WO1988008619A1 - Procede et equipement pour produire des materiaux supraconducteurs de haute qualite, et materiaux supraconducteurs ainsi obtenus - Google Patents

Procede et equipement pour produire des materiaux supraconducteurs de haute qualite, et materiaux supraconducteurs ainsi obtenus Download PDF

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Publication number
WO1988008619A1
WO1988008619A1 PCT/HU1988/000028 HU8800028W WO8808619A1 WO 1988008619 A1 WO1988008619 A1 WO 1988008619A1 HU 8800028 W HU8800028 W HU 8800028W WO 8808619 A1 WO8808619 A1 WO 8808619A1
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Prior art keywords
magnetic field
superconducting
ceramic material
magnetic
temperature
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Application number
PCT/HU1988/000028
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English (en)
Inventor
István PÓCSIK
Original Assignee
Magyar Tudományos Akadémia Központi Fizikai Kutató
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Publication of WO1988008619A1 publication Critical patent/WO1988008619A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00—Magnetic separation
    • B03C1/02—Magnetic separation acting directly on the substance being separated
    • B03C1/021—Separation using Meissner effect, i.e. deflection of superconductive particles in a magnetic field
    • 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

Definitions

  • the subject matter of the present application is a process and equipment for producing high quality super ⁇ conducting materials by means of magnetic field separating applied if necessary at variable temperature. It refers also to a material of improved superconductivity parameters.
  • PRIOR ART As it is well known, Bednorz and M ⁇ ller (Z. f ⁇ r
  • Oxide- -ceramics are produced by high temperature solid state reactions whereon liquid phase components and liquid phase reactions may take important part.
  • the known methods of production exclude that the received material is a homogeneous product.
  • the solid state reaction results in a heap of grains, whose various parameters show a wide distribution; some starting materials might even remain unchanged, particularly those within some of the larger grains. Some of these grains might not show superconductivity at any temperature.
  • the transition temperature from the normal to the superconducting state of these grains shows a wide range distribution. The measured wide temperature range of the transition, which covers sometimes some ten degrees, proves this statement.
  • the sample will be qualified to be super ⁇ conducting, whatever the size of the sample.
  • the conductivity measurement is.not sensitive to the extent of the inhomogeneities. It was experienced also that on decreasing the temperature in some samples the initial fast decrease of the resistivity slowed down, and the whole sample didn't reach the zero resistance state. In this case the existing superconducting domains are simply not connected with each other; hence, the material of the rest of the sample can not be in superconducting state. Inhomogeneity is a typical characteristic feature of these ceramic materials. Apart from the critical temperature, the super ⁇ conducting state is characterized by the critical magnetic field.
  • the sufficiently large magnetic field cancels the superconducting state so the phase transition of the materials into a normal conducting state occurs even when the temperature is below the value beleived to be critical for the normal superconductivity.
  • the critical magnetic field limits the possible magnetic field of superconducting magnets.
  • the critical current can be defined as well which current - for a given geometrical configuration - generates the critical magnetic field at the surface of the conductor.
  • the critical magnetic field values of the known oxide- -ceramics superconductors are extremely large but the critical current values are very low. These data show the strong inhomogeneity of the conductivity of these samples.
  • the object of the present patent application is to provide a modified technology of the production and improved equipment for increasing the required parameter values, i.e. the critical temperature, critical magnetic field and critical current.
  • the object is also to provide a superconducting material of improved quality.
  • the basis of the invention is the recognition that the extent of the inhomogeneity characterizing a super ⁇ conducting material can be considerably lowered when the superconducting and the normal grains ; ⁇ re separated from the reaction products by a magnetic fi: : ld separation technique applying variable temperature, if necessary.
  • the process according to this application gives a further development of the generally known magnetic separa ⁇ tion used in ore-enriching and waste-recycling plants to separate the ferromagnetic components of the material to be treated.
  • the development includes two aspects: on the one hand the application of this technique has been expanded to the separation of strongly diamagnetic materials; on the other hand the separation is performed at low, and, if necessary, at variable temperatures.
  • a green body comprising components showing superconductivity in a defined temperature range, further called superconducting components is produced by the known methods of making superconductive oxide-ceramic materials.-a ⁇ this green body is su&jected to a treatment for improving the superconductivity characteristics thereof.
  • the green body is affected by a high gradient magnetic field for separating the strongly diamagnetic components thereof and enriching it by the superconducting components after ensuring a temperature range wherein the superconducting state of the appropriate components can be expected.
  • the temperature is generally stable, however, it can be changed.
  • the fact is important that the materials in superconducting state show diamagnetic features, i.e. they can not be penetrated by the magnetic field.
  • the green body can be, of course, subjected to heat treatment before applying the magnetic field.
  • the green body to be treated by the magnetic field should preferably be in relative movement to the magnetic field.
  • the separation effect can be improved also by vibrating the green body.
  • the temperature of the green body lies in the range of the superconductivity of the appropriate components and it is stable, however, It can be variable and adjustable, too.
  • By applying more temperature ranges of separating it is possible to collect grains of different superconductivity features. It is expedient that when the green body is transported across the separating magnetic field by a conveyor belt, across the tilted edge of the- conveyor belt the magnetic field make the superconducting grains pick out against gravitation. These grains are collected by the outside edge of the conveyor belt. It is expedient as well, when a mobile magnetic field zone moves along the standing sample, that the super ⁇ conducting grains are concentrated in front of the zone. It is preferred also to apply, together with the space gradient of the magnetic field a gradient in time is used. A pulsing magnetic field carries out the separation very effectively, especially when the pulses of the magnetic field have a saw-tooth shape.
  • each separator is placed one after the other.
  • the first separator is adjusted to the highest critical temperature and this is followed by others for which the temperature is decreased stepwise.
  • These separators extract from the green body the grains which turned out to be superconducting in the given temperature interval.
  • the reverse arrangement with increasing temperature degrees, may be applied, too.
  • FIG. 1 shows the general operational principle of the proposed equipment and the realization thereof in general when means for generating magnetic field are located inside a space with variably adjustable temperature range
  • Fig. 2 is a realization of the proposed equipment in general when means for generating magnetic field are located outside a space variably adjustable temperature range
  • Fig. 3 is the schematic view of an equipment making use of the gravitational forces
  • Fig. 4 shows the schematic arrangement of moving means for generating magnetic field in space relation to a green body
  • Fig. 5 shows schematically the embodiment of the proposed equipment working with a tilted edge conveyor belt
  • Fig. 6 shows the schematic view of the proposed equipment in an embodiment working with generating magnetic pulse
  • Fig. 7 shows a series of saw-tooth shape pulses produced by the means for generating magnetic field.
  • the method proposed by the invention is based on the fact that a green body comprising superconducting components includes much filler which can not be super ⁇ conductive at all. Because of the diamagnetic character of the superconductors the green body subjected to a magnetic field can be divided into a part enriched in superconducting components and another part with poor content of such components.
  • the green body produced generally by means of solid-
  • this powdered material should be cooled down to the temperature range wherein at least one of the components is superconductive.
  • This range can be determined by the well known physical methods of stating superconductivity. Because the known superconducting materials show critical temperature lying below 100 K, presently the process of the invention requires ' - a closed space wherein the mentioned low temperature can be held without too big power losses. Of course, if the temperature range of the superconductivity will be higher, the range applied for the separation can be also higher.
  • the green body cooled down to the required temperature range of the superconductivity of its components is subjected in the next step to the influence of a magnetic field preferab- ly characterized by high gradient.
  • This field does not act to the normal component of the green body but makes the diamagnetic component, i.e. the superconductive material separate from the green body, decline from a direction of movement of the green body, if any.
  • the separation of the superconducting components might accomplished with a standing green body, but it is preferred to arrange a relative movement of the means for generating the required magnetic field and of the green body particles. This can be made by one of the following steps: (1) the green body is translated, e.g.
  • the means for generating magnetic field are translated along a path wherein the green body is arranged, and (3) the particles of the green body are forced to fall down ⁇ in a s ⁇ ace wherein the magnetic field of the separation is generated.
  • the separation can be carried out also in more steps, wherein two or more means for generating magnetic field are arranged along the path of movement of the green body and the magnetic fields are assigned to different or equal temperature ranges.
  • magnetron type equipment being the means for generating magnetic field when the wave-form magnetic field is applied for realizing the effect of transporting the supraconducting particles.
  • the super ⁇ conducting particles with regard to their complete diamagnetic susceptibility are pushed in the magnetic field from the higher magnetic intensity space parts to those characterised by lower magnetic intensity. These particles are ideal diamagnets.
  • the superconducting materials proposed by the inven- tion are those obtained by realising the method of the invention, e.g. by means of the equipment shown in the accompanying drawing.
  • the transition width measured from 10 % to 90 % of the full diamagnetic transition is substantially as high as 3 K or is lower, which is very advantageous when compared with the YBA.-.Cu- j O-, oxide-ceramics characterized by transition width 29 K (zur Loye, H. C. et al, Science, 1987, 238, p. 1558 to 1560) or over 10 K observed in the lanthanum based oxide-ceramic systems.
  • the principal arrangement of the equipment according to the invention includes a container 1 being preferably thermally insulated and including controlled means for adjusting and maintaining the internal temperature, regulating means 2 connected by output means B and input means A to the container, a separator unit 3 and means 6 for generating magnetic field, especially an electro ⁇ magnet, the input means A can be applied for forwarding temperature values and other measured data to the regulating means and the output means B serve to forwarding the signals necessary for carrying out the control functions.
  • the means 6 for generating magnetic field are arranged in a space relationship to the separator unit 3 in order to ensure a path 9 whereby the su h 3rconducting particels can be conveyed.
  • This can be done in more ways.
  • a convex pole 4 and a concave pole 5 are arranged in two sides of a path of a green body 7 containing the gi ainy and/or fine powdered material which includes the superconducting particles or superconducting material embedded in the particles.
  • the green body 7 of the powdered, grainy material to be separated is conveyed through the internal space of the container 1 and therein between the convex pole 4 and the concave pole 5 of the means 6.
  • the means 6 generate thereby magnetic field which can be characterized by high space gradient: the intensity of the magnetic field decreases from the convex pole 4 to the concave pole 5.
  • the effect of this magnetic field is that the normal state grains, particles continue their movement unaffected by this field and the superconducting particles or particles containing superconductive parts are strongly repulsed, they deviate strongly from a path 8 of the normal grains, and can be separated therefrom on the path 9.
  • FIG. 1 Another possibility - not shown*in the drawings - is to provide means 6 for generating the magnetic field in form of a tube having a longitudinal, coaxial slot in the mantle wherein the two sides of the slot form the poles 4 and 5. They can be not equally shaped.
  • the magnetic field is generated in this case by wieres forming a longitudinal coil element on the tube mantle.
  • the tube is arranged slightly sloping: the grains to be separated are fed to the upper end of the tube and the superconducting particle are maintained by the wave-trough and led parallel to the mantle in direction of the lower end. the ⁇ on superconductive particles fall down in the internal space of the tube and slide there downwards. At the lower end of the tube the two fractions can be collected separately.
  • Fig. 2 shows another possible realization of the equipment according to the invention which equipment consists of a thermally insulated container 1 with adjustable inside temperature (as shown in Fig. 1 and described in connection with it), regulator means 2, and a separator unit 3.
  • the - difference to the arrangement of Fig. 1 is that the convex pole 4 and the concave pole 5 of the means 6 for generating the magnetic field with perpendicular gradient are located outside the thermally isolated container.
  • Fig. 3 shows the working principle of the separator making use of the gravitational forces.
  • the thermally insulated container and the regulator are not shown here and on the following Figures. Of course, these units are indispensable parts of every embodiment of the equipment but for the sake of simplicity they are not shown them here.
  • the particles of the material 7 to be separated falls from a dispenser 10, e.g. from an end of a belt conveyor or of a glass tube through the high gradient magnetic field generated e.g. by the convex pole 4 and the concave pole 5 of a magnet.
  • the path 8 of the materials in the normal state remains unaffected and these materials reach a container 11 for the normal material.
  • the path 9 of materials in the superconducting state deviates strongly from the other path 8 and the material falls into a container 12 for the superconducting material.
  • Fig. 4 shows an example of the realization of the proposed equipment working with the magnetic field zone method.
  • the material 7 to be separated is arranged in a further container 15 and the magnetic field generated by poles 13 and 14 of a magnet moves along the container 15, the magnetic field generated showing high gradient parallel to the direction of the movement.
  • Fig. 5 presents an example of the realization of the proposed equipment where an edge of a conveyor belt 20 is tilted.
  • the conveyor belt 20 carries the material to -be separated across the magnetic field generated by the poles 4 and 5.
  • the path 8 of the materials in the normal state remains unaffected on the way across the magnetic field
  • the path 9 of the superconducting materials deviates ⁇ ⁇ rom the former: the superconducting grains are drifted against the gravitational field up to the tilted edge of the conveyor belt 20 and these grains fall into the container 12 for the superconducting materials.
  • the particles taken away by the superconducting grains and being not super- conductive slide back to the path 8 on the tilted surface . of the conveyor belt 20.
  • Fig. 6 shows an example of the ralization of the proposed equipment using both spatial and temporal gradients and regulated pulses.
  • the conveyor belt 20 carries the material to be separated into the magnetic field generated by a gradient coils having turns 16 of small and turns 17 of large diameter connected to a current generator 18 for current supply.
  • the magnetic field is generated in form of pulses ensuring high spatial gradient and fast changes.
  • the path 8 of the normal material remains unaffected on the way across the magnetic field, these particles do not leave the conveyor belt 20.
  • the path.9 of the material in the superconducting state deviates strongly whereby the required material in this state is drifted from the conveyor belt 20 along the path 9 into the container 12.
  • Fig. 7 present an optimal shape of magnetic field pulses 19.
  • the linear increase of the pulse profile means a constant gradient for the time of increase.
  • the fast recovery means that only a short time elapses before the whole cycle starts again.
  • the coil should have an air or ferrite core.

Abstract

Dans un procédé de production de matériaux supraconducteurs de haute qualité, le matériau céramique du type oxyde préparé et ayant des constituants supraconducteurs est réglé à une température située dans la plage de la supraconductivité d'au moins un de ces constituants supraconducteurs et est soumis à un champ magnétique non homogène déterminant une trajectoire magnétique de transport du constituant supraconducteur. L'équipement qui comprend des moyens permettant de recevoir un matériau céramique comportant au moins un constituant supraconducteur et des moyens permettant d'effectuer un traitement du matériau céramique, est caractérisé en ce qu'il possède une unité (2) de réglage de la température dans la plage de supraconductivité du matériau céramique et en ce que le traitement est effectué par des moyens (6) permettant de produire un champ magnétique présentant un gradiant spatial élevé destiné à assurer une trajectoire magnétique aux particules du matériau céramique supraconducteur. Est également décrit un matériau supraconducteur à base de céramique oxydée et caractérisé en ce que la largeur de transition mesurée de 10 % à 90 % de la transition diamagnétique totale est pratiquement au plus de 3 K.
PCT/HU1988/000028 1987-04-27 1988-04-27 Procede et equipement pour produire des materiaux supraconducteurs de haute qualite, et materiaux supraconducteurs ainsi obtenus WO1988008619A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
HU1835/87 1987-04-27
HU871835A HUT47761A (en) 1987-04-27 1987-04-27 Method and apparatus for improving the quality of superconducting substances with the method of variable temperature magnetic separation

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WO1988008619A1 true WO1988008619A1 (fr) 1988-11-03

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HU (1) HUT47761A (fr)
WO (1) WO1988008619A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0317643A1 (fr) * 1987-06-09 1989-05-31 Mitsubishi Denki Kabushiki Kaisha Procede de production d'un supraconducteur a base d'oxyde
EP0320083A2 (fr) * 1987-12-09 1989-06-14 Canon Kabushiki Kaisha Appareil de purification pour des particules fines supraconductrices
US5182253A (en) * 1987-12-09 1993-01-26 Canon Kabushiki Kaisha Purification apparatus for superconductor fine particles
US6318558B1 (en) * 1998-02-09 2001-11-20 Hubertus Exner Method and device for separating different electrically conductive particles

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU600345B2 (en) * 1987-03-23 1990-08-09 Semiconductor Energy Laboratory Co. Ltd. Method of manufacturing superconducting ceramics under a magnetic field

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US4171464A (en) * 1977-06-27 1979-10-16 The United State of America as represented by the U. S. Department of Energy High specific heat superconducting composite
WO1988000149A1 (fr) * 1982-09-30 1988-01-14 Gallatin Norman W Attelage de remorque asymetrique a quatre barres

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US4171464A (en) * 1977-06-27 1979-10-16 The United State of America as represented by the U. S. Department of Energy High specific heat superconducting composite
WO1988000149A1 (fr) * 1982-09-30 1988-01-14 Gallatin Norman W Attelage de remorque asymetrique a quatre barres

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NATURE, Vol. 326, No. 6114, issued 1987, 16 April (New York), HOR et al., "Switching Phenomena in a New 90-K Superconductor", see pages 669, 670. *
PHYSICAL REVIEW B, Condensed Matter, Vol. 35, No. 16, 01 June 1987 (01.06.87), FARREL et al., "Weak-field magnetization of superconductinf Y1Ba2Cu3Ox: Relationship to microstructure", see pages 8797-8799. *
PHYSICAL REVIEW B, Condensed Matter, Vol. 36, No. 1, 01 July 1987 (01.07.87), YESHURUN et al., "Magnetic properties of a high-Tc superconductor 4Ba2Cu3O7: Reentrylike features, paramagnetism and glassy behaviour", see pages 840-842. *
SCIENTIFIC INSTRUMENTS, Vol. 20, No. 10, October 1987, VIEIRA et al., "A Simple Device for quick separation of high-Tc superconducting materials", see pages 1292-1293. *
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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0317643A4 (fr) * 1987-06-09 1990-06-05 Mitsubishi Electric Corp Procede de production d'un supraconducteur a base d'oxyde.
EP0317643A1 (fr) * 1987-06-09 1989-05-31 Mitsubishi Denki Kabushiki Kaisha Procede de production d'un supraconducteur a base d'oxyde
US5268353A (en) * 1987-06-09 1993-12-07 Mitsubishi Denki Kabushiki Kaisha Method for separating superconductor powder from nonsuperconductive powder
EP0588451A2 (fr) * 1987-12-09 1994-03-23 Canon Kabushiki Kaisha Appareil de purification pour des particules fines supraconductrices
US5182253A (en) * 1987-12-09 1993-01-26 Canon Kabushiki Kaisha Purification apparatus for superconductor fine particles
EP0320083A3 (en) * 1987-12-09 1990-05-16 Canon Kabushiki Kaisha Purification apparatus for superconductor fine particles
EP0320083A2 (fr) * 1987-12-09 1989-06-14 Canon Kabushiki Kaisha Appareil de purification pour des particules fines supraconductrices
EP0588450A2 (fr) * 1987-12-09 1994-03-23 Canon Kabushiki Kaisha Appareil de purification pour des particules fines super conductrices
EP0588452A2 (fr) * 1987-12-09 1994-03-23 Canon Kabushiki Kaisha Appareil de purification pour des particules fines supraconductrices
EP0588451A3 (en) * 1987-12-09 1994-05-18 Canon Kk Purification apparatus for superconductor fine particles
EP0588450A3 (en) * 1987-12-09 1994-05-18 Canon Kk Purification apparatus for superconductor fine particles
EP0588452B1 (fr) * 1987-12-09 1997-10-01 Canon Kabushiki Kaisha Appareil et procédé de purification pour des particules fines supraconductrices
US6318558B1 (en) * 1998-02-09 2001-11-20 Hubertus Exner Method and device for separating different electrically conductive particles

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AU1703688A (en) 1988-12-02
HUT47761A (en) 1989-03-28

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