Cast aluminum alloy 411Z. 2 as-cast spectrum single-point standard sample as well as preparation method and application thereof

Abstract

The invention relates to the technical field of alloy materials, in particular to a cast aluminum alloy 411Z. 2 as-cast spectrum single-point standard sample and a preparation method and application thereof. The component content and the structure state of the single-point standard sample are highly close to those of a product, the accuracy of an analysis result can be improved, the working efficiency is improved, the detection cost is reduced, and the domestic blank is filled. According to the preparation method provided by the invention, a standard sample is obtained through component design, material selection, weighing, smelting, refining and casting, and standard values of the element components of the standard sample are obtained through primary inspection of uniformity, processing, uniformity inspection of a finished product, valuing and mathematical statistics and reduction. The component content and the structure state of the finally prepared single-point standard sample are highly close to those of a product, the accuracy of an analysis result can be improved, and the method is suitable for accurate detection and control of aluminum alloy components of the cast aluminum alloy 411Z. 2 and correction of a detection instrument.

Description

Technical Field

[0001] The invention relates to the technical field of alloy materials, and in particular to a cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample and a preparation method and application thereof. Background Art

[0002] Usually in the production process of cast aluminum alloy, the aluminum liquid in the smelting furnace is sampled and analyzed on a photoelectric direct reading spectrometer. The smelting workers then control the composition of the aluminum liquid based on the analysis results to obtain products with qualified composition.

[0003] The analysis method of photoelectric direct reading spectrometer is a relative measurement method. This method first excites the standard sample of known composition, calibrates the working curve of the spectrometer, obtains the emission light intensity of different elements, and then excites the sample to be tested, and compares the emission light intensity of the element in the sample with the emission light intensity of the corresponding element in the standard sample, so as to obtain the element content of the test sample. The quality of the standard sample will directly affect the calibration effect, and then affect the accuracy of the analysis result. Therefore, the element content, type, and organizational state of the standard sample need to be highly close to the cast aluminum alloy product, and have good uniformity and stability.

[0004] As the trend of lightweighting of automobiles in my country accelerates, the demand for cast aluminum alloy 411Z.2 is increasing day by day because it can meet the needs of thin-walled, high-strength and high-toughness, which is conducive to the lightweighting of body parts and obtains great advantages in the cost and performance of body structural parts. At present, most of the standard samples used for analysis of cast aluminum alloys in China are in the state of secondary extrusion, which is inconsistent with the organizational state of cast aluminum alloy product 411Z.2. Although some samples are in the cast state (gravity casting process), the types and contents of component elements are not close to those of cast aluminum alloy product 411Z.2, and the uniformity is poor. Multiple standard samples need to be used for calibration during analysis, which is costly and cannot meet the requirements of fast and accurate measurement of the composition of cast aluminum alloy 411Z.2. There is a gap in the field of single-point standard samples that can be directly used to analyze 411Z.2 products in China. Summary of the invention

[0005] In view of the shortcomings of the prior art, the present invention provides a cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample and a preparation method and application thereof. The component content and organizational state of the single-point standard sample are highly similar to those of the product, which can improve the accuracy of the analysis results, improve work efficiency, reduce detection costs, and fill the domestic gap.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] The first aspect of the present invention provides a cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample, which comprises the following components by mass percentage: Si 9.6-10.1%, Fe 0.10-0.16%, Cu 0.032-0.038%, Mn 0.410-0.440%, Mg0.0030-0.0190%, Cr 0.0035-0.0045%, Ni 0.0050-0.0060%, Zn 0.0220-0.0380%, Ti0.070-0.100%, Sr 0.0165-0.0170%, Mo 0.0300-0.130%, Zr 0.140-0.150% and the balance Al, and the organizational state of the single-point standard sample is as-cast;

[0008] The preparation method of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample comprises the following steps:

[0009] (1) raw materials are prepared according to the components of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample, the raw materials comprising: 411Z.2 cast aluminum alloy ingot, 99.7% pure aluminum ingot, industrial pure magnesium, industrial pure zinc, Al-40% Cu alloy ingot, Al-10% Mn alloy ingot, Al-20% Si alloy ingot, Al-10% Fe alloy ingot, Al-3% Cr alloy ingot, Al-20% Ni alloy ingot, Al-3% Ti alloy ingot, Al-5% Mo alloy ingot, Al-5% Zr alloy ingot, aluminum titanium boron thin rod and Al-10% Sr alloy ingot;

[0010] (2) smelting the 411Z.2 cast aluminum alloy ingot, 99.7% pure aluminum ingot, industrial pure magnesium, industrial pure zinc, Al-40% Cu alloy ingot, Al-10% Mn alloy ingot, Al-20% Si alloy ingot, Al-10% Fe alloy ingot, Al-3% Cr alloy ingot, Al-20% Ni alloy ingot, Al-3% Ti alloy ingot, Al-5% Mo alloy ingot, and Al-5% Zr alloy ingot at 710-770° C., and obtaining a molten liquid after the raw materials are completely melted. The molten liquid is successively refined, slag-scraped, and stirred to obtain a molten alloy liquid, and a chemical composition sample is taken for analysis to ensure that it meets the design composition requirements;

[0011] (3) After the chemical composition reaches the design composition requirements, the temperature of the molten alloy liquid is adjusted to a first static temperature of 710-770°C, and then the molten alloy liquid at the first static temperature is subjected to a first static, a first refining, a first slag removal, a degassing refining and a second slag removal, wherein the additives for the degassing refining include the aluminum titanium boron thin rod and the Al-10% Sr alloy ingot, and the degassing refining is performed for 10-20 minutes; the temperature of the alloy liquid obtained by the second slag removal is adjusted to a second static temperature of 720-750°C, and the second static is performed for 10-15 minutes to obtain a static alloy liquid, and the static alloy liquid is subjected to a component analysis;

[0012] (4) filtering and casting the static alloy liquid with qualified component analysis in sequence, with the casting temperature being 700-720° C., and cooling to obtain a Φ65 mm×(4100-4300) mm single-point standard sample cast rod;

[0013] (5) The single-point standard sample cast rod is subjected to initial inspection, processing, average inspection and calibration in sequence to obtain a cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample.

[0014] Preferably, the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample, measured in mass percentage, includes the following components: Si 9.6-10.1%, Fe 0.114-0.156%, Cu 0.033-0.037%, Mn 0.412-0.438%, Mg0.0035-0.0188%, Cr 0.0035-0.0045%, Ni 0.0050-0.0060%, Zn 0.0225-0.0375%, Ti0.071-0.098%, Sr 0.0165-0.0170%, Mo 0.0302-0.128%, Zr 0.140-0.148% and the balance Al.

[0015] Further preferably, the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample, in terms of mass percentage, comprises the following components: Si 10.03%, Fe 0.155%, Cu 0.036%, Mn 0.435%, Mg 0.0188%, Cr0.0044%, Ni0.0057%, Zn 0.0228%, Ti 0.072%, Sr 0.0170%, Mo 0.126%, Zr 0.140% and the balance Al,

[0016] Or: Si 9.64%, Fe 0.116%, Cu 0.034%, Mn 0.415%, Mg 0.0037%, Cr0.0036%, Ni 0.0050%, Zn 0.037%, Ti 0.097%, Sr 0.0166%, Mo 0.0304%, Zr 0.147% and the balance Al.

[0017] Preferably, the mass of the refining agent used in the refining in step (2) is 1.5‰ of the total mass of the raw material. The refining agent used is a composition of 20% potassium fluoroaluminate, 10% sodium chloride and 70% potassium chloride.

[0018] Preferably, the first standing is carried out in a 1000kg standing furnace, and after the second slagging, hydrogen measurement and component detection are carried out in sequence. The hydrogen measurement method is preferably a reduced pressure density method. After the component detection result reaches the component content, the second standing is carried out.

[0019] Preferably, the temperature of the first static state is 740±5°C; the refining agent used in the first refining is a composition of 20% potassium fluoroaluminate, 10% sodium chloride and 70% potassium chloride. The degassing equipment used for the degassing refining is preferably a graphite rotor refiner, and the gas used in the graphite rotor refiner is preferably argon with a purity of ≥99.95%. The degassing refining time is 15 minutes; the temperature of the second static state is 730-740°C; the second static state time is 15 minutes.

[0020] Preferably, the amount of the aluminum-titanium-boron thin rods used is 1.5‰ of the total mass of the raw materials; the amount of the Al-10% Sr alloy ingots used is 0.0049% of the total mass of the raw materials.

[0021] Preferably, the filtering is preferably carried out in a bipolar filtering device, and the casting is preferably carried out in a horizontal hot top semi-continuous casting device equipped with a Φ65mm*8 crystallizer.

[0022] Preferably, the casting temperature is 700-720°C, more preferably 710±5°C; the casting speed is 200-250 mm / min, more preferably 250 mm / min; the cooling method is water cooling, and the water pressure of the water cooling is 0.04-0.06 MPa.

[0023] Preferably, the initial inspection includes the following steps: after cutting off at least 250 mm at both ends of the single-point standard sample cast rod, a sample with a length of 20 to 30 mm is obtained from the two ends, 1 / 4, and 3 / 4 of the sampled cast rod, respectively, and the sample is subjected to low-power inspection and initial inspection of composition uniformity to obtain a cast rod with a qualified initial inspection result. In the present invention, the initial inspection of composition uniformity is preferably carried out with reference to YS / T409 "Technical Specifications for Standard Samples for Analysis of Nonferrous Metal Products", and the result of the initial inspection of composition uniformity is preferably determined with reference to the requirements of GB / T15000 "Guidelines for Standard Sample Work" and YS / T409 "Technical Specifications for Standard Samples for Analysis of Nonferrous Metal Products", and the statistical method for the result of the initial inspection of composition uniformity is preferably the range method.

[0024] Preferably, the processing is to sequentially lathe and cut the cast rods with qualified initial inspection results to obtain spectral samples of Φ58*35mm. The average inspection preferably includes the following steps: sequentially numbering the spectral samples, randomly selecting 20 spectral samples, and using a direct reading spectrometer to detect three different parts of the spectral sample cross section to obtain the composition data of the spectral samples, and the composition data is statistically analyzed using variance analysis.

[0025] Preferably, the determination includes the following steps: selecting 2 cast rods with qualified initial inspection results as determination sampling samples, cutting 300mm long cast rods from the head, middle and tail of the determination sampling samples in turn as rods for processing chemical samples, making the rods for processing chemical samples into alloy chips to obtain chemical samples, chemically determining the chemical samples to obtain initial data, and processing the initial data to obtain the final determination result. The chemical determination preferably selects eight laboratories with standard sample determination qualifications to conduct joint determination using national standard methods based on multiple different principles, and the national standard methods are preferably one or more analysis methods in GB / T 20975 "Chemical Analysis Methods for Aluminum and Aluminum Alloys". In the present invention, the number of groups of the initial data is preferably 8, and the number of data within the group of the initial data is preferably 4. The processing includes the following steps: performing range determination on the data within the group of the initial data to obtain the original data; performing the Shapiro-Wilk normality test, the Grubbs test and the Cochran test on the original data in turn, and then determining the standard value and the expanded uncertainty and rounding in turn to obtain the final fixed value result. The range of the data within the group of the initial data is preferably determined according to the allowable difference of GB / T 20975 "Chemical Analysis Methods for Aluminum and Aluminum Alloys", and the data that does not meet the allowable difference is preferably eliminated and the original laboratory is required to review it. The present invention obtains the original data after the range of the data within the group of the data is determined to be qualified. In the present invention, the rounding is preferably performed according to GB8170 "Data Rounding Rules".

[0026] The second aspect of the present invention provides the use of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample in a direct reading spectrometer.

[0027] Preferably, the application comprises working curve correction.

[0028] Preferably, the spectrum detection instrument is a photoelectric direct-reading spectrometer.

[0029] The advantages and positive effects of the present invention are:

[0030] (1) The component content and organizational state of the cast aluminum alloy 411Z.2 cast spectrum single-point standard sample of the present invention are highly similar to the product, which can reduce the types of standard samples used under existing detection conditions, which is beneficial to reducing detection costs and improving detection efficiency, and has a curve correction effect on the detection instrument, which is beneficial to improving the accuracy of detection.

[0031] (2) The method provided by the present invention adopts an intermediate alloy and a process flow of melting, standing and casting, which is conducive to forming a good cast structure of the cast aluminum alloy and improving the uniformity of the composition, and is conducive to ensuring the reproducibility of the spectral response of the single-point standard sample during use, thereby ensuring the accuracy of the test results.

[0032] (3) The component content and organizational state of the single-point standard sample provided by the present invention are highly similar to those of the product, which can improve the accuracy of the analysis results and is suitable for direct reading spectrometer detection. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is a metallographic structure photograph of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample prepared in Example 1;

[0034] Figure 2 This is a metallographic structure photograph of a casting product A having a composition similar to that of Example 1;

[0035] Figure 3 This is a metallographic structure photograph of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample prepared in Example 2;

[0036] Figure 4 This is a metallographic structure photograph of the casting product B with a composition similar to that of Example 2;

[0037] Figure 5 This is a comparison of the appearance of the cast rods prepared in Comparative Example 1 and Example 1. DETAILED DESCRIPTION

[0038] The present invention is further described in detail below through specific examples. The following examples are only illustrative and not restrictive, and the protection scope of the present invention cannot be limited thereto.

[0039] Example 1

[0040] A cast aluminum alloy 411Z.2 cast spectrum single-point standard sample, calculated by mass percentage, includes the following components: the composition design is in accordance with the requirements of GB / T8733-2016 Casting Aluminum Alloy Ingot for 411Z.2 chemical composition, and can meet the requirements of enterprise product composition. Since this cast aluminum alloy is modified by strontium, adding Mo and Zr can improve its performance. Therefore, the design of Sr, Mo and Zr is added in the composition design. Specifically, it is composed of the following design components according to the mass percentage ratio: Si 10.03%, Fe 0.155%, Cu 0.036%, Mn 0.435%, Mg 0.0188%, Cr 0.0044%, Ni0.0057%, Zn 0.0228%, Ti 0.072%, Sr 0.0170%, Mo 0.126%, Zr 0.140% and the balance Al, and the organizational state of the single-point standard sample is cast.

[0041] The preparation method of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample comprises the following steps:

[0042] Step 1: Use the existing cast aluminum alloy ingot 411Z.2 as the raw material, and then adjust it with the following materials: 99.7% pure aluminum ingot for Al, industrial pure magnesium for Mg, industrial pure zinc for Zn, and high-quality intermediate alloys that have passed the segregation test: Al-40% Cu alloy ingot, Al-10% Mn alloy ingot, Al-20% Si alloy ingot, Al-10% Fe alloy ingot, Al-3% Cr alloy ingot, Al-20% Ni alloy ingot, Al-3% Ti alloy ingot, Al-10% Sr alloy ingot, Al-5% Mo alloy ingot, Al-5% Zr alloy ingot.

[0043] Step 2: Convert the mass percentage of the designed components into the mass of the selected raw materials and auxiliary materials to be weighed;

[0044] Step 3: adding the weighed cast aluminum alloy ingot 411Z.2 and 99.7% pure aluminum ingot, industrial pure magnesium, industrial pure zinc, Al-40% Cu alloy ingot, Al-10% Mn alloy ingot, Al-20% Si alloy ingot, Al-10% Fe alloy ingot, Al-3% Cr alloy ingot, Al-20% Ni alloy ingot, Al-3% Ti alloy ingot, Al-5% Mo alloy ingot and Al-5% Zr alloy ingot into a 1000kg smelting furnace for smelting, the smelting aluminum liquid temperature is 740℃±5℃, when the charge is completely melted to obtain a molten liquid, evenly sprinkle a refining agent on the molten liquid for refining, slagging and stirring to obtain a smelting alloy liquid, the mass of the refining agent is 1.5‰ of the mass of the raw material, and the component of the refining agent is a composition of 20% potassium fluoroaluminate, 10% sodium chloride and 70% potassium chloride, and taking a chemical composition sample for analysis to meet the design composition requirements;

[0045] Step 4: When the chemical composition of the molten alloy in step 3 reaches the design composition requirements, the temperature of the molten alloy is raised to 740±5°C, and it is tilted into a 1000kg static furnace for the first static state. When the temperature of the aluminum liquid in the static furnace reaches 740±5°C, a 1.5‰ refining agent is used, which is composed of 20% potassium fluoroaluminate, 10% sodium chloride and 70% potassium chloride by mass percentage. The static alloy liquid is refined and the slag is thoroughly skimmed. Then, a graphite rotor refiner is used to refine the static alloy liquid for 15 minutes under the condition of passing argon gas. During the refining process, 1.5‰ Al-Ti-B rods are added to refine the grains and 0.0049% Al-10% Sr alloy ingots are added. After refining, the slag is removed again, and the melt temperature is adjusted to 730±5℃. The second static state is performed, and the hydrogen is measured by the reduced pressure density method until it is qualified, that is, the sample block has no obvious pinholes. The chemical composition sample is taken again for analysis, and the second static state is 15 minutes to obtain the static alloy liquid. After the composition is qualified, check that the casting system is normal and then prepare for casting.

[0046] Step 5: After the static alloy liquid obtained in step 4 is filtered through a bipolar filtering device, it is cast using a hot top semi-continuous casting device with the same level as that of a Φ65mm×8 crystallizer. The process parameters are as follows: the casting temperature is 710±5℃, the casting speed is 250mm / min, and the cooling water pressure is 0.04~0.06Mpa. Finally, eight aluminum alloy cast rods of Φ65mm×(4100~4300)mm are obtained.

[0047] Step 6: Composition uniformity inspection: The composition uniformity inspection is carried out in accordance with the requirements of GB / T15000 "Guidelines for Standard Samples" and YS / T409 "Technical Specifications for Standard Samples for Analysis of Nonferrous Metal Products". After cutting off at least 250mm at both ends of the cast rod obtained in step 5, take 20-30mm samples from both ends and the middle, 1 / 4, and 3 / 4 respectively, a total of 40 samples, for low-power inspection, and then carry out an initial inspection of composition uniformity in accordance with the requirements of YS / T409 "Technical Specifications for Standard Samples for Analysis of Nonferrous Metal Products", and use the range method for statistics.

[0048] Step 7: Process the cast rods that have passed the low-power inspection and the initial uniformity inspection in step 6, and process a total of 600 Φ58×35mm spectral samples. At the same time, select representative cast rods to process chemical samples, and take 300mm lengths from the head, middle, and tail of any two cast rods as rods for processing chemical samples. Number the processed spectral samples in sequence, and then randomly select 20 spectral samples. Check three different parts of the cross section of each sample on the photoelectric direct reading spectrometer to obtain the spectral standard sample composition uniformity data, and use the variance method for statistics.

[0049] Step 8: The rods used for processing chemical samples in step 7 are made into alloy chips to obtain chemical samples. The chemical samples are valued as standard samples. Eight laboratories with standard sample value determination qualifications are used to jointly determine the value using national standard methods with different principles. According to GB / T 20975 "Chemical Analysis Methods for Aluminum and Aluminum Alloys", one or more analysis methods are selected for collaborative value determination analysis and data processing. The data reported by each analysis unit are obtained in total of eight groups of data, each with 4 independent data. First, the suspicious value is determined technically. The range is checked according to the allowable difference of GB / T 20975 "Chemical Analysis Methods for Aluminum and Aluminum Alloys" to check whether there are abnormal values ​​in the group. If there are abnormal values, the original laboratory is required to review the suspicious values. The original data after the suspicious values ​​are eliminated are summarized and tested for normality using the Shapiro-Wilk method. The average value of the data that obeys the normal distribution is taken as a single measurement value to form a new group of data for testing using the Grubbs method, and then the Cochran method is used to test whether the data in each group are of equal precision. The standard value and expanded uncertainty (uncertainty caused by fixed value and uncertainty caused by uniformity) are finally determined through the above tests, and are rounded according to the rules of G8170 "Data Rounding Rules". The standard value and expanded uncertainty of the single-point standard sample of cast aluminum alloy 411Z.2 cast spectrum in this embodiment are shown in Table 1.

[0050] Table 1 Standard values ​​and expanded uncertainties of cast aluminum alloy 411Z.2 as-cast spectrum single-point standard samples prepared in Example 1

[0051]

[0052]

[0053] It can be seen from Table 1 that the determination result of the single-point standard sample prepared in Example 1 fully meets the design requirements and can satisfy the analysis requirements of the product.

[0054] Example 2

[0055] A cast aluminum alloy 411Z.2 cast spectrum single point standard sample, calculated by mass percentage, includes the following components: the composition design is in accordance with the requirements of "GB / T8733-2016 Casting Aluminum Alloy Ingot" for the chemical composition of 411Z.2, and can meet the requirements of the enterprise product composition. Since this cast aluminum alloy is modified by strontium, adding Mo and Zr can improve its performance. Therefore, the design of Sr, Mo and Zr is added in the composition design. Specifically, it is composed of the following design components according to the mass percentage ratio: Si 9.64%, Fe 0.116%, Cu 0.034%, Mn 0.415%, Mg 0.0037%, Cr 0.0036%, Ni0.0050%, Zn 0.0370%, Ti 0.097%, Sr 0.0166%, Mo 0.0304%, Zr 0.147% and the balance Al.

[0056] The types of raw materials are the same as those in Example 1, the quality of each raw material is based on the composition of Example 2, and the remaining steps are the same as those in Example 1. The standard values ​​and expanded uncertainties of the single-point standard sample of the cast spectrum of cast aluminum alloy 411Z.2 in this example are shown in Table 2.

[0057] Table 2 Standard values ​​and expanded uncertainties of single-point standard samples of cast aluminum alloy 411Z.2 as-cast spectrum prepared in Example 2

[0058]

[0059] It can be seen from Table 2 that the determination result of the cast spectrum single-point standard sample of the cast aluminum alloy 411Z.2 prepared in Example 1 fully meets the design requirements and can meet the analysis requirements of the product.

[0060] A similar foreign Mo-containing standard sample with high precision was selected, and the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample prepared in Examples 1 and 2 was compared with the standard value and expanded uncertainty of the same element. The comparison results are shown in Table 3.

[0061] Table 3 Comparison results of technical parameters of cast aluminum alloy 411Z.2 as-cast spectrum single-point standard samples of Example 1 and Example 2 with similar foreign standard samples

[0062]

[0063]

[0064] It can be seen from Table 3 that, except for the expanded uncertainties of Sr and Zr, the expanded uncertainties of elements such as Si, Fe, Cu, Mn, Ti, Cr, Ni, Zn and Mo in the cast aluminum alloy 411Z.2 cast spectrum single-point standard samples prepared in Example 1 and Example 2 are better than those of similar foreign standard samples, indicating that the quality of the cast aluminum alloy 411Z.2 cast spectrum single-point standard samples prepared in Example 1 and Example 2 has basically reached the international advanced level of similar standard samples.

[0065] Example 3

[0066] The cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample prepared in Example 1 and the cast product A with a composition similar to that of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample in Example 1 were sampled, and the samples were processed into metallographic samples. The metallographic structures of the two were observed using a metallographic microscope. The metallographic structure of the single-point standard sample prepared in Example 1 is shown in FIG. Figure 1 The metallographic structure of the casting product A is shown in Figure 2 .

[0067] Depend on Figure 1 and Figure 2 It can be seen that the metallographic structure of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample prepared in Example 1 is close to the metallographic structure of the casting product with similar composition, which is beneficial to improve the accuracy of the composition detection of the sample taken.

[0068] The analysis method in GB / T 20975 "Chemical Analysis Methods for Aluminum and Aluminum Alloys" and the direct reading spectrometer were used to detect the elemental composition of the samples taken from the casting product A. The standard sample used for the direct reading spectrometer type standardization was the cast aluminum alloy 411Z.2 cast spectrum single-point standard sample prepared in Example 1. The comparison of the detection results of the two methods is shown in Table 4.

[0069] Table 4 Comparison of test results of casting product A using chemical analysis and direct reading spectroscopy

[0070]

[0071]

[0072] The comparison results in Table 4 show that the detection value of the cast aluminum alloy 411Z.2 cast spectrum single-point standard sample prepared in Example 1 as a direct reading spectrometer type standard sample is basically consistent with the detection value obtained by the chemical method. The cast aluminum alloy 411Z.2 cast spectrum standard sample prepared in Example 1 can accurately measure the element content of casting products with similar compositions.

[0073] Example 4

[0074] The cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample prepared in Example 2 and the cast product B with a composition similar to that of the standard sample in Example 2 were sampled, and the samples were processed into metallographic samples. The metallographic structures of the two were observed using a metallographic microscope. The metallographic structure of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample prepared in Example 2 is shown in FIG. Figure 3 The metallographic structure of casting product B is shown in Figure 4 .

[0075] Depend on Figure 3 and Figure 4 It can be seen that the metallographic structure of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample prepared in Example 2 is close to the metallographic structure of the casting product with similar composition, which is beneficial to improve the accuracy of the composition detection of the sample taken.

[0076] The analysis method in GB / T 20975 "Chemical Analysis Methods for Aluminum and Aluminum Alloys" and the direct reading spectrometer were used to detect the elemental composition of the samples taken from the casting product B. The standard sample used for the direct reading spectrometer type standardization was the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample prepared in Example 2. The comparison of the detection results of the two methods is shown in Table 5.

[0077] Table 5 Comparison of test results of casting product B using chemical analysis and direct reading spectroscopy

[0078]

[0079] The comparison results in Table 5 show that the detection value of the single-point standard sample prepared in Example 2 as the direct-reading spectrometer type standard sample is basically consistent with the detection value obtained by the chemical method, and the cast aluminum alloy 411Z.2 cast spectrum single-point standard sample prepared in Example 2 can accurately measure the element content of casting products with similar compositions.

[0080] The above comparison results show that the metallographic structure state of the cast aluminum alloy 411Z.2 cast spectrum single-point standard sample prepared in Example 1 and Example 2 is highly similar to the metallographic structure state of the product with similar composition, and, compared with the uncertainty and RSD of similar foreign standard samples, it can be seen that the cast aluminum alloy 411Z.2 cast spectrum single-point standard sample prepared in Example 1 and Example 2 has accurate fixed value and better uniformity of component content, which is more conducive to the instrument to accurately detect the composition of product sampling and improve the accuracy of aluminum liquid composition detection.

[0081] Comparative Example 1

[0082] A cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample, the only difference from Example 1 is that the casting temperature in step 5 is adjusted to 685℃±10℃. During the casting process, the molten liquid is prone to solidification and blocking the crystallizer. Even if it is barely cast into a cast rod, there are many defects on the surface of the cast rod, which is not conducive to the steps after step 5. The appearance comparison of the cast rods prepared in Comparative Example 1 and Example 1 is shown in Figure 5 . Figure 5 The left picture shows the appearance of the cast rod prepared in Comparative Example 1, which is rough and has many defects, and the right picture shows the appearance of the cast rod prepared in Example 1, which is smooth and has fewer defects. This comparative example shows that too low a casting temperature will cause defects in the cast rod, and even make it impossible to cast.

[0083] Comparative Example 2

[0084] A cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample, the difference from Example 1 is that the casting temperature is adjusted to 731°C ± 10°C, then 4 are randomly selected from the 8 cast rods prepared, and the selected 4 cast rods are numbered 1, 2, 3, and 4 in turn, and after cutting off at least 250 mm at both ends, 20-30 mm samples are taken from both ends and the middle, 1 / 4, and 3 / 4, respectively, and the composition is tested according to the same detection method as in Example 1. The results of the Sr element content in the cast rod samples prepared in Comparative Example 2 and Example 1 are shown in Table 6.

[0085] Table 6 Sr element content of cast rod samples prepared in Comparative Example 2 and Example 1

[0086]

[0087] It can be seen from Table 6 that due to the excessively high casting temperature used in this comparative example, the Sr content of the head and tail of the prepared cast rods differs greatly, which is not conducive to the uniformity of the standard sample composition. The Sr content of the cast rod samples obtained at the casting temperature of Example 1 is almost the same in each part, which is conducive to the accuracy of the analysis.

[0088] The embodiments described above are only descriptions of the preferred modes of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.

Claims

1. A cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample, characterized in that: The invention comprises the following components in mass percentage: Si 9.6-10.1%, Fe 0.10-0.16%, Cu 0.032-0.038%, Mn 0.410-0.440%, Mg 0.0030-0.0190%, Cr 0.0035-0.0045%, Ni 0.0050-0.0060%, Zn 0.0220-0.0380%, Ti 0.070-0.100%, Sr 0.0165-0.0170%, Mo 0.0300-0.130%, Zr 0.140-0.150% and the balance Al, wherein the organizational state of the single-point standard sample is as-cast; The preparation method of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample comprises the following steps: (1) raw materials are prepared according to the components of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample, the raw materials comprising: 411Z.2 cast aluminum alloy ingot, 99.7% pure aluminum ingot, industrial pure magnesium, industrial pure zinc, Al-40% Cu alloy ingot, Al-10% Mn alloy ingot, Al-20% Si alloy ingot, Al-10% Fe alloy ingot, Al-3% Cr alloy ingot, Al-20% Ni alloy ingot, Al-3% Ti alloy ingot, Al-5% Mo alloy ingot, Al-5% Zr alloy ingot, aluminum titanium boron thin rod and Al-10% Sr alloy ingot; (2) smelting the 411Z.2 cast aluminum alloy ingot, 99.7% pure aluminum ingot, industrial pure magnesium, industrial pure zinc, Al-40% Cu alloy ingot, Al-10% Mn alloy ingot, Al-20% Si alloy ingot, Al-10% Fe alloy ingot, Al-3% Cr alloy ingot, Al-20% Ni alloy ingot, Al-3% Ti alloy ingot, Al-5% Mo alloy ingot, and Al-5% Zr alloy ingot at 710-770° C., and obtaining a molten liquid after the raw materials are completely melted. The molten liquid is successively refined, slag-scraped, and stirred to obtain a molten alloy liquid, and a chemical composition sample is taken for analysis, and fine-tuning is performed to make it meet the design composition requirements; (3) After the chemical composition reaches the design composition requirements, the temperature of the molten alloy liquid is adjusted to a first static temperature of 710-770°C, and then the molten alloy liquid at the first static temperature is subjected to a first static, a first refining, a first slag removal, a degassing refining and a second slag removal, wherein the additives for the degassing refining include the aluminum titanium boron thin rod and the Al-10% Sr alloy ingot, and the degassing refining is performed for 10-20 minutes; the temperature of the alloy liquid obtained by the second slag removal is adjusted to a second static temperature of 720-750°C, and the second static is performed for 10-15 minutes to obtain a static alloy liquid, and the static alloy liquid is subjected to a component analysis; (4) filtering and casting the static alloy liquid with qualified component analysis in sequence, with the casting temperature being 700-720° C., and cooling to obtain a Φ65 mm×(4100-4300) mm single-point standard sample cast rod; (5) The single-point standard sample cast rod is subjected to initial inspection, processing, average inspection and calibration in sequence to obtain a cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample.

2. The cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample according to claim 1, characterized in that: Calculated in mass percentage, it includes the following components: Si 9.6-10.1%, Fe 0.114-0.156%, Cu 0.033-0.037%, Mn 0.412-0.438%, Mg 0.0035-0.0188%, Cr 0.0035-0.0045%, Ni 0.0050-0.0060%, Zn 0.0225-0.0375%, Ti 0.071-0.098%, Sr 0.0165-0.0170%, Mo 0.0302-0.128%, Zr 0.140-0.148% and the balance Al.

3. The cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample according to claim 2, characterized in that: In terms of mass percentage, it includes the following components: Si 10.03%, Fe 0.155%, Cu 0.036%, Mn 0.435%, Mg 0.0188%, Cr 0.0044%, Ni0.0057%, Zn 0.0228%, Ti 0.072%, Sr 0.0170%, Mo 0.126%, Zr 0.140% and the balance of Al, Or: Si 9.64%, Fe 0.116%, Cu 0.034%, Mn 0.415%, Mg 0.0037%, Cr 0.0036%, Ni0.0050%, Zn 0.0370%, Ti 0.097%, Sr 0.0166%, Mo 0.0304%, Zr 0.147% and the balance Al.

4. The cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample according to claim 1, characterized in that: The mass of the refining agent used in the refining in step (2) is 1.5‰ of the total mass of the raw material.

5. The cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample according to claim 1, characterized in that: The amount of the aluminum-titanium-boron thin rods used is 1.5‰ of the total mass of the raw materials; the amount of the Al-10% Sr alloy ingots used is 0.0049% of the total mass of the raw materials.

6. The cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample according to claim 1, characterized in that: The filtration in step (4) is carried out in a bipolar filtration device, and the casting is carried out in a hot-top semi-continuous casting device at the same level equipped with a Φ65mm*8 crystallizer.

7. The cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample according to claim 1, characterized in that: The casting speed in step (4) is 200-250 mm / min; the cooling method is water cooling, and the water pressure of the water cooling is 0.04-0.06 MPa.

8. Use of the cast aluminum alloy 411Z.2 as-cast spectrum single-point standard sample according to claims 1 to 7 in a direct reading spectrometer.

9. The use according to claim 8, characterized in that: The application includes working curve correction.

10. The use according to claim 8, characterized in that: The direct-reading spectrometer is a photoelectric direct-reading spectrometer.

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