CN102337475A - Method for manufacturing extra-low oxygen low-expansion alloy - Google Patents
Method for manufacturing extra-low oxygen low-expansion alloy Download PDFInfo
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- CN102337475A CN102337475A CN2011103103985A CN201110310398A CN102337475A CN 102337475 A CN102337475 A CN 102337475A CN 2011103103985 A CN2011103103985 A CN 2011103103985A CN 201110310398 A CN201110310398 A CN 201110310398A CN 102337475 A CN102337475 A CN 102337475A
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Abstract
The invention discloses a method for manufacturing an extra-low oxygen low-expansion alloy. The total oxygen content of the extra-low oxygen low-expansion alloy is less than 10ppm. The method for manufacturing the extra-low oxygen low-expansion alloy adopts the technical flows of electric furnace smelting, AOD (Argon Oxygen Decarburization) refining, LF (Ladle Furnace) refining and continuous casting. Therefore, compared with the traditional method for manufacturing a low-expansion alloy, the method disclosed by the invention has the following advantages that the product manufactured by the technical scheme has low oxygen content and high purity so as to obviously improve product quality. While the technical flow is simplified by the technical scheme, the metal yield rate is improved so as to greatly lower production cost.
Description
Technical field
The present invention relates to a kind of steel grade method of manufacture, relate in particular to a kind of method of manufacture of low expansion alloy.
Background technology
Low expansion alloy is a kind of Rhometal, and it is the specific alloy of a kind of nickel content about 36%, also is called as Invar alloy, is at first to be found by the Switzerland physicist Xia Er Edward Yao's nurse (C.E.Guillaume) of recording in 1896.This alloy is very big to the contribution of scientific progress, and therefore this alloy discoverer-Switzerland physicist Ji Yao nurse obtains the Nobel Prize in physics of nineteen twenty.
Most metal and alloys all are volumetric expansions when being heated; Volumetric shrinkage during cooling, but Invar alloy is owing to its ferromegnetism, in certain TR; Unusual thermal expansion with invarable effect; Therefore its coefficient of expansion is extremely low, and sometimes even be zero or negative value, near the mean thermal expansion coefficients room temperature is lower than 1 * 10
-6℃
-1Near this low expansion alloy thermal expansivity magnetic temperature (Curie temperature) significantly reduces, and so-called unusual thermal expansion phenomenon (negative unusual) occurs, thereby near can the be room temperature very wide TR, obtains very little even near the zero coefficient of expansion.The composition of this alloy mainly is the Ni about Fe and 36%, is face-centred cubic structure.
Therefore, Invar alloy is fit to do measuring sensor, mainly is used for resonator cavity, gravity meter member, thermo bimetal's group element material of manufacturer's standard chi, thermo detector, stadimeter, verge ring, slip gauge, microwave equipment, opticinstrument part etc.In addition, this low expansion alloy also is applicable to the glass sealing alloy of electric elements and hard glass, soft glass, ceramic matched seal.Its state has two kinds of hard attitude and soft attitudes, and promptly Invar alloy/involution gold has the lower coefficient of expansion and good plasticity-in-60 ℃~80 ℃ free air temperatures change.Therefore, Invar alloy is applied to being produced on temperature Change scope inside dimension and is bordering on the constant element, is widely used in wireless, precision meter, instrument and other industry.
According to relevant, China's actual usage quantity of low expansion alloy in 2005 has reached about 8000 tons, and its 60% above dependence on import, and state's output is relatively low, and imbalance between supply and demand is very outstanding.In addition, for a long time, international, domestic main employing traditional processing technology, that is: raw material → vacuum oven or antivacuum stove smelting → ingot casting → esr → atmosphere protection heating → hot rolling → cold working → finished product; Perhaps raw material → electrosmelting → AOD → LF refining → static ingot → hot rolling → cold working → finished product.Comparatively speaking, external low expansion alloy quality product is superior to the like product of domestic enterprise.But because traditional processing technology exists single furnace output on the low side, problems such as operation is many, long flow path cause the product lumber recovery very low, and unstable product quality, product cost are higher.Domestic enterprise particularly, because equipment and Technology backwardness, a large amount of formation of surface crack in the low expansion alloy course of processing sometimes cause product inner quality and surface quality relatively poor, and product performance are difficult to satisfy the requirement of product industry standard.
Table 1 has been listed the international manufacturers produce low expansion alloy mode of production and composition characteristic.
Table 1.
Manufacturing concern | The mode of production | Al% in the alloy | Ti% in the alloy | Oxygen level ppm |
France Imphy company | Die casting | 0~0.01 | Trace | 20~60 |
Japan Yakin company | Continuous casting | 0~0.01 | Trace | 20~60 |
U.S. Carpenter company | Die casting | 0~0.01 | Trace | 20~60 |
Thyssen VDM company | Die casting | 0~0.01 | Trace | 20~60 |
Summary of the invention
The object of the present invention is to provide a kind of method of manufacture of ultralow oxygen low expansion alloy; The method of manufacture of this ultralow oxygen low expansion alloy adopts the operational path of electrosmelting → AOD refining → LF refining → continuous casting; Can simplify technical process; And significantly improved the quality and the recovery rate of iron of product, can reduce production costs simultaneously.
The inventive concept of the method for manufacture of ultralow oxygen low expansion alloy of the present invention is through in process of production the content of oxygen being controlled, thereby obtains the product than high cleanliness, and then improves the quality and the recovery rate of iron of product.
According to the foregoing invention purpose, the invention provides a kind of method of manufacture of ultralow oxygen low expansion alloy, the total oxygen content of said ultralow oxygen low expansion alloy comprises the following steps: less than 10ppm
(1) electrosmelting: raw material is carried out electrosmelting, and melting finishes when C in the molten steel >=1.5wt%;
(2) AOD refining: the mixed gas of aerating oxygen and argon gas carries out the AOD refining, behind C≤0.02wt% in the molten steel, adds reductive agent ferrosilicon and aluminium, and the part by weight of said aluminium and ferrosilicon is controlled to be 1/4~1/2, and AOD refining terminal point is control S≤0.003wt%;
(3) LF refining: the bottom feeds argon gas molten steel is stirred, and adopts foamy slag to make slag blanket parcel electric arc, and the composition of said foamy slag is CaO 30-50wt%, SiO
215-25wt%, Al
2O
315-40wt%, MgO 3-15wt%, (MnO+FeO)≤and 0.5wt%, surplus is a unavoidable impurities; In molten steel, add metallic aluminium in the LF refining later stage, LF refining terminal point is control S≤0.001wt%, Al>=0.02wt%;
(4) add Ti0.03-0.1wt% to above-mentioned the completion in the LF purified molten steel, and carry out the soft stirring (be that the furnace bottom Argon stirs, molten steel springs up, but the top slag covers the molten steel face fully, not the exposed steel liquid level) of 5-15min, form TiO in the steel thereby make
2Or TiN fine particle;
(5) continuous casting: adopt induction stirring to make above-mentioned TiO
2Or TiN fine particle uniform distribution, the electric current of induction stirring is 1200-2000A, frequency is 2.5-3.5Hz; The basicity of continuous casting covering slag is 1.0-1.2, and softening temperature is 1000-1150 ℃, and yield point is 1050-1150 ℃, and viscosity is 1.5-2.5poise, and the composition of continuous casting covering slag is CaO:36-40wt%; SiO
2: 30-39wt%; MgO:3-6wt%; Al
2O
3: 4-7wt%; MnO≤1.2wt%; FeO≤1.5wt%, surplus is an impurity; Slab proportion of equiaxed grain>=30% behind the continuous casting; The mass percentage content of slab composition is: C 0-0.03%, Si0-0.30%, Mn 0-0.40%, Ni 35.0-37.0%, P≤0.035%, S≤0.010%, Cr≤0.25%, O≤0.001%, Al>=0.02%, Ti0.03-0.1%, surplus is Fe and unavoidable impurities.
In the present technique scheme, step (2) will be controlled to be 1/4~1/2nd as the aluminium of reductive agent and the part by weight of ferrosilicon, in order to reduce the oxygen in slag and the molten steel rapidly.
When step (3) LF refining, adopt foamy slag technology, be in order to make foamy slag slag blanket thickening parcel electric arc, thereby prevent in the heated by electrodes process that carbon content increases in the liquid alloy.
In step (4), add Ti, through the effective exclusive segment inclusion of the soft stirring of an end time, the purity of assurance alloy, and impel the tiny TiO of formation in the steel
2Or the TiN fine particle, these fine particles can be as the forming core particle in process of setting, and crystal grain that can refinement alloy initial solidification increases proportion of equiaxed grain.
When step (5) continuous casting, the covering slag that continuous casting adopts can further reduce the oxygen level in the alloy.Adopt induction stirring can make the TiO in the alloy
2, TiN molecule uniform distribution, help forming equiax crystal, the material plasticity variation of avoiding inclusion to gather partially causing.
Preferably, in the method for manufacture of above-mentioned ultralow oxygen low expansion alloy, also comprise step (6) continuous casting steel billet reconditioning.
Preferably, in the method for manufacture of above-mentioned ultralow oxygen low expansion alloy, tapping temperature is >=1630 ℃ in the said step (1).
Preferably, in the method for manufacture of above-mentioned ultralow oxygen low expansion alloy, adopt oxygen blast to flux oxygen usage quantity<10m in the said step (1)
3/ t.
Preferably, in the method for manufacture of above-mentioned ultralow oxygen low expansion alloy, tapping temperature is >=1600 ℃ in the said step (2), adds metallic aluminium 0.2-0.4kg/t in the tapping forward direction molten steel.
Preferably, in the method for manufacture of above-mentioned ultralow oxygen low expansion alloy, tapping temperature is 1440-1460 ℃ in the said step (3).
Preferably, in the method for manufacture of above-mentioned ultralow oxygen low expansion alloy, the pulling rate of continuous casting is 0.4-1.0m/min in the said step (5).
The method of manufacture of ultralow oxygen low expansion alloy of the present invention makes its method of manufacture than existing low expansion alloy have the following advantages owing to adopted technique scheme:
1, the method for manufacture of ultralow oxygen low expansion alloy of the present invention has adopted continuous casting production process, thereby makes that whole manufacturing process flow is simple, the good quality of product that finally makes, and recovery rate of iron increases substantially, and has reduced production cost;
2, the method for manufacture of ultralow oxygen low expansion alloy of the present invention makes in the LF refining process and forms foamy slag through control LF slag composition, and parcel electric arc is full of Ar gas in the foamy slag, avoids air to infiltrate, and causes liquid alloy oxygenation;
3, the method for manufacture of ultralow oxygen low expansion alloy of the present invention is through adding an amount of Al and Ti in the LF refining later stage in molten steel; And adopt soft stirring to get rid of the inclusion in the liquid alloy, effectively with the Control for Oxygen Content in the alloy in level less than 10ppm;
4, the method for manufacture of ultralow oxygen low expansion alloy of the present invention adopts induction stirring and proper protection slag can make part inclusion floating in the alloy in the continuous casting step, and being evenly distributed of inclusion, further reduces the oxygen level in the alloy.
Embodiment
Embodiment 1-4
Adopt following step to prepare ultralow oxygen low expansion alloy:
(1) electrosmelting: raw material is carried out electrosmelting, and carry out oxygen blast and flux, oxygen usage quantity<10m
3/ t, melting finishes when C in the molten steel>=1.5wt%, and tapping temperature is controlled at>=1630 ℃, molten steel poured into be transported to the AOD stove in the ladle.
(2) AOD refining: the mixed gas of aerating oxygen and argon gas carries out the AOD refining.Behind C≤0.02wt% in the molten steel; Adding reductive agent ferrosilicon and aluminium reduces; The part by weight of aluminium and ferrosilicon is controlled to be 1/4~1/2, and AOD refining terminal point is control S≤0.003wt%, and tapping temperature is controlled at>=and 1600 ℃; Add metallic aluminium in the tapping forward direction molten steel, then ladle is transported to the LF stove.
(3) LF refining: the bottom feeds argon gas molten steel is stirred, and does not allow exposed molten steel face during stirring.Adopt foamy slag to make slag blanket parcel electric arc, the composition of foamy slag is CaO 30-50wt%, SiO
215-25wt%, Al
2O
315-40wt%, MgO 3-15wt%, (MnO+FeO)≤and 0.5wt%, surplus is a unavoidable impurities; Adopt the line feeding mode in molten steel, to add Al in the LF refining later stage, LF refining terminal point is control S≤0.001wt%, Al>=0.02wt%, and tapping temperature is controlled at 1440-1460 ℃.
(4) adopt the line feeding mode to add the Ti of 0.03-0.1wt% in the LF purified molten steel to above-mentioned the completion, and carry out the soft stirring of 5-15min, make and form TiO in the steel
2Or the TiN fine particle, ladle is transported to vertical continuous caster pours into a mould.
(5) continuous casting: the pulling rate of continuous casting is controlled at 0.4-1.0m/min; Adopt induction stirring to make above-mentioned TiO
2Or TiN fine particle uniform distribution, the electric current of induction stirring is 1200-2000A, frequency is 2.5-3.5Hz; Basicity (the CaO/SiO of continuous casting covering slag
2) be 1.0-1.2, softening temperature is 1000-1150 ℃, and yield point is 1050-1150 ℃, and viscosity is 1.5-2.5poise, and the composition of continuous casting covering slag is CaO:36-40wt%; SiO
2: 30-39wt%; MgO:3-6wt%; Al
2O
3: 4-7wt%; MnO≤1.2wt%; FeO≤1.5wt%; Slab proportion of equiaxed grain>=30% behind the continuous casting; The mass percentage content of slab composition is: C 0-0.03%, Si 0-0.30%, Mn 0-0.40%, Ni 35.0-37.0%, P≤0.035%, S≤0.010%, Cr≤0.25%, O≤0.001%, Al>=0.02%, Ti 0.03-0.1%, surplus is Fe and unavoidable impurities (composition of slab is seen table 2 among this case embodiment 1-4).
(6) continuous casting steel billet is carried out reconditioning, reconditioning can be carried out at normal temperatures, and the reconditioning damage control is at 1-3wt%.
Table 2. (wt%, surplus be Fe and except that S, P other unavoidable impurities)
C | Si | Mn | Cr | Ni | P | S | O | Al | Ti | |
Embodiment 1 | 0.01 | 0.30 | 0.05 | 0.1 | 35.0 | 0.025 | 0.002 | 0.0008 | 0.023 | 0.07 |
Embodiment 2 | 0.03 | 0.30 | 0.18 | 0.1 | 35.6 | 0.029 | 0.003 | 0.0007 | 0.059 | 0.09 |
Embodiment 3 | 0.03 | 0.09 | 0.05 | 0.1 | 36.2 | 0.02 | 0.001 | 0.0006 | 0.05 | 0.03 |
Embodiment 4 | 0.01 | 0.30 | 0.05 | 0.1 | 35.0 | 0.008 | 0.001 | 0.0008 | 0.043 | 0.05 |
Table 3 has been listed the concrete processing parameter of each step among this case embodiment 1-4.
Table 3.
Table 4 has been listed the composition of the middle foamy slag of step (3) of this case embodiment 1-4.
Table 4. (wt%, surplus is other unavoidable impurities)
?CaO | SiO 2 | Al 2O 3 | MgO | MnO+FeO | |
Embodiment 1 | ?30 | 15 | 40 | 14 | 0.3 |
Embodiment 2 | ?50 | 25 | 15 | 8 | 0.5 |
Embodiment 3 | ?35 | 18 | 21 | 10 | 0.2 |
Embodiment 4 | ?40 | 20 | 30 | 3 | 0.1 |
Table 5 has been listed the characteristic of continuous casting covering slag among the embodiment 1-4.
Table 5.
Basicity CaO/SiO 2 | Softening temperature (℃) | Yield point (℃) | Viscosity (poise) | |
Embodiment 1 | 1.0 | 1000 | 1050 | ?1.5 |
Embodiment 2 | 1.2 | 1150 | 1150 | ?2.5 |
Embodiment 3 | 1.1 | 1100 | 1100 | ?2.0 |
Embodiment 4 | 1.05 | 1050 | 1120 | ?1.8 |
Table 6 has been listed the composition of continuous casting covering slag among this case embodiment 1-4.
Table 6. (wt%, surplus is other unavoidable impurities)
CaO | SiO 2 | MgO | Al 2O 3 | MnO | FeO | |
Embodiment 1 | 36 | 30 | 5 | 5 | 1.2 | 0.2 |
Embodiment 2 | 39 | 35 | 4 | 6 | 1.0 | 0.5 |
Embodiment 3 | 40 | 38 | 6 | 4 | 0.5 | 0.8 |
Embodiment 4 | 39 | 39 | 3 | 7 | 0.3 | 1.5 |
Adopt the oxygen level of the product that product oxygen level that the method for manufacture of ultralow oxygen low expansion alloy of the present invention produces produces well below traditional low expansion alloy method of manufacture; The oxygen level of the product of traditional method manufacturing is about about 0.003-0.0045%, exceeds several times of the products that the present technique scheme makes; And the product inclusion that adopts the present technique scheme to produce is evenly distributed, and do not exist inclusion to assemble agglomerating bunch and cause material plasticity variation, and the proportion of equiaxed grain of continuously cast bloom is all more than 30%; In addition, use the present technique scheme to produce the cost of the cost of product well below the method for manufacture production product of traditional low expansion alloy, the production cost of classical production process exceeds 40-60% than present technique scheme.
Be noted that above enumerate be merely specific embodiment of the present invention, obviously the invention is not restricted to above embodiment, many similar variations are arranged thereupon.If those skilled in the art all should belong to protection scope of the present invention from all distortion that content disclosed by the invention directly derives or associates.
Claims (7)
1. the method for manufacture of a ultralow oxygen low expansion alloy, the total oxygen content of said ultralow oxygen low expansion alloy is characterized in that less than 10ppm, comprises the following steps:
(1) electrosmelting: raw material is carried out electrosmelting, and melting finishes when C in the molten steel >=1.5wt%;
(2) AOD refining: the mixed gas of aerating oxygen and argon gas carries out the AOD refining, behind C≤0.02wt% in the molten steel, adds reductive agent ferrosilicon and aluminium, and the part by weight of said aluminium and ferrosilicon is controlled to be 1/4~1/2, and AOD refining terminal point is control S≤0.003wt%;
(3) LF refining: the bottom feeds argon gas molten steel is stirred, and adopts foamy slag to make slag blanket parcel electric arc, and the composition of said foamy slag is CaO 30-50wt%, SiO
215-25wt%, Al
2O
315-40wt%, MgO 3-15wt%, (MnO+FeO)≤and 0.5wt%, surplus is a unavoidable impurities; In molten steel, add Al in the LF refining later stage, LF refining terminal point is control S≤0.001wt%, Al>=0.02wt%;
(4) add Ti0.03-0.1wt% to above-mentioned the completion in the LF purified molten steel, and carry out the soft stirring of 5-15min, make and form TiO in the steel
2Or TiN fine particle;
(5) continuous casting: adopt induction stirring to make above-mentioned TiO
2Or TiN fine particle uniform distribution, the electric current of induction stirring is 1200-2000A, frequency is 2.5-3.5Hz; The basicity of continuous casting covering slag is 1.0-1.2, and softening temperature is 1000-1150 ℃, and yield point is 1050-1150 ℃, and viscosity is 1.5-2.5poise, and the composition of continuous casting covering slag is CaO:36-40wt%; SiO
2: 30-39wt%; MgO:3-6wt%; Al
2O
3: 4-7wt%; MnO≤1.2wt%; FeO≤1.5wt%, surplus is a unavoidable impurities; Slab proportion of equiaxed grain>=30% behind the continuous casting; The mass percentage content of slab composition is: C 0-0.03%, Si 0-0.30%, Mn 0-0.40%, Ni 35.0-37.0%, P≤0.035%, S≤0.010%, Cr≤0.25%, O≤0.001%, Al>=0.02%, Ti 0.03-0.1%, surplus is Fe and unavoidable impurities.
2. the method for manufacture of ultralow oxygen low expansion alloy as claimed in claim 1 is characterized in that, also comprises step (6) continuous casting steel billet reconditioning.
3. according to claim 1 or claim 2 the method for manufacture of ultralow oxygen low expansion alloy is characterized in that tapping temperature is >=1630 ℃ in the said step (1).
4. according to claim 1 or claim 2 the method for manufacture of ultralow oxygen low expansion alloy is characterized in that, adopts oxygen blast to flux oxygen usage quantity<10m in the said step (1)
3/ t.
5. according to claim 1 or claim 2 the method for manufacture of ultralow oxygen low expansion alloy is characterized in that tapping temperature be >=1600 ℃ in the said step (2), adding metallic aluminium 0.2-0.4kg/t in the tapping forward direction molten steel.
6. according to claim 1 or claim 2 the method for manufacture of ultralow oxygen low expansion alloy is characterized in that tapping temperature is 1440-1460 ℃ in the said step (3).
7. according to claim 1 or claim 2 the method for manufacture of ultralow oxygen low expansion alloy is characterized in that the pulling rate of continuous casting is 0.4-1.0m/min in the said step (5).
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CN105088094A (en) * | 2015-08-11 | 2015-11-25 | 宝钢特钢有限公司 | Manufacturing method of nitrogen-controlled austenitic stainless steel large forging piece |
CN106269966A (en) * | 2015-06-06 | 2017-01-04 | 丹阳市凯鑫合金材料有限公司 | A kind of method making invar cold-heading dish circle silk material |
CN115652182A (en) * | 2022-11-04 | 2023-01-31 | 江苏隆达超合金航材有限公司 | Method for controlling gas and inclusions in Invar36 alloy |
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CN106269966A (en) * | 2015-06-06 | 2017-01-04 | 丹阳市凯鑫合金材料有限公司 | A kind of method making invar cold-heading dish circle silk material |
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CN115652182A (en) * | 2022-11-04 | 2023-01-31 | 江苏隆达超合金航材有限公司 | Method for controlling gas and inclusions in Invar36 alloy |
CN115652182B (en) * | 2022-11-04 | 2024-02-02 | 江苏隆达超合金航材有限公司 | Method for controlling gas and inclusion in Invar36 alloy |
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