CN114323849B - Preparation method of cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample - Google Patents
Preparation method of cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample Download PDFInfo
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Abstract
The invention discloses a preparation method of a cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample, which belongs to the technical field of metal materials, wherein the standard sample is prepared by component design, material selection, weighing, smelting, refining and casting, initial inspection and finished product uniformity inspection are uniformly inspected, values are determined, and final component composition data are obtained according to GB8170 data reduction rule, so that the problem that no aluminum alloy 333Z.1 cast spectrum standard sample exists at present is solved. The preparation method is used for preparing the spectrum standard sample suitable for the cast aluminum alloy 333Z.1 aluminum alloy, and the multi-element cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample obtained by the method is used for accurately controlling and detecting the quality of the cast aluminum alloy 333Z.1 aluminum alloy and correcting an instrument.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a preparation method of a cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample.
Background
With the development of modern industry, research and application of cast aluminum alloy are rapidly developed, and the cast aluminum alloy is not only suitable for related industries such as automobiles and machinery, but also relates to the fields of aviation, aerospace and the like. This requires more accurate control of the composition of the cast aluminum alloy.
The control of the components of the cast aluminum alloy is generally carried out by adopting a photoelectric direct-reading spectrometer. Spectroscopic analysis is a relative measurement method, and a standard sample is required to be calibrated in the analysis process for accurate control. As is well known, spectral analysis is mainly influenced by the structural state and a third element, so that a standard sample with the same component content and the same structural state as an analysis sample is needed, and therefore, a standard sample with the same state (as-cast state) and the same component content (single point) needs to be developed for the cast aluminum alloy 333Z.1 standard sample. At present, most of domestic standard samples for analyzing cast aluminum alloy are in a secondary extrusion state; although some parts are in an as-cast state (gravity casting process), the state is consistent with the structure state of the product, but the quality is unstable. And inquiring a standard sample which is not suitable for casting the aluminum alloy 333Z.1 product at a colored information website. Therefore, the cast aluminum alloy 333Z.1 can be detected only by a plurality of standard samples in daily analysis and detection, the accuracy of an analysis result cannot be guaranteed, the working efficiency is reduced, and the detection cost is also improved.
Disclosure of Invention
The invention aims to provide a preparation method of a cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample aiming at the defects in the prior art, the method can be used for preparing the standard sample with good component uniformity, accurate fixed value, good stability and consistent organization state and component content with the product, the accuracy of an analysis result is improved, the working efficiency is improved, the detection cost is reduced, and the domestic blank is filled.
In order to achieve the purpose, the invention provides the following scheme:
a preparation method of a cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample comprises the following steps:
(1) Adding cast aluminum alloy ingots 333Z.1 and 99.7% pure aluminum ingots, industrial pure magnesium, industrial pure zinc, pure lead, pure tin, al-40% Cu, al-10% Mn, al-20% Si, al-10% Fe, al-3% Cr, al-20% Ni and Al-3% Ti into a 1000kg melting furnace for melting, uniformly scattering a refining agent on the melt after the melting is completely finished, refining, slagging and stirring to obtain an aluminum alloy solution, and taking chemical components of the aluminum alloy solution for analysis;
(2) When the chemical composition of the aluminum alloy solution is qualified (the requirement of design composition is met), the aluminum liquid temperature is raised to 740 +/-5 ℃, the aluminum liquid is tilted to a standing furnace of 1000kg, when the aluminum liquid temperature in the standing furnace reaches 740 +/-5 ℃, a refining agent is added to refine the melt, the slag is thoroughly removed, then an argon gas is used for refining and degassing the melt by a graphite rotor refiner, al-Ti-B rods are added during the refining and degassing processes to refine crystal grains, meanwhile, al-10 Sr is added to deteriorate, the slag is removed again after refining, the melt temperature is adjusted to 740 ℃, hydrogen is measured by a reduced pressure density method until the aluminum alloy solution is qualified (the sample block is not provided with obvious pinholes), a chemical composition sample is taken again for analysis, the aluminum alloy solution is stood for 15min, and the aluminum alloy solution is prepared for casting after the composition is qualified;
(3) And (3) carrying out the following steps on the aluminum liquid obtained in the step (2) according to the process parameters: the casting temperature is 700-720 ℃, the casting speed is 250mm/min, and the strength water quantity of the cooling water is 50m 3 /h～60m 3 H is cast to obtain
Total eight aluminum alloy cast bars.
After obtaining the aluminum alloy cast rod, detecting, specifically: (4) After cutting off at least 250mm from two ends of the cast rod obtained in the step (3), respectively taking 40 samples of 20-30 mm from two ends, the middle, 1/4 and 3/4 positions, performing low-power inspection, performing primary inspection on component uniformity according to the requirements of YS/T409 technical Specification for standard samples for analyzing nonferrous metal products, and performing statistics by using a range method;
(5) Processing the qualified casting rods subjected to the low power inspection and the uniformity initial inspection in the step (4) to co-process the casting rods into
Simultaneously processing 800 spectrum standard samples (for value setting) by using representative casting rods (the head, the middle and the tail of any two casting rods are respectively 300 mm), numbering the processed spectrum standard samples in sequence, then randomly extracting 20 spectrum standard samples, carrying out uniformity inspection on three different parts on the section of the extracted sample on a photoelectric direct-reading spectrometer to obtain component uniformity data of the spectrum standard sample, and carrying out statistics by using a variance method;
(6) Performing standard sample valuing on the chemical sample processed in the step (5), performing combined valuing by adopting a plurality of national standard methods of different principles for eight qualified laboratories, wherein each element obtains eight groups of data, each group of 4 independent data, technically judging suspicious values of each element, summarizing and removing the original data after the suspicious values, performing normality test by using a Charperot-Wilck method, testing each group of data which obeys normal or approximate normal by using a Grabas method, removing the suspicious values from mathematical statistics, then testing the equal precision of each group of data by using a Kokren method, finally determining a standard value and an expansion uncertainty (uncertainty synthesis generated by uncertainty and uniformity generated by fixed value), and repairing according to GB8170 data repairing rule.
Further, the smelting temperature in the step (1) is 740 ℃ +/-5 ℃.
Further, the amount of the refining agent in the step (2) is 1.5 per mill relative to the mass of the melt.
Further, the degassing time in the step (2) is 10-20min.
Further, the adding amount of Al-Ti-B rod refined grains in the step (2) relative to the mass of the melt is 1.5 per mill; al-10% Sr 0.0049% based on the mass of the melt.
Further, in the step (3), the bar is cast by using a bipolar filtering device and a homohorizontal hot-top semi-continuous casting device of a crystallizer with the diameter of 65mm multiplied by 8.
The invention also provides a cast aluminum alloy 333Z.1 as-cast state spectrum single-point standard sample prepared by the preparation method of the cast aluminum alloy 333Z.1 as-cast state spectrum single-point standard sample, which contains 0.0049wt% of Sr.
Further, the cast aluminum alloy 333z.1 as-cast spectrum single-point standard sample comprises, by mass, 9.21% of Si, 0.778% of Fe, 2.53% of Cu, 0.280% of Mn, 0.250% of Mg, 0.041% of Cr, 0.053% of Ni, 0.779% of Zn, 0.106% of Ti, 0.037% of Pb, 0.0143% of Sn, 0.0049% of Sr, and the balance of Al.
The invention uses the existing cast aluminum alloy ingot 333Z.1 as raw material, and then uses the following auxiliary materials for component fine adjustment: the Al-Al ingot contains Al99.7% pure Al, mg can be industrial pure Mg, zn can be industrial pure Zn, pb can be pure Pb, sn can be pure Sn, and the high-quality master alloy subjected to segregation test comprises the following components: al-40% Cu, al-10% by weight of Mn, al-20% Si, al-10% by weight of Fe, al-3% by weight of Cr, al-20% by weight of Ni, al-3% by weight of Ti, al-10% by weight of Sr.
The invention also provides application of the cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample in accurate control and detection of the quality of cast aluminum alloy 333Z.1 and correction of an instrument.
The preparation method of the cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample comprises the following process flows: market research → component design → material and tool preparation → smelting → chemical component adjustment → casting of eight cast rods (phi 65mm x 5900 mm) → sampling for metallographic examination and initial examination of cast rod uniformity → wagon processing spectrum standard sample (phi 58mm x 35 mm) and chemical sample (for fixed value) → uniformity examination → fixed value analysis → determination of standard value and expansion uncertainty → comparison with domestic and foreign similar standard samples → production examination.
The invention discloses the following technical effects:
the method can be used for preparing the as-cast spectrum single-point standard sample of the cast aluminum alloy 333Z.1, the spectrum standard sample of the 333Z.1 cast aluminum alloy prepared by the method contains thirteen elements of Si, fe, cu, mn, mg, cr, ni, zn, ti, pb, sn, sr and Al, and can be applied to accurate analysis of the cast aluminum alloy 333Z.1, and the problem that no multi-element cast aluminum alloy spectrum standard sample with the organization state and the component content consistent with those of the cast aluminum alloy 333Z.1 exists in markets at home and abroad and a corresponding preparation method is solved. The composition is also suitable for controlling the compositions of cast aluminum alloys of 380Y.1, 380Y.2 and other brands, and has wide application range. The multi-element casting aluminum alloy 333Z.1 as-cast spectrum single-point standard sample obtained by the method can be used for accurate control, detection and instrument correction of the quality of casting aluminum alloy 333Z.1. The standard sample developed by the invention meets the requirements of GB/T15000 Standard sample guide rules for working and YS/T409 Standard sample technical Specification for analyzing nonferrous metal products.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a metallographic map of the structure state of a single-point standard sample of as-cast spectrum of 333Z.1 cast aluminum alloy of example 1;
FIG. 2 is metallographic atlas of 333Z.1 brand product structure state.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in the present disclosure, it is understood that each intervening value, to the upper and lower limit of that range, is also specifically disclosed. Every intervening value, to the extent any stated value or intervening value in a stated range, and any other stated or intervening value in a stated range, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
The invention is designed according to the requirement range of the GB/T8733-2016 cast aluminum alloy ingot on the chemical components of 333Z.1 and can meet the requirements of the product components of enterprises. Since this cast aluminum alloy is modified with strontium, the Sr design is added to the composition design. The composition of 333Z.1 in GB/T8733-2016 is shown in Table 1.
333Z.1 aluminum alloy chemical composition (%) -specified in Table 1 GB/T8733-2016
Cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample in the implementation not only meets the standard range, but also is close to the product components, and specifically comprises the following design components in percentage by mass: 9.21 percent of Si, 0.778 percent of Fe, 2.53 percent of Cu, 0.280 percent of Mn, 0.250 percent of Mg, 0.041 percent of Cr, 0.053 percent of Ni, 0.779 percent of Zn, 0.106 percent of Ti, 0.037 percent of Pb, 0.0143 percent of Sn, 0.0049 percent of Sr and the balance of Al.
The method comprises the following steps: the existing cast aluminum alloy ingot 333Z.1 is used as a raw material, and then the following materials are used for regulation: 99.7% pure aluminum ingots for Al, industrial pure magnesium for Mg, industrial pure zinc for Zn, pure lead for Pb and pure tin for Sn, and the high-quality master alloys subjected to segregation test are as follows: al-40% Cu, al-10% Mn, al-20% Si, al-10% Fe, al-3% Cr, al-20% Ni, al-3% Ti, al-10% Sr.
Step two: converting the mass percentages of the design components into the mass of the selected raw materials and auxiliary materials to be weighed, and weighing;
step three: adding weighed cast aluminum alloy ingots 333Z.1 and 99.7 percent of pure aluminum ingots, industrial pure magnesium, industrial pure zinc, pure lead and pure tin, al-40 percent of Cu, al-10 percent of Mn, al-20 percent of Si, al-10 percent of Fe, al-3 percent of Cr, al-20 percent of Ni and Al-3 percent of Ti into a 1000kg smelting furnace for smelting, wherein the temperature of the smelted aluminum liquid is 740 +/-5 ℃, after the furnace charge is completely melted, uniformly scattering a refining agent on the melt for refining, slagging off and stirring to obtain an aluminum alloy solution (aluminum liquid), adding the refining agent according to 1.5 per thousand of the mass of the melt, and taking chemical component samples for analysis (to ensure that the chemical component samples meet the design component requirements);
step four, when the chemical components of the aluminum liquid in the step three are analyzed to be qualified (the aluminum liquid meets the design component requirements), the aluminum liquid is tilted to enter a standing furnace of 1000kg when the temperature of the aluminum liquid is raised to 740 +/-5 ℃. When the temperature of the molten aluminum in the standing furnace reaches 740 +/-5 ℃, refining the melt by using 1.5 per mill refining agent (consisting of 20 percent of potassium fluoroaluminate, 10 percent of sodium chloride and 70 percent of potassium chloride in percentage by mass) and completely slagging off, then refining the melt by using a graphite rotor refiner for 15min by using argon, adding 1.5 per mill Al-Ti-B rods in the refining process to refine crystal grains, and adding Al-10 Sr for modification at the moment. And (3) slagging off again after refining, adjusting the temperature of the melt to 740 ℃, measuring hydrogen by adopting a reduced pressure density method until the melt is qualified (no obvious pinhole exists in the detection of the sampled block), taking a chemical component sample again, analyzing, and standing for 15min. And (4) after the components are qualified, checking that all the casting systems are normal, and starting to prepare for casting.
5. Bipolar filtering device for aluminum liquid obtained in step four and
the same-level hot top semi-continuous casting device of the crystallizer comprises the following process parameters: the casting temperature is 700-720 ℃, the casting speed is 250mm/min, and the strength water quantity of the cooling water is 50m 3 /h～60m 3 H is cast to obtain
Total eight aluminum alloy cast bars.
6. Checking the component uniformity of a cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample: and (4) inspecting the uniformity of components according to the requirements of GB/T15000 standard sample operating guide and YS/T409 standard sample technical specification for analyzing nonferrous metal products, cutting off at least 250mm from two ends of the cast rod obtained in the fifth step, respectively taking 40 samples of 20-30 mm from two ends, the middle, 1/4 and 3/4 positions, performing low-power inspection, performing initial inspection on the uniformity of the components according to the requirements of YS/T409 standard sample technical specification for analyzing the nonferrous metal products, and performing statistics by an extreme difference method.
7. And (4) processing the casting rods qualified by the low power inspection and the uniformity initial inspection in the step six to obtain 800 blocks of phi 58 multiplied by 35mm spectrum standard samples, and simultaneously processing chemical samples (for fixed values) by using representative casting rods (the head, the middle and the tail of any two casting rods are respectively 300 mm). Numbering the processed spectrum standard samples in sequence, then randomly extracting 20 spectrum standard samples, checking three different parts on the section of the extracted sample on an optoelectronic direct-reading spectrometer to obtain the component uniformity data of the spectrum standard sample, and counting by using a variance method.
8. And (3) carrying out standard sample value setting on the chemical sample processed in the step seven, carrying out combined value setting by adopting eight national standard methods with different principles for laboratories with standard sample value setting qualification, and selecting one or more accurate and reliable analysis methods in the methods according to GB/T20975 chemical analysis methods for aluminum and aluminum alloy to carry out cooperative value setting analysis and data processing on data reported by each analysis unit. Eight sets of data were obtained, with 4 independent data per set. First, a technical determination of suspicious values is carried out. The range of the method is checked according to the allowable difference of GB/T20975 chemical analysis method for aluminum and aluminum alloy, whether abnormal values exist in the group is checked, if the abnormal values exist, an original laboratory is required to recheck suspicious values, and original data after the suspicious values are removed in a gathering mode are subjected to normality test by using a Charulo-Wilck method. Taking the average value of data which obeys normal distribution as a single measurement value, forming a group of new data, and checking whether the precision among the groups of data is equal or not by using a Grabbs method and then using a Koclen method. Finally determining a standard value and an expansion uncertainty (uncertainty generated by a fixed value and uncertainty generated by uniformity) through the tests, and carrying out reduction according to the rule of G8170 data reduction rule. The standard values and the expansion uncertainties of the as-cast single-point standard sample of 333z.1 cast aluminum alloy of this example are shown in table 2.
TABLE 2 cast aluminum alloy 333Z.1 as-cast spectral single point standard sample values (%) and extended uncertainties (%)
The fixed value result completely meets the design requirement and meets the product analysis requirement.
The comparison data of the cast aluminum alloy 333z.1 as-cast spectrum single-point standard sample and the similar domestic and foreign standard samples in the embodiment is shown in table 3.
TABLE 3 comparison of the extended uncertainty with similar standard samples at home and abroad
By comparing uncertainty data, the level of national standard samples and foreign standard samples is completely achieved.
The metallographic structure of a single-point standard sample of as-cast spectrum of the cast aluminum alloy 333Z.1 of the embodiment is shown in figure 1, and the metallographic structure of a product of 333Z.1 brand is shown in figure 2.
As can be seen from fig. 1 and 2, the organization state of the developed single-point standard sample is close to the organization state of the product.
And (3) stability detection: three times of detection are carried out in one year, various conditions are controlled as much as possible each time, the conditions are consistent, and the measurement result mainly reflects part of errors caused by material change. The precision of the measurement was less than the precision of the assay, and the standard was considered stable over the time interval, and the results are shown in table 4.
TABLE 4
Through the detection: the invention has the advantages of closer component content to the product content, good uniformity and accurate fixed value. The metallographic phase atlas proves that the structure state is closer to that of the product. It is well known that aluminum alloys have good stability due to a dense oxide layer. Meets the development requirements of standard samples. The uncertainty comparison with domestic and foreign standard samples achieves the advanced level of the domestic standard and the foreign standard, fills the domestic blank and achieves the aim of the invention.
The above-described embodiments are only intended to illustrate the preferred embodiments of the present invention, and not to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (7)
1. A preparation method of a cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample is characterized by comprising the following steps:
(1) Casting aluminum alloy ingots 333Z.1 and 99.7% pure aluminum ingots, industrial pure magnesium, industrial pure zinc, pure lead, pure tin, al-40% Cu, al-10% Mn, al-20% Si, al-10% Fe, al-3% Cr, al-20% Ni and Al-3% Ti into a melting furnace, melting, after complete melting, scattering a refining agent, refining, slagging, stirring to obtain an aluminum alloy solution, and taking chemical components of the aluminum alloy solution for analysis;
(2) When the chemical components of the aluminum alloy solution are analyzed to be qualified, the aluminum liquid is raised to 740 +/-5 ℃, the aluminum liquid is tilted to a standing furnace, when the temperature of the aluminum liquid in the standing furnace reaches 740 +/-5 ℃, a refining agent is added to refine the melt, slag is thoroughly removed, the melt is refined and degassed, al-Ti-B rods are added to refine grains in the refining and degassing processes, al-10 Sr is added to deteriorate, slag is removed again after refining, the temperature of the melt is adjusted to 740 ℃, hydrogen is measured by a reduced pressure density method until the aluminum liquid is qualified, a chemical component sample is taken again for analysis, the aluminum liquid is stood for 15min, and the aluminum liquid is prepared for casting after the components are qualified;
(3) And (3) carrying out the following steps on the aluminum liquid obtained in the step (2) according to the process parameters: the casting temperature is 700-720 ℃, the casting speed is 250mm/min, and the strength water amount of the cooling water is 50m 3 /h-60m 3 H is cast to obtain
An aluminum alloy cast bar;
the cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample comprises, by mass, 9.21% of Si, 0.778% of Fe, 2.53% of Cu, 0.280% of Mn, 0.250% of Mg, 0.041% of Cr, 0.053% of Ni, 0.779% of Zn, 0.106% of Ti, 0.037% of Pb, 0.0143% of Sn, 0.0049% of Sr and the balance of Al.
2. The method for preparing the as-cast spectrum single-point standard sample of the cast aluminum alloy 333z.1 as claimed in claim 1, wherein the melting temperature in step (1) is 740 ℃ ± 5 ℃.
3. The method for preparing the as-cast spectrum single-point standard sample of the cast aluminum alloy 333z.1 as claimed in claim 1, wherein the refining agent is used in an amount of 1.5% per mill relative to the mass of the melt in the step (2).
4. The method for preparing the as-cast spectrum single-point standard sample of the cast aluminum alloy 333z.1 as claimed in claim 1, wherein the degassing time in step (2) is 10-20min.
5. The method for preparing the as-cast spectrum single-point standard sample of the cast aluminum alloy 333z.1 as claimed in claim 1, wherein the addition amount of the Al-Ti-B rod refined grains in the step (2) is 1.5% per mill relative to the mass of the melt; al-10% Sr 0.0049% based on the mass of the melt.
6. The method for preparing the as-cast spectrum single-point standard sample of the aluminum alloy 333z.1 according to claim 1, wherein the step (3) is performed by using a bi-polar filter apparatus and a co-level hot-top semi-continuous casting apparatus with a crystallizer of phi 65mm x 8.
7. Use of the as-cast aluminum alloy 333z.1 single-point standard sample for as-cast spectroscopy prepared by the preparation method of any one of claims 1 to 6 for accurate control, detection and instrument calibration of the quality of cast aluminum alloy 333z.1.
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