CN110564984A - Sample control preparation method for casting aluminum-silicon alloy - Google Patents
Sample control preparation method for casting aluminum-silicon alloy Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/043—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with silicon as the next major constituent
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a sample control preparation method for casting aluminum-silicon alloy, which comprises the following steps: s1, designing the components of the aluminum alloy; s2, smelting and casting: adding furnace burden into a crucible resistance furnace according to the proportion, smelting and refining, and pouring a preparation control sample into a water-cooled copper mold after measuring the hydrogen content and the components to be qualified; s3, analysis and inspection: after inspecting the macrostructure, the microstructure and the fracture tissue, selecting qualified sample control for initial inspection, sawing, and peeling the surface; s4, after homogenization treatment, component uniformity and stability analysis are carried out, and a control sample is subjected to value setting; and S5, carrying out finish turning on the surface of the sample control, and processing into a sample control finished product. By adopting the cast aluminum-silicon alloy sample control preparation method, the sample control with uniform and stable chemical components and consistent metallurgical processing process and sample can be prepared, the accuracy of an analysis result is improved, the working efficiency is improved, and the detection cost is reduced.
Description
Technical Field
the invention relates to the technical field of sample control preparation for spectrum detection, in particular to a method for preparing a cast aluminum-silicon alloy sample control.
Background
In direct-reading spectroscopic analysis, in order to make the analysis result more accurate, a spectroscopic control sample needs to be used. Sample control calibration is actually a type normalization of the instrument to reduce analytical errors, and is typically performed prior to sample analysis to calibrate the sample.
The control sample has the performance of accurate fixed value, and the chemical components, the metallurgical processing process and the tissue state of the control sample are preferably consistent with the sample, but the control sample used at present is difficult to be consistent with the detected sample in the aspects of components and process states, and a plurality of control samples are basically needed to calibrate one product, even a standard sample is used to calibrate the result of the detected product, so that the accuracy of the analysis result is influenced, the working efficiency is reduced, and the detection cost is improved. In addition, the aluminum alloy has various types, and has the characteristics of easy oxidation, difficult refining and the like after different microalloying elements are added. At present, a preparation method for covering all samples for aluminum alloy spectrum detection is not available.
Disclosure of Invention
The invention aims to provide a method for preparing a cast aluminum-silicon alloy sample control, which can prepare a sample control with uniform and stable chemical components and consistent metallurgical processing with a sample, improve the accuracy of an analysis result, improve the working efficiency and reduce the detection cost.
In order to realize the aim, the invention provides a casting aluminum-silicon alloy sample control preparation method, which comprises the following steps:
s1, designing sample control elements of the aluminum alloy: according to the characteristics of the detected aluminum alloy product, the designed aluminum alloy sample control element composition and content are consistent with those of the detected product, and furnace burden is selected to comprise high-purity aluminum alloy, other high-purity metals and high-quality intermediate alloy subjected to segregation test;
S2, smelting and casting: adding furnace burden into a crucible resistance furnace according to the proportion, smelting and refining, and pouring a preparation control sample into a water-cooled copper mold after measuring the hydrogen content and the components to be qualified;
S3, analysis and inspection: after inspecting the macrostructure, the microstructure and the fracture tissue, selecting qualified sample control for initial inspection, sawing, and peeling the surface;
S4, after homogenization treatment, component uniformity and stability analysis are carried out, and a control sample is subjected to value setting;
And S5, carrying out finish turning on the surface of the sample control, and processing into a sample control finished product.
Preferably, in step S1, the aluminum alloy sample control design has the same elemental composition and content as the detected product, and is added in the form of Al-Si20 master alloy when the Si content of the product is less than 8%; when the Si content of the product is more than 8 percent, the product is added in the form of Al-Si25 master alloy, and modification and refinement treatment are carried out at the same time, so that the uniform distribution of components and tissues is ensured.
Preferably, in step S2, the order of addition and melting temperature of the pure metal and other master alloys, and the refining process parameters are as follows: (1) adding high-purity aluminum and Al-Si intermediate alloy, Al-Mn intermediate alloy, Al-Ni intermediate alloy and Al-Fe intermediate alloy into a furnace, adding Al-Cu and other intermediate alloys after melting, adding high-purity magnesium and Al-Ti intermediate alloy after deslagging, and adding a modifier before refining; (2) the melting temperature is 740 +/-15 ℃; (3) deslagging and refining at 730 +/-15 ℃; (4) adding 1-3 ‰ of refining agent, removing slag for 5-10min, refining for 15-60min, and detecting hydrogen content after refining, wherein the content is required to be less than or equal to 0.15ml/100 g.
Preferably, in step S2, a filtering device is disposed on the water-cooled copper mold, the sample control cavity has a lower inner diameter of 80mm, an upper inner diameter of 95mm and a depth of 250mm, criss-cross water channels are disposed outside the sample control cavity, the water flow is 20-40L/min, the water channels are wrapped by 20mm thick forged aluminum, and the forged aluminum has an outer diameter of 150 mm.
Preferably, in step S3, a stereomicroscope is used to detect the size of the sample-control grains and the slag inclusion in the fracture, the grain size is required to be better than grade 2, and the fracture has no slag inclusion; detecting defects such as pinholes, pores, slag inclusion and the like in the sample by adopting industrial CT, and requiring no pinholes or slag inclusion; detecting primary crystal silicon by adopting a metallographic microscope, wherein the size of the primary crystal silicon is less than or equal to 10um when the content of Si is less than 10%, and the size of the primary crystal silicon is less than or equal to 50um when the content of Si is more than 10%; and according to the detection result, the sample is controlled to be cut into a cylindrical sample with the diameter of 65 mm multiplied by 50mm by sawing and turning.
Preferably, in step S4, the homogenization heat treatment temperature is in the range of 500-550 ℃, and the homogenization time is 12-24 h; detecting sample control components for more than 10 times by adopting direct-reading spectrometers of different models, different personnel and different manufacturers, removing suspicious values, taking the average value as a final given sample control value, and calculating the standard deviation.
Preferably, in step S5, the sample control surface is turned into a cylindrical sample control product with a diameter of 60X 45 mm.
Therefore, the cast aluminum-silicon alloy sample control preparation method has the following technical effects:
1. The invention specifies the adding forms and the adding sequence of different elements, and the smelting temperature and the refining process parameters are clear at the same time, so that a series of sample controls suitable for different grades of aluminum alloys can be prepared.
2. The invention discloses a water-cooling copper mould for preparing a sample control, which is provided with a filtering device, wherein the filtering device has different specifications. The material of the sample control cavity is red copper, the material of the outer part of the die is forged aluminum, and criss-cross water channels are arranged outside the sample control cavity. The mold can filter the aluminum melt again in the pouring process, reduces slag inclusion, has good heat conductivity and extremely high cooling strength, and is instantly solidified, so that sample control crystal grains are fine and the components are uniform.
3. According to the invention, the standardization of sample control evaluation is realized through the evaluation requirements of crystal grains, microstructures, pinholes, slag inclusion and other defects and hydrogen content.
4. The preparation method can prepare the sample control with uniform and stable chemical components, fine crystal grains and consistent metallurgical processing with the sample, improve the accuracy of an analysis result, improve the working efficiency and reduce the detection cost.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a process flow chart of the cast aluminum-silicon alloy sample control preparation method of the invention.
Detailed Description
Embodiments of the present invention will be further described with reference to the accompanying drawings.
fig. 1 is a process flow diagram of a cast aluminum-silicon alloy sample control preparation method of the invention, and as shown in the figure, the cast aluminum-silicon alloy sample control preparation method comprises the following steps:
S1, designing sample control elements of the aluminum alloy: according to the characteristics of the detected aluminum alloy product, the designed aluminum alloy sample control element composition and content are consistent with those of the detected product, and furnace burden is selected to comprise high-purity aluminum alloy, other high-purity metals and high-quality intermediate alloy subjected to segregation test;
In step S1, the element composition and content of the aluminum alloy sample control design are consistent with those of the detected product, and when the Si content of the product is less than 8%, the product is added in the form of Al-Si20 intermediate alloy; when the Si content of the product is more than 8 percent, the product is added in the form of Al-Si25 master alloy, and modification and refinement treatment are carried out at the same time, so that the uniform distribution of components and tissues is ensured.
s2, smelting and casting: adding furnace burden into a crucible resistance furnace according to the proportion, smelting and refining, and pouring a preparation control sample into a water-cooled copper mold after measuring the hydrogen content and the components to be qualified;
in step S2, the order of addition and melting temperature of the pure metal and other master alloys, and the refining process parameters were as follows: (1) adding high-purity aluminum and Al-Si intermediate alloy, Al-Mn intermediate alloy, Al-Ni intermediate alloy and Al-Fe intermediate alloy into a furnace, adding Al-Cu and other intermediate alloys after melting, adding high-purity magnesium and Al-Ti intermediate alloy after deslagging, and adding a modifier before refining; (2) the melting temperature is 740 +/-15 ℃; (3) deslagging and refining at 730 +/-15 ℃; (4) adding 1-3 ‰ of refining agent, removing slag for 5-10min, refining for 15-60min, and detecting hydrogen content after refining, wherein the content is required to be less than or equal to 0.15ml/100 g.
In step S2, a filtering device is arranged on the water-cooled copper mold, the inner diameter of the lower part of the sample control cavity is 80mm, the inner diameter of the upper part of the sample control cavity is 95mm, the depth of the sample control cavity is 250mm, criss-cross water channels are arranged outside the sample control cavity, the water quantity is 20-40L/min, the outer surfaces of the water channels are wrapped by forged aluminum with the thickness of 20mm, and the outer diameter of the forged aluminum is 150 mm.
S3, analysis and inspection: after inspecting the macrostructure, the microstructure and the fracture tissue, selecting qualified sample control for initial inspection, sawing, and peeling the surface;
In step S3, a stereomicroscope is adopted to detect the size of sample control crystal grains and fracture slag inclusion, the grain size is required to be superior to grade 2, and the fracture has no slag inclusion; detecting defects such as pinholes, pores, slag inclusion and the like in the sample by adopting industrial CT, and requiring no pinholes or slag inclusion; detecting primary crystal silicon by adopting a metallographic microscope, wherein the size of the primary crystal silicon is less than or equal to 10um when the content of Si is less than 10%, and the size of the primary crystal silicon is less than or equal to 50um when the content of Si is more than 10%; and according to the detection result, the sample is controlled to be cut into a cylindrical sample with the diameter of 65 mm multiplied by 50mm by sawing and turning.
S4, after homogenization treatment, component uniformity and stability analysis are carried out, and a control sample is subjected to value setting;
in step S4, the homogenization heat treatment temperature is in the range of 500-550 ℃, and the homogenization time is 12-24 h; detecting sample control components for more than 10 times by adopting direct-reading spectrometers of different models, different personnel and different manufacturers, removing suspicious values, taking the average value as a final given sample control value, and calculating the standard deviation.
And S5, carrying out finish turning on the surface of the sample control, and processing into a sample control finished product.
In step S5, the sample control surface is turned into a cylindrical sample control product with a diameter of 60X 45 mm.
example one
a cast aluminum-silicon alloy sample control preparation method comprises the following steps:
(1) According to the characteristics of the detected product, the sample control is suitable for the following alloy compositions: 6.5 to 7.5 percent of Si, 0.25 to 0.45 percent of Mg, 0.05 to 0.15 percent of Fe, 0.05 to 0.15 percent of Ti and 0.010 to 0.030 percent of Sr, and the selected furnace burden comprises high-purity aluminum alloy, high-purity magnesium and intermediate alloys such as Al-Fe15, Al-Ti10, Al-Sr10, Al-Si25 and the like.
(2) preheating furnace burden, adding into a crucible resistance furnace according to the furnace burden proportion, adding high-purity aluminum, Al-Si20 intermediate alloy and Al-Fe15 intermediate alloy along with the furnace, melting at 740 ℃, adding high-purity magnesium and Al-Ti intermediate alloy after deslagging, and adding Al-Sr10 alterant and Al-Ti5B1 refiner before refining. The refining temperature is 730 ℃, the dosage of the slag removing agent is 1.5 per mill, the slag removing time is 5min, and the refining time is 30 min. The hydrogen content was measured after refining and found to be 0.13ml/100 g. The water quantity in the water-cooling copper die is set to be 25L/min, and the specification of the filtering device is set to be 30 ppi.
(3) detecting the size of sample control crystal grains and fracture slag inclusion by using a stereo microscope, wherein the grain size is grade 2, and the fracture has no slag inclusion; controlling the sample to have no pinholes or slag inclusion; the Si phase and the alpha-Al phase are uniformly distributed, and the control sample meeting the requirement is selected according to the detection result to be sawed and turned into a cylindrical control sample with the diameter of 65 mm multiplied by 50 mm.
(4) Controlling the temperature of the sample homogenization treatment to be 545-550 ℃, controlling the heat treatment time to be 18-20h, and carrying out component homogenization analysis, wherein the results are shown in the following table:
| Element(s) | Si | Fe | Mg | Ti | Sr |
| standard deviation of | 0.055 | 0.0012 | 0.0014 | 0.0014 | 0.0008 |
| Relative Standard Deviation (SD) | 0.69％ | 0.84％ | 0.40％ | 1.18％ | 3.63％ |
Three types of spectrometers of American thermoelectricity and Germany OBLF are adopted, 5 persons detect and detect sample control components for 15 times, suspicious values are removed, the average value is a final given sample control value, and the standard deviation is calculated.
(5) And carrying out finish turning on the surface of the control sample, processing the control sample into a control sample finished product, and inspecting the control sample to be qualified.
Example two
A cast aluminum-silicon alloy sample control preparation method comprises the following steps:
(1) According to the characteristics of the detected product, the sample control is suitable for the following alloy compositions: 9.5 to 11.5 percent of Si, 1.5 to 3.5 percent of Cu, 0.60 to 0.80 percent of Fe, 0.05 to 0.15 percent of Ti, 0.20 to 0.30 percent of Mg and 0.20 to 0.30 percent of Mn. The furnace burden comprises high-purity aluminum alloy, high-purity magnesium, Al-Fe15, Al-Ti10, Al-Cu40, Al-Si50, Al-Mn10 and other intermediate alloys.
(2) Preheating furnace burden, adding into a crucible resistance furnace according to the furnace burden proportion, adding high-purity aluminum, Al-Si50, Al-Mn10 and Al-Fe15 intermediate alloy along with the furnace, melting at the temperature of 770 ℃, adding Al-Cu40 intermediate alloy after melting, adding high-purity magnesium, Al-Ti intermediate alloy and Al-Ti5B1 refiner after refining. The refining temperature is 740 ℃, the dosage of the deslagging agent is 2.5 per mill, the deslagging time is 7min, and the refining time is 20 min. The hydrogen content was measured after refining and found to be 0.14ml/100 g. The water amount in the water-cooled copper die is set to be 28L/min, and the specification of the filtering device is set to be 20 ppi.
(3) Detecting the size of sample-control crystal grains and fracture slag inclusion by using a stereo microscope, wherein the grain size is grade 1, and the fracture has no slag inclusion; controlling the sample to have no pinholes or slag inclusion; the Si phase without primary crystal and the alpha-Al phase are distributed evenly, and the control sample which meets the requirements is selected according to the detection result to be sawed and turned into a cylindrical control sample with phi 65 multiplied by 50 mm.
(4) controlling the temperature of the sample homogenization treatment to be 550-560 ℃, treating for 24h, and carrying out component homogenization analysis, wherein the results are as follows:
| element(s) | Si | Fe | Cu | Mn | Mg | Ti |
| Standard deviation of | 0.12 | 0.016 | 0.011 | 0.008 | 0.0015 | 0.0016 |
| Relative Standard Deviation (SD) | 1.12％ | 2.28％ | 0.47％ | 2.92％ | 0.62％ | 1.25％ |
Three types of spectrometers of American thermoelectricity and Germany OBLF are adopted, 5 persons detect and detect sample control components for 15 times, suspicious values are removed, the average value is a final given sample control value, and the standard deviation is calculated.
(5) and carrying out finish turning on the surface of the control sample, processing the control sample into a control sample finished product, and inspecting the control sample to be qualified.
Therefore, the cast aluminum-silicon alloy sample control preparation method can be used for preparing the sample control with uniform and stable chemical components and consistent metallurgical processing process and sample, the accuracy of an analysis result is improved, the working efficiency is improved, and the detection cost is reduced.
finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (7)
1. A cast aluminum-silicon alloy sample control preparation method is characterized by comprising the following steps:
s1, designing sample control elements of the aluminum alloy: according to the characteristics of the detected aluminum alloy product, the designed aluminum alloy sample control element composition and content are consistent with those of the detected product, and furnace burden is selected to comprise high-purity aluminum alloy, other high-purity metals and high-quality intermediate alloy subjected to segregation test;
s2, smelting and casting: adding furnace burden into a crucible resistance furnace according to the proportion, smelting and refining, and pouring a preparation control sample into a water-cooled copper mold after measuring the hydrogen content and the components to be qualified;
S3, analysis and inspection: after inspecting the macrostructure, the microstructure and the fracture tissue, selecting qualified sample control for initial inspection, sawing, and peeling the surface;
S4, after homogenization treatment, component uniformity and stability analysis are carried out, and a control sample is subjected to value setting;
And S5, carrying out finish turning on the surface of the sample control, and processing into a sample control finished product.
2. The cast aluminum-silicon alloy sample control preparation method according to claim 1, characterized in that: in step S1, the element composition and content of the aluminum alloy sample control design are consistent with those of the detected product, and when the Si content of the product is less than 8%, the product is added in the form of Al-Si20 intermediate alloy; when the Si content of the product is more than 8 percent, the product is added in the form of Al-Si25 master alloy, and modification and refinement treatment are carried out at the same time, so that the uniform distribution of components and tissues is ensured.
3. A cast Al-Si alloy sample control preparation method according to claim 1, characterized in that in step S2, the order of addition and melting temperature of pure metal and other intermediate alloy, and refining process parameters are as follows: (1) adding high-purity aluminum and Al-Si intermediate alloy, Al-Mn intermediate alloy, Al-Ni intermediate alloy and Al-Fe intermediate alloy along with a furnace, adding Al-Cu intermediate alloy after melting, adding high-purity magnesium and Al-Ti intermediate alloy after deslagging, and adding a modifier before refining; (2) the melting temperature is 740 +/-15 ℃; (3) deslagging and refining at 730 +/-15 ℃; (4) adding 1-3 ‰ of refining agent, removing slag for 5-10min, refining for 15-60min, and detecting hydrogen content after refining, wherein the content is required to be less than or equal to 0.15ml/100 g.
4. the cast aluminum-silicon alloy sample control preparation method according to claim 1, characterized in that: in step S2, a filtering device is arranged on the water-cooled copper mold, the inner diameter of the lower part of the sample control cavity is 80mm, the inner diameter of the upper part of the sample control cavity is 95mm, the depth of the sample control cavity is 250mm, criss-cross water channels are arranged outside the sample control cavity, the water quantity is 20-40L/min, the outer surfaces of the water channels are wrapped by forged aluminum with the thickness of 20mm, and the outer diameter of the forged aluminum is 150 mm.
5. a cast Al-Si alloy sample control preparation method according to claim 1The method is characterized in that: in step S3, a stereomicroscope is adopted to detect the size of sample control crystal grains and fracture slag inclusion, the grain size is required to be superior to grade 2, and the fracture has no slag inclusion; detecting defects of pinholes, pores and slag inclusion in the sample by adopting industrial CT, wherein the defects of pinholes, pores and slag inclusion are required to be free; detecting primary crystal silicon by adopting a metallographic microscope, wherein the size of the primary crystal silicon is less than or equal to 10um when the content of Si is less than 10%, and the size of the primary crystal silicon is less than or equal to 50um when the content of Si is more than 10%; according to the detection result, the sample is controlled and cut by saw cuttingThe sample is controlled by the column.
6. The cast aluminum-silicon alloy sample control preparation method according to claim 1, characterized in that: in step S4, the homogenization heat treatment temperature is in the range of 500-550 ℃, and the homogenization time is 12-24 h; detecting sample control components for more than 10 times by adopting direct-reading spectrometers of different models, different personnel and different manufacturers, removing suspicious values, taking the average value as a final given sample control value, and calculating the standard deviation.
7. The cast aluminum-silicon alloy sample control preparation method according to claim 1, characterized in that: in step S5, the sample control surface is turned intoThe cylindrical sample control finished product is obtained.
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| CN111074113A (en) * | 2020-01-02 | 2020-04-28 | 苏州先准电子科技有限公司 | Production process for in-situ generation of zirconium boride particle reinforced aluminum-silicon-based composite material |
| CN111074113B (en) * | 2020-01-02 | 2021-12-24 | 苏州先准电子科技有限公司 | Production process for in-situ generation of zirconium boride particle reinforced aluminum-silicon-based composite material |
| CN117191522A (en) * | 2023-09-15 | 2023-12-08 | 南通众福新材料科技有限公司 | Single-point control sample block for controlling high-strength and high-toughness aluminum alloy material and preparation method thereof |
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