CN116183324A - Aluminum alloy 8011 component standard sample and preparation method thereof - Google Patents
Aluminum alloy 8011 component standard sample and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of metal materials, and particularly relates to an aluminum alloy 8011 component standard sample and a preparation method thereof. The invention aims to solve the problem that the analysis result is not representative due to the lack of a standard sample which is compared with an analysis sample in the existing 8011 aluminum alloy spectrum and chemical analysis. It consists of Si 0.69-0.72%, fe 0.74-0.76%, cu 0.81-0.84%, mn 0.13-0.15%, mg 0.22-0.24%, cr 0.025-0.027%, ni 0.028-0.031%, zn 0.082-0.085%, ti 0.046-0.048% and Al for the rest. The method comprises the following steps: weighing raw materials; smelting; casting; homogenizing heat treatment. The invention is used for 8011 aluminum alloy spectrum and chemical analysis.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to an aluminum alloy 8011 component standard sample and a preparation method thereof.
Background
The 8XXX series aluminum alloy is pure aluminum alloy added with silicon, iron and a small amount of other elements, mainly pure aluminum has low performance, and ferrosilicon is needed to be added to improve strength, performance index, recrystallization temperature and the like. Most of the application is aluminum foil, and the aluminum foil is generally applied to medical packaging and disposable lunch box packaging. The direct-reading spectrometer for spectrum analysis is also applied to air conditioner cooling fins and the like, the existing direct-reading spectrometer for spectrum analysis is provided with a permanent curve of a required element, after standardization, only an as-cast spectrum single-point standard sample is required to be subjected to curve correction, and because a third element of spectrum analysis has influence on an analysis result, a standard sample with consistent component content and consistent organization state with the analysis sample is required. Therefore, a standard sample of the aluminum alloy 8011 component needs to be developed to meet the spectrum analysis requirements of the aluminum alloy 8011 and the similar aluminum alloys.
The direct-reading spectrometer analysis is simple and efficient, but has the limitation, such as the reasons of larger component segregation, special shape and the like of the product, so that the analysis result is not representative, an ICP analysis method can be adopted at the moment, the ICP method also has the interference of a third element, and the content of a standard sample is required to be consistent with that of an analysis sample, so that the standard sample of the component of the aluminum alloy 8011 is required to be developed so as to meet the chemical analysis requirements of the aluminum alloy 8011 and similar aluminum alloys. However, at present, no method suitable for the standard sample of the aluminum alloy 8011 component exists in the markets at home and abroad.
Disclosure of Invention
The invention aims to solve the problem that the analysis result is not representative due to the lack of a standard sample which is compared with an analysis sample in the existing 8011 aluminum alloy spectrum and chemical analysis, and provides an aluminum alloy 8011 component standard sample and a preparation method thereof.
A standard sample of aluminum alloy 8011 comprises, by mass, 0.69-0.72% of Si, 0.74-0.76% of Fe, 0.081-0.084% of Cu, 0.13-0.15% of Mn, 0.022-0.024% of Mg, 0.025-0.027% of Cr, 0.028-0.031% of Ni, 0.082-0.085% of Zn, 0.046-0.048% of Ti and the balance of Al.
The preparation method of the aluminum alloy 8011 component standard sample is completed by the following steps:
1. weighing: according to the mass percentage, 0.69-0.72% of Si, 0.74-0.76% of Fe, 0.081-0.084% of Cu, 0.13-0.15% of Mn, 0.022-0.024% of Mg, 0.025-0.027% of Cr, 0.028-0.031% of Ni, 0.082-0.085% of Zn, 0.046-0.048% of Ti and the balance of Al are mixed, and aluminum ingots, industrial pure magnesium, industrial pure zinc, alSi20 intermediate alloy, alCu40 intermediate alloy, alMn10 intermediate alloy, alFe10 intermediate alloy, alCr3 intermediate alloy, alTi5B0.2 intermediate alloy and AlNi20 intermediate alloy are respectively weighed as smelting raw materials;
2. smelting: adding an aluminum ingot, industrial pure zinc, an AlSi20 intermediate alloy, an AlCu40 intermediate alloy, an AlMn10 intermediate alloy, an AlFe10 intermediate alloy, an AlCr3 intermediate alloy, an AlTi5B0.2 intermediate alloy and an AlNi20 intermediate alloy into a small smelting furnace, heating to 780-810 ℃, adding a refining agent for slagging after materials in the furnace are completely melted, and adding industrial pure magnesium after slagging is finished to obtain an aluminum alloy solution;
3. casting: introducing the aluminum alloy melt into a holding furnace at 760-790 ℃ and introducing argon, then adding aluminum titanium boron wires at a speed of 90mm/min for purification and refinement, and casting after standing for 30-35 min to obtain an aluminum alloy cast ingot;
4. and (3) placing the aluminum alloy cast ingot into an annealing furnace for homogenizing heat treatment, and then cooling the aluminum alloy cast ingot at room temperature to obtain an aluminum alloy 8011 component standard sample.
The invention has the beneficial effects that:
the aluminum alloy 8011 component standard sample prepared by the method contains Si, fe, cu, mn, mg, cr, ni, zn, ti nine elements, can be suitable for 8011 aluminum alloy, and solves the problem that the multi-element aluminum alloy spectrum and chemical standard sample which are not suitable for 8011 aluminum alloy materials in the domestic and foreign markets and the corresponding preparation method are not available. The standard sample is a standard sample with the same component as the chemical sample in spectrum, and provides a basis for the use of modern instruments and the correction between instruments. The standard sample prepared by the invention meets the requirements of GB/T15000 standard sample working guide and YS/T409 standard sample technical Specification for nonferrous metal product analysis. The method is suitable for 8011 aluminum alloy spectrum and chemical analysis.
Drawings
FIG. 1 is a diagram showing the microstructure of a standard sample of the composition of aluminum alloy 8011 in the examples;
fig. 2 is a physical diagram of a standard sample of the aluminum alloy 8011 composition in the example.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.
The first embodiment is as follows: the aluminum alloy 8011 component standard sample in the embodiment consists of, by mass, 0.69-0.72% of Si, 0.74-0.76% of Fe, 0.081-0.084% of Cu, 0.13-0.15% of Mn, 0.022-0.024% of Mg, 0.025-0.027% of Cr, 0.028-0.031% of Ni, 0.082-0.085% of Zn, 0.046-0.048% of Ti and the balance of Al.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the aluminum alloy 8011 component standard sample consists of 0.703% Si, 0.744% Fe, 0.0821% Cu, 0.144% Mn, 0.0228% Mg, 0.0261% Cr, 0.0293% Ni, 0.083% Zn, 0.0463% Ti and the balance Al according to mass percentage. The other is the same as in the first embodiment.
And a third specific embodiment: the first difference between this embodiment and the specific embodiment is that: aluminum alloy 8011 component standard sample the aluminum alloy 8011 component standard sample consists of, by mass, 0.708% si, 0.751% fe, 0.0829% cu, 0.146% mn, 0.0232% mg, 0.0265% cr, 0.0299% ni, 0.0833% zn, 0.047% ti, and the balance Al. The other is the same as in the first embodiment.
The specific embodiment IV is as follows: the preparation method of the aluminum alloy 8011 component standard sample in the embodiment is completed by the following steps:
1. weighing: according to the mass percentage, 0.69-0.72% of Si, 0.74-0.76% of Fe, 0.081-0.084% of Cu, 0.13-0.15% of Mn, 0.022-0.024% of Mg, 0.025-0.027% of Cr, 0.028-0.031% of Ni, 0.082-0.085% of Zn, 0.046-0.048% of Ti and the balance of Al are mixed, and aluminum ingots, industrial pure magnesium, industrial pure zinc, alSi20 intermediate alloy, alCu40 intermediate alloy, alMn10 intermediate alloy, alFe10 intermediate alloy, alCr3 intermediate alloy, alTi5B0.2 intermediate alloy and AlNi20 intermediate alloy are respectively weighed as smelting raw materials;
2. smelting: adding an aluminum ingot, industrial pure zinc, an AlSi20 intermediate alloy, an AlCu40 intermediate alloy, an AlMn10 intermediate alloy, an AlFe10 intermediate alloy, an AlCr3 intermediate alloy, an AlTi5B0.2 intermediate alloy and an AlNi20 intermediate alloy into a small smelting furnace, heating to 780-810 ℃, adding a refining agent for slagging after materials in the furnace are completely melted, and adding industrial pure magnesium after slagging is finished to obtain an aluminum alloy solution;
3. casting: introducing the aluminum alloy melt into a holding furnace at 760-790 ℃ and introducing argon, then adding aluminum titanium boron wires at a speed of 90mm/min for purification and refinement, and casting after standing for 30-35 min to obtain an aluminum alloy cast ingot;
4. and (3) placing the aluminum alloy cast ingot into an annealing furnace for homogenizing heat treatment, and then cooling the aluminum alloy cast ingot at room temperature to obtain an aluminum alloy 8011 component standard sample.
In the embodiment, the effective crystallization height of the hot top short crystallizer is small, the cooling speed of the cast ingot is improved, the intra-crystal structure of the cast ingot is thinner, the liquid cavity of the cast ingot is shallower, and the transition zone is narrower, so that the density of the cast ingot is improved, and the chemical components are distributed more uniformly along the section of the cast ingot.
In this embodiment, the aluminum ingot is an aluminum ingot of 99.99% or more grade.
In this embodiment, B is not analyzed and is only helpful for the casting process.
Fifth embodiment: the fourth difference between this embodiment and the third embodiment is that: in the second step, the refining agent is RJ1-1 refining agent, and the adding amount is 6-7 kg/t. The other is the same as in the fourth embodiment.
Specific components of the RJ1-1 refining agent according to the present embodiment are referred to YS/T491-2005.
Specific embodiment six: the fourth difference between this embodiment and the third embodiment is that: in the third step, argon is introduced with the purity more than or equal to 99.996 percent and the gas flow rate is 16nm 3 /hr. The other is the same as in the fourth embodiment.
Seventh embodiment: the fourth difference between this embodiment and the third embodiment is that: and in the third step, the adding amount of the aluminum titanium boron wire is 3kg/t. The other is the same as in the fourth embodiment.
Eighth embodiment: the fourth difference between this embodiment and the third embodiment is that: and in the third step, semi-continuous hot top casting is adopted, a hot top short crystallizer with the specification of phi 65mm and the effective height of 8-10 mm is adopted, the casting temperature is 670-700 ℃, the casting speed is 165-180 mm/min, and the cooling water strength is 0.05-0.10 MPa. The other is the same as in the fourth embodiment.
Detailed description nine: the fourth difference between this embodiment and the third embodiment is that: parameters of the homogenization heat treatment in the fourth step: the average fire temperature is 445-480 ℃ and the heat preservation time is 24 hours. The other is the same as in the fourth embodiment.
Detailed description ten: the fourth difference between this embodiment and the third embodiment is that: in the fourth step, the aluminum alloy 8011 component standard sample is in a block shape or a chip shape. The other is the same as in the fourth embodiment.
The following examples are used to verify the benefits of the present invention:
embodiment one: the preparation method of the aluminum alloy 8011 component standard sample is completed by the following steps:
1. weighing: according to the mass percentage, 0.708 percent of Si, 0.751 percent of Fe, 0.0829 percent of Cu, 0.146 percent of Mn, 0.0232 percent of Mg, 0.0265 percent of Cr, 0.0299 percent of Ni, 0.0833 percent of Zn, 0.047 percent of Ti and the balance of Al are proportioned, respectively weighing an aluminum ingot, industrial pure magnesium, industrial pure zinc, alSi20 master alloy, alCu40 master alloy, alMn10 master alloy, alFe10 master alloy, alCr3 master alloy, alTi5B0.2 master alloy and AlNi20 master alloy as smelting raw materials;
2. smelting: adding an aluminum ingot, industrial pure zinc, an AlSi20 intermediate alloy, an AlCu40 intermediate alloy, an AlMn10 intermediate alloy, an AlFe10 intermediate alloy, an AlCr3 intermediate alloy, an AlTi5B0.2 intermediate alloy and an AlNi20 intermediate alloy into a small smelting furnace, heating to 785 ℃, adding a refining agent to carry out slag skimming after materials in the furnace are completely melted, and adding industrial pure magnesium after slag skimming is finished to obtain an aluminum alloy solution;
3. casting: introducing aluminum alloy melt into a heat preservation furnace at 785 ℃ and introducing argon, then adding aluminum titanium boron wires at a speed of 90mm/min for purification and refinement, standing for 35min, and casting by adopting a hot top short crystallizer with a specification of phi 65mm and an effective height of 8-10 mm, wherein the casting temperature is 686 ℃, the casting speed is 170mm/min and the cooling water strength is 0.07MPa, so as to obtain an aluminum alloy cast ingot;
4. and (3) placing the aluminum alloy cast ingot into an annealing furnace for homogenizing heat treatment, wherein the homogenizing temperature is 475 ℃, the heat preservation time is 24 hours, and then cooling the aluminum alloy cast ingot at room temperature to obtain an aluminum alloy 8011 component standard sample.
In the second embodiment, the model of the refining agent is RJ1-1, the specific components refer to YS/T491-2005, and the adding amount is 6Kg/T.
Argon is introduced in the third step of the embodiment: argon purity is more than or equal to 99.996%, and gas flow is 16nm 3 /hr。
In the third step of the embodiment, the adding amount of the aluminum titanium boron wire is 3 Kg/ton of aluminum alloy solution.
The casting described in step three of this example uses a semi-continuous "hot top" casting.
The standard sample of the aluminum alloy 8011 component prepared in the embodiment takes 55-60 mm as a sample at the two ends and the middle after cutting off at least 300mm at each end; the metallographic examination of the sample structure is carried out strictly according to GB/T3246.2-2012 Standard of method for inspecting the macrostructure of deformed aluminum and aluminum alloy products, and the internal structure of the prepared standard sample is compact and has no defects of air holes, slag inclusion and the like as can be seen from figures 1 and 2.
The aluminum alloy 8011 component standard sample prepared in the embodiment is processed into 200-250 samples with phi 55 multiplied by 35mm, then 20 samples are randomly selected, numbered according to the sequence, and spectral standard sample component uniformity inspection is carried out according to the requirements of YS/T409 standard sample technical Specification for nonferrous metal product analysis; checking three different parts on the section of the extracted sample on a photoelectric spectrometer, and counting the variance of the checking result to obtain the component uniformity data of the spectrum standard sample;
the aluminum alloy 8011 component standard sample prepared in the embodiment is processed into aluminum alloy scraps of 1mm, and the processing parameters are as follows: the translation speed of the milling cutter is 45-55 mm/min, the rotation speed of the milling cutter is 55-65 mm/min, the milling chip depth is 0.8-1.2 mm, the aluminum alloy chips are fully and evenly mixed by a quartering method, and the aluminum alloy chips are screened: taking 16-mesh undersize and 32-mesh oversize; 50 g/bottle of chemical sample 200 bottles, randomly extracting 20 bottles, numbering according to the sequence, measuring the element content of the sample according to YS/T409 standard sample technical Specification for nonferrous metal product analysis, and performing chemical standard sample component uniformity inspection, wherein the detection method is shown in Table 1; wherein, the minimum sample weighing amount for the chemical standard sample component uniformity test is 0.1g, and the test result is counted by a variance method.
Table 1 detection method
| Element(s) | Analysis method | Element(s) | Analysis method |
| Si | Silicon molybdenum blue spectrophotometry | Ni | Flame atomic absorption spectrometry |
| Fe | O-phenanthroline spectrophotometry | Zn | Flame atomic absorption spectrometry |
| Cu | Flame atomic absorption spectrometry | Ti | Dianthipine methane spectrophotometry |
| Mn | Potassium periodate spectrophotometry | ||
| Mg | CDTA titration | ||
| Cr | Flame atomic absorption spectrometry |
And (3) setting: (1) Except for northeast light alloy limited liability company, 7 furniture units with standard sample fixed value qualification are specially invited to perform fixed value analysis, and the chemical samples are sent to 7 units to perform fixed value analysis; (2) According to GB/T20975 'aluminum and aluminum alloy chemical analysis method', one or more accurate and reliable analysis methods in the method are selected for carrying out collaborative fixed value analysis and data processing on data reported by each analysis unit; (3) The extremely poor is checked according to the allowable difference of YS/T409 standard sample technical Specification for nonferrous metal product analysis, if abnormal value appears, the original laboratory is required to recheck the suspicious value, and the original value after rechecking and rejecting is summarized and checked to check the normalization of all data by the Charpy-Weilck method.
According to YS/T409 standard sample technical specification for nonferrous metal product analysis, taking the average value of data which is subjected to normal distribution as a single measurement value to form a group of new data, checking whether the data of each group are of equal precision or not by using a Grabbs method, then checking whether the data of each group are of equal precision by using a Ke-clen method, after processing each group of data, calculating the arithmetic average value and standard deviation of each group of data, and carrying out modification on the effective digit of a standard value according to GB8170 data modification rule, wherein the obtained data is the standard value and standard deviation of an aluminum alloy 8011 component standard sample.
The standard values and the extension uncertainties of the aluminum alloy chemical standard samples obtained in the embodiment are shown in table 2, the standard values and the extension uncertainties of the aluminum alloy spectrum standard samples are shown in table 3, and as can be seen from tables 2 and 3, the standard samples prepared in the embodiment are not only suitable for chemical analysis of 8011 aluminum alloy, but also standard samples with the same components as the chemical samples in spectrum, and provide basis for use of modern instruments and correction between instruments.
TABLE 2 Standard values and spread uncertainty for Spectrum Standard samples
TABLE 3 standard values and spread uncertainty for chemical standard samples
Claims (10)
1. The aluminum alloy 8011 component standard sample is characterized by comprising, by mass, 0.69-0.72% of Si, 0.74-0.76% of Fe, 0.081-0.084% of Cu, 0.13-0.15% of Mn, 0.022-0.024% of Mg, 0.025-0.027% of Cr, 0.028-0.031% of Ni, 0.082-0.085% of Zn, 0.046-0.048% of Ti and the balance of Al.
2. An aluminum alloy 8011 composition standard sample according to claim 1, wherein the aluminum alloy 8011 composition standard sample is composed of, by mass, 0.703% si, 0.744% fe, 0.0821% cu, 0.144% mn, 0.0228% mg, 0.0261% cr, 0.0293% ni, 0.083% zn, 0.0463% ti, and the balance Al.
3. An aluminum alloy 8011 composition standard sample according to claim 2, wherein the aluminum alloy 8011 composition standard sample is composed of, by mass, 0.708% si, 0.751% fe, 0.0829% cu, 0.146% mn, 0.0232% mg, 0.0265% cr, 0.0299% ni, 0.0833% zn, 0.047% ti, and the balance Al.
4. The method for preparing the aluminum alloy 8011 component standard sample according to claim 1, wherein the method for preparing the aluminum alloy 8011 component standard sample is completed by the following steps:
1. weighing: according to the mass percentage, 0.69-0.72% of Si, 0.74-0.76% of Fe, 0.081-0.084% of Cu, 0.13-0.15% of Mn, 0.022-0.024% of Mg, 0.025-0.027% of Cr, 0.028-0.031% of Ni, 0.082-0.085% of Zn, 0.046-0.048% of Ti and the balance of Al are mixed, and aluminum ingots, industrial pure magnesium, industrial pure zinc, alSi20 intermediate alloy, alCu40 intermediate alloy, alMn10 intermediate alloy, alFe10 intermediate alloy, alCr3 intermediate alloy, alTi5B0.2 intermediate alloy and AlNi20 intermediate alloy are respectively weighed as smelting raw materials;
2. smelting: adding an aluminum ingot, industrial pure zinc, an AlSi20 intermediate alloy, an AlCu40 intermediate alloy, an AlMn10 intermediate alloy, an AlFe10 intermediate alloy, an AlCr3 intermediate alloy, an AlTi5B0.2 intermediate alloy and an AlNi20 intermediate alloy into a small smelting furnace, heating to 780-810 ℃, adding a refining agent for slagging after materials in the furnace are completely melted, and adding industrial pure magnesium after slagging is finished to obtain an aluminum alloy solution;
3. casting: introducing the aluminum alloy melt into a holding furnace at 760-790 ℃ and introducing argon, then adding aluminum titanium boron wires at a speed of 90mm/min for purification and refinement, and casting after standing for 30-35 min to obtain an aluminum alloy cast ingot;
4. and (3) placing the aluminum alloy cast ingot into an annealing furnace for homogenizing heat treatment, and then cooling the aluminum alloy cast ingot at room temperature to obtain an aluminum alloy 8011 component standard sample.
5. The method for preparing a standard sample of aluminum alloy 8011 ingredients according to claim 4, wherein in the second step, the refining agent is RJ1-1 refining agent, and the adding amount is 6-7 kg/t.
6. The method for preparing a standard sample of aluminum alloy 8011 ingredients according to claim 4, wherein argon is introduced in the third step to have a purity of 99.996% or more and a gas flow of 16nm 3 /hr。
7. The method for preparing a standard sample of aluminum alloy 8011 ingredients according to claim 4, wherein the adding amount of the aluminum titanium boron wire in the third step is 3kg/t.
8. The method for preparing a standard sample of aluminum alloy 8011 ingredients according to claim 4, wherein in the third step, semi-continuous hot top casting is adopted, a hot top short crystallizer with the specification of phi 65mm and the effective height of 8-10 mm is adopted, the casting temperature is 670-700 ℃, the casting speed is 165-180 mm/min, and the cooling water strength is 0.05-0.10 MPa.
9. The method for preparing a standard sample of aluminum alloy 8011 composition according to claim 4, wherein the parameters of the homogenizing heat treatment in the fourth step are as follows: the average fire temperature is 445-480 ℃ and the heat preservation time is 24 hours.
10. The method for preparing a standard sample of aluminum alloy 8011 according to claim 4, wherein in the fourth step, the standard sample of aluminum alloy 8011 is in the form of a block or chip.
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