CN1459034A - 磁性薄膜干涉器件或颜料及其制造方法、含这种磁性薄膜干涉器件的印刷油墨或涂料组合物、秘密文件以及应用 - Google Patents
磁性薄膜干涉器件或颜料及其制造方法、含这种磁性薄膜干涉器件的印刷油墨或涂料组合物、秘密文件以及应用 Download PDFInfo
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- CN1459034A CN1459034A CN02800567A CN02800567A CN1459034A CN 1459034 A CN1459034 A CN 1459034A CN 02800567 A CN02800567 A CN 02800567A CN 02800567 A CN02800567 A CN 02800567A CN 1459034 A CN1459034 A CN 1459034A
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- Prior art keywords
- layer
- magnetic
- ovp
- pigment
- magnetic film
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- 230000005291 magnetic effect Effects 0.000 title claims abstract description 120
- 239000000049 pigment Substances 0.000 title claims abstract description 31
- 238000007639 printing Methods 0.000 title claims description 16
- 239000008199 coating composition Substances 0.000 title claims description 12
- 238000004519 manufacturing process Methods 0.000 title description 5
- 239000010409 thin film Substances 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 26
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 239000000696 magnetic material Substances 0.000 claims description 64
- 239000003795 chemical substances by application Substances 0.000 claims description 46
- 239000003989 dielectric material Substances 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 28
- 239000006096 absorbing agent Substances 0.000 claims description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 27
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- 239000004411 aluminium Substances 0.000 claims description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 22
- 230000008021 deposition Effects 0.000 claims description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 18
- 230000003287 optical effect Effects 0.000 claims description 15
- 239000011651 chromium Substances 0.000 claims description 11
- 238000003475 lamination Methods 0.000 claims description 10
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052804 chromium Inorganic materials 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 230000000903 blocking effect Effects 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 230000005294 ferromagnetic effect Effects 0.000 claims description 3
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 238000002310 reflectometry Methods 0.000 claims description 3
- 238000013517 stratification Methods 0.000 claims description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims 2
- 229910052684 Cerium Inorganic materials 0.000 claims 1
- 229910052692 Dysprosium Inorganic materials 0.000 claims 1
- 229910052691 Erbium Inorganic materials 0.000 claims 1
- 229910052693 Europium Inorganic materials 0.000 claims 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 1
- 229910052689 Holmium Inorganic materials 0.000 claims 1
- 229910052765 Lutetium Inorganic materials 0.000 claims 1
- 229910052779 Neodymium Inorganic materials 0.000 claims 1
- 229910052777 Praseodymium Inorganic materials 0.000 claims 1
- 229910052772 Samarium Inorganic materials 0.000 claims 1
- 229910052771 Terbium Inorganic materials 0.000 claims 1
- 229910052775 Thulium Inorganic materials 0.000 claims 1
- 229910052769 Ytterbium Inorganic materials 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 229910052797 bismuth Inorganic materials 0.000 claims 1
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- 229910052802 copper Inorganic materials 0.000 claims 1
- 230000002452 interceptive effect Effects 0.000 claims 1
- 229910052746 lanthanum Inorganic materials 0.000 claims 1
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- 238000010298 pulverizing process Methods 0.000 claims 1
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- 229910052727 yttrium Inorganic materials 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
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- 239000000976 ink Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 139
- 238000000151 deposition Methods 0.000 description 18
- 239000010408 film Substances 0.000 description 16
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- 238000010894 electron beam technology Methods 0.000 description 8
- 230000009471 action Effects 0.000 description 7
- 229910001004 magnetic alloy Inorganic materials 0.000 description 7
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- 238000010884 ion-beam technique Methods 0.000 description 6
- 229910000859 α-Fe Inorganic materials 0.000 description 6
- 230000005415 magnetization Effects 0.000 description 5
- NVIVJPRCKQTWLY-UHFFFAOYSA-N cobalt nickel Chemical compound [Co][Ni][Co] NVIVJPRCKQTWLY-UHFFFAOYSA-N 0.000 description 4
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 4
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 4
- 229910003321 CoFe Inorganic materials 0.000 description 3
- 239000002223 garnet Substances 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
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- 230000005389 magnetism Effects 0.000 description 2
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- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 2
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- 230000004044 response Effects 0.000 description 2
- 229910000684 Cobalt-chrome Inorganic materials 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 229910017709 Ni Co Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910003267 Ni-Co Inorganic materials 0.000 description 1
- 229910003262 Ni‐Co Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- ZDZZPLGHBXACDA-UHFFFAOYSA-N [B].[Fe].[Co] Chemical compound [B].[Fe].[Co] ZDZZPLGHBXACDA-UHFFFAOYSA-N 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- WAIPAZQMEIHHTJ-UHFFFAOYSA-N [Cr].[Co] Chemical compound [Cr].[Co] WAIPAZQMEIHHTJ-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000005303 antiferromagnetism Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229940090961 chromium dioxide Drugs 0.000 description 1
- 229910021563 chromium fluoride Inorganic materials 0.000 description 1
- IAQWMWUKBQPOIY-UHFFFAOYSA-N chromium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Cr+4] IAQWMWUKBQPOIY-UHFFFAOYSA-N 0.000 description 1
- AYTAKQFHWFYBMA-UHFFFAOYSA-N chromium(IV) oxide Inorganic materials O=[Cr]=O AYTAKQFHWFYBMA-UHFFFAOYSA-N 0.000 description 1
- GUTLYIVDDKVIGB-IGMARMGPSA-N cobalt-59 atom Chemical compound [59Co] GUTLYIVDDKVIGB-IGMARMGPSA-N 0.000 description 1
- 239000010952 cobalt-chrome Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
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- 238000002425 crystallisation Methods 0.000 description 1
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- 230000001066 destructive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000002889 diamagnetic material Substances 0.000 description 1
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- 230000008020 evaporation Effects 0.000 description 1
- 230000005308 ferrimagnetism Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000005352 galvanomagnetic phenomena Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000012943 hotmelt Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- JSUSQWYDLONJAX-UHFFFAOYSA-N iron terbium Chemical compound [Fe].[Tb] JSUSQWYDLONJAX-UHFFFAOYSA-N 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000002680 magnesium Chemical class 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000005408 paramagnetism Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
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Classifications
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- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/22—Absorbing filters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0078—Pigments consisting of flaky, non-metallic substrates, characterised by a surface-region containing free metal
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
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-
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/42—Magnetic properties
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- C—CHEMISTRY; METALLURGY
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- C09C2200/1008—Interference pigments characterized by the core material the core comprising at least one inorganic oxide, e.g. Al2O3, TiO2 or SiO2 comprising at least one metal layer adjacent to the core material, e.g. core-M or M-core-M
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/306—Thickness of an absorbing layer
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/308—Total thickness of the pigment particle
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2220/00—Methods of preparing the interference pigments
- C09C2220/20—PVD, CVD methods or coating in a gas-phase using a fluidized bed
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
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- Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
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- Y10T428/12868—Group IB metal-base component alternative to platinum group metal-base component [e.g., precious metal, etc.]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明公开磁性的OVP，所述的颜料由薄层絮片组成，这些絮片具有金属－介电材料－金属的基本结构，使产生与观察角度有关的颜色现象，除了所述与观察角度有关的颜色现象以外，还具有引入的磁性质，能使其与具有类似颜色现象但没有所述磁性质的OVP区分开。本发明还公开制备这类颜料的方法，以及这类颜料作为安全要素在油墨、涂料、和制品中的应用。
Description
发明领域
本发明属于光学上可变化的颜料领域。具体而言，本发明叙述了一种磁性薄膜干涉器件，制造这种磁性薄膜干涉器件的方法、磁性薄膜干涉颜料、印刷油墨或涂料组合物、秘密文件以及这种磁性薄膜干涉器件的应用，一切根据专利权利要求的规定。
发明背景
可以采用各种类型光学上可变化的器件作为银行票据和秘密文件有效的防伪手段。大部分世界范围印刷的货币都依靠这种光学上可变化的复制保护器件，自从1987年它们第一次在货币上出现时起，人们已经从其中学会采用光学上可变化的油墨(OVITM)印刷的特性。
光学上可变化的颜料(OVP)具有与观察角度有关的颜色现象，这种颜色现象不能采用采色复制设备再现。现今可以在市场上买到各种不同类型的OVP材料。
采用物理蒸气沉积方法制造的第一种类型的OVP，具有非常明亮的颜色。将这种类型的OVP制成蒸气沉积薄膜Fabry-Pérot谐振器叠片。在现有技术中，描述了金属-介电材料-金属简单夹层，以及金属-介电材料-金属-介电材料-金属双夹层的层顺序。顶部的金属层必须是可部分反射/部分透射的，使光能够进出Fabry-Pérot谐振器叠片。
在载体箔上，将所述光学上可变化的薄膜材料制成连续的片。然后可将其与载体分离，粉碎成颜料，该颜料由直径20-30μm，厚度约1μm的絮片组成。可将这种颜料配制成油墨或涂料组合物，优选应用于网板印刷或凹版印刷。
所述颜料的光学可变性与干涉效应有关。投射在所述金属-介电材料-金属类型的OVP絮片上的入射光，一部分在顶部金属层上被反射，一部分穿过介电层透射，并在底部金属层上反射回去。入射光的这两部分反射，最终重新结合并互相干涉。最终是相长干涉还是相消干涉取决于介电层的厚度和入射光的波长。在白色入射光的情况下，具有确定波长的某些白光成分被反射，而具有其它波长的其它成分却未被反射。这就产生了光谱选择作用，从而产生颜色现象。
顶部反射的部分光和底部反射的部分光的路径差异，显然取决于入射角度，因此产生了所得到的干涉颜色。
另一种，也就是第二种类型的OVP，是基于一些涂覆的铝絮片。采用化学蒸气沉积(CVD)或采用湿法化学沉积，在使用机械方法压平的铝颗粒上涂覆介电材料层，随后涂覆金属层或第二介电材料层。通过与上述相同的作用产生干涉色。这种类型的OVP在制造上比第一种类型便宜，但颜色不如第一种类型明亮，而与角度有关的色移却比第一种类型小。
大量“光学上可变化的”和“虹彩”颜料，只是为了装饰目的(汽车和玩具等的涂料和漆)生产的，因此公众可以以涂料组合物的形式买到。如果不能确定“安全OVP”和“装饰OVP”之间的明显差异，在光学上可变化的油墨特性，对银行票据的安全潜力就会降低。伪造者显然能利用彩色复印机，借助于市场上可以买到的装饰涂料或喷漆伪造银行的票据，加入缺少的光学上可变化的特性。
由于这些和其它原因，必须制造在材料上与只用于装饰，在市场上可以买到类型的OVP有差异的安全OVP。制造这种OVP的有效途径是给安全OVP掺杂隐藏的磁性。这种“磁性OVP”显然能将不同安全水平的引入相应的的标记文件中：i)简单的“有/无磁性”特征；ii)特征磁性的识别；iii)具有磁性或非磁性特征的印刷图案；和iv)磁性数据的载体，将磁性信息存储在印刷的具有磁性特征的OVP中。
在US 4,838,648中已经提出了这种磁性的OVP。为此目的，将特定的磁性材料加入OVP的结构中。US 4,838,648的OVP是金属(反射剂)-介电材料-金属(吸收剂)多层Fabry-Pérot类型的，优选采用钴-镍比为80∶20的磁性合金作为反射剂层。另外，但不是优选方案，磁性合金也可以吸收剂层的形式存在。根据US 4,838,648的器件，具有值得注意的缺点，i)光学性能降低，特别是由于钴-镍合金的反射率较低，与铝相比具有较低的色度，和ii)缺乏选择磁性材料的灵活性。后者的磁性合金，显然应当同时起磁性材料和优良反射剂的作用，只有非常少的材料能满足这两个条件。
本发明的第一个目的是提供安全的OVP，它通过引入特定的磁性质，使安全OVP在材料上与装饰OVP不同。
本发明的另一个目的是在不降低OVP色度和色移性质的情况下，将所述的磁性质引入所述的OVP中。
本发明的另一个目的是提供其磁性材料的选择灵活性尽可能大的所述磁性OVP。
本发明的另一个目的是提供安全的OVP，这种OVP可以在不明显增加生产成本的情况下，采用与生产“普通的”非磁性OVP使用的相同设备和方法制造。
发明概述
本发明涉及一种由OVP制造的磁性薄膜干涉器件，该OVP具有与观察角度有关的颜色现象。这种OVP是由多层的叠片组成的，该叠片包括至少一层反射光的反射剂层、至少一层透过光的介电材料层、至少一层吸收光的吸收剂层、和至少一层磁性材料层。反射剂层将磁性材料层与介电材料层分开。
根据磁性OVP第一个优选的实施方案，将磁性材料层配置在两个反射剂层之间。磁性材料层被对称地封闭在两个反射剂层之间，使其沿着两个反射剂层侧具有相同的光学性质。
根据磁性OVP第二个优选的实施方案，磁性材料层只与一层反射剂层邻接，使其只沿一个反射剂层侧具有光学性质。
根据本发明的磁性OVP具有独特的优点，可采用所公开的层顺序，能将相应非磁性OVP的颜色与角色移准确地匹配，同时提供种类广泛的磁性OVP。
可将磁性薄膜干涉器件粉碎，获得磁性薄膜干涉颜料。可将所述的磁性薄膜干涉颜料加到印刷油墨或涂料中，和/或秘密文件上。
通过一些附图和实施例进一步说明本发明：
图1示出具有5层结构的常规OVP薄层。
图2示出根据本发明具有磁性质的磁性OVP第一个优选实施方案的横截面。采用7层结构。
图3示出根据本发明具有磁性质的磁性OVP第二个优选实施方案的横截面。采用4层结构。
图1示出上述具有5层结构的第一种类型OVP的横截面。这种颜料由絮片组成，絮片的大小约20-30μm，厚度约1μm。为了在两侧提供相同的光学性质，所述的絮片具有对称的“吸收剂/介电材料/反射剂/介电材料/吸收剂”层结构。吸收剂层1，1′，优选是薄的(例如约3-5nm)铬层或类似的耐腐蚀金属层，它们起入射光分束器、反射和透射部件的作用。介电材料层2，2′优选低介电常数的材料，例如氟化镁(MgF2；n＝1.38)或二氧化硅，能产生与大角度有关的色移。介电材料层2，2′的厚度决定了OVP的颜色，其厚度为约200-800nm(例如金色-绿色：440nm MgF2，绿色-蓝色：385nm MgF2)。中间反射全部光的反射剂层3，优选铝或任何其它反射大的金属或金属合金，厚度为约10-100nm。
图2示出根据本发明的磁性OVP第一个优选实施方案的层顺序示意图。所述的磁性OVP包括二层吸收剂层1，1′、二层介电材料层2，2′、和二层反射剂层3，3′。将至少一层磁性材料的磁性材料层4，配置在所述的反射剂层3，3′之间，获得对称的“吸收剂/介电材料/反射剂/磁性材料/反射剂/介电材料/吸收剂7层结构。
图3示出根据本发明的磁性OVP第二个优选实施方案的层顺序示意图。所述的磁性OVP包括一层吸收剂层1、一层介电材料层2、和至少一层与一层反射剂层3邻接的磁性材料层4。在这个实施方案中，需要4-层结构。优选在涂覆脱模剂R的载体箔C上，沉积铬吸收剂层1，接着沉积氟化镁介电材料层2，和铝反射剂层3。最后沉积磁性材料的磁性材料层4。随后采用例如适宜的胶结方法，将该装置施加到基片上，使磁性材料层对着基片。
磁性材料层4可以是任何类型的磁性材料，例如铁、钴、镍；磁性合金，例如Ni-Co或Nd-Fe-B；无机氧化物，例如Fe2O3，Fe3O4，二氧化铬CrO2，铁酸盐MFe2O4(M是一种离子或离子混合物，M选自Mg2+、Ca2+、Sr2+、Ba2+、Mn2+、Co2+、Fe2+、Ni2+、Cu2+、Zn2+等)，石榴子石A3B5O12(A＝三价稀土离子或三价稀土离子的混合物，B是一种离子或离子的混合物，B选自Al3+、Cr3+、Fe3+、Ga3+、Bi3+等)，六铁酸盐(hexaferrites)MFe12O19，其中M选自二价离子Ca2+、Sr2+、Ba2+等，和钙钛矿等。
在本发明的上下文中，显然可以使用任何类型的非抗磁性材料，为磁性OVP提供特定的磁性质。所述的磁性质，例如可以是强(超)顺磁性；铁磁性；铁氧体磁性；反铁磁性；和反铁氧体磁性等。这种材料可以是软磁性的低矫顽磁性、中矫顽磁性、或硬磁性类型、或可以将其设计成利用巴克豪森(Barkhausen)效应进行检测。这种磁性质还可以产生0奥斯特至高达10,000奥斯特的剩余磁性。
磁性材料的沉积是采用与沉积介电材料层或上述第一种类型的非磁性OVP的金属层使用的相同的方法进行的。显然可以利用借助于电子束的热蒸发方法沉积MgF2、铬、或铝。磁性合金，例如钴-镍、或铁-钴-硼，在熔点和蒸发特性方面可以与铬相比，因此可以采用类似的方法进行沉积，使沉积在材料居里(Curie)或尼尔(Neel)温度以上的源温度下进行的。就氧化物材料的沉积而言，一般需要较高的沉积温度，但这些材料实际上可以利用电子束技术沉积。对于比较复杂的化学组合物的沉积，可以采用借助离子束的蒸发方法。
磁性材料层4经由优良的反射光材料，例如铝、铝合金、铬、银、和金等制成的反射剂层3，3′覆盖。这使磁性OVP在优良的光学性能以及客户指定的磁性质方面同时达到最佳化。采用这种方法，可以生产不同种类的安全OVP，每一种都具有完全相同的颜色现象和色移性质，但却具有不同的磁性质。采用本领域技术人员已知的相应磁性检测装置，可以很容易地将它们互相区分开，以及将它们与具有相同光学现象的非磁性OVP区分开。
此外，还可以将最初获得的光学上可变化的磁性薄膜产品，直接用作光学上可变化的安全箔，可优选采用热压印(hot-stamping)或冷压印(cold stamping)，或相关的施加方法，将其施加到文件或商品上。
为了安全目的，可以方便利用的另一种性质是薄膜磁性材料的磁化或磁滞曲线的具体形式。由于它们第三维尺寸受到限制，这些材料往往具有非常高的方形磁滞曲线以及可变化的矫顽磁性值，矫顽磁性值显然取决于层的厚度和沉积磁性材料层使用的参数。也可以将这些材料设计成具有显著的巴克豪森效应，利用这种效应，能采用电子产品监视(EAS)应用的已知技术检测它们。另一种方案，可以通过选择适宜的磁性材料，例如无定形的磁性合金或低磁饱和度的磁性石榴子石，利用非线性的磁化效应进行检测。因此为具有磁效应和磁性质的OVP设计开辟了广阔的领域，只是基于常规的OVP与常规的磁性材料混合是非常困难伪造的。
显然可以采用与制造常规5层非磁性OVP所需要的相同类型的真空沉积设备来分别制造所述的7层磁性OVP和4层磁性OVP。
在磁性OVP中可以存在一层以上的磁性材料。在多层磁性材料的情况下，所述的各层可以是相同或不同的磁性材料；而且所述的磁性材料层，可以是互相邻接的，也可以是利用非磁性材料层互相隔开的。所述的磁性材料层4可以是多层的叠片，优选成层的超点阵。成层的超点阵已显示出不同寻常的电磁效应，例如Giant磁阻效应、非线性高频响应、和不同寻常的核磁共振签字等。
此外，根据本发明的磁性OVP还可以载带另外的公开或隐藏的性能，例如标记、微纹理、冷光、射频或微波谐振吸收等。
实施例
在图2所示的磁性OVP第一个优选实施方案中，磁性材料层4包括在OVP叠片的二个全反射剂层3，3′之间。为了提供最佳的光学和磁性作用条件，采用“标准的”OVP层顺序——铬/氟化镁/铝完成光学作用。为了以任何所需的磁性元素、合金或化合物附加层的形式，在其内部容纳磁性功能，铝层“被分成二部分”。
在涂覆脱膜剂R的载体箔C上，沉积第一铬吸收剂层1，接着沉积第一氟化镁介电材料层2和第一铝反射剂层3。然后沉积磁性材料的磁性材料层4，接着沉积第二铝反射剂层3′。然后沉积第二氟化镁介电材料层2′和第二铬吸收剂层1′，制成磁性OVP多层叠片。
本领域的技术人员应当注意，可以采用任何类型的磁性材料——无定形或结晶的，例如磁性金属类的铁、钴、和镍等；或磁性合金，例如钴-镍、钴-铬、铽-铁、和钕-铁-硼等；或磁性耐熔化合物，例如来自铁酸盐、六铁酸盐、石榴子石、和钙钛矿等的简单或复杂的氧化物，作为二层铝反射剂层之间中等的磁性材料层。
1.软磁性的绿色-蓝色OVP
在磁性OVP的第一个优选的实施方案中，采用软磁性的铁作为磁性作用的载体。采用借助于电子束的热蒸发方法，按下列顺序将7层材料沉积在涂覆剥离剂R的载体箔C上：
1.铬金属，3.5nm厚(第一吸收剂层1)
2.MgF2，385nm厚(第一介电材料层2)
3.金属铝，40nm厚(第一反射剂层3)
4.金属铁，200nm厚(磁性材料层4)
5.金属铝，40nm厚(第二反射剂层3′)
6.MgF2，385nm厚(第二介电材料层2′)
7.金属铬，3.5nm厚(第二吸收剂层1′)，入射角为直角的总光学路径：530nm。
在完成沉积之后，从载体箔C上取下薄膜产品，粉碎成颜料，应用在油墨和涂料组合物中。
在磁性OVP第一个优选实施方案的变形方案中，磁性材料层4是由金属镍制成的，得到低矫顽磁性的光学上可变化的颜料。
在磁性OVP第一个优选实施方案的另一个方案中，磁性材料层4是由金属钴制成的，得到中等矫顽磁性的光学上可变化的颜料，而且这种颜料在其自己的磁场中，在214MHz范围内，采用钴-59核磁共振检测是灵敏的。
在磁性OVP第一个优选实施方案的另一个方案中，磁性材料层4是由金属钆制成的，得到的光学上可变化的颜料，在钆金属的居里温度16℃以下是铁磁性的。
2.低矫顽磁性的金色-绿色OVP
在磁性OVP第一个优选实施方案的另一个方案中，采用组成为Fe50Co25Si10B15的、低矫顽磁性的、无定形的、巴克豪森活性的EAS材料作为磁性作用的载体。采用借助于电子束的热蒸发方法，按下列顺序将7层材料沉积在涂覆脱模剂R的载体箔C上：
1.金属铬，3.5nm厚(第一吸收剂层1)
2.MgF2，440nm厚(第一介电材料层2)
3.金属铝，40nm厚(第一反射剂层3)
4.Fe50Co25Si10B15，500nm厚(磁性材料层4)
5.金属铝，40nm厚(第二反射剂层3′)
6.MgF2，440nm厚(第二介电材料层2′)
7.金属铬，3.5nm厚(第二吸收剂层1′)，入射角为直角的总光学路径：605nm。
也可以利用借助于氩离子束的热蒸发方法，方便地沉积复杂的无定形的Fe50Co25Si10B15合金。
在完成沉积之后，从载体上取下薄膜产品，粉碎成颜料，应用在油墨和涂料组合物中。
这种材料在1奥斯特以下的磁场范围内，磁化作用的变化具有明显的巴克豪森不连续性。
3.中等矫顽磁性的绿色-蓝色OVP
在磁性OVP第一个优选实施方案的另一个方案中，采用组成为CoFe2O4的中等矫顽磁性的铁酸钴，作为磁性作用的载体。采用借助于电子束的热蒸发方法，按下列顺序将7层材料沉积在涂覆脱模剂(R)的载体箔(C)上：
1.金属铬，3.5nm厚(第一吸收剂层1)
2.MgFe2，385nm厚(第一介电材料层2)
3.金属铝，40nm厚(第一反射剂层3)
4.CoFe2O4，100nm厚(磁性材料层4)
5.金属铝，40nm(第二反射层3′)
6.MgF2，385nm厚(第二介电材料层2′)
7.金属铬，3.5nm厚(第二吸收剂层1′)，入射角为直角的总光学路径：530nm。
也可以利用借助于氩离子束的热蒸发方法，方便地沉积CoFe2O4铁酸盐材料。
在完成沉积之后，从载体上取下薄膜产品，粉碎成颜料，应用在油墨和涂料组合物中。
包含根据这个实施方案制造的磁性OVP的光学上可变化的修补插入码，可以成功地用作安全信息，例如客运票、银行卡、信用卡和出入卡中的隐式交叉检验信息的磁存储器的磁道。
4.高矫顽磁性的绿色-蓝色OVP
在磁性OVP第一个优选实施方案的另一个方案中，采用组成为BaFe12O19的高矫顽磁性的铁酸钡，作为磁性作用的载体。采用借助于电子束的热蒸发方法，按下列顺序将7层材料沉积到涂覆脱模剂R的载体箔C上：
1.金属铬，3.5nm厚(第一吸收剂层1)
2.MgF2，385nm厚(第一介电材料层2)
3.金属铝，40nm厚(第一反射剂层3)
4.BaFe12O19，300nm厚(磁性材料层4)
5.金属铝，40nm厚(第二反射层3′)
6.MgF2，385nm厚(第二介电材料层2′)
7.金属铬，3.5nm厚(第二吸收剂层1′)，入射角为直角的总光学路径：530nm。
也可采用借助于氩离子束的热蒸发方法，方便地沉积铁酸盐材料BaFe12O19。
在完成沉积之后，从载体上取下薄膜产品，粉碎成颜料，应用在油墨和涂料组合物中。
可以成功地使用包含根据优选实施方案的这种方案制造的磁性OVP的光学上可变化的插入码，作为不可逆地书写磁性安全信息，例如在信用卡或出入卡中的隐式证实信息的磁道。为了书写所述的安全信息，需要一种特殊的通常得不到的硬件，将3000奥斯特矫顽磁性的铁酸钡材料磁化。
可将根据前述实施方案的OVP加到油墨或涂料组合物中，再采用任何印刷或涂敷方法，例如凹版印刷、丝网印刷、或转移印刷施加到商品上；采用另一种方案，可将它们模制或层压到塑料材料中。
本发明还公开具有磁性质的光学上可变化的箔，它可根据与所述光学上可变化的颜料的相同的原理制造。这类箔显然包括至少4层的叠片，在其顶部包括一个光学部件和至少一层附加的磁性材料层。
在光学上可变化的箔中，可以存在一层以上的磁性材料的磁性材料层4。在多个磁性材料层4的情况下，所述的磁性材料层可以互相邻接，或被非磁性材料层互相隔开。而且，磁性材料层4可以是相同或不同的磁性材料。此外，根据本发明的光学上可变化的箔还可以载带附加的公开或隐藏的性质，例如标记、微纹理、冷光、射频或微波谐振吸收等。
采用适宜的转移技术，例如热压印或冷压印，与适宜的胶一起将箔的磁性材料层侧施加到基片上。
5.中等矫顽磁性的金色-绿色OVP箔
在磁性OVP第二个优选的实施方案中，采用中等矫顽磁性的铁氧化物作为OVP箔中磁性作用的载体。采用借助于电子束的热蒸发方法，按下列顺序将4层材料沉积在涂覆脱模剂R的载体箔C上：
1.金属铬，3.5nm厚(吸收剂层1)
2.MgF2，440nm厚(介电材料层2)
3.金属铝，40nm厚(反射剂层3)
4.Fe2O3，500nm厚(磁性材料层4)，入射角为直角的总光学路径：605nm。
也可以采用借助于氩离子束的热蒸发方法，方便地沉积Fe2O3。
在完成沉积之后，使用热熔体胶组合物涂覆箔，采用细长的热压印模，将箔施加到秘密文件上，制成光学上可变化的磁道。然后采用磁性方法，将证实信息写入所述的安全磁道中。
6.可活化-钝化的EAS绿色-蓝色OVP箔
在磁性OVP第二个优选实施方案的变化方案中，采用多层磁性材料作为磁性作用的载体。该器件由Fe60Co15Si10B15的巴克豪森-活性EAS层，和接着的低矫顽磁性镍层组成。采用借助于电子束的热蒸发方法，按下列顺序沉积到涂覆脱模剂R的载体箔C上：
1.金属铬，3.5nm厚(吸收剂层1)
2.MgF2，385nm厚(介电材料层2)
3.金属铝，40nm厚(反射剂层3)
4.Fe60Co15Si10B15，200nm厚(第一磁性材料层4)
5.金属镍，200nm厚(第二磁性材料层4)，入射角为直角的总光学路径：530nm。
也可以采用借助于氩离子束的热蒸发方法，方便地沉积Fe60Co15Si10B15材料。
在完成沉积之后，采用预印刷、UV-活化胶插入码、和冷压印模，以光学上可变化的磁性安全密封形式，将箔施加到秘密文件上。
如果镍层是磁化状态，Fe60Co15Si10B15层将不会对巴克豪森询问信息组起反应，询问信息组是最大磁场强度在5奥斯特以下的交变磁场。然而在去磁循环结束时，可以通过它的特性响应，检测巴克豪森-活性材料。然后通过镍层重新磁化再被保护。
Claims (15)
1.一种具有与观察角度有关的颜色现象的磁性薄膜干涉器件，其中包括多层叠片，该叠片包括至少一层反射光的反射剂层(3，3′)、至少一层透过光的介电材料层(2，2′)、至少一层吸收光的吸收剂层(1，1′)、和至少一层磁性材料层(4)，其中所述的磁性材料层(4)通过反射剂层(3)与介电材料层(2)隔开。
2.根据权利要求1的磁性薄膜干涉器件，其中所述的磁性材料层(4)配置在二个反射剂层(3，3′)之间。
3.根据权利要求1或2的磁性薄膜干涉器件，其中所述的磁性材料层(4)是磁性金属或磁性金属合金层，其中包括选自铁、钴、镍、和钆的化学元素。
4.根据权利要求1-3之一的磁性薄膜干涉器件，其中所述的磁性材料层(4)是无机氧化物和/或通式MFe2O4的铁酸盐层，M是选自{Mg、Mn、Co、Fe、Ni、Cu、Zn}的双电荷离子的元素或元素混合物，和/或通式A3B5O12的石榴子石，A是选自{Y、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、或Bi}的三电荷离子的元素或元素混合物，B是选自{Fe、Al、Ga、Ti、V、Cr、Mn、或Co}的三电荷离子的元素或元素混合物。
5.根据权利要求1-4之一的磁性薄膜干涉器件，其中所述的反射剂层(3，3′)选自铝、铝合金、铬、镍、银、和金。
6.根据权利要求1-5之一的磁性薄膜干涉器件，其中所述的磁性材料层(4)是磁性的多层叠片，优选成层的超点阵。
7.根据权利要求6的磁性薄膜干涉器件，其中所述的多层叠片，包含至少两种不同磁性的材料或至少一种磁性的和至少一种非磁性的材料。
8.一种生产磁性薄膜干涉器件的方法，该器件是由光学上可变化的颜料制成的，该颜料具有与观察角度有关的颜色现象，该器件包括多层的叠片，其中包括至少一层反射光的反射剂层(3，3′)、至少一层透过光的介电材料层(2，2′)、至少一层吸收光的吸收剂层(1，1′)、和至少一层磁性材料层(4)，该方法包括以下步骤：
a)在吸收剂层(1，1′)的一侧上沉积介电材料层(2，2′)，
b)在所述的介电层(2，2′)上沉积反射剂层(3，3′)，和
c)在所述的反射剂层(3，3′)上沉积磁性材料层(4)。
9.生产根据权利要求8的磁性薄膜干涉器件的方法，其中包括：
d)在所述的磁性材料层(4)上沉积第二反射剂层(3′)
e)在所述的第二反射剂层(3′)上沉积第二介电材料层(2′)，和
f)在所述的第二介电材料层(2′)上沉积第二吸收剂层(1′)。
10.一种磁性薄膜干涉颜料，该颜料是粉碎权利要求1-7之一的磁性薄膜干涉器件制备的。
11.一种印刷油墨或涂料组合物，其中包含根据权利要求10的磁性薄膜干涉颜料。
12.一种包括权利要求1-7之一的磁性薄膜干涉器件的秘密文件，其中通过印刷或涂覆技术，或通过转移技术，优选通过热压印或冷压印，将磁性薄膜干涉器件施加到基片上。
13.一种薄膜干涉器件，例如箔或颜料，其包括含铁磁性材料的第一层，和含选自对光具有反射性能的材料的第二层，其中第一层的铁磁性质大于第二层的铁磁性质，其中第二层的反射性质大于第一层的反射性质。
14.根据权利要求1-7、10、和13之一的薄膜干涉器件，在通过其光学干涉性质和通过其磁性质来证实信息项中的应用。
15.根据权利要求14的应用，其中干涉器件是涂料组合物或涂料的一部分。
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| EP01105952A EP1239307A1 (en) | 2001-03-09 | 2001-03-09 | Magnetic thin film interference device |
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