EP0997918A1 - Herstellung einer Magnetschicht - Google Patents
Herstellung einer Magnetschicht Download PDFInfo
- Publication number
- EP0997918A1 EP0997918A1 EP99201371A EP99201371A EP0997918A1 EP 0997918 A1 EP0997918 A1 EP 0997918A1 EP 99201371 A EP99201371 A EP 99201371A EP 99201371 A EP99201371 A EP 99201371A EP 0997918 A1 EP0997918 A1 EP 0997918A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- support
- ions
- magnetic layer
- soft magnetic
- process according
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 7
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002923 metal particle Substances 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 25
- -1 nickel(II) ions Chemical class 0.000 claims description 20
- 229910052759 nickel Inorganic materials 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000000696 magnetic material Substances 0.000 claims description 7
- 238000011026 diafiltration Methods 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 229940005740 hexametaphosphate Drugs 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 238000000108 ultra-filtration Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 241000478345 Afer Species 0.000 claims 1
- 229910001429 cobalt ion Inorganic materials 0.000 claims 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 239000012736 aqueous medium Substances 0.000 abstract description 8
- 238000006722 reduction reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
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- 150000003839 salts Chemical class 0.000 description 5
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 4
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- 239000003795 chemical substances by application Substances 0.000 description 3
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- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
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- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 2
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 125000005907 alkyl ester group Chemical group 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
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- 230000001419 dependent effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- DEFVIWRASFVYLL-UHFFFAOYSA-N ethylene glycol bis(2-aminoethyl)tetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)CCOCCOCCN(CC(O)=O)CC(O)=O DEFVIWRASFVYLL-UHFFFAOYSA-N 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
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- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910000697 metglas Inorganic materials 0.000 description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229960003330 pentetic acid Drugs 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 229920006267 polyester film Polymers 0.000 description 2
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- 239000012266 salt solution Substances 0.000 description 2
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- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 2
- 235000011046 triammonium citrate Nutrition 0.000 description 2
- 239000001393 triammonium citrate Substances 0.000 description 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical class OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 description 1
- FCKYPQBAHLOOJQ-NXEZZACHSA-N 2-[[(1r,2r)-2-[bis(carboxymethyl)amino]cyclohexyl]-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)[C@@H]1CCCC[C@H]1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-NXEZZACHSA-N 0.000 description 1
- 241000238366 Cephalopoda Species 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical group [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- FCKYPQBAHLOOJQ-UHFFFAOYSA-N Cyclohexane-1,2-diaminetetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)C1CCCCC1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical class [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000007754 air knife coating Methods 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 125000002877 alkyl aryl group Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 125000004103 aminoalkyl group Chemical group 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
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- 239000000460 chlorine Substances 0.000 description 1
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- 150000001868 cobalt Chemical class 0.000 description 1
- 238000001246 colloidal dispersion Methods 0.000 description 1
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- 125000004185 ester group Chemical group 0.000 description 1
- OUDSFQBUEBFSPS-UHFFFAOYSA-N ethylenediaminetriacetic acid Chemical compound OC(=O)CNCCN(CC(O)=O)CC(O)=O OUDSFQBUEBFSPS-UHFFFAOYSA-N 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
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- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
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- 125000000623 heterocyclic group Chemical group 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
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- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- SYXUBXTYGFJFEH-UHFFFAOYSA-N oat triterpenoid saponin Chemical compound CNC1=CC=CC=C1C(=O)OC1C(C=O)(C)CC2C3(C(O3)CC3C4(CCC5C(C)(CO)C(OC6C(C(O)C(OC7C(C(O)C(O)C(CO)O7)O)CO6)OC6C(C(O)C(O)C(CO)O6)O)CCC53C)C)C4(C)CC(O)C2(C)C1 SYXUBXTYGFJFEH-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 229910000889 permalloy Inorganic materials 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
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- 239000000843 powder Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
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- 150000007949 saponins Chemical class 0.000 description 1
- 235000017709 saponins Nutrition 0.000 description 1
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 1
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- 238000004544 sputter deposition Methods 0.000 description 1
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- 229910000586 vicalloy Inorganic materials 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0027—Thick magnetic films
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/16—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates the magnetic material being applied in the form of particles, e.g. by serigraphy, to form thick magnetic films or precursors therefor
Definitions
- the present invention relates to the preparation of particular types of magnetic layers and to their use in an anti-theft system.
- H a ferromagnetic sample that is initially demagnetized
- B a particular flux density
- the value of H is decreased again the decreasing flux density does not follow the path of increase but decreases at a rate less than that at which it rose.
- H has reached zero again the value of B is not reduced to zero but to a value called the retentivity or remanence.
- the sample has retained a permanent magnetization.
- the value of B may be reduced to zero by reversing th magnetic field to negative and increasing its value to the so-called coercive force or coercivity.
- H By further increasing H to negative values and then again reversing its direction a hysteresis loop as represented in fig. 1 is completed.
- a so-called soft ferromagnetic material shows a rather low coercive force ; a so-called semi-soft ferromagnetic material shows a rather high coercive force.
- This properties are used in a special type of anti-theft labels, e.g. for preventing the theft from clothes out of shops, called EM-EAS labels ( E lectro M agnetic E lectronic A rticle S urveillance).
- the principle works as follows.
- a label carrier is covered on one side with a soft magnetic layer having a coercive force of about 0.5 Oe, and on the other side with a semi-soft magnetic layer having a coercive force of about 100 Oe.
- the detection zone consists of a transmitter which transmits an alternating magnetic field with a force Z M positioned between 0.5 and 100 Oe, and of a receiver.
- the semi-soft magnetic layer consists of a nickel mesh
- the soft magnetic layer consists of a complex alloy of Ni a Fe b Co c (Mo) d B e .
- the problem with these magnetic layers is the fact that they are nowadays applied by means of sputtering in vacuo, a cumbersome and expensive technique.
- aqueous solution of nickel(II) ions is prepared.
- a most suitable salt is Ni(NO 3 ) 2 .6H 2 O.
- the solution is acidified with a small amount of nitric acid.
- the nickel ions in the solution are reduced to highly dispersed metallic nickel particles of nanosize by means of the addition of a reducing agent.
- a preferred reducing agent is KBH 4 .
- the reducing agent can be added to the original nickel salt solution as a solid powder. More preferably, the reducing agent may be dissolved separately in a second aqueous medium and added to the nickel salt solution according to a single jet or a double jet procedure. Preferably, according to the double jet principle, the aqueous medium containing the nickel ions and the second solution containing the reducing agent are added together to a third aqueous medium.
- the second aqueous solution comprising the reducing agent preferably also contains sulphite ions which strongly enhance the chemical stability of this solution.
- a protective binder is preferably added to one or more of the three aqueous solutions involved.
- this protective binder is added to the third aqueous medium wherein both others are jetted.
- a particularly preferred protective binder is carboxymethylcellulose (CMC).
- CMC carboxymethylcellulose
- Other possible binders include gelatin, arabic gum, poly(acrylic acid), cellulose derivatives and other polysaccharides.
- a complexing agent is present in one of the three aqueous media described above.
- a preferred complexant is simply the well-known ethylenediaminetetraacetic acid (EDTA) or a homologous compound or a salt thereof.
- EDTA ethylenediaminetetraacetic acid
- Another preferred one is citrate, e.g. triammonium citrate.
- Suitable complexants include diethylenetriamine-pentaacetic acid (DTPA), trans-1,2-diaminocyclohexane-N,N,N',N'-tetraacetic acid (CDTA), ethyleneglycol-O,O'-bis(2-aminoethyl)-N,N,N',N'-tetraacetic acid (EGTA), N-(2-hydroxyethyl)ethylenediamine-N,N,N'-triacetic acid (HEDTA), etc.
- the complexing agent is preferably present in the third aqueous medium to which the other solutions are added according to the double jet principle.
- the superfluous salts are first removed from the aqueous medium by a washing process, preferably involving ultrafiltration and/or diafiltration. Additionally or alternatively centrifugation can be used.
- a so-called dispersing aid can be present.
- this compound is added to the diafiltration liquid at the last stage of the preparation.
- Suitable dispersing aids in the case of nickel are phosphates, more particularly a hexametaphosphate such as sodium hexametaphosphate.
- the hexametaphosphate adsorbs to the surface of the alloy particles so that they become negatively charged. By electrostatic repulsion they are kept in dispersion.
- the phosphate inhibits further oxidation of the surface of the formed nanoparticles.
- the thin nickel oxide shell that will be formed inevitably around the nanoparticles since the reducing medium disappears during the washing step will be passivated by the hexametaphosphate.
- the nickel particles are ultrafiltrated e.g. through a Fresenius F60 cartridge and subsequently diafiltrated against a solution of sodium hexametaphosphate in water/ethanol (98.5/1.5).
- the hexametaphosphate is also preferably added to the third aqueous solution.
- the obtained final colloidal composition is coated on the substrate by means of a conventional coating technique, such as slide hopper, curtain coating and air-knife coating.
- a conventional coating technique such as slide hopper, curtain coating and air-knife coating.
- Suitable coating agents include non-ionic agents such as saponins, alkylene oxides e.g. polyethylene glycol, polyethylene glycol/polypropylen glycol condensation products, polyethylene glycol alkyl esters or polyethylene glycol alkylaryl esters, polyethylene glycol esters, polyethylene glycol sorbitan esters, polyalkylene glycol alkylamines or alkylamides, silicone-polyethylene oxide adducts, glycidol derivaties, fatty acid esters of polyhydric alcohols and alkyl esters of saccharides; anionic agenst comprising an acid group such as a carboxy, sulpho, phospho, sulphuric or phosphoric ester group; ampholytic agents such as aminoacids, aminoalkyl sulphonic acids, aminoalkyl sulphates or phosphates, alkyl betaines, and amine-N-oxides; and cationic agents such as aklylamine salt
- Useful transparent organic resin supports include e.g. cellulose nitrate film, cellulose acetate film, polyvinylacetal film, polystyrene film, polyethylene terephthalate film, polycarbonate film, polyvinylchloride film or poly- ⁇ -olefin films such as polyethylene or polypropylene film.
- the thickness of such organic resin film is preferably comprised between 0.05 and 0.35 mm.
- the support is a polyethylene terephthalate layer provided with a subbing layer. This subbing layer can be applied before or after stretching of the polyester film support.
- the polyester film support is preferably biaxially stretched at an elevated temperature of e.g.
- the stretching may be accomplished in two stages, transversal and longitudinal in either order or simultaneously.
- the subbing layer when present, is preferably applied by aqueous coating between the longitudinal and transversal stretch, in a thickness of 0.1 to 5 mm.
- the subbing layer preferably contains, as described in EP 0 464 906, a homopolymer or copolymer of a monomer comprising covalently bound chlorine. Examples of said homopolymers or copolymers suitable for use in the subbing layer are e.g.
- polyvinyl chloride polyvinylidene chloride; a copolymer of vinylidene chloride, an acrylic ester and itaconic acid; a copolymer of vinyl chloride and vinylidene chloride; a copolymer of vinyl chloride and vinyl acetate; a copolymer of butylacrylate, vinyl acetate and vinyl chloride or vinylidene chloride; a copolymer of vinyl chloride, vinylidene chloride and itaconic acid; a copolymer of vinyl chloride, vinyl acetate and vinyl alcohol, etc.
- Polymers that are water dispersable are preferred since they allow aqueous coating of the subbing layer which is ecologically advantageous.
- the support may be opaque, such as a paper support, e.g. a plain paper support or a polyolefin coated paper. Furtheron glass, e.g. thin glass packed on roll can be used.
- the coated substantially pure nickel layer is ferromagnetic of the so-called semi-soft type.
- the nickel ions are not the sole ion type undergoing reduction but they are mixed with one or more other types of ions.
- Preferred types of salts for admixture with the nickel salt are iron salts, cobalt salts or molybdene salts, or mixtures of those.
- soft magnetic layers By choosing the appropriate type(s) of ions and the appropriate admixture ratio(s) so-called soft magnetic layers can be prepared.
- a support preferably a paper support
- a semi-soft magnetic layer based on substantially pure nickel prepared according to the present invention
- a soft magnetic layer based on an admixture of nickel particles with other metal particles prepared according to the present invention.
- the resulting labels can be used in a EM-EAS system ( E lectro M agnetic E lectronic A rticle S urveillance). Furtheron, such a label can also be produced when a semi-soft magnetic layer prepared according to the present invention is applied to a commercially available soft magnetic layer on a support.
- PERMALLOY (trade mark of Western Electric), METGLAS (trade mark of Allied Signal Co.), and ATALANTE (trade mark of IST/Bekaert).
- Particularly useful METGLAS products are type 2705M, consisting of Co 69 Fe 4 Ni 1 B 12 Si 12 , and type 2826MB, consisting of Fe 40 Ni 38 Mo 4 B 12 .
- such a label can also be produced when a soft magnetic layer prepared according to the present invention is applied to a commercially available semi-soft magnetic layer on a support.
- Examples of such commercial products are VICALLOY (trade mark of Telecon Metals Ltd.), AMOKROME (trade mark of Arnold Engineering), and CROVAK (trade mark of Vacuumschmelze GmbH).
- the Ni-Fe-dispersion was prepared as follows:
- solution 1 at a flow rate of 12.4 ml/min was simultaneously added with solution 2 at 12.4 ml /min.
- the NiFe dispersion was ultrafiltrated through a Fresenius F60 cartridge and diafiltrated with a 0.36 % solution of sodium hexametaphosphate in water/ethanol (98.5/1.5).
- the dispersion was stirred and 10 ml of a 12.5% solution of Saponine Quillaya (Schmittmann) in water/ethanol (80/20) was added. This is the Ni-Fe dispersion.
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Soft Magnetic Materials (AREA)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP19990201371 EP0997918B1 (de) | 1998-10-26 | 1999-04-29 | Herstellung einer Magnetschicht |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP98203868 | 1998-10-26 | ||
EP98203868 | 1998-10-26 | ||
EP19990201371 EP0997918B1 (de) | 1998-10-26 | 1999-04-29 | Herstellung einer Magnetschicht |
Publications (2)
Publication Number | Publication Date |
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EP0997918A1 true EP0997918A1 (de) | 2000-05-03 |
EP0997918B1 EP0997918B1 (de) | 2004-07-14 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP19990201371 Expired - Lifetime EP0997918B1 (de) | 1998-10-26 | 1999-04-29 | Herstellung einer Magnetschicht |
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EP (1) | EP0997918B1 (de) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5767156A (en) * | 1980-10-13 | 1982-04-23 | Nec Corp | Electroless plating bath |
JPS583963A (ja) * | 1981-06-29 | 1983-01-10 | Nec Corp | 無電解めつき方法 |
JPH02108221A (ja) * | 1988-10-18 | 1990-04-20 | Mitsubishi Kasei Corp | 磁気記録媒体 |
EP0793242A1 (de) * | 1996-02-28 | 1997-09-03 | Unitika Ltd. | Magnetisches Element und dessen Herstellungsverfahren |
-
1999
- 1999-04-29 EP EP19990201371 patent/EP0997918B1/de not_active Expired - Lifetime
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5767156A (en) * | 1980-10-13 | 1982-04-23 | Nec Corp | Electroless plating bath |
JPS583963A (ja) * | 1981-06-29 | 1983-01-10 | Nec Corp | 無電解めつき方法 |
JPH02108221A (ja) * | 1988-10-18 | 1990-04-20 | Mitsubishi Kasei Corp | 磁気記録媒体 |
EP0793242A1 (de) * | 1996-02-28 | 1997-09-03 | Unitika Ltd. | Magnetisches Element und dessen Herstellungsverfahren |
Non-Patent Citations (3)
Title |
---|
PATENT ABSTRACTS OF JAPAN vol. 006, no. 143 (C - 117) 3 August 1982 (1982-08-03) * |
PATENT ABSTRACTS OF JAPAN vol. 007, no. 069 (C - 158) 23 March 1983 (1983-03-23) * |
PATENT ABSTRACTS OF JAPAN vol. 014, no. 325 (P - 1075) 12 July 1990 (1990-07-12) * |
Also Published As
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EP0997918B1 (de) | 2004-07-14 |
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