WO2005093865A1 - Revetement anti-adherence pour produire des fils en materiau composite - Google Patents
Revetement anti-adherence pour produire des fils en materiau composite Download PDFInfo
- Publication number
- WO2005093865A1 WO2005093865A1 PCT/DE2005/000470 DE2005000470W WO2005093865A1 WO 2005093865 A1 WO2005093865 A1 WO 2005093865A1 DE 2005000470 W DE2005000470 W DE 2005000470W WO 2005093865 A1 WO2005093865 A1 WO 2005093865A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- release agent
- solvent
- heat treatment
- salt
- coating
- Prior art date
Links
- 239000011248 coating agent Substances 0.000 title claims abstract description 41
- 238000000576 coating method Methods 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000004020 conductor Substances 0.000 title description 21
- 239000002131 composite material Substances 0.000 title description 5
- 230000000181 anti-adherent effect Effects 0.000 title 1
- 239000003911 antiadherent Substances 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 150000003839 salts Chemical class 0.000 claims abstract description 14
- 239000002887 superconductor Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 22
- 239000011265 semifinished product Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 238000004804 winding Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000001680 brushing effect Effects 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 239000011877 solvent mixture Substances 0.000 claims 4
- 238000007654 immersion Methods 0.000 claims 3
- 150000004760 silicates Chemical class 0.000 claims 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims 3
- 230000008020 evaporation Effects 0.000 claims 2
- 238000001704 evaporation Methods 0.000 claims 2
- 238000005507 spraying Methods 0.000 claims 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical class OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 1
- 229910052783 alkali metal Inorganic materials 0.000 claims 1
- 150000001340 alkali metals Chemical class 0.000 claims 1
- -1 alkalis Substances 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 claims 1
- 238000007740 vapor deposition Methods 0.000 claims 1
- 238000007669 thermal treatment Methods 0.000 abstract 2
- 229910017053 inorganic salt Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 6
- 235000011151 potassium sulphates Nutrition 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000011241 protective layer Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000005496 tempering Methods 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000000399 optical microscopy Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 238000009681 x-ray fluorescence measurement Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004870 electrical engineering Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000011214 refractory ceramic Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- 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
- H10N60/0268—Manufacture or treatment of devices comprising copper oxide
- H10N60/0801—Manufacture or treatment of filaments or composite wires
Definitions
- the actual superconducting substance or one which is converted to a superconductor in the course of final heat treatments, is usually combined with another metal, usually not superconducting, e.g. Cu, Ag or other metal alloys, and you get a composite workpiece.
- This composite workpiece is e.g. obtained by the "powder in the tube” technique: the superconductor or the pre-substance (also called precursor) is filled into a metal tube and this is sealed on both sides. If necessary, this is evacuated beforehand.
- the superconductor is produced in one or more final heat treatments (also referred to in the specialist literature as annealing treatment).
- this step includes sintering, an alloy or a phase transition or combinations thereof.
- This heat treatment can be carried out to protect the materials or to influence the phase formation process - under a defined atmosphere or in a vacuum.
- the treatment temperatures to be used here are higher than those of the tempering steps; they can even come close to the melting temperature of the surrounding metals.
- This type of production - first mechanical forming and then one or more heat treatments that require protection against mutual contact of the material - is also used in numerous other areas. Here are a few examples without restricting the process to them: memory metals, thermocouples, powder-insulated wires. As long as the material to be treated is not yet finished, it is also called semi-finished product.
- [D4] provides an overview of the materials commonly used today and the associated manufacturing processes.
- the coating is removed after completion of the heat treatment, as possible mechanical forming steps follow or the end product is required without a coating.
- EP 322619A1 discloses a method according to which a layer of zirconium oxide, aluminum oxide or compounds made of aluminum oxide and other metal oxides ensures the connection between an oxide-ceramic material and a carrier and at the same time prevents chemical reactions and interactions between the substances.
- the coating must adhere well to the wire so that it does not flake off during the heat treatment.
- the removal is therefore very expensive by mechanical brushing or grinding. This is very time-consuming and can even damage or destroy the sensitive materials. In addition, the removal is usually not complete and residues interfere with further processing.
- the reason for the mechanical, disadvantageous removal of the coating is due to the fact that the coating materials used are so chemically and thermally inert that gentle detachment with solvents, acids or bases is not possible.
- the inventive method allows comparably simple application, a good-quality, thin protection during maintenance 'meà and a substantially improved removal of the protective layer. At the same time, the simpler handling makes the process cheaper and the surface quality of the wire better.
- the coating agent or method according to the invention is based on the use of soluble release agents or a combination of soluble and insoluble release agents.
- the solubility of the release agent makes it possible, on the one hand, to produce stable coating solutions without the known and undesirable phenomenon of sedimentation in suspensions, and on the other hand, this solubility enables the coating or the release agent to be simply washed off after the heat treatment without the need for mechanical treatment.
- the coating and separation systems can be adapted to the individual requirements in a wide range.
- the semi-finished product is provided with a protective layer of release agent before a heat treatment.
- a protective layer of release agent before a heat treatment.
- further mechanical treatments e.g. drawing, rolling without being restricted to this
- tempering steps can be carried out.
- the semi-finished product is drawn through a bath with a solution of solvent and salt.
- the semi-finished product is drawn through a bath with a suspension of slurry and separating agent.
- the solution can be applied to one or both sides by means of a meterable (manual or automatic) device for applying liquids and / or suspensions.
- the solvent or carrier liquid is then removed. This can be done by drying at room temperature or in an oven.
- the temperature is chosen so that the semi-finished product or the substances contained therein are not damaged or undergo phase changes.
- the material to be dried can be subjected to targeted temperature gradients in one Continuous furnace or corresponding temperature profiles are exposed in a closed furnace.
- a so-called rewinder is used.
- the semi-finished product is wound from a first spool or carrier onto a second spool or carrier.
- the application to the second coil or carrier can be done tightly or loosely with a distance between the individual turns. For this purpose, it may be necessary to control the winding force and speed precisely.
- a second belt to be run along can also serve as a spacer, which is removed again before further processing.
- the salt solution is applied to the semi-finished product between this first and second coil or carrier. If the solvent is removed in a continuous furnace, there is a continuous furnace after the device for solvent application and before the second coil or carrier, through which the semi-finished product provided with solution is carried out for drying.
- a solution with 12% by weight potassium sulfate (K2S04, 99%; Roth) is prepared in deionized (VE) water.
- the solution is kept constant at a temperature of 30-40 ° C.
- the solution is applied on one side and continuously to an HTS ribbon conductor using a capillary.
- the strip conductor surface is wetted with the solution.
- the order is at a feed rate of 3m / min. Drying takes place in a 3m long drying section at 480 ° C.
- FIG. 1 and FIG. 2 show cross sections of coated strip conductors. 1 and FIG. 2 on the left represent a strip conductor coated according to Example 1, FIG. 2 on the right a strip conductor coated conventionally (according to the prior art) with aluminum oxide suspension. It can clearly be seen that the coating with potassium sulfate according to the example results in a significantly thinner coating, since here the minimum layer thickness does not depend on the size of the dispersed particles.
- the coating is removed by simply rinsing with water solves. The removal takes place in a pass through a water basin with a downstream scraper.
- an inert gas e.g. nitrogen
- FIG. 3 shows X-ray fluorescence measurements (XRF) of the conductor surface with and without coatings / release agents.
- XRF X-ray fluorescence measurements
- Soda water glass (Roth) was used for the coating.
- the solution is applied on one side and continuously to the HTS strip conductor by means of a capillary on the strip conductor surface.
- the application takes place with a feed of 2.5m / min. Drying takes place in a divided, 3 m long drying section at a pre-drying temperature of 120 ° C and a final drying temperature of 500 ° C.
- the coating is removed by ultrasound-assisted rinsing with 1-molar sodium hydroxide solution. The removal takes place in a pass through an ultrasound tank with a downstream scraper.
- the solution is applied on one side and continuously to the HTS strip conductor by means of a capillary on the strip conductor surface.
- the application takes place with a feed of 3m / min. Drying takes place in a divided, 3 m long drying section at a predrying temperature of 200 ° C and a final drying temperature of 500 ° C.
- the coating is removed by ultrasound-assisted rinsing with demineralized water. The removal takes place in a pass through an ultrasound tank with a downstream scraper.
- a soluble component also makes it possible to remove the inherently insoluble particles from the strip conductor to be protected by destroying the cohesion of the separating layer upon contact with the solvent.
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
La présente invention concerne un procédé pour produire des supraconducteurs présentant un revêtement intégral ou partiel, au moins temporaire avec un sel organique ou minéral. L'invention se caractérise en ce que ledit sel est appliqué avant de subir au moins un traitement thermique, les résidus de solvants qu'il contient, sont éliminés, puis le sel est à nouveau éliminé après un ou plusieurs traitements thermiques et/ou autres étapes de production. L'invention a également pour objet un dispositif pour mettre en oeuvre le procédé.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE112005001268T DE112005001268A5 (de) | 2004-03-23 | 2005-03-16 | Antihaftbeschichtung für die Herstellung von Kompositwerkstoff-Drähten |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102004014596.2 | 2004-03-23 | ||
| DE102004014596A DE102004014596A1 (de) | 2004-03-23 | 2004-03-23 | Antihaftbeschichtung für die Herstellung von Kompositwerkstoff-Drähten |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2005093865A1 true WO2005093865A1 (fr) | 2005-10-06 |
Family
ID=34965622
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/DE2005/000470 WO2005093865A1 (fr) | 2004-03-23 | 2005-03-16 | Revetement anti-adherence pour produire des fils en materiau composite |
Country Status (2)
| Country | Link |
|---|---|
| DE (2) | DE102004014596A1 (fr) |
| WO (1) | WO2005093865A1 (fr) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009028174A1 (de) | 2009-07-31 | 2011-02-03 | Bruker Hts Gmbh | Zinkoxid als Trennmittel bei der Wärmebehandlung von HTSL-Drähten, insbesondere bandförmigen HTSL-Drähten |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19815096A1 (de) * | 1998-04-03 | 1999-10-14 | Siemens Ag | Im Herstellungsprozeß von Hochtemperatur-supraleitenden Bandleitern anzuwendendes Beschichtungsverfahren |
| US6365554B1 (en) * | 1994-04-29 | 2002-04-02 | American Superconductor Corporation | Separating layer for heat treating superconducting wire |
| WO2003023872A1 (fr) * | 2001-09-10 | 2003-03-20 | Industrial Research Limited | Agents de demoulage pour bandes et fils supraconducteurs haute temperature a revetement metallique |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD286189B5 (de) * | 1989-07-18 | 1994-03-03 | Bergmann Borsig Gmbh | Schutzmittel fuer bohrungen oder ausarbeitungen gegen verzunderung bei der waermebehandlung von bauteilen |
| DE4409691A1 (de) * | 1994-03-22 | 1995-09-28 | Ebg Elektromagnet Werkstoffe | Verfahren zur Herstellung von Elektroblechen mit einem Glasüberzug |
-
2004
- 2004-03-23 DE DE102004014596A patent/DE102004014596A1/de not_active Ceased
-
2005
- 2005-03-16 WO PCT/DE2005/000470 patent/WO2005093865A1/fr active Application Filing
- 2005-03-16 DE DE112005001268T patent/DE112005001268A5/de not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6365554B1 (en) * | 1994-04-29 | 2002-04-02 | American Superconductor Corporation | Separating layer for heat treating superconducting wire |
| DE19815096A1 (de) * | 1998-04-03 | 1999-10-14 | Siemens Ag | Im Herstellungsprozeß von Hochtemperatur-supraleitenden Bandleitern anzuwendendes Beschichtungsverfahren |
| WO2003023872A1 (fr) * | 2001-09-10 | 2003-03-20 | Industrial Research Limited | Agents de demoulage pour bandes et fils supraconducteurs haute temperature a revetement metallique |
Also Published As
| Publication number | Publication date |
|---|---|
| DE102004014596A1 (de) | 2005-10-27 |
| DE112005001268A5 (de) | 2007-05-31 |
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