points of the characteristics of the molybdenum alloy grain size, the second phase distribution, the lanthanum oxide component, the corrosion potential and the hardness, which are measured in the steps, one by one, and expanding the data points into a rare earth molybdenum alloy multi-scale performance database by means of machine learning.
Example 3
The molybdenum alloy used in this example is a cerium oxide-doped molybdenum alloy prepared in a high-throughput manner, and the mass fraction of cerium oxide in the alloy changes in a stepwise increase from 0% to 0.9%. In this embodiment, the transition section of the composition with the doping weight fraction of cerium oxide of 0.5% -0.6% is selected.
(1) Characterization of high-flux molybdenum alloy micro-area micro-morphology and components
1) For convenience of experiment, the following FIG. 1
The bar sample of about 20mm in length was processed into a long sample of 20 mm. times.7 mm. times.4 mm, as shown in FIG. 2. The surface of a 7mm by 20mm molybdenum bar was equally divided into 140 small square areas of 1mm by 1mm as shown in figure 3.
2) And (3) polishing the surface of the sample by using sand paper and a polishing machine, removing surface scratches, corroding the surface by using a molybdenum alloy corrosive liquid prepared from 10 mass percent of potassium ferricyanide and sodium hydroxide for 40s at room temperature.
3) 140 small areas on the surface of the SEM + EDS (scanning electron microscope + electron energy spectrum) sample are respectively photographed and subjected to component analysis, so that the microstructure of the molybdenum alloy with different doping components and the content of doped cerium oxide in 140 different areas are obtained. And observing the microstructures of different areas, and counting the grain sizes of the different areas and the distribution condition of the second phase particles, thereby establishing the relationship between the content of the cerium oxide and the grain sizes of the molybdenum alloy and the distribution condition of the second phase particles.
(2) Molybdenum cerium alloy micro-area electrochemical characterization
And (3) polishing the surface of the sample by using sand paper and a polishing machine, removing surface scratches, and scanning the surface of the sample by using SKP (scanning Kelvin probe measurement technology) to obtain a change model diagram and data points of the metal surface potential. The data was processed, divided into 140 cells in units of 1mm × 1mm, and the average potential value was calculated for each cell. And (3) corresponding the corrosion data with the components and the crystal grain data in the step (2) to establish the relationship between the components, the crystal grain size and the corrosion resistance.
(3) Molybdenum cerium alloy micro-zone hardness characterization
The surface of the sample was polished by sandpaper and a polishing machine to remove scratches on the surface, and the surface of the sample was divided into 140 small areas of 1mm × 1 mm. The hardness of the sample surface was measured with a Vickers hardness tester, set at a pressure value of 300g, and an indentation time of 15 seconds. In order to reduce the error, 3 to 5 points are taken for each small area to be tested, and the average value is taken to be the hardness value of the point. And (3) counting the hardness values of 140 micro-areas, and corresponding the hardness values to the cerium oxide components, the grain sizes and the corrosion resistance one by one to establish the relationship between the components, the grain sizes, the corrosion resistance and the hardness.
(4) Sorting data to build database
And (3) correspondingly setting 140 data points of the characteristics of the molybdenum alloy grain size, the second phase distribution, the cerium oxide component, the corrosion potential and the hardness, which are measured in the steps, one by one, and expanding the data points into a rare earth molybdenum alloy multi-scale performance database by means of machine learning.
From the above embodiments, it can be seen that, by adopting the method of the present invention, for the component transition sections with different rare earth metal oxide doping impurity amount fractions, the corresponding relationship of the grain size, the corrosion potential and the molybdenum alloy hardness along with the change of the rare earth metal oxide content can be obtained, and the method is expanded into a rare earth molybdenum alloy multi-scale performance database by means of machine learning, so as to realize the multi-dimensional multi-scale characterization of the molybdenum alloy performance, thereby providing an effective method with convenient experiment and low cost for the research and development of high-performance molybdenum alloy.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (9)
1. A method for characterizing the performance of a high-flux molybdenum alloy in a multi-scale micro-area is characterized by comprising the following steps:
step 1, preparing a high-flux molybdenum alloy:
preparing molybdenum alloy rods doped with rare earth metal oxides with different mass fractions by a powder metallurgy solid-liquid doping mode, preparing molybdenum powder doped with the rare earth metal oxides with different mass fractions into a molybdenum rod in a component gradient mode, and taking a component transition region formed between two different components as a strip sample;
step 2, representing the microstructure and the components of the surface of the high-flux molybdenum alloy:
polishing the surface of the strip sample of the component transition area obtained in the step 1, removing surface scratches, and corroding the surface by using a molybdenum alloy corrosive liquid;
the surface of the molybdenum strip is uniformly divided into a plurality of small square areas with the size of 1 multiplied by 1mm, the small areas on the surface of the sample are scanned by using an electron microscope and an electron energy spectrum, and molybdenum alloy microstructures with different doping components and the contents of rare earth metal oxides in different areas are obtained by respectively photographing;
counting the sizes of the crystal grains in different areas, and establishing a relation between the content of the rare earth metal oxide and the size of the crystal grains of the molybdenum alloy;
step 3, representing the corrosion resistance of the high-flux molybdenum alloy micro-area:
polishing the surface of the strip sample of the component transition area obtained in the step 1, removing surface scratches, and scanning the surface of the sample by using a scanning Kelvin probe measurement method to obtain a change data point of the metal surface potential;
equally dividing the surface of the sample into a plurality of units by taking 1 x 1mm as a unit, and calculating the average potential value of each unit; corresponding the corrosion resistance data of the surface of the sample with the content of the rare earth metal oxide and the size of the molybdenum alloy crystal grain in the step 2, and establishing a relation between the content of the rare earth metal oxide, the size of the molybdenum alloy crystal grain and the corrosion resistance;
step 4, representing the hardness of the high-flux molybdenum alloy micro-area:
polishing the surface of the strip sample in the component transition area obtained in the step (1), removing surface scratches, equally dividing the surface of the molybdenum strip into a plurality of small square areas of 1 multiplied by 1mm, and testing the surface hardness of the sample by using a Vickers hardness tester with the set pressure value of 300g and the indentation time of 15 s;
taking more than 3 points for testing in each small area, and taking the average value as the hardness value of the area; the hardness value is in one-to-one correspondence with the rare earth metal oxide components, grain size and corrosion resistance, and the relationship between the content of the rare earth metal oxide, the grain size of the molybdenum alloy, the corrosion resistance and the hardness is established;
step 5, sorting data and establishing a database:
and (3) corresponding the data points of the characteristics of the content of the rare earth metal oxide, the grain size of the molybdenum alloy, the corrosion resistance and the hardness, which are measured in the steps, one by one, and expanding the data points into a multi-scale performance database of the rare earth molybdenum alloy by means of machine learning.
2. The method for characterizing the multi-scale micro-domain properties of high throughput molybdenum alloys of claim 1, wherein said rare earth metal oxide is lanthanum oxide or cerium oxide.
3. The method for characterizing the multi-scale micro-domain performance of a high-throughput molybdenum alloy according to claim 1, wherein the molybdenum alloy etching solution is prepared from 10% by mass of potassium ferricyanide and 10% by mass of sodium hydroxide.
4. The method for characterizing the multi-scale micro-domain performance of the high-throughput molybdenum alloy according to claim 1, wherein in the step 2, the surface of the sample is corroded for 40-60s at room temperature.
5. The method for characterizing the multi-scale micro-domain properties of the high-throughput molybdenum alloy according to claim 1, wherein the scanning Kelvin probe measurement method scans the surface of the sample with a step size of 0.1mm, i.e. a potential value is taken every 0.1 mm.
6. The method for characterizing the multi-scale micro-region performance of the high-throughput molybdenum alloy according to claim 1, wherein the mass fraction of the rare earth metal oxide in a composition transition region formed between different compositions has a distribution that the content increases from low to high or decreases from high to low, and the multi-scale performance corresponding to each region changes accordingly.
7. The method for characterizing the multi-scale micro-domain properties of a high throughput molybdenum alloy of claim 6, wherein the rare earth oxide content-molybdenum alloy grain size relationship is such that the molybdenum alloy grain size decreases with increasing rare earth oxide content.
8. The method for characterizing the multi-scale micro-domain properties of a high throughput molybdenum alloy of claim 6, wherein the relationship between rare earth oxide content-molybdenum alloy grain size-corrosion resistance is such that as the rare earth oxide content increases, the molybdenum alloy grain size decreases and the corrosion resistance increases.
9. The method of characterizing multi-scale micro-domain properties of a high-throughput molybdenum alloy of claim 6, wherein the relationship between rare earth metal oxide content-molybdenum alloy grain size-corrosion resistance-hardness is such that as rare earth metal oxide content increases, grain size decreases, corrosion resistance increases, and hardness increases.
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