EP1070273A1 - Lamelle couvre-objet adhesive et procede de microscopie - Google Patents

Lamelle couvre-objet adhesive et procede de microscopie

Info

Publication number
EP1070273A1
EP1070273A1 EP99919805A EP99919805A EP1070273A1 EP 1070273 A1 EP1070273 A1 EP 1070273A1 EP 99919805 A EP99919805 A EP 99919805A EP 99919805 A EP99919805 A EP 99919805A EP 1070273 A1 EP1070273 A1 EP 1070273A1
Authority
EP
European Patent Office
Prior art keywords
cover
optically transparent
specimen
slide
polymeric film
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.)
Withdrawn
Application number
EP99919805A
Other languages
German (de)
English (en)
Inventor
Michael Govek
Audrey S. Huang
Linda C. Chaffee
Michael L. Ruegsegger
Cynthia M. Hogerton
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
3M Innovative Properties Co
Original Assignee
3M Innovative Properties Co
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by 3M Innovative Properties Co filed Critical 3M Innovative Properties Co
Publication of EP1070273A1 publication Critical patent/EP1070273A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/36—Embedding or analogous mounting of samples
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00—Microscopes
    • G02B21/34—Microscope slides, e.g. mounting specimens on microscope slides
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/36—Embedding or analogous mounting of samples
    • G01N2001/364—Embedding or analogous mounting of samples using resins, epoxy

Definitions

  • the invention relates generally to the preparation of specimen slides for optical microscopy, and more specifically to a cover for covering the specimen mounted to the slide and a preparation method.
  • Solvent-based or melt-based sealing agents may be used to accomplish this.
  • Solvent-based or melt-based sealing agents may be used to accomplish this.
  • the solvent evaporates, the resin adheres the cover slip to the slide and protects the specimen.
  • This procedure has two disadvantages. Firstly, it takes some time for the solvent to evaporate completely and until that occurs the slide cannot be handled without risking damaging the visualization of the finished slide by smearing the resin.
  • cover slips of polymeric material which are less brittle than those made of glass.
  • cover slips of polymeric material which are less brittle than those made of glass.
  • cover slips of polymeric material which are less brittle than those made of glass.
  • a sealing agent as a coating on the roll material, which is then activated in the applying machine, or at the time the cover slip is applied to the slide, by the application of a solvent.
  • coverslips of this type are available from Sakura Finetek under the name Tissue-TekTM Coverslipping Film, and KP Tape available from Klinipath Corporation of Germany. However, it is still not possible to handle a slide prepared in this way immediately, and it remains rather difficult to remove such a cover slip when restaining of the specimen is required.
  • the invention provides a combination comprising a slide suitable for optical microscopy to which a specimen has been applied, and an optically transparent cover adhered to the slide over the specimen; wherein the cover comprises an optically transparent polymeric film with opposite first and second major surfaces, and a contact responsive adhesive on the first major surface which is in contact with the slide.
  • a low adhesion backsize is provided on the second major surface of the optically transparent film.
  • Regularly spaced grid lines are also preferably provided along the cover. The grid lines provide a convenient way to gauge the size of specimens or features of specimens.
  • the cover is sufficiently flexible to be capable of being supplied in a substantially continuous roll form.
  • the invention provides a method for preparation of an optical microscopy slide comprising: (a) placing a specimen on a slide; (b) covering the specimen with a cover comprising an optically transparent polymeric film having a contact responsive adhesive on a major surface thereof; and (c) adhering the contact responsive adhesive to the slide.
  • the method also preferably includes (1) providing covers in the form of a roll of a substantially continuous optically transparent polymeric film having a contact responsive adhesive on a major surface thereof; and (2) separating a cover from the roll before covering the specimen with a cover comprising an optically transparent polymeric film having a contact responsive adhesive on a major surface thereof.
  • a wetting agent can be applied to the cover or the specimen before the cover is adhered to the slide to improve viewing of the specimen.
  • Some compositions suitable for use as wetting agents include xylene, d- limonene, mineral oil, and ethanol.
  • Fig. 1 is a top view of a microscope slide with a specimen mounted thereon, sealed in place by a cover according to an embodiment of the present invention
  • Figure 2 is a cross-section side view of the microscope slide and cover of Figure 1 taken substantially along section lines 2-2;
  • Figure 3 is a cross-sectional view similar to figure 2 illustrating a second preferred embodiment of the invention.
  • microscope slide 10 is shown with specimen 12 mounted thereon.
  • specimen 12 is seen in this view through the transparent substance of cover 14.
  • Fig. 2 the same assembly is seen in cross-section side view, and more of the structural details can be made out.
  • the cover 14 comprises an optically transparent polymeric film 16 having a first side or major surface 18.
  • a layer of contact responsive adhesive 20 is provided on the first major surface 18 of the optically transparent polymeric film 16.
  • Figure 3 illustrates the cover 14 with an optional layer of an optically transparent scratch resistant coating 24 on a second, opposite side or major surface 22 of the optically transparent polymeric film 16.
  • an optional layer of a low adhesion backsize 26 which helps the cover 14 unroll easily if convenience for the user prompts the cover slip film being delivered as a roll of indefinite or substantially continuous length material.
  • the optically transparent scratch resistant coating can be any optically transparent hard coating known to be compatible and to bond to the optically transparent polymeric films. Many such materials are commercially available.
  • the refractive index of each of the components of the cover 14 are near the refractive index of the glass microscope slide 10.
  • Commercially available glass slides typically have a n D of approximately 1.51, and preferred materials for use in the cover have refractive indexes that approximate this value. Accordingly, preferred materials have refractive indexes of at least 1.45, and more preferably of at least 1.47. While materials having a refractive index as high as 1.65 are considered useful, materials with refractive indexes between about 1.47 and 1.55 are most preferred.
  • the luminous transmittance of light (measured according to ASTM Dl 003-95) through the cover should be maximized.
  • the cover should possess a luminous transmittance of at least about 85%, and more preferably at least about 94%. Accordingly, the luminous transmittance of cover components (e.g., optically transparent polymeric film) should be selected to maximize luminous transmittance and preferably the total transmittance of each component of the cover is at least 85%.
  • optically transparent polymeric film 16 it has been found that thicknesses of between about 100 to 250 microns give the best results. Thicknesses within this range provide good flexibility for use in roll form with automated application systems while maintaining sufficient strength for coating and handling of the film and cover. While many types of transparent polymeric films could be used, examples of films that are considered suitable include cellulose diacetate, cellulose triacetate, polyethylene terephthalate, styrene-acrylonitrile, and polymethyl methacrylate films. One particularly preferred material is film made from polymethyl methacrylate resin that is commercially available as V045-UVA10-100 from Atohaas Americas, Inc. of Philadelphia, Pennsylvania.
  • the polymeric film may be activated by a corona, plasma flame or actinic radiation treatment shortly before the application of the layer of contact responsive adhesive in order to improve the bonding between the polymeric film and the contact responsive adhesive. It is also considered to be within the scope of the invention to provide an intermediate or "tie" layer between the polymeric film and the contact responsive adhesive. The selection of an appropriate tie layer material will depend upon the type of contact responsive adhesive and optically transparent polymeric film used in the invention.
  • tie layers are useful in this invention, for example, chlorine-containing polymers like polyvinyl chloride, vinyl chloride/vinyl acetate copolymers, polyvinylidene chloride, polycarbodiimide and ethylene vinyl acetate polymers and copolymers, acid or anhydride-modified polyethylene, propylene and ethylene vinyl acetate polymers and copolymers may be used in the invention.
  • chlorine-containing polymers like polyvinyl chloride, vinyl chloride/vinyl acetate copolymers, polyvinylidene chloride, polycarbodiimide and ethylene vinyl acetate polymers and copolymers, acid or anhydride-modified polyethylene, propylene and ethylene vinyl acetate polymers and copolymers may be used in the invention.
  • the contact responsive adhesives useful in the invention are pressure sensitive adhesives that adhere relatively quickly and strongly to the target surface (i.e., slide specimen mounted thereon) yet exhibit essentially no surface tack to the skin when coated on the optically transparent polymeric film.
  • the contact responsive adhesives used in the invention bond to the target surface without need for solvent activation.
  • covers prepared with "solvent activated” adhesives will not substantially adhere to the target until the solvent used to dissolve and activate the adhesive is partially or completely evaporated.
  • substantially adhere means that the cover adheres strongly enough to the target to permit handling and use (e.g., viewing ) of the target.
  • a contact responsive adhesive used in the invention should immediately bond and be resistant to shear loading, such that dwell time prior to use of the target is unnecessary or so short it is relatively unnoticeable to the technician preparing the target.
  • the adhesive should not bond so aggressively to the target that it cannot be removed from the target without causing significance damage to the specimen.
  • the contact responsive adhesives coated on the optically transparent film will typically exhibit 180° peel adhesion values of between about 0.1 to 2.8 N/25 mm width, and preferably between about 0.2 to 1.4 N/25 mm width. (The 180° peel adhesion is measured according to the technique described in the Examples.) Adhesives that produce values higher than 2.8 N/25 mm width are generally too adherent to permit removal of the cover without some damage to the specimen. Adhesives that produce values less than 0.1 generally do not adhere sufficiently to the target to remain bonded during handling and storage of the target.
  • the contact responsive adhesive will not migrate from the cover to the target when the cover is separated from the target. Most preferably, the adhesive will not flow or creep during storage or block (i.e., form a permanent bond) to the target or to adjacent targets stored in close proximity.
  • the contact responsive adhesive when coated on the optically transparent polymeric film, demonstrates a dynamic shear strength to the target surface (as measured by the test described in WO94/21742) of greater than about 2 kN/m 2 , more preferably greater than about 4 kN/m 2 , and most preferably greater than 6 kN/m 2 at ambient temperature. In some cases, it may be necessary to adjust the coating weight/coating thickness to achieve the desired peel adhesion value.
  • Some of the adhesives useful in the invention may be crosslinked to increase their internal or cohesive strength and reduce peel values to a desired level. This is an especially useful technique to use when the contact responsive adhesive comprises BACN or BACNI polymers. Such crosslinking can also help prevent blocking and help maintain a relatively constant peel strength over time.
  • the contact responsive adhesive will substantially retain its advantageous balance of properties throughout extended storage periods. Accordingly, a technician can remove the cover from specimen slides prepared with adhesives, restain or otherwise rejuvenate the specimen, and adhere a new cover to the slide even after the slide has been stored for an extended period of time (e.g., 2 to 10 years).
  • Such preferred contact responsive adhesives will generally maintain a substantially constant 180° peel adhesion over a long time period (e.g., 5 to 10 years), and will not exhibit significant build-up of 180° peel adhesion over time. Because specimen slides are sometimes stored at relatively high humidity conditions, the preferred contact responsive adhesives will not become solvated, or undergo significant impairment of optical or adhesion properties after contact with water (e.g., up to 24 hours immersion at ambient temperature).
  • the contact responsive adhesive is also resistant to UV and oxidative degradation processes that lead to the discoloration of adhesives that impairs their optical properties.
  • Commonly available antioxidants and UV stabilizers can be added to the contact responsive adhesives to improve their optical and oxidative stability.
  • acrylonitrile copolymers (e.g., butadiene-acrylonitrile polymers (BACN polymers), butadiene-acrylonitrile-isoprene polymers (BACNI polymers)); styrene copolymers
  • tackifiers may be used, although they are generally only preferred for use in adhesives comprising styrene copolymers.
  • Detackifying agents also may be added, although they are less desirable as additives because many detackifying agents (e.g., talc) can impair the adhesive's optical properties.
  • detackifying agents will be removed from commercially available polymeric materials if they are present in sufficient amount to impair optical properties.
  • Plasticizers such as those commercially available under the trademark "Irganox” from Ciba Geigy as B561, 1010 and 1076, or from Shell Chemical Company as lonox 330, or from Bayer Leverkusen as Antioxidant ZKF
  • antioxidants e.g., organophosphites and phenolics such as those commercially available under the trademark "Irganox” from Ciba Geigy as B561, 1010 and 1076, or from Shell Chemical Company as lonox 330, or from Bayer Leverkusen as Antioxidant ZKF
  • UV stabilizers e.g., hindered amines and benzotriazoles such as those commercially available from Ciba Geigy as Tinuvin 292 and Tinuvin 328
  • the exact quantity of such materials may be varied to suit the desires of the compounder, provided that the resulting adhesive possesses the advantageous balance of bonding properties and necessary optical properties.
  • only antioxidants or UV stabilizers are combined with the polymeric materials to
  • acrylonitrile copolymers and adhesive formulations based on such polymers are described in the art, for example, U.S. Patent Nos. 5,196,266 and 5,316,849 describe a number of useful copolymers and adhesive formulations.
  • the aforementioned patents are incorporated herein by reference with respect to the polymers and adhesive compositions disclosed therein.
  • the acrylonitrile copolymers should contain less than about 24 wt. %, preferably less than about 20 wt. percent, and most preferably less than about 15 wt. % acrylonitrile units.
  • Particularly preferred among the class of acrylonitrile copolymers are the BACN polymers and BACNI polymers.
  • the BACN and BACNI polymers typically have about 24 to 50 wt. % acrylonitrile units and from about 2 to 20% by weight isoprene units. Preferably, such polymers contain about 20 to 50 wt. % and more preferably about 15 to 50 wt. % acrylonitrile units.
  • the BACN or BACNI polymer is compounded with a small amount of antioxidant (less than about 5 wt. % and preferably about 1 to 3 wt. % based on total polymer weight), UV stabilizer (less than about 3 wt. %, and preferably less than 0.5 wt. %, based on total polymer weight) before it is coated on the optically transparent film.
  • crosslinking agent is compounded with the polymers and other ingredients of the adhesive composition.
  • a small amount of 2-(4-methoxyphenyl)-4,6-bis(trichloromethyl)-l,3,5-triazine can be added to promote cross linking.
  • the coated film then can be exposed to an electron beam or high energy light source (such as Sylvania H33CO-400 boosted with a variable power source) until the desired degree of crosslinking is achieved.
  • the energy level required to crosslink the coating will, among other things, depend upon the coating thickness.
  • copolymers examples include polymers available under the trademarks of: "Nipol” and “Zetpol” from Zeon Chemicals Incorporated of Louisville, Kentucky (e.g., Nipol DN-4550 , Nipol DN-3380 , Nipol DN-3350 , Nipol DN-401L, Nipol DN-1201L, Zetpol 2000L, Zetpol 0020, Zetpol 1010, Zetpol 2010L and Zetpol ZSC 2095) ; "Hycar” from B.F. Goodrich Chemicals Inc. of Richfield, OH (e.g., Hycar 1022); and “Goodyear” from Goodyear Tire and Rubber Co. of Akron, OH (e.g., Goodyear N-206).
  • Nipol and “Zetpol” from Zeon Chemicals Incorporated of Louisville, Kentucky
  • Nipol DN-4550 e.g., Nipol DN-3380 , Nipol DN-3350 , Nipol DN-401L, Nipol DN-1201L,
  • Adhesive compositions comprising BACN and/or BACNI polymers are presently preferred.
  • Commercially available acrylonitrile copolymers may contain sufficient antioxidants, UV stabilizers and crosslinking agent to eliminate any need to compound the polymeric material with additional stabilizers and crosslinking agents.
  • Adhesives prepared using styrene copolymers are also useful in the invention.
  • such adhesives are prepared using styrene/butadiene/styrene block copolymers (SBS polymers), styrene/isoprene/styrene block copolymers (SIS polymers) or styrene/ethylene/butylene/styrene block copolymers (SEBS polymers).
  • SBS polymers styrene/butadiene/styrene block copolymers
  • SIS polymers styrene/isoprene/styrene block copolymers
  • SEBS polymers styrene/ethylene/butylene/styrene block copolymers
  • compositions based on SEBS or SI block copolymers preferably have a composite mid-block glass transition (CMTg) of about 225 to 240° Kelvin.
  • compositions based on SBS copolymers preferably have a CMTg of about 215 to 235° Kelvin.
  • adhesion properties of these compositions can be varied by varying the styrene content of the composition (by selection of copolymer and varying the copolymer content of the composition) and the CMTg of the composition, one can vary the types and amounts of components to secure appropriate 180° adhesion values for the contact responsive adhesive.
  • compositions which have copolymer content near the higher end of the range i.e., 50 to 80 parts by weight
  • a CMTg near the higher end of the range or that even exceeds the range i.e., 240° Kelvin + 10° K or 235°K + 10°K
  • compositions which contain an amount of copolymer that is at the lower end of the range (i.e., 20 to 45 parts by weight) and a CMTg at the lower end of the range (i.e., 225°K + 10°K or 215°K + 10°K) have a good balance and adhesion properties for this application.
  • Compositions with copolymer content at the higher end of the range, but a CMTg at the lower end of the range also generally have a good balance of adhesion properties for this application.
  • compositions with a copolymer content at the lower end of the range and a CMTg at the higher end of the range or slightly exceeding it will be too tacky for this application.
  • compositions may be able to be slightly reformulated (e.g., by reducing the content of tackifier resin or increasing the composition's styrene content) to adjust tackiness to an acceptable level.
  • SEBS copolymers are the preferred styrene copolymers for use in this invention because they are colorless or nearly colorless, and have good long-term age stability with respect to discoloration of an adhesive.
  • tackifier resins made from the polymerization of a feed stream consisting mainly of unsaturated species containing four to six carbon atoms such as "Wingtack” 10, “Wingtack Plus” and Wingtack” 95 available from the Goodyear Tire and Rubber Company, "Escorez” 1310, available from Exxon
  • Preferred tackifying resins include the aliphatic hydrocarbon resins, the hydrogenated resins and the polyterpene resins. Especially preferred are the hydrogenated aliphatic and the hydrogenated aliphatic/aromatic hydrocarbon resins.
  • the liquid plasticizer oils suitable for use in the adhesive of the invention include naphthenic oils such as "Shellflex” 371, available from Shell Chemical Co., paraffinic oils, aromatic oils, and mineral oils such as "Kaydol” oil, available from Witco Chemical Corp.
  • Preferred liquid plasticizers include naphthenic oil and mineral oil. Additionally, small amounts of antioxidants and UV stabilizers are advantageously compounded into the composition prior to coating of the adhesive composition.
  • examples of commercially available styrene copolymers useful in the invention include: SIS copolymers sold under the trademark "Kraton” by Shell Chemical Company, such as 1107 and 1111, those sold under the trademark "Enichem” by Enichem U.S.A.
  • SEBS copolymers such as SOL T, those sold under the trademark “Quintac” by Nippon-Zeon such as 3430 and 3530, those sold under the trademark “Finaprene” by Fina Chemical Company such as 424; SBS copolymers such as “Kraton” 1101 and “Kraton” 1102, those sold under the trademark “Stereon” by Firestone Synthetic Latex and Rubber Company such as 840 A, “Enichem” Sol T 1205 and “Enichem” Sol T 161 C; and SEBS copolymers “Kraton” 1657, “Kraton” 1654X, “Kraton” 1652, “Kraton” 1651, and “Kraton” 1650. Especially preferred are the SEBS copolymers.
  • Suitable acrylate copolymer adhesives for use in this invention include those comprising units derived from about 20 to 100 wt. % of a mixture of (a) at least about 20 to 50 wt. % of an acrylate ester of a C 4 to C 12 alcohol, wherein a homopolymer of the acrylate ester would have a glass transition temperature (Tg) less than about -50°C; (b) about 0 to 50 wt.
  • Tg glass transition temperature
  • Such copolymers may also contain additional units derived from, for example, chain transfer agents, acrylamide functional disubstituted acetyl aryl ketone photoinitiator and so forth depending upon the method used to polymerize the copolymer.
  • Representative examples of monomers of type (a) include: n-butyl acrylate, 2-ethylhexyl acrylate, isooctyl acrylate and isononyl acrylate.
  • monomers of type (b) include ethyl acrylate and phenoxyethyl acrylate.
  • Representative examples of monomers of type (c) include isobornyl acrylate or N-vinyl caprolactum.
  • the acrylate copolymers can be made according to various known methods. Examples of useful methods are described in U.S. Patent Nos. 5,654,387, 5,728,786, 5,616,670, 5,202,361, 5,840,783, 5,648,425, and 5,506,279, which descriptions regarding polymerization are incorporated by reference herein.
  • the 180° peel adhesion of such adhesives can be further modified through crosslinking (to increase internal cohesiveness) and additives such as plasticizers. Detackifiers should be avoided when their use would impair the optical properties of the adhesive.
  • covers according to the invention may be provided pre-cut to a size suitable for use, it is also possible to deliver the cover in the form of a roll of indefinite length material for automated application. When this is done, an optional low adhesion backsize is presently contemplated to be desirable to minimize the force needed to unwind the roll.
  • Coatings useful in preparing low adhesion backsizes are known in the art.
  • particularly preferred materials include coatings comprising urethane, acrylic, silicone and fluorocarbon polymers and many such coatings are commercially available.
  • suitable coatings include 100% solids, UV cured, platinum catalyzed silicone system known as "6200" or "8000" silicone series from DCP-Lohja of Westchester, IL.
  • a release liner may be provided to minimize the force needed to unwind the film.
  • a polyester release liner prepared with the above platinum catalyzed silicone layer, commercially available from DCP-Lohja of Westchester, IL is currently considered suitable.
  • the contact responsive adhesive composition can be coated on the optically transparent polymeric film using conventional techniques, such as solvent coating by methods such as reverse roll, knife-over-roll, gravure, wire wound rod, floating knife or air knife, hot-melt coating such as by slot orifice coaters, roll coaters or extrusion coaters, at appropriate coating weights.
  • a UV activated initiator may be included and the monomer mixture may be partially cured by UV exposure into a viscous liquid. This viscous liquid can be coated out by any conventional technique.
  • U.S. Patent No. 5,230,701 (Meyer et al.), which is herein incorporated by reference, discloses suitable adhesive coating methods.
  • the adhesive may be first coated on a liner material, using one of the aforementioned techniques, and then laminated to the optically transparent film (e.g., using a roller to apply pressure) to form the cover.
  • the liner can then be used as a carrier for the cover or it can be removed.
  • the adhesive composition can be subjected to a cure step after coating (e.g., by UV radiation or electron beam radiation) to crosslink the coating.
  • adhesive coatings of about 13 to 51 microns are used in this invention. It may be desirable to print indicia on the cover slip film, especially in the form of grid lines with a predetermined spacing. This permits the viewer of the specimen to gauge the size of the specimen, or to count objects within an area.
  • 180° Peel adhesion was measured essentially according to ASTM D3330 using a model SP101B testing machine with type SPM-04 modifications (commercially available from IMASS of Hingham, MA), except that a glass target surface and peel rate of 229 cm/min were used.
  • the refractive index was measured using an ABBE-3L refractometer (Bausch & Lomb, Rochester, NY) or a Metricon Model 2010 Prism Coupler (Metricon, Pennington,
  • a contact responsive adhesive formulation was prepared by placing 30.2 liters of methylethylketone into a 38 liter Ross mixer and stirring at 20 rpm using only paddles. While stirring, 8.2 kilograms BACNI polymer (Nipol DN 1201L from Zeon Chemicals of Louisville, KY) was added in approximately l A kilogram blocks. At 24 and 48 hours the mixing paddles were raised and clumps of the polymer attached to the paddles were knocked off. The mixture was stirred for a total of 76 hours at approximately 23°C. The adhesive was then coated onto a release liner using a knife coater with a 356 micron wet gap. The coated construction was dried at 65°C to obtain a 50 micron coating.
  • the release liner was a 35 micron thick polyester terephthalate film coated on one side with a silicone release coating and coated on the other side with an anti-blocking agent.
  • the release liner coated with adhesive was then fabricated into a cover tape by laminating the adhesive-coated release liner onto a 76 micron thick, oriented polymethylmethacrylate film. Orientation was imparted to the film by stretching the film 2.25 times in the machine direction and 2.3 times in the cross direction.
  • the refractive index of the adhesive was measured and found to be 1.515.
  • the 180° peel adhesion of the cover to glass was found to be 0.28 N/25 mm width, an acceptable value for the invention.
  • Test strips were prepared from the cover tape by cutting pieces of 20 cm x 2.54 cm in size. These pieces were hand laminated to glass plates using a 3.8 cm diameter rubber hand roller and glass. In some of the examples, a wetting agent was applied to the glass plate at the rate of two drops per 3 cm of tape length before lamination. The 180° peel adhesion of the laminates was then measured both initially, and at various times after lamination for two wetting agents. The 180° peel adhesion data, and wetting agents are presented in Table 1.
  • wetting agents can lower the initial 180° adhesion values. However, they rapidly improve over time. As will be described later, the cover demonstrates excellent initial resistance to shear loads. This indicates even when wetting agents are used. Accordingly, even though the initial peel adhesion may not immediately be optimum, slides with the cover can be handled immediately. The specimens were inspected by eye with a microscope under high magnification, and the subjective image quality was found to be excellent.
  • test strips were prepared from the cover tape in order to test the resistance of a cover to a shear load when a wetting agent is used. Additional 24 mm x about 75 mm test strips were prepared and hand mounted onto glass microscope slides containing three drops of a wetting agent. The slides were then over-rolled with a 2.0 kg rubber roller and allowed to dwell for a specified period. The resistance of the cover-slide bond to a shear load was evaluated by measuring the ease with which the cover could be displaced along the slide by first supporting the slide with the thumb on the side carrying the cover and four fingers on the opposite side and then applying a shear force with the thumb,
  • the luminous transmittance and haze of the cover was measured.
  • the method described in ASTM D 1003-95 was used to measure transmittance and haze.
  • Haze- GuardTM Optical Tester (available from B YK-Gardner USA of Silver Spring, MD) was used to carry out the measurements.
  • the % luminous transmittance was 94.8%>, the haze was 2.32%, and the clarity was 99.6%.
  • Example 2 This example illustrates the preparation of an optically transparent film with a scratch- resistant coating.
  • a 0.5 m length of 6 inch wide PMMA film was coated with a hydantoin hexacrylate solution (20% in toluene), containing Irgacure® 1173, commercially available from Ciba Specialty Chemicals of Tarrytown, NY) in an amount of 4 parts by weight to 100 parts of hydantoin hexacrylate.
  • the scratch-resistant coating was done in a drawdown fashion with a #7 Meyer rod.
  • the coating was allowed to dry and was UV cured under a F300 lamp (from Fusion UV Systems of Gaithersberg, MD), at 50 fpm. Coating thickness was about 2.5 microns.
  • Example 3 This example illustrates the preparation of another optically transparent film with a scratch-resistant coating.
  • a 0.5 m length of PMMA film 15 cm wide was coated with Gafgard® 233, commercially available from International Specialty Products of Wayne NJ, mixed with Esacure KB1, commercially available from Sartomer of Exton, PA, in an amount of 4 parts by weight to 100 parts of the monomer. Coating was done in a drawdown fashion with a #3 Meyer rod. The coating was UV cured under a F300 lamp at 100 fpm. Coating thickness was measured as about 9 microns.
  • the coating adhesion to the substrate was tested according to ASTM D3359 resulting in a value of 5.
  • the coating was tested for hardness according to ASTM D3363, resulting in a 3h hardness rating.
  • This example illustrates the preparation of a coverslip film comprising a contact responsive adhesive containing ultraviolet light stabilizers.
  • the adhesive was prepared using a similar procedure to that described in Example 1 except that 0.29 grams of Tinuvin 292 (Ciba Specialty Chemicals) was added to 79.1 grams of the adhesive composition prepared in Example 1. The resulting mixture was stirred until uniform.
  • a cover tape was prepared using a procedure similar to that described in Example 1 except that the new adhesive composition was used and the coating thickness was 71 microns. The refractive index of the tape was 1.514 and the 180° peel adhesion of this coverslip tape to glass was 1.45 N/25 mm wide.
  • a stabilized contact responsive adhesive composition was prepared by adding 0.21 grams of Tinuvin 292 and 0.578 grams of Tinuvin 328 (both commercially available from Ciba Specialty Chemicals) to 87.16 grams of the adhesive of Example 1. Once again, the mixture was stirred until uniform. The resulting composition was used to prepare a cover tape using a procedure similar to that described in Example 1 except that the new adhesive
  • the refractive index of the adhesive was 1.5169 and the 180° peel test value of the cover tape to glass was 0.70 N/25 mm wide.
  • the resulting solutions were coated directly onto 76 micron thick polyester terephthalate films using a knife coater with a 259 micron wet gap. The coated constructions were dried at 65°C.
  • Example 6 and Comparative Example Cl and Example 8 and Comparative Example C2 have similar amounts of copolymer and similar CMTgs.
  • the 180° peel adhesion in the composition of Comparative Example Cl are unacceptable for this application.
  • the 180° peel adhesion probably could be improved to an acceptable level by increasing the copolymer content or decreasing the amount of tackifier resin.
  • Examples 10 to 12 and Comparative Example C-4 Adhesive formulations were prepared by solvating a BACN polymer in methylethylketone solvent. This adhesive solution was prepared at 25 wt% solids and coated onto a release liner 50 micron thick polyester terephthalate film coated on both sides with a silicone release coat using a knife coater with a 127 micron wet gap. The coated construction was dried at 65°C and the coated release liner was laminated to a 76 micron thick, oriented polymethylmethacrylate film (orientation was imparted by stretching the film 2.25 times in the machine direction and 2.3 times in the cross direction).
  • the acrylonitrile copolymer, % acrylonitrile monomer in the copolymer, Mooney viscosity of the copolymer, refractor index of the adhesive compound, total transmittance, haze, clarity, coating thickness and 180° peel adhesion values are presented in Table 4.
  • Example BACN 1 Viscosity Index (%) (%) (%) (%) (microns) (N/25 mm width)
  • This mixture was knife coated between two layers of 51 micron thick poly(ethylene terephthalate) (PET) film that were coated with premium silicone release coatings. Coating calipers were about 51 microns. The coating was exposed to a bank of blacklight bulbs with an intensity of 2.0 mW/cm 2 for about 5.0 minutes providing an irradiated dose of about 556 mJ/cm 2 .
  • the described procedure is similar to some of the Examples (particularly Example 9) of U.S. Patent No. 5,506,279, which is hereby incorporated by reference.
  • 180° peel adhesion of the sample measured again at a peel rate of 30 cm min.
  • 180° peel adhesion value was 5.6 N/25 mm width and the sample adhered very strongly to the slide.

Landscapes

  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Optics & Photonics (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Adhesive Tapes (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Microscoopes, Condenser (AREA)

Abstract

L'invention concerne une combinaison comprenant une lamelle conçue pour la microscopie optique sur laquelle est déposé un échantillon et un couvre-objet optiquement transparent collé à la lamelle reposant sur l'échantillon. Ledit couvre-objet comprend un film polymère optiquement transparent ayant des première et seconde surfaces principales opposées et un adhésif sensible au contact enduit sur la première surface principale et en contact avec la lamelle.
EP99919805A 1998-04-09 1999-04-09 Lamelle couvre-objet adhesive et procede de microscopie Withdrawn EP1070273A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US8115998P 1998-04-09 1998-04-09
US81159P 1998-04-09
PCT/US1999/007800 WO1999053357A1 (fr) 1998-04-09 1999-04-09 Lamelle couvre-objet adhesive et procede de microscopie

Publications (1)

Publication Number Publication Date
EP1070273A1 true EP1070273A1 (fr) 2001-01-24

Family

ID=22162464

Family Applications (1)

Application Number Title Priority Date Filing Date
EP99919805A Withdrawn EP1070273A1 (fr) 1998-04-09 1999-04-09 Lamelle couvre-objet adhesive et procede de microscopie

Country Status (4)

Country Link
EP (1) EP1070273A1 (fr)
JP (1) JP2002511600A (fr)
AU (1) AU3744299A (fr)
WO (1) WO1999053357A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102015008336A1 (de) 2015-06-23 2016-12-29 Island Polymer Industries Gmbh Hochtransparente beschichtete Cellulosetriacetatfolie und Anlösemedium
CN111057446A (zh) * 2019-12-31 2020-04-24 嘉兴晶铸生物科技有限公司 一种uvled固化载玻片封固方法

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7351470B2 (en) 1998-02-19 2008-04-01 3M Innovative Properties Company Removable antireflection film
US6800378B2 (en) 1998-02-19 2004-10-05 3M Innovative Properties Company Antireflection films for use with displays
US6589650B1 (en) * 2000-08-07 2003-07-08 3M Innovative Properties Company Microscope cover slip materials
DE19952139C1 (de) * 1999-10-28 2000-12-21 Sibyll Weiner Transparenter Objektträger für die optische Mikroskopie
JP2002303707A (ja) * 2001-02-02 2002-10-18 Three M Innovative Properties Co 光学フィルタ及びタッチパネル型ディスプレー用フィルター
EP1425352B1 (fr) 2001-09-11 2005-01-12 3M Innovative Properties Company Revetements durs nanocomposites resistant aux taches et procedes de fabrication
US7468161B2 (en) * 2002-04-15 2008-12-23 Ventana Medical Systems, Inc. Automated high volume slide processing system
US11249095B2 (en) 2002-04-15 2022-02-15 Ventana Medical Systems, Inc. Automated high volume slide processing system
US20050094263A1 (en) * 2003-10-31 2005-05-05 Vincent Vaccarelli Microscope slide designed for educational purposes
WO2005085799A1 (fr) * 2004-03-04 2005-09-15 Merck Patent Gmbh Moyen pour recouvrir des preparations microscopiques
EP2356423B1 (fr) 2008-11-12 2024-08-07 Ventana Medical Systems, Inc. Procédés et appareils permettant de chauffer des lames portant des échantillons
IT1392180B1 (it) * 2008-12-11 2012-02-22 Bouty Spa Un sistema matriciale auto-adesivo comprendente un copolimero a blocchi stirenico
DE102009020663A1 (de) * 2009-05-11 2010-11-25 Carl Zeiss Ag Mikroskopie eines Objektes mit einer Abfolge von optischer Mikroskopie und Teilchenstrahlmikroskopie
GB2482726A (en) * 2010-08-13 2012-02-15 Invicta Plastics Ltd Specimen slide for microscope
JP2013185920A (ja) * 2012-03-07 2013-09-19 Pathology Institute 組織アレイシートの製造方法およびその製造装置
WO2014071959A1 (fr) 2012-11-07 2014-05-15 Morgan Adhesives Company Matériaux pour lamelles de microscopie
DE102013105220B3 (de) * 2013-05-22 2013-12-24 Leica Biosystems Nussloch Gmbh Vorrichtung zur Handhabung von Objektträgern mit wahlweise aufnehmbaren Glas- oder Tape-Eindeckmodulen
CN106053165A (zh) * 2016-05-16 2016-10-26 常州大学 一种观察痰液黏蛋白微观结构的光学新方法
JP2018010093A (ja) * 2016-07-12 2018-01-18 一般社団法人白亜会 プレパラート作製キット
JP7092294B2 (ja) * 2017-12-13 2022-06-28 学校法人東海大学 超薄膜から成る生体組織被覆用材料、及びそれで被覆された生体組織
CN109943239B (zh) * 2017-12-21 2021-02-19 哈尔滨格林标本技术开发有限公司 一种无毒组织切片封片胶的制备方法
WO2021187262A1 (fr) * 2020-03-16 2021-09-23 富士フイルム株式会社 Film de recouvrement
WO2024176739A1 (fr) * 2023-02-21 2024-08-29 富士フイルム株式会社 Film de recouvrement

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH400607A (de) * 1962-12-27 1965-10-15 Merz & Dade Ag Objektträger mit Deckelement für mikroskopische Untersuchung
US4077830A (en) * 1974-09-09 1978-03-07 Tapecon, Inc. Laminate and method for protecting photographic element
US4203797A (en) * 1977-05-09 1980-05-20 Cytologiska Centrallaboratoriet Ab Method of and apparatus for applying cover-slips to slides carrying specimens for microscopic examination
FR2542876A1 (fr) * 1983-03-14 1984-09-21 Jouet Cie Gle Complexe pour la realisation d'une plaquette d'examen microscopique
JPS6238408A (ja) * 1985-08-13 1987-02-19 Fuji Photo Film Co Ltd 顕微鏡用カバ−フイルム
US5812312A (en) * 1997-09-04 1998-09-22 Lorincz; Andrew Endre Microscope slide

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9953357A1 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102015008336A1 (de) 2015-06-23 2016-12-29 Island Polymer Industries Gmbh Hochtransparente beschichtete Cellulosetriacetatfolie und Anlösemedium
WO2016206672A1 (fr) 2015-06-23 2016-12-29 Island Polymer Industries Gmbh Film de triacétate de cellulose revêtu à haute transparence et solvant
CN111057446A (zh) * 2019-12-31 2020-04-24 嘉兴晶铸生物科技有限公司 一种uvled固化载玻片封固方法

Also Published As

Publication number Publication date
JP2002511600A (ja) 2002-04-16
AU3744299A (en) 1999-11-01
WO1999053357A1 (fr) 1999-10-21

Similar Documents

Publication Publication Date Title
WO1999053357A1 (fr) Lamelle couvre-objet adhesive et procede de microscopie
US6402875B1 (en) Repeated use of an adhesive-film laminate
EP0704509B1 (fr) Composition adhésive sensible à la pression et feuilles adhésives utilisant cette composition
US6063838A (en) Blended pressure-sensitive adhesives
JP5179491B2 (ja) 光学補償されたアクリル系粘着剤組成物、これを含む偏光板及び液晶表示素子
US6630238B2 (en) Blended pressure-sensitive adhesives
US6632522B1 (en) Blended pressure-sensitive adhesives
CA2042065C (fr) Adhesif sensible a la pression contenant un agent collant
WO2002012857A1 (fr) Lamelle couvre-objets pour microscope
WO2008057488A2 (fr) Adhésifs thermofusibles acryliques
WO2007061242A1 (fr) Composition d'adhesif autocollant acrylique
CN107109166B (zh) 具有低酸含量的增粘丙烯酸酯压敏粘合剂
KR19990023969A (ko) 압감성 접착제 조성물 및 이 조성물로 제조된 압감성 접착제를 사용한 압감성 접착 시이트
WO1997023577A1 (fr) Adhesifs melanges adherant sous l'effet d'une pression
CA2101629A1 (fr) Compositions adhesives autocollantes, specifiques pour l'intervalle de temperature; materiel adhesif et methodes d'utilisation
JP2010189545A (ja) 両面粘着シートおよび粘着型光学部材
JPH0356598B2 (fr)
JP2017181546A (ja) 偏光フィルム、粘着剤層付偏光フィルム、偏光フィルムの製造方法、及び画像表示装置
JPH0519684B2 (fr)
JP2005115028A (ja) 粘着剤層と偏光板又は位相差板からなる積層体
JPH01146977A (ja) 粘着剤
KR20200087806A (ko) 레이저 절단 접착제를 위한 이형 라이너
US5028485A (en) Pressure sensitive adhesive composition
JP2002214439A (ja) 粘着型光学フィルム
JP2017122210A (ja) 接着テープ及びその使用

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20000927

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): DE GB IT

17Q First examination report despatched

Effective date: 20010206

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION HAS BEEN WITHDRAWN

18W Application withdrawn

Effective date: 20030129