CA2445104A1 - Method for the preparation of highly densified superconductor massive bodies of mgb2, relevant solid end-products and their use - Google Patents

Method for the preparation of highly densified superconductor massive bodies of mgb2, relevant solid end-products and their use Download PDF

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CA2445104A1
CA2445104A1 CA002445104A CA2445104A CA2445104A1 CA 2445104 A1 CA2445104 A1 CA 2445104A1 CA 002445104 A CA002445104 A CA 002445104A CA 2445104 A CA2445104 A CA 2445104A CA 2445104 A1 CA2445104 A1 CA 2445104A1
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boron
magnesium
powders
preform
crystalline boron
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CA2445104C (en
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Giovanni Giunchi
Sergio Ceresara
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Edison SpA
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00—Superconducting devices
    • H10N60/01—Manufacture or treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
    • C04B35/58057—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on magnesium boride, e.g. MgB2
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/653—Processes involving a melting step
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00—Superconducting devices
    • H10N60/01—Manufacture or treatment
    • H10N60/0856—Manufacture or treatment of devices comprising metal borides, e.g. MgB2
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/401—Alkaline earth metals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/421—Boron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5292—Flakes, platelets or plates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase

Abstract

A method is described for the preparation of superconductor massive bodies of MgB2, having a density close to the theorical value, which comprises the following passages: mechanical activation of crystalline boron with the formation of activated powders; formation of a porous preform of said powders;
assembly of the porous boron preform and massive precursors of metallic magnesium in a container and sealing thereof in an atmosphere of inert gas or with a low oxygen content; thermal treatment of the boron and magnesium as assembled above, at a temperature higher than 700 ~C for a time greater than 30 minutes, with the consequent percolation of the magnesium, in liquid phase, through the activated crystalline boron powders.

Claims (25)

1. A method for the preparation of superconductor mas-sine bodies of MgB2, having a density close to the theo-retical value, which comprises the following steps:

a) mechanical activation of crystalline boron with the formation of activated powders;

b) formation of a porous preform of activated powders of crystalline boron;

c) assembly of the porous boron preform and massive pre-cursors of metallic magnesium in a container and seal-ing thereof in an atmosphere of inert gas or with a low oxygen content;

d) thermal treatment of the boron and magnesium as assem-bled above, at a temperature higher than 700°C for a time greater than 30 minutes, with the consequent per-colation of the magnesium, in liquid phase, through the activated crystalline boron powders.
2. The method according to claim 1, characterized in that the mechanical activation passage a) of crystalline boron consists in grinding flakes of crystalline boron by repeated crushing effected by high load compression.
3. The method according to claim 1, characterized in that the activated crystalline boron powders have an av-erage volumetric particle diameter ranging from 30 to 70 micrometres and have a type of crystallinity equal to that of the starting crystalline boron flakes.
4. The method according to claim 1, characterized in that the preform of activated crystalline boron powders is prepared with the usual powder compacting techniques.
5. The method according to claim 1, characterized in that the preform of activated crystalline boron powders is prepared in the container itself by directly pouring the activated crystalline boron powder inside and com-pacting it.
6. The method according to claim 1, characterized in that the preform of activated crystalline boron powders has an apparent density higher than 50% of the theoreti-cal density of the crystalline boron (2.35 g/cm3).
7. The method according to claim 1, characterized in that the preform of activated crystalline boron powders has a purity higher than or equal to 99.4%.
8. The method according to claim 1, characterized in that the preform of activated crystalline boron powders has a shape similar to that of the end-product.
9. The method according to claim 1, characterized in that the preform of activated crystalline boron powders contains up to 20% atomic of magnesium in the form of magnesium powder having a particle-size lower than that of boron.
10. The method according to claim 1, characterized in that the preform of activated crystalline boron powders consists of activated crystalline boron powders, surface-coated by metallic magnesium.
11. The method according to claim 1, characterized in that the combining step c) of the porous boron preform and massive precursors of metallic magnesium in a con-tamer is effected with massive precursors of metallic magnesium having a purity higher than 99%.
12. The method according to claim 1, characterized in that in step c) there is an excess of Mg which is such that the atomic ratio Mg/B is greater than 0.5.
13. The method according to claim 1, characterized in that the atomic ratio Mg/B is higher than or equal to 0.55.
14. The method according to claim 1, characterized in that the container used in step c) consists of a material which cannot be attacked by the boron and magnesium at temperatures up to 1000°C.
15. The method according to claim 14, characterized in that the material is Nb, Ta, MgO, BN.
16. The method according to claim 1, characterized in that the container used in step c) consists of any mate-rial resistant to high temperatures, internally lined by a sheath of a material which cannot be attacked by the boron and magnesium at temperatures up to 1000°C.
17. The method according to claim 1, characterized in that step d) comprises thermal treatment at temperatures ranging from 800° to 1000°C, for 1-3 hours.
18. The method according to claim 1, characterized in that the percolation in step d) is effected by infiltra-tion of a porous preform of activated crystalline boron powder, immersed in molten metal maintained under a pres-sure of inert gas.
19. The method according to claim 1, characterized in that in step c) the massive precursors of metallic Mg consist of massive bodies of magnesium and one or more lower-melting metals or equivalent alloys.
20. The method according to claim 19, characterized in that the lower-melting metals are present in such a quan-tity as to reach as far as possible the percentage corre-sponding to the eutectic point of the equivalent alloy.
21. The method according to claim 19, characterized in that the atomic ratio low-melting metal + magnesium/boron is greater than 0.55 and contemporaneously the atomic ra-do magnesium/boron is greater than 0.5.
22. The method according to claim 19, characterized in that the lower-melting metals are selected from Ga, Sn, In and Zn.
23. A superconductor massive body or solid end-product of MgB2, having a density close to the theoretical value, obtained by the method according to any of claims 1 to 22.
24. Use of the superconductor massive body or solid end-product of MgB2, according to claim 23, as a target for vacuum deposition technologies of thin films, such as la-ser ablation and radio-frequency sputtering.
25. Use of the superconductor massive body or solid end-product of MgB2, according to claim 23, as electric cur-rent cut-ins, variable induction elements in current limitation systems, permanent magnets to be used in levi-tation systems, for medical magnetic resonance systems, for elementary particle accelerators and detectors, for energy accumulation systems, for linear or non-linear mo-tors, for power generators.
CA2445104A 2001-05-11 2002-05-10 Method for the preparation of highly densified superconductor massive bodies of mgb2, relevant solid end-products and their use Expired - Fee Related CA2445104C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
ITMI2001A000978 2001-05-11
IT2001MI000978A ITMI20010978A1 (en) 2001-05-11 2001-05-11 METHOD FOR PREPARATION OF MGB2 SUPERCONDUCTIVE MASSIVE BODIES HIGHLY DENSIFIED RELATIVE SOLID MANUFACTURES AND THEIR USE
PCT/IB2002/001594 WO2002093659A2 (en) 2001-05-11 2002-05-10 Method for the preparation of higly densified superconductor massive bodies of mgb2

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CA2445104A1 true CA2445104A1 (en) 2002-11-21
CA2445104C CA2445104C (en) 2011-06-21

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US (1) US7396506B2 (en)
EP (1) EP1390992B1 (en)
JP (1) JP4431313B2 (en)
KR (1) KR100904321B1 (en)
CN (1) CN100452467C (en)
AT (1) ATE335287T1 (en)
AU (1) AU2002258044B2 (en)
CA (1) CA2445104C (en)
DE (1) DE60213588T2 (en)
ES (1) ES2269685T3 (en)
HK (1) HK1069012A1 (en)
IL (2) IL158460A0 (en)
IT (1) ITMI20010978A1 (en)
RU (1) RU2264366C2 (en)
WO (1) WO2002093659A2 (en)

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JP2006127898A (en) * 2004-10-28 2006-05-18 Sumitomo Electric Ind Ltd Sintered body, manufacturing method of sintered body, superconductive wire rod, superconductive apparatus, and manufacturing method of superconductive wire rod
DE102006017435B4 (en) * 2006-04-07 2008-04-17 Leibniz-Institut Für Festkörper- Und Werkstoffforschung Dresden E.V. Powder for the preparation of MgB2 superconductors and process for the preparation of these powders
JP2011518409A (en) * 2008-03-30 2011-06-23 ヒルズ， インコーポレイテッド Superconducting wire and cable and manufacturing method thereof
US8812069B2 (en) * 2009-01-29 2014-08-19 Hyper Tech Research, Inc Low loss joint for superconducting wire
KR101044890B1 (en) * 2009-02-18 2011-06-28 한국원자력연구원 FABRICATION METHOD OF MgB2 SUPERCONDUCTING WIRE
DE102009010112B3 (en) 2009-02-21 2010-09-02 Bruker Eas Gmbh A method for superconducting bonding of MgB 2 superconducting wires over a MgB 2 matrix of a Mg-infiltrated boron powder compact
IT1398934B1 (en) * 2009-06-18 2013-03-28 Edison Spa SUPERCONDUCTIVE ELEMENT AND RELATIVE PREPARATION PROCEDURE
JP2013229237A (en) * 2012-04-26 2013-11-07 Univ Of Tokyo Superconduction wire material, precursor of superconduction wire material, method of manufacturing the same, and precursor of superconduction multi-core conductor
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IL158460A (en) 2011-02-28
JP2005508278A (en) 2005-03-31
RU2003130954A (en) 2005-04-10
ATE335287T1 (en) 2006-08-15
CN100452467C (en) 2009-01-14
EP1390992A2 (en) 2004-02-25
IL158460A0 (en) 2004-05-12
DE60213588T2 (en) 2007-08-02
ITMI20010978A0 (en) 2001-05-11
JP4431313B2 (en) 2010-03-10
KR20030092102A (en) 2003-12-03
RU2264366C2 (en) 2005-11-20
US20040124086A1 (en) 2004-07-01
ES2269685T3 (en) 2007-04-01
CN1537335A (en) 2004-10-13
US7396506B2 (en) 2008-07-08
CA2445104C (en) 2011-06-21
WO2002093659A2 (en) 2002-11-21
KR100904321B1 (en) 2009-06-23
ITMI20010978A1 (en) 2002-11-11
AU2002258044B2 (en) 2007-03-15
DE60213588D1 (en) 2006-09-14
HK1069012A1 (en) 2005-05-06
EP1390992B1 (en) 2006-08-02
WO2002093659A3 (en) 2003-10-16

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