CN111451275A - Preparation method of Nd/Sm rare earth metal foil - Google Patents
Preparation method of Nd/Sm rare earth metal foil Download PDFInfo
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- CN111451275A CN111451275A CN201910988449.6A CN201910988449A CN111451275A CN 111451275 A CN111451275 A CN 111451275A CN 201910988449 A CN201910988449 A CN 201910988449A CN 111451275 A CN111451275 A CN 111451275A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/40—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/46—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling metal immediately subsequent to continuous casting
- B21B1/466—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling metal immediately subsequent to continuous casting in a non-continuous process, i.e. the cast being cut before rolling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
Abstract
The invention belongs to the technical field of metal material processing, and provides a preparation method of Nd/Sm rare earth metal foil, which comprises the following steps: smelting Nd/Sm rare earth metal in an argon atmosphere by adopting a suspension smelting furnace or a medium-frequency induction smelting furnace and casting into an ingot; machining, removing the skin of the cast ingot, and cutting into cylindrical blanks; extruding and cogging, namely putting the blank into a heating furnace to preheat to 520-650 ℃, preserving heat for 0.5-3 h, and then extruding to obtain a strip blank; annealing in vacuum, namely annealing the strip blank for 1-2 hours at 490-620 ℃ in a vacuum state; cold rolling, namely performing multi-pass cold rolling in groups, wherein the reduction deformation of each group is 6-25%, and annealing in an argon atmosphere after 2-4 groups of cold rolling to obtain a metal crude foil; and finishing, namely, after the surface of the metal crude foil is treated, trimming to obtain the Nd/Sm rare earth metal foil.
Description
Technical Field
The invention belongs to the technical field of metal material processing, and particularly relates to a preparation method of a Nd/Sm rare earth metal foil.
Background
The elements of rare earth metal neodymium and samarium are respectively Nd and Sm, and the high-purity Nd/Sm metal foil is used as a detection material for detecting the fluence of activated neutrons, so that the operation is convenient and fast, and the experimental result is accurate. However, the preparation process of the high-purity Nd/Sm rare earth metal foil is difficult, the requirement on processing conditions is high, the technology in the aspect is immature, and relevant reports are not found. The difficulty in preparing the foil is reflected in the following two aspects: firstly, Nd/Sm rare earth metal is difficult to roll at low temperature, pass deformation is low, processing time is long, and a product is easy to crack; secondly, at high temperature, Nd/Sm rare earth metal has large reaction activity, high oxidation speed, reduced product purity and increased reject ratio, and the requirement of the neutron activation detection piece is difficult to achieve.
The prior related patents include a manufacturing method CN108296304A of a small-diameter L a/Ce/Pr/Eu rare earth metal wire, a high-strength high-toughness aluminum alloy plate containing rare earth scandium and erbium and a preparation method CN107841665A of the aluminum alloy plate, and the preparation methods of other metals and alloy foils are not suitable for high-purity Nd/Sm rare earth metals.
The high-purity Nd/Sm rare earth metal foil is easy to oxidize in the rolling process, difficult in process, long in production period, high in rejection rate and difficult to roll and form.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of Nd/Sm rare earth metal foil, which comprises the following steps:
casting: the method comprises the steps of taking Nd/Sm rare earth metal as a raw material, smelting in an argon atmosphere by adopting a suspension smelting furnace or a medium-frequency induction smelting furnace, and casting into an ingot;
machining: removing an oxide layer on the surface of the cast ingot by machining until the surface of the cast ingot has metallic luster, and then cutting the cast ingot into cylindrical blanks of Nd/Sm rare earth metal;
extrusion and cogging: the method comprises the steps of putting a cylindrical blank into a heating furnace, heating and preheating to 520-650 ℃, preserving heat for 0.5-3 h, and then putting the cylindrical blank into an extruder for extrusion cogging to obtain a Nd/Sm rare earth metal strip blank with the thickness of 3.0-4.8 mm;
and (3) vacuum annealing: comprises the steps of putting a strip blank into a vacuum annealing furnace, and annealing for 1-2 h at 490-620 ℃ in a vacuum state;
cold rolling: the method comprises the steps of carrying out multi-pass cold rolling on a strip blank subjected to vacuum annealing, taking 4-8 passes as a group, wherein the reduction of each pass in the same group is the same, the reduction deformation of each group is 6-25%, and annealing is carried out for 0.5-1.5 h at 380-550 ℃ in an argon atmosphere after every 2-4 groups; after the last group is finished, annealing for 0.5-1.5 h at 360-500 ℃ in an argon atmosphere; obtaining a metal coarse foil with the thickness of 0.02-0.15 mm and the width of 50-120 mm;
and (3) finishing: comprises the steps of treating the surface of a metal coarse foil, and cutting to obtain the Nd/Sm rare earth metal foil.
Preferably, in the fusion casting step, the purity of the Nd/Sm rare earth metal raw material is not less than 99.95%.
Preferably, in the machining step, the diameter of the ingot after the surface oxide layer is removed is 55-58 mm.
Preferably, in the extrusion cogging step, the preheating temperature is 560-600 ℃.
Preferably, in the extrusion cogging step, the temperature is kept for 1-2 hours.
Preferably, in the vacuum annealing step, the annealing temperature is 520-580 ℃.
Preferably, in the vacuum annealing step, the annealing temperature is 530-560 ℃, and the annealing time is 1.5 h.
Preferably, in the cold rolling step, the amount of reduction deformation per set is 10% to 20%.
Preferably, in the cold rolling step, annealing is carried out for 0.5-1.5 h at 430-500 ℃ under argon atmosphere after every 2-4 groups.
Preferably, in the finishing step, the surface treatment method includes vacuum polishing.
According to the preparation method of the Nd/Sm rare earth metal foil, the surface oxide layer of the cast ingot is removed by machining, and the subsequent process is carried out in a vacuum or inert gas environment, so that metal is isolated from air, the metal is prevented from being oxidized, and the purity of the material is ensured. In the processing process, cold rolling passes are performed in groups, the reduction deformation of cold rolling is strictly controlled, the breakage of foil materials is reduced, and the rejection rate is reduced. And annealing treatment is inserted between cold rolling pass groups, so that various structural defects and residual stress caused in the rolling process are improved or eliminated, and deformation and cracking are effectively prevented. The high-purity Nd/Sm rare earth metal foil product prepared by the preparation method of the Nd/Sm rare earth metal foil provided by the invention has the advantages of excellent comprehensive mechanical property, high purity, clean appearance and consistent crystal grain size; the preparation method of the Nd/Sm rare earth metal foil is simple in production process, short in period and high in yield, and can realize industrial mass production.
Drawings
FIG. 1 is a flow chart of the method for preparing Nd/Sm rare earth metal foil of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention to solve the technical problems, the present invention will be further described in detail with reference to the accompanying drawings and specific embodiments, which are provided for illustrative purposes and are not drawn to scale or scale completely, and therefore, the accompanying drawings and specific embodiments are not limited to the protection scope of the present invention.
The process of the preparation method of the Nd/Sm rare earth metal foil shown in figure 1 comprises the following steps:
casting S10: the method comprises the steps of taking Nd/Sm rare earth metal as a raw material, smelting in an argon atmosphere by adopting a suspension smelting furnace or a medium-frequency induction smelting furnace, and casting into an ingot;
machining S20: removing an oxide layer on the surface of an ingot by machining until metal luster appears and the diameter is 55-58 mm, and then cutting into Nd/Sm rare earth metal cylindrical blanks;
extrusion cogging S30: the method comprises the steps of putting a cylindrical blank into a heating furnace, heating and preheating to 520-650 ℃, preserving heat for 0.5-3 h, and then putting the cylindrical blank into an extruder for extrusion cogging to obtain a Nd/Sm rare earth metal strip blank with the thickness of 3.0-4.8 mm;
vacuum annealing S40: comprises the steps of putting a strip blank into a vacuum annealing furnace, and annealing for 1-2 h at 490-620 ℃ in a vacuum state;
cold rolling S50: the method comprises the steps of carrying out multi-pass cold rolling on a strip blank subjected to vacuum annealing, generally carrying out 100-400 passes, taking every 4-8 passes as a group, wherein the reduction of each pass in the same group is the same, the reduction deformation of each group is 6-25%, and annealing at 380-550 ℃ for 0.5-1.5 h in an argon atmosphere after every 2-4 groups; after the last group is finished, annealing for 0.5-1.5 h at 360-500 ℃ in an argon atmosphere; obtaining a metal coarse foil with the thickness of 0.02-0.15 mm and the width of 50-120 mm;
finishing S60: comprises the steps of treating the surface of a metal coarse foil, and cutting to obtain the Nd/Sm rare earth metal foil.
In order to better understand the technical solution of the present invention, the following will be further described with reference to specific examples of the method for preparing metal ytterbium foils with different specifications.
In a first specific embodiment, a process for preparing a high-purity rare earth metal Nd foil with a thickness of 0.15mm includes the following steps:
casting: taking a high-purity rare earth metal Nd with the purity of 99.95 percent as a raw material, adopting a medium-frequency induction smelting furnace, smelting in an argon atmosphere and casting into an ingot;
machining: removing an oxide layer on the surface of the cast ingot by using a machining vehicle until metal luster appears, and cutting the cast ingot into a high-purity Nd cylindrical blank with the diameter of 58 mm;
extrusion and cogging: putting the cylindrical blank into a heating furnace, flushing argon as protective atmosphere, heating and preheating to 600 ℃, keeping the temperature for 0.5h, then putting the cylindrical blank into an extruder for extrusion cogging to obtain a strip blank with the thickness of 3.6mm, and putting the strip blank into an oil bath for cooling;
and (3) vacuum annealing: putting the strip blank into a vacuum annealing furnace, and annealing for 1h at 580 ℃ in a vacuum state;
cold rolling: carrying out 100-pass cold rolling on the strip after vacuum annealing, taking 4 passes as a group, totally dividing the strip into 25 groups, wherein the reduction of each pass in the same group is the same, the reduction deformation of each group is 12%, and carrying out primary annealing for 0.5h at 480 ℃ in an argon atmosphere after 4 groups to obtain a crude foil; annealing at 450 ℃ for 1h under the protection of argon after the last group of rolling,
and (3) finishing: and after the rough foil is subjected to vacuum polishing treatment, trimming to obtain the high-purity rare earth metal Nd foil with the thickness of 0.15mm and the width of 85 mm.
In a second specific embodiment, a process for preparing a high-purity rare earth metal Nd foil with a thickness of 0.10mm includes the following steps:
casting: taking a high-purity rare earth metal Nd with the purity of 99.95 percent as a raw material, adopting a medium-frequency induction smelting furnace, smelting in an argon atmosphere and casting into an ingot;
machining: removing an oxide layer on the surface of the cast ingot by using a machining vehicle until metal luster appears, and cutting the cast ingot into a high-purity Nd cylindrical blank with the diameter of 58 mm;
extrusion and cogging: putting the cylindrical blank into a heating furnace, flushing argon as protective atmosphere, heating and preheating to 600 ℃, keeping the temperature for 0.5h, then putting the cylindrical blank into an extruder for extrusion cogging to obtain a strip blank with the thickness of 3.2mm, and putting the strip blank into an oil bath for cooling;
and (3) vacuum annealing: putting the strip blank into a vacuum annealing furnace, and annealing for 1h at 600 ℃ in a vacuum state;
cold rolling: carrying out 128-pass cold rolling on the strip after vacuum annealing, taking 4 passes as a group, dividing into 32 groups in total, wherein the reduction of each pass in the same group is the same, the reduction of each group is 10 percent, namely the reduction of the first group of 4 passes is kept to be 0.32mm (namely 10 percent of the reduction of the thickness of 3.2 mm), so as to obtain a 2.88mm thin plate, the reduction of the second group is adjusted to be kept to be 0.288mm (namely 10 percent of the reduction of the thickness of 2.88 mm), and the like, and the reduction of the last two groups is 12 percent and 15 percent in sequence; annealing for 0.5h at 480 ℃ in an argon atmosphere once after 4 groups to obtain a crude foil; annealing at 450 ℃ for 1h under the protection of argon after the last group of rolling,
and (3) finishing: and after the rough foil is subjected to vacuum polishing treatment, trimming to obtain the high-purity rare earth metal Nd foil with the thickness of 0.10mm and the width of 85 mm.
In a third specific embodiment, a process for preparing a high-purity rare earth metal Sm foil with a thickness of 0.06mm comprises the following steps:
casting: taking high-purity rare earth metal Sm with the purity of 99.99 percent as a raw material, adopting a suspension smelting furnace, smelting in an argon atmosphere and casting into an ingot;
machining: removing an oxide layer on the surface of the cast ingot by machining until the cast ingot has metallic luster, and cutting the cast ingot into a high-purity Sm cylindrical blank with the diameter of 58 mm;
extrusion and cogging: putting the cylindrical blank into a heating furnace under the protection of argon, heating and preheating to 560 ℃, keeping the temperature for 1h, and then putting the cylindrical blank into an extruder for extrusion cogging to obtain a strip blank with the thickness of 3.0 mm;
and (3) vacuum annealing: putting the strip blank into a vacuum annealing furnace, and annealing for 1h at 520 ℃ in a vacuum state;
cold rolling: carrying out 194-pass cold rolling on the strip after vacuum annealing, wherein the first 50-pass cold rolling is divided into 10 groups by taking each 5-pass cold rolling as a group, the reduction deformation of each group is 8%, then the rest 144-pass cold rolling is divided into 24 groups by taking each 6-pass cold rolling as a group, the reduction deformation of each group is 12%, annealing is carried out for 0.5h at 500 ℃ under argon atmosphere after each 3 groups, and then annealing is carried out for 1h at 400 ℃ under argon atmosphere on the rolled foil to obtain a crude foil;
and (3) finishing: and (4) carrying out vacuum grinding and polishing on the crude foil, and then trimming to finally obtain the high-purity rare earth metal Sm foil with the thickness of 0.06mm and the width of 80 mm.
In a fourth specific embodiment, a process for preparing a high-purity Sm foil of rare earth metal with a thickness of 0.02mm includes the following steps:
casting: taking high-purity rare earth metal Sm with the purity of 99.995 percent as a raw material, adopting a suspension smelting furnace, smelting in an argon atmosphere and casting into an ingot;
machining: removing an oxide layer on the surface of the cast ingot by machining until the cast ingot has metallic luster, and cutting the cast ingot into a high-purity Sm cylindrical blank with the diameter of 58 mm;
extrusion and cogging: putting the cylindrical blank into a heating furnace under the protection of argon, heating and preheating to 560 ℃, keeping the temperature for 1h, and then putting the cylindrical blank into an extruder for extrusion cogging to obtain a strip blank with the thickness of 3.0 mm;
and (3) vacuum annealing: putting the strip blank into a vacuum annealing furnace, and annealing for 1h at 520 ℃ in a vacuum state;
cold rolling: carrying out 246-pass cold rolling on the strip after vacuum annealing, dividing the strip into 41 groups by taking each 6 passes as a group, reducing the deformation amount of the first 12 groups of 72 passes by 10%, then reducing the deformation amount of each remaining group by 12%, annealing the strip for 40min at 500 ℃ in an argon atmosphere after passing through 3 groups, and annealing the rolled foil for 1h at 420 ℃ in the argon atmosphere to obtain a crude foil;
and (3) finishing: and (3) grinding and polishing the crude foil in vacuum, and then trimming to finally obtain the high-purity rare earth metal Sm foil with the thickness of 0.02mm and the width of 50 mm.
The embodiment shows that the high-purity Nd/Sm rare earth metal foil product prepared by the preparation method of the Nd/Sm rare earth metal foil provided by the invention has the advantages of excellent comprehensive mechanical property, high purity, clean appearance and consistent crystal grain size; the preparation method of the Nd/Sm rare earth metal foil is simple in production process, short in period, high in yield, capable of avoiding oxidation and capable of realizing industrial mass production. The Nd/Sm metal foil prepared by the invention is used as a detection sheet for neutron activation detection, and the experimental result is reliable.
The present invention is capable of other embodiments, and various changes and modifications can be made by one skilled in the art without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of Nd/Sm rare earth metal foil is characterized by comprising the following steps:
casting: the method comprises the steps of taking Nd/Sm rare earth metal as a raw material, smelting in an argon atmosphere by adopting a suspension smelting furnace or a medium-frequency induction smelting furnace, and casting into an ingot;
machining: removing an oxide layer on the surface of the cast ingot by machining until the surface of the cast ingot has metallic luster, and then cutting the cast ingot into cylindrical blanks of Nd/Sm rare earth metal;
extrusion and cogging: the method comprises the steps of putting a cylindrical blank into a heating furnace, heating and preheating to 520-650 ℃, preserving heat for 0.5-3 h, and then putting the cylindrical blank into an extruder for extrusion cogging to obtain a band blank of Nd/Sm rare earth metal;
and (3) vacuum annealing: comprises the steps of putting a strip blank into a vacuum annealing furnace, and annealing for 1-2 h at 490-620 ℃ in a vacuum state;
cold rolling: the method comprises the steps of carrying out multi-pass cold rolling on a strip blank subjected to vacuum annealing, taking 4-8 passes as a group, wherein the reduction of each pass in the same group is the same, the reduction deformation of each group is 6-25%, and annealing is carried out for 0.5-1.5 h at 380-550 ℃ in an argon atmosphere after every 2-4 groups; after the last group is finished, annealing for 0.5-1.5 h at 360-500 ℃ in an argon atmosphere; obtaining a metal crude foil;
and (3) finishing: comprises the steps of treating the surface of a metal coarse foil, and cutting to obtain the Nd/Sm rare earth metal foil.
2. The method of claim 1, wherein the purity of the Nd/Sm rare earth metal feedstock is not less than 99.95% during the fusion casting step.
3. The method for preparing Nd/Sm rare earth metal foil according to claim 1, wherein in the machining step, the diameter of the ingot after the surface oxide layer is removed is 55-58 mm.
4. The method of claim 1, wherein the preheating temperature is 560 to 600 ℃ in the step of extrusion cogging.
5. The method for preparing Nd/Sm rare earth metal foil according to claim 1, wherein in the step of extrusion cogging, heat preservation is carried out for 1-2 hours.
6. The method of claim 1, wherein the annealing temperature in the vacuum annealing step is 520 to 580 ℃.
7. The method for preparing Nd/Sm rare earth metal foil according to claim 1, wherein in the step of vacuum annealing, the annealing temperature is 530-560 ℃ and the annealing time is 1.5 h.
8. The method of claim 1, wherein the reduction of each set is 10 to 20% in the cold rolling step.
9. The method for preparing Nd/Sm rare earth metal foil according to claim 1, wherein in the step of cold rolling, annealing is performed once at 430-500 ℃ for 0.5-1.5 hours under argon atmosphere after every 2-4 groups.
10. The production method of an Nd/Sm rare earth metal foil according to any one of claims 1 to 9, characterized in that, in the finishing step, the surface treatment method comprises vacuum polishing.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102126112A (en) * | 2011-03-16 | 2011-07-20 | 中南大学 | Preparation method of electromagnetic shielding multi-layer composite material in electric vacuum device |
| JP2014124659A (en) * | 2012-12-26 | 2014-07-07 | Mitsubishi Alum Co Ltd | Electrolytic capacitor aluminum foil and manufacturing method thereof |
| CN104428435A (en) * | 2012-04-10 | 2015-03-18 | 新日铁住金株式会社 | Steel sheet suitable as impact absorbing member, and method for manufacturing same |
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- 2019-10-17 CN CN201910988449.6A patent/CN111451275A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126112A (en) * | 2011-03-16 | 2011-07-20 | 中南大学 | Preparation method of electromagnetic shielding multi-layer composite material in electric vacuum device |
| CN104428435A (en) * | 2012-04-10 | 2015-03-18 | 新日铁住金株式会社 | Steel sheet suitable as impact absorbing member, and method for manufacturing same |
| JP2014124659A (en) * | 2012-12-26 | 2014-07-07 | Mitsubishi Alum Co Ltd | Electrolytic capacitor aluminum foil and manufacturing method thereof |
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Address after: 108 Longyuan 2nd Road, Longping hi tech park, Furong district, Changsha City, Hunan Province Applicant after: Hunan rare earth metal materials Research Institute Co.,Ltd. Address before: 108 Longyuan 2nd Road, Longping hi tech park, Furong district, Changsha City, Hunan Province Applicant before: HUNAN RARE EARTH METAL MATERIAL Research Institute |