CN1837786A - Primary magnesium ingot standard spectrum sample and preparation method thereof - Google Patents
Primary magnesium ingot standard spectrum sample and preparation method thereof Download PDFInfo
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- CN1837786A CN1837786A CNA2006100781158A CN200610078115A CN1837786A CN 1837786 A CN1837786 A CN 1837786A CN A2006100781158 A CNA2006100781158 A CN A2006100781158A CN 200610078115 A CN200610078115 A CN 200610078115A CN 1837786 A CN1837786 A CN 1837786A
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Abstract
This invention relates to a primary magnesium ingot standard spectrum sample and preparation method, <0}Wherein, it comprises as weight percent: Si 0.001~0.045, Fe 0.0018~0.033, Cu 0.0004~0.027, Ni 0.0002~0.011, Pb 0.0019~0.045, Zn 0.006~0.053, Mn 0~0.16, Al 0~0.26 and Ti 0~0.003. This invention has even and stable ingredient fit to Mg-alloy ingredient check.
Description
Technical field
The present invention relates to a kind of primary magnesium ingot standard spectrum sample and preparation method thereof, belong to the manufacturing field of alloy.
Background technology
Magnesium and magnesium alloy are the minimum structural metallic materials of density, and its specific strength is higher than steel, and have good antifatigue and damping performance.Therefore, be used to make transport facility and the Aero-Space parts have special significance.Country attaches great importance to the development and the development of magnesium and magnesium alloy, and State Council has classified the development of magnesium and magnesium alloy materials as one of the Tenth Five-Year Plan (2001-2005) main project of national economy and social development.
As a kind of development of new material, be unable to do without the chemical composition analysis check, and chemical composition analysis be unable to do without standard model.We can say that the development of standard model is an a kind of fundamental research of development of new structural metallic materials.Southwestern Aluminum (group) company limited had developed MgAlMn, MgAlZn, three serial magnesium alloy standard models of MgAlSi in 2002, had satisfied above-mentioned needs well.But because the development of magnesium material is very fast, many new materials constantly are developed, and all need corresponding standard specimen.Therefore, magnesium standard specimen breach is very big, can not adapt to the demand for development of country, Chongqing City's magnesium industry far away, also has many standard specimens suddenly to wait to develop.
Reach reasons such as safety technique owing to the magnesium chemical activity by force, determined that magnesium and magnesium alloy standard specimen development difficulty is more much bigger than aluminium standard specimen.Technical difficult points is as follows:
(1) ingot casting easily produces slag inclusion, and some element casting yield alters a great deal, and is restive, and especially micro-Pb, elements such as Ti, Ni are difficult to add in the magnesium; And easily segregation such as Fe, Ti, Mn, Pb etc.
(2) chemical constitution is adjusted difficulty: because no suitable standard specimen can't be formulated the on-the-spot sample analysis rules, bring very big difficulty for adjustment standard specimen ingot casting chemical constitution.In addition, Pb, Zn, three elements of Ti (generally not requiring), former remelting does not require analysis with magnesium ingot.And Pb, Zn, three elements of Ti have been increased in the new standard primary magnesium ingot standard.
3. safety related technical problems: the chemical activity of magnesium is very strong, in molten condition, very easily with oxygen, nitrogen and water generation chemical action.At bath surface as strictly protection, very fast oxidizing fire just during near 800 ℃.In technological process, liquid metal is directly met water and is just produced the blast of splashing property, must strictly note.In addition, harmful gas and dust all should be dealt carefully with.
4. pure magnesium standard specimen surface anti-oxidation, anticorrosion problem also are difficult points.
Summary of the invention
The object of the present invention is to provide a kind of primary magnesium ingot standard spectrum sample, to satisfy the needs of alloy production.
The present invention adopts following technical scheme: a kind of primary magnesium ingot standard spectrum sample, it is characterized in that, and in pure magnesium, evenly contain the element of following weight number percent:
Si?0.001~0.045,Fe?0.0018~0.033,Cu?0.0004~0.027,
Ni?0.0002~0.011,Pb?0.0019~0.045,Zn?0.006~0.053,
Mn?0~0.16,Al?0~0.26,Ti?0~0.003。
The present invention also provides a kind of preparation method of primary magnesium ingot standard spectrum sample, and this method comprises following process:
1) melting
(1) furnace temperature is elevated to about 400 ℃-450 ℃ and carries out baker, be sprinkled into the flux of furnace charge to 1%, add intermediate alloy required among magnesium ingot, Mg-Si, Mg-Mn, Mg-Ni, the Mg-Cu then as required, be sprinkled into the fusing that heats up of 1% flux;
(2) when metal all melts the back and is superheated to 950 ℃-970 ℃, be sprinkled into stirring in the molten metal, while being sprinkled into the doubly excessive reduced iron powder of 5-7, then add rafifinal, Al-Ti, pure zinc, fine aluminium; In reinforced process, constantly be sprinkled into flux protection molten metal pressure surface to prevent the scaling loss of magnesium;
(3) sample analysis: treat to stir secondary behind whole metal moltens; Be 9-11 minute at interval at every turn, skim then; The then sample analysis of back of skimming according to analysis result, is adjusted its chemical constitution till adhere to specification;
(4) refining: treat that chemical constitution is qualified back with Ar gas refining 6-8 minute, left standstill 12-15 minute;
2) casting: cast with semicontinuous casting machine, the graphite funnel carries out separatory, and cooling water pressure is controlled at 0.06MPa-0.07MPa, adjust temperature to 820 ℃-830 ℃, casting speed is controlled at 70mm/ branch-75mm/ branch, and being cast as diameter at last is the 192mm cylinder ingots, i.e. the standard specimen ingot casting;
3) standard specimen homogenizing cast ingot
The control furnace temperature is placed on the standard specimen ingot casting in the stove at 420 ℃-430 ℃, is cooled to room temperature with furnace temperature in insulation under 370 ℃ of-410 ℃ of temperature after 12 hours;
4) processing such as extruding, sawing
The standard specimen ingot casting that homogenising is handled is squeezed into the bar of diameter 45mm again through 2000 tons of oil pressure extruders, sawing becomes the small cylindrical of φ 45 * 40mm again, promptly is last standard model;
5) the standard specimen surface anticorrosion is handled: the oxidation colouring is carried out on the standard model surface, made the surface be golden yellow.
Primary magnesium ingot standard spectrum sample provided by the invention can be used in the check of magnesium alloy composition, can satisfy the needs that magnesium alloy is produced.The preparation method of primary magnesium ingot standard spectrum sample provided by the invention, solved the technical barrier of primary magnesium ingot standard spectrum sample preparation, can prepare the primary magnesium ingot standard spectrum sample that can meet the demands, this sample composition is evenly reasonable, and good stability is difficult for oxidation.
Description of drawings
Fig. 1 is the metallographic macrograph of E4133 primary magnesium ingot standard spectrum sample.
Embodiment
Below in conjunction with specific embodiment primary magnesium ingot standard spectrum sample of the present invention and preparation method thereof is described further.
Embodiment 1
Standard specimen number is the primary magnesium ingot standard spectrum sample of E4131, evenly contains whole elements of following weight percent: Si 0.010, Fe 0.003, Cu 0.0010, Mn 0.015, Ni 0.0004, Al 0.010, Pb 0.0040, Ti 0.0003, Zn 0.010 in pure magnesium.
Embodiment 2
Standard specimen number is the primary magnesium ingot standard spectrum sample of E4132, evenly contains whole elements of following weight percent: Si 0.060, Fe 0.030, Cu 0.007, Mn 0.100, Ni 0.010, Pb 0.040, Ti 0.0002, Zn 0.050 in pure magnesium.
Embodiment 3
Standard specimen number is the primary magnesium ingot standard spectrum sample of E4133, evenly contains whole elements of following weight percent: Si 0.020, Fe 0.010, Cu 0.010, Mn 0.020, Ni 0.002, Al 0.015, Pb 0.010 in pure magnesium.
Embodiment 4
Standard specimen number is the primary magnesium ingot standard spectrum sample of E4134, evenly contains whole elements of following weight percent: Si 0.040, Fe 0.007, Cu 0.015, Mn 0.025, Ni 0.004, Al 0.25, Pb 0.015, Ti 0.001, Zn 0.020 in pure magnesium.
Embodiment 5
Standard specimen number is the primary magnesium ingot standard spectrum sample of E4135, evenly contains whole elements of following weight percent: Si 0.002, Fe 0.002, Cu 0.0005, Mn 0.005, Ni 0.0003, Al 0.005, Pb 0.002, Zn 0.007 in pure magnesium.
Embodiment 6
Standard specimen number is the primary magnesium ingot standard spectrum sample of E4136, evenly contains whole elements of following weight percent: Si 0.015, Fe 0.020, Cu 0.025, Mn 0.150, Ni 0.005, Pb 0.020, Ti 0.0025, Zn 0.025 in pure magnesium.
Embodiment 7
Standard specimen number is the primary magnesium ingot standard spectrum sample of E4137, evenly contains whole elements of following weight percent: Si 0.030, Fe 0.005, Cu 0.005, Ni 0.0015, Al 0.010, Pb 0.006, Ti 0.0001, Zn 0.015 in pure magnesium.
Embodiment 8
The preparation method of primary magnesium ingot standard spectrum sample, this method comprises following process successively:
1) melting
(1) furnace temperature is elevated to about 400 ℃-450 ℃ and carries out baker, be sprinkled into the flux of furnace charge to 1%, add intermediate alloy required among magnesium ingot, Mg-Si, Mg-Mn, Mg-Ni, the Mg-Cu then as required, be sprinkled into the fusing that heats up of 1% flux;
(2) when metal all melts the back and is superheated to 950 ℃-970 ℃, be sprinkled into stirring in the molten metal, while being sprinkled into the doubly excessive reduced iron powder of 5-7, then add rafifinal (the aluminium mass content is below 99.999%), Al-Ti, pure zinc, fine aluminium (the aluminium mass content is 99.7%-99.8%); In reinforced process, constantly be sprinkled into flux protection molten metal pressure surface to prevent the scaling loss of magnesium;
(3) sample analysis: treat to stir secondary behind whole metal moltens; Be 9-11 minute at interval at every turn, skim then; The then sample analysis of back of skimming according to analysis result, is adjusted its chemical constitution till adhere to specification;
(4) refining: treat that chemical constitution is qualified back with Ar gas refining 6-8 minute, left standstill 12-15 minute;
2) casting: cast with semicontinuous casting machine, the graphite funnel carries out separatory, and cooling water pressure is controlled at 0.06MPa-0.07MPa, adjust temperature to 820 ℃-830 ℃, casting speed is controlled at 70mm/ branch-75mm/ branch, and being cast as diameter at last is the 192mm cylinder ingots, i.e. the standard specimen ingot casting;
3) standard specimen homogenizing cast ingot
The control furnace temperature is placed on the standard specimen ingot casting in the stove at 420 ℃-430 ℃, is cooled to room temperature with furnace temperature, so that each element is even in insulation under 370 ℃ of-410 ℃ of temperature after 12 hours;
4) processing such as extruding, sawing
The standard specimen ingot casting that homogenising is handled is squeezed into the bar of diameter 45mm again through 2000 tons of oil pressure extruders, sawing becomes the small cylindrical of φ 45 * 40mm again, promptly is last standard model;
5) the standard specimen surface anticorrosion is handled: the oxidation colouring is carried out on the standard model surface, made the surface be golden yellow, in case oxidation corrosion etc.
Check: to adopting the standard model of the method preparation in the present embodiment, carried out uniformity testing, initial survey comprises metallographic structure check and ingotism check.Fig. 1 is the metallographic macrograph (1: 2) of the E4133 among the embodiment 3, by the metallographic specimen macroscopic examination, proves ingot structure densification, evenly, pore-free, loose and defective such as be mingled with.The ingotism check, by radially checking (Da Weite check) and vertically segregation check (t check), the result shows footpath, vertically equal segregation-free.
According to GB/T15000 and YS/T409-1998 regulation, adopted range method to carry out uniformity testing, for eliminating the influence of instrument drift and light source fluctuation, adopt the blocked operation method to substitute continued operation method in the past and carried out uniformity testing, the result shows that each element is all qualified.
Claims (8)
1, a kind of primary magnesium ingot standard spectrum sample, it is characterized in that, the element that evenly contains following weight number percent in pure magnesium: Si 0.001~0.045, and Fe 0.0018~0.033, Cu0.0004~0.027, Ni 0.0002~0.011, Pb 0.0019~0.045, and Zn 0.006~0.053, and Mn 0~0.16, Al 0~0.26, and Ti 0~0.003.
2, primary magnesium ingot standard spectrum sample as claimed in claim 1 is characterized in that evenly containing whole elements of following weight percent: Si 0.010, Fe 0.003, Cu 0.0010, Mn 0.015, Ni 0.0004, Al 0.010, Pb 0.0040, Ti 0.0003, Zn 0.010 in pure magnesium.
3, primary magnesium ingot standard spectrum sample as claimed in claim 1 is characterized in that evenly containing whole elements of following weight percent: Si 0.060, Fe 0.030, Cu 0.007, Mn 0.100, Ni 0.010, Pb 0.040, Ti 0.0002, Zn 0.050 in pure magnesium.
4, primary magnesium ingot standard spectrum sample as claimed in claim 1 is characterized in that evenly containing whole elements of following weight percent: Si 0.020, Fe 0.010, Cu 0.010, Mn 0.020, Ni 0.002, Al 0.015, Pb 0.010 in pure magnesium.
5, primary magnesium ingot standard spectrum sample as claimed in claim 1 is characterized in that evenly containing whole elements of following weight percent: Si 0.040, Fe 0.007, Cu 0.015, Mn 0.025, Ni 0.004, Al 0.25, Pb 0.015, Ti 0.001, Zn 0.020 in pure magnesium.
6, primary magnesium ingot standard spectrum sample as claimed in claim 1 is characterized in that evenly containing whole elements of following weight percent: Si 0.002, Fe 0.002, Cu 0.0005, Mn 0.005, Ni 0.0003, Al 0.005, Pb 0.002, Zn 0.007 in pure magnesium.
7, primary magnesium ingot standard spectrum sample as claimed in claim 1 is characterized in that evenly containing whole elements of following weight percent: Si 0.015, Fe 0.020, Cu 0.025, Mn 0.150, Ni 0.005, Pb 0.020, Ti 0.0025, Zn 0.025 in pure magnesium.
8, as the preparation method of the described primary magnesium ingot standard spectrum sample of arbitrary claim in the claim 1 to 7, it is characterized in that this method comprises following process successively:
1) melting
(1) furnace temperature is elevated to about 400 ℃-450 ℃ and carries out baker, be sprinkled into the flux of furnace charge to 1%, add intermediate alloy required among magnesium ingot, Mg-Si, Mg-Mn, Mg-Ni, the Mg-Cu then as required, be sprinkled into the fusing that heats up of 1% flux;
(2) when metal all melts the back and is superheated to 950 ℃-970 ℃, be sprinkled into stirring in the molten metal, while being sprinkled into the doubly excessive reduced iron powder of 5-7, then add rafifinal, Al-Ti, pure zinc, fine aluminium; In reinforced process, constantly be sprinkled into flux protection molten metal pressure surface to prevent the scaling loss of magnesium;
(3) sample analysis: treat to stir secondary behind whole metal moltens; Be 9-11 minute at interval at every turn, skim then; The then sample analysis of back of skimming according to analysis result, is adjusted its chemical constitution till adhere to specification;
(4) refining: treat that chemical constitution is qualified back with Ar gas refining 6-8 minute, left standstill 12-15 minute;
2) casting: cast with semicontinuous casting machine, the graphite funnel carries out separatory, and cooling water pressure is controlled at 0.06MPa-0.07MPa, adjust temperature to 820 ℃-830 ℃, casting speed is controlled at 70mm/ branch-75mm/ branch, and being cast as diameter at last is the 192mm cylinder ingots, i.e. the standard specimen ingot casting;
3) standard specimen homogenizing cast ingot
The control furnace temperature is placed on the standard specimen ingot casting in the stove at 420 ℃-430 ℃, is cooled to room temperature with furnace temperature in insulation under 370 ℃ of-410 ℃ of temperature after 12 hours;
4) extruding, sawing processing
The standard specimen ingot casting that homogenising is handled is squeezed into the bar of diameter 45mm again through 2000 tons of oil pressure extruders, sawing becomes the small cylindrical of φ 45 * 40mm again, promptly is last standard model;
5) the standard specimen surface anticorrosion is handled: the oxidation colouring is carried out on the standard model surface, made the surface be golden yellow.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103667835A (en) * | 2012-09-24 | 2014-03-26 | 天津德盛镁科技发展有限公司 | Method for preparing high-purity standard substance of magnesium alloy spectra |
CN104198239A (en) * | 2014-08-15 | 2014-12-10 | 哈尔滨东安发动机(集团)有限公司 | ZM-6 magnesium alloy spectrographic standard substance |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103667835A (en) * | 2012-09-24 | 2014-03-26 | 天津德盛镁科技发展有限公司 | Method for preparing high-purity standard substance of magnesium alloy spectra |
CN104198239A (en) * | 2014-08-15 | 2014-12-10 | 哈尔滨东安发动机(集团)有限公司 | ZM-6 magnesium alloy spectrographic standard substance |
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