CN104390826A - Preparation method of 6016 aluminum alloy spectrum standard sample - Google Patents
Preparation method of 6016 aluminum alloy spectrum standard sample Download PDFInfo
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- CN104390826A CN104390826A CN201410763307.7A CN201410763307A CN104390826A CN 104390826 A CN104390826 A CN 104390826A CN 201410763307 A CN201410763307 A CN 201410763307A CN 104390826 A CN104390826 A CN 104390826A
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Abstract
The invention belongs to the field of alloys, and particularly relates to a preparation method of a 6016 aluminum alloy spectrum standard sample. The preparation method provided by the invention comprises the following steps: (a) carrying out melt blending on an aluminum source, a silicon source, an iron source, a copper source, a manganese source, a magnesium source, a chromium source, a nickel source, a zinc source and a titanium source to obtain an aluminum alloy melt, wherein the aluminum alloy melt comprises 1.1-1.5wt% of Si, 0.1-0.5wt% of Fe, 0.095-0.2wt% of Cu, 0.07-0.1wt% of Mn, 0.5-0.6wt% of Mg, 0.01-0.1wt% of Cr, 0.02-0.05wt% of Ni, 0.025-0.2wt% of Zn, 0.02-0.15wt% of Ti and the balance of Al; (b) carrying out casting, homogenizing heat treatment and extrusion on the aluminum alloy melt in sequence to obtain the 6016 aluminum alloy spectrum standard sample. Component analysis is carried out on a 6016 aluminum alloy sample to be tested by adopting an atomic emission spectroscopy spectral line intensity standard curve corrected by the 6016 aluminum alloy standard sample prepared with the method, and the result of the component analysis coincides with the result of the component analysis by adopting a chemical analysis method.
Description
Technical field
The invention belongs to alloy field, particularly relate to a kind of preparation method of 6016 Aluminum alloy spectral standard samples.
Background technology
So-called aluminium alloy, adds other appropriate elements exactly, the essence of aluminium is improved in commercial-purity aluminium, to meet the various needs in industrial and life.Because aluminium alloy proportion is little, specific strength is high, has good combination property, therefore, is widely used in the aspects such as aircraft industry, auto manufacturing, power instrument, instrument and civilian vessel manufacture.
In the research and development and production run of aluminium alloy, need to analyze the chemical composition in aluminium alloy, thus reach the strict object controlling each chemical composition content, and then avoid stokehold composition in alloy production process out of control, ensure the quality of alloy product simultaneously.The chemical composition detection method of alloy mainly contains chemical analysis and photoelectric spectrophotometric method, chemical method due to its operation cumbersome, poor reproducibility, analytical cycle long (analytical cycle is more than 4 hours), and relate to heavy metal pollution, thus limit the use of this method; And photoelectric spectrophotometric method because of its fast, accurately, environmental protection, the feature such as easy and simple to handle, be widely used in national economy every profession and trades such as industrial and mining enterprises, commodity inspection, scientific research institutions.But according to photoelectric spectrophotometric method principle, its application has individual condition precedent: before analyzing any alloy, corresponding alloy standard model must be had to correct Spectroscopic analysis results, to ensure precision of analysis.
6016 aluminium alloys are a kind of aluminum alloy for vehicle body plate newly developed, and its chemical composition has singularity.Due to the requirement of spectral standard sample demand fulfillment composition accuracy, and it is corresponding with 6016 aluminium alloys on composition to there is no suitable standard model in existing standard sample, the Spectroscopic analysis results of special 6016 aluminum alloy standard samples of development to 6016 aluminium alloys is therefore needed to correct.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of preparation method of 6016 Aluminum alloy spectral standard samples, the standard model adopting method provided by the invention to obtain can be used for the correction of 6016 aluminum alloy spectrum analysis results.
The invention provides a kind of preparation method of 6016 Aluminum alloy spectral standard samples, comprise the following steps:
A), aluminium source, silicon source, source of iron, Tong Yuan, manganese source, magnesium source, chromium source, nickel source, zinc source and titanium source melt blending, obtain aluminium alloy melt;
Described aluminium alloy melt comprises: the Al of Ni, the Zn of 0.025 ~ 0.2wt% of the Mg of the Cu of the Si of 1.1 ~ 1.5wt%, the Fe of 0.1 ~ 0.5wt%, 0.095 ~ 0.2wt%, the Mn of 0.07 ~ 0.1wt%, 0.5 ~ 0.6wt%, the Cr of 0.01 ~ 0.1wt%, 0.02 ~ 0.05wt%, the Ti of 0.02 ~ 0.15wt% and surplus;
B), described aluminium alloy melt after casting, homogenising thermal treatment and extruding, obtains 6016 Aluminum alloy spectral standard samples successively.
Preferably, described step a) is specially:
A1), aluminium source, silicon source, source of iron, Tong Yuan, manganese source, chromium source, nickel source and titanium source melt blending, obtain the first alloy melt;
A2), described first alloy melt and zinc source melt blending, obtain the second alloy melt;
A3), described second alloy melt and magnesium source melt blending, obtain aluminium alloy melt.
Preferably, described silicon source is Al-Si intermediate alloy; Described source of iron is Al-Fe intermediate alloy; Described copper source is Al-Cu intermediate alloy; Described manganese source is Al-Mn intermediate alloy; Described chromium source is Al-Cr intermediate alloy; Described nickel source is Al-Ni intermediate alloy; Described titanium source is Al-Ti intermediate alloy; Described zinc source is zinc; Described magnesium source is magnesium; Described aluminium source is aluminium and the intermediate alloy containing aluminium.
Preferably, the mode of described casting is that hot direct casting is made.
Preferably, the temperature of described casting is 735 ~ 745 DEG C.
Preferably, the speed of described casting is 72 ~ 78mm/min.
Preferably, the cooling water pressure in described casting process is 0.06 ~ 0.08MPa.
Preferably, the heat treated temperature of described homogenising is 515 ~ 530 DEG C; The heat treated temperature retention time of described homogenising is 12 ~ 14h.
Preferably, the temperature of described extruding is 430 ~ 450 DEG C; The speed of described extruding is 3 ~ 5mm/s.
Preferably, described aluminium alloy melt comprises: the Al of Ni, the Zn of 0.027 ~ 0.031wt% of the Mg of the Cu of the Si of 1.14 ~ 1.18wt%, the Fe of 0.123 ~ 0.137wt%, 0.096 ~ 0.106wt%, the Mn of 0.076 ~ 0.082wt%, 0.51 ~ 0.534wt%, the Cr of 0.014 ~ 0.018wt%, 0.02 ~ 0.022wt%, the Ti of 0.02 ~ 0.022wt% and surplus.
Compared with prior art, the invention provides a kind of preparation method of 6016 Aluminum alloy spectral standard samples, comprise the following steps: a), aluminium source, silicon source, source of iron, Tong Yuan, manganese source, magnesium source, chromium source, nickel source, zinc source and titanium source melt blending, obtain aluminium alloy melt; Described aluminium alloy melt comprises: the Al of Ni, the Zn of 0.025 ~ 0.2wt% of the Mg of the Cu of the Si of 1.1 ~ 1.5wt%, the Fe of 0.1 ~ 0.5wt%, 0.095 ~ 0.2wt%, the Mn of 0.07 ~ 0.1wt%, 0.5 ~ 0.6wt%, the Cr of 0.01 ~ 0.1wt%, 0.02 ~ 0.05wt%, the Ti of 0.02 ~ 0.15wt% and surplus; B), described aluminium alloy melt after casting, homogenising thermal treatment and extruding, obtains 6016 Aluminum alloy spectral standard samples successively.Experimental result shows, 6016 Aluminum alloy spectral standard samples adopting method provided by the invention obtained are organized fine and closely woven, even, pore-free, the metallurgical imperfection such as to be mingled with, radial, longitudinal equal segregation-free, and chemical composition is even; The obtained standard model of method provided by the invention is adopted to have good stability, the term of validity at least 10 years; The atomic emission spectrum line strength typical curve adopting 6016 aluminum alloy standard samples obtained by the present invention to correct carries out constituent analysis to 6016 aluminium alloy testing samples, and its result conforms to the result adopting chemical analysis to carry out constituent analysis.Illustrate that 6016 Aluminum alloy spectral standard samples adopting method provided by the invention to obtain can meet production and the research and development use of 6016 aluminium alloys, namely can be used for the correction of 6016 aluminum alloy spectrum analysis results, and then improve 6016 aluminium alloy production efficiency and product qualities.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only embodiments of the invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to the accompanying drawing provided.
Fig. 1 is the metal lographic examination test piece of aluminium alloy cast ingot provided by the invention and the sampling point schematic diagram of segregation inspection test piece;
Fig. 2 be ingot casting component segregation provided by the invention inspection get a position view;
The metallographic macrograph of the aluminium alloy cast ingot test piece that Fig. 3 provides for the embodiment of the present invention 1.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of preparation method of 6016 Aluminum alloy spectral standard samples, comprise the following steps:
A), aluminium source, silicon source, source of iron, Tong Yuan, manganese source, magnesium source, chromium source, nickel source, zinc source and titanium source melt blending, obtain aluminium alloy melt;
Described aluminium alloy melt comprises: the Al of Ni, the Zn of 0.025 ~ 0.2wt% of the Mg of the Cu of the Si of 1.1 ~ 1.5wt%, the Fe of 0.1 ~ 0.5wt%, 0.095 ~ 0.2wt%, the Mn of 0.07 ~ 0.1wt%, 0.5 ~ 0.6wt%, the Cr of 0.01 ~ 0.1wt%, 0.02 ~ 0.05wt%, the Ti of 0.02 ~ 0.15wt% and surplus;
B), described aluminium alloy melt after casting, homogenising thermal treatment and extruding, obtains 6016 Aluminum alloy spectral standard samples successively.
In the present invention, first by aluminium source, silicon source, source of iron, Tong Yuan, manganese source, magnesium source, chromium source, nickel source, zinc source and titanium source melt blending, aluminium alloy melt is obtained.Wherein, described silicon source is preferably Al-Si intermediate alloy, and in described Al-Si intermediate alloy, Si content is preferably 20 ~ 30wt%; Described source of iron is preferably Al-Fe intermediate alloy, and in described Al-Fe intermediate alloy, Fe content is preferably 15 ~ 20wt%; Described copper source is preferably Al-Cu intermediate alloy, and in described Al-Cu intermediate alloy, Cu content is preferably 40 ~ 50wt%; Described manganese source is preferably Al-Mn intermediate alloy, and in described Al-Mn intermediate alloy, Mn content is preferably 15 ~ 20wt%; Described chromium source is preferably Al-Cr intermediate alloy, and in described Al-Cr intermediate alloy, Cr content is preferably 4 ~ 10wt%; Described nickel source is preferably Al-Ni intermediate alloy, and in described Al-Ni intermediate alloy, Ni content is preferably 20 ~ 30wt%; Described titanium source is preferably Al-Ti intermediate alloy, and in described Al-Ti intermediate alloy, Ti content is preferably 4 ~ 10wt%; Described zinc source is preferably zinc; Described magnesium source is preferably magnesium; Described aluminium source is preferably aluminium and the intermediate alloy containing aluminium.Described aluminium alloy melt comprises the Si of 1.1 ~ 1.5wt%, the Fe of 0.1 ~ 0.5wt%, the Cu of 0.095 ~ 0.2wt%, the Mn of 0.07 ~ 0.1wt%, the Mg of 0.5 ~ 0.6wt%, the Cr of 0.01 ~ 0.1wt%, the Ni of 0.02 ~ 0.05wt%, the Zn of 0.025 ~ 0.2wt%, the Ti of 0.02 ~ 0.15wt% and the Al of surplus, preferably include the Si of 1.14 ~ 1.18wt%, the Fe of 0.123 ~ 0.137wt%, the Cu of 0.096 ~ 0.106wt%, the Mn of 0.076 ~ 0.082wt%, the Mg of 0.51 ~ 0.534wt%, the Cr of 0.014 ~ 0.018wt%, the Ni of 0.02 ~ 0.022wt%, the Zn of 0.027 ~ 0.031wt%, the Ti of 0.02 ~ 0.022wt% and the Al of surplus.In an embodiment provided by the invention, described aluminium alloy melt comprises the Al of the Si of 1.16 ± 0.02wt%, the Fe of 0.13 ± 0.007wt%, the Cu of 0.101 ± 0.005wt%, the Mn of 0.079 ± 0.003wt%, the Mg of 0.522 ± 0.012wt%, the Cr of 0.016 ± 0.002wt%, Ni, the Zn of 0.029 ± 0.002wt% of 0.021 ± 0.001wt%, the Ti of 0.021 ± 0.001wt% and surplus.
In the present invention, described aluminium source, silicon source, source of iron, Tong Yuan, manganese source, magnesium source, chromium source, nickel source, zinc source and titanium source melt blending, the process obtaining aluminium alloy melt is specially:
A1), aluminium source, silicon source, source of iron, Tong Yuan, manganese source, chromium source, nickel source and titanium source melt blending, obtain the first alloy melt;
A2), described first alloy melt and zinc source melt blending, obtain the second alloy melt;
A3), described second alloy melt and magnesium source melt blending, obtain aluminium alloy melt.
In the process of above-mentioned obtained aluminium alloy melt, first by aluminium source, silicon source, source of iron, Tong Yuan, manganese source, chromium source, nickel source and titanium source melt blending.The temperature of the present invention to described melt blending is not particularly limited, and can make above-mentioned source metal melting, is preferably 730 ~ 780 DEG C.After aluminium source, silicon source, source of iron, Tong Yuan, manganese source, chromium source, nickel source and titanium source melt blending are even, obtain the first alloy melt.
Then, described first alloy melt and zinc source melt blending.The temperature of the present invention to described melt blending is not particularly limited, and can make above-mentioned source metal melting, is preferably 730 ~ 780 DEG C.For preventing Zn in the first alloy melt and zinc source melt blending process from sinking to the bottom, in the present invention, preferably in the first alloy melt and zinc source melt blending process, strong mixing is carried out to mixed system.Until the first alloy melt and zinc source melt blending evenly after, obtain the second alloy melt.
Finally, described second alloy melt and magnesium source melt blending.The temperature of the present invention to described melt blending is not particularly limited, and can make above-mentioned source metal melting, is preferably 730 ~ 780 DEG C.Until the second alloy melt and magnesium source melt blending evenly after, obtain aluminium alloy melt.
After obtaining aluminium alloy melt, described melt is cast.The mode of the present invention to described casting is not particularly limited, and preferably adopts heat top casting to cast.The temperature of described casting is preferably 735 ~ 745 DEG C.The speed of described casting is preferably 72 ~ 78mm/min.Cooling water pressure in described casting process is preferably 0.06 ~ 0.08MPa.
After aluminium alloy melt completes casting, obtain aluminium alloy cast ingot.Homogenising thermal treatment and extruding are carried out to described aluminium alloy cast ingot.The heat treated temperature of described homogenising is preferably 515 ~ 530 DEG C; The heat treated temperature retention time of described homogenising is preferably 12 ~ 14h.The temperature of described extruding is preferably 430 ~ 450 DEG C; The speed of described extruding is preferably 3 ~ 5mm/s.The present invention is not particularly limited extruding equipment used, is preferably 2000 tons of oil pressure extruders well known to those skilled in the art.After extruding terminates, obtain 6016 Aluminum alloy spectral standard samples.
For ensureing the quality of standard model, the present invention preferably first cuts inspection test piece from the aluminium alloy cast ingot that casting obtains, and microstructure examination and component segregation inspection are carried out to inspection test piece, to be tested qualified after, then homogenising thermal treatment and extruding are carried out to aluminium alloy cast ingot.In the present invention, described in be up to the standards and refer to that Structure of Aluminum Alloy Ingots is fine and closely woven, even, pore-free, the metallurgical imperfection such as to be mingled with, and ingot casting is radial, longitudinal equal segregation-free.
In an embodiment provided by the invention, metal lographic examination test piece and segregation inspection test piece cut according to position shown in Fig. 1, Fig. 1 is the metal lographic examination test piece of aluminium alloy cast ingot provided by the invention and the sampling point schematic diagram of segregation inspection test piece, wherein, L=120 ~ 220mm, 1 and 4 for metallographic specimen cut position, 2 and 3 for component segregation test piece cut position, the present invention is preferably by ingot casting railway carriage before sampling, and the thickness of described railway carriage is 4 ~ 6mm, is preferably 5mm.
In the present invention, described component segregation inspection is preferably carried out according to following steps:
A little spectral analysis is carried out to component segregation inspection test piece by getting shown in Fig. 2, Fig. 2 be ingot casting component segregation provided by the invention inspection get a position view.Wherein, each inspection test piece respectively gets A1 ~ A5 five groups of data from center to edge.Represent the radial component segregation degree of ingot casting by the size of each inspection test piece five groups of data component differences, No. 2 and five extents getting the data of a position corresponding to No. 3 inspection test pieces represent ingot casting longitudinal direction component segregation degree.Described radial component segregation inspection adopts Da Weite (DARVID) inspection; Described longitudinal component segregation inspection adopts t inspection.
In order to ensure the quality of standard model, the present invention preferably carries out definite value inspection to 6016 obtained Aluminum alloy spectral standard samples.In one embodiment of the invention, the standard model that described aluminium alloy cast ingot obtains after homogenising thermal treatment and extruding is bar, and the definite value inspection of described bar is preferably carried out according to following steps:
Cut the bar of three sections of 180 ~ 220mm from the head of every root bar, middle part, afterbody, be processed into graininess with drilling and milling machine and special cutter, packing after the sample that is mixed, obtain the sample of definite value inspection.After obtaining the sample of definite value inspection, sample is delivered to professional inspection mechanism and detect.
Above-mentioned 6016 obtained Aluminum alloy spectral standard sample sawings after the assay was approved, are become standard model block, and stamp the marking by definite value, and after surperficial turnning and milling is bright and clean, warehouse-in is preserved.
6016 Aluminum alloy spectral standard samples adopting method provided by the invention obtained are organized fine and closely woven, even, pore-free, the metallurgical imperfection such as to be mingled with, and radial, longitudinal equal segregation-free, chemical composition is even, and sample stability is good, the term of validity at least 10 years.Experimental result shows, the atomic emission spectrum line strength typical curve adopting 6016 Aluminum alloy spectral standard samples obtained by the present invention to correct carries out constituent analysis to 6016 aluminium alloy testing samples, and its result conforms to the result adopting chemical analysis to carry out constituent analysis.Illustrate that the standard model adopting method provided by the invention to obtain can meet production and the research and development use of 6016 aluminium alloys, namely can be used for the correction of 6016 aluminum alloy spectrum analysis results, and then improve 6016 aluminium alloy production efficiency and product qualities.
For the purpose of clearer, be described in detail below by following examples.
Embodiment 1
By the percentage composition of table 1, fine aluminium, Al-20wt%Si intermediate alloy, Al-15wt%Fe intermediate alloy, Al-40wt%Cu intermediate alloy, Al-15wt%Mn intermediate alloy, Al-4wt%Cr intermediate alloy, Al-20wt%Ni intermediate alloy and Al-20wt%Ti intermediate alloy are added in stove, melt blending at 760 DEG C, obtains the first alloy melt.In the first alloy melt, add pure zinc by the percentage composition of table 1, stir, obtain the second alloy melt.Add pure magnesium by the composition of table 1 than in the second alloy solution, stir, obtain aluminium alloy melt.Under agitation, adopt hot direct casting to make and cast aluminium alloy melt, described casting temperature is 735 DEG C, and casting speed is 78mm/min, and water pressure of cooling water is 0.06MPa, after casting terminates, obtains the aluminium alloy cast ingot bar that diameter is 162mm.
The chemical composition mass percent of 6016 Aluminum alloy spectral standard samples in table 1 embodiment 1
Carry out metallographic structure and component segregation inspection to above-mentioned aluminium alloy cast ingot bar, this process is specially:
First, carry out railway carriage to aluminium alloy cast ingot bar, railway carriage thickness is 5mm.Then, cut inspection test piece according to part shown in Fig. 1, Fig. 1 is the metal lographic examination test piece of aluminium alloy cast ingot provided by the invention and the sampling point schematic diagram of segregation inspection test piece, wherein, L=120 ~ 220mm, 1 and 4 for metallographic specimen cut position, 2 and 3 for component segregation test piece cut position.Sample according to mode shown in Fig. 2 and spectral analysis carried out to component segregation inspection test piece, Fig. 2 be ingot casting component segregation provided by the invention inspection get a position view.Wherein, each inspection test piece respectively gets A1 ~ A5 five groups of data from center to edge.
Metallographic high power and low power inspection are carried out to No. 1 and No. 4 test pieces, result shows that test piece is organized fine and closely woven, even, pore-free, the metallurgical imperfection such as to be mingled with, wherein the metallographic macrograph of No. 1 test piece as shown in Figure 3, the metallographic macrograph of the aluminium alloy cast ingot test piece that Fig. 3 provides for the embodiment of the present invention 1.
Carry out the inspection of radial component segregation and the inspection of longitudinal component segregation to No. 2 and No. 3 test pieces, wherein, described radial component segregation inspection adopts Da Weite (DARVID) inspection, is specially:
If R/S > d α is .n, radial direction has segregation
If R/S≤d α is .n, radial segregation-free
In formula, R is extreme difference, and S is standard deviation, and d α .n is the statistical constant (in the present embodiment d α .n=2.753) relevant with α .n.
Described longitudinal component segregation inspection adopts t inspection, is specially:
If t
0>t
α ν, then longitudinally segregation is had; If t
0≤ t
α ν, then longitudinal segregation-free.
In formula:
be two test pieces mean values separately, n counts for getting (n=5), S
1, S
2be the standard deviation of two test pieces, t
α νstatistical constant (the t in the present embodiment determined by α ν=n-1
α νget 2.306).
Testing result shows, No. 2 and No. 3 radial segregation-frees equal to longitudinal direction of test piece.
After the metallographic structure inspection of aluminium alloy cast ingot bar and component segregation passed examination, homogenising thermal treatment is carried out to aluminium alloy cast ingot bar, the heat treated metal heat preservation temperature of described homogenising is 515 DEG C, temperature retention time is 14h, after insulation terminates, be cooled to room temperature, obtain the alloy pig after Homogenization Treatments.
Alloy pig after Homogenization Treatments is extruded in 2000 tons of oil pressure extruders, the temperature of extruding is 430 DEG C, and extrusion speed is 3mm/s, obtains the bar that diameter is 55mm after extruding, bar sawing is become the small cylinder of ф 55 × 35mm, be 6016 Aluminum alloy spectral standard samples.The standard model obtained is stamped the marking, and the bright and clean rear warehouse-in of surperficial turnning and milling is preserved.
Embodiment 2
By the percentage composition of table 2, fine aluminium, Al-20wt%Si intermediate alloy, Al-15wt%Fe intermediate alloy, Al-40wt%Cu intermediate alloy, Al-15wt%Mn intermediate alloy, Al-4wt%Cr intermediate alloy, Al-20wt%Ni intermediate alloy and Al-20wt%Ti intermediate alloy are added in stove, melt blending at 760 DEG C, obtains the first alloy melt.In the first alloy melt, add pure zinc by the percentage composition of table 2, stir, obtain the second alloy melt.Add pure magnesium by the composition of table 2 than in the second alloy solution, stir, obtain aluminium alloy melt.Under agitation, adopt hot direct casting to make and cast aluminium alloy melt, described casting temperature is 745 DEG C, and casting speed is 72mm/min, and water pressure of cooling water is 0.08MPa, after casting terminates, obtains the aluminium alloy cast ingot bar that diameter is 162mm.
The chemical composition mass percent of 6016 Aluminum alloy spectral standard samples in table 2 embodiment 2
Carry out metallographic structure and component segregation inspection to above-mentioned aluminium alloy cast ingot bar, this process is specially:
First, carry out railway carriage to aluminium alloy cast ingot bar, railway carriage thickness is 5mm.Then, cut inspection test piece according to part shown in Fig. 1, Fig. 1 is the metal lographic examination test piece of aluminium alloy cast ingot provided by the invention and the sampling point schematic diagram of segregation inspection test piece, wherein, L=120 ~ 220mm, 1 and 4 for metallographic specimen cut position, 2 and 3 for component segregation test piece cut position.
Carry out metallographic high power and low power inspection to No. 1 and No. 4 test pieces, result shows that test piece is organized fine and closely woven, even, pore-free, the metallurgical imperfection such as to be mingled with.
A little spectral analysis is carried out to component segregation inspection test piece by getting shown in Fig. 2, Fig. 2 be ingot casting component segregation provided by the invention inspection get a position view.Wherein, each inspection test piece respectively gets A1 ~ A5 five groups of data from center to edge.Represent the radial component segregation degree of ingot casting by the size of each inspection test piece five groups of data component differences, No. 2 and five extents getting the data of a position corresponding to No. 3 inspection test pieces represent ingot casting longitudinal direction component segregation degree.
Described radial component segregation inspection adopts Da Weite (DARVID) inspection, is specially:
If R/S > d α is .n, radial direction has segregation
If R/S≤d α is .n, radial segregation-free
In formula, R is extreme difference, and S is standard deviation, and d α .n is the statistical constant (in the present embodiment d α .n=2.753) relevant with α .n.
Described longitudinal component segregation inspection adopts t inspection, is specially:
If t
0>t
α ν, then longitudinally segregation is had; If t
0≤ t
α ν, then longitudinal segregation-free.
In formula:
be two test pieces mean values separately, n counts for getting (n=5), S
1, S
2be the standard deviation of two test pieces, t
α νstatistical constant (the t in the present embodiment determined by α ν=n-1
α νget 2.306).
Testing result shows, No. 2 and No. 3 radial segregation-frees equal to longitudinal direction of test piece.
After the metallographic structure inspection of aluminium alloy cast ingot bar and component segregation passed examination, homogenising thermal treatment is carried out to aluminium alloy cast ingot bar, the heat treated metal heat preservation temperature of described homogenising is 530 DEG C, temperature retention time is 12h, after insulation terminates, be cooled to room temperature, obtain the alloy pig after Homogenization Treatments.
Alloy pig after Homogenization Treatments is extruded in 2000 tons of oil pressure extruders, the temperature of extruding is 430 DEG C, and extrusion speed is 5mm/s, obtains the bar that diameter is 55mm after extruding, bar sawing is become the small cylinder of ф 55 × 35mm, be 6016 Aluminum alloy spectral standard samples.The standard model obtained is stamped the marking, and the bright and clean rear warehouse-in of surperficial turnning and milling is preserved.
Embodiment 3
By the percentage composition of table 3, fine aluminium, Al-20wt%Si intermediate alloy, Al-15wt%Fe intermediate alloy, Al-40wt%Cu intermediate alloy, Al-15wt%Mn intermediate alloy, Al-4wt%Cr intermediate alloy, Al-20wt%Ni intermediate alloy and Al-20wt%Ti intermediate alloy are added in stove, melt blending at 760 DEG C, obtains the first alloy melt.In the first alloy melt, add pure zinc by the percentage composition of table 3, stir, obtain the second alloy melt.Add pure magnesium by the composition of table 3 than in the second alloy solution, stir, obtain aluminium alloy melt.Under agitation, adopt hot direct casting to make and cast aluminium alloy melt, described casting temperature is 740 DEG C, and casting speed is 76mm/min, and water pressure of cooling water is 0.07MPa, after casting terminates, obtains the aluminium alloy cast ingot bar that diameter is 162mm.
The chemical composition mass percent of 6016 Aluminum alloy spectral standard samples in table 3 embodiment 3
Carry out metallographic structure and component segregation inspection to above-mentioned aluminium alloy cast ingot bar, this process is specially:
First, carry out railway carriage to aluminium alloy cast ingot bar, railway carriage thickness is 5mm.Then, cut inspection test piece according to part shown in Fig. 1, Fig. 1 is the metal lographic examination test piece of aluminium alloy cast ingot provided by the invention and the sampling point schematic diagram of segregation inspection test piece, wherein, L=120 ~ 220mm, 1 and 4 for metallographic specimen cut position, 2 and 3 for component segregation test piece cut position.
Carry out metallographic high power and low power inspection to No. 1 and No. 4 test pieces, result shows that test piece is organized fine and closely woven, even, pore-free, the metallurgical imperfection such as to be mingled with.
A little spectral analysis is carried out to component segregation inspection test piece by getting shown in Fig. 2, Fig. 2 be ingot casting component segregation provided by the invention inspection get a position view.Wherein, each inspection test piece respectively gets A1 ~ A5 five groups of data from center to edge.Represent the radial component segregation degree of ingot casting by the size of each inspection test piece five groups of data component differences, No. 2 and five extents getting the data of a position corresponding to No. 3 inspection test pieces represent ingot casting longitudinal direction component segregation degree.
Described radial component segregation inspection adopts Da Weite (DARVID) inspection, is specially:
If R/S > d α is .n, radial direction has segregation
If R/S≤d α is .n, radial segregation-free
In formula, R is extreme difference, and S is standard deviation, and d α .n is the statistical constant (in the present embodiment d α .n=2.753) relevant with α .n.
Described longitudinal component segregation inspection adopts t inspection, is specially:
If t
0>t
α ν, then longitudinally segregation is had; If t
0≤ t
α ν, then longitudinal segregation-free.
In formula:
be two test pieces mean values separately, n counts for getting (n=5), S
1, S
2be the standard deviation of two test pieces, t
α νstatistical constant (the t in the present embodiment determined by α ν=n-1
α νget 2.306).
Testing result shows, No. 2 and No. 3 radial segregation-frees equal to longitudinal direction of test piece.
After the metallographic structure inspection of aluminium alloy cast ingot bar and component segregation passed examination, homogenising thermal treatment is carried out to aluminium alloy cast ingot bar, the heat treated metal heat preservation temperature of described homogenising is 520 DEG C, temperature retention time is 13h, after insulation terminates, be cooled to room temperature, obtain the alloy pig after Homogenization Treatments.
Alloy pig after Homogenization Treatments is extruded in 2000 tons of oil pressure extruders, the temperature of extruding is 430 DEG C, and extrusion speed is 4mm/s, obtains the bar that diameter is 55mm after extruding, bar sawing is become the small cylinder of ф 55 × 35mm, be 6016 Aluminum alloy spectral standard samples.The standard model obtained is stamped the marking, and the bright and clean rear warehouse-in of surperficial turnning and milling is preserved.
Embodiment 4
The uniformity testing of standard model
Uniformity testing is carried out to 6016 Aluminum alloy spectral standard samples prepared by embodiment 1, according to GB/T15000 " standard model work directive/guide " and YS/T409 " nonferrous metal product analysis standard model technical manual " regulation, variance method is adopted to carry out uniformity testing to sample random sampling, in checkout procedure, for eliminating the impact of instrument drift and light source fluctuation, adopt blocked operation method to substitute former continued operation method and carry out uniformity testing, assay is in table 4, and table 4 is 6016 aluminum alloy standard sample variance method assays.
Table 46016 aluminum alloy standard sample variance method assay
As shown in Table 4, each Elemental redistribution in 6016 Aluminum alloy spectral standard samples that embodiment 1 is obtained is even.
Embodiment 5
The definite value inspection of standard model
The final definite value of standard model is one of most critical index of standard model, definite value must be accurately and reliably, according to GB/T15000 " standard model work directive/guide " and YS/T409 " nonferrous metal product analysis standard model technical manual " regulation, through the 6016 Aluminum alloy spectral standard samples analysis definite values that eight laboratory cooperations such as national light metal Quality Supervision and Inspection Center are obtained to embodiment 1, in 6016 Aluminum alloy spectral standard samples, each element definite value analytical approach is as shown in table 5, and table 5 is each cooperation experiment room definite value analytical approach.
Table 5 each cooperation experiment room definite value analytical approach
Analyze data to cooperation experiment room definite value in accordance with the following methods to process:
(1) Figure correction: undertaken, error ending method by GB/T 8170-2008 " expression of Figure correction rule and limiting figure and judgement ".
(2) Rod Dixon inspection: the result quoted each cooperation experiment room with Rod Dixon test criterion is tested by mean value and accepted or rejected, and Rod Dixon assay is in table 6, and table 6 is 6016 aluminum alloy standard sample Rod Dixon assays.
(3) Normal distribution test: with the normality of each cell mean of Shapiro-Wilk test, assay is in table 7, and table 7 is 6016 aluminum alloy standard sample Xia Piluo assays.
(4) equally accurate inspection: carry out equally accurate inspection by Cochran-test method to each group of data, assay is in table 8, and table 8 is 6016 aluminum alloy standard sample equally accurate assays.
Table 66016 aluminum alloy standard sample Rod Dixon assay (unit: wt%)
As shown in Table 6, assay is as good as constant value.
Table 76016 aluminum alloy standard sample Xia Piluo assay (unit: wt%)
As shown in Table 7, assay is normal distribution.
Table 86016 aluminum alloy standard sample equally accurate assay (unit: wt%)
| Element | Group number | Number in group | Degree of confidence | Critical value | Maximum variance | Variance and | Statistic | Assay |
| Si | 8 | 4 | 0.05 | 0.4377 | 0.000121 | 0.000429 | 0.2821 | Equally accurate |
| Fe | 8 | 4 | 0.05 | 0.4377 | 0.000025 | 0.000079 | 0.3165 | Equally accurate |
| Cu | 8 | 4 | 0.05 | 0.4377 | 0.000009 | 2.18E-05 | 0.4134 | Equally accurate |
| Mn | 8 | 4 | 0.05 | 0.4377 | 2.56E-06 | 7.62E-06 | 0.3360 | Equally accurate |
| Mg | 8 | 4 | 0.05 | 0.4377 | 0.000036 | 0.000154 | 0.2338 | Equally accurate |
| Cr | 8 | 4 | 0.05 | 0.4377 | 1.44E-06 | 3.77E-06 | 0.3820 | Equally accurate |
| Ni | 8 | 4 | 0.05 | 0.4377 | 4.9E-07 | 1.21E-06 | 0.4050 | Equally accurate |
| Zn | 8 | 4 | 0.05 | 0.4377 | 4.9E-07 | 1.78E-06 | 0.2753 | Equally accurate |
| Ti | 8 | 4 | 0.05 | 0.4377 | 6.4E-07 | 1.73E-06 | 0.3699 | Equally accurate |
As shown in Table 8, assay is equally accurate.
Known by Data Management Analysis result, detect data, genuine and believable, data without exception.Calculate the standard value detecting data and standard deviation by the following method:
Standard value
The standard deviation of single measurement:
Synthetic standards deviation (S):
In formula:
S
l 2---the uneven variance of interblock;
S
w 2---uneven variance in block.
The result of calculation of standard value and standard deviation is in table 9, and table 9 is 6016 aluminum alloy standard sample synthetic standards deviation result of calculations.
Table 96016 aluminum alloy standard sample synthetic standards deviation result of calculation
Note: with the value of * after synthetic standards deviation, to show in block not mean square deviation and interblock not mean square deviation can not ignore.
The standard model obtained to embodiment 1 according to the result of calculation of table 9 carries out definite value, and the results are shown in Table 10, table 10 is 6016 aluminum alloy standard sample definite value results.
Table 106016 aluminum alloy standard sample definite value result (unit: wt%)
| Si | Fe | Cu | Mn | Mg | |
| Standard value | 1.16 | 0.130 | 0.101 | 0.079 | 0.522 |
| Single measurement standard deviation | 0.02 | 0.007 | 0.005 | 0.003 | 0.013 |
| Expanded uncertainty | 0.02 | 0.007 | 0.005 | 0.003 | 0.012 |
| Data group number | 8 | 8 | 8 | 8 | 8 |
| Cr | Ni | Zn | Ti | ||
| Standard value | 0.016 | 0.021 | 0.029 | 0.021 | |
| Single measurement standard deviation | 0.002 | 0.001 | 0.002 | 0.001 | |
| Expanded uncertainty | 0.002 | 0.001 | 0.002 | 0.001 | |
| Data group number | 8 | 8 | 8 | 8 |
Note: expanded uncertainty is
k=2.365 (α=0.05, level of significance; ν=m-1=7, degree of freedom).
Embodiment 6
Produce examination
In order to check the effect of standard model of the present invention, 6016 aluminum alloy standard samples embodiment of the present invention 1 prepared are spectral intensity typical curve QSG750, ARL4460 two import spectrometers correcting Si, Fe, Cu, Mn, Mg, Cr, Ni, Zn and Ti as spectrum standard sample in model.
Two spectrometers after using above-mentioned typical curve to correct respectively and chemical analysis carry out constituent analysis to 6016 aluminium alloy testing samples, and the results are shown in Table 11, table 11 is the production result of appraisal.Wherein, the chemical analysis of testing sample carries out with reference to GB/T15000 " standard model work directive/guide " and YS/T409 " nonferrous metal product analysis standard model technical manual ".
The table 11 production result of appraisal (unit: wt%)
| Si | Fe | Cu | Mn | Mg | Cr | Ni | Zn | Ti | Instrument and method |
| 1.13 | 0.21 | 0.12 | 0.063 | 0.51 | 0.008 | 0.005 | 0.010 | 0.021 | QSG750 |
| 1.12 | 0.20 | 0.13 | 0.060 | 0.52 | 0.010 | 0.005 | 0.011 | 0.021 | ARL4460 |
| 1.13 | 0.21 | 0.13 | 0.061 | 0.51 | 0.008 | 0.005 | 0.011 | 0.021 | Chemistry |
As shown in Table 11, the spectrometer analysis result of testing sample conforms to chemical analysis analysis result, illustrate that 6016 Aluminum alloy spectral standard samples that embodiment 1 provides can meet the production of 6016 aluminium alloys and research and develop use, namely can be used for the correction of 6016 aluminum alloy spectrum analysis results, and then improve 6016 aluminium alloy production efficiency and product qualities.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a preparation method for 6016 Aluminum alloy spectral standard samples, comprises the following steps:
A), aluminium source, silicon source, source of iron, Tong Yuan, manganese source, magnesium source, chromium source, nickel source, zinc source and titanium source melt blending, obtain aluminium alloy melt;
Described aluminium alloy melt comprises: the Al of Ni, the Zn of 0.025 ~ 0.2wt% of the Mg of the Cu of the Si of 1.1 ~ 1.5wt%, the Fe of 0.1 ~ 0.5wt%, 0.095 ~ 0.2wt%, the Mn of 0.07 ~ 0.1wt%, 0.5 ~ 0.6wt%, the Cr of 0.01 ~ 0.1wt%, 0.02 ~ 0.05wt%, the Ti of 0.02 ~ 0.15wt% and surplus;
B), described aluminium alloy melt after casting, homogenising thermal treatment and extruding, obtains 6016 Aluminum alloy spectral standard samples successively.
2. preparation method according to claim 1, is characterized in that, described step a) is specially:
A1), aluminium source, silicon source, source of iron, Tong Yuan, manganese source, chromium source, nickel source and titanium source melt blending, obtain the first alloy melt;
A2), described first alloy melt and zinc source melt blending, obtain the second alloy melt;
A3), described second alloy melt and magnesium source melt blending, obtain aluminium alloy melt.
3. preparation method according to claim 1, is characterized in that, described silicon source is Al-Si intermediate alloy; Described source of iron is Al-Fe intermediate alloy; Described copper source is Al-Cu intermediate alloy; Described manganese source is Al-Mn intermediate alloy; Described chromium source is Al-Cr intermediate alloy; Described nickel source is Al-Ni intermediate alloy; Described titanium source is Al-Ti intermediate alloy; Described zinc source is zinc; Described magnesium source is magnesium; Described aluminium source is aluminium and the intermediate alloy containing aluminium.
4. preparation method according to claim 1, is characterized in that, the mode of described casting is that hot direct casting is made.
5. preparation method according to claim 1, is characterized in that, the temperature of described casting is 735 ~ 745 DEG C.
6. preparation method according to claim 1, is characterized in that, the speed of described casting is 72 ~ 78mm/min.
7. preparation method according to claim 1, is characterized in that, the cooling water pressure in described casting process is 0.06 ~ 0.08MPa.
8. preparation method according to claim 1, is characterized in that, the heat treated temperature of described homogenising is 515 ~ 530 DEG C; The heat treated temperature retention time of described homogenising is 12 ~ 14h.
9. preparation method according to claim 1, is characterized in that, the temperature of described extruding is 430 ~ 450 DEG C; The speed of described extruding is 3 ~ 5mm/s.
10. preparation method according to claim 1, it is characterized in that, described aluminium alloy melt comprises: the Al of Ni, the Zn of 0.027 ~ 0.031wt% of the Mg of the Cu of the Si of 1.14 ~ 1.18wt%, the Fe of 0.123 ~ 0.137wt%, 0.096 ~ 0.106wt%, the Mn of 0.076 ~ 0.082wt%, 0.51 ~ 0.534wt%, the Cr of 0.014 ~ 0.018wt%, 0.02 ~ 0.022wt%, the Ti of 0.02 ~ 0.022wt% and surplus.
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