Aluminum alloy 8a02 component standard sample and preparation method thereof

Abstract

The application relates to an aluminum alloy 8A02 component standard sample and a preparation method thereof, and belongs to the technical field of metal materials, in particular to an aluminum alloy 8A02 component standard sample and a preparation method thereof. The application aims at solving the problem that the existing 8A02 aluminum alloy spectrum and chemical analysis lacks standard samples for comparison with analysis samples, and the analysis result is not representative. The application is composed of 0.096-0.100% Si, 0.077-0.080% Fe, 0.0083-0.0087% Cu, 0.0048-0.0050% Mn, 0.027-0.029% Mg, 0.0047-0.0049% Cr, 0.0047-0.0050% Ni, 0.035-0.037% Zn, 0.0032-0.0034% Ti, 0.177-0.181% Sn, 0.241-0.245% Bi, and the balance of Al. The method comprises the following steps: weighing raw materials, melting, casting and homogenizing heat treatment. The standard sample is a standard sample with the same component as the spectrum and chemical sample, and provides a basis for the use of modern instruments and the calibration between instruments. The prepared aluminum alloy 8A02 component standard sample is used for the spectrum and chemical analysis of the 8A02 aluminum alloy.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of metal materials, and particularly relates to an aluminum alloy 8A02 component standard sample and a preparation method thereof. BACKGROUND

[0002] 8XXX series aluminum alloy is a pure aluminum alloy added with silicon, iron and a small amount of other elements. The performance of pure aluminum is low, and silicon and iron are added to improve strength, performance index, recrystallization temperature and the like. Most applications are aluminum foil, heat exchanger strip, electric water heater sacrificial anode and the like. The existing direct-reading spectrometer for spectral analysis is provided with a required element permanent curve. After standardization, only the cast-state spectral single-point standard sample is needed to perform curve correction. Since the third element of spectral analysis has an influence on the analysis result, a standard sample consistent with the component content and the organization state of the analysis sample is more needed. Therefore, the aluminum alloy 8A02 component standard sample needs to be developed to meet the spectral analysis needs of the aluminum alloy 8A02 and similar aluminum alloys.

[0003] Although the direct-reading spectrometer analysis is simple and efficient, it has limitations. For example, the product component segregation is large, the shape is special, and the like, so that the analysis result is not representative. At this time, the ICP analysis method can be used. The ICP method also has the interference of the third element, and the component content of the standard sample needs to be consistent with that of the analysis sample. Therefore, the aluminum alloy 8A02 component standard sample needs to be developed to meet the chemical analysis needs of the aluminum alloy 8A02 and similar aluminum alloys. However, there is no method suitable for the aluminum alloy 8A02 component standard sample on the market at home and abroad at present. SUMMARY

[0004] The application aims to solve the problem that the existing 8A02 aluminum alloy spectral and chemical analysis lacks a standard sample for comparison with the analysis sample, resulting in that the analysis result is not representative, and provides an aluminum alloy 8A02 component standard sample and a preparation method thereof.

[0005] An aluminum alloy 8A02 component standard sample is composed of 0.096-0.100% Si, 0.077-0.080% Fe, 0.0083-0.0087% Cu, 0.0048-0.0050% Mn, 0.027-0.029% Mg, 0.0047-0.0049% Cr, 0.0047-0.0050% Ni, 0.035-0.037% Zn, 0.0032-0.0034% Ti, 0.177-0.181% Sn, 0.241-0.245% Bi and the balance of Al in terms of mass percentage.

[0006] The preparation method of the aluminum alloy 8A02 component standard sample is completed according to the following steps:

[0007] I. Weighing: according to the mass percentage of 0.096-0.100% Si, 0.077-0.080% Fe, 0.0083-0.0087% Cu, 0.0048-0.0050% Mn, 0.027-0.029% Mg, 0.0047-0.0049% Cr, 0.0047-0.0050% Ni, 0.035-0.037% Zn, 0.0032-0.0034% Ti, 0.177-0.181% Sn, 0.241-0.245% Bi and the balance of Al, the aluminum ingot, industrial pure magnesium, industrial pure zinc, industrial pure tin, AlSi20 intermediate alloy, AlCu40 intermediate alloy, AlMn10 intermediate alloy, AlFe10 intermediate alloy, AlCr3 intermediate alloy, AlTi5B0.2 intermediate alloy, AlNi20 intermediate alloy and AlBi5 intermediate alloy are weighed as smelting raw materials;

[0008] II. Smelting: the aluminum ingot, industrial pure zinc, industrial pure tin, AlSi20 intermediate alloy, AlCu40 intermediate alloy, AlMn10 intermediate alloy, AlFe10 intermediate alloy, AlCr3 intermediate alloy, AlNi20 intermediate alloy and AlBi5 intermediate alloy weighed in step I are added into a smelting furnace, and the temperature is raised to 770-790 DEG C, when the materials in the furnace are completely melted, the refining agent is added to remove slag, after the slag removal is finished, the industrial pure magnesium is added, and the aluminum alloy solution is obtained;

[0009] III. Casting: the aluminum alloy melt obtained in step II is introduced into a holding furnace at 750-780 DEG C and argon is introduced, then the AlTi5B0.2 intermediate alloy is added at a speed of 90mm / min to purify and refine, and is placed for 30-35min, then casting is carried out, and the aluminum alloy ingot is obtained;

[0010] IV. The aluminum alloy ingot obtained in step III is placed into an annealing furnace for homogenization heat treatment, and then is cooled at room temperature, and the aluminum alloy 8A02 component standard sample is obtained.

[0011] The present application has the beneficial effects that:

[0012] The aluminum alloy 8A02 component standard sample prepared by the method has Si, Fe, Cu, Mn, Mg, Cr, Ni, Zn, Ti, Sn and Bi eleven elements, can be applied to the 8A02 aluminum alloy, solves the problem that there is no multi-element aluminum alloy spectroscopy and chemical standard sample and corresponding preparation method suitable for the 8A02 aluminum alloy material in the domestic and foreign markets. The standard sample is a spectroscopy and chemical sample with the same component, which provides a basis for the use of modern instruments and the calibration between instruments. The standard sample prepared by the method meets the requirements of GB / T 15000 "Standard Sample Work Guide" and YS / T 409 "Technical Specification for Standard Sample for Non-ferrous Metal Product Analysis".

[0013] The aluminum alloy 8A02 component standard sample prepared by the method is used for 8A02 aluminum alloy spectroscopy and chemical analysis. BRIEF DESCRIPTION OF DRAWINGS

[0014] Figure 1 is a low-magnification microstructure diagram of the aluminum alloy 8A02 component standard sample in Example 1;

[0015] Figure 2 is a physical diagram of the aluminum alloy 8A02 component standard sample in Example 1. DETAILED DESCRIPTION

[0016] Specific embodiment one: the aluminum alloy 8A02 component standard sample in the embodiment is composed of 0.096-0.100% Si, 0.077-0.080% Fe, 0.0083-0.0087% Cu, 0.0048-0.0050% Mn, 0.027-0.029% Mg, 0.0047-0.0049% Cr, 0.0047-0.0050% Ni, 0.035-0.037% Zn, 0.0032-0.0034% Ti, 0.177-0.181% Sn, 0.241-0.245% Bi and the balance of Al in terms of mass percentage.

[0017] Specific embodiment two: the aluminum alloy 8A02 component standard sample in the embodiment is composed of 0.0965% Si, 0.0772% Fe, 0.00834% Cu, 0.00482% Mn, 0.0274% Mg, 0.00473% Cr, 0.00471% Ni, 0.0351% Zn, 0.00322% Ti, 0.177% Sn, 0.241% Bi and the balance of Al in terms of mass percentage. The other is the same as that in specific embodiment one.

[0018] Detailed implementation three: the aluminum alloy 8A02 composition standard sample aluminum alloy 8A02 composition standard sample is composed of 0.0997% Si, 0.0799% Fe, 0.00872% Cu, 0.00503% Mn, 0.0294% Mg, 0.00487% Cr, 0.00501% Ni, 0.0368% Zn, 0.00338% Ti, 0.181% Sn, 0.245% Bi and the balance of Al in mass percent. The others are the same as in detailed implementation one or two.

[0019] Detailed implementation four: the preparation method of the aluminum alloy 8A02 composition standard sample in this embodiment is completed by the following steps:

[0020] I. Weighing: ingredients are prepared according to 0.096-0.100% Si, 0.077-0.080% Fe, 0.0083-0.0087% Cu, 0.0048-0.0050% Mn, 0.027-0.029% Mg, 0.0047-0.0049% Cr, 0.0047-0.0050% Ni, 0.035-0.037% Zn, 0.0032-0.0034% Ti, 0.177-0.181% Sn, 0.241-0.245% Bi and the balance of Al in mass percent, and aluminum ingots, industrial pure magnesium, industrial pure zinc, industrial pure tin, AlSi20 intermediate alloy, AlCu40 intermediate alloy, AlMn10 intermediate alloy, AlFe10 intermediate alloy, AlCr3 intermediate alloy, AlTi5B0.2 intermediate alloy, AlNi20 intermediate alloy and AlBi5 intermediate alloy are weighed as smelting raw materials;

[0021] II. Smelting: the aluminum ingots, industrial pure zinc, industrial pure tin, AlSi20 intermediate alloy, AlCu40 intermediate alloy, AlMn10 intermediate alloy, AlFe10 intermediate alloy, AlCr3 intermediate alloy, AlNi20 intermediate alloy and AlBi5 intermediate alloy weighed in step I are added to a smelting furnace, and the temperature is raised to 770-790°C. After the materials in the furnace are completely melted, a refining agent is added for slagging. After the slagging is completed, industrial pure magnesium is added to obtain an aluminum alloy solution;

[0022] III. Casting: the aluminum alloy melt obtained in step II is introduced into a holding furnace at 750-780°C and argon is introduced, and then AlTi5B0.2 intermediate alloy is added at a speed of 90 mm / min for purification and refinement. After standing for 30-35 min, casting is performed to obtain an aluminum alloy ingot;

[0023] Four, the aluminum alloy ingot obtained in step three is put into an annealing furnace for homogenization heat treatment, and then cooled at room temperature to obtain an aluminum alloy 8A02 component standard sample.

[0024] The effective crystallization height of the hot top short crystallizer in the embodiment is small, the cooling speed of the ingot is increased, the intracrystalline structure of the ingot is thinner, the liquid cavity of the ingot is shallower, and the transition zone of the ingot is narrower, so that the density of the ingot is increased, and the distribution of the chemical components along the cross section of the ingot is more uniform.

[0025] The aluminum ingot in the embodiment is an aluminum ingot with a purity of 99.99% or above.

[0026] In the embodiment, B is not analyzed, and is only helpful for the casting process.

[0027] Specific embodiment five: different from the specific embodiment four, the refining agent in step two is RJ1-1 refining agent, and the adding amount is 5-6 kg / t. The others are the same as the specific embodiment four.

[0028] The specific components of the RJ1-1 refining agent in the embodiment refer to YS / T 491-2005.

[0029] Specific embodiment six: different from the specific embodiment four or five, the purity of the argon gas in step three is greater than or equal to 99.996%, and the gas flow is 15 nm 3 / hr. The others are the same as the specific embodiment four or five.

[0030] Specific embodiment seven: different from one of the specific embodiments four to six, the AlTi5B0.2 intermediate alloy in step three is an aluminum titanium boron wire, and the adding amount is 3 kg / t. The others are the same as one of the specific embodiments four to six.

[0031] Specific embodiment eight: different from one of the specific embodiments four to seven, the casting in step three adopts semi-continuous "hot top" casting, the hot top short crystallizer with a specification of Φ65 mm and an effective height of 8-10 mm is used for casting, the casting temperature is 670-700 ℃, the casting speed is 170-190 mm / min, and the cooling water intensity is 0.05-0.10 MPa. The others are the same as one of the specific embodiments four to seven.

[0032] Specific embodiment nine: different from one of the specific embodiments four to eight, the parameters of the homogenization heat treatment in step four are that the homogenization temperature is 460-490 ℃, and the holding time is 24 h. The others are the same as one of the specific embodiments four to eight.

[0033] Specific implementation ten: the difference between this implementation and one of specific implementations four to nine is that the shape of the aluminum alloy 8A02 component standard sample in step four is blocky or chipped. The others are the same as one of specific implementations four to nine.

[0034] The content of the application is not limited to the content of each of the above implementations, and the combination of one or several specific implementations can also achieve the purpose of the application.

[0035] Example one: an aluminum alloy 8A02 component standard sample, consisting of 0.0982% Si, 0.0794% Fe, 0.00852% Cu, 0.00493% Mn, 0.0285% Mg, 0.00487% Cr, 0.00476% Ni, 0.0365% Zn, 0.00333% Ti, 0.179% Sn, 0.243% Bi, and the balance of Al, by mass percent.

[0036] The preparation method of the aluminum alloy 8A02 component standard sample is completed by the following steps:

[0037] I. Weighing: according to the mass percentage of 0.0982% Si, 0.0794% Fe, 0.00852% Cu, 0.00493% Mn, 0.0285% Mg, 0.00487% Cr, 0.00476% Ni, 0.0365% Zn, 0.00333% Ti, 0.179% Sn, 0.243% Bi, and the balance of Al, the ingredients are weighed, and the aluminum ingot, industrial pure magnesium, industrial pure zinc, industrial pure tin, AlSi20 intermediate alloy, AlCu40 intermediate alloy, AlMn10 intermediate alloy, AlFe10 intermediate alloy, AlCr3 intermediate alloy, AlTi5B0.2 intermediate alloy, AlNi20 intermediate alloy and AlBi5 intermediate alloy are used as smelting raw materials;

[0038] II. Smelting: the aluminum ingot, industrial pure zinc, industrial pure tin, AlSi20 intermediate alloy, AlCu40 intermediate alloy, AlMn10 intermediate alloy, AlFe10 intermediate alloy, AlCr3 intermediate alloy, AlNi20 intermediate alloy and AlBi5 intermediate alloy weighed in step one are added to a small smelting furnace, heated to 790℃, and when the materials in the furnace are completely melted, the refining agent is added to remove slag, and after the slag removal is completed, the industrial pure magnesium is added to obtain an aluminum alloy solution;

[0039] III. Casting: The aluminum alloy melt obtained in step II was introduced into a holding furnace at 780°C and argon was introduced, then aluminum titanium boron wire (AlTi5B0.2 master alloy) was added at a speed of 90 mm / min for purification and refinement, and was left for 35 min, then casting was performed, the hot top short crystallizer with a specification of Φ65 mm and an effective height of 8-10 mm was used, the casting temperature was 684°C, the casting speed was 175 mm / min, and the cooling water intensity was 0.06 MPa, to obtain an aluminum alloy ingot;

[0040] IV. The aluminum alloy ingot obtained in step III was placed into an annealing furnace for homogenization heat treatment, the homogenization temperature was controlled at 480°C, the holding time was 24 h, then cooling was performed at room temperature, to obtain an aluminum alloy 8A02 component standard sample.

[0041] The refining agent in step II of the embodiment has a model of RJ1-1, and the specific components refer to YS / T 491-2005, and the addition amount is 6 Kg / t.

[0042] In step III of the embodiment, argon is introduced, the purity of the argon is ≥99.996%, and the gas flow is 15 nm 3 / hr.

[0043] In step III of the embodiment, the addition amount of the aluminum titanium boron wire is 3 Kg per ton of aluminum alloy solution.

[0044] In step III of the embodiment, the casting uses semi-continuous "hot top" casting.

[0045] After the aluminum alloy 8A02 component standard sample prepared in the embodiment is cut by at least 300 mm at both ends, 55-60 mm is taken at both ends and the middle as samples; the microstructure of the samples is checked by metallographic examination according to the standard of GB / T 3246.2-2012 "Deformed aluminum and aluminum alloy products macrostructure inspection method", and the results show that Figure 1 and Figure 2 It can be seen from the above that the internal structure of the prepared standard sample is compact, and has no defects such as pores and slag.

[0046] The aluminum alloy 8A02 component standard sample prepared in the embodiment is processed into 200-250 pieces of Φ55x35 mm samples, then 20 pieces of samples are randomly selected, sequentially numbered, and the composition uniformity of the spectroscopic standard sample is checked according to the requirements of YS / T 409 "Technical specification for standard samples for non-ferrous metal product analysis"; the three different parts on the cross section of the extracted sample are checked on a photoelectric spectrometer, and the test results are statistically analyzed by variance to obtain the composition uniformity data of the spectroscopic standard sample.

[0047] The aluminum alloy 8A02 component standard sample prepared in the embodiment is processed into 1mm aluminum alloy chips, and the processing parameters are as follows: milling cutter translation speed 90mm / min~110mm / min, milling cutter rotation speed 25mm / min~35mm / min, and milling chip depth 5mm~6mm. The aluminum alloy chips are fully mixed by four-fold method, sieved: 16 mesh undersize and 32 mesh oversize are taken; 100 bottles of 50g / bottle chemical samples are randomly taken 20 bottles, sequentially numbered, the sample element content is determined according to YS / T 409 “Technical Specification for Standard Sample of Non-ferrous Metal Product Analysis”, the chemical standard sample component uniformity is checked, and the detection method is shown in Table 1; wherein, the minimum sample weight for the chemical standard sample component uniformity test is 0.1g, and the test results are statistically analyzed by variance method.

[0048] Table 1

[0049] Element Analysis method Element Analysis method Si Silicomolybdenum blue spectrophotometry Ni Dimethylglyoxime spectrophotometry Fe Phenanthroline spectrophotometry Zn Flame atomic absorption spectrometry Cu Flame atomic absorption spectrometry Ti Diantipyryl methane spectrophotometry Mn Potassium periodate spectrophotometry Sn Inductively coupled plasma atomic emission spectrometry Mg Flame atomic absorption spectrometry Bi Potassium iodide spectrophotometry Cr Diphenylcarbazide photometry

[0050] (1) Except for Northeast Light Alloy Co., Ltd., 7 units with standard sample value setting qualification are invited to set values, and the above chemical samples are sent to the 7 units for value setting analysis; (2) according to GB / T 20975 “Chemical Analysis Method of Aluminum and Aluminum Alloy”, one or more accurate and reliable analysis methods are selected for collaborative value setting analysis and data processing; (3) the range is checked according to YS / T 409 “Technical Specification for Standard Sample of Non-ferrous Metal Product Analysis” to check whether there is an abnormal value in the group, if there is an abnormal value, the original value after rechecking and eliminating is required to be rechecked, and the normality of all data is tested by Shapiro-Wilk method.

[0051] According to YS / T 409 “Technical Specification for Standard Sample of Non-ferrous Metal Product Analysis”, the average value of the data subject to normal distribution is taken as a single determination value, a new group of data is constructed, and the Grubbs method is used for testing, and then the Cochran method is used for testing whether the precision of each group of data is equal, after processing each group of data, the arithmetic mean and standard deviation of each group of data are calculated, the effective number of digits of the standard value is rounded according to GB 8170 “Data Rounding Rules”, and the obtained data is the standard value and standard deviation of the aluminum alloy 8A02 component standard sample.

[0052] The standard value and expanded uncertainty of the aluminum alloy chemical standard sample obtained in the embodiment are shown in Table 2, and the standard value and expanded uncertainty of the aluminum alloy spectral standard sample are shown in Table 3. As shown in Tables 2 and 3, the standard sample prepared in the embodiment is not only suitable for chemical analysis of 8A02 aluminum alloy, but also is a spectral and chemical sample of the same component standard sample, which provides a basis for the use of modern instruments and the calibration between instruments.

[0053] Table 2

[0054]

[0055] Table 3

[0056]

Claims

1. An aluminum alloy 8A02 composition standard sample, characterized by The aluminum alloy 8A02 component standard sample is composed of 0.096-0.100% Si, 0.077-0.080% Fe, 0.0083-0.0087% Cu, 0.0048-0.0050% Mn, 0.027-0.029% Mg, 0.0047-0.0049% Cr, 0.0047-0.0050% Ni, 0.035-0.037% Zn, 0.0032-0.0034% Ti, 0.177-0.181% Sn, 0.241-0.245% Bi and the balance of Al in terms of mass percentage.

2. The aluminum alloy 8A02 composition reference material according to claim 1, characterized in that The aluminum alloy 8A02 component standard sample is composed of 0.0965% Si, 0.0772% Fe, 0.00834% Cu, 0.00482% Mn, 0.0274% Mg, 0.00473% Cr, 0.00471% Ni, 0.0351% Zn, 0.00322% Ti, 0.177% Sn, 0.241% Bi and the balance of Al in terms of mass percentage.

3. The method of claim 1, wherein the aluminum alloy 8A02 composition reference material is prepared by the steps of: The preparation method of the aluminum alloy 8A02 component standard sample is completed by the following steps: ​ I. Weighing: according to the mass percentage of 0.096-0.100% Si, 0.077-0.080% Fe, 0.0083-0.0087% Cu, 0.0048-0.0050% Mn, 0.027-0.029% Mg, 0.0047-0.0049% Cr, 0.0047-0.0050% Ni, 0.035-0.037% Zn, 0.0032-0.0034% Ti, 0.177-0.181% Sn, 0.241-0.245% Bi and the balance of Al, the ingredients are prepared, and the aluminum ingot, industrial pure magnesium, industrial pure zinc, industrial pure tin, AlSi20 intermediate alloy, AlCu40 intermediate alloy, AlMn10 intermediate alloy, AlFe10 intermediate alloy, AlCr3 intermediate alloy, AlTi5B0.2 intermediate alloy, AlNi20 intermediate alloy and AlBi5 intermediate alloy are weighed as smelting raw materials; II. Smelting: the aluminum ingot, industrial pure zinc, industrial pure tin, AlSi20 intermediate alloy, AlCu40 intermediate alloy, AlMn10 intermediate alloy, AlFe10 intermediate alloy, AlCr3 intermediate alloy, AlNi20 intermediate alloy and AlBi5 intermediate alloy weighed in step I are added to a smelting furnace, heated to 770-790°C, and after the materials in the furnace are completely melted, a refining agent is added for slagging, and after the slagging is completed, industrial pure magnesium is added to obtain an aluminum alloy solution; III. Casting: the aluminum alloy melt obtained in step II is introduced into a holding furnace at 750-780°C and argon is introduced, then AlTi5B0.2 intermediate alloy is added at a speed of 90mm / min for purification and refinement, and after standing for 30-35min, casting is carried out to obtain an aluminum alloy ingot; Four, the aluminum alloy ingot obtained in step three is put into an annealing furnace for homogenization heat treatment, and then cooled at room temperature to obtain an aluminum alloy 8A02 component standard sample.

4. The preparation method of the aluminum alloy 8A02 component standard sample according to claim 3, characterized in that The refining agent in step two is RJ1-1 refining agent, and the adding amount is 5-6 kg / t.

5. The method of claim 3, wherein the aluminum alloy 8A02 composition standard sample is prepared by the steps of: The purity of argon gas in step three is ≥ 99.996%, and the gas flow rate is 15 nm 3 / hr. ​ 6. The preparation method of the aluminum alloy 8A02 component standard sample according to claim 3, characterized in that The AlTi5B0.2 intermediate alloy in step three is aluminum titanium boron wire, and the adding amount is 3 kg / t.

7. The method of claim 3, wherein the aluminum alloy 8A02 composition standard sample is prepared by the steps of: In step three, the casting adopts semi-continuous "hot top" casting, the hot top short crystallizer with a specification of Φ65 mm and an effective height of 8-10 mm is used, the casting temperature is 670-700 ℃, the casting speed is 170-190 mm / min, and the cooling water intensity is 0.05-0.10 MPa. ​ 8. The method of claim 3, wherein the aluminum alloy 8A02 composition standard sample is prepared by the steps of: In step four, the homogenization heat treatment parameters are as follows: homogenization temperature is 460-490 ℃, and the holding time is 24 h. ​ 9. The method of claim 3, wherein the aluminum alloy 8A02 composition standard sample is prepared by the steps of: In step four, the aluminum alloy 8A02 component standard sample is in the form of blocks or scraps. ​

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