CN114323849A - 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 an as-cast spectrum single-point standard sample of cast aluminum alloy 333Z.1, which belongs to the technical field of metal materials, and is characterized in that the standard sample is prepared by component design, material selection, weighing, smelting, refining and casting, the initial inspection and finished product uniformity inspection are uniformly inspected, the value is determined, and the final component composition data is obtained according to the revision of GB8170 data revision rule, so that the problem that no aluminum alloy spectrum standard sample suitable for cast aluminum alloy 333Z.1 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 state 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 that requires calibration of a standard sample during analysis to allow accurate control. Since it is known that spectral analysis is mainly affected by the texture state and the third element, a standard sample having the same composition content and texture state as the analysis sample is more required, and therefore, a standard sample of the cast aluminum alloy 333Z.1 needs to be developed, which has the same texture (as-cast condition) and composition content (single point). 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 quality is not stable, and the state is consistent with the structure state of the product. No standard samples suitable for cast aluminum alloy 333Z.1 products were queried at the color information website. Therefore, several standard samples are needed in daily analysis and detection to finish the detection of the cast aluminum alloy 333Z.1, the accuracy of an analysis result cannot be guaranteed, the working efficiency is reduced, and the detection cost is also increased.
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 tissue 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 ingot 333Z.1, 99.7% pure aluminum ingot, 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 smelting furnace for smelting, after complete melting, uniformly scattering a refining agent on the melt for refining, skimming and stirring to obtain an aluminum alloy solution, and analyzing the chemical components of the aluminum alloy solution;
(2) when the chemical components of the aluminum alloy solution are analyzed to be qualified (the requirement of design components is met), the aluminum liquid is heated to 740 +/-5 ℃, the aluminum liquid is tilted to a standing furnace of 1000kg, when the temperature of the aluminum liquid in the standing furnace reaches 740 +/-5 ℃, a refining agent is added to refine the melt, the slag is thoroughly removed, then a graphite rotor refiner is used for refining and degassing the melt by adopting argon, Al-Ti-B rods are added in 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 temperature of the melt is adjusted to 740 ℃, hydrogen is measured by adopting a reduced pressure density method until the aluminum liquid is qualified (a sampled block has no obvious pinhole), 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 quantity of the cooling water is 50m3/h～60m3H is cast to obtain
Total eight aluminum alloy cast bars.
After the aluminum alloy cast rod is obtained, detection is carried out, and the method specifically comprises the following steps: (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 the two ends, the middle, 1/4 and 3/4, carrying out low-power inspection, carrying out primary inspection on component uniformity according to the requirements of YS/T409 technical Specification for standard samples for analyzing nonferrous metal products, and carrying out statistics by using a range difference 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 determination) by using representative casting rods (300 mm is taken at the head, the middle and the tail of any two casting rods), 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 spectrum standard sample component uniformity data, and carrying out statistics by using a variance method;
(6) carrying out standard sample value determination on the chemical sample processed in the step (5), carrying out combined value determination by adopting eight qualified laboratories with various national standard methods with different principles, wherein each element obtains eight groups of data in total, each group has 4 independent data, technically judging suspicious values of each element, summarizing and removing the suspicious values, carrying out normality test on the original data 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, testing the equal precision of each group of data by using a Kokern method, finally determining a standard value and an expanded uncertainty (uncertainty generated by the fixed value and uncertainty generated by uniformity are synthesized) through the tests, and carrying out reduction according to GB8170 data reduction 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 10-20 min.
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; the amount of Al-10% Sr added relative to the mass of the melt was 0.0049%.
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 single-point standard sample of as-cast spectrum, which contains 0.0049 wt% of Sr and is prepared by the preparation method of the cast aluminum alloy 333Z.1 single-point standard sample of as-cast spectrum.
Further, the as-cast spectrum single-point standard sample of the cast aluminum alloy 333Z.1 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 fine adjustment of components: the aluminum ingot contains 99.7 percent of pure aluminum, Mg can be industrially pure magnesium, Zn can be industrially pure zinc, Pb can be pure lead, Sn can be pure tin, and the high-quality master alloy subjected to segregation test is as follows: al-40% of Cu, Al-10% of Mn, Al-20% of Si, Al-10% of Fe, Al-3% of Cr, Al-20% of Ni, Al-3% of Ti and Al-10% of Sr.
The invention also provides application of the cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample in accurate control, detection and instrument correction of the quality of the cast aluminum alloy 333Z.1 aluminum alloy.
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 into eight cast rods (phi 65mm x 5900mm) → sampling for metallographic examination and initial examination of cast rod uniformity → wagon processing spectrum standard sample (phi 58mm x 35mm) and chemical sample (for fixed value) → uniformity examination → fixed value analysis → fixed value and expanded uncertainty → comparison with domestic and foreign 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 333Z.1 spectral standard sample of the 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 the accurate analysis of the 333Z.1 of the cast aluminum alloy, and the problem that no multi-element spectral standard sample of the cast aluminum alloy with the structure state and the component content consistent with those of the 333Z.1 in domestic and foreign markets and a corresponding preparation method are solved. The composition is also suitable for controlling the composition of cast aluminum alloys of grades such as 380Y.1, 380Y.2 and the like, and has wide application range. The multi-element cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample obtained by the method can be used for accurate control and detection of the quality of the cast aluminum alloy 333Z.1 and correction of instruments. 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 phase diagram of a structure state of a single-point standard sample of an as-cast spectrum 333Z.1 of cast aluminum alloy in example 1;
FIG. 2 is a metallographic map of the structure state of a 333Z.1 brand product.
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. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between 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 GB/T8733-2016 cast aluminum alloy ingot on 333Z.1 chemical composition during composition design, and can meet the requirements of enterprise product composition. Since this cast aluminum alloy is modified with strontium, the Sr design is added to the composition design. The 333Z.1 content of GB/T8733-2016 is shown in Table 1.
TABLE 1 GB/T8733-2016 Specification 333Z.1 aluminum alloy chemical composition (%)
The 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 was used as a raw material, and then the following materials were used for adjustment: 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% of Cu, Al-10% of Mn, Al-20% of Si, Al-10% of Fe, Al-3% of Cr, Al-20% of Ni, Al-3% of Ti and Al-10% of 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: weighing 333Z.1 cast aluminum alloy ingots, 99.7% pure aluminum ingots, industrial pure magnesium, industrial pure zinc, pure lead and pure tin, wherein Al-40% of Cu, Al-10% of Mn, Al-20% of Si, Al-10% of Fe, Al-3% of Cr, Al-20% of Ni and Al-3% of Ti are added into a 1000kg smelting furnace for smelting, the temperature of the molten aluminum is 740 +/-5 ℃, when furnace burden is completely melted, refining agent is uniformly scattered on the melt for refining, slagging-off and stirring to obtain aluminum alloy solution (aluminum liquid), the refining agent is added according to 1.5 per mill of the melt mass, and chemical component samples are taken for analysis (so as to 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 molten aluminum in a standing furnace reaches 740 +/-5 ℃, refining the melt by using 1.5 per mill refining agent (which consists of 20 percent of potassium fluoroaluminate, 10 percent of sodium chloride and 70 percent of potassium chloride in percentage by mass) and thoroughly skimming the slag, then refining the melt by using argon gas for 15min by using a graphite rotor refiner, adding 1.5 per mill Al-Ti-B rods in the refining process to refine grains, and adding Al-10 percent of 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 15 min. And (4) after the components are qualified, checking that all the casting systems are normal, and starting to prepare for casting.
Fifthly, the bipolar filtering device for the aluminum liquid obtained in the 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 50m3/h～60m3H is cast to obtain
Total eight aluminum alloy cast bars.
Sixthly, checking the component uniformity of the cast aluminum alloy 333Z.1 as-cast spectrum single-point standard sample: and (3) checking the component uniformity 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 step five, respectively taking 40 samples of 20-30 mm from two ends and the middle, 1/4 and 3/4, performing low-power check, performing initial component uniformity check according to the requirements of YS/T409 Standard sample technical Specification for analyzing nonferrous metal products, and performing statistics by using a range difference method.
Seventhly, processing the casting rods qualified by the low power inspection and the uniformity initial inspection in the step six to obtain 800 blocks of spectrum standard samples with the diameter of 58 multiplied by 35mm, and simultaneously processing chemical samples (for fixed values) by 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.
Eighthly, valuing the standard sample of the chemical sample processed in the step seven, jointly valuating by adopting eight national standard methods with different principles for laboratories with standard sample valuing qualification, and performing collaborative value-fixing analysis and data processing on data reported by each analysis unit by selecting one or more accurate and reliable analysis methods in the methods according to GB/T20975 aluminum and aluminum alloy chemical analysis method. Eight sets of data were obtained, with 4 independent data per set. First, a technical suspicious value determination is performed. 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 the 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 extended uncertainties of the as-cast single-point standard samples of the cast aluminum alloy 333Z.1 of this example are shown in Table 2.
TABLE 2 Standard value (%) and extended uncertainty (%) of as-cast spectrum single point standard sample of cast aluminum alloy 333Z.1
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 of the embodiment and the similar domestic and foreign standard samples are 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 the cast aluminum alloy 333Z.1 single-point standard sample with as-cast spectrum in the embodiment is shown in FIG. 1, and the metallographic structure of the product with 333Z.1 trademark is shown in FIG. 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 merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
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 ingot 333Z.1, 99.7% pure aluminum ingot, 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 smelting furnace, smelting, after complete melting, scattering a refining agent, refining, slagging off and stirring to obtain an aluminum alloy solution, and analyzing chemical components of the aluminum alloy solution;
(2) when the chemical components of the aluminum alloy solution are qualified by analysis, the aluminum liquid is tilted to a standing furnace when the temperature of the aluminum liquid is increased to 740 +/-5 ℃, a refining agent is added to refine the melt when the temperature of the aluminum liquid in the standing furnace reaches 740 +/-5 ℃, slag is completely 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 melt is qualified, a chemical component sample is taken again for analysis, the chemical component sample is placed for 15min, and casting is prepared 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 quantity of the cooling water is 50m3/h-60m3H is cast to obtain
An aluminum alloy cast bar.
2. The method for preparing the as-cast spectrum single-point standard sample of aluminum alloy 333Z.1 of claim 1, wherein the smelting temperature in step (1) is 740 ℃ ± 5 ℃.
3. The method for preparing the as-cast spectrum single-point standard sample of 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 step (2).
4. The method for preparing the as-cast spectrum single-point standard sample of aluminum alloy 333Z.1 of claim 1, wherein the degassing time in step (2) is 10-20 min.
5. The method for preparing the as-cast spectrum single-point standard sample of the cast aluminum alloy 333Z.1 of claim 1, wherein the Al-Ti-B rod refined grains added in step (2) are 1.5% o relative to the mass of the melt; the amount of Al-10% Sr added relative to the mass of the melt was 0.0049%.
6. The method for preparing the as-cast spectrum single-point standard sample of aluminum alloy 333Z.1 according to claim 1, wherein the step (3) comprises casting the ingot with a bi-polar filter and a hot-top semi-continuous casting apparatus having a crystallizer with a diameter of 65mm x 8.
7. The method of making the as-cast single-point spectrum standard for the as-cast aluminum alloy 333Z.1 of claim 1, wherein the as-cast single-point spectrum standard for the as-cast aluminum alloy 333Z.1 comprises 0.0049 wt% Sr.
8. The as-cast spectrum single-point standard sample of aluminum alloy 333Z.1 of claim 7, wherein the composition, in mass percent, is Si 9.21%, Fe 0.778%, Cu 2.53%, Mn 0.280%, Mg 0.250%, Cr 0.041%, Ni 0.053%, Zn 0.779%, Ti 0.106%, Pb 0.037%, Sn 0.0143%, Sr 0.0049%, and balance Al.
9. Use of the as-cast aluminum alloy 333Z.1 single-point standard sample of as-cast spectrum of claim 8 for accurate control, inspection and instrumental calibration of the quality of cast aluminum alloy 333Z.1 aluminum alloy.
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